Sample records for amberlite xad-7 resin

  1. Re-evaluation of solid-phase adsorption and desorption techniques for isolation of trace organic pollutants from chlorinated water.

    PubMed

    Onodera, S; Nagatsuka, A; Rokuhara, T; Asakura, T; Hirayama, N; Suzuki, S

    1993-07-16

    Amberlite XAD resin and activated carbon columns were tested for their abilities to concentrate trace organic pollutants in chlorinated water. Both XAD-2 and XAD-7 resin columns (20 ml) were capable of adsorbing about 30% of total organic halogen (TOX) present in 20 l of drinking water (pH 7) containing about 100 micrograms/l of TOX, whereas the carbon column (10 ml) adsorbed over 90% of TOX. The adsorption capacity of XAD-7 resin was found to be strongly dependent on the solution pH, as compared with those of XAD-2 and carbon adsorbents. Soxhlet and sonication extractions were also evaluated for their abilities to recover the adsorbed organics from the adsorbents, by measurements of TOX, chromatographable compounds and mutagenicity in the eluates. Soxhlet extraction gave higher recoveries than sonication, as measured with the above indices, but these differences were generally small (ca. 20%), with exception of the carbon extracts. The XAD-2 and XAD-7 extracts of drinking water also showed about 3-4 times higher mutagenic activity than the carbon extracts.

  2. Isolation of organic acids from large volumes of water by adsorption on macroporous resins

    USGS Publications Warehouse

    Aiken, George R.; Suffet, I.H.; Malaiyandi, Murugan

    1987-01-01

    Adsorption on synthetic macroporous resins, such as the Amberlite XAD series and Duolite A-7, is routinely used to isolate and concentrate organic acids from forge volumes of water. Samples as large as 24,500 L have been processed on site by using these resins. Two established extraction schemes using XAD-8 and Duolite A-7 resins are described. The choice of the appropriate resin and extraction scheme is dependent on the organic solutes of interest. The factors that affect resin performance, selectivity, and capacity for a particular solute are solution pH, resin surface area and pore size, and resin composition. The logistical problems of sample handling, filtration, and preservation are also discussed.

  3. Determination of trace heavy metals in soil and sediments by atomic spectrometry following preconcentration with Schiff bases on Amberlite XAD-4.

    PubMed

    Kara, Derya; Fisher, Andrew; Hill, Steve J

    2009-06-15

    A matrix separation and analyte preconcentration system using Amberlite XAD copolymer resins functionalized by Schiff base reactions coupled with atomic spectrometry has been developed. Three different functionalized Amberlite XAD resins were synthesized using 4-phenylthiosemicarbazide, 2,3-dihydroxybenzaldehyde and 2-thiophenecarboxaldehyde as reagents. These resins could be used to preconcentrate transition and other trace heavy metal analytes from nitric acid digests of soil and sediment samples. Analyte retention was shown to work well at pH 6.0. After treatment of the digests with sodium fluoride and buffering to pH 6, samples that contain extremely large concentrations of iron were analysed for trace analytes without the excess iron overloading the capacity of the resin. The analytes Cd, Co, Cu, Ni and Pb were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with 0.1M HNO(3) directly to the detection system. Flame atomic absorption spectrometry was used as a means of detection during the studies. The efficiency of the chelating resin and the accuracy of the proposed method were evaluated by the analysis of soil (SO-2) and sediment (LGC 6157 and MESS-3) certified reference materials.

  4. Isolation of hydrophilic organic acids from water using nonionic macroporous resins

    USGS Publications Warehouse

    Aiken, G.R.; McKnight, Diane M.; Thorn, K.A.; Thurman, E.M.

    1992-01-01

    A method has been developed for the isolation of hydrophilic organic acids from aquatic environments using Amberlite* * Use of trade names in this report is for identification purposes only and does not constitute endorsement by the U.S. Geological Survey. XAD-4 resin. The method uses a two column array of XAD-8 and XAD-4 resins in series. The hydrophobic organic acids, composed primarily of aquatic fulvic acid, are removed from the sample on XAD-8, followed by the isolation of the more hydrophilic organic acids on XAD-4. For samples from a number of diverse environments, more of the dissolved organic carbon was isolated on the XAD-8 resin (23-58%) than on the XAD-4 resin (7-25%). For these samples, the hydrophilic acids have lower carbon and hydrogen contents, higher oxygen and nitrogen contents, and are lower in molecular weight than the corresponding fulvic acids. 13C NMR analyses indicate that the hydrophilic acids have a lower concentration of aromatic carbon and greater heteroaliphatic, ketone and carboxyl content than the fulvic acid. ?? 1992.

  5. EVALUATION OF METHODS FOR THE ISOLATION OR CONCENTRATION OF ORGANIC SUBSTANCES FROM WATER USING XAD-4 QUATERNARY RESIN

    EPA Science Inventory

    A synthetic resin (Amberlite XAD-4 Quaternary in the OH- form) was evaluated as an adsorption medium for the concentration/isolation of acids, amines, aldehydes, carbohydrates, chlorobiphenyls, esters, hydrocarbons, ketones, phenols, polynuclear aromatic hydrocarbons, and trihalo...

  6. Equilibrium and heat of adsorption of diethyl phthalate on heterogeneous adsorbents.

    PubMed

    Zhang, Weiming; Xu, Zhengwen; Pan, Bingcai; Hong, Changhong; Jia, Kun; Jiang, Peijuan; Zhang, Qingjian; Pan, Bingjun

    2008-09-01

    Removal of phthalate esters from water has been of considerable concern recently. In the present study, the adsorptive removal performance of diethyl phthalate (DEP) from water was investigated with the aminated polystyrene resin (NDA-101) and oxidized polystyrene resin (NDA-702). In addition, the commercial homogeneous polystyrene resin (XAD-4) and acrylic ester resin (Amberlite XAD-7) as well as coal-based granular activated carbon (AC-750) were chosen for comparison. The corresponding equilibrium isotherms are well described by the Freundlich equation and the adsorption capacities for DEP followed the order NDA-702 > NDA-101 > AC-750 > XAD-4 > XAD-7. Analysis of adsorption mechanisms suggested that these adsorbents spontaneously adsorb DEP molecules driven mainly by enthalpy change, and the adsorption process was derived by multiple adsorbent-adsorbate interactions such as hydrogen bonding, pi-pi stacking, and micropore filling. The information related to the adsorbent surface heterogeneity and the adsorbate-adsorbate interaction was obtained by Do's model. All the results indicate that heterogeneous resins NDA-702 and NDA-101 have excellent potential as an adsorption material for the removal of DEP from the contaminated water.

  7. Comparison of humic substances isolated from peatbog water by sorption on DEAE-cellulose and amberlite XAD-2

    USGS Publications Warehouse

    Hejzlar, J.; Szpakowska, B.; Wershaw, R. L.

    1994-01-01

    Aquatic humic substances (AHS) were isolated from peatbog water by adsorption (1) on diethylaminoethyl cellulose (DEAE-C) and (2) on Amberlite XAD-2 (XAD) to compare yields of the methods and the composition of the isolated AHS. To provide a detailed comparison, the isolates were fractionated using size-exclusion and hydrophobic-interaction chromatography on Sephadex G-50. The fractions were characterized by ultraviolet-visible, infrared and 13C-nuclear magnetic spectroscopies and analyzed for elemental, functional-group, carbohydrate and amino acid compositions. More AHS adsorbed onto DEAE-C than onto XAD-2 (94 and 74%, respectively). However, only 76% of the AHS adsorbed onto DEAE-C was recovered using 0.1 M NaOH, whereas 98% of the AHS adsorbed onto XAD was released by consecutive elution with 1 M NH4OH (91%) and methanol (7%). Four main fractions of different composition were obtained from each of the alkali-desorbed AHS samples by Sephadex-gel chromatography. General agreement was found in relative amounts, spectroscopic characteristics and composition of corresponding fractions of both isolates except nitrogen content, which was significantly higher in AHS isolated with XAD, apparently due to the reaction of AHS with NH4OH used for the desorption from the resin.Aquatic humic substances (AHS) were isolated from peatbog water by adsorption (1) on diethylaminoethyl cellulose (DEAE-C) and (2) on Amberlite XAD-2 (XAD) to compare yields of the methods and the composition of the isolated AHS. To provide a detailed comparison, the isolates were fractionated using size-exclusion and hydrophobic-interaction chromatography on Sephadex G-50. The fractions were characterized by ultraviolet-visible, infrared and 13C-nuclear magnetic spectroscopies and analyzed for elemental, functional-group, carbohydrate and amino acid compositions. More AHS adsorbed onto DEAE-C than onto XAD-2 (94 and 74%, respectively). However, only 76% of the AHS adsorbed onto DEAE-C was recovered using 0.1 M NaOH, whereas 98% of the AHS adsorbed onto XAD was released by consecutive elution with 1 M NH4OH (91%) and methanol (7%). Four main fractions of different composition were obtained from each of the alkali-desorbed AHS samples by Sephadex-gel chromatography. General agreement was found in relative amounts, spectroscopic characteristics and composition of corresponding fractions of both isolates except nitrogen content, which was significantly higher in AHS isolated with XAD, apparently due to the reaction of AHS with NH4OH used for the desorption from the resin.

  8. Simultaneous spectrophotometric determination of trace amounts of uranium, thorium, and zirconium using the partial least squares method after their preconcentration by alpha-benzoin oxime modified Amberlite XAD-2000 resin.

    PubMed

    Ghasemi, Jahan B; Zolfonoun, E

    2010-01-15

    A new solid phase extraction method for separation and preconcentration of trace amounts of uranium, thorium, and zirconium in water samples is proposed. The procedure is based on the adsorption of U(VI), Th(IV) and Zr(IV) ions on a column of Amberlite XAD-2000 resin loaded with alpha-benzoin oxime prior to their simultaneous spectrophotometric determination with Arsenazo III using orthogonal signal correction partial least squares method. The enrichment factor for preconcentration of uranium, thorium, and zirconium was found to be 100. The detection limits for U(VI), Th(IV) and Zr(IV) were 0.50, 0.54, and 0.48microgL(-1), respectively. The precision of the method, evaluated as the relative standard deviation obtained by analyzing a series of 10 replicates, was below 4% for all elements. The practical applicability of the developed sorbent was examined using synthetic seawater, natural waters and ceramic samples.

  9. Flame Atomic Absorption Spectrometric Determination of Trace Metal Ions in Environmental and Biological Samples After Preconcentration on a Newly Developed Amberlite XAD-16 Chelating Resin Containing p-Aminobenzene Sulfonic Acid.

    PubMed

    Islam, Aminul; Ahmad, Akil; Laskar, Mohammad Asaduddin

    2015-01-01

    Amberlite® XAD-16 was functionalized with p-aminobenzene sulfonic acid via an azo spacer in order to prepare a new chelating resin, which was then characterized by water regain value, hydrogen ion capacity, elemental analyses, and IR spectral and thermal studies. The maximum uptake of Cu(II), Ni(II), Zn(II), Co(II), Cr(III), Fe(III), and Pb(II) ions was observed in the pH range 4.0-6.0 with the corresponding half-loading times of 6.5, 7.0, 8.0, 9.0, 11.0, 8.5, and 16.5 min. The sorption data followed Langmuir isotherms and a pseudo-second-order model. Thermodynamic quantities, ΔH and ΔS, based on the variation of the distribution coefficient with temperature were also evaluated. High preconcentration factors of 60-100 up to a low preconcentration limit of 4.0-6.6 μg/L have been achieved for the metal ions. The validity of the method was checked by analyzing standard reference materials and recoveries of trace metals after spiking. The analytical applications of the method were explored by analyzing natural water, mango pulp, mint leaves, and fish.

  10. Selective adsorption of flavor-active components on hydrophobic resins.

    PubMed

    Saffarionpour, Shima; Sevillano, David Mendez; Van der Wielen, Luuk A M; Noordman, T Reinoud; Brouwer, Eric; Ottens, Marcel

    2016-12-09

    This work aims to propose an optimum resin that can be used in industrial adsorption process for tuning flavor-active components or removal of ethanol for producing an alcohol-free beer. A procedure is reported for selective adsorption of volatile aroma components from water/ethanol mixtures on synthetic hydrophobic resins. High throughput 96-well microtiter-plates batch uptake experimentation is applied for screening resins for adsorption of esters (i.e. isoamyl acetate, and ethyl acetate), higher alcohols (i.e. isoamyl alcohol and isobutyl alcohol), a diketone (diacetyl) and ethanol. The miniaturized batch uptake method is adapted for adsorption of volatile components, and validated with column breakthrough analysis. The results of single-component adsorption tests on Sepabeads SP20-SS are expressed in single-component Langmuir, Freundlich, and Sips isotherm models and multi-component versions of Langmuir and Sips models are applied for expressing multi-component adsorption results obtained on several tested resins. The adsorption parameters are regressed and the selectivity over ethanol is calculated for each tested component and tested resin. Resin scores for four different scenarios of selective adsorption of esters, higher alcohols, diacetyl, and ethanol are obtained. The optimal resin for adsorption of esters is Sepabeads SP20-SS with resin score of 87% and for selective removal of higher alcohols, XAD16N, and XAD4 from Amberlite resin series are proposed with scores of 80 and 74% respectively. For adsorption of diacetyl, XAD16N and XAD4 resins with score of 86% are the optimum choice and Sepabeads SP2MGS and XAD761 resins showed the highest affinity towards ethanol. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Sorption of methyl tert-butyl ether (MTBE) and tert-butyl alcohol (TBA) to synthetic resins.

    PubMed

    Bi, Erping; Haderlein, Stefan B; Schmidt, Torsten C

    2005-10-01

    Methyl tert-butyl ether (MTBE) is a widely used gasoline oxygenate. Contamination of MTBE and its major degradation product tert-butyl alcohol (TBA) in groundwater and surface water has received great attention. However, sorption affinity and sorption mechanisms of MTBE and TBA to synthetic resins, which can be potentially used in removal of these contaminants from water, in passive sampling, or in enrichment of bacteria, have not been studied systemically. In this study, kinetic and equilibrium sorption experiments (single solute and binary mixtures) on four synthetic resins were conducted. The sorption affinity of the investigated sorbents for MTBE and TBA decreases in the order Ambersorb 563>Optipore L493>Amberlite XAD4>Amberlite XAD7, and all show higher sorption affinity for MTBE than for TBA. Binary experiments with o-xylene, a major compound of gasoline as co-contaminant, imply that all resins preferentially sorb o-xylene over MTBE or TBA, i.e., there is sorption competition. In the equilibrium aqueous concentration (Ceq) range (0.1-139.0 mg/L for MTBE, and 0.01-48.4 mg/L for TBA), experimental and modeling results as well as sorbent characteristics indicate that micropore filling and/or some other type of adsorption process (e.g., adsorption to specific sites of high sorption potential at low concentrations) rather than partitioning were the dominant sorption mechanisms. Optipore L493 has favourable sorption and desorption characteristics, and is a suitable sorbent, e.g., in bacteria enrichment or passive sampling for moderately polar compounds. However, for highly polar compounds such as TBA, Ambersorb 563 might be a better choice, especially in water treatment.

  12. Purification of alpha-glucosidae and invertase from bakers' yeast on modified polymeric supports.

    PubMed

    Lothe, R R; Purohit, S S; Shaikh, S S; Malshe, V C; Pandit, A B

    1999-01-01

    In the present work Amberlite XAD-16 and Indion NPA-1, Polystyrene Divinylbenzene macroreticular spherical resins, have been evaluated quantitatively as supports for the adsorption and isolation of the yeast proteins and the enzymes, invertase and alpha-glucosidase. Modification of these supports has been carried out by surface grafting using acrylate polymers to reduce the hydrophobicity and nonspecific adsorption of proteins. Good grafting efficiency, in excess of 90%, has been obtained using ultrasonic irradiation for the surface activation of polystyrene resins. XAD-16 has higher adsorption capacities for the total yeast proteins as well as for both the enzymes, alpha-glucosidase and invertase, than NPA-1 in its respective native and grafted form. Adsorption capacities of XAD-16 and NPA-1 in their respective native and grafted forms for alpha-glucosidase are higher than the capacities for invertase. Nonspecific adsorption of total proteins has been reduced considerably after the grafting of acrylate polymers on hydrophobic supports. At the same time selectivity for the adsorption of both the enzymes has been enhanced on grafted supports. The overall solid-liquid adsorption mass transfer coefficient values (Kla) estimated for adsorption of invertase on XAD are lower than those for alpha-glucosidase. Native and grafted resins could be regenerated and reused for adsorption of alpha-glucosidase for two regeneration cycles studied. Storage stability of invertase and alpha-glucosidase is the same on native and grafted form of XAD-16 and is more than the enzymes in the free form.

  13. Synthesis and application of Amberlite xad-4 functionalized with alizarin red-s for preconcentration and adsorption of rhodium (III)

    PubMed Central

    2012-01-01

    A new chelating resin was prepared by coupling Amberlite XAD-4 with alizarin red-s through an azo spacer, characterized by infra-red spectroscopy and thermal analysis and studied for Rh(III) preconcentration using inductively coupled plasma atomic emission spectroscopy (ICP-AES) for rhodium monitoring in the environment. The optimum pH for sorption of the metal ion was 6.5. The sorption capacity was found 2.1 mg/g of resin for Rh(III). A recovery of 88% was obtained for the metal ion with 1.5 M HCl as eluting agent. Kinetic adsorption data were analyzed by adsorption and desorption times of Rh(III) on modified resin. Scat chard analysis revealed that the homogeneous binding sites were formed in the polymers. The linear regression equation was Q/C = –1.3169Q + 27.222 (R2 = 0.9239), for Rh were formed in the SPE sorbent,Kd and Qmax for the affinity binding sites were calculated to be 0.76 μmol/mL and 20.67 μmol/g, respectively. The equilibrium data and parameters of Rh(III) adsorption on modified resin were analyzed by Langmuir, Freundlich, Temkin and Redlich–Peterson models. The experimental adsorption isotherm was in good concordance with Langmuir and Freundlich models (R2 > 0.998) and based on the Langmuir isotherm the maximum amount of adsorption (qmax) was 4.842 mg/g. The method was applied for rhodium ions determination in environmental samples. with high recovery (>80%). PMID:23369526

  14. Synthesis and application of Amberlite xad-4 functionalized with alizarin red-s for preconcentration and adsorption of rhodium (III).

    PubMed

    Sid Kalal, Hossein; Panahi, Homayon Ahmad; Hoveidi, Hassan; Taghiof, Mohammad; Menderjani, Mahnaz Taheri

    2012-09-18

    A new chelating resin was prepared by coupling Amberlite XAD-4 with alizarin red-s through an azo spacer, characterized by infra-red spectroscopy and thermal analysis and studied for Rh(III) preconcentration using inductively coupled plasma atomic emission spectroscopy (ICP-AES) for rhodium monitoring in the environment. The optimum pH for sorption of the metal ion was 6.5. The sorption capacity was found 2.1 mg/g of resin for Rh(III). A recovery of 88% was obtained for the metal ion with 1.5 M HCl as eluting agent. Kinetic adsorption data were analyzed by adsorption and desorption times of Rh(III) on modified resin. Scat chard analysis revealed that the homogeneous binding sites were formed in the polymers. The linear regression equation was Q/C = -1.3169Q + 27.222 (R2 = 0.9239), for Rh were formed in the SPE sorbent,Kd and Qmax for the affinity binding sites were calculated to be 0.76 μmol/mL and 20.67 μmol/g, respectively. The equilibrium data and parameters of Rh(III) adsorption on modified resin were analyzed by Langmuir, Freundlich, Temkin and Redlich-Peterson models. The experimental adsorption isotherm was in good concordance with Langmuir and Freundlich models (R2 > 0.998) and based on the Langmuir isotherm the maximum amount of adsorption (qmax) was 4.842 mg/g. The method was applied for rhodium ions determination in environmental samples. with high recovery (>80%).

  15. Characterization of anthocyanins and proanthocyanidins in wild and domesticated Mexican blackberries (Rubus spp.).

    PubMed

    Cuevas-Rodríguez, Edith O; Yousef, Gad G; García-Saucedo, Pedro A; López-Medina, José; Paredes-López, Octavio; Lila, Mary Ann

    2010-06-23

    This study was designed to characterize and compare wild, commercial, and noncommercial cultivated blackberry genotypes grown in Michoacan, Mexico. Six genotypes, including WB-3, WB-7, WB-10, and WB-11 (all wild blackberry types), Tupy (a commercial cultivar), and UM-601 (a cultivated breeding line), were selected and profiled for anthocyanins and proanthocyanidins by separating extracts over Amberlite XAD-7 resin and Sephadex LH-20 columns. Subsequent high-performance liquid chromatography (HPLC) and liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) analyses revealed that the major anthocyanin for all genotypes was cyanidin 3-O-glucoside. The proanthocyanidins (condensed tannins) were present in mono- to hexamer forms. Also, hydrolyzable tannins, ellagitannins, were characterized in the blackberry fruits. The average anthocyanin concentration in Sephadex LH-20 fractions was 49.2 mg/g in the commercial cultivar Tupy, while in the wild genotypes and the breeding line, the range was 361.3-494.9 mg/g (cyanidin 3-O-glucoside equivalent). The proanthocyanidin concentration varied widely among wild genotypes (417.5-1343.6 mg/g, catechin equivalent). This study demonstrated that the use of Amberlite XAD-7 followed by Sephadex LH-20 chromatography, with subsequent HPLC and LC-ESI-MS analyses, was able to effectively separate and characterize the diverse polyphenolics in blackberry genotypes. These results suggest that recommendations for dietary intake of blackberries for human health benefits need to take into account the source, because of the wide inherent variation in bioactive polyphenolic content in different blackberry genotypes.

  16. Kinetic, equilibrium and thermodynamic studies on sorption of uranium and thorium from aqueous solutions by a selective impregnated resin containing carminic acid.

    PubMed

    Rahmani-Sani, Abolfazl; Hosseini-Bandegharaei, Ahmad; Hosseini, Seyyed-Hossein; Kharghani, Keivan; Zarei, Hossein; Rastegar, Ayoob

    2015-04-09

    In this work, the removal of uranium and thorium ions from aqueous solutions was studied by solid-liquid extraction using an advantageous extractant-impregnated resin (EIR) prepared by loading carminic acid (CA) onto Amberlite XAD-16 resin beads. Batch sorption experiments using CA/XAD-16 beads for the removal of U(VI) and Th(IV) ions were carried out as a function of several parameters, like equilibration time, metal ion concentration, etc. The equilibrium data obtained from the sorption experiments were adjusted to the Langmuir isotherm model and the calculated maximum sorption capacities in terms of monolayer sorption were in agreement with those obtained from the experiments. The experimental data on the sorption behavior of both metal ions onto the EIR beads fitted well in both Bangham and intra-particle diffusion kinetic models, indicating that the intra-particle diffusion is the rate-controlling step. The thermodynamic studies at different temperatures revealed the feasibility and the spontaneous nature of the sorption process for both uranium and thorium ions. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. [Analysis and separation of organic and inorganic speciations of soluble zinc in edible flowers].

    PubMed

    Peng, Shan-shan; Huang, Guo-qing

    2005-02-01

    Considering the medicinal effects of the edible flowers, the authors studied the separation of trace element zinc's soluble organic and inorganic speciations in water decoction of three edible flowers: Chrysanthemum, Cottonrose hibiscus and Honeysucker by using the 0.45 microm membrane filter and amberlite XAD-2 macroreticular resins. And trace element zinc contents were determined by atomic absorption spectrometry. The optimal conditions for separation had been established. This study verifies the economic value of developing edible flowers, and provides theoretical basis for developing edible flowers as the third functional food materials.

  18. Quantitative evaluation of XAD-8 and XAD-4 resins used in tandem for removing organic solutes from water

    USGS Publications Warehouse

    Malcolm, R.L.; MacCarthy, P.

    1992-01-01

    The combined XAD-8 and XAD-4 resin procedure for the isolation of dissolved organic solutes from water was found to isolate 85% or more of the organic solutes from Lake Skjervatjern in Norway. Approximately 65% of the dissolved organic carbon (DOC) was first removed on XAD-8 resin, and then an additional 20% of the DOC was removed on XAD-4 resin. Approximately 15% of the DOC solutes (primarily hydrophilic neutrals) were not sorbed or concentrated by the procedure. Of the 65% of the solutes removed on XAD-8 resin, 40% were fulvic acids, 16% were humic acids, and 9% were hydrophobic neutrals. Approximately 20% of the hydrophilic solutes that pass through the XAD-8 resin were sorbed solutes on the second resin, XAD-4 (i.e., they were hydrophobic relative to the XAD-4 resin). The fraction sorbed on XAD-4 resin was called XAD-4 acids because it represented approximately 85-90% of the hydrophilic XAD-8 acid fraction according to the original XAD-8 fractionation procedure. The recovery of hydrophobic acids (fulvic acids and humic acids) and the hydrophobic neutral fraction from XAD-8 resin was essentially quantitative at 96%, 98%, and 86%, respectively. The recovery of XAD-4 acids from the XAD-4 resin was only about 50%. The exact reason for this moderately low recovery is unknown, but could result from ??-?? bonding between these organic solutes and the aromatic matrix of XAD-4. The hydrophobic/hydrophilic solute separation on XAD-8 resin for water from background Side A and Side B of the lake was almost identical at 65 and 67%, respectively. This result suggested that both sides of the lake are similar in organic chemical composition even though the DOC variation from side to side is 20%.

  19. Solid sorbent air sampling and analytical procedure for methyl-, dimethyl-, ethyl-, and diethylamine

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Elskamp, C.J.; Schultz, G.R.

    1986-01-01

    A sampling and analytical procedure for methyl-, dimethyl-, ethyl-, and diethylamine was developed in order to avoid problems typically encountered in the sampling and analysis of low molecular weight aliphatic amines. Samples are collected with adsorbent tubes containing Amberlite XAD-7 resin coated with the derivatizing reagent, NBD chloride (7-chloro-4-nitrobenzo-2-oxa-1,3-diazole). Analysis is performed by high performance liquid chromatography with the use of a fluorescence and/or UV/visible detector. All four amines can be monitored simultaneously, and neither collection nor storage is affected by humidity. Samples are stable at room temperature for at least two weeks. The methodology has been tested for eachmore » of the four amines at sample loadings equivalent to air concentration ranges of 0.5 to 30 ppm for a sample volume of 10 liters. The method shows promise for determining other airborne primary and secondary low molecular weight aliphatic amines.« less

  20. Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent for preconcentrations of Cd2+ and Co2+ and their determination by ICP-OES.

    PubMed

    Özdemir, Sadin; Okumuş, Veysi; Kılınç, Ersin; Bilgetekin, Havin; Dündar, Abdurrahman; Ziyadanogˇulları, Berrin

    2012-09-15

    This article reports a method that is used for the preconcentration and determination of Cd(2+) and Co(2+) in vegetables, using Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent. The concentrations of metals were determined by inductively coupled plasma-optical spectrometry (ICP-OES). Critical parameters, such as the pH of the solution, flow rate, the amount of biosorbent, type and volume of eluent, and the sample volume, that affect the solid-phase extraction (SPE) procedure were optimized. The optimum extraction conditions were determined as being a pH of 6.0 for Cd(2+) and of 5.0 for Co(2+); a sample flow rate of 2.0 mL min(-1); 200.0mg of biosorbent; and 5.0 mL of 1.0 mol L(-1) HCl as eluent. The capacities of the biosorbent for metal uptake were found to be 11.3 and 9.8 mg g(-1) for Cd(2+) and Co(2+) ions, respectively. Limit of quantitations (LOQs) were found to be 0.67 and 0.82 ng mL(-1), respectively, for Cd(2+) and Co(2+). The linear working curves were observed to be in the linear range from 1.0 to 50.0 ng mL(-1), and possessed high correlation coefficients. The use of the SPE method showed 50.7- and 35.7-fold improvements in the sensitivities of ICP-OES. The developed method was successfully applied to NCS ZC-73014 (a certified reference tea sample). Relative standard deviations (RSD) were lower than 5.0%. The Cd(2+) and Co(2+) concentrations in the different parts (leave, root, stem, and fruit) of purslane, onion, rocket, okra, and aubergine were determined after microwave digestion and solid-phase extraction by P. eryngii immobilized on Amberlite XAD-16. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Purification of bioactive phenolics from Phanerochaete chysosporium biomass extract on selected macroporous resins

    NASA Astrophysics Data System (ADS)

    Idris, Z. M.; Dzahir, M. I. H. M.; Jamal, P.; Barkat, A. A.; Xian, R. L. W.

    2017-06-01

    In this study, two different types of macroporous resins known as XAD-7HP and HP-20 were evaluated for the adsorption and desorption properties against bioactive phenolics extracted from Phanerochaete chrysosporium. From the previous static sorption studies, it was found that the adsorption capacity for both resins had has no significant difference. Then, the kinetic adsorption data were analyzed with both pseudo-first-order and pseudo-second-order equations and the later performed better. The adsorption isotherm data were fitted well by both Langmuir and Freundlich models. Meanwhile in desorption study, HP-20 and XAD-7HP gave 90.52% and 88.28% recoveries, respectively. Considering the desorption results of the macroporous resins, HP-20 and XAD-7HP were packed in chromatography column to further purify the phenolics. For dynamic adsorption, breakthrough capacity of HP-20 (0.522) was found to be higher than XAD-7HP (0.131). Different ethanol concentrations (30% to 50% (v/v)) were investigated at fixed flowrate (1 ml/min) on phenolics recovery from both types of resins. The highest recovery of bioactive phenolics was 94.3% using XAD-7HP resins at 50% (v/v) of ethanol. Only 77.1% of bioactive phenolics were recovered using HP-20 resin at the same experimental conditions. The purified extract subsequently was analyzed using HPLC. The results showed that three phenolics (gallic acid 3,4-dihydroxybenzoic acid and 4-hydroxybenzoic acid) were identified with higher concentrations as compared to non-purified extract. Finally, the purified extract was tested for scavenging activity against DPPH, and it showed that the activity increased significantly to 90.80% from 59.94% in non-purified extract.

  2. Adsorption of four perfluorinated acids on non ion exchange polymer sorbents.

    PubMed

    Senevirathna, S T M L D; Tanaka, S; Fujii, S; Kunacheva, C; Harada, H; Shivakoti, B R; Dinh, H; Ariyadasa, T

    2011-01-01

    Perfluorinated compounds (PFCs) have attracted global concern due to their ubiquitous distribution and properties of persistence, bio accumulation and toxicity. The process of adsorption has been identified as an effective technique to remove PFCs in water. Different non ion-exchange polymeric adsorbents were tested with regard to their sorption kinetics and isotherms at low PFCs concentrations. Selected PFCs were perfluorobutanoic acid (PFBA), perfluoroheptanoic acid (PFHpA), perfluorooctanoic acid (PFOA) and perfluorodecanoic acid (PFDA) and the tested polymers were three types of Dowex optopores (V-493, V503, and L493), Amberlite XAD-4, and Filtrasorb 400 (Granular Activated Carbon-GAC). We observed the selective adsorption of PFCs on synthetic polymers. For PFDA, Amberlite XAD-4 gave the Freundlich adsorption constant of 2,965 (microg PFCs/g sorbent)(microg PFCs/L)(-n), which was higher than that of GAC (121.89 (microg PFCs/g sorbent) (microg PFCS/L)(-n)). In the case of PFBA, GAC showed better performance (13.36) (microg PFCs/g sorbent) microg PFCS/L)(-n) than synthetic polymers (0.62-5.23) (microg PFCs/g sorbent) (microg PFCS/L)(-n). Adsorption kinetics of all adsorbents were well described (R2 = 0.85-1) by pseudo-second order kinetic model. Sorption capacity was influenced by initial PFCs concentration for all adsorbents. GAC reached the equilibrium concentration within 4 hours, Amberlite XAD 4 reached it within 10 hours and other polymers took more than 70 hours.

  3. Development of a simple and fast voltammetric procedure for determination of trace quantity of Se(IV) in natural lake and river water samples.

    PubMed

    Grabarczyk, Malgorzata; Korolczuk, Mieczyslaw

    2010-03-15

    A simple and fast cathodic stripping voltammetric procedure for determination of trace quantity of Se(IV) in natural samples containing high concentrations of surfactants and humic substances was developed. The procedure exploiting selenium accumulation (from sample solution spiked with 0.1 mol L(-1) HClO(4) and 4 x 10(-4)mol L(-1) Cu(NO(3))(2)) as Cu(2)Se was employed as the initial method. The deposited Cu(2)Se was stripped by differential pulse cathodic potential scan. The interference from dissolved organic matter such as surfactants and humic substances was eliminated by adding Amberlite XAD-7 resin to the voltammetric cell. The whole procedure was applied to a single cell, which allows one to monitor the voltammetric scan. Optimum conditions for removing the surfactants and humic substances due to their adsorption on XAD-7 resin were evaluated. The method was tested on synthetic samples spiked with surfactants and humic substances. The calibration graph for Se(IV) under optimized conditions following the accumulation of 30s was linear in the range from 2 x 10(-9) to 2 x 10(-7)mol L(-1) and was found to obey the equation y=0.74x-0.61, where y and x are the peak current (nA) and Se(IV) concentration (nmol L(-1)), respectively. The linear correlation coefficient was r=0.9993. The relative standard deviation for determination of Se(IV) at the concentration of 1 x 10(-8)mol L(-1) was 3.7% (n=5). The detection limit estimated from three times the standard deviation for low Se(IV) concentration and accumulation time of 30s was about 7.8 x 10(-10)mol L(-1). The presented procedure was successfully applied to selenium determination in TMRAIN-95 certified reference material and to real samples including spiked lake and river waters for selenium speciation. (c) 2009 Elsevier B.V. All rights reserved.

  4. Color and polyphenolic stability in extracts produced from muscadine grape (Vitis rotundifolia) pomace.

    PubMed

    Cardona, Jorge A; Lee, Joon-Hee; Talcott, Stephen T

    2009-09-23

    The muscadine grape ( Vitis rotundifolia ) industry of the southern United States is largely devoid of value-added processes that capture the phytochemical content of wine and juice byproducts. Methods to recover and stabilize polyphenolics from muscadine grape pomace following juice manufacture were evaluated in laboratory-scale and pilot-scale trials. In laboratory-scale trials using osmotic equilibration, water-based extracts from juice pomace initially extracted 31-42% of total polyphenolics, 26-32% of total ellagic acid, and 36-62% of total anthocyanins. When adsorbed onto Amberlite XAD-4 resin to concentrate polyphenolics, these extracts lost 10.5% of their total ellagic acid from inefficient adsorption to the solid phase support. Subsequent pilot-scale trials were evaluated using hot water extracts from grape juice pomace followed by aerobic yeast fermentation to remove sugars and comparison to reversed phase C(18) and Amberlite XAD-4. Extracts were also concentrated using spray-drying and vacuum evaporation. Fermentation had a minor impact on the retention of most polyphenolic compounds evaluated, yet resulted in a 16.3% decrease in antioxidant capacity. Spray-drying resulted in a 30.3% loss in total anthocyanins, a 21.5% loss in total phenolics, and a 23.3% decrease in antioxidant activity, whereas vacuum evaporation had no deleterious impact on these parameters. The physiology of the muscadine grape and its unique phytochemical composition has limited utilization of pomace from wine and juice manufacture. However, these studies demonstrated the potential to extract and concentrate polyphenolic-rich extracts for use in value-added applications.

  5. Comparison of extracts and toxicities of organic compounds in drinking water concentrated by single and composite XAD resins.

    PubMed

    Zhou, Xue; Xiang, Lunhui; Wu, Fenghong; Peng, Xiaoling; Xie, Hong; Wang, Jiachun; Yang, Kedi; Lu, Wenqing; Wu, Zhigang

    2013-12-01

    We compared extracts and toxicities of organic compounds (OCs) in drinking water concentrated by composite XAD-2/8 resin (mixed with an equal volume of XAD-2 and XAD-8 resins) with those extracted by single XAD-2 (non-polar) and XAD-8 (polar) resins. Drinking water was processed from raw water of the Han River and the Yangtze River in Wuhan section, China. The extraction efficiency of all resins was controlled at 30%. The types of extracted OCs were detected by gas chromatography-mass spectrometry, and the cytotoxicity and genotoxicity were assessed by MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) and comet assays, respectively, in human hepatoma HepG2 cells. Our results showed that XAD-2/8 extracted a larger variety of OCs, compared with XAD-8 and XAD-2. The cytotoxicity and genotoxicity of extracted OCs were in the order of XAD-8> XAD-2/8> XAD-2 at almost all tested concentrations after 24 h treatment (P < 0.05). Our findings suggest that single XAD resin selectively extracts either polar or non-polar OCs, which would lead to over- or under-estimation of the toxicity of drinking water. Nevertheless, composite resin extracts both polar and non-polar OCs, and could be utilized as a useful extraction technique to evaluate the level and toxicity of OCs in drinking water.

  6. Microbial 7α-Hydroxylation of 3-Ketobisnorcholenol

    PubMed Central

    Despreaux, Carl W.; Rittweger, Karen R.; Palleroni, Norberto J.

    1986-01-01

    The transformation of 22-hydroxy-23,24-bisnorchol-4-en-3-one to 7α-22-dihydroxy-23,24-bisnorchol-4-en-3-one by Botryodiploida theobromae, Lasiodiplodia theobromae, and various Botryosphaeria strains is described. Factors affecting the reaction were incubation temperature, sonication of the substrate, and addition of 2,2′-dipyridyl, extra carbohydrate, and Amberlite XAD-7. The enzyme responsible for the reaction appeared to be very specific and was not characteristic of all members of the genera listed above. PMID:16347069

  7. Detection of bioactive exometabolites produced by the filamentous marine cyanobacterium Geitlerinema sp.

    PubMed

    Caicedo, Nelson H; Kumirska, Jolanta; Neumann, Jennifer; Stolte, Stefan; Thöming, Jorg

    2012-08-01

    Marine cyanobacteria are noted for their ability to excrete metabolites with biotic properties. This paper focuses on such exometabolites obtained from the culture of the marine filamentous cyanobacterium Geitlerinema sp. strain, their purification and subsequent analyses. By this means the recoveries of the active compounds, a prerequisite for properly determining their concentration, are quantified here for the first time. We demonstrate a new procedure using Amberlite XAD-1180 resin in combination with the eluent isopropanol for extraction of the culture media and gas chromatography as simplified chemical analysis. This procedure reduced necessary bacteria cultivation time (from 150 to 21 days) at low volumes of culture media (300 mL) required for identification of two selected bioactive compounds: 4,4'-dihydroxybiphenyl and harmane.

  8. Effect of Temperature to Adsorption Capacity and Coefficient Distribution on Rare Earth Elements Adsorption (Y, Gd, Dy) Using SIR

    NASA Astrophysics Data System (ADS)

    Aziz, N.; Mindaryani, A.; Supranto; Taftazani, A.; Biyantoro, D.

    2018-04-01

    The use of REE like element of Yttrium (Y) as a superconducting material requires a purity of more than 90%, so it needs to increase the purity of Y from the settling process. The purpose of this research is to study the separation process of REE that is Y, Gd, Dy elements from REE hydroxide (REE(OH)3) using SIR method are consisting of Amberlite XAD-16 resin impregnated with Di-(2-ethylhexyl) phosphate ( D2EHPA) and Tributyl Phosphate (TBP) and determine the isotherm model on REE adsorption and determine the kinetic model of pseudo adsorption reaction. This research was started by activating XAD-16 resin and is mixed with TBP-D2EHPA solvents so it will form SIR, then it is conducted on variation of SIR composition, temperature variation of adsorption process, determination of equilibrium equation and kinetic sorption occurring in SIR adsorption based on experimental data of liquid concentration as function of time. Based on the calculation result, the most effective SIR composition for REE separation is 0.75 g, the equilibrium equation for Y, Gd and Dy follows the Henry equilibrium model and the pseudo kinetic model of the reaction order Y, Gd, and Dy is followed by the pseudo reaction of order 2 The result of separation of LTJ with SIR is said to be effective from another method because purity is obtained that is 96.73% and qualify as a super conductor material.

  9. Investigation of the Effluents Produced during the Functioning of Black and White Colored Smoke Devices.

    DTIC Science & Technology

    1986-01-31

    and 4% diatomaceous earth (binder). Modified EPA Method 5 Sampling Train F The modified EPA Method 5 sampling train used was similar to the one...the fiber glass filter paper were taken by the Amberlite XAD-2. The XAD-2 is a porous polymer adsorbent used to sample organic vapors in effluents...from different kinds of combustion processes. Although a careful clean-up procedure was taken to wash the adsorbents before using, the polymer may still

  10. Separation of cyclic lipopeptide puwainaphycins from cyanobacteria by countercurrent chromatography combined with polymeric resins and HPLC.

    PubMed

    Cheel, José; Urajová, Petra; Hájek, Jan; Hrouzek, Pavel; Kuzma, Marek; Bouju, Elodie; Faure, Karine; Kopecký, Jiří

    2017-02-01

    Puwainaphycins are a recently described group of β-amino fatty acid cyclic lipopeptides of cyanobacterial origin that possess interesting biological activities. Therefore, the development of an efficient method for their isolation from natural sources is necessary. Following the consecutive adsorption of the crude extract on Amberlite XAD-16 and XAD-7 resins, countercurrent chromatography (CCC) was applied to separate seven puwainaphycin variants from a soil cyanobacterium (Cylindrospermum alatosporum CCALA 988). The resin-enriched extract was first fractionated by CCC into fractions I and II with use of the n-hexane-ethyl acetate-ethanol-water (1:5:1:5, v/v/v/v) system at a flow rate of 2 mL min -1 and a rotational speed of 1400 rpm. The CCC separation of fraction I, with use of the ethyl acetate-ethanol-water (5:1:5, v/v/v) system, afforded compounds 1 and 2. The CCC separation of fraction II, with use of the n-hexane-ethyl acetate-ethanol-water (1:5:1:5, v/v/v/v) system, afforded compounds 3-7. In both cases, the lower phases were used as mobile phases at a flow rate of 1 mL min -1 with a rotational speed of 1400 rpm and a temperature of 28 °C. The CCC target fractions obtained were repurified by semipreparative high-performance liquid chromatography (HPLC), leading to compounds 1-7 with purities of 95 %, 95 %, 99 %, 99 %, 95 %, 99 %, and 90 % respectively, as determined by HPLC-electrospray ionization high-resolution mass spectrometry (ESI-HRMS). The chemical identity of the isolated puwainaphycins (compounds 1-7) was confirmed by ESI-HRMS and NMR analyses. Three new puwainaphycin variants (compounds 1, 2, and 5) are reported for the first time. This study provides a new approach for the isolation of puwainaphycins from cyanobacterial biomass. Graphical Abstract Separation of cyclic lipopeptide puwainaphycins from cyanobacteria by countercurrent chromatography combined with polymeric resins and HPLC. Compounds 1 (12-hydroxy-4-methyl-Ahtea-Puw-F), 2 (11-chloro-4-methyl-Ahdoa-Puw-F), 3 (4-methyl-Ahdoa-Puw-F), 4 (4-methyl-Ahdoa-Puw-G), 5 (12-chloro-4-methyl-Ahtea-Puw-F), 6 (4-methyl-Ahtea-Puw-F) and 7 (4-methyl-Ahtea-Puw-G). Ahtea: 3-amino-2-hydroxy tetradecanoic acid. Ahdoa: 3-amino-2-hydroxy dodecanoic acid.

  11. Evaluation of sampling and analytical methods for nicotine and polynuclear aromatic hydrocarbon in indoor air. Final report, 1 February 1987-30 March 1987

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chuang, J.C.; Kuhlman, M.R.; Hannan, S.W.

    1987-11-01

    The objective of this project was to evaluate a potential collection medium, XAD-4 resin, for collecting nicotine and polynuclear aromatic hydrocarbon (PAH) and to determine whether one collection system and one analytical method will allow quantification of both compound classes in air. The extraction efficiency study was to determine the extraction method to quantitatively remove nicotine and PAH from XAD-4 resin. The results showed that a two-step Soxhlet extraction consisting of dichloromethane followed by ethyl acetate resulted in the best recoveries for both nicotine and PAH. In the sampling efficiency study, XAD-2 and XAD-4 resin were compared, in parallel, formore » collection of PAH and nicotine. Quartz fiber filters were placed upstream of both adsorbents to collect particles. Prior to sampling, both XAD-2 and XAD-4 traps were spiked with known amounts (2 microgram) of perdeuterated PAH and D3-nicotine. The experiments were performed with cigarette smoking and nonsmoking conditions. The spiked PAH were retained well in both adsorbents after exposure to more than 300 cu. m. of indoor air. The spiked XAD-4 resin gave higher recoveries for D3-nicotine than did the spiked XAD-2 resin. The collection efficiency for PAH for both adsorbents is very similar but higher levels of nicotine were collected on XAD-4 resin.« less

  12. Synthesis, characterization and physicochemical studies of new chelating resin 1, 8-(3, 6-dithiaoctyl)-4-polyvinylbenzenesulphonate (dpvbs) and its metallopolymer Cu(II), Ni(II), Co(II) and Fe(III) complexes

    NASA Astrophysics Data System (ADS)

    Khalil, Tarek E.; Elbadawy, Hemmat A.; El-Dissouky, Ali

    2018-02-01

    A new chelating resin, 1,8-(3,6-dithiaoctyl)-4-polyvinylbenzenesulphonate (dpvbs) has been synthesized by coupling Amberlite XAD-16 with (2,2‧-ethylenedithio) diethanol using pyridine/CH2Cl2 mixture as a solvent. The chelating resin and its metallopolymer Cu(II), Ni(II), Co(II) and Fe(III) complexes have been synthesized and characterized by EDS, SEM, XPS, elemental analysis, spectral (IR, UV/Vis, EPR). The thermal analysis of the resin and its metallopolymer complexes indicated an endothermic spontaneous sorption mechanism with the liberation of water of hydration of the metal ions and that adsorbed by the free resin. At the solid liquid interface, the degrees of freedom increased during the sorption of the metal ions onto the resin. The surface area of polymer support and its metallopolymer complexes are estimated by (BJH) method. The batch equilibrium method was used for studying the metal sorption and selectivity at different pH values and different contact times at room temperature. ICP-AES was used to estimate the metal capacity of the resin for sorption of Cu(II), Ni(II), Co(II) and Fe(III) from aqueous solutions utilizing the batch equilibrium method. The sorption tendency of the metal ions by the resin was found to be: Cu(II) > Fe(III) > Co(II) > Ni(II). Adsorption kinetics was found to be fit the pseudo-second order model.

  13. Selective recovery of gold from waste mobile phone PCBs by hydrometallurgical process.

    PubMed

    Kim, Eun-young; Kim, Min-seuk; Lee, Jae-chun; Pandey, B D

    2011-12-30

    The leaching of gold from the scrap mobile phone PCBs by electro-generated chlorine as an oxidant and its recovery by ion exchange process was investigated. The leaching experiments were carried out by employing separate leaching reactor connected with the anode compartment of a Cl(2) gas generator. The leaching of gold increased with increase in temperature and initial concentration of chlorine, and was favorable even at low concentration of acid, whereas copper leaching increased with increase in concentration of acid and decrease in temperature. In a two-stage leaching process, copper was mostly dissolved (97%) in 165 min at 25°C during the 1st stage leaching in 2.0 mol/L HCl by electro-generated chlorine at a current density of 714A/m(2) along with a minor recovery of gold (5%). In the 2nd stage gold was mostly leached out (93% recovery, ∼67 mg/L) from the residue of the 1st stage by the electro-generated chlorine in 0.1 mol/L HCl. Gold recovery from the leach liquor by ion exchange using Amberlite XAD-7HP resin was found to be 95% with the maximum amount of gold adsorbed as 46.03 mg/g resin. A concentrated gold solution, 6034 mg/L with 99.9% purity was obtained in the ion exchange process. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. Analysis of the effects of stirring condition of separation of thorium in the elution process of monazite partial solution by solvent impregnated resin method

    NASA Astrophysics Data System (ADS)

    Prassanti, R.; Putra, D. S.; Kusuma, B. P.; Nawawi, F. W.

    2018-01-01

    Monazite is a natural mineral which contains abundant valuable element such as Radioactive Element and Rare Earth Element(REE). In this experiment, it is proven that solution of residual Thorium Sulfate from Monazite mineral process, can be seperated selectively by using extracting method of Solvent Impregnated Resin(SIR), with the elutant solution HNO3. In the earlier process, Thorium solution is conditioned at PH 1 by using H2SO4. Then REE, Thorium and Uranium elements are seperated. This seperation is conducted by using adsorption method by Amberlite XAD-16 Resin, which has been impregnated by Tributhyl Phosphate extractant. It is continued with elution process, which is aimed to obtain Thorium solution of a higher level of concentration. This elution process is conducted by using HNO3, with the elution variables of the lenght of mixing and amount concentration elutant. Based on this experiment, SIR extracting method is able to dissolve Thorium solution until 63,2%grade and a higher level of %grade about 92,40%. It can be concluded that this SIR method can extracted Thorium elements selectively, improve extracting process recovery, and determine optimum stripping condition in the 45th minutes with elutant concentration of 1,0M HNO3.

  15. Metal complexes of the nanosized ligand N-benzoyl-N‧-(p-amino phenyl) thiourea: Synthesis, characterization, antimicrobial activity and the metal uptake capacity of its ligating resin

    NASA Astrophysics Data System (ADS)

    Elhusseiny, Amel F.; Eldissouky, Ali; Al-Hamza, Ahmed M.; Hassan, Hammed H. A. M.

    2015-11-01

    The new nanosized N-benzoyl-N‧-(p-amino phenyl) thiourea ligand H2L was synthesized by nanoprecipitation method. The [Cu (H2L)2 Cl]·2H2O, [Zn (H2L)2(OAc)2], [Cd (H2L)2Cl2] and [Hg (H2L)2Cl2] complexes were synthesized and characterized by various physicochemical methods. Results revealed that the ligand act as hypodentate and bonded to the metal ion via the sulfur atom forming mononuclear non-electrolyte diamagnetic complex. Magnetic moment results indicated a reduction of Cu (II) to Cu (I) during the coordination process. Thermal studies demonstrated variable stabilities of the complexes and [Zn (H2L)2(OAc)2] exhibited the highest thermal stability while [Hg (H2L)2Cl2] was volatile. The prepared compounds were screened against different pathogenic microorganisms. The ligand performed high antibacterial activity against certain bacterial strain compared to its complexes, and the standard bacteriocide in use. The ligand was successfully immobilized on modified Amberlite XAD-16 forming the hypodentate ligating resin PS-SO2-H2L. The new resin was characterized and the extent of metal adsorption reached maximum at pH 6.0 for Cu (II), Cd (II) and Ag (I), with an adsorption amount of 4.3, 4.0 and 3.7 mmol g-1 respectively. The nanosized H2L represents a new category of promising adsorbent that would have a practical impact on biological and water treatment applications.

  16. CTEPP STANDARD OPERATING PROCEDURE FOR PRE-CLEANING FILTERS AND XAD-2 (SOP-5.10)

    EPA Science Inventory

    This SOP summarizes the method for pre-cleaning XAD-2 resin and quartz fiber filters. The procedure provides a cleaning method to help reduce potential background contamination in the resin and filters.

  17. Evaluation of polymeric adsorbent resins for efficient detoxification of liquor generated during acid pretreatment of lignocellulosic biomass.

    PubMed

    Sandhya, Soolamkandath Variem; Kiran, Kumar; Kuttiraja, Mathiyazhakan; Preeti, Varghese Elizabeth; Sindhu, Raveendran; Vani, Sankar; Kumar, Sukumaran Rajeev; Pandey, Ashok; Binod, Parameswaran

    2013-11-01

    Production of fuel ethanol from lignocellulosic biomass conventionally includes biomass pretreatment, hydrolysis, and fermentation. The liquor generated during dilute acid pretreatment of biomass contains considerable quantities of pentose sugars as well as various degradation products of sugars and lignin, like furfural, hydroxymethyl furfural (HMF), organic acids, aldehydes and others, which are known to be inhibitory for microbial growth. This pentose rich liquor is a potent resource which can be used to produce alcohol or other value added metabolites by microbial fermentation. However, the presence of these inhibitory compounds is a major hindrance and their removal is essential for efficient utilization of this byproduct stream. In the present work, the polymeric adsorbent resins, XAD-4, XAD-7 and XAD-16 were evaluated for their ability to adsorb fermentation inhibitors like furfural and HMF from the acid pretreated liquor. These resins could remove 55-75% of furfural and 100% of HMF and more than 90% sugar remained un-adsorbed in the pretreated liquor. Desorption of furfural from stationary phase was evaluated by using ethanol and hot water. The results suggest that these polymeric resins may be used for detoxification of acid pretreatment liquor with selective removal of sugar degradation products without affecting the sugar content in the solution.

  18. Enzymatic determination of carbon-14 labeled L-alanine in biological samples

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Serra, F.; Palou, A.; Pons, A.

    A method for determination of L-alanine-specific radioactivity in biological samples is presented. This method is based on the specific enzymatic transformation of L-alanine to pyruvic acid hydrazone catalyzed by the enzyme L-alanine dehydrogenase, formation of the pyruvic acid 2,4-dinitrophenylhydrazone derivative, and quantitative trapping in Amberlite XAD-7 columns, followed by radioactivity counting of the lipophilic eluate. No interferences from other UC-labeled materials such as D-glucose, glycerol, L-lactate, L-serine, L-glutamate, L-phenylalanine, glycine, L-leucine, and L-arginine were observed. This inexpensive and high-speed method is applicable to the simultaneous determination of L-alanine-specific radioactivity for a large number of samples.

  19. Experiments on Anion Exchange with Amberlite Ir-120 Resin; ENSAYOS DE INTERCAMBIO ANIONICO CON RESINA AMBERLITA Ir-120

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Cellini, R.F.; Palomino, J.V.

    1956-01-01

    The ion exchange of the uranyl ion on Amberlite Ir-120 resin was studied with different uranyl ion concentrations. Elution with sulfuric acid was investlgated and the elution curve for the experimental conditions was determined. From the concentrations of the ions of Cu/sup 2+/, Ni/sup 2+/, Fe/sup 3+/, Cd/sup 2+/, Mn/sup 2+/, and Cr/sup 3+/ the maximum exchange capacity was tested and elation curves with 4 N sulfuric acid were obtained. (tr-auth)

  20. RECOVERY OF MUTAGENICITY FROM DISINFECTED WATER BY XAD RESIN ADSORPTION COMPARED TO REVERSE OSMOSIS

    EPA Science Inventory

    Recovery of Mutagenicity from Disinfected Water Samples by XAD Resin Adsorption Compared to Reverse Osmosis

    K. M. Schenck1, T. F. Speth1, R. J. Miltner1, M. Sivaganesan1 and J. E. Simmons2

    1U.S. EPA, Office of Research and Development, NRMRL
    2U.S. EPA, Office of...

  1. Prediction of the sorption capacities and affinities of organic chemicals by XAD-7.

    PubMed

    Yang, Kun; Qi, Long; Wei, Wei; Wu, Wenhao; Lin, Daohui

    2016-01-01

    Macro-porous resins are widely used as adsorbents for the treatment of organic contaminants in wastewater and for the pre-concentration of organic solutes from water. However, the sorption mechanisms for organic contaminants on such adsorbents have not been systematically investigated so far. Therefore, in this study, the sorption capacities and affinities of 24 organic chemicals by XAD-7 were investigated and the experimentally obtained sorption isotherms were fitted to the Dubinin-Ashtakhov model. Linear positive correlations were observed between the sorption capacities and the solubilities (SW) of the chemicals in water or octanol and between the sorption affinities and the solvatochromic parameters of the chemicals, indicating that the sorption of various organic compounds by XAD-7 occurred by non-linear partitioning into XAD-7, rather than by adsorption on XAD-7 surfaces. Both specific interactions (i.e., hydrogen-bonding interactions) as well as nonspecific interactions were considered to be responsible for the non-linear partitioning. The correlation equations obtained in this study allow the prediction of non-linear partitioning using well-known chemical parameters, namely SW, octanol-water partition coefficients (KOW), and the hydrogen-bonding donor parameter (αm). The effect of pH on the sorption of ionizable organic compounds (IOCs) could also be predicted by combining the correlation equations with additional equations developed from the estimation of IOC dissociation rates. The prediction equations developed in this study and the proposed non-linear partition mechanism shed new light on the selective removal and pre-concentration of organic solutes from water and on the regeneration of exhausted XAD-7 using solvent extraction.

  2. CHEMICAL ANALYSIS OF REVERSE OSMOSIS MEMBRANE AND XAD RESIN ADSORPTION CONCENTRATES OF WATER DISINFECTED BY CHLORINATION OR OZONATION/CHLORINATION PROCESSES

    EPA Science Inventory


    Chemical Analysis of Reverse Osmosis Membrane and XAD Resin Adsorption Concentrates of Water Disinfected by Chlorination or Ozonation/Chlorination Processes.

    J. E. Simmons1, S.D. Richardson2, K.M. Schenck3, T. F. Speth3, R. J. Miltner3 and A. D. Thruston2

    1 NHEE...

  3. Enrichment of antioxidants in black garlic juice using macroporous resins and their protective effects on oxidation-damaged human erythrocytes.

    PubMed

    Zou, Ying; Zhao, Mouming; Yang, Kun; Lin, Lianzhu; Wang, Yong

    2017-08-15

    The black garlic juice is popular for its nutritive value. Enrichment of antioxidants is needed to make black garlic extract an effective functional ingredient. Five macroporous resins were evaluated for their capacity in adsorbing antioxidants in black garlic juice. XAD-16 resin was chosen for further study due to its high adsorption and desorption ratios. Pseudo-second-order kinetics (q e =625μmol Trolox equiv/g dry resin, k 2 =0.0001463) and Freundlich isotherm models (ΔH=-10.1547kJ/mol) were suitable for describing the whole exothermic and physical adsorption processes of the antioxidants from black garlic juice on XAD-16 resin. The antioxidants and phenolics were mostly enriched in 40% ethanol fraction by XAD-16 resin column chromatography. The black garlic extract and its fractions could protect erythrocytes against AAPH-induced hemolysis in dose-dependent manners. The pretreatment of AAPH-damaged erythrocytes with 40% ethanol fractions (2.5mg/mL) significantly decreased the hemolysis ratios from 53.58% to 3.79%. The 40% ethanol fraction possessing strong intracellular antioxidant activity could be used as a functional food ingredient. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Process for the preparation of lactic acid and glyceric acid

    DOEpatents

    Jackson, James E [Haslett, MI; Miller, Dennis J [Okemos, MI; Marincean, Simona [Dewitt, MI

    2008-12-02

    Hexose and pentose monosaccharides are degraded to lactic acid and glyceric acid in an aqueous solution in the presence of an excess of a strongly anionic exchange resin, such as AMBERLITE IRN78 and AMBERLITE IRA400. The glyceric acid and lactic acid can be separated from the aqueous solution. Lactic acid and glyceric acid are staple articles of commerce.

  5. BROAD SPECTRUM ANALYSIS FOR TRACE ORGANIC POLLUTANTS IN LARGE VOLUMES OF WATER BY XAD RESINS-COLUMN DESIGN-FACTS AND MYTHS.

    USGS Publications Warehouse

    Gibs, J.; Wicklund, A.; Suffet, I.H.

    1986-01-01

    The 'rule of thumb' that large volumes of water can be sampled for trace organic pollutants by XAD resin columns which are designed by small column laboratory studies or pure compounds is examined and shown to be a problem. A theory of multicomponent breakthrough is presented as a frame of reference to help solve the problem and develop useable criteria to aid the design of resin columns. An important part of the theory is the effect of humic substances on the breakthrough character of multicomponent chemical systems.

  6. Adsorption of saponin compound in Carica papaya leaves extract using weakly basic ion exchanger resin

    NASA Astrophysics Data System (ADS)

    Abidin, Noraziani Zainal; Janam, Anathasia; Zubairi, Saiful Irwan

    2016-11-01

    Adsorption of saponin compound in papaya leaves juice extract using Amberlite® IRA-67 resin was not reported in previous studies. In this research, Amberlite® IRA-67 was used to determine the amount of saponin that can be adsorbed using different weights of dry resin (0.1 g and 0.5 g). Peleg model was used to determine the maximum yield of saponin (43.67 mg) and the exhaustive time (5.7 days) prior to a preliminary resin-saponin adsorption study. After adsorption process, there was no significant difference (p>0.05) in total saponin content (mg) for sample treated with 0.1 g (3.79 ± 0.55 mg) and sample treated with 0.5 g (3.43 ± 0.51 mg) dry weight resin. Long-term kinetic adsorption of resin-saponin method (>24 hours) should be conducted to obtain optimum freed saponin extract. Besides that, sample treated with 0.1 g dry weight resin had high free radical scavenging value of 50.33 ± 2.74% compared to sample treated with 0.5 g dry weight resin that had low free radical scavenging value of 24.54 ± 1.66% dry weights. Total saponin content (mg), total phenolic content (mg GAE) and free radical scavenging activity (%) was investigated to determine the interaction of those compounds with Amberlite® IRA-67. The RP-HPLC analysis using ursolic acid as standard at 203 nm showed no peak even though ursolic acid was one of the saponin components that was ubiquitous in plant kingdom. The absence of peak was due to weak solubility of ursolic acid in water and since it was only soluble in solvent with moderate polarity. The Pearson's correlation coefficient for total saponin content (mg) versus total phenolic content (mg GAE) and radical scavenging activity (%) were +0.959 and +0.807. Positive values showed that whenever there was an increase in saponin content (mg), the phenolic content (mg GAE) and radical scavenging activity (%) would also increase. However, as the resin-saponin adsorption was carried out, there was a significant decrease of radical scavenging activity (%) as the amount of the resin increased. Moreover, the saponin amount did not show any reduction as the amount of resin resin increased. Therefore, there was other active ingredient which has the antioxidant properties were affected by the adsoprtion process. For that reason, the kinetic equilibrium of resin-saponin adsorption studies against the ratio of resin-to-extract has to be carried out to determine the efficacy of the extract therapeutic properties prior to the cell culture studies.

  7. Immobilization of a Commercial Lipase from Penicillium camembertii (Lipase G) by Different Strategies

    PubMed Central

    Mendes, Adriano A.; Freitas, Larissa; de Carvalho, Ana Karine F.; de Oliveira, Pedro C.; de Castro, Heizir F.

    2011-01-01

    The objective of this work was to select the most suitable procedure to immobilize lipase from Penicillium camembertii (Lipase G). Different techniques and supports were evaluated, including physical adsorption on hydrophobic supports octyl-agarose, poly(hydroxybutyrate) and Amberlite resin XAD-4; ionic adsorption on the anionic exchange resin MANAE-agarose and covalent attachment on glyoxyl-agarose, MANAE-agarose cross-linked with glutaraldehyde, MANAE-agarose-glutaraldehyde, and epoxy-silica-polyvinyl alcohol composite. Among the tested protocols, the highest hydrolytic activity (128.2 ± 8.10 IU·g−1 of support) was achieved when the lipase was immobilized on epoxy-SiO2-PVA using hexane as coupling medium. Lipase immobilized by ionic adsorption on MANAE-agarose also gave satisfactory result, attaining 55.6 ± 2.60 IU·g−1 of support. In this procedure, the maximum loading of immobilized enzyme was 9.3 mg·g−1 of gel, and the highest activity (68.8 ± 2.70 IU·g−1 of support) was obtained when 20 mg of protein·g−1 was offered. Immobilization carried out in aqueous medium by physical adsorption on hydrophobic supports and covalent attachment on MANAE-agarose-glutaraldehyde and glyoxyl-agarose was shown to be unfeasible for Lipase G. Thermal stability tests revealed that the immobilized derivative on epoxy-SiO2-PVA composite using hexane as coupling medium had a slight higher thermal stability than the free lipase. PMID:21811674

  8. Isolation and identification of flavonoids, including flavone rotamers, from the herbal drug 'Crataegi folium cum flore' (hawthorn).

    PubMed

    Rayyan, S; Fossen, T; Solheim Nateland, H; Andersen, O M

    2005-01-01

    Twelve flavonoids, including seven flavones, four flavonols and one flavanone, were isolated from methanolic extract of the herbal drug 'Crataegi folium cum flore' (hawthorn leaves and flowers) by a combination of CC (over Amberlite XAD-7 and Sephadex LH-20) and preparative HPLC. Their structures, including that of the novel flavonol 8-methoxykaempferol 3-O-(6"-malonyl-beta-glucopyranoside), were elucidated by homo- and heteronuclear NMR and electrospray/MS. The 1H- and 13C-NMR of all compounds, including rotameric pairs of five flavone C-glycosides, were assigned. The presence and relative proportion of each rotamer was shown by various NMR experiments, including two-dimensional nuclear Overhauser and exchange spectroscopy, to depend on solvent, linkage position and structure of the C-glycosyl substituent.

  9. Anthocyanin determination in blueberry extracts from various cultivars and their antiproliferative and apoptotic properties in B16-F10 metastatic murine melanoma cells.

    PubMed

    Bunea, Andrea; Rugină, Dumitriţa; Sconţa, Zoriţa; Pop, Raluca M; Pintea, Adela; Socaciu, Carmen; Tăbăran, Flaviu; Grootaert, Charlotte; Struijs, Karin; VanCamp, John

    2013-11-01

    Blueberry consumption is associated with health benefits contributing to a reduced risk for cardiovascular disease, diabetes and cancer. The aim of this study was to determine the anthocyanin profile of blueberry extracts and to evaluate their effects on B16-F10 metastatic melanoma murine cells. Seven blueberry cultivars cultivated in Romania were used. The blueberry extracts were purified over an Amberlite XAD-7 resin and a Sephadex LH-20 column, in order to obtain the anthocyanin rich fractions (ARF). The antioxidant activity of the ARF of all cultivars was evaluated by ABTS, CUPRAC and ORAC assays. High performance liquid chromatography followed by electrospray ionization mass spectrometry (HPLC-ESI-MS) was used to identify and quantify individual anthocyanins. The anthocyanin content of tested cultivars ranged from 101.88 to 195.01 mg malvidin-3-glucoside/100g fresh weight. The anthocyanin rich-fraction obtained from cultivar Torro (ARF-T) was shown to have the highest anthocyanin content and antioxidant activity, and inhibited B16-F10 melanoma murine cells proliferation at concentrations higher than 500 μg/ml. In addition, ARF-T stimulated apoptosis and increased total LDH activity in metastatic B16-F10 melanoma murine cells. These results indicate that the anthocyanins from blueberry cultivar could be used as a chemopreventive or adjuvant treatment for metastasis control. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. Macroporous resin purification of peptides with umami taste from soy sauce.

    PubMed

    Zhuang, Mingzhu; Zhao, Mouming; Lin, Lianzhu; Dong, Yi; Chen, Huiping; Feng, Mengying; Sun-Waterhouse, Dongxiao; Su, Guowan

    2016-01-01

    In this study, the performance and separation characteristics of four macroporous resins for purifying umami peptides from soy sauce were examined. Results showed that the resins could separate the peptides of soy sauce, and the particle diffusion kinetics model was suitable for describing the whole exothermic (ΔH < 43 kJ/mol) adsorption process on the SP-825 and HP-20 resins, while the pseudo-second-order kinetics model accurately described the XAD-16 and HP-2 MGL resins. Furthermore, the adsorption processes of the peptides followed the Freundlich model. The XAD-16 resin was the most effective resin for the enrichment of peptides due to its high adsorption and total desorption capacities. Interestingly, the umami peptides were enriched in the deionized water fraction. This study provides new insights into exploring performance and separation characteristics of macroporous resins on soy sauce, and indicated that peptide may be the contributor to the umami taste in Chinese soy sauce. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Characterization of dissolved organic material in the interstitial brine of Lake Vida, Antarctica

    NASA Astrophysics Data System (ADS)

    Cawley, Kaelin M.; Murray, Alison E.; Doran, Peter T.; Kenig, Fabien; Stubbins, Aron; Chen, Hongmei; Hatcher, Patrick G.; McKnight, Diane M.

    2016-06-01

    Lake Vida (LV) is located in the McMurdo Dry Valleys (Victoria Valley, East Antarctica) and has no inflows, outflows, or connectivity to the atmosphere due to a thick (16 m), turbid ice surface and cold (<-20 °C) subsurface alluvium surrounding the lake. The liquid portion of LV has a salinity about seven times that of seawater and is entrained in ice and sediment below the ice cap. This subzero (-13.4 °C), anoxic brine supports a microbial community, which has low levels of activity and has been isolated from the atmosphere for at least 2800 14C years before present. The brine has high dissolved organic carbon concentration (DOC; 580 mg-C L-1 or greater); the study of which provides a unique opportunity to better understand biological and/or abiotic processes taking place in an isolated saline ecosystem with no external inputs. We isolated two sub-fractions of LV dissolved organic matter (DOM) by chemical separation using XAD-8 and XAD-4 resins in series. This separation was followed by physical separation using ultrafiltration to isolate a higher molecular weight (HMW) fraction that was retained by the membrane and a salty, dilute low molecular weight fraction. This analytical path resulted in three, low salt sub-fractions and allowed comparison to other Antarctic lake DOM samples isolated using similar procedures. Compared to other Antarctic lakes, a lower portion of the DOC was retained by XAD-8 (∼10% vs. 16-24%) resin, while the portions retained by XAD-4 (∼8%) resin and the 1 kDa ultrafiltration membrane (∼50%) were similar. The 14C radiocarbon ages of the XAD-8 (mean 3940 ybp), XAD-4 (mean 4048 ybp) and HMW (mean 3270 ybp) fractions are all older than the apparent age of ice-cover formation (2800 ybp). Ultrahigh resolution mass spectrometry showed that compounds with two and three nitrogen atoms in the molecular formulas were common in both the LV-XAD8 and LV-XAD4 fractions, consistent with microbial production and processing. The long-term oxidation of LVBr DOM by abiotic oxidants including perchlorate and chlorate may explain the low portion in the XAD8 fraction and the lack of aromatic carbon, as measured by 13C NMR spectroscopy, found for all but the most hydrophobic fraction, LV-XAD8. Overall, the chemical characteristics of Lake Vida brine DOM suggest that legacy DOM sealed and concentrated within the brine has been altered due to a combination of both biological and abiotic chemical reactions.

  12. Formation of natural indigo derived from woad (Isatis tinctoria L.) in relation to product purity.

    PubMed

    Garcia-Macias, Paulina; John, Philip

    2004-12-29

    There is an increasing commercial demand for naturally sourced indigo that meets the purity standards set by the synthetic product. This study concerns the indigo made from leaves of woad (Isatis tinctoria L.), and in particular its interaction with particulate impurities arising from soil and plant materials. Also, a more reliable method using N-methyl-2-pyrrolidone has been developed for the spectrophotometric determination of indigo. In a novel application of fluorescence spectroscopy, indoxyl intermediates in indigo formation are shown to be stable for minutes. The main indigo precursor from woad can be adsorbed onto Amberlite XAD16 in conformity with a Langmuir isotherm, but indigo precursors break down on this and other resin beads to yield indigo and red compounds. Indigo made from indoxyl acetate aggregates into particles, the size distribution of which can be modified by the inclusion of a fine dispersion of calcium hydroxide. Bright field microscopy of indigo products made under defined conditions and scanning electron microscopy combined with energy-dispersive X-ray analysis reveal the relationship of indigo with particulate materials. A model illustrating the interaction of indigo with particulate contaminants is developed on the basis of the results obtained, and recommendations are made for improving the purity of natural indigo.

  13. Isolation of antioxidative phenolic glucosides from lemon juice and their suppressive effect on the expression of blood adhesion molecules.

    PubMed

    Miyake, Yoshiaki; Mochizuki, Mika; Okada, Miki; Hiramitsu, Masanori; Morimitsu, Yasujiro; Osawa, Toshihiko

    2007-08-01

    Phenolic glucosides having radical scavenging activity were examined from the fraction eluted with 20% methanol on Amberlite XAD-2 resin applied to lemon (Citrus limon) juice by using reversed phase chromatography. Four phenolic glucosides were identified as 1-feruloyl-beta-D-glucopyranoside, 1-sinapoyl-beta-D-glucopyranoside, 6,8-di-C-glucosylapigenin and 6,8-di-C-glucosyldiosmetin by (1)H-NMR, (13)C-NMR, and MS analyses. They exhibited radical scavenging activity for 1,1-diphenyl-2-picrylhydrazyl (DPPH) and superoxide, although the activity was low in comparison with eriocitrin, a potent antioxidant in lemon fruit, and the eriodictyol of its aglycone. The phenolic compounds in lemon juice were examined for their suppressive effect on the expression of blood adhesion molecules by measuring the expression of intercellular adhesion molecule-1 (ICAM-1) in human umbilical vein endothelial cells (HUVECs) induced by necrosis factor-alpha (TNF-alpha). 6,8-Di-C-glucosylapigenin, apigenin, and diosmentin of the flavones were found to significantly suppress the expression of ICAM-1 at 10 muM (P<0.05). The phenolic glucosides isolated in this study were contained in comparative abundance in daidai (Citrus aurantium) and niihime (Citrus unshiu x Citrus tachibana) among the sour citrus juices.

  14. Metabolism of difebarbamate in man.

    PubMed

    Vachta, J; Valter, K; Siegfried, B

    1990-01-01

    The metabolism of 1,3-bis(3-butoxy-2-carbamoyloxypropyl)-5-ethyl-5-phenyl- (1H,3H,5H)-pyrimidine-2,4,6-trione (difebarbamate) in man was studied. Human volunteers received a single oral dose of 25 mg/kg difebarbamate. Urine was extracted with Amberlite XAD-2 resin and the extracts were separated by preparative HPLC after enzymatic hydrolysis. Four major metabolites were isolated and their structures were determined using NMR and mass spectrometry. The oxygen dealkylation led to the formation of two metabolites: 1-(3-butoxy-2-carbamoyloxypropyl)-3-(2-carbamoyloxy-3-hydrox ypropyl)-5-ethyl-5- phenyl-(1H, 3H, 5H)-pyrimidine-2,4,6,-trione and 1,3-bis(2-carbamoyloxy-3-hydroxypropyl)-5-ethyl-5-phenyl-(1H,3H,5H )- pyrimidine-2,4,6,-trione. The hydrolysis of the carbamoyloxy group with the oxygen dealkylation led to the formation of 1-(2-carbamoyloxy-3-hydroxypropyl)-3-(2,3-dihydroxypropyl)-5-ethyl - 5-phenyl-(1H,3H,5H)-pyrimidine-2,4,6,-tione, whereas the 4-hydroxylation of the benzene ring together with the oxygen dealkylation led to the formation of 1,3-bis(2-carbamoyloxy-3-hydroxypropyl)-5-ethyl-5-(4-hydroxyphenyl )-(1H,3H,5H)- pyrimidine-2,4,6,-trione. No traces of the parent drug were found.

  15. Do prevailing XAD extraction methods used to generate extracts from disinfected water adequately link extract toxicology to disinfected water chemistry?

    EPA Science Inventory

    Motivation: It is common to use XAD resins to extract disinfection byproducts (DBPs) from disinfected water. The resulting extract is used in toxicological assays to study the effects of DBP mixtures and has been considered representative of the original disinfected water. Howeve...

  16. Determination of alkylbenzenesulfonate surfactants in groundwater using macroreticular resins and carbon-13 nuclear magnetic resonance spectrometry

    USGS Publications Warehouse

    Thurman, E.M.; Willoughby, T.; Barber, L.B.; Thorn, K.A.

    1987-01-01

    Alkylbenzenesulfonate surfactants were determined in groundwater at concentrations as low as 0.3 mg/L. The method uses XAD-8 resin for concentration, followed by elution with methanol, separation of anionic and nonionic surfactants by anion exchange, quantitation by titration, and identification by 13C nuclear magnetic resonance spectrometry. Laboratory standards and field samples containing straight-chain and branched-chain alkylbenzenesulfonates, sodium dodecyl sulfate, and alkylbenzene ethoxylates were studied. The XAD-8 extraction of surfactants from groundwater was completed in the field, which simplified sample preservation and reduced the cost of transporting samples.

  17. Analysis of Organohalogen Products From Chlorination of Natural Waters Under Simulated Biofouling Control Conditions

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Bean, R. M.; Mann, D. C.; Riley, R. G.

    1980-06-01

    The products of low-level chlorination of natural waters from ten locations across the continental United States have been studied, with emphasis on volatile and lipophilic organohalogen components. A specially designed apparatus permitted continuous sampling and chlorination of water in a manner analogous to some types of cooling water treatments. Volatile components were analyzed using headspace, purge-and-trap, and resin adsorption methods. The less-volatile components were collected by passing large volumes of the chlorinated water over XAD-2 columns. Total organic halogen collected on XAD resins was compared with the halogen contribution of haloform compounds. The XAD samples were further separated into fractionsmore » according to molecular weight and polarity using liquid chrOmatography. These studies indicate that haloforms are the most abundant lipophilic halogenated products formed from low-level chlorination of natural waters, but that other halogenated lipophilic material is also formed.« less

  18. Preparation, bioactivity, and application of novel biocidal materials

    NASA Astrophysics Data System (ADS)

    Wu, Rong

    In this study, several novel N-halamine precursors were synthesized. These surface coupling agents were bonded to the surfaces of cotton fabric, cotton gauze, paper, glass, and sand. Once they were activated using household bleach, the surfaces and materials became biocidal. Possible uses for the biocidal cotton are in protective garments for hospital personnel and those who must fight against bioterrorism. The treated cotton gauze may be used to make an antimicrobial mask to stop infective pathogen transcontamination. Biocidal sand has the potential to be used as a disinfectant in a filter for wastewater or municipal water treatment. In fact, the N-halamine siloxanes can be applied to many other surfaces. The results of biocidal efficacy of some of the treated surfaces will be presented in this study. Several new hydantoinyl diols and quaternary ammonium hydantoinyl diols were prepared in this work also. They were copolymerized with commercial water borne acrylic polyol and commercial isocyanate to form polyurethane coatings. The biocidal polyurethane coatings were produced after activation by chlorination. Those diols also reacted with a two-component epoxy paint to render the paint antimicrobial. Several novel biocidal polymeric resins were synthesized by attachment of N-halamine moieties to the commercial polymer supported beads such as Merrifield resin and Amberlite IRA-67 ionic resin. The Merrifield resin and Amberlite IRA-67 ionic resin also were grafted with N-halamine functionality as well as with the N,N-dimethyl-dodecylamine moiety via 1,2-dichloroethane. Finally, several quaternary ammonium N-halamine polymers were prepared. Direct copolymerization of (triethoxysilyl)propyl-7,7,9,9-tetramethyl-1,3,8-triazaspiro-[4,5]-decane-2,4-dione (TTDD-Si), or 3-(trimethoxysilyl)propyl-5,5-dimethylhydantoin (BA-1 ') with 3-(trimethoxysilylpropyl)dimethyloctadecyl ammonium chloride (DC 5700) produced dual functionality and water soluble biocidal materials and surfaces. (Abstract shortened by UMI.)

  19. Improvement of side-effects and treatment on the experimental colitis in mice of a resin microcapsule-loading hydrocortisone sodium succinate.

    PubMed

    Dong, Kai; Zhang, Hefeng; Yan, Yan; Sun, Jinyao; Dong, Yalin; Wang, Ke; Zhang, Lu; Shi, Xianpeng; Xing, Jianfeng

    2017-03-01

    Extensive or long-time use of corticosteroids often causes many toxic side-effects. The ion exchange resins and the coating material, Eudragit, can be used in combination to form a new oral delivery system to deliver corticosteroids. The resin microcapsule (DRM) composed by Amberlite 717 and Eudragit S100 was used to target hydrocortisone (HC) to the colon in order to improve its treatment effect on ulcerative colitis (UC) and reduce its toxic side-effects. Hydrocortisone sodium succinate (HSS) was sequentially encapsulated in Amberlite 717 and Eudragit S100 to prepare the HSS-loaded resin microcapsule (HSS-DRM). The scanning electron microscopy (SEM) was employed to investigate the morphology and structure of HSS-DRM. The in vitro release and in vivo studies of pharmacokinetics and intestinal drug residues in rat were used to study the colon-targeting of HSS-DRM. The mouse induced by 2,4,6-trinitrobenzenesulfonic acid was used to study the treatment of HSS-DRM on experimental colitis. SEM study showed good morphology and structure of HSS-DRM. In the in vitro release study, > 80% of HSS was released in the colon environment (pH 7.4). The in vivo studies showed good colon-targeting of HSS-DRM (T max  = 0.97 h, C max  = 118.28 µg/mL of HSS; T max  = 2.16 h, C max  = 64.47 µg/mL of HSS-DRM). Moreover, the HSS-DRM could reduce adverse reactions induced by HSS and had good therapeutic effects on the experimental colitis. The resin microcapsule system has good colon-targeting and can be used in the development of colon-targeting preparations.

  20. Monoterpene alcohol metabolism: identification, purification, and characterization of two geraniol dehydrogenase isoenzymes from Polygonum minus leaves.

    PubMed

    Hassan, Maizom; Maarof, Nur Diyana; Ali, Zainon Mohd; Noor, Normah Mohd; Othman, Roohaida; Mori, Nobuhiro

    2012-01-01

    NADP(+)-dependent geraniol dehydrogenase (EC 1.1.1.183) is an enzyme that catalyzes the oxidation of geraniol to geranial. Stable, highly active cell-free extract was obtained from Polygonum minus leaves using polyvinylpolypyrrolidone, Amberlite XAD-4, glycerol, 2-mercaptoethanol, thiourea, and phenylmethylsulfonylfluoride in tricine-NaOH buffer (pH 7.5). The enzyme preparation was separated into two activity peaks, geraniol-DH I and II, by DEAE-Toyopearl 650M column chromatography at pH 7.5. Both isoenzymes were purified to homogeneity in three chromatographic steps. The geraniol-DH isoenzymes were similar in molecular mass, optimal temperature, and pH, but the isoelectric point, substrate specificity, and kinetic parameters were different. The K(m) values for geraniol of geraniol-DH I and II appeared to be 0.4 mM and 0.185 mM respectively. P. minus geraniol-DHs are unusual among geraniol-DHs in view of their thermal stability and optimal temperatures, and also their high specificity for allylic alcohols and NADP(+).

  1. Characterization of a novel chelating resin of enhanced hydrophilicity and its analytical utility for preconcentration of trace metal ions.

    PubMed

    Islam, Aminul; Laskar, Mohammad Asaduddin; Ahmad, Akil

    2010-06-15

    A stable extractor of metal ions was synthesized through azo linking of p-hydroxybenzoic acid with Amberlite XAD-4 and was characterized by elemental analyses, infrared spectral and thermal studies. Its water regain value and hydrogen ion capacity were found to be 15.80 and 7.52mmolg(-1), respectively. Both batch and column methods were employed to study the sorption behavior for the metal ions which were subsequently determined by flame atomic absorption spectrophotometry. The optimum pH range for Co(II), Ni(II), Cu(II), Zn(II), and Pb(II) ions were 10.0, 8.0-9.0, 7.0, 7.0-8.0 and 7.0-8.0, respectively. The half-loading time, t(1/2), are 6.0, 8.0, 8.0, 8.0 and 4.0min, respectively. Comparison of breakthrough and overall capacities of the metals ascertains the high degree of column utilization (>75%). The breakthrough capacities for Co(II), Ni(II), Cu(II), Zn(II), and Pb(II) ions were found to be 0.46, 0.43, 0.42, 0.09 and 0.06mmolg(-1) with the corresponding preconcentration factor of 460, 460, 460, 360 and 260, respectively. The limit of preconcentration was in the range of 4.3-7.6microgL(-1). The detection limit for Co(II), Ni(II), Cu(II), Zn(II) and Pb(II) were found to be 0.47, 0.45, 0.50, 0.80, and 1.37microgL(-1), respectively. The Student's t (t-test) values for the analysis of standard reference materials were found to be less than the critical Student's t values at 95% confidence level. The AXAD-4-HBA has been successfully applied for the analysis of natural water, multivitamin formulation, infant milk substitute, hydrogenated oil and fish.

  2. [The problem of hemoperfusion in poisonings: ineffectiveness in maprotiline poisoning].

    PubMed

    Hofmann, V; Riess, W; Descoeudres, C; Studer, H

    1980-02-23

    A case of self-poisoning with maprotiline presenting with coma stage III was treated by resin hemoperfusion for 9 hours using an XAD-4 resin cartridge. Plasma levels of about 800 ng/ml maprotilin were initially found. After 5 hours of hemoperfusion progredient clinical improvement was noticed without decreasing tendency of the blood drug levels. The theoretical extraction efficiency calculated from the maprotiline blood levels and the perfusion rate yielded 50 mg for maprotiline and 16 mg for desmethylmaprotiline and was in good agreement with 60.5 mg of maprotiline and 17.3 mg of desmethylmaprotiline recovered from the resin cartridge at the end of the hemoperfusion. The in vitro binding capacity for maprotiline was estimated to be 230 mg per g of resin. These results demonstrate that XAD-4 resin efficiently binds maprotiline. However, because of the very low blood concentrations due to the large volume of distribution, whole body concentrations are minimally affected by resin hemoperfusion. Main complications consisted in thrombocytopenia extending over 24 hours after stopping hemoperfusion, anemia, a short initial decrease of blood pressure and an episode of premature ventricular beats.

  3. Concentrations and distributions of metals associated with dissolved organic matter from the Suwannee River (GA, USA)

    USGS Publications Warehouse

    Kuhn, M. Keshia; Neubauer, Elisabeth; Hofmann, Thilo; von der Kammer, Frank; Aiken, George R.; Maurice, Patricia A.

    2015-01-01

    Concentrations and distributions of metals in Suwannee River (SR) raw filtered surface water (RFSW) and dissolved organic matter (DOM) processed by reverse osmosis (RO), XAD-8 resin (for humic and fulvic acids [FA]), and XAD-4 resin (for “transphilic” acids) were analyzed by asymmetrical flow field-flow fractionation (AsFlFFF). SR samples were compared with DOM samples from Nelson's Creek (NLC), a wetland-draining stream in northern Michigan; previous International Humic Substances Society (IHSS) FA and RO samples from the SR; and an XAD-8 sample from Lake Fryxell (LF), Antarctica. Despite application of cation exchange during sample processing, all XAD and RO samples contained substantial metal concentrations. AsFlFFF fractograms allowed metal distributions to be characterized as a function of DOM component molecular weight (MW). In SR RFSW, Fe, Al, and Cu were primarily associated with intermediate to higher than average MW DOM components. SR RO, XAD-8, and XAD-4 samples from May 2012 showed similar MW trends for Fe and Al but Cu tended to associate more with lower MW DOM. LF DOM had abundant Cu and Zn, perhaps due to amine groups that should be present due to its primarily algal origins. None of the fractograms showed obvious evidence for mineral nanoparticles, although some very small mineral nanoparticles might have been present at trace concentrations. This research suggests that AsFlFFF is important for understanding how metals are distributed in different DOM samples (including IHSS samples), which may be key to metal reactivity and bioavailability.

  4. ISOLATING AND EVALUATING ORGANIC TOXICANTS IN SEDIMENTS: EVALUATION OF AN EXPERIMENTAL APPROACH

    EPA Science Inventory

    Most solid-phase sediment toxicity identification and evaluation (TIE) techniques for organic chemicals have been focused on solid phase sorptive techniques, such as amending contaminated sediments with the carbonaceous resin, Ambersorb, coconut charcoal, or XAD resin to reduce t...

  5. Selective concentration of aromatic bases from water with a resin adsorbent

    USGS Publications Warehouse

    Stuber, H.A.; Leenheer, J.A.

    1983-01-01

    Aromatic bases are concentrated from water on columns of a resin adsorbent and recovered by aqueous-acid elution. The degree of concentration attainable depends on the ratio of the capacity factor (k) of the neutral form of the amine to that of the ionized form. Capacity factors of ionic forms of amines on XAD-8 resin (a methylacrylic ester polymer) are greater than zero, ranging from 20 to 250 times lower than those of their neutral forms; they increase with increasing hydrophobicity of the amine. Thus, desorption by acid is an edition (k during desorption >0) rather than a displacement (k during desorption = 0) process. The degree of concentration attainable on XAD-8 resin varies with the hydrophobicity of the amine, being limited for hydrophilic solutes (for example, pyridine) by small neutral-form k's, reaching a maximum for amines of intermediate hydrophobicity (for example, quinoline), and decreasing for more hydrophobc solutes (for example, acridine) because of their large ionic-form k's.

  6. Treatment of aqueous diethyl phthalate by adsorption using a functional polymer resin.

    PubMed

    Xu, Zhengwen; Zhang, Weiming; Pan, Bingcai; Lv, Lu; Jiang, Zhengmao

    2011-01-01

    To study the adsorptive separation efficiency, adsorption and desorption performances of diethyl phthalate (DEP) were investigated with a functional polymer resin (NDA-702). A macroporous polymer resin (XAD-4) and a coal-based granular activated carbon (AC-750) were chosen for comparison. The kinetic adsorption data obeyed the pseudo-second-order rate model, and the adsorption processes were limited by both film and intraparticle diffusions. Adsorption equilibrium data were well fitted by the Freundlich equation, and the larger uptake and higher selection of NDA-702 than AC-750 and XAD-4 was probably due to the microporous structure, phenyl rings and polar groups on NDA-702. Thermodynamic adsorption studies indicated that the test adsorbents spontaneously adsorbed DEP, driven mainly by enthalpy change. Continuous fixed-bed runs demonstrated that there no significant loss of the resin's adsorption capacity and there was complete regeneration of NDA-702. The results suggest that NDA-702 has excellent potential as an adsorption material for water treatment.

  7. Ellagitannins from Raspberry (Rubus idaeus L.) Fruit as Natural Inhibitors of Geotrichum candidum.

    PubMed

    Klewicka, Elżbieta; Sójka, Michał; Klewicki, Robert; Kołodziejczyk, Krzysztof; Lipińska, Lidia; Nowak, Adriana

    2016-07-13

    The paper presents the chemical characteristics of ellagitannins isolated from raspberry (Rubus idaeus L.) fruit and their in vitro and in situ antifungal activity against Geotrichum candidum ŁOCK 0511. The study investigated a complex preparation containing various raspberry ellagitannins at a concentration of 86% w/w, as well as pure lambertianin C and sanguiin H-6. The ellagitannin preparation was obtained by extracting raspberry press cake and purifying the extract using Amberlite XAD resin, while individual compounds were isolated by means of preparative HPLC. The complex preparation was analyzed for the content of ellagitannins, anthocyanins, and flavan-3-ols using HPLC and LC-MS. The antifungal activity of the complex ellagitannin preparation and the isolated ellagitannins was determined for the strain Geotrichum candidum. The MIC and MFC values (10.0 mg/mL and 30.0 mg/mL, respectively) were found to be the same for lambertianin C, sanguiin H-6, and the complex ellagitannin preparation. The fungistatic activity of the studied ellagitannin preparation at a concentration of 10 mg/mL, as determined by the poisoned medium method, was 65.2% following 6 day incubation of Geotrichum candidum, with the linear growth rate of only 16.2 mm/day. The corresponding parameters for the control sample were 0% and 56 mm/day, respectively. The study demonstrated both in vitro and in situ antifungal activity of raspberry ellagitannins against Geotrichum candidum.

  8. EFFECT OF THE DECHLORINATING AGENT, ASCORBIC ACID, ON THE MUTAGENICITY OF CHLORINATED WATER SAMPLES

    EPA Science Inventory

    XAD resin adsorption has been widely used to concentrate the organic compounds present in chlorinated drinking waters prior to mutagenicity testing. Previous work has shown that mutagenic artifcats can arise due to the reaction of residual chlorine with the resins. Althrough the ...

  9. Reproductive responses of male fathead minnows exposed to wastewater treatment plant effluent, effluent treated with XAD8 resin, and an environmentally relevant mixture of alkylphenol compounds

    USGS Publications Warehouse

    Barber, L.B.; Lee, K.E.; Swackhamer, D.L.; Schoenfuss, H.L.

    2007-01-01

    On-site, continuous-flow experiments were conducted during August and October 2002 at a major metropolitan wastewater treatment plant (WWTP) to determine if effluent exposure induced endocrine disruption as manifested in the reproductive competence of sexually mature male fathead minnows (Pimephales promelas). The fathead minnows were exposed in parallel experiments to WWTP effluent and WWTP effluent treated with XAD8 macroreticular resin to remove the hydrophobic-neutral fraction which contained steroidal hormones, alkylphenolethoxylates (APEs), and other potential endocrine disrupting compounds (EDCs). The effluent composition varied on a temporal scale and the continuous-flow experiments captured the range of chemical variability that occurred during normal WWTP operations. Exposure to WWTP effluent resulted in vitellogenin induction in male fathead minnows, with greater response in October than in August. Concentrations of ammonia, APEs, 17??-estradiol, and other EDCs also were greater in October than in August, reflecting a change in effluent composition. In the October experiment, XAD8 treatment significantly reduced vitellogenin induction in the male fathead minnows relative to the untreated effluent, whereas in August, XAD8 treatment had little effect. During both experiments, XAD8 treatment removed greater than 90% of the APEs. Exposure of fish to a mixture of APEs similar in composition and concentration to the WWTP effluent, but prepared in groundwater and conducted at a separate facility, elicited vitellogenin induction during both experiments. There was a positive relation between vitellogenin induction and hepatosomatic index (HSI), but not gonadosomatic index (GSI), secondary sexual characteristics index (SSCI), or reproductive competency. In contrast to expectations, the GSI and SSCI increased in males exposed to WWTP effluent compared to groundwater controls. The GSI, SSCI, and reproductive competency were positively affected by XAD8 treatment of the WWTP effluent. ?? 2007 Elsevier B.V. All rights reserved.

  10. Reproductive responses of male fathead minnows exposed to wastewater treatment plant effluent, effluent treated with XAD8 resin, and an environmentally relevant mixture of alkylphenol compounds.

    PubMed

    Barber, Larry B; Lee, Kathy E; Swackhamer, Deborah L; Schoenfuss, Heiko L

    2007-04-20

    On-site, continuous-flow experiments were conducted during August and October 2002 at a major metropolitan wastewater treatment plant (WWTP) to determine if effluent exposure induced endocrine disruption as manifested in the reproductive competence of sexually mature male fathead minnows (Pimephales promelas). The fathead minnows were exposed in parallel experiments to WWTP effluent and WWTP effluent treated with XAD8 macroreticular resin to remove the hydrophobic-neutral fraction which contained steroidal hormones, alkylphenolethoxylates (APEs), and other potential endocrine disrupting compounds (EDCs). The effluent composition varied on a temporal scale and the continuous-flow experiments captured the range of chemical variability that occurred during normal WWTP operations. Exposure to WWTP effluent resulted in vitellogenin induction in male fathead minnows, with greater response in October than in August. Concentrations of ammonia, APEs, 17beta-estradiol, and other EDCs also were greater in October than in August, reflecting a change in effluent composition. In the October experiment, XAD8 treatment significantly reduced vitellogenin induction in the male fathead minnows relative to the untreated effluent, whereas in August, XAD8 treatment had little effect. During both experiments, XAD8 treatment removed greater than 90% of the APEs. Exposure of fish to a mixture of APEs similar in composition and concentration to the WWTP effluent, but prepared in groundwater and conducted at a separate facility, elicited vitellogenin induction during both experiments. There was a positive relation between vitellogenin induction and hepatosomatic index (HSI), but not gonadosomatic index (GSI), secondary sexual characteristics index (SSCI), or reproductive competency. In contrast to expectations, the GSI and SSCI increased in males exposed to WWTP effluent compared to groundwater controls. The GSI, SSCI, and reproductive competency were positively affected by XAD8 treatment of the WWTP effluent.

  11. Fractional, biodegradable and spectral characteristics of extracted and fractionated sludge extracellular polymeric substances.

    PubMed

    Wei, Liang-Liang; Wang, Kun; Zhao, Qing-Liang; Jiang, Jun-Qiu; Kong, Xiang-Juan; Lee, Duu-Jong

    2012-09-15

    Correlation between fractional, biodegradable and spectral characteristics of sludge extracellular polymeric substances (EPS) by different protocols has not been well established. This work extracted sludge EPS using alkaline extractants (NH₄OH and formaldehyde + NaOH) and physical protocols (ultrasonication, heating at 80 °C or cation exchange resin (CER)) and then fractionated the extracts using XAD-8/XAD-4 resins. The alkaline extractants yielded more sludge EPS than the physical protocols. However, the physical protocols extracted principally the hydrophilic components which were readily biodegradable by microorganisms. The alkaline extractants dissolved additional humic-like substances from sludge solids which were refractory in nature. Different extraction protocols preferably extracted EPS with distinct fractional, biodegradable and spectral characteristics which could be applied in specific usages. Copyright © 2012 Elsevier Ltd. All rights reserved.

  12. An efficient green synthesis of 2-arylbenzothiazole analogues as potent antibacterial and anticancer agents.

    PubMed

    Chhabra, Mohit; Sinha, Sohini; Banerjee, Swagata; Paira, Priyankar

    2016-01-01

    We have demonstrated a novel and green approach for the synthesis of 2-substituted benzothiazole analogues. A number of 2-aryl and heteroaryl benzothiazole scaffolds were synthesized using Amberlite IR-120 resin under microwave irradiation. The catalytic role and reusability of the resin was well established here. 2-Substituted benzothiazole analogues (3a-l) were also tested against several bacterial strains (Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Salmonella) and cancer cell lines (MCF-7 and HeLa). The stability of compound 2-phenyl benzothiazole (3a) and 2-pyridin-2-yl-benzothiazole (3k) in GSH (0.01mM dissolved in DMSO) was measured by UV-Vis spectroscopy. Compound 3k also shows remarkable fluorescence in MeOH. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Chemistry and potential mutagenicity of humic substances in waters from different watersheds in Britain and Ireland

    USGS Publications Warehouse

    Watt, B.E.; Malcolm, R.L.; Hayes, M.H.B.; Clark, N.W.E.; Chipman, J.K.

    1996-01-01

    Humic substances are amorphous organic macromolecules responsible for the hue of natural waters. They are also known to be precursors of mutagens formed on chlorination prior to distribution of drinking water. In this study humic substances from the waters of primary streams, from major rivers, and from reservoirs were isolated and fractionated into humic acids (HA), fulvic acids (FA) and XAD-4 acids using columns of XAD-8 and of XAD-4 resins in tandem, and the fractions from the different sources were chlorinated and assayed for mutagenicity. CPMAS 13C NMR spectroscopy showed marked differences in compositions not only between HA, FA, and XAD-4 acids from the same water samples, but also between the same fractions from water samples from different watersheds. There were found to be strong similarities between the fractions from watersheds which had closely related soil types. Aromaticity was greatest in HAs, and lowest in XAD-4 acids, and carboxyl contents and aliphatic character were greatest in the XAD-4 acids. Carbon content decreased in the order HA > FA > XAD-4 acids, and amino acids and neutral sugars contents decreased in the order HA > XAD-4 > FA. Titration data complemented aspects of the NMR data, demonstrating that carboxyl content decreased in the order XAD-4 acids > FA > HA, and indicated that phenolic character was highest in HAs and lowest in the XAD-4 acids. All samples tested gave rise to bacterial mutagens on chlorination. Although the mutagenicities were of the same order of magnitude for the chlorinated humic samples from the different sources, the samples which showed the greatest number of revertant bacterial colonies were from the Thames and Trent, large rivers with humic materials from diverse environments, and relatively high in amino acid contents.

  14. Denuder sampling techniques for the determination of gas-phase carbonyl compounds: a comparison and characterisation of in situ and ex situ derivatisation methods.

    PubMed

    Kahnt, Ariane; Iinuma, Yoshiteru; Böge, Olaf; Mutzel, Anke; Herrmann, Hartmut

    2011-05-15

    Two denuder sampling techniques have been compared for the analysis of gaseous carbonyl compounds. One type of denuder was coated with XAD-4 resin and the other type of denuder was coated with XAD-4 and 2,4-dinitrophenylhydrazine (DNPH) to derivatise gaseous carbonyl compounds to their hydrazone forms simultaneously. A detailed protocol for the denuder coating procedure is described. The collection efficiency under dry (RH <3%) and humid conditions (RH 50%) as well as filter positive artefacts were evaluated. The XAD-4/DNPH coated denuders showed significantly less break-through potential and hence collection than the XAD-4-only coated denuders. The performance of the XAD-4/DNPH denuder was better under humid conditions with no detected break-through for hydroxyacetone, methacrolein, methylglyoxal, campholenic aldehyde and nopinone. Calibration experiments were performed in a simulation chamber and carbonyl-hydrazone concentrations determined in the extracts of both the denuder types were related to the mixing ratios of gaseous carbonyl compounds in the chamber to overcome losses and errors associating with the denuder sampling, extraction and sample preparation. The application of on-tube conversion for the XAD-4/DNPH denuders resulted in higher R(2) values than the XAD-4 denuder, ranging up to 0.991 for nopinone. The XAD-4-only coated denuders showed acceptable calibration curves only for lower vapour pressure carbonyl compounds though larger relative standard deviations (RSD) were observed. Carbonyl compounds that were formed during the oxidation of nopinone were collected using the XAD-4/DNPH denuders. The results showed that the denuder sampling device was able to provide reproducible nopinone mixing ratios that remained in the chamber after about 1h of the oxidation. One isomer of oxo-nopinones was tentatively identified from off-line HPLC/(-)ESI-TOFMS analysis. Based on the TOFMS response of the nopinone-DNPH derivative, the oxo-nopinone molar yield of 0.7±0.1% (n=3) was determined from the reaction of nopinone with OH radicals. Depending on target analytes, accuracy and sensitivity requirements, the present method can be employed for the determination of gaseous carbonyl compounds that are formed during the oxidation of monoterpenes. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. On the real performance of cation exchange resins in wastewater treatment under conditions of cation competition: the case of heavy metal pollution.

    PubMed

    Prelot, Benedicte; Ayed, Imen; Marchandeau, Franck; Zajac, Jerzy

    2014-01-01

    Sorption performance of cation-exchange resins Amberlite® IRN77 and Amberlite™ IRN9652 toward Cs(I) and Sr(II) has been tested in single-component aqueous solutions and simulated waste effluents containing other monovalent (Effluent 1) or divalent (Effluent 2) metal cations, as well as nitrate, borate, or carbonate anions. The individual sorption isotherms of each main component were measured by the solution depletion method. The differential molar enthalpy changes accompanying the ion-exchange between Cs+ or Sr2+ ions and protons at the resin surface from single-component nitrate solutions were measured by isothermal titration calorimetry and they showed a higher specificity of the two resins toward cesium. Compared to the retention limits of both resins under such idealized conditions, an important depression in the maximum adsorption capacity toward each main component was observed in multication systems. The overall effect of ion exchange process appeared to be an unpredictable outcome of the individual sorption capacities of the two resins toward various cations as a function of the cation charge, size, and concentration. The cesium retention capacity of the resins was diminished to about 25% of the "ideal" value in Effluent 1 and 50% in Effluent 2; a further decrease to about 15% was observed upon concomitant strontium addition. The uptake of strontium by the resins was found to be less sensitive to the addition of other metal components: the greatest decrease in the amount adsorbed was 60% of the ideal value in the two effluents for Amberlite® IRN77 and 75% for Amberlite™ IRN9652. It was therefore demonstrated that any performance tests carried out under idealized conditions should be exploited with much caution to predict the real performance of cation exchange resins under conditions of cation competition.

  16. Adsorption induced enzyme denaturation: the role of polymer hydrophobicity in adsorption and denaturation of alpha-chymotrypsin on allyl glycidyl ether (AGE)-ethylene glycol dimethacrylate (EGDM) copolymers.

    PubMed

    Lahari, Challa; Jasti, Lakshmi S; Fadnavis, Nitin W; Sontakke, Kalpana; Ingavle, Ganesh; Deokar, Sarika; Ponrathnam, Surendra

    2010-01-19

    Effects of changes in hydrophobicity of polymeric support on structure and activity of alpha-chymotrypsin (E.C. 3.4.21.1) have been studied with copolymers of allyl glycidyl ether (AGE) and ethylene glycol dimethacrylate (EGDM) with increasing molar ratio of EGDM to AGE (cross-link density 0.05 to 1.5). The enzyme is readily adsorbed from aqueous buffer at room temperature following Langmuir adsorption isotherms in unexpectedly large amounts (25% w/w). Relative hydrophobicity of the copolymers has been assessed by studying adsorption of naphthalene and Fmoc-methionine by the series of copolymers from aqueous solutions. Polymer hydrophobicity appears to increase linearly on increasing cross-link density from 0.05 to 0.25. Further increase in cross-link density causes a decrease in naphthalene binding but has little effect on binding of Fmoc-Met. Binding of alpha-chymotrypsin to these copolymers follow the trend for Fmoc-methionine binding, rather than naphthalene binding, indicating involvement of polar interactions along with hydrophobic interactions during binding of protein to the polymer. The adsorbed enzyme undergoes extensive denaturation (ca. 80%) with loss of both tertiary and secondary structure on contact with the copolymers as revealed by fluorescence, CD and Raman spectra of the adsorbed protein. Comparison of enzyme adsorption behavior with Eupergit C, macroporous Amberlite XAD-2, and XAD-7 suggests that polar interactions of the EGDM ester functional groups with the protein play a significant role in enzyme denaturation.

  17. Trace analysis of endocrine disrupting compounds in environmental water samples by use of solid-phase extraction and gas chromatography with mass spectrometry detection.

    PubMed

    Azzouz, Abdelmonaim; Ballesteros, Evaristo

    2014-09-19

    A novel analytical method using a continuous solid-phase extraction system in combination with gas chromatography-mass spectrometry for the simultaneous separation and determination of endocrine disrupting compounds (EDCs) is reported. The method was applied to major EDCs of various types including parabens, alkylphenols, phenylphenols, bisphenol A and triclosan in water. Samples were preconcentrated by using an automatic solid-phase extraction module containing a sorbent column, and retained analytes eluted with acetonitrile for derivatization with a mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and trimethylchlorosilane. A number of variables potentially influencing recovery of the target compounds such as the type of SPE sorbent (Silica gel, Florisil, RP-C18, Amberlite XAD-2 and XAD-4, Oasis HLB and LiChrolut EN), eluent and properties of the water including pH and ionic strength, were examined. LiChrolut EN was found to be the most efficient sorbent for retaining the analytes, with ∼100% efficiency. The ensuing method was validated with good analytical results including low limits of detection (0.01-0.08ng/L for 100mL of sample) and good linearity (r(2)>0.997) throughout the studied concentration ranges. The method exhibited good accuracy (recoveries of 90-101%) and precision (relative standard deviations less than 7%) in the determination of EDCs in drinking, river, pond, well, swimming pool and waste water. Waste water samples were found to contain the largest number and highest concentrations of analytes (3.2-390ng/L). Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Genotoxicity of wastewaters used for irrigation of food crops.

    PubMed

    Ansari, Mohd Ikram; Malik, Abdul

    2009-04-01

    In most towns of India, wastewater coming from both industrial and domestic sources and without any treatment is used to irrigate the agricultural crops. This practice has been polluting the soil, and pollutants could possibly reach the food chain. For the above reasons, the wastewaters of Ghaziabad City (India), which is used for irrigation, were sampled (at two different sites) and monitored for the presence of genotoxic agents from January 2005 to June 2007. Gas chromatographic analysis showed the presence of certain OC (DDE, DDT, Dieldrin, Aldrin, and Endosulfan) and OP (Dimethoate, Malathion, Methlyparathion, and Chlorpyrifos) pesticides in both the sampling sites. Wastewater samples were concentrated using XAD resins (XAD-4 and XAD-8) and liquid-liquid extraction procedures, and the extracts were assayed for genotoxic potential by Ames Salmonella/microsome test, DNA repair defective mutants, and bacteriophage lambda systems. The test samples exhibited significant mutagenicity with TA98, TA97a, and TA100 strains with the probable role of contaminating pesticides in the wastewater. However, XAD-concentrated samples were more mutagenic in both sites as compared to liquid-liquid-extracted samples. The damage in the DNA repair defective mutants in the presence of XAD-concentrated water samples were also found to be higher to that of liquid-liquid-extracted water samples at the dose level of 20 muL/mL culture. All the mutants invariably exhibited significant decline in their colony-forming units as compared to their isogenic wild-type counterparts. The survival was decreased by 81.7 and 75.5% in polA(-) strain in site I, and 76.0 and 73.5% in site II in polA(-) under the same experimental conditions after 6 h of treatment with XAD-concentrated and liquid-liquid-extracted samples, respectively. A significant decrease in the survival of bacteriophage lambda was also observed when treated with the test samples. Copyright 2008 Wiley Periodicals, Inc.

  19. Characterization and copper binding of humic and nonhumic organic matter isolated from the South Platte River: Evidence for the presence of nitrogenous binding site

    USGS Publications Warehouse

    Croue, J.-P.; Benedetti, M.F.; Violleau, D.; Leenheer, J.A.

    2003-01-01

    Humic substances typically constitute 40-60% of the dissolved organic matter (DOM) in surface waters. However, little information is available regarding the metal binding properties of the nonhumic hydrophilic portion of the DOM. In this study, humic and nonhumic DOM samples were isolated from the South Platte River (Colorado, DOC = 2.6 mg??L-1, SUVA254 = 2.4 L/mg??m) using a two-column array of XAD-8 and XAD-4 resins. The three major isolated fractions of DOM, which accounted for 57% of the bulk DOM, were characterized using a variety of analytical tools. Proton and copper binding properties were studied for each fraction. The main objective of this work was to compare the structural and chemical characteristics of the isolated fractions and test models describing DOM reactivity toward metal ions. The characterization work showed significant structural differences between the three isolated fractions of DOM. The hydrophobic acid fraction (i.e., humic substances isolated from the XAD-8 resin) gave the largest C/H, C/O, and C/N ratios and aromatic carbon content among the three isolated fractions. The transphilic acid (TPHA) fraction ("transphilic" meaning fraction of intermediate polarity isolated from the XAD-4 resin) was found to incorporate the highest proportion of polysaccharides, whereas the transphilic neutral (TPHN) fraction was almost entirely proteinaceous. The gradual increase of the charge with pH for the three DOM fractions is most likely caused by a large distribution of proton affinity constants for the carboxylic groups, as well as a second type of group more generally considered to be phenolic. In the case of the DOM fraction enriched in proteinaceous material (i.e., TPHN fraction), the results showed that the amino groups are reponsible for the charge reversal. For low copper concentrations, nitrogen-containing functional groups similar to those of amino acids are likely to be involved in complexation, in agreement with previously published data.

  20. Comparison of methods to determine selenium species in saturation extracts of soils from the western San Joaquin Valley, California

    USGS Publications Warehouse

    Fio, John L.; Fujii, Roger

    1988-01-01

    Undigested organic matter in some of the extracts inhibited selenium detection when using the digestion and Sep-Pac C18 methods, but the interference was removed by using the XAD-8 method. Combining XAD-8 resin and activated charcoal was an unacceptable method, because the activated charcoal removed selenite and selenate. Ninety-eight percent of the selenium in the extracts was selenate and about 100 percent of the isolated organic selenium was associated with the humic acid fraction of dissolved-organic matter.

  1. Neutron Activated Samarium-153 Microparticles for Transarterial Radioembolization of Liver Tumour with Post-Procedure Imaging Capabilities

    PubMed Central

    Hashikin, Nurul Ab. Aziz; Yeong, Chai-Hong; Abdullah, Basri Johan Jeet; Ng, Kwan-Hoong; Chung, Lip-Yong; Dahalan, Rehir; Perkins, Alan Christopher

    2015-01-01

    Introduction Samarium-153 (153Sm) styrene divinylbenzene microparticles were developed as a surrogate for Yttrium-90 (90Y) microspheres in liver radioembolization therapy. Unlike the pure beta emitter 90Y, 153Sm possess both therapeutic beta and diagnostic gamma radiations, making it possible for post-procedure imaging following therapy. Methods The microparticles were prepared using commercially available cation exchange resin, Amberlite IR-120 H+ (620–830 μm), which were reduced to 20–40 μm via ball mill grinding and sieve separation. The microparticles were labelled with 152Sm via ion exchange process with 152SmCl3, prior to neutron activation to produce radioactive 153Sm through 152Sm(n,γ)153Sm reaction. Therapeutic activity of 3 GBq was referred based on the recommended activity used in 90Y-microspheres therapy. The samples were irradiated in 1.494 x 1012 n.cm-2.s-1 neutron flux for 6 h to achieve the nominal activity of 3.1 GBq.g-1. Physicochemical characterisation of the microparticles, gamma spectrometry, and in vitro radiolabelling studies were carried out to study the performance and stability of the microparticles. Results Fourier Transform Infrared (FTIR) spectroscopy of the Amberlite IR-120 resins showed unaffected functional groups, following size reduction of the beads. However, as shown by the electron microscope, the microparticles were irregular in shape. The radioactivity achieved after 6 h neutron activation was 3.104 ± 0.029 GBq. The specific activity per microparticle was 53.855 ± 0.503 Bq. Gamma spectrometry and elemental analysis showed no radioactive impurities in the samples. Radiolabelling efficiencies of 153Sm-Amberlite in distilled water and blood plasma over 48 h were excellent and higher than 95%. Conclusion The laboratory work revealed that the 153Sm-Amberlite microparticles demonstrated superior characteristics for potential use in hepatic radioembolization. PMID:26382059

  2. Structural properties of dissolved organic carbon in deep horizons of an arable soil.

    NASA Astrophysics Data System (ADS)

    Lavaud, A.; Croué, Jp; Berwick, L.; Steffens, M.; Chabbi, A.

    2010-05-01

    The objective of this work is to quantity the DOC that percolates in deep horizons of an arable soil, and to characterize the structural properties of the main fractions. The study was conducted on the long term observatory for environmental research- biogeochemical cycles and biodiversity Lusignan site-France. DOC collected using lysimeter plates inserted to a depth of 105 cm was fractionated into 3 fractions using the two column array of XAD-8 and XAD-4 resins. The HPO (hydrophobic) fraction (i.e. humic substances) isolated from the XAD-8 resin, the TPH (Transphilic) fraction from the XAD-4 resin and the HPI (hydrophilic) fraction which corresponds to the DOC that does not adsorbed onto the two resins under the acid condition used (pH 2). DOM adsorbed onto the resins is recovered with a 75%/25% acetonitrile/water mixture and lyophilized. The hydrophilic fraction is purified according the protocol proposed by Aiken and Leenheer (1993). The isolated fractions were subjected to several characterization tools: UV/Vis, fluorescence EEM, HPSEC/UV/DOC, 13C NMR, 14C dating, FT-IR, pyrolysis, thermochemolysis and MSSV GC/MS. The DOC content ranged from 1 to 2.5 mg / L between winter and the middle of spring and then to 4-5 mg / L in summer time. For all isolated fractions HPSEC analyses indicated the predominance of low molecular structures with a low aromatic character. Fluorescence EEM confirmed the non-humic character of the DOM. 13C-NMR spectra showed that the aromatic character decreased from HPO to TPH, and HPI character. Molecular size follows the same trend. HPI DOM was found to be strongly enriched in carboxyl groups. The 14C concentration of the HPO fraction corresponds to an apparent calibrated age around AD 1500. For the same fraction isolated from the 0 - 30 cm horizon, the measured 14C concentration 131.9 pMC corresponds to that in the atmosphere around AD 1978. Significant input of terpenoid derived organic matter was confirmed in the HPO fraction of DOC, results supported by the data of 13C NMR, FT-IR and Micro Scale Sealed Vessel / pyrolysis GC / MS. Flash pyrolysis GC / MS chromatogram highlight the presence of phenol and alkyl phenols, generally attributed to structures polyhydroxyaromatic structures. Acetamide, a pyrolysis product of amino sugars constituents of microbial cell wall is also significantly present. The thermochimiolysis (TMAH)/GC/ MS confirmed the presence of hydroxy aromatic structures in the extracts; however, their precise origin (lignin, tannins ...) remains uncertain.

  3. Application of the diffusive gradients in thin films technique for available potassium measurement in agricultural soils: effects of competing cations on potassium uptake by the resin gel.

    PubMed

    Zhang, Yulin; Mason, Sean; McNeill, Ann; McLaughlin, Michael J

    2014-09-09

    The utilization of Amberlite (IRP-69 ion-exchange resin, 100-500 wet mesh) as the binding phase in the diffusive gradients in thin films (DGT) technique has shown potential to improve the assessment of plant-available K in soils. The binding phase has recently been optimized by using a mixed Amberlite and ferrihydrite (MAF) gel which results in linear K uptake over extended deployment periods and in solutions with higher K concentrations. As restriction of K uptake by Ca on the Amberlite based resin gel has been previously proposed, potential competing effects of Ca(2+), Mg(2+) and NH(4+) on K uptake by the MAF gel were investigated. These cations had no effect on K elution efficiency which was 85%. However, K uptake by the MAF gel was restricted in the presence of competing cations in solution. Consequently, the diffusion coefficient of K decreased in the presence of cations compared to previous studies but was stable at 1.12×10(-5)cm(2)s(-1) at 25°C regardless of cation concentrations. Uptake of K by the DGT device was affected by the presence of excessive Ca in more than 30% of twenty typical Australian agricultural soils. However, this problem could be circumvented by using a shorter deployment time than the normal 24 h. Moderate correlation of concentrations of K extracted by DGT with Colwell K (extracted by NaHCO(3), R(2)=0.69) and NH4OAc K (R(2)=0.61) indicates that DGT measures a different pool of K in soils than that measured by the standard extractants used. In addition, the MAF gel has the ability to measure Ca and Mg simultaneously. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Selenium speciation methods and application to soil saturation extracts from San Joaquin Valley, California

    USGS Publications Warehouse

    Fio, John L.; Fujii, Roger

    1990-01-01

    Methods to determine soluble concentrations of selenite, selenate, and organic Se were evaluated on saturation extracts of soil samples collected from three sites on the Panoche Creek alluvial fan in the western San Joaquin Valley, California. The methods were used in combination with hydride-generation atomic-absorption spectrometry for detection of Se, and included a selective chemical-digestion method and three chromatographic methods using XAD-8 resin, Sep-Pak C18 cartridge, and a combination of XAD-8 resin and activated charcoal. The chromatography methods isolate dissolved organic matter that can inhibit Se detection by hydride-generation atomic-absorption spectrometry. Isolation of hydrophobic organic matter with XAD-8 did not affect concentrations of selenite and selenate, and the isolated organic matter represents a minimal estimation of organic Se. Ninety-eight percent of the Se in the extracts was selenate and about 100% of the isolated organic Se was associated with the humic acid fraction of dissolved organic matter. The depth distribution of Se species in the soil saturation extracts support a hypothesis that the distribution of soluble Se and salinity in these soils is the result of evaporation from a shallow water table and leaching by irrigation water low in Se and salinity.

  5. A comparison of surface water natural organic matter in raw filtered water samples, XAD, and reverse osmosis isolates.

    PubMed

    Maurice, Patricia A; Pullin, Michael J; Cabaniss, Stephen E; Zhou, Qunhui; Namjesnik-Dejanovic, Ksenija; Aiken, George R

    2002-05-01

    This research compared raw filtered waters (RFWs), XAD resin isolates (XAD-8 and XAD-4), and reverse osmosis (RO) isolates of several surface water samples from McDonalds Branch, a small freshwater fen in the New Jersey Pine Barrens (USA). RO and XAD-8 are two of the most common techniques used to isolate natural organic matter (NOM) for studies of composition and reactivity; therefore, it is important to understand how the isolates differ from bulk (unisolated) samples and from one another. Although, any comparison between the isolation methods needs to consider that XAD-8 is specifically designed to isolate the humic fraction, whereas RO concentrates a broad range of organic matter and is not specific to humics. The comparison included for all samples: weight average molecular weight (Mw), number average molecular weight (Mn), polydispersity (rho), absorbance at 280 nm normalized to moles C (epsilon280) (RFW and isolates); and for isolates only: elemental analysis, % carbon distribution by 13C NMR, and aqueous FTIR spectra. As expected, RO isolation gave higher yield of NOM than XAD-8, but also higher ash content, especially Si and S. Mw decreased in the order: RO > XAD-8 > RFW > XAD-4. The Mw differences of isolates compared with RFW may be due to selective isolation (fractionation), or possibly in the case of RO to condensation or coagulation during isolation. 13C NMR results were roughly similar for the two methods, but the XAD-8 isolate was slightly higher in 'aromatic' C and the RO isolate was slightly higher in heteroaliphatic and carbonyl C. Infrared spectra indicated a higher carboxyl content for the XAD-8 isolates and a higher ester:carboxyl ratio for the RO isolates. The spectroscopic data thus are consistent with selective isolation of more hydrophobic compounds by XAD-8, and also with potential ester hydrolysis during that process, although further study is needed to determine whether ester hydrolysis does indeed occur. Researchers choosing between XAD and RO isolation methods for NOM need to consider first the purpose of the isolation; i.e., whether humic fractionation is desirable. Beyond that, they should consider the C yield and ash content, as well as the potential for alteration of NOM by ester hydrolysis (XAD) or condensation/coagulation (RO). Furthermore, the RO and XAD methods produce different fractions or isolates so that researchers should be careful when comparing the compositions and reactivities of NOM samples isolated by these two different techniques.

  6. A comparison of surface water natural organic matter in raw filtered water samples, XAD, and reverse osmosis isolates

    USGS Publications Warehouse

    Maurice, P.A.; Pullin, M.J.; Cabaniss, S.E.; Zhou, Q.; Namjesnik-Dejanovic, K.; Aiken, G.R.

    2002-01-01

    This research compared raw filtered waters (RFWs), XAD resin isolates (XAD-8 and XAD-4), and reverse osmosis (RO) isolates of several surface water samples from McDonalds Branch, a small freshwater fen in the New Jersey Pine Barrens (USA). RO and XAD-8 are two of the most common techniques used to isolate natural organic matter (NOM) for studies of composition and reactivity; therefore, it is important to understand how the isolates differ from bulk (unisolated) samples and from one another. Although, any comparison between the isolation methods needs to consider that XAD-8 is specifically designed to isolate the humic fraction, whereas RO concentrates a broad range of organic matter and is not specific to humics. The comparison included for all samples: weight average molecular weight (Mw), number average molecular weight (Mn), polydispersity (??), absorbance at 280nm normalized to moles C (??280) (RFW and isolates); and for isolates only: elemental analysis, % carbon distribution by 13C NMR, and aqueous FTIR spectra. As expected, RO isolation gave higher yield of NOM than XAD-8, but also higher ash content, especially Si and S. Mw decreased in the order: RO>XAD-8>RFW>XAD-4. The Mw differences of isolates compared with RFW may be due to selective isolation (fractionation), or possibly in the case of RO to condensation or coagulation during isolation. 13C NMR results were roughly similar for the two methods, but the XAD-8 isolate was slightly higher in 'aromatic' C and the RO isolate was slightly higher in heteroaliphatic and carbonyl C. Infrared spectra indicated a higher carboxyl content for the XAD-8 isolates and a higher ester:carboxyl ratio for the RO isolates. The spectroscopic data thus are consistent with selective isolation of more hydrophobic compounds by XAD-8, and also with potential ester hydrolysis during that process, although further study is needed to determine whether ester hydrolysis does indeed occur. Researchers choosing between XAD and RO isolation methods for NOM need to consider first the purpose of the isolation; i.e., whether humic fractionation is desirable. Beyond that, they should consider the C yield and ash content, as well as the potential for alteration of NOM by ester hydrolysis (XAD) or condensation/coagulation (RO). Furthermore, the RO and XAD methods produce different fractions or isolates so that researchers should be careful when comparing the compositions and reactivities of NOM samples isolated by these two different techniques. ?? 2002 Published by Elsevier Science Ltd.

  7. Field Calibration of XAD-Based Passive Air Sampler on the Tibetan Plateau: Wind Influence and Configuration Improvement.

    PubMed

    Gong, Ping; Wang, Xiaoping; Liu, Xiande; Wania, Frank

    2017-05-16

    The passive air sampler based on XAD-2 resin (XAD-PAS) has proven useful for collecting atmospheric persistent organic pollutants (POPs) in remote regions. Whereas laboratory studies have shown that, due to the open bottom of its housing, the passive sampling rate (PSR) of the XAD-PAS is susceptible to wind and other processes causing air turbulence, the sampler has not been calibrated in the field at sites experiencing high winds. In this study, the PSRs of the XAD-PAS were calibrated at three sites on the Tibetan Plateau, covering a wide range in temperature (T), pressure (P) and wind speed (v). At sites with low wind speeds (i.e., in a forest and an urban site), the PSRs are proportional to the ratio T 1.75 / P; at windy sites with an average wind speed above 3 m/s, the influence of v on PSRs cannot be ignored. Moreover, the open bottom of the XAD-PAS housing causes the PSRs to be influenced by wind angle and air turbulence caused by sloped terrain. Field calibration, wind speed measurements, and computational fluid dynamics (CFD) simulations indicate that a modified design incorporating an air spoiler consisting of 4 metal sheets dampens the turbulence caused by wind angle and sloped terrain and caps the PSR at ∼5 m 3 /day, irrespective of ambient wind. Therefore, the original XAD-PAS with an open bottom is suitable for deployment in urban areas and other less windy places, the modified design is preferable in mountain regions and other places where air circulation is complicated and strong.

  8. Antioxidant Activity of Mulberry Fruit Extracts

    PubMed Central

    Arfan, Muhammad; Khan, Rasool; Rybarczyk, Anna; Amarowicz, Ryszard

    2012-01-01

    Phenolic compounds were extracted from the fruits of Morus nigra and Morus alba using methanol and acetone. The sugar-free extracts (SFEs) were prepared using Amberlite XAD-16 column chromatography. All of the SFEs exhibited antioxidant potential as determined by ABTS (0.75–1.25 mmol Trolox/g), DPPH (2,2-diphenyl-1-picrylhydrazyl) (EC50 from 48 μg/mL to 79 μg/mL), and reducing power assays. However, a stronger activity was noted for the SFEs obtained from Morus nigra fruits. These extracts also possessed the highest contents of total phenolics: 164 mg/g (methanolic SFE) and 173 mg/g (acetonic SFE). The presence of phenolic acids and flavonoids in the extracts was confirmed using HPLC method and chlorogenic acid and rutin were found as the dominant phenolic constituents in the SFEs. PMID:22408465

  9. A Simplified Method for Sampling and Analysis of High Volume Surface Water for Organic Contaminants Using XAD-2

    USGS Publications Warehouse

    Datta, S.; Do, L.V.; Young, T.M.

    2004-01-01

    A simple compressed-gas driven system for field processing and extracting water for subsequent analyses of hydrophobic organic compounds is presented. The pumping device is a pneumatically driven pump and filtration system that can easily clarify at 4L/min. The extraction device uses compressed gas to drive filtered water through two parallel XAD-2 resin columns, at about 200 mL/min. No batteries or inverters are required for water collection or processing. Solvent extractions were performed directly in the XAD-2 glass columns. Final extracts are cleaned-up on Florisil cartridges without fractionation and contaminants analyzed by GC-MS. Method detection limits (MDLs) and recoveries for dissolved organic contaminants, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and pesticides are reported along with results of surface water analysis for the San Francisco Bay, CA.

  10. Comprehensive isolation of natural organic matter from water for spectral characterizations and reactivity testing

    USGS Publications Warehouse

    Leenheer, J.A.; Croue, J.-P.; Benjamin, M.; Korshin, G.V.; Hwang, C.J.; Bruchet, A.; Aiken, G.R.

    2000-01-01

    A variety of approaches were tested to comprehensively isolate natural organic matter (NOM) from water. For waters with high NOM concentrations such as the Suwannee River, Georgia, approaches that used combinations of membrane concentrations, evaporative concentrations, and adsorption on nonionic XAD resins, ion exchange resins and iron oxide coated sand isolated over 90% of the NOM. However, for waters with low NOM concentrations, losses of half of the NOM were common and desalting of NOM isolates was a problem. A new comprehensive approach was devised and tested on the Seine River, France in which 100 L of filtered water was sodium softened by ion exchange and vacuum evaporated to 100 mL. Colloids (32% of the NOM) were isolated using a 3,500 Dalton membrane by dialysis against 0.1 M HCl and 0.2 M HF to remove salts and silica. On the membrane permeate, hydrophobic NOM (42%) was isolated using XAD-8 resin and hydrophilic NOM (26%) was isolated using a variety of selective desalting precipitations. The colloid fraction was characterized by IR and NMR spectroscopy as N-acetylamino sugars. ?? 2000 American Chemical Society.

  11. ISOLATING AND FRACTIONATING ORGANIC TOXICANTS IN SEDIMENTS: EVALUATION OF AN EXPERIMENTAL APPROACH

    EPA Science Inventory

    Most solid-phase sediment TIE techniques for organic chemicals have been focused on solid phase sorptive techniques, such as amending contaminated sediments with the carbonaceousresin, Ambersorb coconut charcoal, or XAD resin to reduce toxicity caused by organic contaminants. Cha...

  12. A new process for the management of olive oil mill waste water and recovery of natural antioxidants.

    PubMed

    Agalias, Apostolis; Magiatis, Prokopios; Skaltsounis, Alexios-Leandros; Mikros, Emmanuel; Tsarbopoulos, Anthony; Gikas, Evagelos; Spanos, Ioannis; Manios, Thrasyvoulos

    2007-04-04

    The high polyphenol content of the wastewater is the major environmental problem caused by the olive mills. A pilot scale system for the treatment of the olive oil mills wastewater was developed aiming at the recovery of high added value-contained polyphenols and the reduction of the environmental problems. The treatment system consists of three main successive sections: The first one includes successive filtration stages aiming at the gradual reduction of the wastewater suspended solids up to a limit of 25 microm. The second section includes passing of the filtered wastewater through a series of adsorbent resins (XAD16 and XAD7HP) in order to achieve the de-odoring and decolorization of the wastewater and the removal/ recovery of the polyphenol and lactone content. The third section of the procedure includes the thermal evaporation and recovery of the organic solvents mixture, which has been used in the resin regeneration process, and finally the separation of the polyphenols and other organic substance contents using fast centrifuge partition chromatography. The final outcome of the whole procedure is (i) an odorless yellowish wastewater with a 99.99% reduced content in polyphenols and 98% reduced COD, (ii) an extract rich in polyphenols and lactones with high antioxidant activity and high added value, (iii) an extract containing the coloring substances of the olive fruit, and (iv) pure hydroxytyrosol.

  13. Distribution of polycyclic aromatic hydrocarbons in southern Chesapeake Bay surface water: Evaluation of three methods for determining freely dissolved water concentrations

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Gustafson, K.E.; Dickhut, R.M.

    1997-03-01

    Gas sparging, semipermeable-membrane devices (SPMDs), and filtration with sorption of dissolved polycyclic aromatic hydrocarbons (PAHs) to XAD-2 resin were evaluated for determining the concentrations of freely dissolved PAHs in estuarine waters of southern Chesapeake Bay at sites ranging from rural to urban and highly industrialized. Gas sparging had significant sampling artifacts due to particle scavenging by rising bubbles, and SPMDs were kinetically limited for four-ring and larger PAHs relative to short-term temporal changes in water concentrations. Filtration with sorption of the dissolved contaminant fraction to XAD-2 resin was found to be the most accurate and feasible method for determining concentrationsmore » of freely dissolved PAHs in estuarine water. Concentrations and distribution coefficients of dissolved and particulate PAHs were measured using the filtration/XAD-2 method. Concentrations of PAHs in surface waters of southern Chesapeake Bay were higher than those reported for the northern bay; concentrations in the Elizabeth River were elevated relative to all other sites. A gradient for particulate PAHs was observed from urban to remote sites. No seasonal trends were observed in dissolved or particle-bound PAH fractions at any site. Distributions of dissolved and particulate PAHs in surface waters of the Chesapeake Bay are near equilibrium at all locations and during all seasons.« less

  14. Improvement of the fermentability of oxalic acid hydrolysates by detoxification using electrodialysis and adsorption.

    PubMed

    Jeong, So-Yeon; Trinh, Ly Thi Phi; Lee, Hong-Joo; Lee, Jae-Won

    2014-01-01

    A two-step detoxification process consisting of electrodialysis and adsorption was performed to improve the fermentability of oxalic acid hydrolysates. The constituents of the hydrolysate differed significantly between mixed hardwood and softwood. Acetic acid and furfural concentrations were high in the mixed hardwood, whereas 5-hydroxymethylfurfural (HMF) concentration was relatively low compared with that of the mixed softwood. The removal efficiency of acetic acid reached 100% by electrodialysis (ED) process in both hydrolysates, while those of furfural and HMF showed very low, due to non-ionizable properties. Most of the remaining inhibitors were removed by XAD-4 resin. In the mixed hardwood hydrolysate without removal of the inhibitors, ethanol fermentation was not completed. Meanwhile, both ED-treated hydrolysates successfully produced ethanol with 0.08 and 0.15 g/Lh ethanol productivity, respectively. The maximum ethanol productivity was attained after fermentation with 0.27 and 0.35 g/Lh of detoxified hydrolysates, which were treated by ED, followed by XAD-4 resin. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Comparison of magnetic carboxymethyl chitosan nanoparticles and cation exchange resin for the efficient purification of lysine-tagged small ubiquitin-like modifier protease.

    PubMed

    Li, Junhua; Zhang, Yang; Shen, Fei; Yang, Yanjun

    2012-10-15

    A fusion tag that can be purified by the cheap ion-exchanger based on the ionic binding force may provide a cost-effective scheme over other affinity fusion tags. Small ubiquitin-like modifier (SUMO) protease derived from Saccharomyces cerevisiae was fused with a poly lysine tag containing 10 lysine residues at its C-terminus and then expressed in Escherichia coli. The ionic binding force provided by the ploy lysine tag allowed the selective recovery of the small ubiquitin-like modifier protease from recombinant E. coli cell extracts. A preliminary comparative study of the adsorption and elution of poly lysine tagged SUMO protease on Amberlite Cobalamion and magnetite carboxymethyl chitosan nanoparticles was performed. Amberlite Cobalamion and magnetite nanoparticles had the similar elution profile due to the common functional groups - carboxyl groups. The maximum dynamic adsorption capacity of Amberlite Cobalamion and magnetite nanoparticles reached 36.8 and 211.4 mg/g, respectively. The lysine-tagged protease can be simply purified by magnetite nanoparticles from cell extracts with higher purity than that by Amberlite Cobalamion. The superparamagnetic nanoparticles possess the advantages of highly specific, fast and excellent binding of a larger amount of lysine tagged SUMO modifier protease, and it is also easier to separate from the crude biological process liquors compared with the conventional separation techniques of polycationic amino acids fusion proteins. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. Immobilization of Pseudomonas fluorescens lipase on hydrophobic supports and application in biodiesel synthesis by transesterification of vegetable oils in solvent-free systems.

    PubMed

    Lima, Lionete N; Oliveira, Gladson C; Rojas, Mayerlenis J; Castro, Heizir F; Da Rós, Patrícia C M; Mendes, Adriano A; Giordano, Raquel L C; Tardioli, Paulo W

    2015-04-01

    This work describes the preparation of biocatalysts for ethanolysis of soybean and babassu oils in solvent-free systems. Polystyrene, Amberlite (XAD-7HP), and octyl-silica were tested as supports for the immobilization of Pseudomonas fluorescens lipase (PFL). The use of octyl-silica resulted in a biocatalyst with high values of hydrolytic activity (650.0 ± 15.5 IU/g), immobilization yield (91.3 ± 0.3 %), and recovered activity (82.1 ± 1.5 %). PFL immobilized on octyl-silica was around 12-fold more stable than soluble PFL, at 45 °C and pH 8.0, in the presence of ethanol at 36 % (v/v). The biocatalyst provided high vegetable oil transesterification yields of around 97.5 % after 24 h of reaction using babassu oil and around 80 % after 48 h of reaction using soybean oil. The PFL-octyl-silica biocatalyst retained around 90 % of its initial activity after five cycles of transesterification of soybean oil. Octyl-silica is a promising support that can be used to immobilize PFL for subsequent application in biodiesel synthesis.

  17. Determination of mycotoxins produced by Fusarium isolates from banana fruits by capillary gas chromatography and high-performance liquid chromatography.

    PubMed

    Jiménez, M; Mateo, R

    1997-08-22

    A method of analysis for trichothecenes (nivalenol, deoxynivalenol, 3- and 15-acetyldeoxynivalenol, diacetoxyscirpenol, neosolaniol, T-2 tetraol, T-2 and HT-2 toxins), zearalenone and zearalenols, and another method for determination of fumonisin B1 are described and applied to cultures of Fusarium isolated from bananas. Both methods were adapted from different techniques of extraction, clean-up and determination of these mycotoxins. The first method involves extraction with methanol-1% aqueous sodium chloride, clean-up of extracts by partition with hexane and dichloromethane, additional solid reversed-phase clean-up and analysis of two eluates by both high-performance liquid chromatography with ultraviolet detection and capillary gas chromatography. The method for fumonisin B1 implies extraction with aqueous methanol, concentration, clean-up with water and methanol on Amberlite XAD-2 column, formation of a fluorescent 4-fluoro-7-nitrobenzofurazan derivative and analysis by high-performance liquid chromatography with fluorescence detection. Both procedures give good limits of detection and recoveries, and are considered suitable for the detection and quantification of the studied toxins in corn and rice cultures of Fusarium spp. isolated from banana fruits.

  18. Characterization and purification of anthocyanins from black peanut (Arachis hypogaea L.) skin by combined column chromatography.

    PubMed

    Zhao, Zhenlei; Wu, Min; Zhan, Yali; Zhan, Kanghua; Chang, Xiulian; Yang, Hongshun; Li, Zhanming

    2017-10-13

    Black peanut skins as a byproduct from peanut industry contain abundant anthocyanins, evaluated as 8.61±0.27mg/g dry black peanut skins, are currently poorly exploited. In this work, four anthocyanins and three major flavonols were detected and identified by HPLC-PDA-ESI-MS/MS from the acidified water extract of black peanut skins of Arachis hypogaea L. After preliminary removal of flavonols by ethyl acetate (EtOAc), further purification of the anthocyanins was conducted using a combination of Amberlite XAD-7HP and ODS-AQ-HG column chromatography methods. Two most abundant monomeric anthocyanins cyanidin-3-O-sophoroside (5.77±0.42mg) and cyanidin-3-O-sambubioside (4.10±0.17mg) were eventually obtained from 2g dry black peanut skins, and their purities were determined by HPLC-PDA as 97.29% and 98.28% at the yields of 87.47% and 64.27% on the basis of their total amount in the crude extracts, respectively. These sequential treatments can be easily adapted to large-scale fractionation of pure anthocyanin monomers. Copyright © 2017. Published by Elsevier B.V.

  19. Enantioselective synthesis of (S)-naproxen using immobilized lipase on chitosan beads.

    PubMed

    Gilani, Saeedeh L; Najafpour, Ghasem D; Heydarzadeh, Hamid D; Moghadamnia, Aliakbar

    2017-06-01

    S-naproxen by enantioselective hydrolysis of racemic naproxen methyl ester was produced using immobilized lipase. The lipase enzyme was immobilized on chitosan beads, activated chitosan beads by glutaraldehyde, and Amberlite XAD7. In order to find an appropriate support for the hydrolysis reaction of racemic naproxen methyl ester, the conversion and enantioselectivity for all carriers were compared. In addition, effects of the volumetric ratio of two phases in different organic solvents, addition of cosolvent and surfactant, optimum pH and temperature, reusability, and inhibitory effect of methanol were investigated. The optimum volumetric ratio of two phases was defined as 3:2 of aqueous phase to organic phase. Various water miscible and water immiscible solvents were examined. Finally, isooctane was chosen as an organic solvent, while 2-ethoxyethanol was added as a cosolvent in the organic phase of the reaction mixture. The optimum reaction conditions were determined to be 35 °C, pH 7, and 24 h. Addition of Tween-80 in the organic phase increased the accessibility of immobilized enzyme to the reactant. The optimum organic phase compositions using a volumetric ratio of 2-ethoxyethanol, isooctane and Tween-80 were 3:7 and 0.1% (v/v/v), respectively. The best conversion and enantioselectivity of immobilized enzyme using chitosan beads activated by glutaraldehyde were 0.45 and 185, respectively. © 2017 Wiley Periodicals, Inc.

  20. PROBING REACTIVITY OF DISSOLVED ORGANIC MATTER FOR DISINFECTION BY-PRODUCT FORMATION USING XAD-8 RESIN ADSORPTION AND ULTRAFILTRATION FRACTIONATION. (R828045)

    EPA Science Inventory

    The disinfection by-product (DBP) reactivity (yield and speciation upon reaction with chlorine) of dissolved organic matter (DOM) isolated from two surface waters was investigated. The source waters, each having significantly different specific ultraviolet absorbance (SUVA

  1. Simultaneous Preconcentration and Determination of Brilliant Blue and Sunset Yellow in Foodstuffs by Solid-Phase Extraction Combined UV-Vis Spectrophotometry.

    PubMed

    Bişgin, Abdullah Taner

    2018-05-29

    Background: Brilliant Blue and Sunset Yellow, two highly water-soluble synthetic food dyes, are the most popular food dyes used and consumed. Although they are not highly toxic, some health problems can be observed when excessive amounts of food products containing these dyes are consumed. Objectives: The aim of the study was to develop a simultaneous UV-Vis combined solid-phase extraction method, based on the adsorption onto Amberlite XAD-8 resin, for determination of Brilliant Blue and Sunset Yellow dyes. Methods: Sample solution was poured into the reservoir of the column and permitted to gravitationally pass through the column at 2 mL/min flow rate. Adsorbed dyes were eluted to 5 mL of final volume with 1 mol/L HNO₃ in ethanol solution by applying a 2 mL/min flow rate. Dye concentrations of the solution were determined at 483 and 630 nm for Sunset Yellow and Brilliant Blue, respectively. Results: The detection limits of the method for Brilliant Blue and Sunset Yellow were determined as 0.13 and 0.66 ng/mL, respectively. Preconcentration factor was 80. Brilliant Blue contents of real food samples were found to be between 11 and 240 μg/g. Sunset Yellow concentrations of foodstuffs were determined to be between 19 and 331 μg/g. Conclusions: Economical, effective, and simple simultaneous determination of Brilliant Blue and Sunset Yellow was achieved by using a solid-phase extraction combined UV-Vis spectrometry method. Highlights: The method is applicable and suitable for routine analysis in quality control laboratories without the need for expert personnel and high operational costs because the instrumentation is simple and inexpensive.

  2. Adsorptive removal of fermentation inhibitors from concentrated acid hydrolyzates of lignocellulosic biomass.

    PubMed

    Sainio, Tuomo; Turku, Irina; Heinonen, Jari

    2011-05-01

    Adsorptive purification of concentrated acid hydrolyzate of lignocellulose was investigated. Cation exchange resin (CS16GC), neutral polymer adsorbent (XAD-16), and granulated activated carbon (GAC) were studied to remove furfural, HMF, and acetic acid from a synthetic hydrolyzate containing 20 wt.% H(2)SO(4). Adsorption isotherms were determined experimentally. Loading and regeneration were investigated in a laboratory scale column. GAC has the highest adsorption capacity, but regeneration with water was not feasible. XAD-16 and CS16GC had lower adsorption capacities but also shorter cycle times due to easier regeneration. Productivity increased when regenerating with 50 wt.% EtOH(aq) solution. To compare adsorbents, process performance was quantified by productivity and fraction of inhibitors removed. GAC yields highest performance when high purity is required and ethanol can be used in regeneration. For lower purities, XAD-16 and GAC yield approximately equal performance. When using ethanol must be avoided, CS16GC offers highest productivity. Copyright © 2011 Elsevier Ltd. All rights reserved.

  3. [Extraction and purification technologies of total flavonoids from Aconitum tanguticum].

    PubMed

    Li, Yan-Rong; Yan, Li-Xin; Feng, Wei-Hong; Li, Chun; Wang, Zhi-Min

    2014-04-01

    To optimize the extraction and purification technologies of total flavonoids from Aconitum tanguticum whole plant. With the content of total flavonoids as index, the optimum extraction conditions for the concentration, volume of alcohol, extracting time and times were selected by orthogonal optimized; Comparing the adsorption quantity (mg/g) and resolution (%), four kinds of macroporous adsorption resins including D101, AB-8, X-5 and XAD-16 were investigated for the enrichment ability of total flavonoids from Aconitum tanguticum; Concentration and pH value of sample, sampling amount, elution solvent and loading and elution velocity for the optimum adsorption resin were determined. The content of total flavonoids in Aconitum tanguticum was about 4.39%; The optimum extraction technique was 70% alcohol reflux extraction for three times,each time for one hour, the ratio of material and liquid was 1:10 (w/v); The optimum purification technology was: using XAD-16 macroporous resin, the initial concentration of total flavonoids of Aconitum tanguticum was 8 mg/mL, the sampling amount was 112 mg/g dry resin, the pH value was 5, the loading velocity was 3 mL/min, the elution solvent was 70% ethanol and the elution velocity was 5 mL/min. Under the optimum conditions, the average content of total flavonoids was raised from 4.39% to 46.19%. The optimum extraction and purification technologies for total flavonoids of Aconitum tanguticum were suitable for industrial production for its simplicity and responsibility.

  4. Ion exchange treatment of rinse water generated in the galvanizing process.

    PubMed

    Marañón, Elena; Fernández, Yolanda; Castrillón, Leonor

    2005-01-01

    A study was conducted of the viability of using the cationic exchange resins Amberlite IR-120 and Lewatit SP-112 to treat rinse water generated in the galvanizing process as well as acidic wastewater containing zinc (Zn) and iron (Fe). Solutions containing either 100 mg/L of Zn at pH 5.6 (rinse water) or Fe and Zn at concentrations of 320 and 200 mg/L at pH 1.5 (acidic water), respectively, were percolated through packed beds until the resins were exhausted. Breakthrough capacities obtained ranged between 1.1 and 1.5 meq metal/mL resin. The elution of metal and the regeneration of resins were performed with hydrochloric acid. The influence of the flowrate used during the loading stage was also studied, with 0.5 bed volumes/min (3.2 cm/min) found to be the optimum flowrate.

  5. Structural properties of dissolved organic carbon in deep soil horizons of an arable and temporarily grassland.

    NASA Astrophysics Data System (ADS)

    Lavaud, A.; Chabbi, A.; Croue, J. P.

    2009-04-01

    It is commonly accepted that dissolved organic carbon (DOC) is the bio-available fraction of the largest amount of soil organic matter (SOM), even if it does represent only a very small proportion. Because most of the studies on DOC dynamics were mainly restricted to forest soils, studies on the factors governing the dynamics of DOC in deep soil horizons (>1 m) in arable system are still very little limited. The objective of this work is to better define the proportion of DOC in deep soil horizons and indicate their main characteristics and structural properties. The study was conducted on the long term observatory for environmental research- biogeochemical cycles and biodiversity Lusignan site). DOC collected using lysimeters plates inserted to a depth of 105 cm was fractionated into 3 fractions using the two column array of XAD-8 and XAD-4 resins. The HPO (hydrophobic) fraction (i.e. humic substances) isolated from the XAD-8 resin, the TPH (Transphilic) fraction from the XAD-4 resin and the HPI (hydrophilic) fraction which corresponds to the DOC that does not adsorbed onto the two resins under the acid condition used (pH 2). DOM adsorbed onto the resins is recovered with a 75%/25% acetonitrile/water mixture and lyophilized. Depend on the amount of material; the chemical composition of DOC was performed using UV254 nm, fluorescence EEM, NMR and HPSEC/UV/COD. The results show that the concentration and structural properties of DOC in deep soil horizon were similar to those of groundwater (low SUVA (1.2 m-1.L.mg C-1), structures composed mainly of low molecular weight). Because of the relatively recent establishment of the treatment, the monitoring of the dynamics of the DOC concentrations did not show significant differences between arable and grassland. However, the temporal dynamic shows a slight increase in the DOC content regardless of the of land use. DOC concentrations between winter and the middle of spring tend to double going from 1 to 2.5 mg / L and then to 4-5 mg / L in summer time. The structural analysis reveals significant input of terpenoid derived organic matter was confirmed in the HPO fraction of DOC a results supported by the data of 13C NMR, Infra Red and Micro Scale Sealed Vessel / pyrolysis GC / MS. The chromatographic profiles obtained by flash pyrolysis GC / MS highlight the presence of phenol and alkyl phenols, generally attributed to structures polyhydroxyaromatiques (lignin / tannins), but acetamide, pyrolysis product of amino sugars constituents of the wall microbial cells. The thermochimiolyse (TMAH) / GC / MS confirmed the presence of hydroxy aromatic structures in the extracts, however, their precise origin (lignin, tannins ...) remains uncertain. The results so far indicate that the DOC in deep soil horizons is marked by low aromaticity and dominated by small size molecules. This would consist of carbon derived from terpenoids, lignin degraded and amino sugars.

  6. RECOVERY OF MUTAGENICITY FROM DISINFECTED WATER SAMPLES BY XAD RESIN ADSORPTION COMPARED TO REVERSE OSMOSIS

    EPA Science Inventory

    the presence of a complex misture of disinfection byproducts in drinking waters continues to cause concern over the potential long-term health effects of exposure to these compounds. Most of these compounds are present at ug/L levels or less. Consequently, some method of concentr...

  7. Photovoltaic performance of TiO2 electrode adsorbed with gardenia yellow purified by nonionic polymeric sorbent in dye-sensitized solar cells.

    PubMed

    Kwon, Oh Oun; Kim, Eui Jin; Lee, Jae Hyeok; Kim, Tae Young; Park, Kyung Hee; Kim, Sang Yook; Suh, Hwa Jin; Lee, Hyo Jung; Lee, Jae Wook

    2015-02-05

    To improve the photovoltaic conversion efficiency in dye-sensitized solar cells (DSSCs), TiO2 electrode adsorbed with gardenia yellow purified by nonionic polymeric sorbent was successfully formulated on nanoporous TiO2 surface. Adsorption and desorption properties of crude gardenia yellow solution on a macroporous resin, XAD-1600, were investigated to purify gardenia yellow because of its strong adsorption and desorption abilities as well as high selectivity. To this end, adsorption equilibrium and kinetic data were measured and fitted using adsorption isotherms and kinetic models. Adsorption and desorption breakthrough curves in a column packed with XAD-1600 resin was obtained to optimize the separation process of gardenia yellow. The photovoltaic performance of the photo-electrode adsorbed with the crude and purified gardenia yellow in DSSCs was compared from current-voltage measurements. The results showed that the photovoltaic conversion efficiency was highly dependent on how to separate and purify gardenia yellow as a photosensitizer. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Chemical and spectroscopic characterization of dissolved humic substances in a mangrove-fringed estuary in the eastern coast of Hainan Island, China

    NASA Astrophysics Data System (ADS)

    Zhang, Yaoling; Du, Jinzhou; Peng, Bo; Zhang, Fenfen; Zhao, Xin; Zhang, Jing

    2013-03-01

    Mangrove-derived dissolved organic matter (DOM) has an important effect on estuarine and coastal area on a large scale. In order to improve the understanding of origin, composition, and fate of DOM in mangrove-fringed estuarine and coastal areas, dissolved humic substances (DHS) were isolated from one mangrove pore-water sample and one near-shore seawater sample downstream the mangrove pore-water site in the eastern coast of Hainan Island, South China. Fulvic acids, humic acids and XAD-4 fractions were obtained from the two water samples by using a two-column array of XAD-8 and XAD-4 resins. Chemical and spectroscopic methods were used to analyze the features of these DHS. Compared to the mangrove pore-water DHS, the near-shore seawater DHS were found rich in 13C with lower C/N ratios and more aliphatic compounds and carbohydrates, but less aromatic structures and carboxyl groups. As for the three fractions of the two DHS, XAD-4 fractions contain more aliphatics, carbohydrates, carboxyl groups, and enrich in 13C with respect to both fulvic and humic acids. Photo-oxidation transformation and contribution from marine-derived DOM were considered as the main reasons resulted in the difference in compositional features for these DHS in this study.

  9. A simple and sensitive determination of histamine and N tau-methylhistamine in biological fluids by high-performance liquid chromatography with electrochemical detection.

    PubMed

    Houdi, A A; Crooks, P A; Van Loon, G R; Schubert, C A

    1987-05-01

    The determination of picomolar levels of histamine and its major metabolite, N tau-methylhistamine, in biological fluids was achieved using reversed-phase liquid chromatography coupled with electrochemical detection. A simple sample purification procedure for blood and urine samples was carried out prior to analysis using an Amberlite CG-50 cation-exchange resin, which afforded an excellent recovery of both compounds.

  10. Optimization of extraction parameters by using response surface methodology, purification, and identification of anthocyanin pigments in Melastoma malabathricum fruit.

    PubMed

    Anuar, Nordiyanah; Mohd Adnan, Ahmad Faris; Saat, Naziz; Aziz, Norkasmani; Mat Taha, Rosna

    2013-01-01

    Anthocyanins not just have various benefits in food industry but also have been used as natural colourants in cosmetic, coating products and as potential natural photosensitizers in solar cell. Thus, the main purpose of this study was to obtain information on the maximum yield of anthocyanin that can be recovered from Melastoma malabathricum fruit. Factors such as extraction temperature, extraction time, and solid to liquid ratio were identified to be significantly affecting anthocyanin extraction efficiency. By using three-level three-factor Box-Behnken design, the optimized conditions for anthocyanin extraction by acidified methanol (R (2) = 0.972) were temperature of 60°C, time of 86.82 min, and 0.5 : 35 (g/mL) solid to liquid ratio while the optimum extraction conditions by acidified ethanol (R (2) = 0.954) were temperature of 60°C, time of 120 min, and 0.5 : 23.06 (g/mL) solid to liquid ratio. The crude anthocyanin extract was further purified by using Amberlite XAD-7 and Sephadex LH-20 column chromatography. Identification of anthocyanins revealed the presence of cyanidin dihexoside, cyanidin hexoside, and delphinidin hexoside as the main anthocyanins in M. malabathricum fruit.

  11. Feruloylated and nonferuloylated arabino-oligosaccharides from sugar beet pectin selectively stimulate the growth of Bifidobacterium spp. in human fecal in vitro fermentations.

    PubMed

    Holck, Jesper; Lorentzen, Andrea; Vigsnæs, Louise K; Licht, Tine R; Mikkelsen, Jørn D; Meyer, Anne S

    2011-06-22

    The side chains of the rhamnogalacturonan I fraction in sugar beet pectin are particularly rich in arabinan moieties, which may be substituted with feruloyl groups. In this work the arabinan-rich fraction resulting from sugar beet pulp based pectin production was separated by Amberlite XAD hydrophobic interaction and membrane separation into four fractions based on feruloyl substitution and arabino-oligosaccharide chain length: short-chain (DP 2-10) and long-chain (DP 7-14) feruloylated and nonferuloylated arabino-oligosaccharides, respectively. HPAEC, SEC, and MALDI-TOF/TOF analyses of the fractions confirmed the presence of singly and doubly substituted feruloylated arabino-oligosaccharides in the feruloyl-substituted fractions. In vitro microbial fermentation by human fecal samples (n = 6 healthy human volunteers) showed a selective stimulation of bifidobacteria by both the feruloylated and the nonferuloylated long-chain arabino-oligosaccharides to the same extent as the prebiotic fructo-oligosaccharides control. None of the fractions stimulated the growth of the potential pathogen Clostridium difficile in monocultures. This work provides a first report on the separation of potentially bioactive feruloylated arabino-oligosaccharides from sugar beet pulp and an initial indication of the potentially larger bifidogenic effect of relatively long-chain arabino-oligosaccharides as opposed to short-chain arabino-oligosaccharides.

  12. Bacteriocinogenic Potential of Enterococcus faecium Isolated from Wine.

    PubMed

    Dündar, Halil

    2016-09-01

    A total of 145 lactic acid bacteria isolated from a variety of Turkish red wines during malolactic fermentation were screened to find bacteriocin-producing strains. Among them, 14 isolates of Enterococcus faecium were identified to produce bacteriocins. PCR screening revealed that some isolates harbored entA and entB genes while some harbored entA, entB and entP genes. An isolate designated as Ent. faecium H46 was selected to characterize its bacteriocins. The bacteriocins were purified to homogeneity from culture supernatant by Amberlite XAD-16, cation-exchange and reverse-phase chromatography. MALDI-TOF mass spectrometry analysis identified the bacteriocins as enterocin A and enterocin B. The presence of Ent. faecium is noteworthy since it is not associated with wine fermentation. However, it has been reported as an important wine spoilage organism due to its potential to produce tyramine. Although species of Enterococcus is not known as wine bacteria, contamination by Ent. faecium may arise from grapes or wineries equipments used for wine production.

  13. Identification of didecyldimethylammonium salts and salicylic acid as antimicrobial compounds in commercial fermented radish kimchi.

    PubMed

    Li, Jing; Chaytor, Jennifer L; Findlay, Brandon; McMullen, Lynn M; Smith, David C; Vederas, John C

    2015-03-25

    Daikon radish (Raphanus sativus) fermented with lactic acid bacteria, especially Leuconostoc or Lactobacillus spp., can be used to make kimchi, a traditional Korean fermented vegetable. Commercial Leuconostoc/radish root ferment filtrates are claimed to have broad spectrum antimicrobial activity. Leuconostoc kimchii fermentation products are patented as preservatives for cosmetics, and certain strains of this organism are reported to produce antimicrobial peptides (bacteriocins). We examined the antimicrobial agents in commercial Leuconostoc/radish root ferment filtrates. Both activity-guided fractionation with Amberlite XAD-16 and direct extraction with ethyl acetate gave salicylic acid as the primary agent with activity against Gram-negative bacteria. Further analysis of the ethyl acetate extract revealed that a didecyldimethylammonium salt was responsible for the Gram-positive activity. The structures of these compounds were confirmed by a combination of (1)H- and (13)C NMR, high-performance liquid chromatography, high-resolution mass spectrometry, and tandem mass spectrometry analyses. Radiocarbon dating indicates that neither compound is a fermentation product. No antimicrobial peptides were detected.

  14. Mathematical modeling of the adsorption/desorption characteristics of anthocyanins from muscadine (Vitis rotundifolia cv. Noble) juice pomace on Amberlite FPX66 resin in a fixed bed column.

    PubMed

    Uzdevenes, Chad G; Gao, Chi; Sandhu, Amandeep K; Yagiz, Yavuz; Gu, Liwei

    2018-03-24

    Muscadine grape pomace, a by-product of juicing and wine-making, contains significant amounts of anthocyanin 3,5-diglucosides, known to be beneficial to human health. The objective of this research was to use mathematical modeling to investigate the adsorption/desorption characteristics of these anthocyanins from muscadine grape pomace on Amberlite FPX66 resin in a fixed bed column. Anthocyanins were extracted using hot water and ultrasound, and the extracts were loaded onto a resin column at five bed depths (5, 6, 8, 10 and 12 cm) using three flow rates (4, 6 and 8 mL min -1 ). It was found that adsorption on the column fitted the bed depth service time (BDST) model and the empty bed residence time (EBRT) model. Desorption was achieved by eluting the column using ethanol at four concentrations (25, 40, 55 and 70% v/v) and could be described with an empirical sigmoid model. The breakthrough curves of anthocyanins fitted the BDST model for all three flow rates with R 2 values of 0.983, 0.992 and 0.984 respectively. The EBRT model was successfully employed to find the operating lines, which allow for column scale-up while still achieving similar results to those found in a laboratory operation. Desorption with 40% (v/v) ethanol achieved the highest recovery rate of anthocyanins at 79.6%. The mathematical models established in this study can be used in designing a pilot/industrial- scale column for the separation and concentration of anthocyanins from muscadine juice pomace. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

  15. Factors influencing antibiotics adsorption onto engineered adsorbents.

    PubMed

    Xia, Mingfang; Li, Aimin; Zhu, Zhaolian; Zhou, Qin; Yang, Weiben

    2013-07-01

    The study evaluated the adsorption of two antibiotics by four engineered adsorbents (hypercrosslinked resin MN-202, macroporous resin XAD-4, activated carbon F-400, and multi-walled carbon nanotubes (MWCNT)) from aqueous solutions. The dynamic results demonstrated the dominant influence of pore size in adsorption. The adsorption amounts of antibiotics on XAD-4 were attributed to the hydrophobic effect, whereas steric hindrance or micropore-filling played a main role in the adsorption of antibiotics by F-400 because of its high microporosity. Aside from F-400, similar patterns of pH-dependent adsorption were observed, implying the importance of antibiotic molecular forms to the adsorption process for adsorbents. Increasing the ionic concentration with CaC12 produced particular adsorption characteristics on MWCNT at pH 2.0 and F-400 at pH 8.0, which were attributed to the highly available contact surfaces and molecular sieving, respectively. Its hybrid characteristics incorporating a considerable portion of mesopores and micropores made hypercross linked MN-202 a superior antibiotic adsorbent with high adsorption capacity. Furthermore, the adsorption capacity of MWCNT on the basis of surface area was more advantageous than that of the other adsorbents because MWCNT has a much more compact molecular arrangement.

  16. Comparison of polyurethane foam and XAD-2 sampling matrices to measure airborne organophosphorus pesticides and their oxygen analogs in an agricultural community

    PubMed Central

    Armstrong, Jenna L.; Fenske, Richard A.; Yost, Michael G.; Tchong-French, Maria; Yu, Jianbo

    2013-01-01

    Side-by-side active air sampling for the organophosphorus (OP) pesticide, chlorpyrifos (CPF) and its oxygen analog, chlorpyrifos-oxon (CPF-O) was conducted with two recommended air sampling matrices: OSHA Versatile Sampling (OVS) tubes with XAD-2 resin, polyurethane foam (PUF) tubes, and passive PUF deposition disks. The study compared the proportion of artificially transformed CPF-O in the laboratory and in the field during a tree fruit application in Washington State. Lab results demonstrated that the NIOSH-recommended OVS tubes artificially transformed up to 32% of CPF to CPF-O during the sampling process, whereas PUF tubes had little to no artificial transformation (≤ 0.1%). In the field, the proportion of CPF-O in the sample was significantly higher on OVS tubes than on PUF tubes (p < 0.001), confirming that OVS tubes were converting a significant portion of CPF to CPF-O. In addition, PUF tubes reported measurable levels CPF-O in the field even when no artificial transformation was expected. We conclude that the PUF matrix is the superior sampling medium for OP oxygen analogs when compared to XAD-2 resin. Community-located PUF tube samples 24 hours post-application had considerably higher levels CPF-O (16–21 ng/m3) than near field samples during application (2–14 ng/m3), suggesting that the oxygen analog is volatile and formed during atmospheric transport. It is recommended that worker and community risk assessments begin to take into consideration the presence of the more toxic oxygen analogs when measuring for OP pesticide mixtures. PMID:23466277

  17. Synthesis and characterization of an N-(2-hydroxyethyl)-ethylenediaminetriacetic acid resin

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Lai, Yuet Fan

    1977-10-01

    A chelating ion-exchange resin with N-(2-hydroxyethyl)ethylene-diaminetriacetic acid (HEDTA) used as the ligand chemically bonded to XAD-4 by an ester linkage, HEDTA-4, was synthesized. It is stable under normal experimental conditions with the liquid chromatograph. The structure of the resin was confirmed by an infrared spectrum, and by potentiometric titrations. The capacity of the resin was also obtained by potentiometric titration and by a nitrogen analysis. The resin was used to pack a column of 5 mm internal diameter and 5 cm long. The effect of pH on the retention of different metal ions on the resin was studied. It wasmore » found that the resin was most selective for chromium(III), copper(II), lead(II), mercury(II), uranium(VI), zirconium(IV) and zinc(II) at a pH of less than 3. Furthermore, the resin proves to be functioning with a chelating mechanism rather than ion-exchange, and it can concentrate trace metal ions in the presence of a large excess of calcium and magnesium. This makes the resin potentially useful for purifying and analyzing drinking water.« less

  18. Organic Compounds, Trace Elements, Suspended Sediment, and Field Characteristics at the Heads-of-Tide of the Raritan, Passaic, Hackensack, Rahway, and Elizabeth Rivers, New Jersey, 2000-03

    USGS Publications Warehouse

    Bonin, Jennifer L.; Wilson, Timothy P.

    2006-01-01

    Concentrations of suspended sediment, particulate and dissolved organic carbon, trace elements, and organic compounds were measured in samples from the heads-of-tide of the five tributaries to the Newark and Raritan Bays during June 2000 to June 2003. The samples were collected as part of the New Jersey Department of Environmental Protection Toxics Reduction Workplan/Contaminant Assessment Reduction Program. Samples of streamwater were collected at water-quality sampling stations constructed near U.S. Geological Survey gaging stations on the Raritan, Passaic, Hackensack, Rahway, and Elizabeth Rivers. Sampling was conducted during base-flow conditions and storms. Constituent concentrations were measured to determine the water quality and to calculate the load of sediment and contaminants contributed to the bays from upstream sources. Water samples were analyzed for suspended sediment, dissolved organic carbon, particulate organic carbon, and specific conductance. Samples of suspended sediment and water were analyzed for 98 distinct polychlorinated biphenyl congeners, 7 dioxins, 10 furans, 27 pesticides, 26 polycyclic aromatic hydrocarbons, and the trace elements cadmium, lead, mercury, and methyl-mercury. Measurements of ultra-low concentrations of organic compounds in sediment and water were obtained by collecting 1 to 3 grams of suspended sediment on glass fiber filters and by passing at least 20 liters of filtered water through XAD-2 resin. The extracted sediment and XAD-2 resin were analyzed for organic compounds by high- and low-resolution gas chromatography mass-spectrometry that uses isotope dilution procedures. Trace elements in filtered and unfiltered samples were analyzed for cadmium, lead, mercury, and methyl-mercury by inductively coupled charged plasma and mass-spectrometry. All constituent concentrations are raw data. Interpretation of the data will be completed in the second phase of the study.

  19. A Two-Step Bioconversion Process for Canolol Production from Rapeseed Meal Combining an Aspergillus niger Feruloyl Esterase and the Fungus Neolentinus lepideus

    PubMed Central

    Odinot, Elise; Fine, Frédéric; Sigoillot, Jean-Claude; Navarro, David; Laguna, Oscar; Bisotto, Alexandra; Peyronnet, Corinne; Lecomte, Jérôme; Faulds, Craig B.

    2017-01-01

    Rapeseed meal is a cheap and abundant raw material, particularly rich in phenolic compounds of biotechnological interest. In this study, we developed a two-step bioconversion process of naturally occurring sinapic acid (4-hydroxy-3,5-dimethoxycinnamic acid) from rapeseed meal into canolol by combining the complementary potentialities of two filamentous fungi, the micromycete Aspergillus niger and the basidiomycete Neolentinus lepideus. Canolol could display numerous industrial applications because of its high antioxidant, antimutagenic and anticarcinogenic properties. In the first step of the process, the use of the enzyme feruloyl esterase type-A (named AnFaeA) produced with the recombinant strain A. niger BRFM451 made it possible to release free sinapic acid from the raw meal by hydrolysing the conjugated forms of sinapic acid in the meal (mainly sinapine and glucopyranosyl sinapate). An amount of 39 nkat AnFaeA per gram of raw meal, at 55 °C and pH 5, led to the recovery of 6.6 to 7.4 mg of free sinapic acid per gram raw meal, which corresponded to a global hydrolysis yield of 68 to 76% and a 100% hydrolysis of sinapine. Then, the XAD2 adsorbent (a styrene and divinylbenzene copolymer resin), used at pH 4, enabled the efficient recovery of the released sinapic acid, and its concentration after elution with ethanol. In the second step, 3-day-old submerged cultures of the strain N. lepideus BRFM15 were supplied with the recovered sinapic acid as the substrate of bioconversion into canolol by a non-oxidative decarboxylation pathway. Canolol production reached 1.3 g/L with a molar yield of bioconversion of 80% and a productivity of 100 mg/L day. The same XAD2 resin, when used at pH 7, allowed the recovery and purification of canolol from the culture broth of N. lepideus. The two-step process used mild conditions compatible with green chemistry. PMID:29036919

  20. Hydrometallurgical Separation of Niobium and Tantalum: A Fundamental Approach

    NASA Astrophysics Data System (ADS)

    Nete, Motlalepula; Purcell, Walter; Nel, Johann T.

    2016-02-01

    A mixture of pure Ta2O5 and Nb2O5 was dissolved using two different fluxes, namely NH4F·HF and Na2HPO4/NaH2PO4·H2O. Selective precipitation and ion exchange were used as separation techniques. Selective precipitation using p-phenylediamine in a fluoride matrix resulted in the isolation of 73(3)% tantalum accompanied by 23(5)% niobium. A separation factor of 11(4) was obtained. A single solvent extraction step using methyl-isobutyl ketone at a 4 M H2SO4 yielded excellent Ta and Nb separation in the fluoride solution with 80% of the Ta and only 2% Nb recovered in the organic layer. A two-step extraction recovered 100% Ta at 0.5-4 M H2SO4 with a separation factor of ~2000. A study of the extraction mechanism indicated that the stability of the protonated compounds such as H2TaF7/H2NbOF5 is in the extraction and separation determining steps in this process. A K' (double de-protonated constant) of approximately 0.2 was calculated for H2TaF7. Only 91.7% Nb and 73.4% Ta were recovered from anion separation using strong Amberlite resin and 96.1% Nb and 52.3% using the weak Dowex Marathon resin from fluoride dissolution.

  1. Preparative Purification of Polyphenols from Aronia melanocarpa (Chokeberry) with Cellular Antioxidant and Antiproliferative Activity.

    PubMed

    Gao, Ningxuan; Wang, Yuehua; Jiao, Xinyao; Chou, Shurui; Li, Enhui; Li, Bin

    2018-01-10

    The aim of this study was the purification process of polyphenols from Aronia melanocarpa (chokeberry), and the purification parameters were optimised by adsorption and desorption tests. By comparing adsorption and desorption ability of polyphenols from chokeberry on six kinds of macroporous resin, XAD-7 resin was selected. Experiments prove that the best purification parameters of static adsorption and desorption were sample pH = 4.0 with 4 h of adsorption; and desorption solvent is 95% ethanol (pH = 7.0) with 2 h of desorption. The best dynamic parameters were 9.3 bed volume (BV) of sample loading amount at a feeding flow rate of 2 BV/h, and washing the column with 5.8 BV of water, followed by subsequent elution with an eluent volume of 5.0 mL at an elution flow rate of 2 BV/h. Next the antioxidant and antiproliferative activity of polyphenols from chokeberry, blueberries, haskap berries was studied on HepG2 human liver cancer cells. The results show that polyphenol from chokeberry has a strong antioxidant effect. Taking into account the content of polyphenols in fruit, polyphenols from chokeberry represent a very valuable natural antioxidant source with antiproliferative products.

  2. Selective degradation of organic dyes by a resin modified Fe-based metal-organic framework under visible light irradiation

    NASA Astrophysics Data System (ADS)

    Araya, Tirusew; Chen, Chun-cheng; Jia, Man-ke; Johnson, David; Li, Ruiping; Huang, Ying-ping

    2017-02-01

    Metal organic frameworks (MOFs), a new class of porous crystalline materials have attracted attention because of potential applications in environmental remediation. In this work, an Fe-based MOF, FeBTC (BTC = 1,3,5-tricarboxylic acid), was successfully modified with Amberlite IRA-200 resin to yield a novel heterogeneous photocatalyst, A@FeBTC. The modification resulted in higher photocatalytic activity than FeBTC under the same conditions. After 60 min of visible light illumination (λ ≥ 420 nm) 99% of rhodamine B was degraded. The modification lowers the zeta potential, enhancing charge-based selective adsorption and subsequent photocatalytic degradation of cationic dye pollutants. The composite also improved catalyst stability and recyclability by significantly reducing loss of iron leaching. Photoluminescence studies show that introduction of the resin reduces the recombination rate of photogenerated charge carriers thereby improving the photocatalytic activity of the composite. Finally, a plausible photocatalytic reaction mechanism is proposed.

  3. Isolation and characterization of Chinese standard fulvic acid sub-fractions separated from forest soil by stepwise elution with pyrophosphate buffer.

    PubMed

    Bai, Yingchen; Wu, Fengchang; Xing, Baoshan; Meng, Wei; Shi, Guolan; Ma, Yan; Giesy, John P

    2015-03-04

    XAD-8 adsorption technique coupled with stepwise elution using pyrophosphate buffers with initial pH values of 3, 5, 7, 9, and 13 was developed to isolate Chinese standard fulvic acid (FA) and then separated the FA into five sub-fractions: FApH3, FApH5, FApH7, FApH9 and FApH13, respectively. Mass percentages of FApH3-FApH13 decreased from 42% to 2.5%, and the recovery ratios ranged from 99.0% to 99.5%. Earlier eluting sub-fractions contained greater proportions of carboxylic groups with greater polarity and molecular mass, and later eluting sub-fractions had greater phenolic and aliphatic content. Protein-like components, as well as amorphous and crystalline poly(methylene)-containing components were enriched using neutral and basic buffers. Three main mechanisms likely affect stepwise elution of humic components from XAD-8 resin with pyrophosphate buffers including: 1) the carboxylic-rich sub-fractions are deprotonated at lower pH values and eluted earlier, while phenolic-rich sub-fractions are deprotonated at greater pH values and eluted later. 2) protein or protein-like components can be desorbed and eluted by use of stepwise elution as progressively greater pH values exceed their isoelectric points. 3) size exclusion affects elution of FA sub-fractions. Successful isolation of FA sub-fractions will benefit exploration of the origin, structure, evolution and the investigation of interactions with environmental contaminants.

  4. Isolation and Characterization of Chinese Standard Fulvic Acid Sub-fractions Separated from Forest Soil by Stepwise Elution with Pyrophosphate Buffer

    PubMed Central

    Bai, Yingchen; Wu, Fengchang; Xing, Baoshan; Meng, Wei; Shi, Guolan; Ma, Yan; Giesy, John P.

    2015-01-01

    XAD-8 adsorption technique coupled with stepwise elution using pyrophosphate buffers with initial pH values of 3, 5, 7, 9, and 13 was developed to isolate Chinese standard fulvic acid (FA) and then separated the FA into five sub-fractions: FApH3, FApH5, FApH7, FApH9 and FApH13, respectively. Mass percentages of FApH3-FApH13 decreased from 42% to 2.5%, and the recovery ratios ranged from 99.0% to 99.5%. Earlier eluting sub-fractions contained greater proportions of carboxylic groups with greater polarity and molecular mass, and later eluting sub-fractions had greater phenolic and aliphatic content. Protein-like components, as well as amorphous and crystalline poly(methylene)-containing components were enriched using neutral and basic buffers. Three main mechanisms likely affect stepwise elution of humic components from XAD-8 resin with pyrophosphate buffers including: 1) the carboxylic-rich sub-fractions are deprotonated at lower pH values and eluted earlier, while phenolic-rich sub-fractions are deprotonated at greater pH values and eluted later. 2) protein or protein-like components can be desorbed and eluted by use of stepwise elution as progressively greater pH values exceed their isoelectric points. 3) size exclusion affects elution of FA sub-fractions. Successful isolation of FA sub-fractions will benefit exploration of the origin, structure, evolution and the investigation of interactions with environmental contaminants. PMID:25735451

  5. Characterization of product capture resin during microbial cultivations.

    PubMed

    Frykman, Scott; Tsuruta, Hiroko; Galazzo, Jorge; Licari, Peter

    2006-06-01

    Various bioactive small molecules produced by microbial cultivation are degraded in the culture broth or may repress the formation of additional product. The inclusion of hydrophobic adsorber resin beads to capture these products in situ and remove them from the culture broth can reduce or prevent this degradation and repression. These product capture beads are often subjected to a dynamic and stressful microenvironment for a long cultivation time, affecting their physical structure and performance. Impact and collision forces can result in the fracturing of these beads into smaller pieces, which are difficult to recover at the end of a cultivation run. Various contaminating compounds may also bind in a non-specific manner to these beads, reducing the binding capacity of the resin for the product of interest (fouling). This study characterizes resin bead binding capacity (to monitor bead fouling), and resin bead volume distributions (to monitor bead fracture) for an XAD-16 adsorber resin used to capture epothilone produced during myxobacterial cultivations. Resin fouling was found to reduce the product binding capacity of the adsorber resin by 25-50%. Additionally, the degree of resin bead fracture was found to be dependent on the cultivation length and the impeller rotation rate. Microbial cultivations and harvesting processes should be designed in such a way to minimize bead fragmentation and fouling during cultivation to maximize the amount of resin and associated product harvested at the end of a run.

  6. Calibration of polydimethylsiloxane and XAD-Pocket passive air samplers (PAS) for measuring gas- and particle-phase SVOCs

    NASA Astrophysics Data System (ADS)

    Okeme, Joseph O.; Saini, Amandeep; Yang, Congqiao; Zhu, Jiping; Smedes, Foppe; Klánová, Jana; Diamond, Miriam L.

    2016-10-01

    Polydimethylsiloxane (PDMS) has seen wide use as the stationary phase of gas chromatographic columns, a passive sampler in water, and recently as a personal exposure sampler, while styrene divinyl-benzene copolymer (XAD) has been used extensively as a passive air sampler outdoors and indoors. We have introduced PDMS and XAD-Pocket as new indoor passive air samplers (PASs). The XAD-Pocket was designed to maximize the surface area-to-volume ratio of XAD and to minimize obstruction of air flow by the sampler housing. Methods were developed to expedite the use of these PASs for measuring phthalates, novel brominated flame-retardants (NFRs) and polybrominated diphenyl ethers (PBDEs) indoors. Sampling rates, Rs, (m3 day-1), were measured during a 7-week calibration study. Variability within and between analyte groups was not statistically significant. As a result, generic values of 0.8 ± 0.4 and 0.5 ± 0.3 m3 day-1 dm-2 are recommended for PDMS and XAD-Pocket for a 50-day deployment time, respectively. PDMS has a higher uptake rate and is easier to use than XAD-Pocket.

  7. Size and resin fractionations of dissolved organic matter and trihalomethane precursors from four typical source waters in China.

    PubMed

    Wei, Qunshan; Wang, Dongsheng; Wei, Qia; Qiao, Chunguang; Shi, Baoyou; Tang, Hongxiao

    2008-06-01

    Dissolved organic matter (DOM) and its potential to form disinfection by-products (DBPs) during drinking water treatment raise challenges to water quality control. Understanding both chemical and physical characteristics of DOM in source waters is key to better water treatment. In this study, the DOM from four typical source waters in China was fractionated by XAD resin adsorption (RA) and ultrafiltration (UF) techniques. The trihalomethane formation potential (THMFP) of all fractions in the DOM were investigated to reveal the major THM precursors. The fraction distributions of DOM could be related to their geographical origins in a certain extent. The dominant chemical fraction as THM precursors in the DOM from south waters (East-Lake reservoir in Shenzhen and Peal rivers in Guangzhou) was hydrophobic acid (HoA). The size fraction with molecular weight (MW) <1 kDa in both south waters had the highest THMFP. The results of cluster analysis showed that the parameters of fractions including DOC percentage (DOC%), UV254%, SUVA254 (specific UV254 absorbance) and THMFP were better for representing the differences of DOM from the studied waters than specific THMFP (STHMFP). The weak correlation between SUVA254 and STHMFP for either size or XAD fractions suggests that whether SUVA254 can be used as an indicator for the reactivity of THM formation is highly dependent on the nature of organic matter.

  8. High-throughput and selective solid-phase extraction of urinary catecholamines by crown ether-modified resin composite fiber.

    PubMed

    Chen, LiQin; Wang, Hui; Xu, Zhen; Zhang, QiuYue; Liu, Jia; Shen, Jun; Zhang, WanQi

    2018-08-03

    In the present study, we developed a simple and high-throughput solid phase extraction (SPE) procedure for selective extraction of catecholamines (CAs) in urine samples. The SPE adsorbents were electrospun composite fibers functionalized with 4-carboxybenzo-18-crown-6 ether modified XAD resin and polystyrene, which were packed into 96-well columns and used for high-throughput selective extraction of CAs in healthy human urine samples. Moreover, the extraction efficiency of packed-fiber SPE (PFSPE) was examined by high performance liquid chromatography coupled with fluorescence detector. The parameters affecting the extraction efficiency and impurity removal efficiency were optimized, and good linearity ranging from 0.5 to 400 ng/mL was obtained with a low limit of detection (LOD, 0.2-0.5 ng/mL) and a good repeatability (2.7%-3.7%, n = 6). The extraction recoveries of three CAs ranged from 70.5% to 119.5%. Furthermore, stable and reliable results obtained by the fluorescence detector were superior to those obtained by the electrochemical detector. Collectively, PFSPE coupled with 96-well columns was a simple, rapid, selective, high-throughput and cost-efficient method, and the proposed method could be applied in clinical chemistry. Copyright © 2018 Elsevier B.V. All rights reserved.

  9. Optimization of the diffusive gradients in thin films (DGT) method for simultaneous assay of potassium and plant-available phosphorus in soils.

    PubMed

    Zhang, Yulin; Mason, Sean; McNeill, Ann; McLaughlin, Michael J

    2013-09-15

    Potassium (K) and phosphorus (P) are two important macronutrients for crops, and are usually applied to soils as granular fertilizer before seeding. Therefore, accurate soil tests prior to planting to predict crop response to fertilizers are important in optimizing crop yields. Traditional methods used for testing both available K and P in soils, which are based on chemical extraction procedures, are to be soil-type dependent, and the predictive relationships across a broad range of soils are generally poor. The diffusive gradients in thin films (DGT) technique, based on diffusion theory, is extensively used to measure the diffusive supply of trace elements, metals and some nutrients in soils and water. When DGT is used to assess plant-available P in soils, a good relationship is found between crop response to P fertilizer and concentrations of P in soil measured by DGT, and therefore the DGT method provides a more precise recommendation of P fertilizer requirements. Adaptation of the DGT method to measure plant-available K in soils has already been attempted [1], but limitations were reported due to the non-uniform size of the resin gel, decreased K binding rate of the gel at long deployment times and a limited ability to measure a wide range of K concentrations. To eliminate these problems, a new resin gel has been developed by combining Amberlite and ferrihydrite. This mixed Amberlite and ferrihydrite (MAF) gel has improved properties in terms of handling and even distribution of Amberlite in the gel. The elution efficiencies of the MAF gel for K and P were 90% and 96%, respectively. The diffusion coefficient of K through the diffusive gel was 1.30 × 10(-5)cm(2)s(-1) at 22 ± 1°C and was stable through time. Since ferrihydrite is already used in DGT P testing, the ability of the MAF gel to assess available P simultaneously was also assessed. The MAF gel performed the same as the traditional ferrihydrite gel for available P assessment in a wide variety of agricultural soils. This means that the newly developed gel has the potential to measure K and plant-available P in soils simultaneously. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Cu(II) binding by a pH-fractionated fulvic acid

    USGS Publications Warehouse

    Brown, G.K.; Cabaniss, S.E.; MacCarthy, P.; Leenheer, J.A.

    1999-01-01

    The relationship between acidity, Cu(II) binding and sorption to XAD resin was examined using Suwannee River fulvic acid (SRFA). The work was based on the hypothesis that fractions of SRFA eluted from an XAD column at various pH's from 1.0 to 12.0 would show systematic variations in acidity and possibly aromaticity which in turn would lead to different Cu(II) binding properties. We measured equilibrium Cu(II) binding to these fractions using Cu2+ ion-selective electrode (ISE) potentiometry at pH 6.0. Several model ligands were also examined, including cyclopentane-1,2,3,4-tetracarboxylic acid (CP-TCA) and tetrahydrofuran-2,3,4,5-tetracarboxylic acid (THF-TCA), the latter binding Cu(II) much more strongly as a consequence of the ether linkage. The SRFA Cu(II) binding properties agreed with previous work at high ionic strength, and binding was enhanced substantially at lower ionic strength, in agreement with Poisson-Boltzmann predictions for small spheres. Determining Cu binding constants (K(i)) by non-linear regression with total ligand concentrations (L(Ti)) taken from previous work, the fractions eluted at varying pH had K(i) similar to the unfractionated SRFA, with a maximum enhancement of 0.50 log units. We conclude that variable-pH elution from XAD does not isolate significantly strong (or weak) Cu(II)-binding components from the SRFA mixture. Copyright (C) 1999 Elsevier Science B.V.

  11. Antioxidant, antimalarial and antimicrobial activities of tannin-rich fractions, ellagitannins and phenolic acids from Punica granatum L.

    PubMed

    Reddy, Muntha K; Gupta, Sashi K; Jacob, Melissa R; Khan, Shabana I; Ferreira, Daneel

    2007-05-01

    The Punica granatum L. (pomegranate) by-product POMx was partitioned between water, EtOAc and n-BuOH, and the EtOAc and n-BuOH extracts were purified by XAD-16 and Sephadex LH-20 column chromatography to afford ellagic acid (1), gallagic acid (2), punicalins (3), and punicalagins (4). Compounds 1 - 4 and the mixture of tannin fractions (XAD-16 eluates) were evaluated for antioxidant, antiplasmodial, and antimicrobial activities in cell-based assays. The mixture of tannins (TPT), XAD-EtOAc, XAD-H2O, XAD-PJ and XAD-BuOH, exhibited IC50 values against reactive oxygen species (ROS) generation at 0.8 - 19 microg/mL. Compounds 1 - 4 showed IC50 values of 1.1, 3.2, 2.3 and 1.4 microM, respectively, against ROS generation and no toxicity up to 31.25 microg/mL against HL-60 cells. Gallagic acid (2) and punicalagins (4) exhibited antiplasmodial activity against Plasmodium falciparum D6 and W2 clones with IC50 values of 10.9, 10.6, 7.5 and 8.8 microM, respectively. Fractions XAD-EtOAc, XAD-BuOH, XAD-H2O and XAD-PJ compounds 1 - 4 revealed antimicrobial activity when assayed against Escherichia coli, Pseudomonas aeruginosa, Candida albicans, Cryptococcus neoformans, methicillin-resistant Staphylococcus aureus (MRSA), Aspergillus fumigatus and Mycobacterium intracellulare. Compounds 2 and 4 showed activity against P. aeruginosa, C. neoformans, and MRSA. This is the first report on the antioxidant, antiplasmodial and antimicrobial activities of POMx isolates, including structure-activity relationships (SAR) of the free radical inhibition activity of compounds 1 - 4. Our results suggest a beneficial effect from the daily intake of POMx and pomegranate juice (PJ) as dietary supplements to augment the human immune system's antioxidant, antimalarial and antimicrobial capacities.

  12. Polyphenolic content, in vitro antioxidant activity and chemical composition of extract from Nephelium lappaceum L. (Mexican rambutan) husk.

    PubMed

    Hernández, Cristian; Ascacio-Valdés, Juan; De la Garza, Heliodoro; Wong-Paz, Jorge; Aguilar, Cristóbal Noé; Martínez-Ávila, Guillermo Cristian; Castro-López, Cecilia; Aguilera-Carbó, Antonio

    2017-12-01

    To determinate the recovery of total polyphenolic compounds content, in vitro antioxidant activity and HPLC/ESI/MS characterization of extract from Nephelium lappaceum L. (Mexican rambutan). The rambutan husk extract was obtained by aqueous extraction and a polyphenolic fraction was recovered using Amberlite XAD-16. The total polyphenolic compounds content was determined by the Folin Ciocalteu and butanol-HCI methods. In vitro antioxidant activity was performed using ABTS and ferric reducing antioxidant power methods. Mexican rambutan husk showed a total polyphenolic content of 582 mg/g and an evident antioxidant activity by ABTS and ferric reducing antioxidant power analysis. The HPLC/ESI/MS assay allowed the identification of 13 compounds, most of which belong to ellagitannins. Geraniin, corilagin and ellagic acid were present in the sample; the mineral composition was also evaluated. Rambutan husk cultivated in Mexico is a promising source for the recovery of added value bioactive compounds with antioxidant activity, which have potential applications as bioactive antioxidant agents for the treatment of diseases. Copyright © 2017 Hainan Medical University. Production and hosting by Elsevier B.V. All rights reserved.

  13. Recovery of carboxylic acids produced during dark fermentation of food waste by adsorption on Amberlite IRA-67 and activated carbon.

    PubMed

    Yousuf, Ahasa; Bonk, Fabian; Bastidas-Oyanedel, Juan-Rodrigo; Schmidt, Jens Ejbye

    2016-10-01

    Amberlite IRA-67 and activated carbon were tested as promising candidates for carboxylic acid recovery by adsorption. Dark fermentation was performed without pH control and without addition of external inoculum at 37°C in batch mode. Lactic, acetic and butyric acids, were obtained, after 7days of fermentation. The maximum acid removal, 74%, from the Amberlite IRA-67 and 63% from activated carbon was obtained from clarified fermentation broth using 200gadsorbent/Lbroth at pH 3.3. The pH has significant effect and pH below the carboxylic acids pKa showed to be beneficial for both the adsorbents. The un-controlled pH fermentation creates acidic environment, aiding in adsorption by eliminating use of chemicals for efficient removal. This study proposes simple and easy valorization of waste to valuable chemicals. Copyright © 2016 Elsevier Ltd. All rights reserved.

  14. Water Quality Research Program: Recent Developments in the Analysis of Metals in Water, Wastewater, and Other Matrices.

    DTIC Science & Technology

    1987-11-01

    for various types of samples and acids. The system features PFA -closed vessels that will tolerate up to 100 psi, a Teflon-lined cavity that reduces...complexes. Selec- tivity is accomplished by masking agents and pH adjustment and sorption on a small XAD-4 resin column. Evaporation of solvent 119...same pH, Cr(VI) is selectively reduced to Cr(III) and accumulated by adsorption at -0.3 V versus SCE (Batley and Matousek 1980). 150. Sorption , ion

  15. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) coupled to XAD fractionation: Method to algal organic matter characterization.

    PubMed

    Nicolau, Rudy; Leloup, Maud; Lachassagne, Delphine; Pinault, Emilie; Feuillade-Cathalifaud, Geneviève

    2015-05-01

    This work is focused on the development of an analytical procedure for the improvement of the Organic Matter structure characterization, particularly the algal matter. Two fractions of algal organic matter from laboratory cultures of algae (Euglena gracilis) and cyanobacteria (Microcystis aeruginosa) were extracted with XAD resins. The fractions were studied using laser desorption ionization (LDI) and Matrix-Assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF). A comparison with the natural organic matter characteristics from commercial humic acids and fulvic acids extracted from Suwannee River was performed. Results show that algal and natural organic matters have unique quasi-polymeric structures. Significant repeating patterns were identified. Different fractions extracted from organic matter with common origin had common structures. Thus, 44, 114 and 169Da peaks separation for fractions from E. gracilis organic matter and 28, 58 and 100Da for M. aeruginosa ones were clearly observed. Using the developed protocol, a structural scheme and organic matter composition were obtained. The range 600-2000Da contained more architectural composition differences than the range 100-600Da, suggesting that organic matter is composed of an assembly of common small molecules. Associated to specific monomers, particular patterns were common to all samples but assembly and resulting structure were unique for each organic matter. Thus, XAD fractionation coupled to mass spectroscopy allowed determining a specific fingerprint for each organic matter. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Carbon Isotope Composition as an Indicator of DOC Sources to a Stream During Events in a Temperate Forested Catchment

    NASA Astrophysics Data System (ADS)

    Doctor, D. H.; Sebestyen, S. D.; Aiken, G. R.; Shanley, J. B.; Kendall, C.; Boyer, E. W.

    2006-12-01

    Increased DOC flux in streams and rivers is commonly observed during high runoff regimes, however DOC concentrations alone do not provide information about multiple sources or pathways of DOC to streams. In an effort to gain this information, we measured DOC concentrations and stable carbon isotope composition (δ13C-DOC) on samples collected at high-frequency during events at Sleepers River Research Watershed in Vermont, USA. During snowmelt and storm events, peaks in stream DOC concentration (up to 10.5 mg/L) were coincident with peaks in flow. Stream water δ13C-DOC measurements ranged between -23.7‰ and - 28.9‰ and indicated changing sources of DOC during events; the highest δ13C-DOC values occurred consistently at the lowest flows, and the lowest δ13C-DOC values occurred with peaks in discharge. Water samples collected from shallow wells and stacked soil lysimeters showed the highest DOC concentrations in the most shallow (<0.5 m) lysimeter waters, and the lowest concentrations in the deeper (>1.5 m) well waters. Wells and lysimeters exhibited a range of δ13C-DOC values similar to those observed in the stream; however, samples collected from shallow horizons at nested wells and lysimeters consistently showed lower δ13C-DOC values than those from greater depths. Maple leaf litter collected from across the watershed provided an end-member of fresh organic material, with average δ13C composition of -31.3±0.7‰ (n=57), which is lower than the lowest measured DOC values in any of the stream, well, or lysimeter waters. A subset of stream waters were fractionated onto XAD4 and XAD8 resins; the hydrophobic acid fraction (XAD8) had consistently lower δ13C values than the transphilic acid fraction (XAD4), and both of these were lower than those of the bulk DOC. Samples with lower δ13C-DOC values also exhibited higher SUVA-254 values, i.e. greater aromaticity. Thus, lower δ13C-DOC values are interpreted as an indicator of relatively "fresh", more aromatic and more biologically labile material while higher δ13C-DOC values indicate relatively more degraded material. Since lower δ13C-DOC values were observed in the shallowest well and lysimeter waters and in stream water during periods of highest DOC flux, we surmise that fresh DOC is mobilized to the stream along relatively shallow flowpaths during high flows, and that a second source of more degraded DOC supplies background concentrations to the stream at lower flows.

  17. Stabilization of pH in solid-matrix hydroponic systems

    NASA Technical Reports Server (NTRS)

    Frick, J.; Mitchell, C. A.

    1993-01-01

    2-[N-morpholino]ethanesulfonic acid (MES) buffer or Amberlite DP-1 (cation-exchange resin beads) were used to stabilize substrate pH of passive-wicking, solid-matrix hydroponic systems in which small canopies of Brassica napus L. (CrGC 5-2, genome : ACaacc) were grown to maturity. Two concentrations of MES (5 or 10 mM) were included in Hoagland 1 nutrient solution. Alternatively, resin beads were incorporated into the 2 vermiculite : 1 perlite (v/v) growth medium at 6% or 12% of total substrate volume. Both strategies stabilized pH without toxic side effects on plants. Average seed yield rates for all four pH stabilization treatments (13.3 to 16.9 g m-2 day-1) were about double that of the control (8.2 g m-2 day-1), for which there was no attempt to buffer substrate pH. Both the highest canopy seed yield rate (16.9 g m-2 day-1) and the highest shoot harvest index (19.5%) occurred with the 6% resin bead treatment, even though the 10 mM MES and 12% bead treatments maintained pH within the narrowest limits. The pH stabilization methods tested did not significantly affect seed oil and protein contents.

  18. Determination of the total concentration and speciation of metal ions in river, estuarine and seawater samples.

    PubMed

    Alberti, Giancarla; Biesuz, Raffaela; Pesavento, Maria

    2008-12-01

    Different natural water samples were investigated to determine the total concentration and the distribution of species for Cu(II), Pb(II), Al(III) and U(VI). The proposed method, named resin titration (RT), was developed in our laboratory to investigate the distribution of species for metal ions in complex matrices. It is a competition method, in which a complexing resin competes with natural ligands present in the sample to combine with the metal ions. In the present paper, river, estuarine and seawater samples, collected during a cruise in Adriatic Sea, were investigated. For each sample, two RTs were performed, using different complexing resins: the iminodiacetic Chelex 100 and the carboxylic Amberlite CG50. In this way, it was possible to detect different class of ligands. Satisfactory results have been obtained and are commented on critically. They were summarized by principal component analysis (PCA) and the correlations with physicochemical parameters allowed one to follow the evolution of the metals along the considered transect. It should be pointed out that, according to our findings, the ligands responsible for metal ions complexation are not the major components of the water system, since they form considerably weaker complexes.

  19. Separation and purification of γ-aminobutyric acid from fermentation broth by flocculation and chromatographic methodologies.

    PubMed

    Gao, Qiang; Duan, Qiang; Wang, Depei; Zhang, Yunze; Zheng, Chunyang

    2013-02-27

    To date, the multifunctional γ-aminobutyric acid (GABA) is mainly produced by microbial fermentation in industry. The purpose of this study was to find an effective method for separation and purification of 31.2 g/L initial GABA from the fermentation broth of Enterococcus raffinosus TCCC11660. To remove the impurities from fermentation broth, flocculation pretreatment using chitosan and sodium alginate was first implemented to facilitate subsequent filtration. Ultrafiltration followed two discontinuous diafiltration steps to effectively remove proteins and macromolecular pigments, and the resulting permeate was further decolored by DA201-CII resin at a high decoloration ratio and GABA recovery. Subsequently, ion exchange chromatography (IEC) with Amberlite 200C resin and gradient elution were applied for GABA separation from glutamate and arginine. Finally, GABA crystals of 99.1% purity were prepared via warm ethanol precipitation twice. Overall, our results reveal that the successive process including flocculation, filtration, ultrafiltration, decoloration, IEC, and crystallization is promising for scale-up GABA extraction from fermentation broth.

  20. Novel diffusive gradients in thin films technique to assess labile sulfate in soil.

    PubMed

    Hanousek, Ondrej; Mason, Sean; Santner, Jakob; Chowdhury, Md Mobaroqul Ahsan; Berger, Torsten W; Prohaska, Thomas

    2016-09-01

    A novel diffusive gradients in thin films (DGT) technique for sampling labile soil sulfate was developed, based on a strong basic anion exchange resin (Amberlite IRA-400) for sulfate immobilization on the binding gel. For reducing the sulfate background on the resin gels, photopolymerization was applied instead of ammonium persulfate-induced polymerization. Agarose cross-linked polyacrylamide (APA) hydrogels were used as diffusive layer. The sulfate diffusion coefficient in APA gel was determined as 9.83 × 10(-6) ± 0.35 × 10(-6) cm(2) s(-1) at 25 °C. The accumulated sulfate was eluted in 1 mol L(-1) HNO3 with a recovery of 90.9 ± 1.6 %. The developed method was tested against two standard extraction methods for soil sulfate measurement. The obtained low correlation coefficients indicate that DGT and conventional soil test methods assess differential soil sulfate pools, rendering DGT a potentially important tool for measuring labile soil sulfate.

  1. Studies on the potent bacterial mutagen, 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone: aqueous stability, XAD recovery and analytical determination in drinking water and in chlorinated humic acid solutions.

    PubMed

    Meier, J R; Knohl, R B; Coleman, W E; Ringhand, H P; Munch, J W; Kaylor, W H; Streicher, R P; Kopfler, F C

    1987-12-01

    3-Chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX) was detected by gas chromatography/mass spectrometry in drinking water samples from 3 locations in the U.S.A., and also in a chlorinated humic acid solution. MX appears to account for a significant proportion of the mutagenicity of these samples, as measured in the Ames test using strain TA100 without metabolic activation. Studies on recovery of MX from spiked water samples by XAD-2/8 resin adsorption/acetone elution indicated that sample acidification prior to resin adsorption was essential to the effective recovery of MX. The stability of MX in aqueous solution was pH and temperature dependent. At 23 degrees C the order of stability, based on persistence of mutagenic activity was found to be: pH 2 greater than pH 4 greater than pH 8 greater than pH 6. The half-life at pH 8 and 23 degrees C was 4.6 days. One of the degradation products has been tentatively identified as 2-chloro-3-(dichloromethyl)-4-oxo-2-butenoic acid, an open form of MX which appears to be in the "E" configuration. Overall, these results suggest that MX is formed during water chlorination as a result of reaction of chlorine with humic substances, and that a substantial fraction of the MX formed is likely to persist throughout the distribution system.

  2. Unique reversibility in extraction mechanism of U compared to solvent extraction for sorption of U(VI) and Pu(IV) by a novel solvent impregnated resin containing trialkyl phosphine oxide functionalized ionic liquid.

    PubMed

    Paramanik, M; Panja, S; Dhami, P S; Yadav, J S; Kaushik, C P; Ghosh, S K

    2018-07-15

    Novel Solvent Impregnated Resin (SIR) material was prepared by impregnating a trialkyl phosphine oxide functionalized ionic liquid (IL) into an inert polymeric material XAD-7. A series of SIR materials were prepared by varying the IL quantity. Sorption of both U(VI) and Pu(IV) were found to increase with increasing IL concentration in SIR up to an optimum IL concentration of 435 mg g -1 of SIR beyond which no effect of IL concentration was observed. A change of mechanism of sorption for U(VI) by SIR was observed in comparison to solvent extraction. The dependency of U(VI) sorption with nitric acid concentration showed a reverse trend compared to solvent extraction studies while for Pu(IV) the trend remained same as observed with solvent extraction. Sorption of both the radionuclides was found to follow pseudo second order mechanism and Langmuir adsorption isotherm. Distribution co-efficient measurements on IL impregnated SIR showed highly selective sorption of U(VI) and Pu(IV) over other trivalent f-elements and fission products from nitric acid medium. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Antioxidant and antimicrobial effects of phenolic compounds extracts of Northeast Portugal honey.

    PubMed

    Estevinho, Letícia; Pereira, Ana Paula; Moreira, Leandro; Dias, Luís G; Pereira, Ermelinda

    2008-12-01

    Phenolic compounds of dark and clear honeys from Trás-os-Montes of Portugal were extracted with Amberlite XAD-2 and evaluated for their antioxidant and antimicrobial activities. The antioxidant effect was studied using the in vitro test capacity of scavenge the 2,2-diphenyl-1-picryhydrazyl (DPPH) free radical and of reducing power of iron (III)/ferricyanide complex. The antimicrobial activity was screened using three Gram-positive bacteria (Bacillus subtilis, Staphylococcus aureus, Staphylococcus lentus) and three Gram-negative bacteria (Pseudomonas aeruginosa, Klebsiella pneumoniae and Escherichia coli). The results obtained from the partial identification of honey phenolic compounds by high-performance liquid chromatography with a diode array detector showed that p-hydroxibenzoic acid, cinnamic acid, naringenin, pinocembrin and chrysin are the phenolic compounds present in most of the samples analyzed. Antioxidant potential was dependent of honey extract concentration and the results showed that dark honey phenolic compounds had higher activity than the obtained from clear honey. In the biological assays, results showed that S. aureus were the most sensitive microrganisms and B. subtilis, S. lentus, K. pneumoniae and E. coli were each moderately sensitive to the antimicrobial activity of honey extracts. Nevertheless, no antimicrobial activity was observed in the test with P. aeruginosa.

  4. Ion Exchange Technology Development in Support of the Urine Processor Assembly Precipitation Prevention Project for the International Space Station

    NASA Technical Reports Server (NTRS)

    Mitchell, Julie L.; Broyan, James L.; Pickering, Karen D.; Adam, Niklas; Casteel, Michael; Callahan, Michael; Carrier, Chris

    2012-01-01

    In support of the Urine Processor Assembly Precipitation Prevention Project (UPA PPP), multiple technologies were explored to prevent CaSO4 2H2O (gypsum) precipitation during the on-orbit distillation process. Gypsum precipitation currently limits the water recovery rate onboard the International Space Station (ISS) to 70% versus the planned 85% target water recovery rate. Due to its ability to remove calcium cations in pretreated augmented urine (PTAU), ion exchange was selected as one of the technologies for further development by the PPP team. A total of 13 ion exchange resins were evaluated in various equilibrium and dynamic column tests with solutions of dissolved gypsum, urine ersatz, PTAU, and PTAU brine at 85% water recovery. While initial evaluations indicated that the Purolite SST60 resin had the highest calcium capacity in PTAU (0.30 meq/mL average), later tests showed that the Dowex G26 and Amberlite FPC12H resins had the highest capacity (0.5 meq/mL average). Testing at the Marshall Spaceflight Center (MSFC) integrates the ion exchange technology with a UPA ground article under flight-like pulsed flow conditions with PTAU. To date, no gypsum precipitation has taken place in any of the initial evaluations.

  5. Potential Dermal Exposure to Flonicamid and Risk Assessment of Applicators During Treatment in Apple Orchards.

    PubMed

    Zhao, Mei-Ai; Yu, Aili; Zhu, Yong-Zhe; Kim, Jeong-Han

    2015-01-01

    Exposure and risk assessments of flonicamid for applicators were performed in apple orchards in Korea. Fifteen experiments were done with two experienced applicators under typical field conditions using a speed sprayer. In this study, cotton gloves, socks, masks, and dermal patches were used to monitor potential dermal exposure to flonicamid, and personal air samplers with XAD-2 resin and glass fiber filter were used to monitor potential inhalation exposure. The analytical methods were validated for the limit of detection, limit of quantitation, reproducibility, linearity of the calibration curve, and recovery of flonicamid from various exposure matrices. The results were encouraging and acceptable for an exposure study. The applicability of XAD-2 resin was evaluated via a trapping efficiency and breakthrough test. During the mixing/loading, the average total dermal exposure was 22.6 μg of flonicamid, corresponding to 4.5×10(-5)% of the prepared amount. For the spraying, the potential dermal exposure was 9.32 mg, and the ratio to applied amount was 1.9 × 10(-2%). The primary exposed body parts were the thigh (2.90 mg), upper arm (1.75 mg), and lower leg (1.66 mg). By comparison, absorbable quantity of exposure was small, only 1.62 μg (3.2×10(-6)%). The margin of safety (MOS) were calculated for risk assessment, in all sets of trials, MOS > 1, indicating the exposure level of flonicamid was considered to be safe in apple orchards. Although this was a limited study, it provided a good estimate of flonicamid exposure for orchard applicators.

  6. Presence of organophosphorus pesticide oxygen analogs in air samples

    NASA Astrophysics Data System (ADS)

    Armstrong, Jenna L.; Fenske, Richard A.; Yost, Michael G.; Galvin, Kit; Tchong-French, Maria; Yu, Jianbo

    2013-02-01

    A number of recent toxicity studies have highlighted the increased potency of oxygen analogs (oxons) of several organophosphorus (OP) pesticides. These findings were a major concern after environmental oxons were identified in environmental samples from air and surfaces following agricultural spray applications in California and Washington State. This paper reports on the validity of oxygen analog measurements in air samples for the OP pesticide, chlorpyrifos. Controlled environmental and laboratory experiments were used to examine artificial formation of chlorpyrifos-oxon using OSHA Versatile Sampling (OVS) tubes as recommended by NIOSH method 5600. Additionally, we compared expected chlorpyrifos-oxon attributable to artificial transformation to observed chlorpyrifos-oxon in field samples from a 2008 Washington State Department of Health air monitoring study using non-parametric statistical methods. The amount of artificially transformed oxon was then modeled to determine the amount of oxon present in the environment. Toxicity equivalency factors (TEFs) for chlorpyrifos-oxon were used to calculate chlorpyrifos-equivalent air concentrations. The results demonstrate that the NIOSH-recommended sampling matrix (OVS tubes with XAD-2 resin) was found to artificially transform up to 30% of chlorpyrifos to chlorpyrifos-oxon, with higher percentages at lower concentrations (<30 ng m-3) typical of ambient or residential levels. Overall, the 2008 study data had significantly greater oxon than expected by artificial transformation, but the exact amount of environmental oxon in air remains difficult to quantify with the current sampling method. Failure to conduct laboratory analysis for chlorpyrifos-oxon may result in underestimation of total pesticide concentration when using XAD-2 resin matrices for occupational or residential sampling. Alternative methods that can accurately measure both OP pesticides and their oxygen analogs should be used for air sampling, and a toxicity equivalent factor approach should be used to determine potential health risks from exposures.

  7. A new sampler for collecting separate dry and wet atmospheric depositions of trace organic chemicals

    NASA Astrophysics Data System (ADS)

    Waite, Don T.; Cessna, Allan J.; Gurprasad, Narine P.; Banner, James

    Studies conducted in Saskatchewan and elsewhere have demonstrated the atmospheric transport of agricultural pesticides and other organic contaminants and their deposition into aquatic ecosystems. To date these studies have focused on ambient concentrations in the atmosphere and in wet precipitation. To measure the dry deposition of organic chemicals, a new sampler was designed which uses a moving sheet of water to passively trap dry particles and gasses. The moving sheet of water drains into a reservoir and, during recirculation through the sampler, is passed through an XAD-2 resin column which adsorbs the trapped organic contaminants. All surfaces which contact the process water are stainless steel or Teflon. Chemicals collected can be related to airborne materials depositing into aquatic ecosystems. The sampler has received a United States patent (number 5,413,003 - 9 May 1996) with the Canadian patent pending. XAD-2 resin adsorption efficiencies for 10 or 50 μg fortifications of ten pesticides ranged from 76% for atrazine (2-chloro-4-ethylamino-6-isopropylamino- S-triazine) to 110% for triallate [ S-(2,3,3-trichloro-2-phenyl)bis(1-methylethyl)carbamothioate], dicamba (2-methoxy-3,6-dichlorobenzoic acid) and toxaphene (chlorinated camphene mixture). Field testing using duplicate samplers showed good reproducibility and amounts trapped were consistent with those from high volume and bulk pan samplers located on the same site. Average atmospheric dry deposition rates of three chemicals, collected for 5 weeks in May and June, were: dicamba, 69 ng m -2 da -1; 2,4-D (2,4-dichlorophenoxyacetic acid), 276 ng m -2 da -1: and, γ-HCH ( γ-1, 2, 3, 4, 5, 6-hexachlorocyclohexane), 327 ng m -2 da -1.

  8. Processing scale-up of sicklepod (Senna obtusifolia L.) seed.

    PubMed

    Harry-O'Kuru, Rogers E; Mohamed, Abdellatif

    2009-04-08

    Sicklepod (Senna obtusifolia L.) is an invasive weed species especially of soybean and other field crops in the southeastern United States. The seeds contain a small amount (5-7%) of a highly colored fat as well as various phenolics, proteins, and galactomannans. The color of sicklepod seed oil is such that the presence of a small amount of the weed seed in a soybean crush lowers the quality of the soybean oil. Sicklepod is very prolific, and even volunteer stands yield >1000 lb of seed per acre, and prudence calls for tapping the potential of this weed as an alternative economic crop in the affected region. Pursuant to this, we have shown in laboratory-scale work the feasibility of separating the components of sicklepod seed. However, at kilogram and higher processing quantities, difficulties arise leading to modification of the earlier approach in order to efficiently separate components of the defatted seed meal. In a version for cleanly separating the proteins, the defatted meal was extracted with 0.5 M NaCl solution to remove globular proteins. Prolamins were extracted from the pellet left after salt extraction using 80% ethanol, and glutelins were then obtained in 0.1 N alkali from the residual solids left from ethanol treatment. In a pilot-scale version for water-soluble polysaccharides, the defatted meal was stirred with deionized water (DI) and centrifuged. The pooled centrifugates were heated to 92 degrees C (20-25 min), filtered, cooled to room temperature, and passed through a column of Amberlite XAD-4 to separate the polysaccharides from the anthraquinones. Senna obtusifolia L. is a one-stop-shop of a seed (from food components to medicinals).

  9. Diffusive gradients in thin films measurement of sulfur stable isotope variations in labile soil sulfate.

    PubMed

    Hanousek, Ondrej; Santner, Jakob; Mason, Sean; Berger, Torsten W; Wenzel, Walter W; Prohaska, Thomas

    2016-11-01

    A diffusive gradient in thin films (DGT) technique, based on a strongly basic anion exchange resin (Amberlite IRA-400), was successfully tested for 34 S/ 32 S analysis in labile soil sulfate. Separation of matrix elements (Na, K, and Ca) that potentially cause non-spectral interferences in 34 S/ 32 S analysis by MC ICP-MS (multi-collector inductively coupled plasma-mass spectrometry) during sampling of sulfate was demonstrated. No isotopic fractionation caused by diffusion or elution of sulfate was observed below a resin gel disc loading of ≤79 μg S. Above this threshold, fractionation towards 34 S was observed. The method was applied to 11 different topsoils and one mineral soil profile (0-100 cm depth) and compared with soil sulfate extraction by water. The S amount and isotopic ratio in DGT-S and water-extractable sulfate correlated significantly (r 2  = 0.89 and r 2  = 0.74 for the 11 topsoils, respectively). The systematically lower 34 S/ 32 S isotope ratios of the DGT-S were ascribed to mineralization of organic S.

  10. Tannins and terpenoids as major precursors of Suwannee River fulvic acid

    USGS Publications Warehouse

    Leenheer, Jerry A.; Rostad, Colleen E.

    2004-01-01

    Suwannee River fulvic acid (SRFA) was fractionated into 7 fractions by normal-phase chromatography on silica gel followed by reverse-phase fractionation on XAD-8 resin that produced 18 subfractions. Selected major subfractions were characterized by 13C-nuclear magnetic resonance (NMR), infrared spectrometry, and elemental analyses. 13C-NMR spectra of the subfractions were more indicative of precursor structures than unfractionated SRFA, and gave spectral profiles that indicated SRFA mass was about equally split between tannin precursors and terpenoid precursors. Lignin precursors were minor components. Synthesis of 13C-NMR data with elemental data for subfractions derived from both tannin and terpenoid precursors revealed high ring contents and low numbers of carbon per rings which is indicative of fused ring structures that are extensively substituted with carboxyl and methyl groups. These results ruled out extended chain structures for SRFA. This information is useful for determining sources and properties of fulvic acid in drinking water supplies as tannins are more reactive with chlorine to produce undesirable disinfection by-products than are terpenoids.

  11. New phenolic grape skin products from Vitis vinifera cv. Pinot Noir.

    PubMed

    Kneknopoulos, Petros; Skouroumounis, George K; Hayasaka, Yoji; Taylor, Dennis K

    2011-02-09

    Anthocyanins and their related compounds were extracted from grape skins of Pinot noir, using 50% aqueous methanol, and purified by solid phase extraction chromatography using XAD-7 resin to obtain a pigment-rich fraction. This fraction was subjected to multilayer coil countercurrent chromatography (MLCCC) using a quaternary solvent system consisting of tert-butyl methyl ether/n-butanol/acetonitrile/water acidified with 0.01% trifluoroacetic acid (2:2:0.1-1.8:5) (v/v/v/v) in a step gradient elution to separate anthocyanin oligomers from grape anthocyanins. In the process of the characterization of the MLCCC fractions by electrospray mass spectrometry, two noncolored anthocyanin derivatives were found and characterized on the basis of their mass spectral data. As a result, these compounds have been tentatively identified as coupling products between both hydrated malvidin-3-glucoside and peonidin-3-glucoside, with 2-S-glutathionyl caffeoyl tartaric acid (GRP). It is therefore proposed that grape skins contain this new class of coupling product, and a possible chemical pathway for their formation is suggested.

  12. Diffusive gradients in thin-films (DGT) for in situ sampling of selected endocrine disrupting chemicals (EDCs) in waters.

    PubMed

    Chen, Wei; Pan, Suhong; Cheng, Hao; Sweetman, Andrew J; Zhang, Hao; Jones, Kevin C

    2018-06-15

    A passive water sampler based on the diffusive gradients in thin-films (DGT) technique was developed and tested for 3 groups of endocrine disrupting chemicals (EDCs, including oestrogens, alkyl-phenols and bisphenols). Three different resins (hydrophilic-lipophilic-balanced (HLB), XAD18 and Strata-XL-A (SXLA)) were investigated for their suitability as the binding phase for DGT devices. Laboratory tests across a range of pH (3.5-9.5), ionic strength (0.001-0.5 M) and dissolved organic matter concentration (0-20 mg L -1 ) showed HLB and XAD18-DGT devices were more stable compared to SXLA-DGT. HLB-DGT and XAD18-DGT accumulated test chemicals with time consistent with theoretical predictions, while SXLA-DGT accumulated reduced amounts of chemical. DGT performance was also compared in field deployments up to 28 days, alongside conventional active sampling at a wastewater treatment plant. Uptake was linear to the samplers over 18 days, and then began to plateau/decline, indicating the maximum deployment time in those conditions. Concentrations provided by the DGT samplers compared well with those provided by auto-samplers. DGT integrated concentrations over the deployment period in a way that grab-sampling cannot. The advantages of the DGT sampler over active sampling include: low cost, ease of simultaneous multi-site deployment, in situ analyte pre-concentration and reduction of matrix interferences compared with conventional methods. Compared to other passive sampler designs, DGT uptake is independent of flow rate and therefore allows direct derivation of field concentrations from measured compound diffusion coefficients. This passive DGT sampler therefore constitutes a viable and attractive alternative to conventional grab and active water sampling for routine monitoring of selected EDCs. Copyright © 2018 Elsevier Ltd. All rights reserved.

  13. Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection.

    PubMed

    Mokbel, Haifaa; Al Dine, Enaam Jamal; Elmoll, Ahmad; Liaud, Céline; Millet, Maurice

    2016-04-01

    An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R (2)) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m(-3), and limits of quantification (LOQs) are between 0.05 and 9.12 ng m(-3) and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere.

  14. Pb-binding to various dissolved organic matter in urban aquatic systems: Key role of the most hydrophilic fraction

    NASA Astrophysics Data System (ADS)

    Pernet-Coudrier, Benoît; Companys, Encarnació; Galceran, Josep; Morey, Margalida; Mouchel, Jean-Marie; Puy, Jaume; Ruiz, Núria; Varrault, Gilles

    2011-07-01

    Dissolved organic matter (DOM) from the treated effluent of a wastewater treatment plant and from the river Seine under high human pressure has been separated into three fractions: hydrophobic (containing humic and fulvic substances), transphilic and hydrophilic using a two column array of XAD-8 and XAD-4 resins. The acid base properties and the binding characteristics with respect to Pb ions (using the new electroanalytical technique AGNES, Absence of Gradients and Nernstian Equilibrium Stripping) have been studied and fitted to NICA (Non-Ideal Competitive Isotherm). We evaluated the binding potential of each DOM fraction in order to better predict the speciation of Pb and, later, its bioavailability in the river. The total binding capacity of the different fractions to Pb, as well as the total titratable charge, reaches its maximum value at the most hydrophilic fraction from the treated effluent. Specific properties of the distribution of the complexing sites within each DOM fraction have been exposed by plotting the conditional affinity spectrum (CAS). The addition of these distributions, weighted according to the respective abundance of each organic fraction, allows for a full description of the Pb binding properties of the whole DOM of a sampling site. Despite its weak aromaticity, the hydrophilic fraction from the wastewater treatment plant effluent exhibits a high lead binding affinity, so that at typical environmental pH and free Pb levels (0.1 μg L -1), Pb is mainly bound to the most hydrophilic fraction of the treated effluent (49% of bound Pb at pH 7). This feature may greatly enhance the transport of Pb and highlights that Pb speciation should also consider other fractions apart from humic and/or fulvic acids when studying surface waters under high human pressure.

  15. Coupling ASE, sylilation and SPME-GC/MS for the analysis of current-used pesticides in atmosphere.

    PubMed

    Raeppel, Caroline; Fabritius, Marie; Nief, Marie; Appenzeller, Brice M R; Millet, Maurice

    2014-04-01

    An analytical methodology using Accelerated Solvent Extraction (ASE) and a sylilation procedure coupled to Solid Phase Micro-Extraction (SPME) and GC/MS was developed for the determination of 31 pesticides of different chemical classes (urea, phenoxy acids, pyrethrenoïds, etc.) commonly used in non-agricultural areas in atmospheric samples. This methodology was developed to evaluate the outdoor atmospheric contamination by non-agricultural pesticides. Pesticides were simultaneously sampled on glass fibre filters and on XAD-2 resin traps by using a low volume sampler (Partisol) for 1 week. Traps were extracted by Accelerated Solvent Extraction (ASE) with acetonitrile and concentrated to 1 mL by using a rotary evaporator. 500 µL of the extract was dissolved in 19.5 mL of 1.5% NaCl acidified water (pH=3) and SPME extracted by PA fibre for 55 min at 50 °C. Since most of the studied pesticides are polar or thermo-labile, a derivatisation step by injection of 2 µL of MtBSTFA just before SPME desorption was done. MtBSTFA was chosen since it delivers very specific ions on electronic impact (m/z=M-57). Detection limits varied between 5 and 179 ng resin(-1) and between 0.3 and 126 ng filter(-1) corresponding to 2 and 750 pg m(-3) and 30 and 1165 pg m(-3) for 168 m(3) of air pumped through traps. Quantification limits varied between 18 and 595 ng resin(-1) and between 1 and 420 ng filter(-1) corresponding to 107 and 3542 pg m(-3) and 6 and 2500 pg m(-3) for 168 m(3) of air pumped through traps. Uncertainties varied between 7.2% and 39.6% and between 7.2% and 53.4% respectively for filter and resin. The method was used for the analysis of atmospheric samples collected in a background urban site of Strasbourg (east of France) during spring and summer 2010. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Biosorption of lead and nickel by biomass of marine algae

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Holan, Z.R.; Volesky, B.

    Screening tests of different marine algae biomass types revealed a high passive biosorptive uptake of lead up to 270 mg Pb/g of biomass in some brown marine algae. Members of the order Fucales performed particularly well in this descending sequence: Fucus > Ascophyllum > Sargassum. Although decreasing the swelling of wetted biomass particles, their reinforcement by crosslinking may significantly affect the biosorption performance. Lead uptakes up to 370 mg Pb/g were observed in crosslinked Fucus vesiculosus and Ascophyllum nodosum. At low equilibrium residual concentrations of lead in solution, however, ion exchange resin Amberlite IR-120 had a higher lead uptake thanmore » the biosorbent materials. An order-of-magnitude lower uptake of nickel was observed in all of the sorbent materials examined.« less

  17. Chemical Composition and Antioxidant Properties of Powders Obtained from Different Plum Juice Formulations.

    PubMed

    Michalska, Anna; Wojdyło, Aneta; Łysiak, Grzegorz P; Figiel, Adam

    2017-01-17

    Among popular crops, plum ( Prunus domestica L.) has received special attention due to its health-promoting properties. The seasonality of this fruit makes it impossible to consume it throughout the year, so new products in a powder form may offer an alternative to fresh consumption and may be used as high-quality natural food ingredients. A 100% plum (cultivar "Valor") juice was mixed with three different concentrations of maltodextrin or subjected to sugars removal by amberlite-XAD column, and dried using the freeze, spray, and vacuum (40, 60, and 80 °C) drying techniques. The identification and quantification of phenolic acids, flavonols, and anthocyanins in plum powders was performed by LC-MS QTof and UPLC-PDA, respectively. l-ascorbic acid, hydroxymethylfurfural, and antioxidant capacity were measured by the Trolox equivalent antioxidant capacity (TEAC) ABTS and ferric reducing antioxidant potential (FRAP) methods in order to compare the influence of the drying methods on product quality. The results indicated that the profile of polyphenolic compounds in the plum juice powders significantly differed from the whole plum powders. The drying of a sugar free plum extract resulted in higher content of polyphenolic compounds, l-ascorbic acid and antioxidant capacity, but lower content of hydroxymethylfurfural, regardless of drying method applied. Thus, the formulation of plum juice before drying and the drying method should be carefully selected in order to obtain high-quality powders.

  18. Isolation and characterization of feruloylated arabinoxylan oligosaccharides from the perennial cereal grain intermediate wheat grass (Thinopyrum intermedium).

    PubMed

    Schendel, Rachel R; Becker, Andreas; Tyl, Catrin E; Bunzel, Mirko

    2015-04-30

    In comparison to the annual grain crops dominating current agricultural production, perennial grain species require fewer chemical and energy inputs and improve soil health and erosion control. The possibility for producing sustainable grain harvests from marginal land areas is motivating research initiatives to integrate perennial grains into commercial cropping and food processing systems. In this study, the feruloylated arabinoxylans from intermediate wheat grass (Thinopyrum intermedium, IWG), a promising perennial grain candidate in agronomic screening studies, were investigated. Insoluble fiber isolated from IWG whole grain flour was subjected to either mildly acidic (50 mM TFA, 100 °C, 2 h) or enzymatic (Driselase) hydrolysis. The liberated feruloylated arabinoxylan oligosaccharides were concentrated with Amberlite XAD-2, separated with gel chromatography (Sephadex LH-20, water), and purified with reversed-phase HPLC (C18, water-MeOH gradient). Thirteen feruloylated oligosaccharides were isolated (including eight structures described for the first time) and identified by LC-ESI-MS and NMR. Linkage-type analysis via methylation analysis, as well as the monosaccharide and phenolic acid profiles of the IWG insoluble fiber were also determined. IWG feruloylated arabinoxylans have a relatively simple structure with only short feruloylated side chains, a lower backbone substitution rate than annual rye and wheat varieties, and a moderate phenolic acid content. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. Determining exhaust fumes exposure in chainsaw operations.

    PubMed

    Neri, F; Foderi, C; Laschi, A; Fabiano, F; Cambi, M; Sciarra, G; Aprea, M C; Cenni, A; Marchi, E

    2016-11-01

    The objective of this study was to investigate the inhalation exposure of forest operators to polycyclic aromatic hydrocarbons (PAHs) and BTEX (benzene, toluene, ethylbenzene and total xylenes) contained in the exhaust fumes released from chainsaws and to suggest possible countermeasures. The study was carried out in four silvicultural treatments (coppice clearcut, conifer thinning, conifer pruning, and sanitary cut), using three types of chainsaw fuel (normal two-stroke petrol mix and two alkylate fuels). Eighty personal air samples were collected; IOM samplers combined with Amberlite XAD-2 sorbent tubes were used for collecting PAHs and Radiello ® samplers were used for BTEX. Results indicate that none of the four silvicultural treatments significantly affected the PAHs and BTEX inhalation exposure of forest workers. On the other hand, statistically significant differences were recorded in the inhalation exposure to PAHs and BTEX when using different fuel types. In particular, the inhalation exposure to PAHs and BTEX was generally one order of magnitude lower when using modern alkylate fuels as compared to the traditional oil and lead-free petrol mixture. The small, non-statistically significant differences in inhalation exposure recorded between the two alkylate fuels suggests that the two fuels might be equivalent in terms of quality. Our study indicates that while forest workers are exposed to PAHs and BTEX, the maximum values are generally well below accepted occupational exposure limits. Copyright © 2016 Elsevier Ltd. All rights reserved.

  20. Chemical Composition and Antioxidant Properties of Powders Obtained from Different Plum Juice Formulations

    PubMed Central

    Michalska, Anna; Wojdyło, Aneta; Łysiak, Grzegorz P.; Figiel, Adam

    2017-01-01

    Among popular crops, plum (Prunus domestica L.) has received special attention due to its health-promoting properties. The seasonality of this fruit makes it impossible to consume it throughout the year, so new products in a powder form may offer an alternative to fresh consumption and may be used as high-quality natural food ingredients. A 100% plum (cultivar “Valor”) juice was mixed with three different concentrations of maltodextrin or subjected to sugars removal by amberlite-XAD column, and dried using the freeze, spray, and vacuum (40, 60, and 80 °C) drying techniques. The identification and quantification of phenolic acids, flavonols, and anthocyanins in plum powders was performed by LC-MS QTof and UPLC-PDA, respectively. l-ascorbic acid, hydroxymethylfurfural, and antioxidant capacity were measured by the Trolox equivalent antioxidant capacity (TEAC) ABTS and ferric reducing antioxidant potential (FRAP) methods in order to compare the influence of the drying methods on product quality. The results indicated that the profile of polyphenolic compounds in the plum juice powders significantly differed from the whole plum powders. The drying of a sugar free plum extract resulted in higher content of polyphenolic compounds, l-ascorbic acid and antioxidant capacity, but lower content of hydroxymethylfurfural, regardless of drying method applied. Thus, the formulation of plum juice before drying and the drying method should be carefully selected in order to obtain high-quality powders. PMID:28106740

  1. Adsorption and desorption properties of macroporous resins for anthocyanins from the calyx extract of roselle (Hibiscus sabdariffa L.).

    PubMed

    Chang, Xiu-Lian; Wang, Dong; Chen, Bi-Yun; Feng, Yong-Mei; Wen, Shao-Hong; Zhan, Peng-Yuan

    2012-03-07

    Adsorption of roselle anthocynins, a natural pigment, onto various macroporous resins was optimized to develop a simple and efficient process for industrial separation and purification of roselle anthocyanins. Nine different macroporous resins (AB-8, X-5, HPD-100, SP-207, XAD-4, LS-305A, DM-21, LS-610B, and LS-305) were evaluated for the adsorption properties of the anthocyanins extracted from the calyx extract of Hibiscus sabdariffa L. The influences of phase contact time, solution pH, initial anthocyanin concentration, and ethanol concentration with different citric acid amounts were studied by the static adsorption/desorption method. The adsorption isotherm data were fitted well to the Langmuir isotherm, and according to this model, LS-610B and LS-305 exhibited the highest monolayer sorption capacities of 31.95 and 38.16 mg/g, respectively. The kinetic data were modeled using pseudo-first-order, pseudo-second-order, and intraparticle diffusion equations. The experimental data were well described by the pseudo-second-order kinetic model. Continuous column adsorption-regeneration cycles indicated negligible capacity loss of LS-305 during operation. The overall yield of pigment product was 49.6 mg/g dried calyces. The content of roselle anthocynins in the pigment product was 4.85%.

  2. Antimicrobial cholic acid derivatives from the Pitch Lake bacterium Bacillus amyloliquefaciens UWI-W23.

    PubMed

    Dobson, Tresha E; Maxwell, Anderson R; Ramsubhag, Adesh

    2018-07-01

    Six cholic acid derivatives (1-6) were isolated from broth cultures of Bacillus amyloliquefaciens UWI-W23, an isolate from the Trinidad Pitch Lake. The compounds were extracted via solvent extraction and/or XAD resin adsorption and purified using silica gel column chromatography. Their structures were elucidated using 1D, 2D NMR and ESI-MS spectrometry and FT-IR spectrophotometry. One of the compounds, taurodeoxycholate (2) is for the first time being reported from a bacterial source while deoxycholate (4) is for the first time being reported from a Gram-positive bacterium. The other compounds have not been previously isolated from Bacillus spp. viz. cholate (1), taurocholic acid (3); glycodeoxycholic acid (5) and glycocholic acid (6). All six compounds exhibited antimicrobial activity against P. aeruginosa and B. cereus with MICs ranging from 7 to 250 µg/mL. Cholate (1) also showed activity against MRSA (MICs = 125 µg/mL) and glycocholic acid (6) against S. cerevisiae (MICs = 15.6 µg/mL). Copyright © 2018 Elsevier Inc. All rights reserved.

  3. Extraction, detection, and quantification of flavano-ellagitannins and ethylvescalagin in a Bordeaux red wine aged in oak barrels.

    PubMed

    Saucier, Cedric; Jourdes, Michael; Glories, Yves; Quideau, Stephane

    2006-09-20

    An extraction procedure and an analytical method have been developed to detect and quantify for the first time a series of ellagitannin derivatives formed in wine during aging in oak barrels. The method involves a preliminary purification step on XAD7 HP resin followed by a second purification step on TSK 40 HW gel. The resulting extract is analyzed for compound identification and quantitative determination by high-performance liquid chromatography-electrospray ionization-mass spectrometry in single ion recording mode. Reference compounds, which are accessible through hemisynthesis from the oak C-glycosidic ellagitannin vescalagin, were used to build calibration curves, and chlorogenic acid was selected as an internal standard. This method enabled us to estimate the content of four flavano-ellagitannins and that of another newly identified wine polyphenol, beta-1-O-ethylvescalagin, in a Bordeaux red wine aged for 18 months in oak barrels. All five ellagitannin derivatives are derived from the nucleophilic substitution reaction of vescalagin with the grape flavan-3-ols catechin and epicatechin or ethanol.

  4. Formation yields of C8 1,4-hydroxycarbonyls from OH + n-octane in the presence of NO.

    PubMed

    Aschmann, Sara M; Arey, Janet; Atkinson, Roger

    2012-12-18

    1,4-Hydroxycarbonyls are major products of the OH radical-initiated reactions of ≥ C₅ n-alkanes in the presence of NO. However, because of a lack of commercially available standards of 1,4-hydroxycarbonyls and difficulties in using gas chromatography for their analysis without prior derivatization, quantification of 1,4-hydroxycarbonyls in OH + alkane reactions has proven difficult. We have used an annular denuder coated with XAD resin and further coated with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine for in situ derivatization of the 1,4-hydroxycarbonyls formed from the OH + n-octane reaction in the presence of NO. Quantification was achieved by using 2,5-hexanedione as an internal standard. Formation yields for (7-hydroxy-4-octanone + 6-hydroxy-3-octanone + 5-hydroxy-2-octanone) and of 4-hydroxyoctanal of 61 ± 11% and 2.1 ± 0.5%, respectively, were obtained. When combined with previously measured or estimated formation yields for octyl nitrates and hydroxyoctyl nitrates, 93 ± 15% of the overall reaction products are accounted for, indicating that no additional reaction pathways remain to be identified.

  5. Ion Exchange Technology Development in Support of the Urine Processor Assembly Precipitation Prevention Project for the International Space Station

    NASA Technical Reports Server (NTRS)

    Mitchell, Julie L.; Broyan, James L.; Pickering, Karen D.; Adam, Niklas; Casteel, Michael; Callaham, Michael; Carrier, Chris

    2011-01-01

    In support of the Urine Processor Assembly Precipitation Prevention Project (UPA PPP), multiple technologies were explored to prevent CaSO4 dot 2H2O (gypsum) precipitation during the on-orbit distillation process. Gypsum precipitation currently limits the water recovery rate onboard the International Space Station (ISS) to 70% versus the planned 85% target water recovery rate. Due to its advanced performance in removing calcium cations in pretreated augmented urine (PTAU), ion exchange was selected as one of the technologies for further development by the PPP team. A total of 12 ion exchange resins were evaluated in various equilibrium and dynamic column tests with solutions of dissolved gypsum, urine ersatz, PTAU, and PTAU brine at 85% water recovery. While initial evaluations indicated that the Purolite SST60 resin had the highest calcium capacity in PTAU (0.30 meq/mL average), later tests showed that the Dowex G26 and Amberlite FPC12H resins had the highest capacity (0.5 meq/mL average). Further dynamic column testing proved that G26 performance is +/- 10% of that value at flow rates of 0.45 and 0.79 Lph under continuous flow, and 10.45 Lph under pulsed flow. Testing at the Marshall Spaceflight Center (MSFC) integrates the ion exchange technology with a UPA ground article under flight-like pulsed flow conditions with PTAU. To date, no gypsum precipitation has taken place in any of the initial evaluations.

  6. Selected organic pollutant emissions from unvented kerosene space heaters

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Traynor, G.W.; Apte, M.G.; Sokol, H.A.

    1990-08-01

    An exploratory study was performed to assess the semivolatile and nonvolatile organic pollutant emissions rates from unvented kerosene space heaters. A well-tuned radiant heater and maltuned convective heater were tested for semivolatile and nonvolatile organic pollutant emissions. Each heater was operated in a 27-m{sup 3} chamber with a prescribed on/off pattern. Organic compounds were collected on Teflon-impregnated glass filters backed by XAD-2 resin and analyzed by gas chromatography/mass spectrometry. Pollutant source strengths were calculated by use of a mass balance equation. The results show that kerosene heaters can emit polycyclic aromatic hydrocarbons (PAHs); nitrated PAHs; alkylbenzenes, phthalates; hydronaphthalenes; aliphatic hydrocarbons,more » alcohols, and ketones; and other organic compounds, some of which are known mutagens.« less

  7. Performance of Spent Mushroom Farming Waste (SMFW) Activated Carbon for Ni (II) Removal

    NASA Astrophysics Data System (ADS)

    Desa, N. S. Md; Ghani, Z. Ab; Talib, S. Abdul; Tay, C. C.

    2016-07-01

    The feasibility of a low cost agricultural waste of spent mushroom farming waste (SMFW) activated carbon for Ni(II) removal was investigated. The batch adsorption experiments of adsorbent dosage, pH, contact time, metal concentration, and temperature were determined. The samples were shaken at 125 rpm, filtered and analyzed using ICP-OES. The fifty percent of Ni(II) removal was obtained at 0.63 g of adsorbent dosage, pH 5-6 (unadjusted), 60 min contact time, 50 mg/L Ni(II) concentration and 25 °C temperature. The evaluated SMFW activated carbon showed the highest performance on Ni(II) removal compared to commercial Amberlite IRC86 resin and zeolite NK3. The result indicated that SMFW activated carbon is a high potential cation exchange adsorbent and suitable for adsorption process for metal removal. The obtained results contribute toward application of developed SMFW activated carbon in industrial pilot study.

  8. An evaluation of MES (2(N-Morpholino)ethanesulfonic acid) and Amberlite IRC-50 as pH buffers for nutrient solution studies

    NASA Technical Reports Server (NTRS)

    Bugbee, B. G.; Salisbury, F. B.

    1985-01-01

    All buffering agents used to stabilize pH in hydroponic research have disadvantages. Inorganic buffers are absorbed and may become phytotoxic. Solid carbonate salts temporarily mitigate decreasing pH but provide almost no protection against increasing pH, and they alter nutrient absorption. Exchange resins are more effective, but we find that they remove magnesium and manganese from solution. We have tested 2(N-Morpholino)ethanesulfonic acid (MES) as a buffering agent at concentrations of 1 and 10 mol m-3 (1 and 10 mM) with beans, corn, lettuce, tomatoes, and wheat. MES appears to be biologically inert and does not interact significantly with other solution ions. Relative growth rates among controls and MES treatments were nearly identical for each species during the trial period. The pH was stabilized by 1 mol m-3 MES. This buffer warrants further consideration in nutrient research.

  9. An intercomparison of three methods for the large-scale isolation of oceanic dissolved organic matter

    USGS Publications Warehouse

    Green, Nelson W.; Perdue, E. Michael; Aiken, George R.; Butler, Kenna D.; Chen, Hongmei; Dittmar, Thorsten; Niggemann, Jutta; Stubbins, Aron

    2014-01-01

    Dissolved organic matter (DOM) was isolated from large volumes of deep (674 m) and surface (21 m) ocean water via reverse osmosis/electrodialysis (RO/ED) and two solid-phase extraction (SPE) methods (XAD-8/4 and PPL) at the Natural Energy Laboratory of Hawaii Authority (NELHA). By applying the three methods to common water samples, the efficiencies of XAD, PPL and RO/ED DOM isolation were compared. XAD recovered 42% of dissolved organic carbon (DOC) from deep water (25% with XAD-8; 17% with XAD-4) and 30% from surface water (16% with XAD-8; 14% with XAD-4). PPL recovered 61 ± 3% of DOC from deep water and 61% from surface water. RO/ED recovered 82 ± 3% of DOC from deep water, 14 ± 3% of which was recovered in a sodium hydroxide rinse, and 75 ± 5% of DOC from surface water, with 12 ± 2% in the sodium hydroxide rinse. The highest recoveries of all were achieved by the sequential isolation of DOC, first with PPL and then via RO/ED. This combined technique recovered 98% of DOC from a deep water sample and 101% of DOC from a surface water sample. In total, 1.9, 10.3 and 1.6 g-C of DOC were collected via XAD, PPL and RO/ED, respectively. Rates of DOC recovery using the XAD, PPL and RO/ED methods were 10, 33 and 10 mg-C h− 1, respectively. Based upon C/N ratios, XAD isolates were heavily C-enriched compared with water column DOM, whereas RO/ED and PPL ➔ RO/ED isolate C/N values were most representative of the original DOM. All techniques are suitable for the isolation of large amounts of DOM with purities suitable for most advanced analytical techniques. Coupling PPL and RO/ED techniques may provide substantial progress in the search for a method to quantitatively isolate oceanic DOC, bringing the entirety of the DOM pool within the marine chemist's analytical window.

  10. Characterization of a high-affinity iron transport system in Acinetobacter baumannii.

    PubMed Central

    Echenique, J R; Arienti, H; Tolmasky, M E; Read, R R; Staneloni, R J; Crosa, J H; Actis, L A

    1992-01-01

    Analysis of a clinical isolate of Acinetobacter baumannii showed that this bacterium was able to grow under iron-limiting conditions, using chemically defined growth media containing different iron chelators such as human transferrin, ethylenediaminedi-(o-hydroxyphenyl)acetic acid, nitrilotriacetic acid, and 2,2'-bipyridyl. This iron uptake-proficient phenotype was due to the synthesis and secretion of a catechol-type siderophore compound. Utilization bioassays using the Salmonella typhimurium iron uptake mutants enb-1 and enb-7 proved that this siderophore is different from enterobactin. This catechol siderophore was partially purified from culture supernatants by adsorption chromatography using an XAD-7 resin. The purified component exhibited a chromatographic behavior and a UV-visible light absorption spectrum different from those of 2,3-dihydroxybenzoic acid and other bacterial catechol siderophores. Furthermore, the siderophore activity of this extracellular catechol was confirmed by its ability to stimulate energy-dependent uptake of 55Fe(III) as well as to promote the growth of A. baumannii bacterial cells under iron-deficient conditions imposed by 60 microM human transferrin. Polyacrylamide gel electrophoresis analysis showed the presence of iron-regulated proteins in both inner and outer membranes of this clinical isolate of A. baumannii. Some of these membrane proteins may be involved in the recognition and internalization of the iron-siderophore complexes. Images PMID:1447137

  11. Evaluation of Rapid, Early Warning Approaches to Track Shellfish Toxins Associated with Dinophysis and Alexandrium Blooms

    PubMed Central

    Hattenrath-Lehmann, Theresa K.; Lusty, Mark W.; Wallace, Ryan B.; Haynes, Bennie; Wang, Zhihong; Broadwater, Maggie; Deeds, Jonathan R.; Morton, Steve L.; Hastback, William; Porter, Leonora; Chytalo, Karen

    2018-01-01

    Marine biotoxin-contaminated seafood has caused thousands of poisonings worldwide this century. Given these threats, there is an increasing need for improved technologies that can be easily integrated into coastal monitoring programs. This study evaluates approaches for monitoring toxins associated with recurrent toxin-producing Alexandrium and Dinophysis blooms on Long Island, NY, USA, which cause paralytic and diarrhetic shellfish poisoning (PSP and DSP), respectively. Within contrasting locations, the dynamics of pelagic Alexandrium and Dinophysis cell densities, toxins in plankton, and toxins in deployed blue mussels (Mytilus edulis) were compared with passive solid-phase adsorption toxin tracking (SPATT) samplers filled with two types of resin, HP20 and XAD-2. Multiple species of wild shellfish were also collected during Dinophysis blooms and used to compare toxin content using two different extraction techniques (single dispersive and double exhaustive) and two different toxin analysis assays (liquid chromatography/mass spectrometry and the protein phosphatase inhibition assay (PP2A)) for the measurement of DSP toxins. DSP toxins measured in the HP20 resin were significantly correlated (R2 = 0.7–0.9, p < 0.001) with total DSP toxins in shellfish, but were detected more than three weeks prior to detection in deployed mussels. Both resins adsorbed measurable levels of PSP toxins, but neither quantitatively tracked Alexandrium cell densities, toxicity in plankton or toxins in shellfish. DSP extraction and toxin analysis methods did not differ significantly (p > 0.05), were highly correlated (R2 = 0.98–0.99; p < 0.001) and provided complete recovery of DSP toxins from standard reference materials. Blue mussels (Mytilus edulis) and ribbed mussels (Geukensia demissa) were found to accumulate DSP toxins above federal and international standards (160 ng g−1) during Dinophysis blooms while Eastern oysters (Crassostrea virginica) and soft shell clams (Mya arenaria) did not. This study demonstrated that SPATT samplers using HP20 resin coupled with PP2A technology could be used to provide early warning of DSP, but not PSP, events for shellfish management. PMID:29342840

  12. Continuous enzymatic hydrolysis of lignocellulosic biomass with simultaneous detoxification and enzyme recovery.

    PubMed

    Gurram, Raghu N; Menkhaus, Todd J

    2014-07-01

    Recovering hydrolysis enzymes and/or alternative enzyme addition strategies are two potential mechanisms for reducing the cost during the biochemical conversion of lignocellulosic materials into renewable biofuels and biochemicals. Here, we show that enzymatic hydrolysis of acid-pretreated pine wood with continuous and/or fed-batch enzyme addition improved sugar conversion efficiencies by over sixfold. In addition, specific activity of the hydrolysis enzymes (cellulases, hemicellulases, etc.) increased as a result of continuously washing the residual solids with removal of glucose (avoiding the end product inhibition) and other enzymatic inhibitory compounds (e.g., furfural, hydroxymethyl furfural, organic acids, and phenolics). As part of the continuous hydrolysis, anion exchange resin was tested for its dual application of simultaneous enzyme recovery and removal of potential enzymatic and fermentation inhibitors. Amberlite IRA-96 showed favorable adsorption profiles of inhibitors, especially furfural, hydroxymethyl furfural, and acetic acid with low affinity toward sugars. Affinity of hydrolysis enzymes to adsorb onto the resin allowed for up to 92 % of the enzymatic activity to be recovered using a relatively low-molar NaCl wash solution. Integration of an ion exchange column with enzyme recovery into the proposed fed-batch hydrolysis process can improve the overall biorefinery efficiency and can greatly reduce the production costs of lignocellulosic biorenewable products.

  13. Copper(II)-based metal affinity chromatography for the isolation of the anticancer agent bleomycin from Streptomyces verticillus culture.

    PubMed

    Gu, Jiesi; Codd, Rachel

    2012-10-01

    The glycopeptide-based bleomycins are structurally complex natural products produced by Streptomyces verticillus used in combination therapy against testicular and other cancers. Bleomycin has a high affinity towards a range of transition metal ions with the 1:1 Fe(II) complex relevant to its mechanism of action in vivo and the 1:1 Cu(II) complex relevant to its production from culture. The affinity between Cu(II) and bleomycin was the underlying principle for using Cu(II)-based metal affinity chromatography in this work to selectively capture bleomycin from crude S. verticillus culture. A solution of standard bleomycin was retained at a binding capacity of 300 nmol mL(-1) on a 1-mL bed volume of Cu(II)-loaded iminodiacetate (IDA) resin at pH 9 via the formation of the heteroleptic immobilized complex [Cu(IDA)(bleomycin)]. Bleomycin was eluted from the resin at pH 5 as the metal-free ligand under conditions where pK(a) (IDA)

  14. Effects of bovine milk lactoperoxidase system on some bacteria.

    PubMed

    Cankaya, M; Sişecioğlu, M; Bariş, O; Güllüce, M; Ozdemir, H

    2010-01-01

    Bovine lactoperoxidase (LPO) was purified from skimmed milk using amberlite CG-50-H+ resin, CM sephadex C-50 ion-exchange chromatography, and sephadex G-100 gel filtration chromatography. Lactoperoxidase was purified 20.45-fold with a yield of 28.8%. Purity of enzyme checked by sodium dodecyl sulphate-polyacrylamide gel electrophoresis method and a single band was observed. Km was 0.25 mM at 20 degrees C, Vmax value was 7.95 micromol/ml min at 20 degrees C (pH 6.0). Antibacterial study was done by disk diffusion method of Kir-by-Bauer using Mueller-Hinton agar medium with slight modification. Bovine LPO showed high antibacterial activity in 100 mM thiocyanate-100 mM H2O2 medium for some bacteria (Brevibacillus centrosaurus, B. choshinensis, B. lyticum, Cedecea davisae, Chryseobacterium indoltheticum, Clavibacter michiganense pv. insidiosum, Kocuria erythromyxa, K. kristinae, K. rosea, K. varians, Paenibacillus validus, Pseudomonas syringae pv. populans, Ralstonia pickettii, Rhodococcus wratislaviensis, Serratia fonticola, Streptomyces violaceusniger, Vibrio cholerae-nonO1) respectively, and compared with well known antibacterial substances (levofloxacin, netilmicin). LPO system has inhibition effects on all type bacteria and concentration is really important such as LPO-100 mM thiocyanate-100 mM H2O2 system was proposed as an effective agent against many factors causing several diseases.

  15. Evaluation of methods for simultaneous collection and determination of nicotine and polynuclear aromatic hydrocarbons in indoor air

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chuang, J.C.; Kuhlman, M.R.; Wilson, N.K.

    1990-01-01

    A study was performed to determine whether one sampling system and one analytical method can be used to measure both polynuclear aromatic hydrocarbons (PAH) and nicotine. The PAH collection efficiencies for both XAD-2 and XAD-4 adsorbents are very similar, but the nicotine collection efficiency was greater for XAD-4. The spiked perdeuterated PAH were retained well in both adsorbents after exposure to more than 300 cu m of air. A two-step Soxhlet extraction, dichloromethane followed by ethylacetate, was used to remove nicotine and PAH from XAD-4. The extract was analyzed by positive chemical ionization or electron impact gas chromatography/mass spectrometry (GC/MS)more » to determine nicotine and PAH. It is shown that one sampling system (quartz fiber filter and XAD-4 in series) and one analytical method (Soxhlet extraction and GC/MS) can be used to measure both nicotine and PAH in indoor air.« less

  16. Evaluation of methods for simultaneous collection and determination of nicotine and polynuclear aromatic hydrocarbons in indoor air

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chuang, J.C.; Kuhlman, M.R.; Wilson, N.K.

    1990-05-01

    A study was performed to determine whether one sampling system and one analytical method can be used to collect and measure both polynuclear aromatic hydrocarbons (PAHs) and nicotine. PAH collection efficiencies for both XAD-2 and XAD-4 adsorbents were very similar, but nicotine collection efficiency was greater for XAD-4. Spiked perdeuterated PAHs were retained well in both adsorbents after exposure to more than 300 m{sup 3} of air. A two-step Soxhlet extraction, dichloromethane followed by ethyl acetate, was used to remove nicotine and PAHs from XAD-4. The extract was analyzed by positive chemical ionization or electron impact gas chromatography/mass spectrometry (GC/MS)more » to determine nicotine and PAHs. It is shown that one sampling system (quartz fiber filter and XAD-4 in series) and one analytical method (Soxhlet extraction and GC/MS) can be used for both nicotine and PAHs in indoor.« less

  17. Emission of polycyclic aromatic hydrocarbons from diesel engine in a bus station, Londrina, Brazil

    NASA Astrophysics Data System (ADS)

    Tavares, Moacir; Pinto, Jurandir P.; Souza, Alexandre L.; Scarmínio, Ieda S.; Cristina Solci, Maria

    2004-09-01

    The concentrations of vapor phase polycyclic aromatic hydrocarbons (PAHs) were measured at the Central Bus Station of Londrina, where only diesel-powered vehicles circulate. The samples were collected within a period of 24 h for 14 consecutive days in January 2002. The semi-volatile PAHs were collected using a cartridge packed with XAD-2 resin, extracted under sonication and subsequently analyzed by gas chromatograph equipped with the flame ionization and mass spectrometer detectors (GC-FID and GC/MS). Ten PAH compounds were found (naphthalene, acenapthylene, acenapthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo(a)anthracene and chrysene). The average concentrations ranged from 1.4±0.3 ng m-3 for benzo(a)anthracene to 348.0±32.7 ng m-3 for phenanthrene. The species that presented higher concentration were phenanthrene (348.0±32.7 ng m-3), fluorene (140.2±17.3 ng m-3) and naphthalene (97.7±10.3 ng m-3). The PAHs with two and three rings were responsible by 90.2% of the total concentration among 10 PAHs. The concentrations of PAHs were lower on Sunday in comparison with the workdays, due to the reduction of bus traffic in the station. Correlations and principal component analysis with Varimax rotation were used to estimate the local PAH emission source profile originating from the diesel exhaust. The ratio PHEN/FLU of 2.5 calculated from the results is suggested as indication from diesel combustion exhaust.

  18. Camptothecin-producing endophytic fungus Trichoderma atroviride LY357: isolation, identification, and fermentation conditions optimization for camptothecin production.

    PubMed

    Pu, Xiang; Qu, Xixing; Chen, Fei; Bao, Jinku; Zhang, Guolin; Luo, Yinggang

    2013-11-01

    Camptothecin (CPT), the third largest anticancer drug, is produced mainly by Camptotheca acuminata and Nothapodytes foetida. CPT itself is the starting material for clinical CPT-type drugs, but the plant-derived CPT cannot support the heavy demand from the global market. Research efforts have been made to identify novel sources for CPT. In this study, three CPT-producing endophytic fungi, Aspergillus sp. LY341, Aspergillus sp. LY355, and Trichoderma atroviride LY357, were isolated and identified from C. acuminata. Most CPT produced by these fungi was found in the fermentation broth, and their corresponding CPT yields were 7.93, 42.92, and 197.82 μg l(-1), respectively. The CPT-producing capability of LY341 and LY355 was completely lost after repeat subculturing. A substantial decrease of CPT production was also observed in the second generation of LY357. However, a stable and sustainable production of CPT was found from the second generation through the eighth generation of LY357. The fermentation medium, time, pH, temperature, and agitation rate were optimized for CPT production. Methyl jasmonate and XAD16 were proven to be an optimum elicitor and adsorbent resin, respectively, in view of that CPT yield was increased 3.4- and 11-fold through their use. A 50- to 75-fold increase of CPT yield was obtained when the optimized fermentation conditions, elicitor, and adsorbent resin were combined and applied to the culture of the seventh and eighth generations of LY357, and the highest CPT yield was 142.15 μg l(-1). The CPT-producing T. atroviride LY357 paves a potential to uncover the mysteries of CPT biosynthesis.

  19. A sensitive LC-MS/MS method for measurement of organophosphorus pesticides and their oxygen analogs in air sampling matrices

    PubMed Central

    ARMSTRONG, JENNA L.; DILLS, RUSSELL L.; YU, JIANBO; YOST, MICHAEL G.; FENSKE, RICHARD A.

    2018-01-01

    A rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed for determination of levels of the organophosphorus (OP) pesticides chlorpyrifos (CPF), azinphos methyl (AZM), and their oxygen analogs chlorpyrifos-oxon (CPF-O) and azinphos methyl-oxon (AZM-O) on common active air sampling matrices. XAD-2 resin and polyurethane foam (PUF) matrices were extracted with acetonitrile containing stable-isotope labeled internal standards (ISTD). Analysis was accomplished in Multiple Reaction Monitoring (MRM) mode, and analytes in unknown samples were identified by retention time (±0.1 min) and qualifier ratio (±30% absolute) as compared to the mean of calibrants. For all compounds, calibration linearity correlation coefficients were ≥0.996. Limits of detection (LOD) ranged from 0.15–1.1 ng/sample for CPF, CPF-O, AZM, and AZM-O on active sampling matrices. Spiked fortification recoveries were 78–113% from XAD-2 active air sampling tubes and 71–108% from PUF active air sampling tubes. Storage stability tests also yielded recoveries ranging from 74–94% after time periods ranging from 2–10 months. The results demonstrate that LC-MS/MS is a sensitive method for determining these compounds from two different matrices at the low concentrations that can result from spray drift and long range transport in non-target areas following agricultural applications. In an inter-laboratory comparison, the limit of quantification (LOQ) for LC-MS/MS was 100 times lower than a typical gas chromatography-mass spectrometry (GC-MS) method. PMID:24328542

  20. A sensitive LC-MS/MS method for measurement of organophosphorus pesticides and their oxygen analogs in air sampling matrices.

    PubMed

    Armstrong, Jenna L; Dills, Russell L; Yu, Jianbo; Yost, Michael G; Fenske, Richard A

    2014-01-01

    A rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed for determination of levels of the organophosphorus (OP) pesticides chlorpyrifos (CPF), azinphos methyl (AZM), and their oxygen analogs chlorpyrifos-oxon (CPF-O) and azinphos methyl-oxon (AZM-O) on common active air sampling matrices. XAD-2 resin and polyurethane foam (PUF) matrices were extracted with acetonitrile containing stable-isotope labeled internal standards (ISTD). Analysis was accomplished in Multiple Reaction Monitoring (MRM) mode, and analytes in unknown samples were identified by retention time (±0.1 min) and qualifier ratio (±30% absolute) as compared to the mean of calibrants. For all compounds, calibration linearity correlation coefficients were ≥0.996. Limits of detection (LOD) ranged from 0.15-1.1 ng/sample for CPF, CPF-O, AZM, and AZM-O on active sampling matrices. Spiked fortification recoveries were 78-113% from XAD-2 active air sampling tubes and 71-108% from PUF active air sampling tubes. Storage stability tests also yielded recoveries ranging from 74-94% after time periods ranging from 2-10 months. The results demonstrate that LC-MS/MS is a sensitive method for determining these compounds from two different matrices at the low concentrations that can result from spray drift and long range transport in non-target areas following agricultural applications. In an inter-laboratory comparison, the limit of quantification (LOQ) for LC-MS/MS was 100 times lower than a typical gas chromatography-mass spectrometry (GC-MS) method.

  1. Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS).

    PubMed

    Ciftci, Harun; Er, Cigdem

    2013-03-01

    In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L(-1) HNO(3) and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L(-1) and 3.91 μg L(-1), respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.

  2. High Pressure Size Exclusion Chromatography (HPSEC) Determination of Dissolved Organic Matter Molecular Weight Revisited: Accounting for Changes in Stationary Phases, Analytical Standards, and Isolation Methods.

    PubMed

    McAdams, Brandon C; Aiken, George R; McKnight, Diane M; Arnold, William A; Chin, Yu-Ping

    2018-01-16

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA 280 ) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA 280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA 280 .

  3. Removal of acutely hazardous pharmaceuticals from water using multi-template imprinted polymer adsorbent.

    PubMed

    Venkatesh, Avinash; Chopra, Nikita; Krupadam, Reddithota J

    2014-05-01

    Molecularly imprinted polymer adsorbent has been prepared to remove a group of recalcitrant and acutely hazardous (p-type) chemicals from water and wastewaters. The polymer adsorbent exhibited twofold higher adsorption capacity than the commercially used polystyrene divinylbenzene resin (XAD) and powdered activated carbon adsorbents. Higher adsorption capacity of the polymer adsorbent was explained on the basis of high specific surface area formed during molecular imprinting process. Freundlich isotherms drawn showed that the adsorption of p-type chemicals onto polymer adsorbent was kinetically faster than the other reference adsorbents. Matrix effect on adsorption of p-type chemicals was minimal, and also polymer adsorbent was amenable to regeneration by washing with water/methanol (3:1, v/v) solution. The polymer adsorbent was unaltered in its adsorption capacity up to 10 cycles of adsorption and desorption, which will be more desirable in cost reduction of treatment compared with single-time-use activated carbon.

  4. Toxic organic pollutants from kerosene space heaters in Iran.

    PubMed

    Keyanpour-Rad, Mansoor

    2004-03-01

    The aim of this study was to investigate qualitatively the emission of toxic organic pollutants from an unventilated conventional kerosene space heater commonly used in Iran. A brand new common convective kerosene space heater, the "Aladdin," was used for this study. The well-tuned convective heater was operated in a 2.6-m(3) test chamber and then the emission was tested for organic pollutants. The emission was collected on Teflon-impregnated glass-fiber filters and XAD-2 resin and then analyzed by gas chromatography-mass spectroscopy. It was found that in addition to the ordinary pollutant gases, the heater emits aliphatic hydrocarbons, alcohols, polyaromatic hydrocarbons and the related nitrated compounds, phthalates, naphthalenes, and some other toxic organic compounds. However, it was found that the heater did not emit fluoranthene, cyclohexane, benzoic acid, and higher-molecular-weight alkylbenzenes, which could have resulted from the combustion of some other types of kerosene.

  5. Validity of using semipermeable membrane devices for determining aqueous concentrations of freely dissolved PAHs

    USGS Publications Warehouse

    Prest, Harry; Petty, J.D.; Huckins, J.N.

    1998-01-01

    An in-depth review of the recent contribution to this journal by Gustafson and Dickhut [1] prompts us to share our concerns regarding some of their conclusions. The paper presents data comparing three techniques for determining aqueous concentrations of freely dissolved polycyclic aromatic hydrocarbons (PAHs) gas sparging, lipid-containing semipermeable membrane devices (SPMDs) of the U.S. Geological Survey (USGS) design, and filtration followed by sorption using XAD-2 resin. Space limitations force us to limit our comments to problems resulting from an apparent lack of understanding of how SPMDs function. Several recent publications [2–13] have described the theoretical and practical considerations of SPMD usage. Gustafson and Dickhut fail to cite any papers describing SPMDs published after 1992, even though some 18 papers have been published in American and European journals since then and several SPMD studies have been presented at many major meetings.

  6. Effectiveness of high-throughput miniaturized sorbent- and solid phase microextraction techniques combined with gas chromatography-mass spectrometry analysis for a rapid screening of volatile and semi-volatile composition of wines--a comparative study.

    PubMed

    Mendes, Berta; Gonçalves, João; Câmara, José S

    2012-01-15

    In this study the feasibility of different extraction procedures was evaluated in order to test their potential for the extraction of the volatile (VOCs) and semi-volatile constituents (SVOCs) from wines. In this sense, and before they could be analysed by gas chromatography-quadrupole first stage masss spectrometry (GC-qMS), three different high-throughput miniaturized (ad)sorptive extraction techniques, based on solid phase extraction (SPE), microextraction by packed sorbents (MEPS) and solid phase microextraction (SPME), were studied for the first time together, for the extraction step. To achieve the most complete volatile and semi-volatile signature, distinct SPE (LiChrolut EN, Poropak Q, Styrene-Divinylbenzene and Amberlite XAD-2) and MEPS (C(2), C(8), C(18), Silica and M1 (mixed C(8)-SCX)) sorbent materials, and different SPME fibre coatings (PA, PDMS, PEG, DVB/CAR/PDMS, PDMS/DVB, and CAR/PDMS), were tested and compared. All the extraction techniques were followed by GC-qMS analysis, which allowed the identification of up to 103 VOCs and SVOCs, distributed by distinct chemical families: higher alcohols, esters, fatty acids, carbonyl compounds and furan compounds. Mass spectra, standard compounds and retention index were used for identification purposes. SPE technique, using LiChrolut EN as sorbent (SPE(LiChrolut EN)), was the most efficient method allowing for the identification of 78 VOCs and SVOCs, 63 and 19 more than MEPS and SPME techniques, respectively. In MEPS technique the best results in terms of number of extractable/identified compounds and total peak areas of volatile and semi-volatile fraction, were obtained by using C(8) resin whereas DVB/CAR/PDMS was revealed the most efficient SPME coating to extract VOCs and SVOCs from Bual wine. Diethyl malate (18.8±3.2%) was the main component found in wine SPE(LiChrolut EN) extracts followed by ethyl succinate (13.5±5.3%), 3-methyl-1-butanol (13.2±1.7%), and 2-phenylethanol (11.2±9.9%), while in SPME(DVB/CAR/PDMS) technique 3-methyl-1-butanol (43.3±0.6%) followed by diethyl succinate (18.9±1.6%), and 2-furfural (10.4±0.4%), are the major compounds. The major VOCs and SVOCs isolated by MEPS(C8) were 3-methyl-1-butanol (26.8±0.6%, from wine total volatile fraction), diethyl succinate (24.9±0.8%), and diethyl malate (16.3±0.9%). Regardless of the extraction technique, the highest extraction efficiency corresponds to esters and higher alcohols and the lowest to fatty acids. Despite some drawbacks associated with the SPE procedure such as the use of organic solvents, the time-consuming and tedious sampling procedure, it was observed that SPE(LiChrolut EN), revealed to be the most effective technique allowing the extraction of a higher number of compounds (78) rather than the other extraction techniques studied. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. The ambient organic aerosol soluble in water: Measurements, chemical characterization, and an investigation of sources

    NASA Astrophysics Data System (ADS)

    Sullivan, Amy P.

    This thesis characterizes the ambient fine organic carbon (OC) aerosol and investigates its sources through the development and deployment of new analytical measurement techniques. Recognizing that OC is highly chemically complex, the approach was to develop methods capable of quantitatively measuring a large chemical fraction of the aerosol instead of specific chemical speciation. The focus is on organic compounds that are soluble in water (WSOC) since little is known about its chemical nature. The results from this thesis show that WSOC has mainly two sources: biomass burning and secondary organic aerosol (SOA). In urban areas, WSOC increases with plume age, and tracks other photochemically produced compounds. Chemical analysis of WSOC suggests that in urban Atlanta, the SOA is mainly small-chain aliphatic compounds indirectly linked to vehicle emissions. A method was first developed for quantitative on-line measurements of WSOC by extending the application of the Particle-into-Liquid Sampler (PILS) from inorganic to organic aerosol measurements. In this approach a PILS captures ambient particles into a flow of purified water, which is then forced through a liquid filter and the carbonaceous content quantified on-line by a Total Organic Carbon (TOC) analyzer. An instrument was first developed for ground-based measurements and then modified for airborne deployment. Ground-based measurements at the St. Louis - Midwest Supersite during the summer of 2003 showed that the fraction of OC that is water-soluble can have a highly diurnal pattern with WSOC to OC ratios reaching 0.80 during the day and lows of 0.40 during the night. During extended periods under stagnation pollution events, this pattern was well correlated with ozone concentrations. The results are consistent with formation of SOA. Airborne PILS-TOC measurements from the NOAA WP-3D during the New England Air Quality Study/Intercontinental Transport and Chemical Transformation (NEAQS/ITCT) 2004 program investigated WSOC sources over the northeastern U.S. and Canada. Two main sources were identified: biomass burning emissions from fires in the Alaska/Yukon region and emissions emanating from urban centers. Biomass burning WSOC was correlated with carbon monoxide (CO) and acetonitrile (R 2 > 0.88). Apart from the biomass burning influence, the highest concentrations were at low altitudes in distinct plumes of enhanced particle concentrations from urban centers. WSOC and CO were highly correlated (R2 > 0.78) in these urban plumes. The ratio of the enhancement in WSOC relative to that of CO was found to be low (˜ 3 microg C/m3/ppmv) in plumes that had been in transit for a short time, and increased with plume age, but appeared to level off at ˜32 microg C/m3/ppmv after approximately one day of transport from the sources. The results suggest WSOC in fine particles is produced from compounds co-emitted with CO and that these emissions are rapidly converted to organic particulate matter within ˜1 day following emission. To further chemically investigate the organic constituents of WSOC, a method for group speciation of the WSOC into hydrophilic and hydrophobic fractions has been developed using a XAD-8 resin column. XAD-8 resin coupled with a TOC analyzer allows for direct quantification. Based on laboratory calibrations with atmospherically relevant standards and 13C-NMR ( 13Carbon-Nuclear Magnetic Resonance) analysis, the hydrophilic fraction (compounds that penetrate the XAD-8 with near 100% efficiency at pH 2) is composed of short-chain carboxylic acids and carbonyls and saccharides. The fraction of WSOC retained by XAD-8, termed the hydrophobic fraction, includes aromatic acids, phenols, organic nitrates, cyclic acids, and carbonyls and mono-/dicarboxylic acids with greater than 3 or 4 carbons. Only aromatic compounds (or aromatic-like compounds with similar properties) can subsequently be extracted from XAD-8 with high efficiency and are referred to as the recovered hydrophobic fraction. By coupling a PILS with this technique, on-line measurements of WSOC, hydrophilic WSOC, and hydrophobic WSOC are possible. Urban measurements from St. Louis and Atlanta, on a carbon mass basis, show an increase in the mean WSOC fraction from winter (51%) to summer (61%), due to increases in the hydrophilic WSOC to OC ratio from 0.25 to 0.35. During a summer Atlanta PM event, WSOC to OC was 0.75, driven largely by increases in the hydrophilic WSOC fraction. The results are consistent with the view that in the summer there are increased amounts of oxygenated polar compounds, that are mainly hydrophilic and possibly from SOA production. These compounds can account for an even larger fraction of OC during stagnation events. The XAD-8 resin can also be used in the first step of a two-step off-line method to isolate chemical fractions of ambient organic aerosol based on acid, neutral, and basic functional groups. The second step is a newly developed method involving size-exclusion chromatography (SEC) to separate the hydrophilic WSOC and recovered hydrophobic WSOC compounds by organic functional group. Calibrations show that hydrophilic WSOC separates into short-chain aliphatic acids, neutrals (e.g. saccharides, polyols, and short-chain carbonyls), and organic bases. The recovered hydrophobic compounds are separated into acids (e.g., aromatic) and neutrals (e.g., phenols). Comparisons are made between XAD-8/SEC results from urban Atlanta summer and winter, and biomass burning samples. During the summer in Atlanta, approximately 20% of the OC (on a carbon mass basis) is due to hydrophilic aliphatic acids and recovered hydrophobic acids. The hydrophilic aliphatic acids are additionally the largest isolated fraction of Atlanta summer WSOC (29% microg C/microg C), suggesting aliphatic acids of less than C4 or C5 are the dominant SOA product, and are also correlated with the recovered hydrophobic acids (R2 = 0.74), elemental carbon (R2 = 0.64), CO (R2 = 0.73), and VOCs (Volatile Organic Compounds) expected from mobile source emissions such as isopentane (R2 = 0.67) and acetylene (R2 = 0.61). Biomass burning samples, however, were dominated by the hydrophilic and recovered hydrophobic neutral compounds. In the winter, when the WSOC is much lower, the samples tended to be a combination of the other two sample types. Combining the results of these various WSOC measurements over Atlanta and its surrounding regions, the data indicate that the source of WSOC is indirectly linked to vehicle emissions. Aircraft measurements show that WSOC is correlated with CO over large regions, and that the ratio of the metropolitan Atlanta DeltaWSOC/DeltaCO is similar to that in urban plumes in the northeastern U.S. Over a wide geographical region (˜100 km) WSOC is comprised of three major chemical groups (> 70%) that increase in concentration under more polluted conditions, and appear to be linked to a similar source. The fraction of the organic aerosol that is water-soluble varies between roughly 0.40 and 0.75 depending on the location, with higher ratios in regions further from mobile source emissions.

  8. Comparison of XAD with other dissolved lignin isolation techniques and a compilation of analytical improvements for the analysis of lignin in aquatic settings

    USGS Publications Warehouse

    Spencer, Robert G. M.; Aiken, George R.; Dyda, Rachael Y.; Butler, Kenna D.; Bergamaschi, Brian; Hernes, Peter J.

    2010-01-01

    This manuscript highlights numerous incremental improvements in dissolved lignin measurements over the nearly three decades since CuO oxidation of lignin phenols was first adapted for environmental samples. Intercomparison of the recovery efficiency of three common lignin phenol concentration and isolation techniques, namely XAD, C18with both CH3OH (C18M) and CH3CN (C18A) used independently for priming and elution steps, and tangential flow filtration (TFF) for a range of aquatic samples including fresh, estuarine and marine waters, was undertaken. With freshwater samples XAD8-1, C18M and TFF were all observed to recover ca. 80–90% of the lignin phenols and showed no fractionation effects with respect to diagnostic lignin parameters. With estuarine and marine samples more lignin phenols were recovered with C18M and XAD8-1 than TFF because of the increased prevalence of low molecular weight lignin phenols in marine influenced samples. For marine systems, differences were also observed between diagnostic lignin parameters isolated via TFF vs. C18M and XAD8-1 as a result of the high molecular weight lignin phenols being less degraded than the bulk. Therefore, it is recommended for future studies of marine systems that only one technique is utilized for ease of intercomparison within studies. It is suggested that for studies solely aimed at recovering bulk dissolved lignin in marine environments that C18M and XAD8-1 appear to be more suitable than TFF as they recover more lignin. Our results highlight that, for freshwater samples, all three common lignin phenol concentration and isolation techniques are comparable to whole water concentrated by rotary evaporation (i.e. not isolated) but, that for marine systems, the choice of concentration and isolation techniques needs to be taken into consideration with respect to both lignin concentration and diagnostic parameters. Finally, as the study highlights XAD8-1 to be a suitable method for the isolation of dissolved lignin phenols from aquatic systems (statistically indistinguishable from C18M, P < 0.1), lignin data representative of whole waters can be produced for IHSS reference materials or other XAD sample archives.

  9. Comparison of XAD with other dissolved lignin isolation techniques and a compilation of analytical improvements for the analysis of lignin in aquatic settings

    USGS Publications Warehouse

    Spencer, R.G.M.; Aiken, G.R.; Dyda, R.Y.; Butler, K.D.; Bergamaschi, B.A.; Hernes, P.J.

    2010-01-01

    This manuscript highlights numerous incremental improvements in dissolved lignin measurements over the nearly three decades since CuO oxidation of lignin phenols was first adapted for environmental samples. Intercomparison of the recovery efficiency of three common lignin phenol concentration and isolation techniques, namely XAD, C18 with both CH3OH (C18M) and CH3CN (C18A) used independently for priming and elution steps, and tangential flow filtration (TFF) for a range of aquatic samples including fresh, estuarine and marine waters, was undertaken. With freshwater samples XAD8-1, C18M and TFF were all observed to recover ca. 80-90% of the lignin phenols and showed no fractionation effects with respect to diagnostic lignin parameters. With estuarine and marine samples more lignin phenols were recovered with C18M and XAD8-1 than TFF because of the increased prevalence of low molecular weight lignin phenols in marine influenced samples. For marine systems, differences were also observed between diagnostic lignin parameters isolated via TFF vs. C18M and XAD8-1 as a result of the high molecular weight lignin phenols being less degraded than the bulk. Therefore, it is recommended for future studies of marine systems that only one technique is utilized for ease of intercomparison within studies. It is suggested that for studies solely aimed at recovering bulk dissolved lignin in marine environments that C18M and XAD8-1 appear to be more suitable than TFF as they recover more lignin. Our results highlight that, for freshwater samples, all three common lignin phenol concentration and isolation techniques are comparable to whole water concentrated by rotary evaporation (i.e. not isolated) but, that for marine systems, the choice of concentration and isolation techniques needs to be taken into consideration with respect to both lignin concentration and diagnostic parameters. Finally, as the study highlights XAD8-1 to be a suitable method for the isolation of dissolved lignin phenols from aquatic systems (statistically indistinguishable from C18M, P < 0.1), lignin data representative of whole waters can be produced for IHSS reference materials or other XAD sample archives. ?? 2010 Elsevier Ltd.

  10. Analysis of Absorption Spectra of Polycyclic Aromatic Hydrocarbons in Gaseous- and Particle- Phase Emissions from Peat Fuel Combustion Under Controlled Conditions

    NASA Astrophysics Data System (ADS)

    Connolly, J. I.; Samburova, V.; Moosmüller, H.; Khlystov, A.

    2015-12-01

    Biomass and fossil fuel burning processes emit important organic pollutants called polycyclic aromatic hydrocarbons (PAHs) into the atmosphere. Smoldering combustion of peat is one of the largest contributors (up to 70%) of carbonaceous species and, therefore, it may be one of the main sources of these PAHs. PAHs can be detrimental to health, they are known to be potent mutagens and suspected carcinogens. They may also contribute to solar light absorption as the particles absorb in the blue and near ultraviolet (UV) region of the solar spectrum ("brown carbon" species). There is very little knowledge and large ambiguity regarding the contribution of PAHs to optical properties of organic carbon (OC) emitted from smoldering biomass combustion. This study focuses on quantifying and analyzing PAHs emitted from peat smoldering combustion to gain more knowledge on their optical properties. Five peat fuels collected in different regions of the world (Russia, USA) were burned under controlled conditions (e.g., relative humidity, combustion efficiency, fuel-moisture content) at the Desert Research Institute Biomass Burning facility (Reno, NV, USA). Combustion aerosols collected on TIGF filters followed by XAD resin cartridges were extracted and analyzed for gas-phase (semi-volatile) and particle-phase PAHs. Filter and XAD samples were extracted separately with dichloromethane followed by acetone using Accelerated Solvent Extractor (ACE 300, Dionex). To determine absorption properties, absorption spectra of extracts and standard PAHs were recorded between 190 and 900 nm with a UV/VIS spectrophotometer (PerkinElmer, Lambda 650). This poster will discuss the potential contribution of PAHs to brown carbon emitted from peat combustion and give a brief comparison with absorption spectra from biomass burning aerosols.

  11. Removal of non-biodegradable organic matter from landfill leachates by adsorption.

    PubMed

    Rodríguez, J; Castrillón, L; Marañón, E; Sastre, H; Fernández, E

    2004-01-01

    Leachates produced at the La Zoreda landfill in Asturias, Spain, were recirculated through a simulated landfill pilot plant. Prior to recirculation, three loads of different amounts of Municipal Solid Waste (MSW) were added to the plant, forming in this way consecutive layers. When anaerobic digestion was almost completed, the leachates from the landfill were recirculated. After recirculation, a new load of MSW was added and two new recirculations were carried out. The organic load of the three landfill leachates recirculated through the anaerobic pilot plant decreased from initial values of 5108, 3782 and 2560 mg/l to values of between 1500 and 1600 mg/l. Despite achieving reductions in the organic load of the leachate, a residual organic load still remained that was composed of non-biodegradable organic constituents such as humic substances. Similar values of the chemical oxygen demand (COD) were obtained when the landfill leachate was treated by a pressurised anoxic-aerobic process followed by ultrafiltration. After recirculation through the pilot plant, physico-chemical treatment was carried out to reduce the COD of the leachate. The pH of the leachate was decreased to a value of 1.5 to precipitate the humic fraction, obtaining a reduction in COD of about 13.5%. The supernatant liquid was treated with activated carbon and different resins, XAD-8, XAD-4 and IR-120. Activated carbon presented the highest adsorption capacities, obtaining COD values for the treated leachate in the order of 200mg/l. Similar results were obtained when treating with activated carbon, the leachate from the biological treatment plant at the La Zoreda landfill; in this case without decreasing the pH.

  12. Recovery of polyphenols from rose oil distillation wastewater using adsorption resins--a pilot study.

    PubMed

    Rusanov, Krasimir; Garo, Eliane; Rusanova, Mila; Fertig, Orlando; Hamburger, Matthias; Atanassov, Ivan; Butterweck, Veronika

    2014-11-01

    The production of rose oil from rose flowers by water steam distillation leaves a water fraction of the distillate as main part of the waste. Therefore, the rose oil distillation wastewater represents a serious environmental problem due to the high content of polyphenols which are difficult to decompose and have to be considered as biopollutants when discarded into the drainage system and rivers. On the other hand, natural polyphenols are valuable compounds with useful properties as bioactive substances. Until now there is no established practice for processing of rose oil distillation wastewater and utilization of contained substances. Thus, it was the aim of this study to develop a strategy to separate this wastewater into a polyphenol depleted water fraction and a polyphenol enriched fraction which could be developed into innovative value-added products. In a first step, the phytochemical profile of rose oil distillation wastewater was determined. Its HPLC-PDA-MS analysis revealed the presence of flavan-3-ols, flavanones, flavonols and flavones. In a second step, the development of a stepwise concentration of rose oil distillation wastewater was performed. The concentration process includes a filtration process to eliminate suspended solids in the wastewater, followed by adsorption of the contained phenolic compounds onto adsorption resins (XAD and SP). Finally, desorption of the polyphenol fraction from the resin matrix was achieved using ethanol and/or aqueous ethanol. The result of the process was a wastewater low in soluble organic compounds and an enriched polyphenol fraction (RF20 SP-207). The profile of this fraction was similar to that of rose oil distillation wastewater and showed the presence of flavonols such as quercetin and kaempferol glycosides as major metabolites. These compounds were isolated from the enriched polyphenol fraction and their structures confirmed by NMR. In summary, a pilot medium scale system was developed using adsorption resins for the recovery of polyphenols from rose oil distillation wastewater suggesting an industrial scalability of the process. Georg Thieme Verlag KG Stuttgart · New York.

  13. Detection of potential genetic hazards in complex environmental mixtures using plant cytogenetics and microbial mutagenesis assays. [Arsenic-contaminated groundwater and power plant fly ash extract

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Constantin, M J; Lowe, K; Rao, T K

    1980-01-01

    Solid wastes have been characterized to determine their potential hazards to humans and the environment. An arsenic-contaminated ground water sample increased the frequency of histidine revertants in Salmonella typhimurium (TA-98) at 0.025 to 5.000 ..mu..l per plate with Aroclor-induced S-9 liver microsomes. When 2.5 to 75 ..mu..l of the XAD-2 concentrate (12.5-fold, v:v) were used, the mutant frequency was increased in strains TA-98, TA-100, and TA-1537; metabolic activation was not required. Only the XAD-2 concentrate was mutagenic in the Saccharomyces cerevisiae haploid strain XL-7-10B; metabolic activation was not required. The mutagenic principal, which is not known, appears to be atmore » the limit of resolution; hence, the XAD-2 concentration is necessary to demonstrate mutagenic activity. The arsenic-contaminated ground water (0.0625 and 0.125 dilutions) and the power plant fly ash extract (undiluted) increased the frequency of bridges and fragements at anaphase in root tip cells of Hordeum. The fly ash sample was negative in the microbial assays. Results emphasize (1) the need for a battery of assays with different organisms and (2) the potential of a simple assay using plant root tip cells to detect mutagenic activity in complex environmental mixtures.« less

  14. Extraction of inhibitor-free metagenomic DNA from polluted sediments, compatible with molecular diversity analysis using adsorption and ion-exchange treatments.

    PubMed

    Desai, Chirayu; Madamwar, Datta

    2007-03-01

    PCR inhibitor-free metagenomic DNA of high quality and high yield was extracted from highly polluted sediments using a simple remediation strategy of adsorption and ion-exchange chromatography. Extraction procedure was optimized with series of steps, which involved gentle mechanical lysis, treatment with powdered activated charcoal (PAC) and ion-exchange chromatography with amberlite resin. Quality of the extracted DNA for molecular diversity analysis was tested by amplifying bacterial 16S rDNA (16S rRNA gene) with eubacterial specific universal primers (8f and 1492r), cloning of the amplified 16S rDNA and ARDRA (amplified rDNA restriction analysis) of the 16S rDNA clones. The presence of discrete differences in ARDRA banding profiles provided evidence for expediency of the DNA extraction protocol in molecular diversity studies. A comparison of the optimized protocol with commercial Ultraclean Soil DNA isolation kit suggested that method described in this report would be more efficient in removing metallic and organic inhibitors, from polluted sediment samples.

  15. High pressure size exclusion chromatography (HPSEC) determination of dissolved organic matter molecular weight revisited: Accounting for changes in stationary phases, analytical standards, and isolation methods

    USGS Publications Warehouse

    McAdams, Brandon C.; Aiken, George R.; McKnight, Diane M.; Arnold, William A.; Chin, Yu-Ping

    2018-01-01

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA280) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA280.

  16. Determination of phenolic priority pollutants utilizing permeation sampling method

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Zhang, Guozheng.

    1990-01-01

    A passive permeation sampling method for the determination of phenolic priority pollutants in water was developed. Phenols in an aqueous solution permeate a polymeric membrane and are collected on a solid adsorbent in a sampling device. Both solvent and thermal desorption techniques were employed to recovery phenolic pollutants collected. In the solvent desorption, phenolic compounds collected on the XAD-7 resin, and then desorbed by acetonitrile. In the thermal desorption, phenolic compounds collected on Tenax-TA were recovered thermally, Separation and quantification is achieved by a SPB-5 capillary column gas chromatography using a flame ionization detector. There are linear relationships between themore » amount of phenolic compounds collected and the products of the exposure times and concentrations over the range from 5 ppb to 20 ppm with precisions no worse than 13%. The permeation rates of the phenolic pollutants depend upon the exposure temperature, solution pH and membrane area. Samples collected can be stored for up to two weeks without loss. This method provides a simple, convenient and inexpensive way for monitoring the time-weighted-average concentration without the use of a pumping system. An automated sampler which combines the permeation and the thermal desorption techniques together was also developed for water sample obtained from grab sampling. The on-line setup provides a high degree of automation. Detection limits at 10 ppb can be achieved using this sampler.« less

  17. Evaluation of nonionic adsorbent resins for removal of inhibitory compounds from corncob hydrolysate for ethanol fermentation.

    PubMed

    Hatano, Ken-ichi; Aoyagi, Naokazu; Miyakawa, Takuya; Tanokura, Masaru; Kubota, Kenji

    2013-12-01

    The aim of this study was to investigate the effect of XAD4-column treatment on removal of several fermentation inhibitors from corncob hydrolysate (CH). From analysis using a model hydrolysate, more than 99% of 5-hydroxy-methyl furfural, furfural and vanillin were removed by this treatment, and more than 97% of the total xylose, glucose and arabinose remained in the detoxified CH (DCH). The resulting DCH was tested as a substrate for ethanol production by Saccharomyces cerevisiae and Pichia stipitis. The highest ethanol levels for S. cerevisiae were 1.40 and 4.92 g l(-1) in CH and DCH, respectively. For P. stipitis, the levels were 0 and 4.73 g l(-1) in the CH and DCH media, respectively. The levels of alcohol volumetric productivity in the DCH medium were 0.374 and 0.200 g l(-1)h(-1) for S. cerevisiae and P. stipitis, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Polycyclic aromatic hydrocarbons in surface soil across the Tibetan Plateau: spatial distribution, source and air-soil exchange.

    PubMed

    Wang, Chuanfei; Wang, Xiaoping; Gong, Ping; Yao, Tandong

    2014-01-01

    There are limited data on polycyclic aromatic hydrocarbons (PAHs) in both the atmosphere and soil of the Tibetan Plateau (TP). Concentrations of PAHs were therefore measured in 13 XAD resin-based passive air samplers and 41 surface (0-5 cm) soil samples across the TP. The average concentration of atmospheric PAHs was 5.55 ng/m(3), which was lower than that reported for other background areas, but higher than the Arctic. Concentrations in the soils fell in a wide range from 5.54 to 389 ng/g, with an average of 59.9 ng/g. Elevation was found to play an important role in determining the spatial distribution of soil PAHs. The air-soil exchange state showed that the soils of the TP will likely remain as a sink for high molecular weight PAHs, but may become a potential "secondary source" for low molecular weight PAHs. Copyright © 2013 Elsevier Ltd. All rights reserved.

  19. Carbonyl atmospheric reaction products of aromatic hydrocarbons in ambient air

    NASA Astrophysics Data System (ADS)

    Obermeyer, Genevieve; Aschmann, Sara M.; Atkinson, Roger; Arey, Janet

    To convert gaseous carbonyls to oximes during sampling, an XAD-4 resin denuder system pre-coated with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine and followed by analysis with methane positive chemical ionization gas chromatography/mass spectrometry was used to measure carbonyls in ambient air samples in Riverside, CA. In conjunction with similar analyses of environmental chamber OH radical-initiated reactions of o- and p-xylene, 1,2,4-trimethylbenzene, ethylbenzene, 4-hydroxy-2-butanone and 1,4-butanediol, we identified benzaldehyde, o-, m- and p-tolualdehyde and acetophenone and the dicarbonyls glyoxal, methylglyoxal, biacetyl, ethylglyoxal, 1,4-butenedial, 3-hexene-2,5-dione, 3-oxo-butanal, 1,4-butanedial and malonaldehyde in the ambient air samples. As discussed, these carbonyls and dicarbonyls can be formed from the OH radical-initiated reactions of aromatic hydrocarbons and other volatile organic compounds emitted into the atmosphere, and we conclude that in situ atmospheric formation is a major source of these carbonyls in our Riverside, CA, ambient air samples.

  20. Glycosidically bound flavor compounds of cape gooseberry (Physalis peruviana L.).

    PubMed

    Mayorga, H; Knapp, H; Winterhalter, P; Duque, C

    2001-04-01

    The bound volatile fraction of cape gooseberry (Physalis peruviana L.) fruit harvested in Colombia has been examined by HRGC and HRGC-MS after enzymatic hydrolysis using a nonselective pectinase (Rohapect D5L). Forty bound volatiles could be identified, with 21 of them being reported for the first time in cape gooseberry. After preparative isolation of the glycosidic precursors on XAD-2 resin, purification by multilayer coil countercurrent chromatography and HPLC of the peracetylated glycosides were carried out. Structure elucidation by NMR, ESI-MS/MS, and optical rotation enabled the identification of (1S,2S)-1-phenylpropane-1,2-diol 2-O-beta-D-glucopyranoside (1) and p-menth-4(8)-ene-1,2-diol 1-O-alpha-L-arabinopyranosyl-(1-6)-beta-D-glucopyranoside (2). Both glycosides have been identified for the first time in nature. They could be considered as immediate precursors of 1-phenylpropane-1,2-diol and p-menth-4(8)-ene-1,2-diol, typical volatiles found in the fruit of cape gooseberry.

  1. 3D-printed lab-on-valve for fluorescent determination of cadmium and lead in water.

    PubMed

    Mattio, Elodie; Robert-Peillard, Fabien; Vassalo, Laurent; Branger, Catherine; Margaillan, André; Brach-Papa, Christophe; Knoery, Joël; Boudenne, Jean-Luc; Coulomb, Bruno

    2018-06-01

    In recent years, the development of 3D printing in flow analysis has allowed the creation of new systems with various applications. Up to now, 3D printing was mainly used for the manufacture of small units such as flow detection cells, preconcentration units or mixing systems. In the present study, a new 3D printed lab-on-valve system was developed to selectively quantify lead and cadmium in water. Different technologies were compared for lab-on-valve 3D printing. Printed test units have shown that stereolithography or digital light processing are satisfactory techniques for creating complex lab-on-valve units. The lab-on-valve system was composed of two columns, eight peripheral ports and a central port, and a coil integrating baffles to increase mixing possibilities. A selective extraction of lead was first carried out by TrisKem Pb™ Resin column. Then, cadmium not retained on the first column was extracted on a second column of Amberlite® IR 120 resin. In a following step, lead and cadmium were eluted with ammonium oxalate and potassium iodide, respectively. Finally, the two metals were sequentially detected by the same Rhod-5N™ fluorescent reagent. This 3D printed lab-on-valve flow system allowed us to quantify lead and cadmium with a linear response from 0.2 to 15 µg L -1 and detection limits of 0.17 and 0.20 µg L -1 for lead and cadmium, respectively, which seems adapted for natural water analysis. Copyright © 2018 Elsevier B.V. All rights reserved.

  2. Effect of natural aquatic humic substances on the photodegradation of estrone.

    PubMed

    Silva, Carla Patrícia; Lima, Diana L D; Groth, Milena B; Otero, Marta; Esteves, Valdemar I

    2016-02-01

    Photodegradation of estrone (E1) was investigated under simulated solar radiation in absence and presence of the different fractions of humic substances (HS), namely humic acids (HA), fulvic acids (FA) and XAD-4 fraction. The pseudo-first order photodegradation rate constants increased from 0.1137 h(-1), in ultrapure (MQ) water, to 0.1774, 0.1943 and 0.3109 h(-1), in presence of HA, FA and XAD-4, respectively. Half-life time decreased from 6.10 h in MQ water to 3.91, 3.57 and 2.23 h in presence of HA, FA and XAD-4, respectively. These results evidence the relevant photosensitizing effect of XAD-4 fraction of HS on the degradation of E1, which, to the best of our knowledge have never been studied. Photodegradation studies were also conducted in organic matter-rich environmental aquatic matrices, namely fresh, estuarine and waste water. After 2 h, photodegradation achieved values ranged between 35.6 and 57.1% in natural water samples, compared with 26.4% in ultrapure water. The higher photodegradation occurred in an estuarine water sample, known to be rich in XAD-4 fraction and poor in HA, indicating that not only the presence of organic matter, but also its type, are determinant in the E1 photodegradation rate. Finally, the use of sodium azide as singlet oxygen ((1)O2) scavenger during the phototransformation of E1 in ultrapure and in two wastewater samples allowed to conclude that (1)O2 has an important role in the E1 photodegradation. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Removal of cyanotoxins from surface water resources using reusable molecularly imprinted polymer adsorbents.

    PubMed

    Krupadam, Reddithota J; Patel, Govind P; Balasubramanian, Rajasekhar

    2012-06-01

    Microcystins (MCs; cyclic heptapeptides) are produced by freshwater cyanobacteria and cause public health concern in potable water supplies. There are more than 60 types of MCs identified to date, of which MC-LR is the most common found worldwide. For MC-LR, the WHO has established a threshold value of 1 μg L(-1) for drinking water. The present MCs removal methods such as coagulation, flocculation, adsorption, and filtration showed low efficiency for removing dissolved MC fraction from surface waters to the stipulated limit prescribed by WHO based on MC health impacts. The search for cost-effective and efficient removal method is still warranted for remediation of dissolved MC-LR-contaminated water resources. Molecularly imprinted polymer (MIP) adsorbent has been prepared using non-covalent imprinting approach. Using MC-LR as a template, itaconic acid as a functional monomer, and ethylene glycol dimethacrylate as a cross-linking monomer, a MIP has been synthesized. Computer simulations were used to design effective binding sites for MC-LR binding in aqueous solutions. Batch binding adsorption assay was followed to determine binding capacity of MIP under the influence of environmental parameters such as total dissolved solids and pH. The adsorptive removal of MC-LR from lake water has been investigated using MIPs. The MIP showed excellent adsorption potential toward MC-LR in aqueous solutions with a binding capacity of 3.64 μg mg(-1) which is about 60% and 70% more than the commercially used powdered activated carbon (PAC) and resin XAD, respectively. Environmental parameters such as total organic carbon (represented as chemical oxygen demand (COD)) and total dissolved solids (TDS) showed no significant interference up to 300 mg L(-1) for MC-LR removal from lake water samples. It was found that the binding sites on PAC and XAD have more affinity toward COD and TDS than the MC-LR. Further, the adsorption capacity of the MIP was evaluated rigorously by its repeated contact with fresh lake water, and it was found that the adsorption capacity of the MIP did not change even after seven adsorption/desorption cycles. The contaminated water of MC-LR (1.0 μg L(-1)) of 3,640 L could be treated by 1 g of MIP with an estimated cost of US $1.5. The adsorption capacity of the MIP is 40% more than commercially used PAC and resins and also the polymer showed reusable potential which is one of the important criteria in selection of cyanotoxins remediation methods.

  4. Toward full spectrum speciation of silver nanoparticles and ionic silver by on-line coupling of hollow fiber flow field-flow fractionation and minicolumn concentration with multiple detectors.

    PubMed

    Tan, Zhi-Qiang; Liu, Jing-Fu; Guo, Xiao-Ru; Yin, Yong-Guang; Byeon, Seul Kee; Moon, Myeong Hee; Jiang, Gui-Bin

    2015-08-18

    The intertransformation of silver nanoparticles (AgNPs) and ionic silver (Ag(I)) in the environment determines their transport, uptake, and toxicity, demanding methods to simultaneously separate and quantify AgNPs and Ag(I). For the first time, hollow fiber flow field-flow fractionation (HF5) and minicolumn concentration were on-line coupled together with multiple detectors (including UV-vis spectrometry, dynamic light scattering, and inductively coupled plasma mass spectrometry) for full spectrum separation, characterization, and quantification of various Ag(I) species (i.e., free Ag(I), weak and strong Ag(I) complexes) and differently sized AgNPs. While HF5 was employed for filtration and fractionation of AgNPs (>2 nm), the minicolumn packed with Amberlite IR120 resin functioned to trap free Ag(I) or weak Ag(I) complexes coming from the radial flow of HF5 together with the strong Ag(I) complexes and tiny AgNPs (<2 nm), which were further discriminated in a second run of focusing by oxidizing >90% of tiny AgNPs to free Ag(I) and trapped in the minicolumn. The excellent performance was verified by the good agreement of the characterization results of AgNPs determined by this method with that by transmission electron microscopy, and the satisfactory recoveries (70.7-108%) for seven Ag species, including Ag(I), the adduct of Ag(I) and cysteine, and five AgNPs with nominal diameters of 1.4 nm, 10 nm, 20 nm, 40 nm, and 60 nm in surface water samples.

  5. Improved coupled-column liquid chromatographic method for the determination of glyphosate and aminomethylphosphonic acid residues in environmental waters.

    PubMed

    Hidalgo, Carmén; Rios, Carolina; Hidalgo, Manuela; Salvadó, Victòria; Sancho, Juan V; Hernández, Félix

    2004-04-30

    An existing method for the determination of glyphosate and its main metabolite aminomethylphosphonic acid (AMPA) in water has been improved. It is based on precolumn derivatization with the fluorescent reagent 9-fluorenylmethylcloroformate (FMOC) followed by large-volume injection in a coupled-column LC system using fluorescence detection (LC-LC-FD). The derivatization step was slightly modified by changing parameters such as volume and/or concentration of sample and reagents to decrease the limits of quantification (LOQ) of glyphosate and AMPA to 0.1 microg/l. Additionally, the use of Amberlite IRA-900 for preconcentration of glyphosate, prior to the derivatization step, was investigated; the LOQ of glyphosate was lowered to 0.02 microg/l. Drinking, surface and ground water spiked with glyphosate and AMPA at 0.1-10 microg/l concentrations were analysed by the improved LC-LC-FD method. Recoveries were 87-106% with relative standard deviations lower than 8%. Drinking and ground water spiked with glyphosate at 0.02 and 0.1 microg/l were analysed after preconcentration on the anion-exchange resin with satisfactory recoveries (94-105%) and precision (better than 8%).

  6. Antibacterial activity and genotypic-phenotypic characteristics of bacteriocin-producing Bacillus subtilis KKU213: potential as a probiotic strain.

    PubMed

    Khochamit, Nalisa; Siripornadulsil, Surasak; Sukon, Peerapol; Siripornadulsil, Wilailak

    2015-01-01

    The antimicrobial activity and probiotic properties of Bacillus subtilis strain KKU213, isolated from local soil, were investigated. The cell-free supernatant (CFS) of a KKU213 culture containing crude bacteriocins exhibited inhibitory effects on Gram-positive bacteria, including Bacillus cereus, Listeria monocytogenes, Micrococcus luteus, and Staphylococcus aureus. The antibacterial activity of the CFS precipitated with 40% ammonium sulfate (AS) remained even after treatment at 60 and 100 °C, at pH 4 and 10 and with proteolytic enzymes, detergents and heavy metals. When analyzed by SDS-PAGE and overlaid with the indicator strains B. cereus and S. aureus, the 40% AS precipitate exhibited inhibitory activity on proteins smaller than 10 kDa. However, proteins larger than 25 kDa and smaller than 10 kDa were still observed on a native protein gel. Purified subtilosin A was prepared by Amberlite XAD-16 bead extraction and HPLC and analyzed by Nano-LC-QTOF-MS. Its molecular mass was found to be 3.4 kDa, and it retained its antibacterial activity. These results are consistent with the detection of the anti-listerial subtilosin A gene of the sbo/alb cluster in the KKU213 strain, which is 100% identical to that of B. subtilis subsp. subtilis 168. In addition to stable and cyclic subtilosin A, a mixture of many extracellular antibacterial peptides was also detected in the KKU213 culture. The KKU213 strain produced extracellular amylase, cellulase, lipase and protease, is highly acid-resistant (pH 2) when cultured in inulin and promotes health and reduces infection of intestinally colonized broiler chickens. Therefore, we propose that bacteriocin-producing B. subtilis KKU213 could be used as a potential probiotic strain or protective culture. Copyright © 2014 Elsevier GmbH. All rights reserved.

  7. Biodegradation of crude oil into nonvolatile organic acids in a contaminated aquifer near Bemidji, Minnesota

    USGS Publications Warehouse

    Thorn, K.A.; Aiken, G.R.

    1998-01-01

    As the result of a pipeline burst, a body of light aliphatic crude oil floats atop the groundwater in a shallow sand and gravel aquifer in a remote area outside Bemidji, Minnesota. Biodegradation has resulted in the formation of a plume of DOC downgradient from the oil body. Groundwater has also been contaminated in an area known as the spray zone, from vertical infiltration of DOC resulting from biodegradation of crude oil in the overlying unsaturated zone. The majority of DOC in the contaminated groundwater is in the form of nonvolatile organic acids (NVOA's) which represent the partial oxidation products of the crude oil constituents. The NVOA's have been classified into three fractions according to their isolation on XAD resins: hydrophobic neutrals (HPO-N), hydrophobic acids (HPO-A) and hydrophilic acids (HPI-A). These fractions of NVOA's were isolated from a well downgradient from the oil body (well 530; DOC=21 mg C/l), from a well in the spray zone (well 603; DOC=15 mg C/l) and from an uncontaminated well upgradient of the oil body where the naturally occurring DOC is 2.9 mg C/l (well 310). The three sets of NVOA's were characterized by elemental analyses, molecular weight determinations, 14C ages and liquid phase 1H and 13C NMR. The crude oil and the saturate, aromatic, resin and asphaltene fractions of the crude oil were similarly analyzed by elemental analysis and NMR. The NVOA's from the contaminated wells were clearly distinguishable from the naturally occurring groundwater DOC. Based upon molecular weights, sulfur contents, aromaticities and the presence of methyl groups bonded to aromatic rings, the characterization data suggests that the NVOA's originate from the C18 or greater alkylaromatic, naphthenoaromatic and sulfur-containing constituents of the crude oil, including possibly the resins and asphaltenes.

  8. Purification and characterization of antimicrobial peptides from fish isolate Carnobacterium maltaromaticum C2: Carnobacteriocin X and carnolysins A1 and A2.

    PubMed

    Tulini, Fabricio L; Lohans, Christopher T; Bordon, Karla C F; Zheng, Jing; Arantes, Eliane C; Vederas, John C; De Martinis, Elaine C P

    2014-03-03

    Carnobacterium maltaromaticum C2, isolated from Brazilian smoked fish (Surubim, Pseudoplatystoma sp.), was found to exert antimicrobial activity against Listeria monocytogenes, an important foodborne pathogen. In this study, the bacteriocins produced by C. maltaromaticum C2 were purified via an extraction with XAD-16 resin, a C18 solid phase extraction, followed by reversed-phase fast protein liquid chromatography. The purified active fractions were characterized using tandem mass spectrometry, permitting the identification of multiple bacteriocins. Carnobacteriocins BM1, B1, and a variant of carnobacteriocin B2 were all found, providing much of the antilisterial activity. Additionally, we herein report the first isolation of the previously predicted antimicrobial peptide carnobacteriocin X. Moreover, C. maltaromaticum C2 produces a novel two-component lantibiotic, termed carnolysin, homologous to enterococcal cytolysin. This lantibiotic is antimicrobially inactive when tested against the non-bacteriocinogenic strain C. maltaromaticum A9b-, likely requiring an additional proteolytic cleavage to reach maturity. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Assessment of organic contaminants in emissions from refuse-derived fuel combustion

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chrostowski, J.; Wait, D.; Kwong, E.

    1985-09-01

    Organic contaminants in emissions from refuse-derived fuel combustion were investigated in a 20-inch-diameter atmospheric fluidized-bed combustor. Combinations of coal/EcoFuel/MSW/toluene were burned inthe combustor with temperatures ranging from 1250 to 1550 degrees F. A Source Assessment Sampling System (SASS) was used to sample the stack gas; Level 1 methodology was used to analyze the organic-contaminant levels. Combustion efficiencies of 93 to 98 percent were achieved in the test burns. Combustion of the EcoFuel generated fewer organic emissions than combustion of coal at similar combustion temperatures. The fine particulate collected by the SASS train filter contained higher concentrations of extractable organics thanmore » the reactor fly ash and the SASS cyclone samples. Combustion of a toluene/EcoFuel mix generated a large number of benzene derivatives not seen in the combustion of pure EcoFuel. Polycyclic aromatic hydrocarbons were the dominant organic compounds contained in the XAD-2 resin extract from coal combustion. A number of different priority pollutants were identified in the samples collected.« less

  10. Organic emissions from coal pyrolysis: mutagenic effects.

    PubMed Central

    Braun, A G; Wornat, M J; Mitra, A; Sarofim, A F

    1987-01-01

    Four different types of coal have been pyrolyzed in a laminar flow, drop tube furnace in order to establish a relationship between polycyclic aromatic compound (PAC) evolution and mutagenicity. Temperatures of 900K to 1700K and particle residence times up to 0.3 sec were chosen to best simulate conditions of rapid rate pyrolysis in pulverized (44-53 microns) coal combustion. The specific mutagenic activity (i.e., the activity per unit sample weight) of extracts from particulates and volatiles captured on XAD-2 resin varied with coal type according to the order: subbituminous greater than high volatile bituminous greater than lignite greater than anthracite. Total mutagenic activity (the activity per gram of coal pyrolyzed), however, varied with coal type according to the order: high volatile bituminous much greater than subbituminous = lignite much greater than anthracite, due primarily to high organic yield during high volatile bituminous coal pyrolysis. Specific mutagenic activity peaked in a temperature range of 1300K to 1500K and generally appeared at higher temperatures and longer residence times than peak PAC production. PMID:3311724

  11. OPERATION SANDSTONE. Nuclear Explosions. 1948. Scientific Director’s Report of Atomic Weapon Tests. Annex 11, Parts 1, 2, and 3. Thermal Effects and Decontamination Studies

    DTIC Science & Technology

    1948-06-30

    formaldehyde 5 allyl resin 7 melamine resin 8 acrylic resin (lucite HC 201 H-3) 9 vinyl resin (Vinylite VS 131D K-3) 10 styrene resin (polystyrere J-7, mfgd...Chlorinated Rubber, CB.4L 24 Neoprene Melamine Resins 7 PoPysulfide Rubber,, IP.3 25 Acrylic Resins 8 Folysulfide Rubber, LP-2A 25A Vinyl Resins 9 Butyl...with the set of original samples. -- 5-- TABLE I. List of Sa,,ples SA2PLE I.O. MATERIAL 1 phenol formaldehyde 2 urea

  12. 40 CFR Table 7 to Subpart Wwww of... - Options Allowing Use of the Same Resin Across Different Operations That Use the Same Resin Type

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 12 2010-07-01 2010-07-01 true Options Allowing Use of the Same Resin Across Different Operations That Use the Same Resin Type 7 Table 7 to Subpart WWWW of Part 63 Protection... Pollutants: Reinforced Plastic Composites Production Pt. 63, Subpt. WWWW, Table 7 Table 7 to Subpart WWWW of...

  13. Design and fabrication of an innovative and environmental friendly adsorbent for boron removal.

    PubMed

    Wei, Yu-Ting; Zheng, Yu-Ming; Chen, J Paul

    2011-03-01

    Boron can pose adverse effects on human beings and plants species. It exists in various water environments and is difficult to be removed by conventional technologies. In this study, an efficient and environmental friendly sorbent was fabricated by the functionalization of a natural biopolymer, chitosan, with N-methylglucamine through atom transfer radical polymerization. The SEM and BET studies revealed that the sorbent had a rougher surface and a more porous structure than the chitosan. At the optimum neutral pH, the maximum sorption capacity was as high as 3.25 mmol/g, much higher than the commercial boron selective resins (e.g., Amberlite IRA-743) and many other synthesized sorbents. Almost 90% of boron sorption occurred within 8 h and the equilibrium was established in 12 h, which was well described by an intraparticle surface diffusion model. The presence of sodium chloride and sodium nitrate had no effect on the boron removal. The boron concentration in seawater could be reduced to less than 0.5 mg/L from 4.8 mg/L when a sorbent dosage of 1.2 g/L was used. It was therefore concluded that the sorption technology from this study could be promising for boron removal from aqueous solutions. Copyright © 2011 Elsevier Ltd. All rights reserved.

  14. Study of natural organic matter fractions in water sources of Tehran.

    PubMed

    Zazouli, M A; Nasseri, S; Mahvi, A H; Mesdaghinia, A R; Gholami, M

    2007-05-15

    Natural Organic Matters (NOMs) are abundant in natural water resources and in many ways may affect the unit operations in water treatment. Although, NOMs are considered harmless but they have been recognized disinfection by-products precursors (DBP(s)) during the chlorination process. Formation of DBP(s) highly depends on the composition and concentration of NOM, which can be broadly divided into two fractions of hydrophobic (humic) and hydrophilic (non-humic) substances. The objective of this study was to determine Natural organic matter and its fractions concentration in the surface water sources of Tehran. Water sampling was conducted monthly between May to July 2006 in three rivers Lar, Jajrood and Karaj as the main drinking water supplying sources in Tehran. Quantitative parameters of pH, EC, UV254 and DOC were studied based on to standard methods. The XAD-7 resin method was used for fractionation of NOM. Results showed that NOM concentrations in Lar, Jajrood and Karaj rivers were 8.53, 12.9 and 11.3 mg L(-1), respectively. The HPO (hydrophobic) fraction was predominant compared to the HPI (hydrophilic) fraction in the all of water samples. The mean of total percent of HPO and HPI fractions were about 57 and 43%, respectively. Since the hydrophobic NOM fraction exhibits higher trihalomethane formation potential (THMFP) than hydrophilic NOM, Tehran water chlorination exhibits higher THMFP than haloacetic acid formation potential (HAAFP). The information obtained from this study may be further employed in the design of the control technique and management strategies for the water treatment plant, especially for DBP(s) reduction.

  15. Can simultaneous contact allergies to phenyl glycidyl ether and epoxy resins of the bisphenol A/F-types be explained by contamination of the epoxy resins?

    PubMed

    Pontén, Ann; Zimerson, Erik; Bruze, Magnus

    2008-11-01

    Simultaneous contact allergies to epoxy resins based on diglycidyl ether of bisphenol A (DGEBA-R) or epoxy resins of the bisphenol F-type and the reactive diluent phenyl glycidyl ether (PGE) have been reported. The reason might be cross-reactivity, exposure to an epoxy resin system with PGE as a component, or contamination by PGE in the epoxy resin. To study contamination by PGE, 20 commercial epoxy resins were analysed for the presence of PGE. To study contact allergy to PGE and its relation to epoxy resins by inserting PGE in the standard series. Among 2227 patients, 7 reacted to PGE. Of 23 (30%) patients, 7 with contact allergy to DGEBA-R and 7/19 (37%) with contact allergy to an epoxy resin of the bisphenol F-type reacted to PGE. All 7 patients with contact allergy to PGE reacted both to the DGEBA-R and to the epoxy resin of the bisphenol F-type. PGE was found in 90% of the investigated resins. The amounts of PGE ranged between 0.004% w/w and 0.18% w/w. Most probably, the presence of PGE as a contaminant in epoxy resins is of minor importance for the sensitization, but possibly the contamination of PGE might elicit contact dermatitis in individuals with a high reactivity to PGE.

  16. Comparison of two common adsorption materials for thermal desorption gas chromatography - mass spectrometry of biogenic volatile organic compounds.

    PubMed

    Marcillo, Andrea; Jakimovska, Viktorija; Widdig, Anja; Birkemeyer, Claudia

    2017-09-08

    Volatile organic compounds (VOCs) are commonly collected from gaseous samples by adsorption to materials such as the porous polymer Tenax TA. Adsorbed compounds are subsequently released from these materials by thermal desorption (TD) and separated then by gas chromatography (GC) with flame ionization (FID) or mass spectrometry (MS) detection. Tenax TA is known to be particularly suitable for non-polar to semipolar volatiles, however, many volatiles from environmental and biological samples possess a rather polar character. Therefore, we tested if the polymer XAD-2, which so far is widely used to adsorb organic compounds from aqueous and organic solvents, could provide a broader coverage for (semi)polar VOCs during gas-phase sampling. Mixtures of volatile compounds covering a wide range of volatility (bp. 20-256°C) and different chemical classes were introduced by liquid spiking into sorbent tubes with one of the two porous polymers, Tenax TA or XAD-2, and analyzed by TD/GC-MS. At first, an internal standard mixture composed of 17 authentic standards was used to optimize desorption temperature with respect to sorbent degradation and loading time for calibration. Secondly, we tested the detectability of a complex standard mixture composed of 57 volatiles, most of them common constituents of the body odor of mammals. Moreover, the performance of XAD-2 compared with Tenax TA was assessed as limit of quantitation and linearity for the internal standard mixture and 33 compounds from the complex standard mixture. Volatiles were analyzed in a range between 0.01-∼250ng/tube depending on the compound and material. Lower limits of quantitation were between 0.01 and 3 ng±<25% RSD (R 2 >0.9). Interestingly, we found different kinetics for compound adsorption with XAD-2, and a partially better sensitivity in comparison with Tenax TA. For these analytes, XAD-2 might be recommended as an alternative of Tenax TA for TD/GC-MS analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. QUANTITATIVE DETERMINATION OF THE URANIUM CONTENT OF URANIUM ORES TECHNOLOGICAL PRODUCTS BY ION EXCHANGE-COMPLEXON SEPARATION (in Hungarian)

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fodor, M.

    An ion exchange-complexion separation meihod was developed for the removal of interfering elements in the determination of the uranium content of recovery solutions. By adding (ethylenediamine)tetraacetic acid to the solution, most of the interfering elements can be brought into an anionic complex. Adjusting the soluiion to pH 7 and letting it pass through an Amberlite IRC-50 type cation exchanger of hydrogen form, the uranium remains on the column whereas the interfering elements pass into the effluent. The method was successfully applied in analyzing the recovery solutions of uranium ores. (auth)

  18. Level 1 environmental assessment performance evaluation. Final report jun 77-oct 78

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Estes, E.D.; Smith, F.; Wagoner, D.E.

    1979-02-01

    The report gives results of a two-phased evaluation of Level 1 environmental assessment procedures. Results from Phase I, a field evaluation of the Source Assessment Sampling System (SASS), showed that the SASS train performed well within the desired factor of 3 Level 1 accuracy limit. Three sample runs were made with two SASS trains sampling simultaneously and from approximately the same sampling point in a horizontal duct. A Method-5 train was used to estimate the 'true' particulate loading. The sampling systems were upstream of the control devices to ensure collection of sufficient material for comparison of total particulate, particle sizemore » distribution, organic classes, and trace elements. Phase II consisted of providing each of three organizations with three types of control samples to challenge the spectrum of Level 1 analytical procedures: an artificial sample in methylene chloride, an artificial sample on a flyash matrix, and a real sample composed of the combined XAD-2 resin extracts from all Phase I runs. Phase II results showed that when the Level 1 analytical procedures are carefully applied, data of acceptable accuracy is obtained. Estimates of intralaboratory and interlaboratory precision are made.« less

  19. H-binding of size- and polarity-fractionated soil and lignite humic acids after removal of metal and ash components.

    PubMed

    Drosos, Marios; Leenheer, Jerry A; Avgeropoulos, Apostolos; Deligiannakis, Yiannis

    2014-03-01

    A fractionation technique, combining dialysis removal of metal and ash components with hydrofluoric acid and pH 10 citrate buffer followed by chromatography of dialysis permeate on XAD-8 resin at decreasing pH values, has been applied to lignite humic acid (lignite-HA) and soil humic acid (soil-HA). H-binding data and non ideal competitive adsorption-Donnan model parameters were obtained for the HA fractions by theoretical analysis of H-binding data which reveal a significant increase of the carboxyl and the phenolic charge for the lignite-HA fractions vs. the parental lignite humic acid (LParentalHA). The fractionated lignite-HA material consisted mainly of permeate fractions, some of which were fulvic acid-like. The fractionated soil-HA material consisted mainly of large macromolecular structures that did not permeate the dialysis membrane during deashing. Chargeable groups had comparable concentrations in soil-HA fractions and parental soil humic acid (SParentalHA), indicating minimal interference of ash components with carboxyl and phenolic (and/or enolic) groups. Fractionation of HA, combined with theoretical analysis of H-binding, can distinguish the supramolecular vs. macromolecular nature of fractions within the same parental HA.

  20. Integration of coagulation and adsorption for removal of N-nitrosodimethylamine (NDMA) precursors from biologically treated municipal wastewater.

    PubMed

    Wang, Miaomiao; Meng, Yingjie; Ma, Defang; Wang, Yan; Li, Fengli; Xu, Xing; Xia, Chufan; Gao, Baoyu

    2017-05-01

    This study investigated the N-nitrosodimethylamine (NDMA) formation potential of various dissolved organic matter (DOM) fractions in biologically treated municipal wastewater by UF fractionation, XAD-8 resin adsorption isolation, and excitation and emission matrix (EEM) fluorescence spectroscopy. Removal of various NDMA precursor fractions was also analyzed to evaluate the efficiency of traditional water treatment processes (coagulation, adsorption, and coagulation-adsorption). Results showed that NDMA were mainly formed by low molecular weight (MW) fractions (<30 kDa) and hydrophilic fractions (HiS) in biologically treated municipal wastewater. Integrated coagulation-adsorption treatments showed the highest reduction capacity for NDMA formation potential (57%), followed by isolated adsorption treatment (50%) and isolated coagulation treatment (28%). The powdered activated carbon (PAC) adsorption process could reduce the high MW precursors (>30 kDa) by 48%, which was higher than other treatments. In contrast, the highest uptake (66%) of low MW precursors (<30 kDa) was achieved by the coagulation-adsorption process. All treatments preferentially removed the hydrophobic acids (HoA) fraction compared to other fractions. Coagulation could remove more fulvic acid-like substances and adsorption could remove more microbial by-products and aromatic proteins.

  1. H-binding of size- and polarity-fractionated soil and lignite humic acids after removal of metal and ash components

    USGS Publications Warehouse

    Drosos, Marios; Leenheer, Jerry A.; Avgeropoulos, Apostolos; Deligiannakis, Yiannis

    2014-01-01

    A fractionation technique, combining dialysis removal of metal and ash components with hydrofluoric acid and pH 10 citrate buffer followed by chromatography of dialysis permeate on XAD-8 resin at decreasing pH values, has been applied to lignite humic acid (lignite-HA) and soil humic acid (soil-HA). H-binding data and non ideal competitive adsorption-Donnan model parameters were obtained for the HA fractions by theoretical analysis of H-binding data which reveal a significant increase of the carboxyl and the phenolic charge for the lignite-HA fractions vs. the parental lignite humic acid (LParentalHA). The fractionated lignite-HA material consisted mainly of permeate fractions, some of which were fulvic acid-like. The fractionated soil-HA material consisted mainly of large macromolecular structures that did not permeate the dialysis membrane during deashing. Chargeable groups had comparable concentrations in soil-HA fractions and parental soil humic acid (SParentalHA), indicating minimal interference of ash components with carboxyl and phenolic (and/or enolic) groups. Fractionation of HA, combined with theoretical analysis of H-binding, can distinguish the supramolecular vs. macromolecular nature of fractions within the same parental HA.

  2. [Mutagenicity study of water samples from a waterworks taking Yangtze River as its water source in Jiangsu Province].

    PubMed

    Xiao, Sanhua; Luo, Lan; Qiao, Qian; Lü, Xuemin; Wang, Yanhui; Feng, Lin; Tang, Fei; Wang, Haiyong; Bie, Nana; Wang, Yuehong

    2017-05-01

    To understand the occurrence and change of mutagencity of water samples in the process of drinking water treatment and distribution in a waterworks taking Yangtze River as its water source in Jiangsu Province. Large volume of inlet water, finished water and tap water samples were extracted by XAD-2 resin. Mutagencities were assessed by Ames test and a mutation ratio( MR) of 2 or greater was judged as a positive result. Compared with the samples with S9, samples without S9 presented more positive results( P = 0. 005). That water treatment elevated MR values( P = 0. 007) while the pipe transport made MR values down( P = 0. 038) was observed in samples without S9. The tap water showed weaker mutagenicities than the raw water in samples with S9( P = 0. 008). Compared to the raw water samples, the finished water samples showed more positive results(-S9) and lower MR values( + S9, P =0. 002). Significant mutagenicities of water samples from the Yangtze Riverand its processed water were presented, and frame shit and direct mutagens deserved special concern.

  3. Mutagens in cooked foods - metabolism and genetic toxicity

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Felton, J.S.; Bjeldanes, L.F.; Hatch, F.T.

    1984-02-17

    Recently developed in our laboratories is an efficient extraction procedure incorporating XAD resin adsorption which yields from 200/sup 0/C grilled ground beef an extract containing 230 Salmonella TA1538 revertants per g fresh weight of original ground beef. These mutagenic components are specific for frameshift-sensitive Salmonella strains and have an absolute requirement for metabolic activation. Normal-phase HPLC separation of methanol-extractable metabolites generated from reaction of 2-amino-3-methylimidazo (4,5-f)quinoline (IQ), a mutagenic component of broiled food with rat liver microsomes resulted in one direct-acting mutagenic peak and a second more polar peak still requiring metabolic activation. Two potent thermally-produced bacterial mutagens, 3-amino-1-methyl-5H-pyrido (4,3-b)more » indole (Trp-P-2) and IQ, were examined in mammalian cells. In excision repair-deficient CHO cells, Trp-P-2 exposure caused cytotoxicity, mutagenicity, sister chromatid exchange, and chromosomal aberrations at concentrations more than 30-fold lower than those for IQ. In normal repair-proficient CHO cells Trp-P-2 was one-half as active and IQ was inactive. Relative to Trp-P-2, IQ is much more potent in the Salmonella bacterial system than in mammalian CHO cells.« less

  4. Effect of volatile hydrocarbon fractions on mobility and earthworm uptake of polycyclic aromatic hydrocarbons from soils and soil/lampblack mixtures.

    PubMed

    Bogan, Bill W; Beardsley, Kate E; Sullivan, Wendy R; Hayes, Thomas D; Soni, Bhupendra K

    2005-01-01

    Studies were conducted to examine the mobility and bioavailability to earthworms (Eisenia fetida) of priority pollutant polycyclic aromatic hydrocarbons (PAH) in a suite of 11 soils and soil/lampblack mixtures obtained from former manufactured-gas plant sites. Contaminant mobility was assessed using XAD4 resins encapsulated in dialysis tubing, which were exposed to slurried soils for 15 d. These experiments showed that mobility of PAH in the different soils strongly correlated to the levels of volatile hydrocarbons (namely, gasoline- and diesel-range organics [GRO and DRO]) that existed in the soils as co-contaminants. Actual PAH bioavailability (as measured by earthworm PAH concentrations) also appeared to depend on GRO + DRO levels, although this was most evident at high levels of these contaminants. These findings are discussed in view of the effects of dieselrange organics on oil viscosity, assuming that the hydrocarbon contaminants in these soils exist in the form of distinct adsorbed oil phases. This study, therefore, extends correlations between carrier-oil viscosity and dissolved solute bioavailability, previously observed in a number of other in vitro and whole-organism tests (and in bacterial mutagenicity studies in soil), to multicellular organisms inhabiting contaminated-soil systems.

  5. Exposure to mutagenic chemicals in foundry and urban environments.

    PubMed

    Barański, B; Palus, J; Janik-Spiechowicz, E

    1989-01-01

    The study was aimed at the estimation of occupational exposure to mutagenic substances in a piston-ring foundry. The following samples were examined: solid phase of aerosol from the foundry and from different places of urban environment together with the foundry workers' urine collected during the 8-hour shift. The mutagenic substances were extracted from the collected material with acetone or concentrated with XAD-2 resin. The mutagenic property was estimated with the Ames' test using S. typhimurium strain TA98 without and with S9 fraction. The highest mutagenic activity was found at the following work-posts: caster, moulder, steerer of an induction furnace, and smelter and in the office rooms and in the flat occupied by heavy smokers. The mutagenic activity of aerosol at some other productive workposts in the foundry was similar to the mutagenic activity of aerosol in the office and flat rooms occupied by nonsmokers or in the street in Lodz. The mutagenic activity of urine from foundry workers was not correlated with the level of the occupational inhalation exposure to the mutagenic substances, however, the mutagenic activity of urine from smoking workers was about 10-20 times higher than from nonsmokers.

  6. Deep ancestry of mammalian X chromosome revealed by comparison with the basal tetrapod Xenopus tropicalis.

    PubMed

    Mácha, Jaroslav; Teichmanová, Radka; Sater, Amy K; Wells, Dan E; Tlapáková, Tereza; Zimmerman, Lyle B; Krylov, Vladimír

    2012-07-16

    The X and Y sex chromosomes are conspicuous features of placental mammal genomes. Mammalian sex chromosomes arose from an ordinary pair of autosomes after the proto-Y acquired a male-determining gene and degenerated due to suppression of X-Y recombination. Analysis of earlier steps in X chromosome evolution has been hampered by the long interval between the origins of teleost and amniote lineages as well as scarcity of X chromosome orthologs in incomplete avian genome assemblies. This study clarifies the genesis and remodelling of the Eutherian X chromosome by using a combination of sequence analysis, meiotic map information, and cytogenetic localization to compare amniote genome organization with that of the amphibian Xenopus tropicalis. Nearly all orthologs of human X genes localize to X. tropicalis chromosomes 2 and 8, consistent with an ancestral X-conserved region and a single X-added region precursor. This finding contradicts a previous hypothesis of three evolutionary strata in this region. Homologies between human, opossum, chicken and frog chromosomes suggest a single X-added region predecessor in therian mammals, corresponding to opossum chromosomes 4 and 7. A more ancient X-added ancestral region, currently extant as a major part of chicken chromosome 1, is likely to have been present in the progenitor of synapsids and sauropsids. Analysis of X chromosome gene content emphasizes conservation of single protein coding genes and the role of tandem arrays in formation of novel genes. Chromosomal regions orthologous to Therian X chromosomes have been located in the genome of the frog X. tropicalis. These X chromosome ancestral components experienced a series of fusion and breakage events to give rise to avian autosomes and mammalian sex chromosomes. The early branching tetrapod X. tropicalis' simple diploid genome and robust synteny to amniotes greatly enhances studies of vertebrate chromosome evolution.

  7. Deep ancestry of mammalian X chromosome revealed by comparison with the basal tetrapod Xenopus tropicalis

    PubMed Central

    2012-01-01

    Background The X and Y sex chromosomes are conspicuous features of placental mammal genomes. Mammalian sex chromosomes arose from an ordinary pair of autosomes after the proto-Y acquired a male-determining gene and degenerated due to suppression of X-Y recombination. Analysis of earlier steps in X chromosome evolution has been hampered by the long interval between the origins of teleost and amniote lineages as well as scarcity of X chromosome orthologs in incomplete avian genome assemblies. Results This study clarifies the genesis and remodelling of the Eutherian X chromosome by using a combination of sequence analysis, meiotic map information, and cytogenetic localization to compare amniote genome organization with that of the amphibian Xenopus tropicalis. Nearly all orthologs of human X genes localize to X. tropicalis chromosomes 2 and 8, consistent with an ancestral X-conserved region and a single X-added region precursor. This finding contradicts a previous hypothesis of three evolutionary strata in this region. Homologies between human, opossum, chicken and frog chromosomes suggest a single X-added region predecessor in therian mammals, corresponding to opossum chromosomes 4 and 7. A more ancient X-added ancestral region, currently extant as a major part of chicken chromosome 1, is likely to have been present in the progenitor of synapsids and sauropsids. Analysis of X chromosome gene content emphasizes conservation of single protein coding genes and the role of tandem arrays in formation of novel genes. Conclusions Chromosomal regions orthologous to Therian X chromosomes have been located in the genome of the frog X. tropicalis. These X chromosome ancestral components experienced a series of fusion and breakage events to give rise to avian autosomes and mammalian sex chromosomes. The early branching tetrapod X. tropicalis’ simple diploid genome and robust synteny to amniotes greatly enhances studies of vertebrate chromosome evolution. PMID:22800176

  8. Optical Fibre Sensor For Measuring pH In Physiological Range

    NASA Astrophysics Data System (ADS)

    Golunski, Witold; Hypszer, Ryszard; Plucinski, Jerzy

    1990-01-01

    The principle of fibre optic pH sensor operation is given in this paper. PH measurement in 7.0-7.5 range is based on changing of optical property of a indicator. The indicator is sensitive to the hydrogen ion concentration in the water solution. Microspheres of the polymer XAD-2 (a styrene-divinylbenzene copolymer) containing bound phenol red were used as a indicator. Such prepared indicator was inserted in optrode. The optrode was connected with transmitter and receiver by a bundle of glass fibres (multicomponent glass). Transmitter was done by using green LED while receiver construction was based on pin photodiode.

  9. Development of a gas chromatography-mass spectrometry method for the determination of pesticides in gaseous and particulate phases in the atmosphere.

    PubMed

    Borrás, E; Sánchez, P; Muñoz, A; Tortajada-Genaro, L A

    2011-08-05

    A reliable multi-residue method for determining gaseous and particulate phase pesticides in atmospheric samples has been developed. This method, based on full scan gas chromatography-mass spectrometry (GC-MS), allowed the proper determination of sixteen relevant pesticides, in a wide range of concentrations and without the influence of interferences. The pesticides were benfluralin, bitertanol, buprofezin, chlorfenvinphos, chlorpyrifos, chlorpyrifos-methyl, ethalfluralin, fenthion, lindane, malathion, methidathion, propachlor, propanil, pyriproxifen, tebuconazol and trifluralin. Comparisons of two types of sampling filters (quartz and glass fibre) and four types of solid-phase cartridges (XAD-2, XAD-4, Florisil and Orbo-49P) showed that the most suitable supports were glass fibre filter for particulate pesticides and XAD-2 and XAD-4 cartridges for gaseous pesticides (>95% recovery). Evaluations of elution solvents for ultrasonic-assisted extraction demonstrated that isooctane is better than ethylacetate, dichloromethane, methanol or a mixture of acetone:hexane (1:1). Recovery assays and the standard addition method were performed to validate the proposed methodology. Moreover, large simulator chamber experiments allowed the best study of the gas-particle partitioning of pesticides for testing the sampling efficiency for the validation of an analytical multiresidue method for pesticides in air. Satisfactory analytical parameters were obtained, with a repeatability of 5±1%, a reproducibility of 13±3% and detection limits of 0.05-0.18 pg m(-3) for the particulate phase and 26-88 pg m(-3) for the gaseous phase. Finally, the methodology was successfully applied to rural and agricultural samples in the Mediterranean area. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Atmospheric transformation of diesel emissions.

    PubMed

    Zielinska, Barbara; Samy, Shar; McDonald, Jacob D; Seagrave, JeanClare

    2010-04-01

    The hypothesis of this study was that exposing diesel exhaust (DE*) to the atmosphere transforms its composition and toxicity. Our specific aims were (1) to characterize the gas- and particle-phase products of atmospheric transformations of DE under the influence of daylight, ozone (O3), hydroxyl (OH) radicals, and nitrate (NO3) radicals; and (2) to explore the biologic activity of DE before and after the transformations took place. The study was executed with the aid of the EUPHORE (European Photoreactor) outdoor simulation chamber facility in Valencia, Spain. EUPHORE is one of the largest and best-equipped facilities of its kind in the world, allowing investigation of atmospheric transformation processes under realistic ambient conditions (with dilutions in the range of 1:300). DE was generated on-site using a modern light-duty diesel engine and a dynamometer system equipped with a continuous emission-gas analyzer. The engine (a turbocharged, intercooled model with common-rail direct injection) was obtained from the Ford Motor Company. A first series of experiments was carried out in January 2005 (the winter 2005 campaign), a second in May 2005 (the summer 2005 campaign), and a third in May and June 2006 (the summer 2006 campaign). The diesel fuel that was used closely matched the one currently in use in most of the United States (containing 47 ppm sulfur and 15% aromatic compounds). Our experiments examined the effects on the composition of DE aged in the dark with added NO3 radicals and of DE aged in daylight with added OH radicals both with and without added volatile organic compounds (VOCs). In order to remove excess nitrogen oxides (NO(x)), a NO(x) denuder was devised and used to conduct experiments in realistic low-NO(x) conditions in both summer campaigns. A scanning mobility particle sizer was used to determine the particle size and the number and volume concentrations of particulate matter (PM) in the DE. O3, NO(x), and reactive nitrogen oxides (NO(y)) were monitored using chemiluminescence and Fourier transform infrared instruments. At the end of the exposures, samples of particle-associated and semivolatile organic compounds (SVOCs) were collected from the chamber for chemical analysis using an XAD-coated annular denuder followed by a filter and XAD cartridge. (XAD is an adsorbent polystyrene divinylbenzene resin used in sampling cartridges.) Samples for toxicity testing were collected using Teflon filters followed by two XAD cartridges. The chemical analyses included determination of organic carbon (OC), elemental carbon (EC), carbon fractions, inorganic ions (e.g., sulfate and nitrate), and speciated organic compounds (polycyclic aromatic hydrocarbons [PAHs], nitro-PAHs, polar compounds, alkanes, hopanes, and steranes). The toxicity tests were performed with extracts of PM combined with the SVOCs. The biologic activity of these extracts was evaluated in vivo by instilling them into the tracheas of rodents and measuring pulmonary toxicity, inflammation, and oxidative-stress responses. Results from the chemical analyses indicated that aging DE in the dark with added NO3 radicals and aging DE in daylight with and without additions led to the formation of additional particles and SVOC mass caused by reactions of VOCs, SVOCs, and inorganic gases. The greatest increase in mass occurred with the addition of VOCs as co-reactants. The proportions of the pyrolized OC (POC) fraction increased in the organic mass, which suggested that highly polar and oligomeric compounds had been formed. Results from the toxicity testing were consistent with the hypothesis that the toxicity of the samples had been affected by changes in their composition (caused both by the atmospheric aging and by changes in the initial composition of the DE presumably associated with changes in the engine, which was new at the outset and accrued wear during the study).

  11. Speciation of cadmium and zinc with application to soil solutions

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Holm, P.E.; Christensen, T.H.; Tjell, J.C.

    1995-01-01

    A two-part method has been developed for determination of Cd and Zn species in 50-mL soil solution samples containing low concentrations of Cd and Zn (1-10 {mu}g Cd L{sup -1} and 50-1000 {mu}g Zn L{sup -1}). The method uses two cation exchange resins (Amberlite CG 120 and Chelex 100) in a batch-column-batch procedure and relies on analytical determinations of Cd and Zn by graphite furnace atomic absorption spectrophotometry. The first part (batch) of the method allows determination of free divalent Cd{sup 2+} and Zn{sup 2+}. This part is experimentally sensitive to cation concentrations and ionic strength and these parameters shouldmore » be controlled during the experimental procedures. However, it is shown that Cd and Zn concentrations and pH do not influence the method. Speciations performed on samples containing chloride and sulfate were in accordance with theoretical calculations. The second part (column-batch) of the method operationally separates the complexed fraction into labile complexes, slowly labile complexes, and stable complexes. Chloro complexes were identified as labile complexes, while EDTA complexes were identified as stable complexes. The method works well with relatively small volumes of sample solutions and at low metal concentrations and may be useful in characterization of Cd and Zn in soil solutions. 12 refs., 6 figs., 3 tabs.« less

  12. COMPARATIVE STUDIES OF THREE METHODS FOR MEASURING PEPSIN ACTIVITY

    PubMed Central

    Loken, Merle K.; Terrill, Kathleen D.; Marvin, James F.; Mosser, Donn G.

    1958-01-01

    Comparison has been made of a simple method originated by Absolon and modified in our laboratories for assay of proteolytic activity using RISA (radioactive iodinated serum albumin—Abbott Laboratories), with the commonly used photometric methods of Anson and Kunitz. In this method, pepsin was incubated with an albumin substrate containing RISA, followed by precipitation of the undigested substrate with trichloroacetic acid and measurement of radioactive digestion products in the supernatant fluid. The I131—albumin bond was shown in the present studies to be altered only by the proteolytic activity, and not by the incubation procedures at various values of pH. Any free iodine present originally in the RISA was removed by a single passage through a resin column (amberlite IRA-400-C1). Pepsin was shown to be most stable in solution at a pH of 5.5. Activity of pepsin was shown to be maximal when it was incubated with albumin at a pH of 2.5. Pepsin activity was shown to be altered in the presence of various electrolytes. Pepsin activity measured by the RISA and Anson methods as a function of concentration or of time of incubation indicated that these two methods are in good agreement and are equally sensitive. Consistently smaller standard errors were obtained by the RISA method of pepsin assay than were obtained with either of the other methods. PMID:13587910

  13. Dissolved organic matter removal during coal slag additive soil aquifer treatment for secondary effluent recharging: Contribution of aerobic biodegradation.

    PubMed

    Wei, Liangliang; Li, Siliang; Noguera, Daniel R; Qin, Kena; Jiang, Junqiu; Zhao, Qingliang; Kong, Xiangjuan; Cui, Fuyi

    2015-06-01

    Recycling wastewater treatment plant (WWTP) effluent at low cost via the soil aquifer treatment (SAT), which has been considered as a renewable approach in regenerating potable and non-potable water, is welcome in arid and semi-arid regions throughout the world. In this study, the effect of a coal slag additive on the bulk removal of the dissolved organic matter (DOM) in WWTP effluent during SAT operation was explored via the matrix configurations of both coal slag layer and natural soil layer. Azide inhibition and XAD-resins fractionation experiments indicated that the appropriate configuration designing of an upper soil layer (25 cm) and a mixture of soil/coal slag underneath would enhance the removal efficiency of adsorption and anaerobic biodegradation to the same level as that of aerobic biodegradation (31.7% vs 32.2%), while it was only 29.4% compared with the aerobic biodegradation during traditional 50 cm soil column operation. The added coal slag would preferentially adsorb the hydrophobic DOM, and those adsorbed organics could be partially biodegraded by the biomass within the SAT systems. Compared with the relatively lower dissolved organic carbon (DOC), ultraviolet light adsorption at 254 nm (UV-254) and trihalomethane formation potential (THMFP) removal rate of the original soil column (42.0%, 32.9%, and 28.0%, respectively), SSL2 and SSL4 columns would enhance the bulk removal efficiency to more than 60%. Moreover, a coal slag additive in the SAT columns could decline the aromatic components (fulvic-like organics and tryptophan-like proteins) significantly. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Effective removal of effluent organic matter (EfOM) from bio-treated coking wastewater by a recyclable aminated hyper-cross-linked polymer.

    PubMed

    Yang, Wenlan; Li, Xuchun; Pan, Bingcai; Lv, Lu; Zhang, Weiming

    2013-09-01

    Effluent organic matter (EfOM) is a complex matrix of organic substance mainly from bio-treated sewage effluent and is considered as the main constraint to further advanced treatment. Here a recyclable aminated hyper-cross-linked polymeric adsorbent (NDA-802) featured with aminated functional groups, large specific surface area, and sufficient micropore region was synthesized for effective removal of EfOM from the bio-treated coking wastewater (BTCW), and its removal characteristics was investigated. It was found that hydrophobic fraction was the main constituent (64.8% of DOC) in EfOM of BTCW, and the hydrophobic-neutral fraction had the highest SUVA level (7.06 L mg(-1) m(-1)), which were significantly different from that in the domestic wastewater. Column adsorption experiments showed that NDA-802 exhibited much higher removal efficiency of EfOM than other polymeric adsorbents D-301, XAD-4, and XAD-7, and the efficiency could be readily sustained according to continuous 28-cycle batch adsorption-regeneration experiments. Moreover, dissolved organic matter (DOM) fractionation and excitation-emission matrix (EEM) fluorescence spectroscopy study indicated that NDA-802 showed attractive adsorption preference as well as high removal efficiency of hydrophobic and aromatic compounds. Possibly ascribed to the presence of functional aminated groups, relatively large specific surface area and micropore region of the unique polymer, NDA-802 possesses high and sustained efficiency for the removal of EfOM, and provides a potential alternative for the advanced treatment. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Ethanol production from SPORL-pretreated lodgepole pine: preliminary evaluation of mass balance and process energy efficiency.

    PubMed

    Zhu, J Y; Zhu, Wenyuan; Obryan, Patricia; Dien, Bruce S; Tian, Shen; Gleisner, Rolland; Pan, X J

    2010-05-01

    Lodgepole pine from forest thinnings is a potential feedstock for ethanol production. In this study, lodgepole pine was converted to ethanol with a yield of 276 L per metric ton of wood or 72% of theoretical yield. The lodgepole pine chips were directly subjected to sulfite pretreatment to overcome recalcitrance of lignocellulose (SPORL) pretreatment and then disk-milled; the recovered cellulose substrate was quais-simultaneously saccharified enzymatically and fermented to ethanol using commercial cellulases and Saccharomyces cerevisiae D5A. The liquor stream from the pretreatment containing hydrolyzed sugars mainly from hemicelluloses was fermented by the same yeast strain after detoxification using an XAD resin column. The SPORL pretreatment was conducted at 180 degrees C for a period of 25 min with a liquor-to-wood ratio of 3:1 (v/w) in a laboratory digester. Three levels of sulfuric acid charge (0.0%, 1.4%, and 2.2% on an oven dried wood basis in w/w) and three levels of sodium bisulfite charge (0.0%, 4.0%, and 8.0% in w/w) were applied. Mechanical and thermal energy consumption for milling and pretreatment were determined. These data were used to determine the efficiency of sugar recoveries and net ethanol energy production values and to formulate a preliminary mass and energy balance.

  16. The impact of iodinated X-ray contrast agents on formation and toxicity of disinfection by-products in drinking water.

    PubMed

    Jeong, Clara H; Machek, Edward J; Shakeri, Morteza; Duirk, Stephen E; Ternes, Thomas A; Richardson, Susan D; Wagner, Elizabeth D; Plewa, Michael J

    2017-08-01

    The presence of iodinated X-ray contrast media (ICM) in source waters is of high concern to public health because of their potential to generate highly toxic disinfection by-products (DBPs). The objective of this study was to determine the impact of ICM in source waters and the type of disinfectant on the overall toxicity of DBP mixtures and to determine which ICM and reaction conditions give rise to toxic by-products. Source waters collected from Akron, OH were treated with five different ICMs, including iopamidol, iopromide, iohexol, diatrizoate and iomeprol, with or without chlorine or chloramine disinfection. The reaction product mixtures were concentrated with XAD resins and the mammalian cell cytotoxicity and genotoxicity of the reaction mixture concentrates was measured. Water containing iopamidol generated an enhanced level of mammalian cell cytotoxicity and genotoxicity after disinfection. While chlorine disinfection with iopamidol resulted in the highest cytotoxicity overall, the relative iopamidol-mediated increase in toxicity was greater when chloramine was used as the disinfectant compared with chlorine. Four other ICMs (iopromide, iohexol, diatrizoate, and iomeprol) expressed some cytotoxicity over the control without any disinfection, and induced higher cytotoxicity when chlorinated. Only iohexol enhanced genotoxicity compared to the chlorinated source water. Copyright © 2017. Published by Elsevier B.V.

  17. Secondary Structures in a Freeze-Dried Lignite Humic Acid Fraction Caused by Hydrogen-Bonding of Acidic Protons with Aromatic Rings.

    PubMed

    Cao, Xiaoyan; Drosos, Marios; Leenheer, Jerry A; Mao, Jingdong

    2016-02-16

    A lignite humic acid (HA) was separated from inorganic and non-HA impurities (i.e., aluminosilicates, metals) and fractionated by a combination of dialysis and XAD-8 resin. Fractionation revealed a more homogeneous structure of lignite HA. New and more specific structural information on the main lignite HA fraction is obtained by solid-state nuclear magnetic resonance (NMR) spectroscopy. Quantitative (13)C multiple cross-polarization (multiCP) NMR indicated oxidized phenyl propane structures derived from lignin. MultiCP experiments, conducted on potassium HA salts titrated to pH 10 and pH 12, revealed shifts consistent with carboxylate and phenolate formation, but structural changes associated with enolate formation from aromatic beta keto acids were not detected. Two-dimensional (1)H-(13)C heteronuclear correlation (2D HETCOR) NMR indicated aryl-aliphatic ketones, aliphatic and aromatic carboxyl groups, phenol, and methoxy phenyl ethers. Acidic protons from carboxyl groups in both the lignite HA fraction and a synthetic HA-like polycondensate were found to be hydrogen-bonded with electron-rich aromatic rings. Our results coupled with published infrared spectra provide evidence for the preferential hydrogen bonding of acidic hydrogens with electron-rich aromatic rings rather than adjacent carbonyl groups. These hydrogen-bonding interactions likely result from stereochemical arrangements in primary structures and folding.

  18. Evaluation of Genotoxic and Mutagenic Activity of Organic Extracts from Drinking Water Sources

    PubMed Central

    Guan, Ying; Wang, Xiaodong; Wong, Minghung; Sun, Guoping; An, Taicheng; Guo, Jun

    2017-01-01

    An increasing number of industrial, agricultural and commercial chemicals in the aquatic environment lead to various deleterious effects on organisms, which is becoming a serious global health concern. In this study, the Ames test and SOS/umu test were conducted to investigate the potential genotoxicity and mutagenicity caused by organic extracts from drinking water sources. Organic content of source water was extracted with XAD-2 resin column and organic solvents. Four doses of the extract equivalent to 0.25, 0.5, 1 and 2L of source water were tested for toxicity. All the water samples were collected from six different locations in Guangdong province. The results of the Ames test and SOS/umu test showed that all the organic extracts from the water samples could induce different levels of DNA damage and mutagenic potentials at the dose of 2 L in the absence of S9 mix, which demonstrated the existence of genotoxicity and mutagenicity. Additionally, we found that Salmonella typhimurium strain TA98 was more sensitive for the mutagen. Correlation analysis between genotoxicity, Organochlorine Pesticides (OCPs) and Polycyclic Aromatic Hydrocarbons (PAHs) showed that most individual OCPs were frame shift toxicants in drinking water sources, and there was no correlation with total OCPs and PAHs. PMID:28125725

  19. Evidence for major input of riverine organic matter into the ocean

    USGS Publications Warehouse

    Cao, Xiaoyan; Aiken, George R.; Butler, Kenna D.; Huntington, Thomas G.; Balch, William M.; Mao, Jingdong; Schmidt-Rohr, Klaus

    2018-01-01

    The changes in the structure of XAD-8 isolated dissolved organic matter (DOM) samples along a river (Penobscot River) to estuary (Penobscot Bay) to ocean (across the Gulf of Maine) transect and from the Pacific Ocean were investigated using selective and two dimensional (2D) nuclear magnetic resonance (NMR) spectroscopy coupled with elemental and carbon isotope analysis. The results provide important insights into the nature of relatively stable structures in the river-to-ocean continuum and the enigma of the fate of terrestrial DOM in the marine system. First, lignin and carboxyl-rich alicyclic molecules (CRAMs), which are indistinguishable from mass spectrometry, were clearly differentiated with NMR spectroscopy. NMR unambiguously showed that CRAMs persisted along the river-to-ocean transect and in the Pacific Ocean, while lignin residues dramatically decreased in abundance from the river to the coastal ocean and the Pacific Ocean. The results challenge a previous conclusion that lignin-derived compounds are refractory and can accumulate in the coastal ocean. The loss of terrestrial plant-derived aromatic compounds such as lignin and tannin residues throughout the sequence of riverine, coastal, and open ocean DOM extracts could also partially explain the decreasing organic carbon recovery by XAD-8 isolation and the change in carbon stable isotope composition from riverine DOM (δ13C −27.6‰) to ocean DOM (δ13C −23.0‰) extracts. The observation, from advanced NMR, of similar CRAM molecules in XAD-8 isolated DOM samples from the Penobscot River to the Penobscot Bay and from the ocean refutes a previous conclusion that XAD-isolated DOM samples from seawater and river are distinctly different. The alicyclic structural features of CRAMs and their presence as the major structural units in DOM extracts from the Penobscot River to Gulf of Maine transect, together with the deduced old 14C age of CRAMs in the ocean, imply that terrestrial CRAMs may persist on timescales long enough to be transported into the ocean.

  20. Perchlorate adsorption and desorption on activated carbon and anion exchange resin.

    PubMed

    Yoon, In-Ho; Meng, Xiaoguang; Wang, Chao; Kim, Kyoung-Woong; Bang, Sunbaek; Choe, Eunyoung; Lippincott, Lee

    2009-05-15

    The mechanisms of perchlorate adsorption on activated carbon (AC) and anion exchange resin (SR-7 resin) were investigated using Raman, FTIR, and zeta potential analyses. Batch adsorption and desorption results demonstrated that the adsorption of perchlorate by AC and SR-7 resin was reversible. The reversibility of perchlorate adsorption by the resin was also proved by column regeneration test. Solution pH significantly affected perchlorate adsorption and the zeta potential of AC, while it did not influence perchlorate adsorption and the zeta potential of resin. Zeta potential measurements showed that perchlorate was adsorbed on the negatively charged AC surface. Raman spectra indicated the adsorption resulted in an obvious position shift of the perchlorate peak, suggesting that perchlorate was associated with functional groups on AC at neutral pH through interactions stronger than electrostatic interaction. The adsorbed perchlorate on the resin exhibited a Raman peak at similar position as the aqueous perchlorate, indicating that perchlorate was adsorbed on the resin through electrostatic attraction between the anion and positively charged surface sites.

  1. Phosphorus recovery as struvite from eutropic waters by XDA-7 resin.

    PubMed

    Li, Huanwen; Ye, Zhiping; Lin, Ying; Wang, Fengying

    2012-01-01

    Phosphorus releases into aquatic environment and its subsequent contribution to eutrophication have resulted in a widespread global pollution issue. However, phosphorus is a non-renewable source. The potential supplies of phosphorus are decreasing worldwide. Therefore, removal and recovery of phosphorus from the eutropic waters is important, emergent and necessary. In this research, experiments for recovering phosphate from eutropic waters by anion exchange combined with struvite precipitation were conducted. The results indicated that the prepared XDA-7 resin was an effective adsorbent for phosphate. The adsorption isotherm of XDA-7 resin was found to be a modified Freundlich type. The maximum phosphate adsorption (20.9 mg/g) occurred in the pH range of 6.0-8.0. Phosphate adsorbed on the XDA-7 resin was effectively desorbed with 8% NaCl solution, and the resin was able to be regenerated with 3% NaClO and 4% NaOH solutions. Phosphate desorbed from the resin was recovered as magnesium ammonium phosphate (struvite). The obtained struvite was analyzed by acid dissolution method, scanning electron microscope (SEM) and Fourier transform infrared spectroscopy (FTIR). The struvite precipitate was found to be 75.8% in purity, a high-value fertilizer.

  2. Microhardness of light- and dual-polymerizable luting resins polymerized through 7.5-mm-thick endocrowns.

    PubMed

    Gregor, Ladislav; Bouillaguet, Serge; Onisor, Ioana; Ardu, Stefano; Krejci, Ivo; Rocca, Giovanni Tommaso

    2014-10-01

    The complete polymerization of luting resins through thick indirect restorations is still questioned. The purpose of this study was to evaluate the degree of polymerization of light- and dual-polymerizable luting resins under thick indirect composite resin and ceramic endocrowns by means of Vickers microhardness measurements. The Vickers microhardness measurements of a light-polymerizable microhybrid composite resin and a dual-polymerizable luting cement directly polymerized in a natural tooth mold for 40 seconds with a high-power light-emitting diode lamp (control) were compared with measurements after indirect irradiation through 7.5-mm-thick composite resin and ceramic endocrowns for 3 × 90 seconds. A test-to-control microhardness values ratio of 0.80 at a depth of 0.5 mm below the surface was assumed as the criterion for adequate conversion. For the Vickers microhardness measurements of a dual-polymerizable luting cement, no differences (P>.05) were found between Vickers microhardness control values and values reported after polymerization through composite resin and ceramic endocrowns. For The Vickers microhardness measurements (±SD) of a light-polymerizable microhybrid composite resin, control values were significantly (P<.05) higher (111 ±3.3) than those reported after polymerization through composite resin (100.5 ±3.8) and ceramic (99.7 ±2.3) endocrowns. However, the hardness values of The Vickers microhardness measurements of a light-polymerizable microhybrid composite resin polymerized through the endocrowns were approximately 10% to 12% lower than those of the control values. Two-way ANOVA showed the influence of the luting material on the Vickers microhardness values (P<.05). The effect of endocrown material was not significant (P>.05). Under the conditions of this in vitro study, Vickers microhardness values of the dual-polymerizable resin cement and the light-polymerizable restorative composite resin irradiated for 3 × 90 seconds with a high irradiance light-emitting diode lamp through 7.5-mm-thick endocrowns reached at least 80% of the control Vickers microhardness values, which means that both materials can be adequately polymerized when they are used for luting thick indirect restorations. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  3. Scintigraphic measurement of regional gut transit in idiopathic constipation

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Stivland, T.; Camilleri, M.; Vassallo, M.

    1991-07-01

    In this study, total gut transit and regional colonic transit in patients with idiopathic constipation were measured scintigraphically. Eight patients with severe constipation were studied, none of whom had evidence of abnormal function of the pelvic floor. 99mTc-radiolabeled Amberlite resin particles with a mixed meal were used to assess gastric emptying and small bowel transit; similar particles labeled with 111In were ingested in a coated capsule that dispersed in the ileocecal region. These were used to quantify colonic transit. Five healthy volunteers were also studied. Two patients showed delayed gastric emptying and two had slow small bowel transit. Seven ofmore » the eight patients had slow colonic transit. In five, delay affected the whole colon (pancolonic inertia); in two, transit in the ascending and transverse colon was normal, but solids moved through the left colon slowly. Mean colonic transit was also measured using radiopaque markers; this technique identified the patients with slow transit, as shown by measurements of overall colonic transit by simultaneous scintigraphy. However, estimated transit through the ascending and transverse colons was considerably shorter by the radiopaque marker technique. In conclusion, idiopathic constipation is characterized by either exaggerated reservoir functions of the ascending and transverse colons and/or impairment of propulsive function in the descending colon. Particle size may influence the result of regional colonic transit tests. Transit delays in other parts of the gut suggest that, in some patients, the condition may be a more generalized motor dysfunction.« less

  4. 21 CFR 177.2450 - Polyamide-imide resins.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ...) For the purpose of this section the polyamide-imide resins are derived from the condensation reaction...) The polyamide-imide resins (CAS Reg. No. 31957-38-7) derived from the condensation reaction of...

  5. 21 CFR 177.2450 - Polyamide-imide resins.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ...) For the purpose of this section the polyamide-imide resins are derived from the condensation reaction...) The polyamide-imide resins (CAS Reg. No. 31957-38-7) derived from the condensation reaction of...

  6. Comparison of stabilities in translucency, fluorescence and opalescence of direct and indirect composite resins.

    PubMed

    Yu, Bin; Lee, Young-Keun

    2013-01-01

    To evaluate translucency, fluorescence and opalescence stabilities of direct and indirect composite resins after aging. One direct (16 shades) and two indirect composite resins (16 and 26 shades) were investigated. Resins were filled in a mold (1 mm thick) and light cured; post-curings were performed for indirect resins. Color was measured before and after 5,000 cycles of thermocycling on a reflection spectrophotometer in reflectance and transmittance modes to calculate parameters for translucency (TP), fluorescence (FL) and opalescence (OP). Differences in the changes of TP, FL and OP after aging by the type of resin were determined by t test, and those were also determined by one-way ANOVA with the factor of the brand or the shade group (P < 0.05). Changes in TP, FL and OP were -1.2 to 0.7, -0.2 to 0.4 and -0.6 to 1.3, respectively, for direct resins; and were -2.0 to 1.8, -0.9 to 0.4 and -2.9 to 3.7, respectively, for indirect resins. Changes in TP were not significantly different by the type of resin, but those in FL and OP were different (P = 0.05). Changes in optical parameters were influenced by the brand or the shade group of the resins (P < 0.05). Stabilities in optical properties of resins varied depending on type, brand or shade group. Aging significantly affected fluorescence and opalescence, but not translucency, of indirect resins compared to those of direct resins.

  7. Assessment of the bioavailability and phytotoxicity of sediment spiked with polycyclic aromatic hydrocarbons.

    PubMed

    Rončević, Srđan; Spasojević, Jelena; Maletić, Snežana; Jazić, Jelena Molnar; Isakovski, Marijana Kragulj; Agbaba, Jasmina; Grgić, Marko; Dalmacija, Božo

    2016-02-01

    Large amounts of sediment are dredged globally every year. This sediment is often contaminated with low concentrations of metals, polycyclic aromatic hydrocarbons, pesticides and other organic pollutants. Some of this sediment is disposed of on land, creating a need for risk assessment of the sediment disposal method, to minimize the degradation of environmental quality and prevent risks to human health. Evaluating the available fractions of certain polycyclic aromatic hydrocarbons is very important, as in the presence of various organisms, they are believed to be easily subject to the processes of bioaccumulation, biosorption and transformation. In order to determine the applicability of applying these methods for the evaluation of pollutant bioavailability in sediments, the desorption kinetics from the sediment of various polycyclic aromatic hydrocarbons in the presence of Tenax and XAD4 were examined over the course of 216 h. Changes in the PAH concentrations in dredged sediments using five different seed plants during a short time of period (10 days) were also followed. Using chemical extraction techniques with Tenax and XAD4, a time of around 24 h is enough to achieve equilibrium for all four PAHs. Results showed good agreement between the seed accumulation and PAH extraction methods with both agents. If we compare the two extraction techniques, XAD4 gave better results for phenanthrene, pyrene and benzo(a)pyrene, and Tenax gave better results for chrysene.

  8. Chemical characterization of fractions of dissolved humic substances from a marginal sea—a case from the Southern Yellow Sea

    NASA Astrophysics Data System (ADS)

    Zhang, Yaoling; Yang, Keli; Du, Jinzhou; Zhang, Fenfen; Dong, Yaping; Li, Wu

    2018-03-01

    Marine dissolved organic matter (DOM) is one of the largest dynamic pools of organic carbon in the global carbon cycle, yet DOM is still chemically poorly characterized. To better understand the origin, composition, and cycling of DOM in the China marginal sea, dissolved humic substances (DHS) were isolated from seawaters in two locations in the Southern Yellow Sea. The DHS were subdivided into fulvic acids (FAs), humic acids (HAs) and the XAD-4 fractions. Complementary analytical approaches were used to characterize the isolated DHS samples including stable carbon isotopic composition, Fourier transform infrared spectroscopy (FTIR), 13C cross polarization magic angle spinning (CP/MAS) nuclear magnetic resonance (NMR), and pyrolysis gas chromatography-mass spectrometry (Py-GC/MS). The results demonstrated that both DHS samples encountered the influences from marine source, indicating that algal and microbial-derived materials are the predominant precursors for the studied samples. The three fractions of DHS showed different properties. FAs presented more aromatic features, whereas HAs contained more aliphatic lipids and proteinaceous materials. The XAD-4 fractions were enriched in 13C and contained more carbohydrates but less aromatic compounds. The lower molecular weight and higher heteroatom content and number of carboxyl groups for the XAD-4 fractions may give them considerable geochemical significance for aspects of trace metal species, bioavailability of pollutants, mineral weathering and water acidification in marine environments.

  9. Order of functionality loss during photodegradation of aquatic humic substances

    USGS Publications Warehouse

    Thorn, Kevin A.; Younger, Steven J.; Cox, Larry G.

    2009-01-01

    The time course photodegradation of the Nordic aquatic fulvic and humic acids and Suwannee River XAD-4 acids subjected to UV irradiation with an unfiltered medium pressure mercury lamp was studied by liquid-state 13C nuclear magnetic resonance. Photodecarboxylation was a significant pathway in all cases. Decreases in ketone, aromatic, and O-alkyl carbons were observed throughout the course of the irradiations, whereas C-alkyl carbons resisted photodegradation. Peaks attributable to the low-molecular-weight photodegradation products bicarbonate, formate, acetate, and succinate grew in intensity with irradiation time. The final products of the irradiations were decarboxylated, hydrophobic, predominantly C-alkyl and O-alkyl materials that were resistant to further photodegradation. The total amount of carbon susceptible to loss appeared to be related mainly to the total concentration of carbonyl and aromatic carbons and partly to the concentration of O-alkyl carbons in the fulvic, humic, and XAD-4 acids. The carbon losses for Nordic fulvic, Nordic Humic, Suwannee fulvic, and Suwannee XAD-4 acids were estimated to be 75, 63, 56, and 17%, respectively. More detailed analyses of the effects of irradiation on the carbonyl functionality in Nordic humic acid and Laurentian soil fulvic acid through reaction with hydroxylamine in conjunction with 15N nuclear magnetic resonance analysis confirmed preferential photodegradation of the quinone/hydroquinone functionality over ketone groups and the loss of ester groups in Laurentian fulvic acid.

  10. Mechanical and anticorrosive properties of graphene/epoxy resin composites coating prepared by in-situ method.

    PubMed

    Zhang, Zhiyi; Zhang, Wenhui; Li, Diansen; Sun, Youyi; Wang, Zhuo; Hou, Chunling; Chen, Lu; Cao, Yang; Liu, Yaqing

    2015-01-20

    The graphene nanosheets-based epoxy resin coating (0, 0.1, 0.4 and 0.7 wt %) was prepared by a situ-synthesis method. The effect of polyvinylpyrrolidone/reduced graphene oxide (PVP-rGO) on mechanical and thermal properties of epoxy resin coating was investigated using nanoindentation technique and thermogravimetric analysis, respectively. A significant enhancement (ca. 213% and 73 °C) in the Young modulus and thermal stability of epoxy resin coating was obtained at a loading of 0.7 wt %, respectively. Furthermore, the erosion resistance of graphene nanosheets-based epoxy resin coating was investigated by electrochemical measurement. The results showed also that the Rrcco (ca. 0.3 mm/year) of graphene nanosheets-based epoxy resin coating was far lower than neat epoxy resin (1.3 mm/year). Thus, this approach provides a novel route for improving erosion resistance and mechanical-thermal stability of polymers coating, which is expected to be used in mechanical-thermal-corrosion coupling environments.

  11. Mechanical and Anticorrosive Properties of Graphene/Epoxy Resin Composites Coating Prepared by in-Situ Method

    PubMed Central

    Zhang, Zhiyi; Zhang, Wenhui; Li, Diansen; Sun, Youyi; Wang, Zhuo; Hou, Chunling; Chen, Lu; Cao, Yang; Liu, Yaqing

    2015-01-01

    The graphene nanosheets-based epoxy resin coating (0, 0.1, 0.4 and 0.7 wt %) was prepared by a situ-synthesis method. The effect of polyvinylpyrrolidone/reduced graphene oxide (PVP-rGO) on mechanical and thermal properties of epoxy resin coating was investigated using nanoindentation technique and thermogravimetric analysis, respectively. A significant enhancement (ca. 213% and 73 °C) in the Young modulus and thermal stability of epoxy resin coating was obtained at a loading of 0.7 wt %, respectively. Furthermore, the erosion resistance of graphene nanosheets-based epoxy resin coating was investigated by electrochemical measurement. The results showed also that the Rrcco (ca. 0.3 mm/year) of graphene nanosheets-based epoxy resin coating was far lower than neat epoxy resin (1.3 mm/year). Thus, this approach provides a novel route for improving erosion resistance and mechanical-thermal stability of polymers coating, which is expected to be used in mechanical-thermal-corrosion coupling environments. PMID:25608656

  12. Microhardness of dual-polymerizing resin cements and foundation composite resins for luting fiber-reinforced posts.

    PubMed

    Yoshida, Keiichi; Meng, Xiangfeng

    2014-06-01

    The optimal luting material for fiber-reinforced posts to ensure the longevity of foundation restorations remains undetermined. The purpose of this study was to evaluate the suitability of 3 dual-polymerizing resin cements and 2 dual-polymerizing foundation composite resins for luting fiber-reinforced posts by assessing their Knoop hardness number. Five specimens of dual-polymerizing resin cements (SA Cement Automix, G-Cem LincAce, and Panavia F2.0) and 5 specimens of dual-polymerizing foundation composite resins (Clearfil DC Core Plus and Unifil Core EM) were polymerized from the top by irradiation for 40 seconds. Knoop hardness numbers were measured at depths of 0.5, 2.0, 4.0, 6.0, 8.0, and 10.0 mm at 0.5 hours and 7 days after irradiation. Data were statistically analyzed by repeated measures ANOVA, 1-way ANOVA, and the Tukey compromise post hoc test (α=.05). At both times after irradiation, the 5 resins materials showed the highest Knoop hardness numbers at the 0.5-mm depth. At 7 days after irradiation, the Knoop hardness numbers of the resin materials did not differ significantly between the 8.0-mm and 10.0-mm depths (P>.05). For all materials, the Knoop hardness numbers at 7 days after irradiation were significantly higher than those at 0.5 hours after irradiation at all depths (P<.05). At 7 days after irradiation, the Knoop hardness numbers of the 5 resin materials were found to decrease in the following order: DC Core Plus, Unifil Core EM, Panavia F2.0, SA Cement Automix, and G-Cem LincAce (P<.05). The Knoop hardness number depends on the depth of the cavity, the length of time after irradiation, and the material brand. Although the Knoop hardness numbers of the 2 dual-polymerizing foundation composite resins were higher than those of the 3 dual-polymerizing resin cements, notable differences were seen among the 5 materials at all depths and at both times after irradiation. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  13. Waterborne Polymeric Films.

    DTIC Science & Technology

    1979-12-01

    resin types: 1) acrylic latex, 2) acrylic solution polymer, 3) epoxy emulsions, 4) polyurethane, 5) butadiene elastomeric latex, 6) polyester/ alkyd , 7...emulsions and the class of polyester/ alkyd resins were evaluated only as network, crosslinked films. -53- j z I, ACRYLIC SOLUTIONLATEX URE THANE ACRYLIC ...amount of "plasticizing" monomer such as ethyl acrylate . 2.3.1.3 Aqueous Polyester Alkyd Resins As indicated in section 2.2.7 of this report,

  14. Tensile bond strength of indirect composites luted with three new self-adhesive resin cements to dentin.

    PubMed

    Türkmen, Cafer; Durkan, Meral; Cimilli, Hale; Öksüz, Mustafa

    2011-08-01

    The aims of this study were to evaluate the tensile bond strengths between indirect composites and dentin of 3 recently developed self-adhesive resin cements and to determine mode of failure by SEM. Exposed dentin surfaces of 70 mandibular third molars were used. Teeth were randomly divided into 7 groups: Group 1 (control group): direct composite resin restoration (Alert) with etch-and-rinse adhesive system (Bond 1 primer/adhesive), Group 2: indirect composite restoration (Estenia) luted with a resin cement (Cement-It) combined with the same etch-and-rinse adhesive, Group 3: direct composite resin restoration with self-etch adhesive system (Nano-Bond), Group 4: indirect composite restoration luted with the resin cement combined with the same self-etch adhesive, Groups 5-7: indirect composite restoration luted with self-adhesive resin cements (RelyX Unicem, Maxcem, and Embrace WetBond, respectively) onto the non-pretreated dentin surfaces. Tensile bond strengths of groups were tested with a universal testing machine at a constant speed of 1 mm/min using a 50 kgf load cell. Results were statistically analyzed by the Student's t-test. The failure modes of all groups were also evaluated. The indirect composite restorations luted with the self-adhesive resin cements (groups 5-7) showed better results compared to the other groups (p<0.05). Group 4 showed the weakest bond strength (p>0.05). The surfaces of all debonded specimens showed evidence of both adhesive and cohesive failure. The new universal self-adhesive resins may be considered an alternative for luting indirect composite restorations onto non-pretreated dentin surfaces.

  15. The effect of long-term disinfection procedures on hardness property of resin denture teeth.

    PubMed

    Campanha, Nara Hellen; Pavarina, Ana Cláudia; Jorge, Janaina Habib; Vergani, Carlos Eduardo; Machado, Ana Lucia; Giampaolo, Eunice Teresinha

    2012-06-01

    The aim of the study was to evaluate the effect of long-term disinfection procedures on the Vickers hardness (VHN) of acrylic resin denture teeth. Five acrylic resin denture teeth (Vipi Dent Plus-V, Trilux-T, Biolux-B, Postaris-P and Artiplus-A) and one composite resin denture teeth (SR-Orthosit-O) were embedded in heat-polymerised acrylic resin within polyvinylchloride tubes. Specimens were stored in distilled water at 37°C for 48 h. Measurements of hardness were taken after the following disinfection procedures: immersion for 7 days in 4% chlorhexidine gluconate or in 1% sodium hypochlorite (CIm and HIm group, respectively) and seven daily cycles of microwave sterilisation at 650 W for 6 min (MwS group). In the WIm group, specimens were maintained in water during the time used to perform the disinfection procedures (7 days). Data were analysed with anova followed by the Bonferroni procedure (α = 0.01). Microwave disinfection decreased the hardness of all acrylic resin denture teeth (p < 0.001). Immersion for 7 days in 4% chlorhexidine gluconate or distilled water had significant effect on the hardness of the acrylic resin denture teeth A (p < 0.01), and 1% sodium hypochlorite on teeth T (p < 0.01). All disinfection procedures decrease the hardness of the composite resin denture teeth (p < 0.01). Teeth O exhibited the highest and teeth V the lowest hardness values in the control group (p < 0.01). Disinfection procedures changed the hardness of resin denture teeth. © 2011 The Gerodontology Society and John Wiley & Sons A/S.

  16. Simultaneous Isolation of Lactoferrin and Lactoperoxidase from Bovine Colostrum by SPEC 70 SLS Cation Exchange Resin

    PubMed Central

    Liang, Yafei; Wang, Xuewan; Wu, Mianbin; Zhu, Wanping

    2011-01-01

    In this work, simultaneous isolation of lactoferrin (Lf) and lactoperoxidase (Lp) from defatted bovine colostrum by one-step cation exchange chromatography with SPEC 70 SLS ion-exchange resin was investigated. A RP-HPLC method for Lf and Lp determination was developed and optimized as the following conditions: detection wavelength of 220 nm, flow rate of 1 mL/min and acetonitrile concentration from 25% to 75% within 20 min. The adsorption process of Lf on SPEC 70 SLS resin was optimized using Lf standard as substrate. The maximum static binding capacity of SPEC 70 SLS resin was of 22.0 mg/g resin at 15 °C, pH 7.0 and adsorption time 3 h. The Lf adsorption process could be well described by the Langmuir adsorption isotherm model, with a maximum adsorption capacity of 21.73 mg/g resin at 15 °C. In batch fractionation of defatted colostrum, the binding capacities of SPEC 70 SLS resin for adsorbing Lf and Lp simultaneously under the abovementioned conditions were 7.60 and 6.89 mg/g resin, respectively, both of which were superior to those of CM Sepharose F.F. or SP Sepharose F.F. resins under the same conditions. As a result, SPEC 70 SLS resin was considered as a successful candidate for direct and economic purification of Lf and Lp from defatted colostrum. PMID:22016715

  17. Dielectric characterization of TiO2, Al2O3 - Nanoparticle loaded epoxy resin

    NASA Astrophysics Data System (ADS)

    Thakor, S. G.; Rana, V. A.; Vankar, H. P.

    2018-05-01

    In present work, the dielectric properties of two different nanoparticle loaded Bisphenol A-epoxy resin were carried out at room temperature. Sample of the neat epoxy resin and nanoparticle loaded epoxy resin in the form of disc were prepared of different weight fraction (i.e 0.5 wt%,0.7 wt%,1 wt%,1.5 wt%,1.7 wt%,2 wt%). TiO2 and Al2O3 nanoparticles were taken as filler in the epoxy resin. Complex permittivity of the prepared samples was measured using Agilent E4980A precision LCR meter in frequency range of 103 Hz to 106 Hz. The dependency of dielectric behavior on type and concentration of nanoparticle in considered frequency range are discussed in detail.

  18. Mutagenic activity associated with by-products of drinking water disinfection by chlorine, chlorine dioxide, ozone and UV-irradiation.

    PubMed Central

    Zoeteman, B C; Hrubec, J; de Greef, E; Kool, H J

    1982-01-01

    A retrospective epidemiological study in The Netherlands showed a statistical association between chlorination by-products in drinking water and cancer of the esophagus and stomach for males. A pilot-plant study with alternative disinfectants was carried out with stored water of the Rivers Rhine and Meuse. It was demonstrated that the increase of direct acting mutagens after treatment with chlorine dioxide is similar to the effect of chlorination. Ozonation of Rhine water reduced the mutagenic activity for Salmonella typhimurium TA 98 both with and without metabolic activation. UV alone hardly affects the mutagenicity of the stored river water for S. typh. TA 98. In all studies, practically no mutagenic activity for S. typh. TA 100 was found. Although remarkable changes in the concentration of individual organic compounds are reported, the identity of the mutagens detected is yet unclear. Compounds of possible interest due to their removal by ozonation are 1,3,3-trimethyloxindole, dicyclopentadiene and several alkylquinolines. Compounds which might be responsible for the increased mutagenicity after chlorination are two brominated acetonitriles and tri(2-chlorethyl) phosphate. Furthermore, the concentration procedure with adsorption on XAD resin and the subsequent elution step may have affected the results. It is proposed to focus further research more on the less volatile by-products of disinfection than on the trihalomethanes. PMID:7151762

  19. Mutagenicity studies in a tyre plant: in vitro activity of workers' urinary concentrates and raw materials.

    PubMed

    Crebelli, R; Paoletti, A; Falcone, E; Aquilina, G; Fabri, G; Carere, A

    1985-07-01

    The possible contribution to urinary mutagenicity of occupational exposures in the rubber industry was studied by assaying the urine concentrates of 72 workmen (44 smokers) employed in a tyre plant. Twenty three clerks (16 smokers) engaged in the administrative department of the same factory served as presumptive unexposed controls. XAD-2 resin concentrates of urine samples were assayed in the plate incorporation test and in the microtitre fluctuation assay with Salmonella typhimurium strains TA1535, TA98, and TA100. Furthermore, the in vitro mutagenicity of the major raw materials in use at the plant was determined in the plate incorporation assay with S typhimurium strains TA1535, TA1537, TA98, and TA100. The results obtained from the urinary mutagenicity study show that smoking habits, but not occupation, were statistically significantly related to the appearance of a urinary mutagenicity that was detectable with strain TA98. A possible synergistic effect of occupation with smoking was observed among tyre builders who were also smokers. The study of the raw materials showed that three technical grade materials were weakly active as mutagens in strain TA98 in the absence (poly-p-dinitrosobenzene) or in the presence of metabolic activation (mixed diaryl-p-phenylendiamines and tetramethyltiuram disulphide). The latter chemical was also weakly active in strain TA100.

  20. Mutagenicity studies in a tyre plant: in vitro activity of workers' urinary concentrates and raw materials.

    PubMed Central

    Crebelli, R; Paoletti, A; Falcone, E; Aquilina, G; Fabri, G; Carere, A

    1985-01-01

    The possible contribution to urinary mutagenicity of occupational exposures in the rubber industry was studied by assaying the urine concentrates of 72 workmen (44 smokers) employed in a tyre plant. Twenty three clerks (16 smokers) engaged in the administrative department of the same factory served as presumptive unexposed controls. XAD-2 resin concentrates of urine samples were assayed in the plate incorporation test and in the microtitre fluctuation assay with Salmonella typhimurium strains TA1535, TA98, and TA100. Furthermore, the in vitro mutagenicity of the major raw materials in use at the plant was determined in the plate incorporation assay with S typhimurium strains TA1535, TA1537, TA98, and TA100. The results obtained from the urinary mutagenicity study show that smoking habits, but not occupation, were statistically significantly related to the appearance of a urinary mutagenicity that was detectable with strain TA98. A possible synergistic effect of occupation with smoking was observed among tyre builders who were also smokers. The study of the raw materials showed that three technical grade materials were weakly active as mutagens in strain TA98 in the absence (poly-p-dinitrosobenzene) or in the presence of metabolic activation (mixed diaryl-p-phenylendiamines and tetramethyltiuram disulphide). The latter chemical was also weakly active in strain TA100. PMID:4015996

  1. Uncertainty Estimation for the Determination of Ni, Pb and Al in Natural Water Samples by SPE-ICP-OES

    NASA Astrophysics Data System (ADS)

    Ghorbani, A.; Farahani, M. Mahmoodi; Rabbani, M.; Aflaki, F.; Waqifhosain, Syed

    2008-01-01

    In this paper we propose uncertainty estimation for the analytical results we obtained from determination of Ni, Pb and Al by solidphase extraction and inductively coupled plasma optical emission spectrometry (SPE-ICP-OES). The procedure is based on the retention of analytes in the form of 8-hydroxyquinoline (8-HQ) complexes on a mini column of XAD-4 resin and subsequent elution with nitric acid. The influence of various analytical parameters including the amount of solid phase, pH, elution factors (concentration and volume of eluting solution), volume of sample solution, and amount of ligand on the extraction efficiency of analytes was investigated. To estimate the uncertainty of analytical result obtained, we propose assessing trueness by employing spiked sample. Two types of bias are calculated in the assessment of trueness: a proportional bias and a constant bias. We applied Nested design for calculating proportional bias and Youden method to calculate the constant bias. The results we obtained for proportional bias are calculated from spiked samples. In this case, the concentration found is plotted against the concentration added and the slop of standard addition curve is an estimate of the method recovery. Estimated method of average recovery in Karaj river water is: (1.004±0.0085) for Ni, (0.999±0.010) for Pb and (0.987±0.008) for Al.

  2. Sampling and analysis of quaternary ammonium compounds (QACs) traces in indoor atmosphere.

    PubMed

    Vincent, Guillaume; Kopferschmitt-Kubler, Marie Christine; Mirabel, Philippe; Pauli, Gabrielle; Millet, Maurice

    2007-10-01

    Quaternary Ammonium Compounds (QACs) are widely found in disinfectants used in hospitals. Benzalkonium chloride (BAC) and didecyldimethylammonium chloride (DDAC) predominate in the disinfecting formulations. These compounds are strong irritants and can play a role in the induction of Occupational Asthma among the professionals of health and cleaning. In order to evaluate the potential health effect of these quaternary ammonium compounds to hospital employers, the development of an analytical method for their quantification in indoor air was developed. DDAC aerosols are trapped by adsorption on XAD-2 resin SKC tube. The air in hospital buildings was sampled using a constant debit Gillian pump at a flow of 1.0 l/min (+/-5%). Ion Chromatography (IC) was chosen for the analysis of DDAC especially for its high sensitivity and specificity. The Limit of Detection (LOD) by IC for DDAC is 0.56 mug/ml. Therefore the LOD of atmospheric DDAC is 28 microg/m(3) with an air volume of 100 l and a desorption volume of 5 ml. All DDAC air samples were lower than the LOD of the analytical method by IC. Under the standard conditions of use of the disinfecting solutions (Surfanios, Ampholysine Plus and Amphospray 41), the insignificant volatility of DDAC would not seem to be able to contaminate the indoor hospital atmosphere during the disinfection process. However, the DDAC can contaminate working atmospheres if it is put in suspension by aerosolisation.

  3. Evolution of nitrogen species in landfill leachates under various stabilization states.

    PubMed

    Zhao, Renzun; Gupta, Abhinav; Novak, John T; Goldsmith, C Douglas

    2017-11-01

    In this study, nitrogen species in landfill leachates under various stabilization states were investigated with emphasis on organic nitrogen. Ammonium nitrogen was found to be approximately 1300mg/L in leachates from younger landfill units (less than 10years old), and approximately 500mg/L in leachates from older landfill units (up to 30years old). The concentration and aerobic biodegradability of organic nitrogen decreased with landfill age. A size distribution study showed that most organic nitrogen in landfill leachates is <1kDa. The Lowry protein concentration (mg/L-N) was analyzed and showed a strong correlation with the total organic nitrogen (TON, mg/L-N, R 2 =0.88 and 0.98 for untreated and treated samples, respectively). The slopes of the regression curves of untreated (protein=0.45TON) and treated (protein=0.31TON) leachates indicated that the protein is more biodegradable than the other organic nitrogen species in landfill leachates. XAD-8 resin was employed to isolate the hydrophilic fraction of leachate samples, and it was found that the hydrophilic fraction proportion in terms of organic nitrogen decreased with landfill age. Solid-state 15 N nuclear magnetic resonance (NMR) was utilized to identify the nitrogen species. Proteinaceous materials were found to be readily biodegradable, while heterocyclic nitrogen species were found to be resistant to biodegradation. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Copper resinate: preparation, characterisation and study of degradation.

    PubMed

    Colombini, M P; Lanterna, G; Mairani, A; Matteini, M; Modugno, F; Rizzi, M

    2001-01-01

    This paper describes a method for the synthesis of Copper Resinate, which disappeared from artists' palettes in the eighteenth century. This was carried out by interpreting ancient recipes following a scientific approach. Its characterisation using Fourier Transform-Infrared Spectrometry and Gas Chromatography-Mass Spectrometry demonstrated that it is a mixture containing copper and oxidised abietic acids, mainly dehydroabietic and 7-oxo-dehydroabietic acids, formed during the preparation of the pigment and the curing of the paint layer. The composition of copper resinate paint layers, artificially aged by U.V. irradiation at 365 nm (UV), heating (T), and exposed to atmospheric pollutants (NOX) in a climatic chamber, was investigated. The combination of irradiation and temperature produced a change in colour along with a significant increase in the recovered amount of 7-oxo-dehydroabietic acid. The identification of copper resinate in a sample from an old painting should be related to the presence of the following resin compounds which are stable in the ageing process: dehydroabietic and 7-oxo-dehydroabietic acid pimaradienic acids. Photo-oxidation of the resin acids co-ordinated with copper seem to be the most probable decay mechanism responsible for the colour change in the pigment.

  5. Differential effects of DEAE negative mode chromatography and gel-filtration chromatography on the charge status of Helicobacter pylori neutrophil-activating protein

    PubMed Central

    Pan, Timothy; Tzeng, Huey-Fen

    2017-01-01

    Helicobacter pylori neutrophil-activating protein (HP-NAP) is involved in H. pylori-associated gastric inflammation. HP-NAP is also a vaccine candidate, a possible drug target, and a potential diagnostic marker for H. pylori-associated diseases. Previously, we purified recombinant HP-NAP by one-step diethylaminoethyl (DEAE) negative mode chromatography by collecting the unbound fraction at pH 8.0 at 4°C. It remains unclear why HP-NAP does not bind to DEAE resins at the pH above its isoelectric point during the purification. To investigate how pH affects the surface net charge of HP-NAP and its binding to DEAE resins during the purification, recombinant HP-NAP expressed in Escherichia coli was subjected to DEAE negative mode chromatography at pH ranging from 7.0 to 9.0 at 25°C and the surface charge of purified HP-NAP was determined by capillary electrophoresis. A minimal amount of HP-NAP was detected in the elution fraction of DEAE Sepharose resin at pH 8.5, whereas recombinant HP-NAP was detected in the elution fraction of DEAE Sephadex resin only at pH 7.0 and 8.0. The purified recombinant HP-NAP obtained from the unbound fractions was not able to bind to DEAE resins at pH 7.0 to 9.0. In addition, the surface charge of the purified HP-NAP was neutral at pH 7.0 to 8.0 and was either neutral or slightly negative at pH 8.5 and 9.0. However, recombinant HP-NAP purified from gel-filtration chromatography was able to bind to DEAE Sepharose resin at pH 7.0 to 9.0 and DEAE Sephadex resin at pH 7.0. At pH 8.5 and 9.0, only the negatively charged species of HP-NAP were found. Thus, recombinant HP-NAP with different charge status can be differentially purified by DEAE negative mode chromatography and gel-filtration chromatography. Furthermore, the charge distribution on the surface of HP-NAP, the presence of impure proteins, and the overall net charge of the resins all affect the binding of HP-NAP to DEAE resins during the negative purification. PMID:28328957

  6. Differential effects of DEAE negative mode chromatography and gel-filtration chromatography on the charge status of Helicobacter pylori neutrophil-activating protein.

    PubMed

    Hong, Zhi-Wei; Yang, Yu-Chi; Pan, Timothy; Tzeng, Huey-Fen; Fu, Hua-Wen

    2017-01-01

    Helicobacter pylori neutrophil-activating protein (HP-NAP) is involved in H. pylori-associated gastric inflammation. HP-NAP is also a vaccine candidate, a possible drug target, and a potential diagnostic marker for H. pylori-associated diseases. Previously, we purified recombinant HP-NAP by one-step diethylaminoethyl (DEAE) negative mode chromatography by collecting the unbound fraction at pH 8.0 at 4°C. It remains unclear why HP-NAP does not bind to DEAE resins at the pH above its isoelectric point during the purification. To investigate how pH affects the surface net charge of HP-NAP and its binding to DEAE resins during the purification, recombinant HP-NAP expressed in Escherichia coli was subjected to DEAE negative mode chromatography at pH ranging from 7.0 to 9.0 at 25°C and the surface charge of purified HP-NAP was determined by capillary electrophoresis. A minimal amount of HP-NAP was detected in the elution fraction of DEAE Sepharose resin at pH 8.5, whereas recombinant HP-NAP was detected in the elution fraction of DEAE Sephadex resin only at pH 7.0 and 8.0. The purified recombinant HP-NAP obtained from the unbound fractions was not able to bind to DEAE resins at pH 7.0 to 9.0. In addition, the surface charge of the purified HP-NAP was neutral at pH 7.0 to 8.0 and was either neutral or slightly negative at pH 8.5 and 9.0. However, recombinant HP-NAP purified from gel-filtration chromatography was able to bind to DEAE Sepharose resin at pH 7.0 to 9.0 and DEAE Sephadex resin at pH 7.0. At pH 8.5 and 9.0, only the negatively charged species of HP-NAP were found. Thus, recombinant HP-NAP with different charge status can be differentially purified by DEAE negative mode chromatography and gel-filtration chromatography. Furthermore, the charge distribution on the surface of HP-NAP, the presence of impure proteins, and the overall net charge of the resins all affect the binding of HP-NAP to DEAE resins during the negative purification.

  7. 40 CFR Appendix A to Subpart Ddd... - Free Formaldehyde Analysis of Insulation Resins by the Hydroxylamine Hydrochloride Method

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ..., readable to 0.01 g or better. 3.2pH meter, standardized to pH 4.0 with pH 4.0 buffer and pH 7 with pH 7.0... N sodium hydroxide solution. 4.2Hydroxylamine hydrochloride solution, 100 grams per liter, pH... stirrer. Confirm that the resin has dissolved. 5.4Adjust the resin/solvent solution to pH 4.0, using the...

  8. 40 CFR Appendix B to Subpart Nnn... - Free Formaldehyde Analysis of Insulation Resins by Hydroxylamine Hydrochloride

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 4.0 with pH 4.0 buffer and pH 7 with pH 7.0 buffer. 3.350-mL burette for 1.0 N sodium hydroxide. 3... hydrochloride solution, 100 grams per liter, pH adjusted to 4.00. 4.3Hydrochloric acid solution, 1.0 N and 0.1 N... magnetic stirrer. Confirm that the resin has dissolved. 5.4Adjust the resin/solvent solution to pH 4.0...

  9. 40 CFR Appendix B to Subpart Nnn... - Free Formaldehyde Analysis of Insulation Resins by Hydroxylamine Hydrochloride

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 4.0 with pH 4.0 buffer and pH 7 with pH 7.0 buffer. 3.350-mL burette for 1.0 N sodium hydroxide. 3... hydrochloride solution, 100 grams per liter, pH adjusted to 4.00. 4.3Hydrochloric acid solution, 1.0 N and 0.1 N... magnetic stirrer. Confirm that the resin has dissolved. 5.4Adjust the resin/solvent solution to pH 4.0...

  10. Combining physico-chemical analysis with a Daphnia magna bioassay to evaluate a recycling technology for drinking water treatment plant waste residuals.

    PubMed

    Chen, Ting; Xu, Yongpeng; Zhu, Shijun; Cui, Fuyi

    2015-12-01

    Recycling water treatment plant (WTP) waste residuals is considered to be a feasible method to enhance the efficiency of pollutant removal. This study also evaluated the safety and water quality of a pilot-DWTP waste residuals recycling technology by combining physical-chemistry analysis with a Daphnia magna assay. The water samples taken from each treatment step were extracted and concentrated by XAD-2 resin and were then analyzed for immobilization and enzyme activity with D. magna. The measured parameters, such as the dissolve organic carbon (DOC), UV254 and THM formation potential (THMFPs) of the recycling process, did not obviously increase over 15 days of continuous operation and were even lower than typical values from a conventional process. The extract concentration ranged from 0 to 2 Leq/ml as measured on the 7th and 15th days and the immobilization of D. magna exposed to water treated by the recycling process was nearly equivalent to that of the conventional process. Both the superoxide dismutase (SOD) and the catalase (CAT) activity assay indicated that a lower dose of water extract (0.5, 1, 1.5 Leq/ml) could stimulate the enzyme activity of D. magna, whereas a higher dose (2 Leq/ml at the sampling point C3, R3, R4 ) inhibits the activity. Moreover, the SOD and CAT activity of D. magna with DOC and UV254 showed a strong concentration-effect relationship, where the concentration range of DOC and UV254 were 4.1-16.2 mg/L and 0.071-4.382 cm(-1), respectively. The results showed that there was no statistically significant difference (p>0.05) between the conventional and recycling treatment processes and the toxicity of water samples in the recycling process did not increase during the 15-day continuous recycling trial. Copyright © 2015 Elsevier Inc. All rights reserved.

  11. Combinatory effects of temperature stress and nonionic organic pollutants on stress protein (hsp70) gene expression in the freshwater sponge Ephydatia fluviatilis

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Mueller, W.E.G.; Koziol, C.; Dapper, J.

    1995-07-01

    This is the first documentation of a heat shock protein (hsp) response in sponges. Subjecting the freshwater sponge Ephydatia fluviatilis to temperature stress (18 to 33 C; 2 h) resulted in an increased expression (>10 times) of the M{sub r}70,000 (hsp70). The induction of hsp70 could be demonstrated on the level of gene expression and by quantification of the hsp70 protein. Temperature stress also resulted in a 25% reduction of sponge cell proliferation. A mixture of nonionic organic compound was extracted from water from the polluted Schwarzbach River (S. Hesse, Germany) by adsorption onto XAD-7 resin. Concentrations of this Schwarzbachmore » River water extract at two and four items ambient levels resulted in decreases in cell proliferation by 53.6 and 99.4%, respectively. However, when cells were exposed to these levels of the Schwarzbach River water extract directly following a temperature stress (33 C for 2 h), cell proliferation was less affected by the extract than the absence of the temperature stress. In addition, the combination of temperature stress and exposure to the Schwarzbach River water extract resulted in higher levels of hsp70 than were observed for each stressor by itself. Northern and Western blotting as well as precipitation assay confirmed the interaction between heat treatment and exposure to different amounts of nonionic organic pollutants on the level of mRNA and protein expression of hsp70. From these data the authors conclude that a sublethal treatment of sponge with heat results in a higher tolerance of the animals to chemical stressors. These results are relevant to the real-world situation where organisms are often exposed simultaneously to a variety of stressors, in contrast to many laboratory exposures that aim to elucidate the effects of individual stressors.« less

  12. Preconcentration determination of arsenic species by sorption of As(V) on Amberlite IRA-410 coupled with fluorescence quenching of L-cysteine capped CdS nanoparticles.

    PubMed

    Hosseini, Mohammad Saeid; Nazemi, Sahar

    2013-10-07

    A simple and accurate method for arsenic speciation analysis in natural and drinking water samples is described in which preconcentration of arsenic as As(V) was coupled with spectrofluorometric determination. The extracted As(V) species with a column containing Amberlite IRA-410 were subjected to L-cysteine capped CdS quantum dots (QDs) and the fluorescence quenching of the QDs due to reduction of As(V) by L-cysteine was considered as a signal relevant to As(V) concentration. The As(III) species were also determined after oxidation of As(III) ions to As(V) with H2O2 and measurement of the total arsenic content. In treatment with 400 mL portions of water samples containing 30 μg L(-1) As(V), the relative standard deviation was 2.8%. The detection limit of arsenic was also found to be 0.75 μg L(-1) (1 × 10(-8) M). The reliability of proposed method was confirmed using certified reference materials. The trace amounts of arsenic species were then determined in different water samples, satisfactorily.

  13. Energy value of paraquat-treated and resin-soaked lobolly pine

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kossuth, S.V.; Roberts, D.R.; Huffman, J.B.

    1984-07-01

    With a basal injector, loblolly pines were treated with 5% paraquat cation (weight/weight basis) and harvested after 18 months. The resin acid, turpentine, moisture content (MC) and energy value were measured in three bolts of the stem. In bolt 1, the first 152 cm above the injection site, the increase in resin acids was 392% and in turpentine, 564%. Within the whole stem (the first two 152 cm bolts and the third bolt to a 7.6 cm inside-bark diameter) resin acids and turpentine increased 203 and 296% respectively. Moisture content was reduced 9%, 8%, and 8% in bolts 1, 2more » and 3, respectively. Turpentine from treated and untreated trees had an average heating value of 19,369 cal/g. When weighted for volume, net energy content was 7.8% greater for treated than control trees because of the increase in resin, including turpentine and the lowered MC.« less

  14. Tooth brush abrasion of paint-on resins for shade modification of crown and bridge resins.

    PubMed

    Fujii, Koichi; Ban, Seiji; McCabe, John F

    2003-09-01

    The purpose of this study was to evaluate the surface roughness and resistance to toothbrush abrasion of three experimental paint-on composite resins developed for the shade modification of crown and bridge resins. The paint-on resins had less filler volume fraction than restorative composites or the crown and bridge resins and consequently were of low viscosity. The maximum surface roughness (Rmax) and the maximum depth loss by abrasion for the paint-on resins following 40,000 cycles of brushing ranged from 2.45 to 4.07 microm and 8.63 to 13.67 microm, respectively. Rmax values were 37.7-67.5% lower than that for the crown and bridge resin subjected to the same test. Wear depth was 19.9-49.4% lower than for the crown and bridge resin. These results suggest that the paint-on resins are expected to have adequate resistance to toothbrush abrasion and may therefore be suitable for clinical use.

  15. Dissolved organic carbon concentrations and compositions, and trihalomethane formation potentials in waters from agricultural peat soils, Sacramento-San Joaquin Delta, California; implications for drinking-water quality

    USGS Publications Warehouse

    Fujii, Roger; Ranalli, Anthony J.; Aiken, George R.; Bergamaschi, Brian A.

    1998-01-01

    Water exported from the Sacramento-San Joaquin River delta (Delta) is an important drinking-water source for more than 20 million people in California. At times, this water contains elevated concentrations of dissolved organic carbon and bromide, and exceeds the U.S. Environmental Protection Agency's maximum contaminant level for trihalomethanes of 0.100 milligrams per liter if chlorinated for drinking water. About 20 to 50 percent of the trihalomethane precursors to Delta waters originates from drainage water from peat soils on Delta islands. This report elucidates some of the factors and processes controlling and affecting the concentration and quality of dissolved organic carbon released from peat soils and relates the propensity of dissolved organic carbon to form trihalomethanes to its chemical composition.Soil water was sampled from near-surface, oxidized, well-decomposed peat soil (upper soil zone) and deeper, reduced, fibrous peat soil (lower soil zone) from one agricultural field in the west central Delta over 1 year. Concentrations of dissolved organic carbon in the upper soil zone were highly variable, with median concentrations ranging from 46.4 to 83.2 milligrams per liter. Concentrations of dissolved organic carbon in samples from the lower soil zone were much less variable and generally slightly higher than samples from the upper soil zone, with median concentrations ranging from 49.3 to 82.3 milligrams per liter. The dissolved organic carbon from the lower soil zone had significantly higher aromaticity (as measured by specific ultraviolet absorbance) and contained significantly greater amounts of aromatic humic substances (as measured by XAD resin fractionation and carbon-13 nuclear magnetic resonance analysis of XAD isolates) than the dissolved organic carbon from the upper soil zone. These results support the conclusion that more aromatic forms of dissolved organic carbon are produced under anaerobic conditions compared to aerobic conditions. Dissolved organic carbon concentration, trihalomethane formation potential, and ultraviolet absorbance were all highly correlated, showing that trihalomethane precursors increased with increasing dissolved organic carbon and ultraviolet absorbance for whole water samples. Contrary to the generally accepted conceptual model for trihalomethane formation that assumes that aromatic forms of carbon are primary precursors to trihalomethanes, results from this study indicate that dissolved organic carbon aromaticity appears unrelated to trihalomethane formation on a carbon-normalized basis. Thus, dissolved organic carbon aromaticity alone cannot fully explain or predict trihalomethane precursor content, and further investigation of aromatic and nonaromatic forms of carbon will be needed to better identify trihalomethane precursors.

  16. Drying-induced physico-chemical changes in cranberry products.

    PubMed

    Michalska, Anna; Wojdyło, Aneta; Honke, Joanna; Ciska, Ewa; Andlauer, Wilfried

    2018-02-01

    Sugar-free cranberry juice (XAD) and juice with 15% of maltodextrin were dried by freeze-, vacuum and spray drying methods. Total phenolics (589-6435mg/kg dry matter) including 5 flavonols, 3 phenolic acids, 2 procyanidins and 5 anthocyanins were stronger affected by juice formulation than by drying methods. Spray drying of juice, regardless of its formulation, was competitive to freeze drying in terms of polyphenols' retention. Increase in temperature up to 100°C during vacuum drying of XAD extracts resulted in degradation of polyphenolics (down to 4%), except chlorogenic acid. Its content increased with rise in temperature and accelerated hydroxymethylfurfural formation. The stronger the impact of drying, the more chlorogenic acid is present in cranberry products. In all powders analysed, formation of furoylmethyl amino acids was noted. Antioxidant capacity of cranberry products was influenced by juice formulation and was linked to content of polyphenols. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Mass spectrometric methodology for the analysis of highly oxidized diterpenoid acids in Old Master paintings.

    PubMed

    Berg; Boon; Pastorova; Spetter

    2000-04-01

    Diterpenoid resins from larch and pine trees and the corresponding fractions in a >100-year-old wax-resin adhesive and varnish and a 200-year-old resin/oil paint sample were analysed with by gas chromatography/mass spectrometry (GC/MS) using several off-line and on-line derivatization methods. The main resin compounds were highly oxidized abietic acids. Important products found are hydroxydehydroabietic acids (OH-DHAs), 7-oxoDHA, di-OH-DHAs and 15-OH-7-oxoDHA. The last two compounds have not been reported to occur in artworks before. Larixyl acetate, an important marker from larch resins, was found to be still present in high amounts in the adhesive. A large number of mass spectra of the different oxidation products and larixol and larixyl acetate are presented and their fragmentation behaviour under electron impact conditions is discussed. An index for the degree of oxidation (IDOX) of the abietic acids is presented as an indicator of the degree of oxidation of the matrix in which the resin is present. The IDOX was 0.10, 0.67, 0.81 and 0.76 for the fresh resins, the dark-aged adhesive, the aged varnish and the resin/oil paint, respectively (measured with pyrolysis (Py)-tetramethylammonium hydroxide (TMAH)-GC/MS). Py-TMAH-GC/MS and direct temperature-resolved mass spectrometry are reliable, valuable and fast techniques for the assessment of the presence and degree of oxidation of diterpenoid resins. Copyright 2000 John Wiley & Sons, Ltd.

  18. Improved Blackbody Simulator

    DTIC Science & Technology

    1974-06-01

    28 - ABS Resins ................... 012 0.02 Carbon & Free-Cutting Steels%,. . . . . 27 - Acrylics ......................... 0.12 0.10 Alloy...Borosilicate Glasses................. 0.7 - Zinc At Its Alloys ................. 65.3 60.5 Alkyds .... .... .............. 010 0.20 Tungsten Carbide Cermet...cast).............47.6 25 ABS Resins ............ .. IS 3 FlowbnFie ........... 7 - Cellulose Acetate ............ &. 1.9 Pajadafi CW

  19. Influence of soil γ-irradiation and spiking on sorption of p,p'-DDE and soil organic matter chemistry.

    PubMed

    Škulcová, Lucia; Scherr, Kerstin E; Chrást, Lukáš; Hofman, Jakub; Bielská, Lucie

    2018-07-15

    The fate of organic chemicals and their metabolites in soils is often investigated in model matrices having undergone various pre-treatment steps that may qualitatively or quantitatively interfere with the results. Presently, effects associated with soil sterilization by γ-irradiation and soil spiking using an organic solvent were studied in one freshly spiked soil (sterilization prior to contamination) and its field-contaminated (sterilization after contamination) counterpart for the model organic compound 1,1-Dichloro-2,2-bis(4-chlorophenyl)ethene (p,p'-DDE). Changes in the sorption and potential bioavailability of spiked and native p,p'-DDE were measured by supercritical fluid extraction (SFE), XAD-assisted extraction (XAD), and solid-phase microextraction (SPME) and linked to qualitative changes in soil organic matter (SOM) chemistry measured by diffuse reflectance infrared Fourier-transform (DRIFT) spectroscopy. Reduced sorption of p,p´-DDE detected with XAD and SPME was associated more clearly with spiking than with sterilization, but SFE showed a negligible impact. Spiking resulted in an increase of the DRIFT-derived hydrophobicity index, but irradiation did not. Spectral peak height ratio descriptors indicated increasing hydrophobicity and hydrophilicity in pristine soil following sterilization, and a greater reduction of hydrophobic over hydrophilic groups as a consequence of spiking. In parallel, reduced sorption of p,p´-DDE upon spiking was observed. Based on the present samples, γ-irradiation appears to alter soil sorptive properties to a lesser extent when compared to common laboratory processes such as spiking with organic solvents. Copyright © 2018. Published by Elsevier Inc.

  20. Effect of sulfuric acid etching of polyetheretherketone on the shear bond strength to resin cements.

    PubMed

    Sproesser, Oliver; Schmidlin, Patrick R; Uhrenbacher, Julia; Roos, Malgorzata; Gernet, Wolfgang; Stawarczyk, Bogna

    2014-10-01

    To examine the influence of etching duration on the bond strength of PEEK substrate in combination with different resin composite cements. In total, 448 PEEK specimens were fabricated, etched with sulfuric acid for 5, 15, 30, 60, 90, 120, and 300 s and then luted with two conventional resin cements (RelyX ARC and Variolink II) and one self-adhesive resin cement (Clearfil SA Cement) (n = 18/subgroup). Non-etched specimens served as the control group. Specimens were stored in distilled water for 28 days at 37°C and shear bond strengths were measured. Data were analyzed nonparametrically using Kruskal-Wallis-H (p < 0.05). Non-etched PEEK demonstrated no bond strength to resin composite cements. The optimal etching duration varied with the type of resin composite: 60 s for RelyX ARC (15.3 ± 7.2 MPa), 90 s for Variolink II (15.2 ± 7.2 MPa), and 120 s for Clearfil SA Cement (6.4 ± 5.9 MPa). Regardless of etching duration, however, the self-etching resin composite cement showed significantly lower shear bond strength values when compared to groups luted with the conventional resin composites. Although sulfuric acid seems to be suitable and effective for PEEK surface pre-treatment, further investigations are required to examine the effect of other adhesive systems and cements.

  1. Synthesis and Thermal Degradation Studies of Melamine Formaldehyde Resins

    PubMed Central

    Ullah, Sami; Bustam, M. A.; Nadeem, M.; Tan, W. L.; Shariff, A. M.

    2014-01-01

    Melamine formaldehyde (MF) resins have been synthesized at different reaction temperature and pH values. Different molar ratios of melamine and formaldehyde were used to synthesize the corresponding resins. The prepared resin samples were characterized by using molecular weight determination viscometry and thermogravimetric analysis (TGA). The maximum percentage of solid content (69.7%) was obtained at pH 8.5 and 75°C temperature. The molecular weight of MF resin was increased with an increase of melamine monomer concentration. The highest residual weight 14.125 wt.% was obtained with sample 10. PMID:25436237

  2. Chemicals having estrogenic activity can be released from some bisphenol A-free, hard and clear, thermoplastic resins.

    PubMed

    Bittner, George D; Denison, Michael S; Yang, Chun Z; Stoner, Matthew A; He, Guochun

    2014-12-04

    Chemicals that have estrogenic activity (EA) can potentially cause adverse health effects in mammals including humans, sometimes at low doses in fetal through juvenile stages with effects detected in adults. Polycarbonate (PC) thermoplastic resins made from bisphenol A (BPA), a chemical that has EA, are now often avoided in products used by babies. Other BPA-free thermoplastic resins, some hypothesized or advertised to be EA-free, are replacing PC resins used to make reusable hard and clear thermoplastic products such as baby bottles. We used two very sensitive and accurate in vitro assays (MCF-7 and BG1Luc human cell lines) to quantify the EA of chemicals leached into ethanol or water/saline extracts of fourteen unstressed or stressed (autoclaving, microwaving, UV radiation) thermoplastic resins. Estrogen receptor (ER)-dependent agonist responses were confirmed by their inhibition with the ER antagonist ICI 182,780. Our data showed that some (4/14) unstressed and stressed BPA-free thermoplastic resins leached chemicals having significant levels of EA, including one polystyrene (PS), and three Tritan™ resins, the latter reportedly EA-free. Exposure to UV radiation in natural sunlight resulted in an increased release of EA from Tritan™ resins. Triphenyl-phosphate (TPP), an additive used to manufacture some thermoplastic resins such as Tritan™, exhibited EA in both MCF-7 and BG1Luc assays. Ten unstressed or stressed glycol-modified polyethylene terephthalate (PETG), cyclic olefin polymer (COP) or copolymer (COC) thermoplastic resins did not release chemicals with detectable EA under any test condition. This hazard survey study assessed the release of chemicals exhibiting EA as detected by two sensitive, widely used and accepted, human cell line in vitro assays. Four PC replacement resins (Tritan™ and PS) released chemicals having EA. However, ten other PC-replacement resins did not leach chemicals having EA (EA-free-resins). These results indicate that PC-replacement plastic products could be made from EA-free resins (if appropriate EA-free additives are chosen) that maintain advantages of re-usable plastic items (price, weight, shatter resistance) without releasing chemicals having EA that potentially produce adverse health effects on current or future generations.

  3. Acetylcholinesterase, butyrylcholinesterase and paraoxonase 1 activities in rats treated with cannabis, tramadol or both.

    PubMed

    Abdel-Salam, Omar M E; Youness, Eman R; Khadrawy, Yasser A; Sleem, Amany A

    2016-11-01

    To investigate the effect of Cannabis sativa resin and/or tramadol, two commonly drugs of abuse on acetylcholinesterase and butyrylcholinesterase activities as a possible cholinergic biomarkers of neurotoxicity induced by these agents. Rats were treated with cannabis resin (5, 10 or 20 mg/kg) (equivalent to the active constituent Δ 9 -tetrahydrocannabinol), tramadol (5, 10 and 20 mg/kg) or tramadol (10 mg/kg) combined with cannabis resin (5, 10 and 20 mg/kg) subcutaneously daily for 6 weeks. Acetylcholinesterase (AChE) and butyrylcholinesterase (BChE) activities were measured in brain and serum. We also measured the activity of paraoxonase-1 (PON1) in serum of rats treated with these agents. (i) AChE activity in brain increased after 10-20 mg/kg cannabis resin (by 16.3-36.5%). AChE activity in brain did not change after treatment with 5-20 mg/kg tramadol. The administration of both cannabis resin (5, 10 or 20 mg/kg) and tramadol (10 mg/kg) resulted in decreased brain AChE activity by 14.1%, 12.9% and 13.6%, respectively; (ii) BChE activity in serum was markedly and dose-dependently inhibited by cannabis resin (by 60.9-76.9%). BChE activity also decreased by 17.6-36.5% by 10-20 mg/kg tramadol and by 57.2-63.9% by the cannabis resin/tramadol combined treatment; (iii) Cannabis resin at doses of 20 mg/kg increased serum PON1 activity by 25.7%. In contrast, tramadol given at 5, 10 and 20 mg/kg resulted in a dose-dependent decrease in serum PON1 activity by 19%, 36.7%, and 46.1%, respectively. Meanwhile, treatment with cannabis resin plus tramadol resulted in 40.2%, 35.8%, 30.7% inhibition of PON1 activity compared to the saline group. These data suggest that cannabis resin exerts different effects on AChE and BChE activities which could contribute to the memory problems and the decline in cognitive function in chronic users. Copyright © 2016 Hainan Medical University. Production and hosting by Elsevier B.V. All rights reserved.

  4. Influence of matrix and filler fraction on biofilm formation on the surface of experimental resin-based composites.

    PubMed

    Ionescu, Andrei; Brambilla, Eugenio; Wastl, Daniel S; Giessibl, Franz J; Cazzaniga, Gloria; Schneider-Feyrer, Sibylle; Hahnel, Sebastian

    2015-01-01

    The aim of this study was to investigate the impact of resin matrix chemistry and filler fraction on biofilm formation on the surface of experimental resin-based composites (RBCs). Specimens were prepared from eight experimental RBC formulations differing in resin matrix blend (BisGMA/TEGDMA in a 7:3 wt% ratio or UDMA/aliphatic dimethacrylate in a 1:1 wt% ratio) and filler fraction (no fillers; 65 wt% dental glass with an average diameter of 7 or 0.7 µm or 65 wt% SiO2 with an average diameter of 20 nm). Surface roughness, surface free energy, and chemical surface composition were determined; surface topography was visualized using atomic force microscopy. Biofilm formation was simulated under continuous flow conditions for a 48 h period using a monospecies Streptococcus mutans and a multispecies biofilm model. In the monospecies biofilm model, the impact of the filler fraction overruled the influence of the resin matrix, indicating lowest biofilm formation on RBCs with nano-scaled filler particles and those manufactured from the neat resin blends. The multispecies model suggested a more pronounced effect of the resin matrix blend, as significantly higher biofilm formation was identified on RBCs with a UDMA/dimethacrylate matrix blend than on those including a BisGMA/TEGDMA matrix blend but analogous filler fractions. Although significant differences in surface properties between the various materials were identified, correlations between the surface properties and biofilm formation were poor, which highlights the relevance of surface topography and chemistry. These results may help to tailor novel RBC formulations which feature reduced biofilm formation on their surface.

  5. Effect of whitening toothpastes on bonding of restorative materials to enamel of primary teeth.

    PubMed

    Abdelmegid, F Y

    2016-01-01

    The aim of this in vitro investigation was to measure shear bond strength (SBS) of a resin composite and a resin-modified glass ionomer to enamel of primary teeth after application of different whitening toothpastes (WTs). Eighty labial enamel surfaces of primary incisors were randomly distributed into 8 groups of 10 each according to the surface treatment and bonding material. G1 and G2, control (brushed with water without WT); G3 and G4, (brushed with Colgate Optic White WT [Colgate-Palmolive Company, New York, NY, USA]), G5 and G6, (brushed with Crest Pro-Health Whitening WT [Procter and Gamble, Cincinnati, OH, USA]) and G7 and G8, (brushed with Arm and Hammer Advance White Extreme Whitening with Stain Defense WT [Church and Dwight Co., Princeton, NJ, USA]). SBS was measured at a crosshead speed of 0.5 mm/min and the type of bond failure was assessed using a stereomicroscope. There was significant difference between SBS of composite resin in groups 1, 3, 5, and 7 (P < 0.001), but no difference between resin-modified glass ionomer in groups 2, 4, 6, and 8 (P < 0.056). SBS of group 1 (control) was greater than groups 3, 5, and 7. There was a significant difference between group 1 and group 2 as well as group 7 and group 8 (P < 0.001). WTs affect SBS of resin composite, but not resin-modified glass ionomer to enamel of primary teeth. No difference of failure modes between different groups of tested materials.

  6. Salivary bisphenol A levels and their association with composite resin restoration.

    PubMed

    Lee, Jung-Ha; Yi, Seung-Kyoo; Kim, Se-Yeon; Kim, Ji-Soo; Son, Sung-Ae; Jeong, Seung-Hwa; Kim, Jin-Bom

    2017-04-01

    Composite resin has been increasingly used in an effort to remove minimal amount of tooth structure and are used for restoring not just carious cavities but also cervical abrasion. To synthesize composite resin, bisphenol A (BPA) is used. The aim of the study was to measure the changes in salivary BPA level related with composite resin restoration. ELISA was used to examine the BPA levels in the saliva collected from 30 volunteers whose teeth were filled with composite resin. Salivary samples were collected immediately before filling and 5 min and 7 d after filling. Wilcoxon signed-ranks test and linear regression were performed to test the significant differences of the changes in BPA levels in saliva. Before a new composite resin filling, there was no significant difference between with and without existing filling of composite resin and BPA level in the saliva was not correlated to the number of filled surfaces with composite resin. However, BPA level in the saliva increased to average 3.64 μg/L from average 0.15 μg/L after filling 5 min. BPA level increased in proportion with the number of filled surfaces. BPA level decreased to average 0.59 after filling 7 d. However it was higher than the BPA level before a new composite resin filling. Considering 50 μg/kg/day as the Tolerable Daily Intake of BPA suggested by European Food Safety Authority, the amount of BPA eluted in saliva after the composite resin filling is considered a safe level that is not a hazard to health at all. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. 49 CFR 173.173 - Paint, paint-related material, adhesives, ink and resins.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 49 Transportation 2 2011-10-01 2011-10-01 false Paint, paint-related material, adhesives, ink and... Than Class 1 and Class 7 § 173.173 Paint, paint-related material, adhesives, ink and resins. (a) When..., paint-related material, adhesives, ink and resins must be packaged as follows: (1) As prescribed in...

  8. 49 CFR 173.173 - Paint, paint-related material, adhesives, ink and resins.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 49 Transportation 2 2013-10-01 2013-10-01 false Paint, paint-related material, adhesives, ink and... Than Class 1 and Class 7 § 173.173 Paint, paint-related material, adhesives, ink and resins. (a) When..., paint-related material, adhesives, ink and resins must be packaged as follows: (1) As prescribed in...

  9. 49 CFR 173.173 - Paint, paint-related material, adhesives, ink and resins.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... 49 Transportation 2 2012-10-01 2012-10-01 false Paint, paint-related material, adhesives, ink and... Than Class 1 and Class 7 § 173.173 Paint, paint-related material, adhesives, ink and resins. (a) When..., paint-related material, adhesives, ink and resins must be packaged as follows: (1) As prescribed in...

  10. 49 CFR 173.173 - Paint, paint-related material, adhesives, ink and resins.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 49 Transportation 2 2014-10-01 2014-10-01 false Paint, paint-related material, adhesives, ink and... Than Class 1 and Class 7 § 173.173 Paint, paint-related material, adhesives, ink and resins. (a) When..., paint-related material, adhesives, ink and resins must be packaged as follows: (1) As prescribed in...

  11. 49 CFR 173.173 - Paint, paint-related material, adhesives, ink and resins.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 49 Transportation 2 2010-10-01 2010-10-01 false Paint, paint-related material, adhesives, ink and... Than Class 1 and Class 7 § 173.173 Paint, paint-related material, adhesives, ink and resins. (a) When..., paint-related material, adhesives, ink and resins must be packaged as follows: (1) As prescribed in...

  12. Cytotoxicity Evaluation of Two Bis-Acryl Composite Resins Using Human Gingival Fibroblasts.

    PubMed

    Gonçalves, Fabiano Palmeira; Alves, Gutemberg; Guimarães, Vladi Oliveira; Gallito, Marco Antônio; Oliveira, Felipe; Scelza, Míriam Zaccaro

    2016-01-01

    Bis-acryl resins are used for temporary dental restorations and have shown advantages over other materials. The aim of this work was to evaluate the in vitro cytotoxicity of two bis-acryl composite resins (Protemp 4 and Luxatemp Star), obtained at 1, 7 and 40 days after mixing the resin components, using a standardized assay employing human primary cells closely related to oral tissues. Human gingival fibroblast cell cultures were exposed for 24 h to either bis-acryl composite resins, polystyrene beads (negative control) and latex (positive control) extracts obtained after incubation by the different periods, at 37 °C under 5% CO2. Cell viability was evaluated using a multiparametric procedure involving sequential assessment (using the same cells) of mitochondrial activity (XTT assay), membrane integrity (neutral red test) and total cell density (crystal violet dye exclusion test). The cells exposed to the resin extracts showed cell viability indexes exceeding 75% after 24 h. Even when cells were exposed to extracts prepared with longer conditioning times, the bis-acryl composite resins showed no significant cytotoxic effects (p>0.05), compared to the control group or in relation to the first 24 h of contact with the products. There were no differences among the results obtained for the bis-acryl composite resins evaluated 24 h, 7 days and 40 days after mixing. It may be concluded that the bis-acryl resins Protemp 4 and Luxatemp Star were cytocompatible with human gingival fibroblasts, suggesting that both materials are suitable for use in contact with human tissues.

  13. Solidification of spent ion exchange resins into the SIAL matrix at the Dukovany NPP, Czech Republic

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Tatransky, Peter; Prazska, Milena; Harvan, David

    2013-07-01

    Based on the decision of the State Office for Nuclear Safety, the Dukovany NPP has been obliged to secure the efficient capacities for the disposal of spent ion exchange resins. Therefore, in September 2010, based on the contract with supplier company AMEC Nuclear Slovakia s.r.o. has begun with pumping and treatment of ion exchange resins from the storage tank 0TW30B02, situated in the auxiliary building. The SIAL{sup R} technology, developed in AMEC Nuclear Slovakia, has been used for the solidification purposes. This technology allows an on-site treatment of various special radioactive waste streams (resins, sludge, sludge/resins and borates) at themore » room temperature. The SIAL{sup R} matrix and technology were licensed by the Czech State Office for Nuclear Safety in 2007. On-site treatment and solidification of spent ion exchange resins at Dukovany NPP involves process of resin removal from tank using remotely operated manipulator, resin transportation, resin separation from free water, resin filling into 200 dm{sup 3} drums and solidification into SIAL{sup R} matrix in 200 dm{sup 3} drums using the FIZA S 200 facility. The final product is observed for compressive strength, leachability, radionuclide composition, dose rate, solids and total weight. After meeting the requirements for final disposal and consolidation, the drums are being transported for the final disposal to the Repository at Dukovany site. During the 3 month's trial operation in 2010, and the normal operation in 2011 and 2012, 189 tons of dewatered resins have been treated into 1960 drums, with total activity higher than 920 GBq. At the end of trial run (2010), 22 tons of dewatered resins were treated into 235 drums. During standard operation approximately 91 tons in 960 drums (2011) and 76 tons in 765 drums (2012) were treated. The weights of resins in the drum ware in the range from 89 - 106 kg and compressive strength limit (10 MPa) has already been achieved 24 hours after fixation. The final measured strength values ranged from 19.0 - 34.7 MPa and real leachability values ranged from 0.03 - 0.65%, far below the 4% limit value. Collective effective dose of all workers in 2012 was 7.7 mSv (12.6 mSv in 2011, 6.2 mSv in 2010). Average individual effective dose in 2012 was 0.55 mSv (14 workers), and maximal individual effective dose was 2.25 mSv. This approach allows fast, safe and cost effective immobilization and transformation of dangerous radioactive waste such as sludge and resins into the solid form, which is suitable for long term storage or disposal. (authors)« less

  14. Characterization of nano-clay reinforced phytagel-modified soy protein concentrate resin.

    PubMed

    Huang, Xiaosong; Netravali, Anil N

    2006-10-01

    Phytagel and nano-clay particles were used to improve the mechanical and thermal properties and moisture resistance of soy protein concentrate (SPC) resin successfully. SPC and Phytagel were mixed together to form a cross-linked structure. The Phytagel-modified SPC resin (PH-SPC) showed improved tensile strength, modulus, moisture resistance, and thermal stability as compared to the unmodified SPC resin. The incorporation of 40% Phytagel and 20% glycerol led to an overall 340% increase in the tensile strength (over 50 MPa) and approximately 360% increase in the Young's modulus (over 710 MPa) of the SPC resin. Nano-clay was uniformly dispersed into PH-SPC resin to further improve the properties. The PH-SPC (40% Phytagel) resin modified with 7% clay nanoparticles (CPH-SPC) had a modulus of 2.1 GPa and a strength of 72.5 MPa. The dynamic mechanical properties such as storage modulus together with the glass transition temperature of the modified resins were also increased by the addition of clay nanoparticles. The moisture resistance of the CPH-SPC resin was higher as compared to both SPC and PH-SPC resins. The thermal stability of the CPH-SPC resin was seen to be higher as compared to the unmodified SPC.

  15. Effects of air-polishing powders on color stability of composite resins.

    PubMed

    Güler, Ahmet Umut; Duran, Ibrahim; Yücel, Ali Çağin; Ozkan, Pelin

    2011-10-01

    The purpose of this study was to investigate the effect of different air-polishing powders on the color stability of different types of composite resin restorative materials. Thirty cylindrical specimens (15×2 mm) were prepared for each of 7 composite resin restorative materials. All specimens were polished with a series of aluminum oxide polishing discs (Sof-Lex). The prepared specimens of each composite resin were randomly divided into 3 groups of 10 specimens each, for control (Group-C) and two air-powder applications (Group-CP: Cavitron Prophy-Jet; Group-PS: Sirona ProSmile prophylaxis powder). A standard air-polishing unit (ProSmile Handly) was used. All specimens were air-powdered for 10 s at 4-bar pressure. The distance of the spray nosel from the specimens was approximately 10 mm and angulation of the nosel was 90°. Specimens were stored in 100 mL of coffee (Nescafe Classic) for 24 h at 37°C. Color measurement of all specimens was recorded before and after exposure to staining agent with a colorimeter (Minolta CR-300). Color differences (∆E*) between the 2 color measurements (baseline and after 24 h storage) were calculated. The data were analyzed with a 2-way ANOVA test, and mean values were compared by the Tukey HSD test (p<0.05). According to the 2-way ANOVA results, composite resin restorative materials, air-polishing powders, and their interaction were statistically significant (p<0.05) For Aelite Aesthetic Enemal, Filtek Z250, Grandio, CeramX Mono, and Quixfil composite resin restorative materials, no significant difference was observed between Group-PS and Group-CP (p>.05) and these groups demonstrated the highest ∆E* values. For Filtek Silorane and IntenS, the highest ∆E* values were observed in Group-PS. The lowest ∆E* values for all composite resin groups were observed in Group-C. When comparing the 7 composite resin restorative materials, Aelite Aesthetic Enemal demonstrated significantly less ∆E* values than the other composite resins tested. The highest ∆E* values were observed in Quixfil. Except for Quixfil, all control groups of composite resins that were polished Sof-Lex exhibited clinically acceptable ∆E values (<3.7). Air-polishing applications increased the color change for all composite resin restorative materials tested. Composite restorations may require re-polishing after air-polishing.

  16. Effects of air-polishing powders on color stability of composite resins

    PubMed Central

    GÜLER, Ahmet Umut; DURAN, Ibrahim; YÜCEL, Ali Çagin; ÖZKAN, Pelin

    2011-01-01

    Objectives The purpose of this study was to investigate the effect of different air-polishing powders on the color stability of different types of composite resin restorative materials. Material and methods Thirty cylindrical specimens (15×2 mm) were prepared for each of 7 composite resin restorative materials. All specimens were polished with a series of aluminum oxide polishing discs (Sof-Lex). The prepared specimens of each composite resin were randomly divided into 3 groups of 10 specimens each, for control (Group-C) and two air-powder applications (Group-CP: Cavitron Prophy-Jet; Group-PS: Sirona ProSmile prophylaxis powder). A standard air-polishing unit (ProSmile Handly) was used. All specimens were air-powdered for 10 s at 4-bar pressure. The distance of the spray nosel from the specimens was approximately 10 mm and angulation of the nosel was 90º. Specimens were stored in 100 mL of coffee (Nescafe Classic) for 24 h at 37ºC. Color measurement of all specimens was recorded before and after exposure to staining agent with a colorimeter (Minolta CR-300). Color differences (∆E*) between the 2 color measurements (baseline and after 24 h storage) were calculated. The data were analyzed with a 2-way ANOVA test, and mean values were compared by the Tukey HSD test (p≤0.05). Results According to the 2-way ANOVA results, composite resin restorative materials, air-polishing powders, and their interaction were statistically significant (p<0.05) For Aelite Aesthetic Enemal, Filtek Z250, Grandio, CeramX Mono, and Quixfil composite resin restorative materials, no significant difference was observed between Group-PS and Group-CP (p>.05) and these groups demonstrated the highest ∆E* values. For Filtek Silorane and IntenS, the highest ∆E* values were observed in Group-PS. The lowest ∆E* values for all composite resin groups were observed in Group-C. When comparing the 7 composite resin restorative materials, Aelite Aesthetic Enemal demonstrated significantly less ∆E* values than the other composite resins tested. The highest ∆E* values were observed in Quixfil. Conclusion Except for Quixfil, all control groups of composite resins that were polished Sof-Lex exhibited clinically acceptable ∆E values (<3.7). Air-polishing applications increased the color change for all composite resin restorative materials tested. Composite restorations may require re-polishing after air-polishing. PMID:21922122

  17. 21 CFR 177.2450 - Polyamide-imide resins.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... polyamide-imide resins are derived from the condensation reaction of substantially equimolar parts of.... 31957-38-7) derived from the condensation reaction of equimolar parts of benzoyl chloride-3,4...

  18. The influence of storage time and pH variation on water sorption by different composite resins.

    PubMed

    Gusmão, George Mário de Araújo Silva; De Queiroz, Thiago Vinicius Veras; Pompeu, Guilherme Ferrer; Menezes Filho, Paulo Fonseca; da Silva, Cláudio Heliomar Vicente

    2013-01-01

    The objective of this work was to assess the influence of storage time and pH cycling on water sorption by different composite resins. Nine resin brands were selected and divided into groups: G1-ROK (SDI), G2-ICE (SDI), G3-GLACIER (SDI), G4-Z350 (3M/ESPE), G5-Z250 (3M/ESPE), G6-TPH 3 (DENTSPLY), G7-ESTHET X (DENTSPLY), G8-SUPRAFILL (SSWHITE), and G9-MASTERFILL (BIODINΒMICS). Ninety specimens, ten per group, were obtained using an aluminum matrix. Specimens measured 10 mm diameter × 2 mm width. The groups were divided into subgroups according to the immersion solution: A - control (n = 05) stored in artificial saliva pH = 7.0 and B-test (n = 05) submitted to seven consecutive days of pH cycling (cariogenic challenger) that consisted of immersion in a pH° = 4.3 solution for 6 h followed by immersion in a pH¹ =7.0 solution for 18 h and stored in artificial saliva pH = 7.0 until the end of the experiment. The specimens were weighed on six occasions: T 0 (after fabrication), T 1 (24 h), T 2 (7 days), T 3 (15 days), T 4 (30 days), T 5 (60 days), and then analyzed. The water sorption was determined by the weight difference between the specimens at the time intervals. The mean weight gain was exactly the same for both the subgroups within group G4. The highest means for the control subgroup were found in groups: G1, G5, G7, G8, and G9. For the pH cycling subgroup, the highest means were found in G2, G3, and G6; however, significant differences between the subgroups compared to the mean-weight gain were found for G1, G5, and G7. The water sorption of composite resins is dependent upon their storage time. The pH cycling created a significant impact on resins G1, G5, and G7. The sorption and solubility of composite resins vary according to their chemical composition.

  19. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kubouchi, Masatoshi; Hojo, Hidemitsu

    The thermal shock resistance of epoxy resin specimens toughened with carboxy-terminated poly(butadiene-acrylonitrile) (CTBN) and poly-glycol were tested using a new notched disk-type specimen. The new thermal shock testing method consists of quenching a notched disk-type specimen and applying a theoretical analysis to the test results to determine crack propagation conditions. For both toughened epoxy resins, this test method evaluated improvements in thermal shock resistance. The thermal shock resistance of epoxy resin toughened with CTBN exhibited a maximum at a 35 parts per hundred resin content of CTBN. The epoxy resin toughened with polyglycol exhibited improved thermal shock resistance with increasingmore » glycol content. 7 refs., 14 figs., 1 tab.« less

  20. Toxicity of organic chemical pollution in groundwater downgradient of a landfill (Grindsted, Denmark)

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Baun, A.; Jensen, S.D.; Bjerg, P.L.

    2000-05-01

    The aim of the present study was to describe the occurrence and distribution of toxicity related to organic chemical contaminants in the leachate plume downgradient of the Grindsted Landfill (Denmark). A total of 27 groundwater samples were preconcentrated by solid-phase extraction (SPE) using XAD-2 as the resin material. This treatment effectively eliminated sample matrix toxicity caused by inorganic salts and natural organic compounds and produced an aqueous concentrate of the nonvolatile chemical contaminants. The SPE extracts were tested in a battery of standardized short-term aquatic toxicity tests with luminescent bacteria (Vibrio fischeri), algae (Selenastrum capricornutum), and crustaceans (Daphnia magna). Additionalmore » genotoxicity tests were made using the umuC test (Salmonella typhimurium). Biotests with algae and luminescent bacteria were the most sensitive tests. On the basis of results with these two bioassays, it was concluded that SPE extracts of groundwater collected close to the landfill were toxic. The toxicity decreased with the distance from the landfill. At distances greater than 80 m from the border of the landfill, the groundwater toxicity was not significantly different from the background toxicity. SPE extracts were not toxic to Daphnia, and no genotoxicity was observed in the umuC test. The overall findings indicate that a battery of biotests applied on preconcentrated groundwater samples can be a useful tool for toxicity characterization and hazard ranking of groundwater polluted with complex chemical mixtures, such as landfill leachates.« less

  1. Comparison of the wear and flexural characteristics of flowable resin composites for posterior lesions.

    PubMed

    Sumino, Natsu; Tsubota, Keishi; Takamizawa, Toshiki; Shiratsuchi, Koji; Miyazaki, Masashi; Latta, Mark A

    2013-01-01

    To determine the localized wear and flexural properties of flowable resin composites for posterior lesions compared with universal resin composites produced by the same manufacturers. Ten specimens of each of three flowable resins, G-ænial Universal Flo, G-ænial Flo and Clearfil Majesty Flow, and the corresponding resin composite materials, Kalore and Clearfil Majesty Esthetics, were prepared in custom fixtures and subjected to 400,000 wear machine cycles to simulate localized wear. The total maximum depth and volume loss of the wear facets was calculated for each specimen using a profilometer. A three-point bending test was performed to determine the flexural strength, modulus of elasticity and resilience. Values were statistically compared using one-way analysis of variance (ANOVA) followed by Tukey's Honestly Significant Difference (HSD) test. The wear depth ranged from 58.3-126.9 m and the volumetric loss ranged from 0.019-0.049 mm(3), with significant differences observed between restorative materials. The wear depth of G-ænial Universal Flo was significantly smaller than those of the other resin composites tested. The flexural strengths and elastic modulus ranged from 90.5-135.1 MPa and from 4.7-7.6 GPa, respectively. A significantly greater flexural strength and higher elastic modulus was found for G-ænial Universal Flo than the other composites. The wear and mechanical properties of the flowable resin composites tested suggested improved performance compared with universal resin composites.

  2. Utilization of a modified special-cubic design and an electronic tongue for bitterness masking formulation optimization.

    PubMed

    Li, Lianli; Naini, Venkatesh; Ahmed, Salah U

    2007-10-01

    A unique modification of simplex design was applied to an electronic tongue (E-Tongue) analysis in bitterness masking formulation optimization. Three formulation variables were evaluated in the simplex design, i.e. concentrations of two taste masking polymers, Amberlite and Carbopol, and pH of the granulating fluid. Response of the design was a bitterness distance measured using an E-Tongue by applying a principle component analysis, which represents taste masking efficiency of the formulation. The smaller the distance, the better the bitterness masking effect. Contour plots and polynomial equations of the bitterness distance response were generated as a function of formulation composition and pH. It was found that interactions between polymer and pH reduced the bitterness of the formulation, attributed to pH-dependent ionization and complexation properties of the ionic polymers, thus keeping the drug out of solution and unavailable to bitterness perception. At pH 4.9 and an Amberlite/Carbopol ratio of 1.4:1 (w/w), the optimal taste masking formulation was achieved and in agreement with human gustatory sensation study results. Therefore, adopting a modified simplex experimental design on response measured using an E-Tongue provided an efficient approach to taste masking formulation optimization using ionic binding polymers. (c) 2007 Wiley-Liss, Inc.

  3. TOTAL PAH EXPOSURES OF NINE PRESCHOOL CHILDREN

    EPA Science Inventory

    This study evaluates the influence of denuder sampling methods and filter collection media on the measurement of semi-volatile organic carbon (SVOC) associated with PM2.5. Two types of collection media, charcoal (activated carbon) and XAD, were used both in diffusion denuders ...

  4. Effect of microwave disinfection on the surface roughness of three denture base resins after tooth brushing.

    PubMed

    Izumida, Fernanda Emiko; Ribeiro, Roberta Chuqui; Giampaolo, Eunice Teresinha; Machado, Ana Lucia; Pavarina, Ana Cláudia; Vergani, Carlos Eduardo

    2011-12-01

    This study investigated the effect of microwave disinfection on the roughness of three heat-polymerised acrylic resins after tooth brushing. Microwave disinfection has been recommended to reduce cross-contamination. However, this procedure may also influence the physical and mechanical properties of acrylic resins. Specimens (40 × 20 × 2 mm) of resins: Lucitone 550 (L), QC 20(QC) and Acron MC (A) were prepared and divided into four groups (n = 10): Control groups 1 (C1) and 2 (C2) - stored in water for 48 h or 7 days; Test groups 1 (MW2) and 2 (MW7) - stored in water for 48 h and disinfected (650 W for 6 min) daily for 2 or 7 days, respectively. After treatments, the specimens were placed in a tooth brushing machine at a rate of 60 reciprocal strokes per minute. The specimens were brushed with 20 000 strokes, which represent approximately 2 years of denture cleansing. The surface roughness (Ra) was evaluated before and after the tooth brushing. Data were analysed by two-way anova and Tukey Honestly Significant Difference (HSD) post hoc tests (α = 0.05). The data revealed significant changes between test groups for A and L resins. Comparison among resins revealed that for MW7, the roughness of A was significantly lower than that of L. After the seven microwave cycles, it could be seen that the roughness values of QC were significantly lower than those of L. The roughness of QC after brushing was not significantly affected by microwave disinfection. For A and L, seven microwave cycles resulted in increased roughness. © 2011 The Gerodontology Society and John Wiley & Sons A/S.

  5. A review of the success and failure characteristics of resin-bonded bridges.

    PubMed

    Miettinen, M; Millar, B J

    2013-07-01

    This literature review was designed to assess and compare the success rates and modes of failure of metal-framed, fibre-reinforced composite and all-ceramic resin-bonded bridges. A Medline search (Ovid), supplemented by hand searching, was conducted to identify prospective and retrospective cohort studies on different resin-bonded bridges within the last 16 years. A total of 49 studies met the pre-set inclusion criteria. Success rates of 25 studies on metal-framed, 17 studies on fibre-reinforced composite and 7 studies on all-ceramic resin-bonded bridges were analysed and characteristics of failures were identified. The analysis of the studies indicated an estimation of annual failure rates per year to be 4.6% (±1.3%, 95% CI) for metal-framed, 4.1% (±2.1%, 95% CI) for fibre-reinforced and 11.7% (±1.8%, 95% CI) for all-ceramic resin-bonded bridges. The most frequent complications were: debonding for metal-framed, resin-bonded bridges (93% of all failures); delamination of the composite veneering material for the fibre-reinforced bridges (41%) and fracture of the framework for the all-ceramic bridges (57%). All types of resin-bonded bridges provide an effective short- to medium-term option, with all-ceramic performing least well and having the least favourable mode of failure. The methods of failures were different for different bridges with metal frameworks performing the best over time.

  6. Separation and purification of epigallocatechin-3-gallate (EGCG) from green tea using combined macroporous resin and polyamide column chromatography.

    PubMed

    Jin, Xin; Liu, Mingyan; Chen, Zaixing; Mao, Ruikun; Xiao, Qinghuan; Gao, Hua; Wei, Minjie

    2015-10-01

    Epigallocatechin-3-gallate (EGCG) is a major bioactive ingredient of green tea that produces beneficial neuroprotective effects. In this paper, to optimize the EGCG enrichment, thirteen macroporous resins with different chemical and physical properties were systemically evaluated. Among the thirteen tested resins, the H-bond resin HPD826 exhibited best adsorption/desorption capabilities and desorption ratio, as well as weakest affinity for caffeine. The absorption of EGCG on the HPD826 resin followed the pseudo-second-order kinetics and Langmuir isotherm model. The separation parameters of EGCG were optimized by dynamic adsorption/desorption experiments with the HPD826 resin column. Under the optimal condition, the content of EGCG in the 30% ethanol eluent increased by 5.8-fold from 7.7% to 44.6%, with the recovery yield of 72.1%. After further purification on a polyamide column, EGCG with 74.8% purity was obtained in the 40-50% ethanol fraction with a recovery rate of 88.4%. In addition, EGCG with 95.1% purity could be easily obtained after one-step crystallization in distilled water. Our study suggests that the combined macroporous resin and polyamide column chromatography is a simple method for large-scale separation and purification of EGCG from natural plants for food and pharmaceutical applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Wettability of southern pine veneer by phenol formaldehyde wood adhesives

    Treesearch

    Chung-Yun Hse

    1972-01-01

    Wettability of southern pine veneers was judged by measuring the contact angles made by 36 phenol formaldehyde resins. Formulation of the resins was by factorial design, the molar ratios of sodium hydroxide to phenol being 0.4, 0.7, and 1.0, the levels of resin solids content in the reaction mixture 37, 40, and 43 percent, and the molar ratios of formaldehyde to phenol...

  8. Wettability of southern pine veneer by phenol formaldehyde wood adhesives

    Treesearch

    C. -Y. Hse

    1972-01-01

    Wettabillty of southern pine veneers was judged by measuring the contact angles made by 36 phenol formaldehyde resins. Formulation of the resins was by factorial design. the molar ratios of sodium hydroxide to phenol being 0.4, 0.7, and 1.0, the levels of resin solids content in the reaction mixture 37, 40, and 43 percent, and the molar ratios of formaldehyde to phenol...

  9. Process Optimization of Bismaleimide (BMI) Resin Infused Carbon Fiber Composite

    NASA Technical Reports Server (NTRS)

    Ehrlich, Joshua W.; Tate, LaNetra C.; Cox, Sarah B.; Taylor, Brian J.; Wright, M. Clara; Faughnan, Patrick D.; Batterson, Lawrence M.; Caraccio, Anne J.; Sampson, Jeffery W.

    2013-01-01

    Engineers today are presented with the opportunity to design and build the next generation of space vehicles out of the lightest, strongest, and most durable materials available. Composites offer excellent structural characteristics and outstanding reliability in many forms that will be utilized in future aerospace applications including the Commercial Crew and Cargo Program and the Orion space capsule. NASA's Composites for Exploration (CoEx) project researches the various methods of manufacturing composite materials of different fiber characteristics while using proven infusion methods of different resin compositions. Development and testing on these different material combinations will provide engineers the opportunity to produce optimal material compounds for multidisciplinary applications. Through the CoEx project, engineers pursue the opportunity to research and develop repair patch procedures for damaged spacecraft. Working in conjunction with Raptor Resins Inc., NASA engineers are utilizing high flow liquid infusion molding practices to manufacture high-temperature composite parts comprised of intermediate modulus 7 (IM7) carbon fiber material. IM7 is a continuous, high-tensile strength composite with outstanding structural qualities such as high shear strength, tensile strength and modulus as well as excellent corrosion, creep, and fatigue resistance. IM7 carbon fiber, combined with existing thermoset and thermoplastic resin systems, can provide improvements in material strength reinforcement and deformation-resistant properties for high-temperature applications. Void analysis of the different layups of the IM7 material discovered the largest total void composition within the [ +45 , 90 , 90 , -45 ] composite panel. Tensile and compressional testing proved the highest mechanical strength was found in the [0 4] layup. This paper further investigates the infusion procedure of a low-cost/high-performance BMI resin into an IM7 carbon fiber material and the optical, chemical, and mechanical analyses performed.

  10. Properties of two composite materials made of toughened epoxy resin and high-strain graphite fiber

    NASA Technical Reports Server (NTRS)

    Dow, Marvin B.; Smith, Donald L.

    1988-01-01

    Results are presented from an experimental evaluation of IM7/8551-7 and IM6/18081, two new toughened epoxy resin, high strain graphite fiber composite materials. Data include ply-level strengths and moduli, notched tension and compression strengths and compression-after-impact assessments. The measured properties are compared with those of other graphite-epoxy materials.

  11. The effect of deodorization on volatile compositions of fucoidan extracted from brown seaweed (Sargassum sp.)

    NASA Astrophysics Data System (ADS)

    Khalafu, Sharifah Habibah Syed; Mustapha, Wan Aida Wan; Lim, Seng Joe; Maskat, Mohamad Yusof

    2016-11-01

    Fucoidan is a biologically active polysaccharide that were made up of complex mixture of fucose, sulfate and uronic acid. This study was conducted to identify the volatile compositions of crude fucoidan and deodorized fucoidans extracted from brown seaweed Sargassum sp. (Fsar). The volatile compositions was also compared with a standard commercial fucoidan (Fysk). Fucoidan was extracted from Sargassum sp. originated in coastal area of Indonesia, by using a low pH acid extraction method. Approximately 20 mL of 1% freshly extracted fucoidan was then subjected to deodorization process by using three different method i.e., by treating it with 10 g activated carbon (Fac), 0.4 g ion exchange resin, Amberlite 67 (Fresin) and 2 mL of 1% calcium carbonate (FCaCO3) and incubated for 12 hrs before further analysis. Forty-six volatile compounds were successfully identified in all of the five samples by using Headspace-Solid Phase Microextraction (HS-SPME) and analysed by using Gas Chromatography Mass Spectrometer (GCMS). In Fsar, 72% of the total volatile constituents were identified as aromatic hydrocarbons, 23% hydrocarbons and 5% alcohols. In Fysk, all compounds detected are in group hydrocarbons. In Fsar, all of the compounds identified were classified as odor active compounds which had a contribution to unpleasant odor in fucoidan. After deodorization, 72% of aromatic hydrocarbons detected in Fsar were reported to be absent in all deodorized fucoidans. Both Fresin and FCaCO3 showed a reduction in peak area percentages of phenol, 2,4-bis (1,1-dimethylethyl)- from Fsar (1.30%) to 0.79 and 1.07% respectively. Meanwhile in Fac, no presence of phenol, 2,4-bis (1,1-dimethylethyl) was reported. These findings are essential to propel the advancement of research in deodorization technologies of marine products, especially fucoidans.

  12. Effects of 4-META/MMA-TBB Resin at Different Curing Stages on Osteoblasts and Gingival Epithelial Cells.

    PubMed

    Morotomi, Takahiko; Hirata-Tsuchiya, Shizu; Washio, Ayako; Kitamura, Chiaki

    2016-01-01

    To assess the effects of different curing stages of 4-META/MMA-TBB resin on osteoblasts and gingival keratinocytes. The MC3T3-E1 murine pre-osteoblastic cell line and GE-1 murine gingival epithelial cell line were cultured with mixtures of Super-Bond C&B at different curing stages, and the cell viability was assessed. The alkaline phosphatase (ALP) activity of the MC3T3-E1 cells was also assessed. The majority of the MC3T3-E1 cells died and showed no ALP activity when cultured with 4-META/MMA-TBB resin during the initial curing phase (1 min of curing). A later curing phase of the 4-META/MMA-TBB resin (7 min of curing) showed cytotoxicity at day 1, but the toxic effect was temporary and the proliferative capacity and ALP activity in the cells were similar to control cells at day 7. Completely cured 4-META/MMA-TBB resin (after 1 or 12 h of curing) did not affect the cell viability or ALP activity of the MC3T3-E1 cells. In contrast, 4-META/MMA-TBB resin showed no effect on the GE-1 cells at any stage of curing. Although 4-META/MMA-TBB resin during the initial curing phase shows toxic effects on MC3T3-E1 cells, that cytotoxicity is minimal at later curing phases. In contrast, neither the uncured nor cured resins affected the GE-1 cells.

  13. Antioxidant activity of a new aromatic geranyl derivative of the resinous exudates from Heliotropium glutinosum Phil.

    PubMed

    Modak, Brenda; Rojas, Macarena; Torres, René; Rodilla, Jesús; Luebert, Federico

    2007-05-21

    Heliotropium glutinosum Phil. (Heliotropiceae) is a resinous bush that grows at a height of 2000 m in Chañaral, Chile. From the resinous exudates of Heliotropium glutinosum Phil. a new aromatic geranyl derivative: 4-methoxy-3-[(2)-7'-methyl-3'-hydroxymethyl-2',6'-octadienyl] phenol (1) and three flavonoids: 5,3'-dihydroxy-7,4'-dimethoxyflavanone (2), 5,4'-dihydroxy-7-methoxyflavanone (3) and 4'-acetyl-5-hydroxy-7-methoxyflavanone (4) were isolated and their structures were determined. Their antioxidant activity were evaluated using the bleaching of ABTS and DPPH derived cation radical methods and expressed in terms of FRE (fast reacting equivalents) and TRE (total reacting equivalents), where FRE is a good measure of the quick protection of a given compound against oxidants and TRE measures the degree of long-term protection of the antioxidant, or how effective it is against a strong oxidative stress.

  14. Composite Properties of Polyimide Resins Made From "Salt-Like" Solution Precursors

    NASA Technical Reports Server (NTRS)

    Cano, Roberto J.; Weiser, Erik S.; SaintClair, Terry L.; Echigo, Yoshiaki; Kaneshiro, Hisayasu

    1997-01-01

    Recent work in high temperature materials at NASA Langley Research Center (LaRC (trademark)) have led to the development of new polyimide resin systems with very attractive properties. The majority of the work done with these resin systems has concentrated on determining engineering mechanical properties of composites prepared from a poly(amide acid) precursor. Three NASA Langley-developed polyimide matrix resins, LaRC (trademark) -IA, LaRC (trademark) -IAX, and LaRC (trademark) -8515, were produced via a salt-like process developed by Unitika Ltd. The 'salt-like' solutions (sixty-five percent solids in NMP) were prepregged onto Hexcel IM7 carbon fiber using the NASA LaRC Multipurpose Tape Machine. Process parameters were determined and composite panels fabricated. Mechanical properties are presented for these three intermediate modulus carbon fiber/polyimide matrix composites and compared to existing data on the same polyimide resin systems and IM7 carbon fiber manufactured via poly(amide acid) solutions (thirty-five percent solids in NMP). This work studies the effects of varying the synthetic route on the processing and mechanical properties of polyimide composites.

  15. Combustible Cartridge Case Characterization

    DTIC Science & Technology

    1984-02-01

    Latex 241 * Nitrocellulose and Kraft /fibers National Starch Resin 78-3730 The beater additive process for manufacturing combustible cartridge cases *is... Kraft Fibers The Kraft fibers were received as sheets weighing approximately 1.3 lb each. The moisture content of the sheets varied from 6 to 7-1/2... Kraft fibers was incorporated into each batch. Resins The resins were supplied as a water emulsion with nominally 50 percent solids. Samples of each

  16. Influence of Hot-Etching Surface Treatment on Zirconia/Resin Shear Bond Strength

    PubMed Central

    Lv, Pin; Yang, Xin; Jiang, Ting

    2015-01-01

    This study was designed to evaluate the effect of hot-etching surface treatment on the shear bond strength between zirconia ceramics and two commercial resin cements. Ceramic cylinders (120 units; length: 2.5 mm; diameter: 4.7 mm) were randomly divided into 12 groups (n = 10) according to different surface treatments (blank control; airborne-particle-abrasion; hot-etching) and different resin cements (Panavia F2.0; Superbond C and B) and whether or not a thermal cycling fatigue test (5°–55° for 5000 cycles) was performed. Flat enamel surfaces, mounted in acrylic resin, were bonded to the zirconia discs (diameter: 4.7 mm). All specimens were subjected to shear bond strength testing using a universal testing machine with a crosshead speed of 1 mm/min. All data were statistically analyzed using one-way analysis of variance and multiple-comparison least significant difference tests (α = 0.05). Hot-etching treatment produced higher bond strengths than the other treatment with both resin cements. The shear bond strength of all groups significantly decreased after the thermal cycling test; except for the hot-etching group that was cemented with Panavia F2.0 (p < 0.05). Surface treatment of zirconia with hot-etching solution enhanced the surface roughness and bond strength between the zirconia and the resin cement. PMID:28793699

  17. Breakthrough of 1,3-dichloropropene and chloropicrin from 600 mg XAD-4 air sampling tubes

    USDA-ARS?s Scientific Manuscript database

    Accurately measuring air concentrations of agricultural fumigants is important for the regulation of air quality. Understanding the conditions under which sorbent tubes can effectively retain such fumigants during sampling is critical in mitigating chemical breakthrough from the tubes and facilitati...

  18. Curing Effects on Interfacial Adhesion between Recycled Carbon Fiber and Epoxy Resin Heated by Microwave Irradiation

    PubMed Central

    Shimamoto, Daisuke; Hotta, Yuji

    2018-01-01

    The interfacial adhesion of recycled carbon fiber (CF) reinforced epoxy composite heated by microwave (MW) irradiation were investigated by changing the curing state of the epoxy resin. The recycled CF was recovered from the composite, which was prepared by vacuum-assisted resin transfer molding, by thermal degradation at 500 or 600 °C. Thermogravimetric analysis showed that the heating at 600 °C caused rough damage to the CF surface, whereas recycled CF recovered at 500 °C have few defects. The interfacial shear strength (IFSS) between recycled CF and epoxy resin was measured by a single-fiber fragmentation test. The test specimen was heated by MW after mixing the epoxy resin with a curing agent or pre-curing, in order to investigate the curing effects on the matrix resin. The IFSSs of the MW-irradiated samples were significantly varied by the curing state of the epoxy resin and the surface condition of recycled CF, resulting that they were 99.5 to 131.7% of oven heated samples Furthermore, rheological measurements showed that the viscosity and shrinking behaviors of epoxy resin were affected based on the curing state of epoxy resin before MW irradiation. PMID:29587422

  19. Curing Effects on Interfacial Adhesion between Recycled Carbon Fiber and Epoxy Resin Heated by Microwave Irradiation.

    PubMed

    Tominaga, Yuichi; Shimamoto, Daisuke; Hotta, Yuji

    2018-03-26

    The interfacial adhesion of recycled carbon fiber (CF) reinforced epoxy composite heated by microwave (MW) irradiation were investigated by changing the curing state of the epoxy resin. The recycled CF was recovered from the composite, which was prepared by vacuum-assisted resin transfer molding, by thermal degradation at 500 or 600 °C. Thermogravimetric analysis showed that the heating at 600 °C caused rough damage to the CF surface, whereas recycled CF recovered at 500 °C have few defects. The interfacial shear strength (IFSS) between recycled CF and epoxy resin was measured by a single-fiber fragmentation test. The test specimen was heated by MW after mixing the epoxy resin with a curing agent or pre-curing, in order to investigate the curing effects on the matrix resin. The IFSSs of the MW-irradiated samples were significantly varied by the curing state of the epoxy resin and the surface condition of recycled CF, resulting that they were 99.5 to 131.7% of oven heated samples Furthermore, rheological measurements showed that the viscosity and shrinking behaviors of epoxy resin were affected based on the curing state of epoxy resin before MW irradiation.

  20. Separation of aliphatic carboxylic acids and benzenecarboxylic acids by ion-exclusion chromatography with various cation-exchange resin columns and sulfuric acid as eluent.

    PubMed

    Ohta, Kazutoku; Ohashi, Masayoshi; Jin, Ji-Ye; Takeuchi, Toyohide; Fujimoto, Chuzo; Choi, Seong-Ho; Ryoo, Jae-Jeong; Lee, Kwang-Pill

    2003-05-16

    The application of various hydrophilic cation-exchange resins for high-performance liquid chromatography (sulfonated silica gel: TSKgel SP-2SW, carboxylated silica gel: TSKgel CM-2SW, sulfonated polymethacrylate resin: TSKgel SP-5PW, carboxylated polymethacrylate resins: TSKgel CM-5PW and TSKgel OA-Pak A) as stationary phases in ion-exclusion chromatography for C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, butyric, isovaleric, valeric, isocaproic, caproic, 2-methylhexanoic and heptanoic acids) and benzenecarboxylic acids (pyromellitic, trimellitic, hemimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic, salicylic acids and phenol) was carried out using diluted sulfuric acid as the eluent. Silica-based cation-exchange resins (TSKgel SP-2SW and TSKgel CM-2SW) were very suitable for the ion-exclusion chromatographic separation of these benzenecarboxylic acids. Excellent simultaneous separation of these benzenecarboxylic acids was achieved on a TSKgel SP-2SW column (150 x 6 mm I.D.) in 17 min using a 2.5 mM sulfuric acid at pH 2.4 as the eluent. Polymethacrylate-based cation-exchange resins (TSKgel SP-5PW, TSKgel CM-5PW and TSKgel OA-Pak A) acted as advanced stationary phases for the ion-exclusion chromatographic separation of these C1-C7 aliphatic carboxylic acids. Excellent simultaneous separation of these C1-C7 acids was achieved on a TSKgel CM-5PW column (150 x 6 mm I.D.) in 32 min using a 0.05 mM sulfuric acid at pH 4.0 as the eluent.

  1. Assessment of surface hardness of acrylic resins submitted to accelerated artificial aging.

    PubMed

    Tornavoi, D C; Agnelli, J A M; Lepri, C P; Mazzetto, M O; Botelho, A L; Soares, R G; Dos Reis, A C

    2012-06-01

    The aim of this study was to assess the influence of accelerated artificial aging (AAA) on the surface hardness of acrylic resins. The following three commercial brands of acrylic resins were tested: Vipi Flash (autopolymerized resin), Vipi Wave (microwave heat-polymerized resin) and Vipi Cril (conventional heat-polymerized resin). To perform the tests, 21 test specimens (65x10x3 mm) were made, 7 for each resin. Three surface hardness readings were performed for each test specimen, before and after AAA, and the means were submitted to the following tests: Kolmogorov-Smirnov (P>0.05), Levene Statistic, Two-way ANOVA, Tukey Post Hoc (P<0.05) with the SPSS Statistical Software 17.0. The analysis of the factors showed significant differences in the hardness values (P<0.05). Before aging, the autopolymerized acrylic resin Vipi Flash showed lower hardness values when compared with the heat-polymerized resin Vipi Cril (P=0.001). After aging, the 3 materials showed similar performance when compared among them. The Vipi Cril was the only one affected by AAA and showed lower hardness values after this procedure (Pp=0.003). It may be concluded that accelerated artificial aging influenced surface hardness of heat-polymerized acrylic resin Vipi Cril.

  2. Improved high-temperature resistant matrix resins

    NASA Technical Reports Server (NTRS)

    Green, H. E.; Chang, G. E.; Wright, W. F.; Ueda, K.; Orell, M. K.

    1989-01-01

    A study was performed with the objective of developing matrix resins that exhibit improved thermo-oxidative stability over state-of-the-art high temperature resins for use at temperatures up to 644 K (700 F) and air pressures up to 0.7 MPa (100 psia). The work was based upon a TRW discovered family of polyimides currently licensed to and marketed by Ethyl Corporation as EYMYD(R) resins. The approach investigated to provide improved thermo-oxidative properties was to use halogenated derivatives of the diamine, 2, 2-bis (4-(4-aminophenoxy)phenyl) hexafluoropropane (4-BDAF). Polyimide neat resins and Celion(R) 12,000 composites prepared from fluorine substituted 4-BDAF demonstrated unexpectedly lower glass transition temperatures (Tg) and thermo-oxidative stabilities than the baseline 4-BDAF/PMDA polymer.

  3. Influence of resin formulation variables on bond quality of southern pine plywood

    Treesearch

    Chung-Yun Hse

    1972-01-01

    Thirty-six resins, ach with two replicates, were factorially prepared with three forumlation variables: molar ratios of sodium hydroxide to phenol of 0.4, 0.7, and 1.0; levels of resin solids content of 37, 40, and 43 percent; and molar ratiios of formaldehyde to phenol of 1.6, 1.9, 2.2, and 2.5. Glue bond quality decreased substantially with a change of NaOH/phenol...

  4. Influence of resin formulation variables on bond quality of southern pine plywood

    Treesearch

    C. -Y. Hse

    1972-01-01

    Thirty-six resins, each with two replicates, were factorially prepared with three formulation variables: molar ratios of sodium hydroxide to phenol of 0.4, 0.7, and 1.0; levels of resin solids content of 37, 40, and 43 percent; and molar ratios of formaldehyde to phenol of 1.6, 1.9, 2.2, and 2.5. Glue bond quality decreased substantially with a change of NaOH/phenol...

  5. Development of an early warning sensor and network for brown-\\0xAD\\0x2010out conditions.

    DOT National Transportation Integrated Search

    2016-03-31

    Brownout conditions on motorways are caused by windblown dust and sand from upwind areas where : soils are susceptible to wind erosion. Owing in part to prolonged droughts that have dried : soils and denuded vegetation and biological crusts, large, m...

  6. COMPARISON OF SAMPLING METHODS FOR SEMI-VOLATILE ORGANIC CARBON (SVOC) ASSOCIATED WITH PM 2.5

    EPA Science Inventory

    This study evaluates the influence of denuder sampling methods and filter collection media on the measurement of semi-volatile organic carbon (SVOC) associated with PM2.5. Two types of collection media, charcoal (activated carbon) and XAD, were used both in diffusion denuders ...

  7. COMPARISON OF SAMPLING METHODS FOR SEMI-VOLATILE ORGANIC CARBON ASSOCIATED WITH PM 2.5

    EPA Science Inventory

    This study evaluates the influence of denuder sampling methods and filter collection media on the measurement of semi-volatile organic carbon (SVOC) associated with PM2.5. Two types of collection media, charcoal (activated carbon) and XAD, were used both in diffusion denuders ...

  8. METHODOLOGY OF AMBIENT AIR MONITORING FOR POLYCYCLIC AROMATIC HYDROCARBONS

    EPA Science Inventory

    In the last decade, several studies of polycyclic aromatic hydrocarbons (PAH) in ambient air in the U.S. specifically investigated (1) the sampling efficiency of two sorbents for PAH in air: XAD-2 and polyurethane foam (PUP); (2) the storage stability of PAH on quartz fiber fil...

  9. ASSESSING THE BIOAVAILABILITY OF PAHS IN FIELD-CONTAMINATED SEDIMENT USING XAD-2 ASSISTED DESORPTION

    EPA Science Inventory

    In the bioremediation of soils/sediments contaminated with polycyclic aromatic hydrocarbons (PAHs) it is imperative to determine the fraction of the PAHs that is amenable to remediation. For example, what fraction of the PAHs is available to the indigenous microorganisms, i.e. bi...

  10. Color stability of microfilled, microhybrid and nanocomposite resins--an in vitro study.

    PubMed

    Nasim, Iffat; Neelakantan, Prasanna; Sujeer, R; Subbarao, C V

    2010-01-01

    The aim of this study was to evaluate the effect of two beverages-Tea and Pepsi on the color stability of three different composite resins after a period of 7 and 30 days. Color stability of a microfilled, microhybrid and nanocomposite was evaluated after storage in Tea, a carbonated drink or Distilled Water for 7 and 30 days. Color measurement was done using reflectance spectrophotometer based on the CIE L*a*b* color scale. Mean values of the different groups were compared using three-way analysis of variance and multiple comparisons of the mean values were done using Tukey-Kramer test with 0.05 as significance level. All tested resin composites showed color change after a period of 7 and 30 days. The color change exhibited by all three groups was significantly different for all three beverages studied, at both time periods (p<0.05). Amongst the resin composites studied microhybrid composite was found to be more color stable. The microfilled composite discolored most in Distilled Water and Pepsi at the 7th and 30th day. The nanocomposite discolored most in Tea at 7th and 30th day. All efforts should be made to minimize discoloration of composite restorations by adopting excellent polishing techniques. Patients should also be educated on the possibility of the restoration to undergo staining under the influence of beverages. Copyright © 2010 Elsevier Ltd. All rights reserved.

  11. Effects of coronal substrates and water storage on the microhardness of a resin cement used for luting ceramic crowns

    PubMed Central

    de MENDONÇA, Luana Menezes; PEGORARO, Luiz Fernando; LANZA, Marcos Daniel Septímio; PEGORARO, Thiago Amadei; de CARVALHO, Ricardo Marins

    2014-01-01

    Composite resin and metallic posts are the materials most employed for reconstruction of teeth presenting partial or total destruction of crowns. Resin-based cements have been widely used for cementation of ceramic crowns. The success of cementation depends on the achievement of adequate cement curing. Objectives To evaluate the microhardness of Variolink® II (Ivoclar Vivadent, Schaan, Liechtenstein), used for cementing ceramic crowns onto three different coronal substrate preparations (dentin, metal, and composite resin), after 7 days and 3 months of water storage. The evaluation was performed along the cement line in the cervical, medium and occlusal thirds on the buccal and lingual aspects, and on the occlusal surface. Material and Methods Thirty molars were distributed in three groups (N=10) according to the type of coronal substrate: Group D- the prepared surfaces were kept in dentin; Groups M (metal) and R (resin)- the crowns were sectioned at the level of the cementoenamel junction and restored with metallic cast posts or resin build-up cores, respectively. The crowns were fabricated in ceramic IPS e.max® Press (Ivoclar Vivadent, Schaan, Liechtenstein) and luted with Variolink II. After 7 days of water storage, 5 specimens of each group were sectioned in buccolingual direction for microhardness measurements. The other specimens (N=5) were kept stored in deionized water at 37ºC for three months, followed by sectioning and microhardness measurements. Results Data were first analyzed by three-way ANOVA that did not reveal significant differences between thirds and occlusal surface (p=0.231). Two-way ANOVA showed significant effect of substrates (p<0.001) and the Tukey test revealed that microhardness was significantly lower when crowns were cemented on resin cores and tested after 7 days of water storage (p=0.007). Conclusion The type of material employed for coronal reconstruction of preparations for prosthetic purposes may influence the cement properties. PMID:25141200

  12. Examining exposure reciprocity in a resin based composite using high irradiance levels and real-time degree of conversion values.

    PubMed

    Selig, Daniela; Haenel, Thomas; Hausnerová, Berenika; Moeginger, Bernhard; Labrie, Daniel; Sullivan, Braden; Price, Richard B T

    2015-05-01

    Exposure reciprocity suggests that, as long as the same radiant exposure is delivered, different combinations of irradiance and exposure time will achieve the same degree of resin polymerization. This study examined the validity of exposure reciprocity using real time degree of conversion results from one commercial flowable dental resin. Additionally a new fitting function to describe the polymerization kinetics is proposed. A Plasma Arc Light Curing Unit (LCU) was used to deliver 0.75, 1.2, 1.5, 3.7 or 7.5 W/cm(2) to 2mm thick samples of Tetric EvoFlow (Ivoclar Vivadent). The irradiances and radiant exposures received by the resin were determined using an integrating sphere connected to a fiber-optic spectrometer. The degree of conversion (DC) was recorded at a rate of 8.5 measurements a second at the bottom of the resin using attenuated total reflectance Fourier Transform mid-infrared spectroscopy (FT-MIR). Five specimens were exposed at each irradiance level. The DC reached after 170s and after 5, 10 and 15 J/cm(2) had been delivered was compared using analysis of variance and Fisher's PLSD post hoc multiple comparison tests (alpha=0.05). The same DC values were not reached after the same radiant exposures of 5, 10 and 15 J/cm(2) had been delivered at an irradiance of 3.7 and 7.5 W/cm(2). Thus exposure reciprocity was not supported for Tetric EvoFlow (p<0.05). For Tetric EvoFlow, there was no significant difference in the DC when 5, 10 and 15J/cm(2) were delivered at irradiance levels of 0.75, 1.2 and 1.5 W/cm(2). The optimum combination of irradiance and exposure time for this commercial dental resin may be close to 1.5 W/cm(2) for 12s. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  13. Physical Properties of a New Sonically Placed Composite Resin Restorative Material

    DTIC Science & Technology

    2013-06-06

    General Dentistry Residency (AEGD-2) 3. School/DepartmenUCenter: Air Force Postgraduate Dental School (AFPDS) 4. Phone: 210-671-9822 5. Type of...9. Date of submission for USU approval: 7 June 2013 CHAIR OR DEPARTMENT HEAD APPROVAL 1. Name: Kraig S. Vandewalle, Director, Dental Research 2...claim of 5mm. INTRODUCTION Composite resin was first introduced in the 1960’s as an alternative to acrylic resins for esthetic dental restorations.1

  14. Bond strength of Bis-GMA and glass ionomer pit and fissure sealants using cyclic fatigue.

    PubMed

    Dewji, H R; Drummond, J L; Fadavi, S; Punwani, I

    1998-02-01

    The aim of the study was to determine the bond strength of glass ionomer and resin-modified glass ionomer sealants compared to Bis-GMA sealants using both static and cyclic fatigue shear testing. Four materials were evaluated: D, a Bis-GMA sealant with 10% phosphoric acid etchant; FC, a resin-modified glass ionomer sealant with 20% polyacrylic acid etchant; FD, a resin-modified glass ionomer sealant with 10% polyacrylic acid etchant; and FSC, a self-cured glass ionomer sealant with no etchant. Gelatin capsules filled with the sealant material were bonded to the enamel surfaces of bovine teeth after appropriate surface conditioning and then tested in shear static and cyclic fatigue. Static and cyclic shear bond strengths, respectively, for each group were (MPa): FC: 21.1+/-2.8 and 17.1+/-3.1; FD: 14.6+/-5.9 and 8.5+/-3.1; D: 10.8+/-4.9 and 4.7+/-2.6; FSC: 8.7 (1.0 and 2.9+/-0.6. The resin-modified glass ionomer sealants had better fatigue bond strength than both Bis-GMA and self-cured glass ionomer sealants with the surface conditioning affecting the bond strength of the resin-modified glass ionomer sealants.

  15. A comparative study of the effects of 4-META/MMA-TBB resin and cyanoacrylate on wound healing of skin defects.

    PubMed

    Kidokoro, Ryo; Nakajima, Kei; Kobayashi, Fumitaka; Takeda, Yukihiro; Matsuzaka, Kenichi; Katakura, Akira; Inoue, Takashi

    2016-01-01

    The purpose of this study was to investigate the healing process of wounded skin following the application of cyanoacrylate or a 4-(2-methacryloxyethyl) trimellitic anhydride/methyl methacrylate-tributylborane resin (4-META resin). Those materials were applied to skin wound areas in rats, and the regenerating tissues were biopsied and examined at days 1, 3, 5, 7, and 14. Paraffin-embedded specimens were sectioned and stained with hematoxylin and eosin or with Azan-Mallory stain. Sections were also immunohistochemically stained with Pan-cytokeratin and CD68 antibodies. In cyanoacrylate-treated wounds, CD68-positive cells were observed in the connective tissue and their number increased up to day 5. The wound surface was completely covered by epithelial tissue at day 14. In 4-META resin-treated wounds, CD68-positive cells appeared in the soft-tissue hybrid layer (STHL) and epithelial tissue had migrated under the STHL by day 5. The wound surface was completely covered by epithelial tissue at day 7. CD68-positive cells were distributed over the entire area of the cyanoacrylate-treated wounds, but accumulated under the STHL in the 4-META resin-treated wounds. In conclusion, the results suggest that covering skin defects with a 4-META resin is an effective strategy to promote wound healing compared to cyanoacrylate. © 2015 Wiley Periodicals, Inc.

  16. Synthesis of CuPF6 -(S)-BINAP loaded resin and its enantioselectivity toward phenylalanine enantiomers.

    PubMed

    Liu, Xiong; Zhou, Wenqi; Xu, Longqi

    2017-09-01

    A type of resin-anchored CuPF 6 -(S)-BINAP was synthesized and identified. The PS-CuPF 6 -(S)-BINAP resin was used to adsorb the phenylalanine enantiomers. The results showed that the adsorption capacity of PS-CuPF 6 -(S)-BINAP resin toward L-phenylalanine was higher than that of resin toward D-phenylalanine. PS-CuPF 6 -(S)-BINAP resin exhibited good enantioselectivity toward L-phenylalanine and D-phenylalanine. The influence of phenylalanine concentration, pH, adsorption time, and temperature on the enantioselectivity of the resin were investigated. The results showed that the enantioselectivity of the resin increased with increasing the phenylalanine concentration, pH, and adsorption time, while it decreased with an increase in temperature. The causes for these influences are discussed. The highest enantioselectivity (α = 2.81) was obtained when the condition of phenylalanine concentration was 0.05 mmol/mL, pH was 8, adsorption time was 12 h, and temperature 5°C. The desorption test for removing D/L-phenylalanine on PS-CuPF 6 -(S)-BINAP resin was also investigated. The desorption ratios of D-phenylalanine and L-phenylalanine at pH of 1 were 95.7% and 94.3%, respectively. This result indicated that the PS-CuPF 6 -(S)-BINAP resin could be regenerated by shaking with an acidic solution. The reusability of the PS-CuPF 6 -(S)-BINAP resin was also assessed and the resin exhibited considerable reusability. © 2017 Wiley Periodicals, Inc.

  17. Enrichment and Purification of Total Ginkgo Flavonoid O-Glycosides from Ginkgo Biloba Extract with Macroporous Resin and Evaluation of Anti-Inflammation Activities In Vitro.

    PubMed

    Zhang, Lihu; Wu, Tingting; Xiao, Wei; Wang, Zhenzhong; Ding, Gang; Zhao, Linguo

    2018-05-13

    In the present study, the performance and separation characteristics of six macroporous resins for the enrichment and purification of total ginkgo flavonoid O -glycosides (TGFs) (quercetin (I), kaempferol (II), isorhamnetin (III)) from Ginkgo Biloba extracts (EGB) are evaluated. The adsorption and desorption properties of TGFs are studied on macroporous resins, including D101, D201, AB-8, HPD400, D301, and D311. Along with the results, AB-8 resin exhibits the best adsorption and desorption capacity for these three ginkgo flavonoid O -glycosides among the six resins. Adsorption isotherms are created on AB-8 resin and fit well to the Langmuir (R² > 0.96) and Freundlich (R² > 0.92, 0.3 < 1/n < 0.7) models. After the treatment with gradient elution on AB-8 resin packed chromatography column, the contents of the three main ginkgo flavonoid O -glycosides (I, II, and III) increase from 8.93%, 9.88%, and 6.11% in the extracts to 30.12%, 35.21%, and 14.14%, respectively, in the product. The recoveries of compounds I, II, and III are 88.76%, 93.78%, and 60.90%, respectively. Additionally, the anti-inflammatory effects of TGFs are evaluated in LPS-treated RAW 264.7 macrophages, and the result demonstrates that TGFs could significantly inhibit LPS-induced NO release in vitro in a dose-dependent manner compared with the control group. These findings suggest that TGFs could potentially be natural antioxidants and anti-inflammatory ingredients that could be used in pharmaceutical products and functional food additives.

  18. Effects of tributylborane-activated adhesive and two silane agents on bonding computer-aided design and manufacturing (CAD/CAM) resin composite.

    PubMed

    Shinohara, Ayano; Taira, Yohsuke; Sawase, Takashi

    2017-10-01

    The present study was conducted to evaluate the effects of an experimental adhesive agent [methyl methacrylate-tributylborane liquid (MT)] and two adhesive agents containing silane on the bonding between a resin composite block of a computer-aided design and manufacturing (CAD/CAM) system and a light-curing resin composite veneering material. The surfaces of CAD/CAM resin composite specimens were ground with silicon-carbide paper, treated with phosphoric acid, and then primed with either one of the two silane agents [Scotchbond Universal Adhesive (SC) and GC Ceramic Primer II (GC)], no adhesive control (Cont), or one of three combinations (MT/SC, MT/GC, and MT/Cont). A light-curing resin composite was veneered on the primed CAD/CAM resin composite surface. The veneered specimens were subjected to thermocycling between 4 and 60 °C for 10,000 cycles, and the shear bond strengths were determined. All data were analyzed using analysis of variance and a post hoc Tukey-Kramer HSD test (α = 0.05, n = 8). MT/SC (38.7 MPa) exhibited the highest mean bond strengths, followed by MT/GC (30.4 MPa), SC (27.9 MPa), and MT/Cont (25.7 MPa), while Cont (12.9 MPa) and GC (12.3 MPa) resulted in the lowest bond strengths. The use of MT in conjunction with a silane agent significantly improved the bond strength. Surface treatment with appropriate adhesive agents was confirmed as a prerequisite for veneering CAD/CAM resin composite restorations.

  19. Highly sensitive determination of polycyclic aromatic hydrocarbons in ambient air dust by gas chromatography-mass spectrometry after molecularly imprinted polymer extraction.

    PubMed

    Krupadam, Reddithota J; Bhagat, Bhagyashree; Khan, Muntazir S

    2010-08-01

    A method based on solid--phase extraction with a molecularly imprinted polymer (MIP) has been developed to determine five probable human carcinogenic polycyclic aromatic hydrocarbons (PAHs) in ambient air dust by gas chromatography-mass spectrometry (GC-MS). Molecularly imprinted poly(vinylpyridine-co-ethylene glycol dimethacrylate) was chosen as solid-phase extraction (SPE) material for PAHs. The conditions affecting extraction efficiency, for example surface properties, concentration of PAHs, and equilibration times were evaluated and optimized. Under optimum conditions, pre-concentration factors for MIP-SPE ranged between 80 and 93 for 10 mL ambient air dust leachate. PAHs recoveries from MIP-SPE after extraction from air dust were between 85% and 97% and calibration graphs of the PAHs showed a good linearity between 10 and 1000 ng L(-1) (r = 0.99). The extraction efficiency of MIP for PAHs was compared with that of commercially available SPE materials--powdered activated carbon (PAC) and polystyrene-divinylbenzene resin (XAD)--and it was shown that the extraction capacity of the MIP was better than that of the other two SPE materials. Organic matter in air dust had no effect on MIP extraction, which produced a clean extract for GC-MS analysis. The detection limit of the method proposed in this article is 0.15 ng L(-1) for benzo[a]pyrene, which is a marker molecule of air pollution. The method has been applied to the determination of probable carcinogenic PAHs in air dust of industrial zones and satisfactory results were obtained.

  20. Controls on dissolved organic carbon quantity and chemical character in temperate rivers of North America

    USGS Publications Warehouse

    Hanley, Kevin W.; Wollheim, Wilfred M.; Salisbury, Joseph; Huntington, Thomas G.; Aiken, George R.

    2013-01-01

    Understanding the processes controlling the transfer and chemical composition of dissolved organic carbon (DOC) in freshwater systems is crucial to understanding the carbon cycle and the effects of DOC on water quality. Previous studies have identified watershed-scale controls on bulk DOC flux and concentration among small basins but fewer studies have explored controls among large basins or simultaneously considered the chemical composition of DOC. Because the chemical character of DOC drives riverine biogeochemical processes such as metabolism and photodegradation, accounting for chemical character in watershed-scale studies will improve the way bulk DOC variability in rivers is interpreted. We analyzed DOC quantity and chemical character near the mouths of 17 large North American rivers, primarily between 2008 and 2010, and identified watershed characteristics that controlled variability. We quantified DOC chemical character using both specific ultraviolet absorbance at 254 nm (SUVA254) and XAD-resin fractionation. Mean DOC concentration ranged from 2.1 to 47 mg C L−1 and mean SUVA254 ranged from 1.3 to 4.7 L mg C−1 m−1. We found a significant positive correlation between basin wetland cover and both bulk DOC concentration (R2 = 0.78; p < 0.0001) and SUVA254 (R2 = 0.91; p < 0.0001), while other land use characteristics were not correlated. The strong wetland relationship with bulk DOC concentration is similar to that found by others in small headwater catchments. However, two watersheds with extremely long surface water residence times, the Colorado and St. Lawrence, diverged from this wetland relationship. These results suggest that the role of riverine processes in altering the terrestrial DOC signal at the annual scale was minimal except in river systems with long surface water residence times. However, synoptic DOC sampling of both quantity and character throughout river networks will be needed to more rigorously test this finding. The inclusion of DOC chemical character will be vital to achieving a more complete understanding of bulk DOC dynamics in large river systems.

  1. Development of a process for separation of mogroside V from Siraitia grosvenorii by macroporous resins.

    PubMed

    Zhang, Min; Yang, Huihua; Zhang, Hongyang; Wang, Yuerong; Hu, Ping

    2011-08-25

    A separation method was developed for the preparative separation and enrichment of the non-caloric sweetener mogroside V from Siraitia grosvenorii. The adsorption properties of six macroporous resins were evaluated. Results showed that HZ 806 resin offered the best adsorption and desorption capacities. Based on the adsorption experiments on HZ 806, the adsorption data were found to fit the Freundlich model well. The pseudo-second-order kinetic model showed the highest correlation with the experimental results. Separation was performed with deionized water and 40% aqueous ethanol solution as mobile phases. In a typical run, 100 g of herb was processed and 3.38 g of mogroside V with a purity of 10.7% was harvested. This separation method provided a 15.1-fold increase in the purification factor from 0.5% to 10.7%. The present study showed that HZ 806 resins were effective for the separation and enrichment of mogroside V from S. grosvenorii.

  2. 40 CFR 1065.1109 - Post-test sampler disassembly and sample extraction.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 33 2014-07-01 2014-07-01 false Post-test sampler disassembly and... Semi-Volatile Organic Compounds § 1065.1109 Post-test sampler disassembly and sample extraction. This... environment as follows after the test: (1) Remove the PM filter, PUF plugs, and all the XAD-2 from the...

  3. QUANTIFICATION OF 2,4-D ON SOLID-PHASE EXPOSURE SAMPLING MEDIA BY LC/MS/MS

    EPA Science Inventory

    Three types of solid phase chemical exposure sampling media: cellulose, polyurethane foam (PUF) and XAD-2, were analyzed for 2,4-D and the amine salts of 2,4-D. Individual samples were extracted into acidified methanol and the extracts were analyzed via LC/MS/MS using electrospra...

  4. Bond Strength of Resin Cements to Dentin Using New Universal Bonding Agents

    DTIC Science & Technology

    2015-06-30

    34Bond Strength of Resin Cements to Dentin Using New Universal Bonding Agents" Materials Repaired with Composite Resin" 7. Intended publication...DoD- or US Gov’t-level policy, communications systems or weapons issues review"). *Note: It is DoD policy that clearance of information or material...University-, DoD- or US Gov’t-level policy, communications systems or weapons issues review"). *Note: It is DoD po/icy that clearance of

  5. Properties and reactivity of aquatic organic matter from an Amazonian floodplain system

    NASA Astrophysics Data System (ADS)

    Perez, M. A. P.; Benedetti, M. F.; Moreira-Turcq, P.

    2009-04-01

    The aim of this study was to characterize the nature of the bulk dissolved organic matter (DOM) in different types of environments in the Amazon River-floodplain system and determine the importance of two different fractions of dissolved organic matter onto adsorption processes that occurs through the transport of organic matter in the Amazon Basin. Seven samples were collected in the Amazon River - "Lago Grande de Curuai" floodplain system, in rising water levels cruise (March 2006). The samples were taken in the Amazon main stem, in white and black floodplain waters, and in the middle of a phytoplaktonic bloom. The bulk, dissolved (i.e. < 0.22 micrometer), hydrophobic (HPO) and transphilic (TPH) fractions extracted by XAD-8 and XAD-4 columns chromatography respectively were isolated. Organic carbon (OC) and total nitrogen (TN) concentrations, Specific UV absorbance (SUVA), Size-Exclusion Chromatography (SEC), d13C and d15N isotopes, and reactivity (acid-base titration) were characterized for these fractions. Adsorption experiments onto mineral phase from de surface sediment of the Curuai floodplain lake (rich in smectite and kaolinite) were realized with HPO and TPH fractions. The OC concentrations in the natural organic matter (Bulk and < 0.22 micrometer fractions) varied between 3.7-5.7 mg/L. The OC and TN concentrations varied between 510 - 528 mg C/g in the HPO fraction, and 408 - 462 mg C/g in the TPH compounds and between 14.3 - 17.6 mg N/g (HPO), and 22.1 - 30.0 mg N/g (TPH). The molecular weight of both fractions (HPO and TPH) didn't present significant variation. Both fractions presented high aromaticity and they were rich in carboxylic groups, although smaller values are systematically reported for the HPO fractions. The OM of the main stem was the most adsorbed, followed by the white water lake, the phytoplanktonic bloom, and black water lake sample. These results helped us to strengthen the hypothesis that the organic matter carried from the river and sediment in the floodplain is closely associated with mineral phase.

  6. 7 CFR 160.3 - Rosin defined.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ...) remains after distillation of the fatty acids from tall oil recovered from wood in the course of its chemical disintegration to produce cellulose. In addition to the free resin acids, rosin may contain relatively small proportions of fatty acids, resin esters and other esters, unsaponifiable resenes, and non...

  7. 7 CFR 160.3 - Rosin defined.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ...) remains after distillation of the fatty acids from tall oil recovered from wood in the course of its chemical disintegration to produce cellulose. In addition to the free resin acids, rosin may contain relatively small proportions of fatty acids, resin esters and other esters, unsaponifiable resenes, and non...

  8. Designing an antibacterial acrylic resin using the cosolvent method -Effect of ethanol on the optical and mechanical properties of a cold-cure acrylic resin.

    PubMed

    Nezu, Takashi; Nagano-Takebe, Futami; Endo, Kazuhiko

    2017-09-26

    Antimicrobial cetylpyridinium chloride (CPC) has low miscibility with acrylic resin monomer but can be homogeneously mixed using ethanol as a cosolvent. This study investigated the effects of ethanol addition on the properties of a cold-cure acrylic resin. Ethanol was an excellent cosolvent for CPC and methyl methacrylate monomer (MMA), but the cured resin exhibited a strong change in coloration to yellow (ΔE* ab >8) and a drastically reduced bending strength (from 97 to 25 MPa) and elastic modulus (from 2.7 to 0.6 GPa) when equal volumes of ethanol and monomer were used together, possibly due to the solvation and deactivation of radicals by ethanol. However, these unfavorable effects diminished when the ethanol/MMA ratio was reduced to 0.25, and became smaller when each specimen was depressurized and excess ethanol was removed. Thus, it may be possible to develop a molecularly uniform antibacterial acrylic resin with acceptable color and strength using this simple technique.

  9. Development of a multifunctional adhesive system for prevention of root caries and secondary caries

    PubMed Central

    Zhang, Ning; Melo, Mary A. S.; Chen, Chen; Liu, Jason; Weir, Michael D.; Bai, Yuxing; Xu, Hockin H. K.

    2015-01-01

    Objectives The objectives of this study were to: (1) develop a novel adhesive for prevention of tooth root caries and secondary caries by possessing a combination of protein-repellent, antibacterial, and remineralization capabilities for the first time; and (2) investigate the effects of 2-methacryloyloxyethyl phosphorylcholine (MPC), dimethylaminohexadecyl methacrylate (DMAHDM), and nanoparticles of amorphous calcium phosphate (NACP) on dentine bond strength, protein-repellent properties, and dental plaque microcosm biofilm response. Methods MPC, DMAHDM and NACP were added into Scotchbond Multi-Purpose primer and adhesive. Dentine shear bond strengths were measured. Adhesive coating thickness, surface texture and dentine-adhesive interfacial structure were examined. Protein adsorption onto adhesive resin surface was determined by the micro bicinchoninic acid method. A human saliva microcosm biofilm model was used to investigate biofilm metabolic activity, colony-forming unit (CFU) counts, and lactic acid production. Results The resin with 7.5% MPC + 5% DMAHDM + 30% NACP did not adversely affect dentine shear bond strength (p > 0.1). The resin with 7.5% MPC + 5% DMAHDM + 30% NACP produced a coating on root dentine with a thickness of approximately 70 μm and completely sealed all the dentinal tubules. The resin with 7.5% MPC + 5% DMAHDM + 30% NACP had 95% reduction in protein adsorption, compared to SBMP control (p < 0.05). The resin with 7.5% MPC + 5% DMAHDM + 30% NACP was strongly antibacterial, with biofilm CFU being four orders of magnitude lower than that of SBMP control. Significance The novel multifunctional adhesive with strong protein-repellent, antibacterial and remineralization properties is promising to coat tooth roots to prevent root caries and secondary caries. The combined use of MPC, DMAHDM and NACP may have wide applicability to bonding agents, cements, sealants and composites to inhibit caries. PMID:26187532

  10. Feasibility study on the development of tough, moisture-resistant laminating resins

    NASA Technical Reports Server (NTRS)

    Brand, R. A.; Harrison, E. S.

    1979-01-01

    The potential of cyanate resins as replacement for epoxy resins in composites with graphite fiber reinforcement was investigated in an effort to provide improved moisture resistance and toughness in laminating systems at a projected cost, handleability, and processing requirements equivalent to 400 K (260 F) curing epoxies. Monomer synthesis, formulation, blending, resin preparation, catalysis studies, prepreg preparation, laminate fabrication, and testing are discussed. A graphite fiber reinforced laminate was developed with 95 percent retention of the original 363 K (180 F) flexural strength and 70 percent retention of the 363 K (180 F) short beam shear strength after 500 hour exposure to 95 + 7 relative humidity at 324 K (120 F).

  11. Influence of ozone and paracetic acid disinfection on adhesion of resilient liners to acrylic resin.

    PubMed

    Ekren, Orhun; Ozkomur, Ahmet

    2016-08-01

    The aim of this study was to evaluate the effect of paracetic acid (PAA) and ozone disinfection on the tensile bond strength (TBS) of silicone-based resilient liners to acrylic resins. One hundred and twenty dumbbell shaped heat-polymerized acrylic resins were prepared. From the mid segment of the specimens, 3 mm of acrylic were grinded off and separated parts were reattached by resilient liners. The specimens were divided into 2 control (control1, control7) and 4 test groups of PAA and ozone disinfection (PAA1, PAA7, ozone1 and ozone7; n=10). While control groups were immersed in distilled water for 10 min (control1) and 7 days (control7), test groups were subjected to PAA (16 g/L) or ozone rich water (4 mg/L) for 1 cycle (10 min for PAA and 60 min for ozone) per day for 7 days prior to tensile tests. Measurements of the TBS were analyzed using 3-way ANOVA and Tukey's HSD test. Adhesive strength of Mollosil decreased significantly by application of ozone disinfection. PAA disinfection had no negative effect on the TBS values of Mollosil and Molloplast B to acrylic resin. Single application of ozone disinfection did not have any negative effect on TBS values of Molloplast B, but prolonged exposure to ozone decreased its adhesive strength. The adhesion of resilient liners to acrylic was not adversely affected by PAA disinfection. Immersion in ozonated water significantly decreased TBS of Mollosil. Prolonged exposure to ozone negatively affects adhesion of Molloplast B to denture base materials.

  12. Comparative study for separation of atmospheric humic-like substance (HULIS) by ENVI-18, HLB, XAD-8 and DEAE sorbents: elemental composition, FT-IR, 1H NMR and off-line thermochemolysis with tetramethylammonium hydroxide (TMAH).

    PubMed

    Fan, Xingjun; Song, Jianzhong; Peng, Ping'an

    2013-11-01

    Humic-like substances (HULIS) are significant constituents of aerosols, and the isolation and characterization of HULIS by solid-phase extraction methods are dependent on the sorbents used. In this study, we used the following five methods: ENVI-18, HLB-M, HLB-N, XAD-8 and DEAE, to isolate atmospheric HULIS at an urban site. Then we conducted a comparative investigation of the HULIS chemical characteristics by means of elemental analysis, Fourier transform infrared spectroscopy, (1)H nuclear magnetic resonance spectroscopy and off-line thermochemolysis with tetramethylammonium hydroxide. The results indicate that HULIS isolated using different methods show many similarities in chemical composition and structure. Some differences were however also observed between the five isolated HULIS: HULISHLB-M contains a relatively high content of OCH group, compared to HULISENVI-18 and HULISXAD-8; HULISXAD-8 contains a relatively high content of hydrophobic and aromatic components, compared to HULISENVI-18 and HULISHLB-M; HULISDEAE contains the highest content of aromatic functional groups, as inferred by (1)H NMR spectra, but a great amount of salts generally present in the HULISDEAE and thereby limited the choices for characterizing the materials (i.e., elemental analysis and TMAH thermochemolysis); HULISHLB-N has relatively high levels of H and N, a high N/C atomic ratio, and includes N-containing functional groups, which suggests that it has been altered by 2% ammonia introduced in the eluents. In summary, we found that ENVI-18, HLB-M, and XAD-8 are preferable methods for isolation and characterization of HULIS in atmospheric aerosols. These results also suggest that caution is required when applying DEAE and HLB-N isolating methods for characterizing atmospheric HULIS. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. 21 CFR 177.1500 - Nylon resins.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ...-benzenedimethanamine, and alpha-(3-aminopropyl)-omega-(3-amino-propoxy)poly- oxyethylene under such conditions that the alpha-(3-amino-propyl)-omega-(3-aminopropoxy) polyoxyethylene monomer content does not exceed 7 percent... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Nylon resins. 177.1500 Section 177.1500 Food and...

  14. Physico-mechanical properties of resin cement light cured through different ceramic spacers.

    PubMed

    Rizzante, Fabio Antonio Piola; Locatelli, Paula Minatel; Porto, Thiago Soares; Borges, Ana Flávia Sanches; Mondelli, Rafael Francisco Lia; Ishikiriama, Sérgio Kiyoshi

    2018-06-04

    The purpose of this in vitro study was to compare the micro hardness, color stability/ΔE, and degree of conversion/DC of a resin cement light cured through different ceramic spacers. Lithium-disilicate ceramic samples were obtained from IPS E-max CAD blocks (HT A1) and IPS in-Ceram (transparent neutral); and divided in 7 groups (n = 8 for each test): CTR/control group; 06 M/0.6 mm monolithic; 12 M/1.2 mm monolithic; 20 M/2.0 mm monolithic; 06B/0.4 + 0.2 mm bilayered; 12B/1.0 + 0.2 mm bilayered; 20B/1.8 + 0.2 mm bilayered. The resin cement (Variolink veneer) was light cured through the ceramic spacers. The resin cement samples were evaluated for ΔE using a spectrophotometer after 24 h, 7days and after aging (24 h in water at 60 °C). Knoop microhardness and DC tests were conducted immediately after light curing, after 24 h and 7days. All experimental groups showed similar microhardness values, although being lower than CTR group. Similar results were observed after 7days. ΔE was similar between all groups after 24 h (except for 12B and 20B), and increased for all groups after 7days and after artificial aging, especially for thicker and bilayer groups. Only 06 M showed values similar to CTR group. DC values were similar to all groups immediately after light curing, increasing after 24 h and 7days. After 7days, only group 20B showed lower DC than CTR group. A tendency of higher DC could be observed for monolithic and thinner ceramics. All test results showed strong correlation (0.9987). Ceramic interposition can reduce mechanical and physical properties of resin cements, especially with thicker and bilayered ceramics. Group 06 M showed the best ΔE overtime. Published by Elsevier Ltd.

  15. Clinical Evaluation of Indirect Particle-Filled Composite Resin CAD/CAM Partial Crowns after 24 Months.

    PubMed

    Zimmermann, Moritz; Koller, Christina; Reymus, Marcel; Mehl, Albert; Hickel, Reinhard

    2017-04-19

    Resin-based CAD/CAM compound materials might be promising for single-tooth restorations. Insufficient clinical data are available for this new material class. The purpose of this study was to describe initial clinical in vivo results for indirect particle-filled composite resin CAD/CAM restorations after 24 months. Indirect particle-filled composite resin restorations were fabricated with a CAD/CAM method (CEREC Bluecam intraoral scanner, CEREC MCXL milling unit) by calibrated dental students. Forty-two partial crown restorations were seated adhesively in 30 patients with caries lesions or insufficient restorations (baseline). Strict inclusion criteria were defined for the patient collective. Follow-up evaluation comprised 40 restorations after 12 months and 33 restorations after 24 months. Evaluation criteria were modified FDI criteria with grades (1) to (5). Rating with FDI criteria (5) was defined as clinical failure. Statistical analysis was performed with Wilcoxon-Test (p < 0.05). The success rate of indirect particle-filled composite resin CAD/CAM restorations after 12 months was 95.0% with two debondings observed. The cumulative success rate for indirect particle-filled composite resin CAD/CAM restorations after 24 months was 85.7% with two tooth fractures and one debonding. Statistically significant differences were found for baseline and 24-month follow-up evaluation for anatomic form and marginal adaptation criterion examined in respect to FDI criteria guidelines (Wilcoxon-Test, p < 0.05). This study demonstrates particle-filled composite resin CAD/CAM restorations having a clinical success rate of 85.7% after 24 months. Adhesive bonding procedures need to be ensured carefully. A longer clinical evaluation period is necessary to draw further conclusions. © 2017 by the American College of Prosthodontists.

  16. Boswellia gum resin/chitosan polymer composites: Controlled delivery vehicles for aceclofenac.

    PubMed

    Jana, Sougata; Laha, Bibek; Maiti, Sabyasachi

    2015-01-01

    This study was undertaken to evaluate the effect of Boswellia gum resin on the properties of glutaraldehyde (GA) crosslinked chitosan polymer composites and their potential as oral delivery vehicles for a non-steroidal anti-inflammatory drug, aceclofenac. The incorporation of resinous material caused a significant improvement in drug entrapment efficiency (∼40%) of the polymer composites. Fourier transform infrared (FTIR) spectroscopic analysis confirmed the formation of chitosan-gum resin composites and did not show any evidence of drug-polymer chemical interaction. Field emission scanning electron microscopy (FE-SEM) suggested the formation of particulate polymer composites up to chitosan:gum resin mass ratio of 1:3. Only 8-17% drug was released into HCl solution (pH 1.2) in 2h. The drug release rate of polymer composites was faster in phosphate buffer solution (pH 6.8). The composites released ∼60-68% drug load in 7h. In same duration, the drug release rate suddenly boosted up to 92% as the concentration of gum resin in the composites was raised to 80%. The drug release mechanism deviated from non-Fickian to case-II type with increasing resin concentration in the composites. Hence, GA-treated Boswellia resin-chitosan composites could be considered as alternative vehicles for oral delivery of aceclofenac. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Bonding resin thixotropy and viscosity influence on dentine bond strength.

    PubMed

    Niem, Thomas; Schmidt, Alexander; Wöstmann, Bernd

    2016-08-01

    To investigate the influence of bonding resin thixotropy and viscosity on dentine tubule penetration, blister formation and consequently on dentine bond strength as a function of air-blowing pressure (air-bp) intensity. Two HEMA-free, acetone-based, one-bottle self-etch adhesives with similar composition except disparate silica filler contents and different bonding resin viscosities were investigated. The high-filler-containing adhesive (G-Bond) featured a lower viscous bonding resin with inherent thixotropic resin (TR) properties compared to the low-filler-containing adhesive (iBond) exhibiting a higher viscous bonding resin with non-thixotropic resin (NTR) properties. Shear bond strength tests for each adhesive with low (1.5bar; 0.15MPa; n=16) and high (3.0bar; 0.30MPa; n=16) air-bp application were performed after specimen storage in distilled water (24h; 37.0±1.0°C). Results were analysed using a Student's t-test to identify statistically significant differences (p<0.05). Fracture surfaces of TR adhesive specimens were morphologically characterised by SEM. Statistically significant bond strength differences were obtained for the thixotropic resin adhesive (high-pressure: 24.6MPa, low-pressure: 9.6MPa). While high air-bp specimens provided SEM images revealing resin-plugged dentine tubules, resin tags and only marginally blister structures, low air-bp left copious droplets and open dentine tubules. In contrast, the non-thixotropic resin adhesive showed no significant bond strength differences (high-pressure: 9.3MPa, low-pressure: 7.6MPa). A pressure-dependent distinct influence of bonding resin thixotropy and viscosity on dentine bond strength has been demonstrated. Stronger adhesion with high air-bp application is explained by improved resin fluidity and facilitated resin penetration into dentine tubules. Filler particles used in adhesive systems may induce thixotropic effects in bonding resin layers, accounting for improved free-flowing resin properties. In combination with high air-bp this effect allows an easy plugging of dentine tubules and elimination of blister structures, both resulting in superior dentine bond strength. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. One pot synthesis of chitosan grafted quaternized resin for the removal of nitrate and phosphate from aqueous solution.

    PubMed

    Banu, H Thagira; Meenakshi, Sankaran

    2017-11-01

    The present study deals with the synthesis of chitosan quaternized resin for efficient removal of nitrate and phosphate from aqueous solution. The resin was characterized with FTIR, SEM with EDX and XRD. Batch method was carried out to optimize various parameters such as contact time, initial concentration of nitrate and phosphate, dosage, pH, co-anions and temperature on the adsorption capacity of the adsorbent. The adsorption process illustrated that the Freundlich isotherm and the pseudo-second order are the best fitted models for the sorption of both anions. The respective negative values of ΔH° and ΔG° revealed that the adsorption of both the anions were exothermic and spontaneous. The removal efficiency of nitrate and phosphate on chitosan quaternized resin were 78% and 90% respectively with 0.1g of adsorbent and the initial concentration as 100mg/L. Nitrate and phosphate anions adsorbed effectively on chitosan quaternized resin by replacing Cl - ions from quaternary site through electrostatic attraction as well as ion-exchange mechanism. Hydrogen bonding also played important role in adsorption process. Even after 7th regeneration cycle the adsorbent retained its adsorption capacity as 23.7mg/g and 30.4mg/g for both nitrate and phosphate respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Enhanced biocatalytic production of L-cysteine by Pseudomonas sp. B-3 with in situ product removal using ion-exchange resin.

    PubMed

    Wang, Pu; He, Jun-Yao; Yin, Jiang-Feng

    2015-03-01

    Bioconversion of DL-2-amino-Δ(2)-thiazoline-4-carboxylic acid (DL-ATC) catalyzed by whole cells of Pseudomonas sp. was successfully applied for the production of L-cysteine. It was found, however, like most whole-cell biocatalytic processes, the accumulated L-cysteine produced obvious inhibition to the activity of biocatalyst and reduced the yield. To improve L-cysteine productivity, an anion exchange-based in situ product removal (ISPR) approach was developed. Several anion-exchange resins were tested to select a suitable adsorbent used in the bioconversion of DL-ATC for the in situ removal of L-cysteine. The strong basic anion-exchange resin 201 × 7 exhibited the highest adsorption capacity for L-cysteine and low adsorption for DL-ATC, which is a favorable option. With in situ addition of 60 g L(-1) resin 201 × 7, the product inhibition can be reduced significantly and 200 mmol L(-1) of DL-ATC was converted to L-cysteine with 90.4 % of yield and 28.6 mmol L(-1 )h(-1) of volumetric productivity. Compared to the bioconversion without the addition of resin, the volumetric productivity of L-cysteine was improved by 2.27-fold using ISPR method.

  20. FT-Raman spectroscopy study of organic matrix degradation in nanofilled resin composite.

    PubMed

    Soares, Luís Eduardo Silva; Nahórny, Sídnei; Martin, Airton Abrahão

    2013-04-01

    This in vitro study evaluated the effect of light curing unit (LCU) type, mouthwashes, and soft drink on chemical degradation of a nanofilled resin composite. Samples (80) were divided into eight groups: halogen LCU, HS--saliva (control); HPT--Pepsi Twist®; HLC--Listerine®; HCP--Colgate Plax®; LED LCU, LS--saliva (control); LPT--Pepsi Twist®; LLC--Listerine®; LCP--Colgate Plax®. The degree of conversion analysis and the measure of the peak area at 2,930 cm-1 (organic matrix) of resin composite were done by Fourier-transform Raman spectroscopy (baseline, after 7 and 14 days). The data were subjected to multifactor analysis of variance (ANOVA) at a 95% confidence followed by Tukey's HSD post-hoc test. The DC ranged from 58.0% (Halogen) to 59.3% (LED) without significance. Differences in the peak area between LCUs were found after 7 days of storage in S and PT. A marked increase in the peak intensity of HLC and LLC groups was found. The soft-start light-activation may influence the chemical degradation of organic matrix in resin composite. Ethanol contained in Listerine® Cool Mint mouthwash had the most significant degradation effect. Raman spectroscopy is shown to be a useful tool to investigate resin composite degradation.

  1. Effect of Light-Cured Resin Cement Application on Translucency of Ceramic Veneers and Light Transmission of LED Polymerization Units.

    PubMed

    Zhang, Lei; Luo, Xiao Ping; Tan, Ren Xiang

    2018-05-31

    To evaluate the effect of light-cured resin cement application based on etching and silanization on the translucent property of ceramic veneers in different thicknesses, testing the hypothesis that the surface treatment and subsequent resin cement application could influence the translucency of ceramic veneers. The relationship between translucency of ceramic veneers and light transmission irradiated by LED polymerization units was also determined. 40 specimens (10 mm diameter) were fabricated from IPS e.max Press HT A2 ceramic ingots, and polished to 0.3 ± 0.01 mm, 0.5 ± 0.01 mm, 0.7 ± 0.01 mm, 1.0 ± 0.01 mm, and 1.5 ± 0.01 mm thick (n = 8/group). One surface of each disc was etched with HF acid, silanized with Monobond-S, and applied with a light-cured resin cement (Variolink N Transparent Base). Before and after the above procedure, the total luminous transmittance (τ) of all specimens was assessed by a spectrophotometer in a wavelength range of 380-780 nm. A handheld radiometer was used to measure the light intensity irradiated by three LED polymerization units. Light transmission (LT) through ceramic specimens after resin cement application was calculated. Data were statistically analyzed using two-way ANOVA (p = 0.05) and Tukey's test. The correlation between translucency (τ) of ceramic veneers after resin cement application and light transmission (LT) of curing units was statistically evaluated using Spearman correlation test (p = 0.05). With the increase of ceramic thickness, the transmittance decreased significantly (p < 0.05). For the 0.3-mm, 0.5-mm, and 0.7-mm-thick groups, the transmittance of ceramic specimens was statistically significantly lower after resin cement application (p < 0.05). The r value of Bluephase C8 was 0.988, 0.977 for Bluphase, and 0.883 for Bluephase 20i, indicating that the light transmission (LT%) was positively correlated to the translucency of ceramic veneers, regardless of the type of curing units. After the light-cured resin cement application based on etching and silanization, the ceramic veneers (less than 0.7-mm thick) were less translucent, and the translucency decreased when the thickness increased. Because of the lower translucency of ceramic veneers, the light intensity of LED units transmitted to resin layer would decrease when curing. © 2018 by the American College of Prosthodontists.

  2. Inhibitory effect of zirconium oxide nanoparticles on Candida albicans adhesion to repaired polymethyl methacrylate denture bases and interim removable prostheses: a new approach for denture stomatitis prevention

    PubMed Central

    Gad, Mohammed M; Al-Thobity, Ahmad M; Shahin, Suliman Y; Alsaqer, Badar T; Ali, Aiman A

    2017-01-01

    Background Despite drawbacks, cold-cured acrylic resin is still the most common material used in denture repair. Zirconia nanoparticles were among the reinforcements added to increase the strength of the resin. The effect on Candida due to the addition of zirconia nanoparticles to the resin has not been investigated. Purpose The aim of this study was to evaluate the effect of zirconia nanoparticles added to cold-cured acrylic resin on Candida albicans adhesion. Materials and methods A total of 120 acrylic resin specimens with dimensions measuring 22×10×2.5 mm3 were prepared and divided into two equal groups. One group (repair) comprised heat-polymerized specimens that were sectioned at the center and prepared to create a 2 mm repair area that was repaired with cold-cured resin reinforced with 0% wt, 2.5% wt, 5% wt, and 7.5% wt zirconia nanoparticles. The second group contained intact cold-cured acrylic resin specimens reinforced with 0% wt, 2.5% wt, 5% wt, and 7.5% wt zirconia nanoparticles. Specimens were incubated at 37°C in artificial saliva containing C. albicans, and the effect of zirconia nanoparticles on C. albicans was assessed using two methods: 1) a slide count method and 2) a direct culture test. Variations in the number of living Candida were observed in relation to the different concentrations of zirconia nanoparticles. Analysis of variance (ANOVA) and post hoc Tukey’s tests were performed for data analysis. If the P-value was ≤0.05, then the difference was considered as statistically significant. Results It was found that C. albicans adhesion to repaired specimens was significantly decreased by the addition of zirconia nanoparticles (P<0.00001) in comparison with the control group. Intact cold-cured groups and groups repaired with cold-cured resin reinforced with 7.5% wt zirconia nanoparticles showed the lowest Candida count. Tukey’s test showed a significant difference between the repaired group and the intact cold-cured group, while the later demonstrated a lower Candida count. Conclusion The addition of zirconia nanoparticles to cold-cured acrylic resin is an effective method for reducing Candida adhesion to repaired polymethyl methacrylate (PMMA) denture bases and cold-cured removable prosthesis. Clinical significance Based on the results of the current study, zirconia nanoparticles have an antifungal effect, which could be incorporated in the repair material for repairing denture bases and in PMMA removable prostheses as a possible approach for denture stomatitis prevention. PMID:28814859

  3. Inhibitory effect of zirconium oxide nanoparticles on Candida albicans adhesion to repaired polymethyl methacrylate denture bases and interim removable prostheses: a new approach for denture stomatitis prevention.

    PubMed

    Gad, Mohammed M; Al-Thobity, Ahmad M; Shahin, Suliman Y; Alsaqer, Badar T; Ali, Aiman A

    2017-01-01

    Despite drawbacks, cold-cured acrylic resin is still the most common material used in denture repair. Zirconia nanoparticles were among the reinforcements added to increase the strength of the resin. The effect on Candida due to the addition of zirconia nanoparticles to the resin has not been investigated. The aim of this study was to evaluate the effect of zirconia nanoparticles added to cold-cured acrylic resin on Candida albicans adhesion. A total of 120 acrylic resin specimens with dimensions measuring 22×10×2.5 mm 3 were prepared and divided into two equal groups. One group (repair) comprised heat-polymerized specimens that were sectioned at the center and prepared to create a 2 mm repair area that was repaired with cold-cured resin reinforced with 0% wt, 2.5% wt, 5% wt, and 7.5% wt zirconia nanoparticles. The second group contained intact cold-cured acrylic resin specimens reinforced with 0% wt, 2.5% wt, 5% wt, and 7.5% wt zirconia nanoparticles. Specimens were incubated at 37°C in artificial saliva containing C. albicans , and the effect of zirconia nanoparticles on C. albicans was assessed using two methods: 1) a slide count method and 2) a direct culture test. Variations in the number of living Candida were observed in relation to the different concentrations of zirconia nanoparticles. Analysis of variance (ANOVA) and post hoc Tukey's tests were performed for data analysis. If the P -value was ≤0.05, then the difference was considered as statistically significant. It was found that C. albicans adhesion to repaired specimens was significantly decreased by the addition of zirconia nanoparticles ( P <0.00001) in comparison with the control group. Intact cold-cured groups and groups repaired with cold-cured resin reinforced with 7.5% wt zirconia nanoparticles showed the lowest Candida count. Tukey's test showed a significant difference between the repaired group and the intact cold-cured group, while the later demonstrated a lower Candida count. The addition of zirconia nanoparticles to cold-cured acrylic resin is an effective method for reducing Candida adhesion to repaired polymethyl methacrylate (PMMA) denture bases and cold-cured removable prosthesis. Based on the results of the current study, zirconia nanoparticles have an antifungal effect, which could be incorporated in the repair material for repairing denture bases and in PMMA removable prostheses as a possible approach for denture stomatitis prevention.

  4. [Curing mode of universal adhesives affects the bond strength of resin cements to dentin].

    PubMed

    Fu, Z R; Tian, F C; Zhang, L; Han, B; Wang, X Y

    2017-02-18

    To determine the effects of curing mode of one-step and two-step universal adhesives on the micro-tensile bond strength (μTBS) of different dual-cure resin cements to dentin. One-step universal adhesive Single Bond Universal (SBU), and two-step universal adhesive OptiBond Versa (VSA) were chosen as the subjects, one-step self-etching adhesive OptiBond All in One (AIO) and two-step self-etching adhesive Clearfil SE Bond (SEB) were control groups, and two dual-cure resin cements RelyX Ultimate (RLX) and Nexus 3 Universal (NX3) were used in this study. In this study, 80 extracted human molars were selected and the dentin surface was exposed using diamond saw. The teeth were divided into 16 groups according to the adhesives (AIO, SBU, SEB, VSA), cure modes of adhesives (light cure, non-light cure) and resin cements (RLX, NX3). The adhesives were applied on the dentin surface following the instruction and whether light cured or not, then the resin cements were applied on the adhesives with 1 mm thickness and light cured (650 mW/cm(2) for 20 s. A resin was built up (5 mm) on the cements and light cured layer by layer. After water storage for 24 h, the specimens were cut into resin-cement-dentin strips with a cross sectional area of 1 mm×1 mm and the μTBS was measured. Regarding one-step universal adhesive (SBU) light cured, the μTBS with RLX [(35.45±7.04) MPa] or NX3 [(26.84±10.39) MPa] were higher than SBU non-light cured with RLX [(17.93±8.93) MPa)] or NX3 [(10.07±5.89) MPa, P<0.001]. Compared with AIO, light-cured SBU combined with RLX presented higher μTBS than AIO group [(35.45±7.04) MPa vs. (24.86±8.42) MPa, P<0.05]. When SBU was not lighted, the μTBS was lower than AIO [(17.93±8.93) MPa vs. (22.28±7.57) MPa, P<0.05]. For two-step universal adhesive (VSA) and control adhesive (SEB), curing mode did not affect the μTBS when used with either RLX or NX3 (25.98-32.24 MPa, P>0.05). Curing mode of one-step universal adhesive may affect the μTBS between dual-cure resin cements and dentin, while for two-step universal adhesive, the curing mode and the type of resin cements did not influence the μTBS.

  5. Improved production and processing of ⁸⁹Zr using a solution target.

    PubMed

    Pandey, Mukesh K; Bansal, Aditya; Engelbrecht, Hendrik P; Byrne, John F; Packard, Alan B; DeGrado, Timothy R

    2016-01-01

    The objectives of the present work were to improve the cyclotron production yield of (89)Zr using a solution target, develop a practical synthesis of the hydroxamate resin used to process the target, and develop a biocompatible medium for (89)Zr elution from the hydroxamate resin. A new solution target (BMLT-2) with enhanced heat dissipation capabilities was designed by using helium-cooled dual foils (0.2 mm Al and 25 μ Havar) and an enhanced water-cooled, elongated solution cavity in the target insert. Irradiations were performed with 14 MeV protons on a 2M solution of yttrium nitrate in 1.25 M nitric acid at 40-μA beam current for 2 h in a closed system. Zirconium-89 was separated from Y by use of a hydroxamate resin. A one-pot synthesis of hydroxamate resin was accomplished by activating the carboxylate groups on a carboxymethyl cation exchange resin using methyl chloroformate followed by reaction with hydroxylamine hydrochloride. After trapping of (89)Zr on hydroxamate resin and rinsing the resin with HCl and water to release Y, (89)Zr was eluted with 1.2 M K2HPO4/KH2PO4 buffer (pH3.5). ICP-MS was used to measure metal contaminants in the final (89)Zr solution. The BMLT-2 target produced 349±49 MBq (9.4±1.2 mCi) of (89)Zr at the end of irradiation with a specific activity of 1.18±0.79 GBq/μg. The hydroxamate resin prepared using the new synthesis method showed a trapping efficiency of 93% with a 75 mg resin bed and 96-97% with a 100-120 mg resin bed. The elution efficiency of (89)Zr with 1.2M K2HPO4/KH2PO4 solution was found to be 91.7±3.7%, compared to >95% for 1 M oxalic acid. Elution with phosphate buffer gave very small levels of metal contaminants: Al=0.40-0.86 μg (n=2), Fe=1.22±0.71 μg (n=3), Y=0.29 μg (n=1). The BMLT-2 target allowed doubling of the beam current for production of (89)Zr, resulting in a greater than 2-fold increase in production yield in comparison with a conventional liquid target. The new one-pot synthesis of hydroxamate resin provides a simpler synthesis method for the (89)Zr trapping resin. Finally, phosphate buffer elutes the (89)Zrfrom the hydroxamate resin in high efficiency while at the same time providing a more biocompatible medium for subsequent use of (89)Zr. Copyright © 2015 Elsevier Inc. All rights reserved.

  6. RADIATION SOURCES

    DOEpatents

    Brucer, M.H.

    1958-04-15

    A novel long-lived source of gamma radiation especially suitable for calibration purposes is described. The source of gamma radiation is denoted mock iodine131, which comprises a naixture of barium-133 and cesium-137. The barium and cesium are present in a barium-cesium ratio of approximately 5.7/1 to 14/1, uniformly dispersed in an ion exchange resin and a filter surrounding the resin comprised of a material of atomic number below approximately 51, and substantially 0.7 to 0.9 millimeter thick.

  7. Outcomes of Radioembolization in the Treatment of Hepatocellular Carcinoma with Portal Vein Invasion: Resin versus Glass Microspheres.

    PubMed

    Biederman, Derek M; Titano, Joseph J; Tabori, Nora E; Pierobon, Elisa S; Alshebeeb, Kutaiba; Schwartz, Myron; Facciuto, Marcelo E; Gunasekaran, Ganesh; Florman, Sander; Fischman, Aaron M; Patel, Rahul S; Nowakowski, Francis S; Kim, Edward

    2016-06-01

    To compare outcomes of yttrium-90 radioembolization performed with resin-based ((90)Y-resin) and glass-based ((90)Y-glass) microspheres in the treatment of hepatocellular carcinoma (HCC) with associated portal vein invasion. A single-center retrospective review (January 2005-September 2014) identified 90 patients ((90)Y-resin, 21; (90)Y-glass, 69) with HCC and ipsilateral portal vein thrombosis (PVT). Patients were stratified according to age, sex, ethnicity, Child-Pugh class, Eastern Cooperative Oncology Group status, α-fetoprotein > 400 ng/mL, extent of PVT, tumor burden, and sorafenib therapy. Outcome variables included clinical and laboratory toxicities (Common Terminology Criteria Adverse Events, Version 4.03), imaging response (modified Response Evaluation Criteria in Solid Tumors), time to progression (TTP), and overall survival (OS). Grade 3/4 bilirubin and aspartate aminotransferase toxicities developed at a 2.8-fold (95% confidence interval [CI], 1.3-6.1) and 2.6-fold (95% CI, 1.1-6.1) greater rate in the (90)Y-resin group. The disease control rate was 37.5% in the (90)Y-resin group and 54.5% in the (90)Y-glass group (P = .39). The median (95% CI) TTP was 2.8 (1.9-4.3) months in the (90)Y-resin group and 5.9 (4.2-9.1) months in the (90)Y-glass group (P = .48). Median (95% CI) survival was 3.7 (2.3-6.0) months in the (90)Y-resin group and 9.4 (7.6-15.0) months in the (90)Y-glass group (hazard ratio, 2.6; 95% CI, 1.5-4.3, P < .001). Additional multivariate predictors of improved OS included age < 65 years, Eastern Cooperative Oncology Group status < 1, α-fetoprotein ≤ 400 ng/mL, and unilobar tumor distribution. Imaging response of (90)Y treatment in patients with HCC and PVT was not significantly different between (90)Y-glass and (90)Y-resin groups. Lower toxicity and improved OS were observed in the (90)Y-glass group. Copyright © 2016 SIR. Published by Elsevier Inc. All rights reserved.

  8. CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING AIR SAMPLES FOR ANALYSIS OF NEUTRAL PERSISTENT ORGANIC POLLUTANTS (SOP-5.12)

    EPA Science Inventory

    The method is for extracting an indoor and outdoor air sample consisting of a quartz fiber filter and an XAD-2 cartridge for analysis of neutral persistent organic pollutants. It covers the extraction and concentration of samples that are to be analyzed by gas chromatography/mass...

  9. Clinical survival of indirect, anterior 3-unit surface-retained fibre-reinforced composite fixed dental prosthesis: Up to 7.5-years follow-up.

    PubMed

    Kumbuloglu, Ovul; Özcan, Mutlu

    2015-06-01

    This prospective clinical study evaluated the performance of indirect, anterior, surface-retained, fibre-reinforced-composite restorations (ISFRCR). Between June-2003 and January-2011, a total of 134 patients (83 females, 51 males, 16-68 years old) received 175 ISFRCRs (local ethical registration number: 14/9/4). All restorations were made indirectly on a plaster model using unidirectional E-glass fibres (everStick C&B, StickTech) in combination with a laboratory resin composite (Dialogue, Schütz Dental) and cemented according to the instructions of 4 resin cements [(RelyX ARC, 3M-ESPE, n=61), Bifix DC, VOCO, n=45), Variolink II (Ivoclar Vivadent, n=32) and Multilink (Ivoclar Vivadent, n=37)]. After baseline recordings, patients were followed at 6 months and thereafter annually up to 7.5 years. The evaluation protocol involved technical (chipping, debonding or fracture of tooth/restoration) and biological failures (caries). Mean observation period was 58 months. Altogether, 13 failures were observed [survival rate: 97.7%] (Kaplan-Meier). One catastrophic fracture [(cement: RelyX ARC), eight partial debonding (cement: Bifix DC (5), Multilink (1), RelyX ARC (1), Variolink II (1)] and four delaminations of veneering composite [(cement: Bifix DC (2), RelyX ARC (1), Multilink (1)] were observed. Except one replacement, all defective restorations were repaired or recemented. Annual failure rate of ISFRCRs was 1.73%. The survival rates with the four resin cements did not show significant differences (RelyX ARC: 98.3%; Bifix DC: 93.5%; Variolink 2: 100%; Multilink: 100%) (p=0.114). Secondary caries did not occur in any of the teeth. The 3-unit anterior indirect surface-retained resin-bonded FRC FDPs showed similar clinical survival rate when cemented with the resin cements tested. Experienced failures in general were due to debonding of the restoration or delamination of the veneering composite. 3-unit surface retained resin-bonded FRC FDPs could be considered minimal invasive and cost-effective alternatives to conventional tooth- or implant-borne FDPs. Failures were mainly repairable in the form of chipping or debonding depending on the resin cement type. Copyright © 2015 Elsevier Ltd. All rights reserved.

  10. Chemical profile and pharmacological effects of the resin and essential oil from Bursera slechtendalii: A medicinal "copal tree" of southern Mexico.

    PubMed

    Villa-Ruano, Nemesio; Pacheco-Hernández, Yesenia; Becerra-Martínez, Elvia; Zárate-Reyes, José Alejo; Cruz-Durán, Ramiro

    2018-05-16

    This study reports on the volatile profile and pharmacological activities of the essential oil and resin from Bursera slechtendalii, an aromatic medicinal tree commercialized in southern Mexico. The essential oil contained 25 volatiles including p-cymen-8-ol (25.4-35.7%), n-hexyl hexanoate (6.8-17.6%) and n-octyl hexanoate (7.6-14.8%), whereas the crystallized resin contained 14 volatiles, including n-octyl acetate (29.6-34.2%), limonene (15.8-18.7%) and n-octyl butyrate (12.6-17-6%). The inhalation of vapors from the resin and essential oil caused a significant anxiolytic-like effect (p < .01) in ICR mice after 20 min of exposure at a dose of 50-150 mg L -1 . The prolonged inhalation of the essential oil (for 40 days, for 15 min, twice a day) produced a significant decrease (p < .01) in total cholesterol and LDL-c content as well as an increase of HDL-c levels in the same murine model. Interestingly, levels of hepatic lipid hydroperoxide decreased, whereas the hepatic activity of superoxide dismutase and glutathione peroxidase was significantly enhanced (P < .05). The detection of p-cymen-8-ol and n-octyl acetate in the plasma of mice strongly suggests their bioavailability and possible role in the biological activities described herein. Also, both the resin and essential oil from B. slechtendalii, as well as their main volatiles, showed a potent repellence activity against Aedes aegypti (p < .01). Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Evaluation of anion exchange resins Tulsion A-30 and Indion-930A by application of radioanalytical technique

    NASA Astrophysics Data System (ADS)

    Singare, P. U.

    2014-07-01

    Radioanalytical technique using 131I and 82Br was employed to evaluate organic based anion exchange resins Tulsion A-30 and Indion-930A. The evaluation was based on performance of these resins during iodide and bromide ion-isotopic exchange reactions. It was observed that for iodide ion-isotopic exchange reaction by using Tulsion A-30 resin, the values of specific reaction rate (min-1), amount of iodide ion exchanged (mmol), initial rate of iodide ion exchange (mmol/min) and log K d were 0.238, 0.477, 0.114, and 11.0, respectively, which was higher than 0.155, 0.360, 0.056, and 7.3, respectively as that obtained by using Indion-930A resins under identical experimental conditions of 40.0°C, 1.000 g of ion exchange resins and 0.003 M labeled iodide ion solution. Also at a constant temperature of 40.0°C, as the concentration of labeled iodide ion solution increases 0.001 to 0.004 M, for Tulsion A-30 resins the percentage of iodide ions exchanged increases from 59.0 to 65.1%, and from 46.4 to 48.8% for Indion-930A resins under identical experimental conditions. The identical trend was observed for both the resins during bromide ion-isotopic exchange reactions. The overall results indicate that under identical experimental conditions, Tulsion A-30 show superior performance over Indion-930A resins. The results of present experimental work have demonstrated that the radioanalytical technique used here can be successfully applied for characterization of different ion exchange resins so as to evaluate their performance under various process parameters.

  12. Effect of resin shades on opacity of ceramic veneers and polymerization efficiency through ceramics.

    PubMed

    Öztürk, Elif; Chiang, Yu-Chih; Coşgun, Erdal; Bolay, Şükran; Hickel, Reinhard; Ilie, Nicoleta

    2013-11-01

    The aim of this study was to assess the effect of different resin cement shades on the opacity and color difference of ceramics and to determine the polymerization efficiency of the resin cement at different shades after curing through ceramics. Two different ceramics (IPS e.max Press and IPS Empress(®)CAD, Ivoclar Vivadent) were used for this study. A light-cured veneer luting resin (Variolink Veneer, Ivoclar Vivadent) in four different shades of HV+1, HV+3, LV-1, and LV-3 was used for the colorimetric measurements. The color and spectral reflectance of the ceramics were measured according to the CIELab color scale relative to the standard illuminant D65 on a reflection spectrophotometer (ColorEye7000A, USA). Color differences (ΔE values) and the contrast ratios (CR) of the different groups of samples were calculated. In order to analyse the polymerization efficiency of the resin cements, the micromechanical properties of the resins were measured with an automatic microhardness indenter (Fisherscope H100C, Germany). The results were analysed using one-way ANOVA and Tukey's HSD post hoc tests (SPSS 18.0). The one-way ANOVA test showed that the values of ΔE and CR of the different specimen groups were significantly different (p<0.05). Group 1 (20.7 ± 0.5) (IPS-CAD without resin cement) exhibited the highest and group 10 (14.8 ± 0.5) (e.max:HV+3) exhibited the lowest ΔE value. Significant differences in the micromechanical properties were identified among the tested resin cements in different shades (p<0.05). Resin cement shade is an important factor for the opacity of a restoration. Furthermore, the resin shade affects the micromechanical properties of the underlying resin cement. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. High performance dental resin composites with hydrolytically stable monomers.

    PubMed

    Wang, Xiaohong; Huyang, George; Palagummi, Sri Vikram; Liu, Xiaohui; Skrtic, Drago; Beauchamp, Carlos; Bowen, Rafael; Sun, Jirun

    2018-02-01

    The objectives of this project were to: 1) develop strong and durable dental resin composites by employing new monomers that are hydrolytically stable, and 2) demonstrate that resin composites based on these monomers perform superiorly to the traditional bisphenol A glycidyl dimethacrylate/triethylene glycol dimethacrylate (Bis-GMA/TEGDMA) composites under testing conditions relevant to clinical applications. New resins comprising hydrolytically stable, ether-based monomer, i.e., triethylene glycol divinylbenzyl ether (TEG-DVBE), and urethane dimethacrylate (UDMA) were produced via composition-controlled photo-polymerization. Their composites contained 67.5wt% of micro and 7.5wt% of nano-sized filler. The performances of both copolymers and composites were evaluated by a battery of clinically-relevant assessments: degree of vinyl conversion (DC: FTIR and NIR spectroscopy); refractive index (n: optical microscopy); elastic modulus (E), flexural strength (F) and fracture toughness (K IC ) (universal mechanical testing); Knoop hardness (HK; indentation); water sorption (W sp ) and solubility (W su ) (gravimetry); polymerization shrinkage (S v ; mercury dilatometry) and polymerization stress (tensometer). The experimental UDMA/TEG-DVBE composites were compared with the Bis-GMA/TEGDMA composites containing the identical filler contents, and with the commercial micro hybrid flowable composite. UDMA/TEG-DBVE composites exhibited n, E, W sp , W su and S v equivalent to the controls. They outperformed the controls with respect to F (up to 26.8% increase), K IC (up to 27.7% increase), modulus recovery upon water sorption (full recovery vs. 91.9% recovery), and stress formation (up to 52.7% reduction). In addition, new composites showed up to 27.7% increase in attainable DC compared to the traditional composites. Bis-GMA/TEGDMA controls exceeded the experimental composites with respect to only one property, the composite hardness. Significantly, up to 18.1% lower HK values in the experimental series (0.458GPa) were still above the clinically required threshold of approx. 0.4GPa. Hydrolytic stability, composition-controlled polymerization and the overall enhancement in clinically-relevant properties of the new resin composites make them viable candidates to replace traditional resin composites as a new generation of strong and durable dental restoratives. Copyright © 2017 The Academy of Dental Materials. All rights reserved.

  14. Effects of blood contamination on resin-resin bond strength.

    PubMed

    Eiriksson, Sigurdur O; Pereira, Patricia N R; Swift, Edward J; Heymann, Harald O; Sigurdsson, Asgeir

    2004-02-01

    Incremental placement and curing of resin composites has been recommended. However, this requires longer operating time, and therefore, increased risk of contamination. The purpose of this study was to evaluate the effects of blood contamination on microtensile bond strengths (microTBS) between resin interfaces and to determine the best decontamination method to re-establish the original resin-resin bond strength. The top surfaces of 64, 4-mm composite blocks (Z-250, Renew, APX, Pertac II) were untreated as the control, or were treated as follows: blood applied and dried on the surface (Treatment 1), blood applied, rinsed, dried (Treatment 2), blood applied, rinsed, and an adhesive applied (Single Bond, One-Step, Clearfil SE, Prompt L-Pop) (Treatment 3). Fresh composite was applied and light-cured in 2-mm increments. After 24 h storage in water, the specimens were sectioned into 0.7-mm thick slabs, trimmed to a cross-sectional area of 1 mm(2), and loaded to failure at a crosshead speed of 1 mm/min using an Instron universal testing machine. Data were analyzed using two-way ANOVA and Fisher's PLSD test (p<0.05). Control values ranged from 45.1 MPa for Pertac II to 71.5 MPa for APX. Untreated blood contamination resulted in resin-resin bond strengths of only 1.0-13.1 MPa. Rinsing raised bond strengths to over 40 MPa for each material. Use of an adhesive further increased bond strengths except for Pertac II. Rinsing blood from contaminated surfaces increases the resin-resin bond strength significantly and the application of an appropriate adhesive increases the bond strength to control levels.

  15. Preparation and characterization of silane-modified SiO2 particles reinforced resin composites with fluorinated acrylate polymer.

    PubMed

    Liu, Xue; Wang, Zengyao; Zhao, Chengji; Bu, Wenhuan; Na, Hui

    2018-04-01

    A series of fluorinated dental resin composites were prepared with two kinds of SiO 2 particles. Bis-GMA (bisphenol A-glycerolate dimethacrylate)/4-TF-PQEA (fluorinated acrylate monomer)/TEGDMA (triethylene glycol dimethacrylate) (40/30/30, wt/wt/wt) was introduced as resin matrix. SiO 2 nanopartices (30nm) and SiO 2 microparticles (0.3µm) were silanized with 3-methacryloxypropyl trimethoxysilane (γ-MPS) and used as fillers. After mixing the resin matrix with 0%, 10%, 20%, 30% SiO 2 nanopartices and 0%, 10%, 20%, 30%, 40%, 50% SiO 2 microparticles, respectively, the fluorinated resin composites were obtained. Properties including double bond conversion (DC), polymerization shrinkage (PS), water sorption (W p ), water solubility (W y ), mechanical properties and cytotoxicity were investigated in comparison with those of neat resin system. The results showed that, filler particles could improve the overall performance of resin composites, particularly in improving mechanical properties and reducing PS of composites along with the addition of filler loading. Compared to resin composites containing SiO 2 microparticles, SiO 2 nanoparticles resin composites had higher DC, higher mechanical properties, lower PS and lower W p under the same filler content. Especially, 50% SiO 2 microparticles reinforced resins exhibited the best flexural strength (104.04 ± 7.40MPa), flexural modulus (5.62 ± 0.16GPa), vickers microhardness (37.34 ± 1.13 HV), compressive strength (301.54 ± 5.66MPa) and the lowest polymerization (3.42 ± 0.22%). Copyright © 2018 Elsevier Ltd. All rights reserved.

  16. Out-Life Characteristics of IM7/977-3 Composites

    NASA Technical Reports Server (NTRS)

    Miller, Sandi G.; Sutter, James K.; Hou, Tan-Hung; Scheiman, Daniel A.; Martin, Richard E.; Maryanski, Michael; Schlea, Michelle; Gardner, John M.; Schiferl, Zack R.

    2010-01-01

    The capability to manufacture large structures leads to weight savings and reduced risk relative to joining smaller components. However, manufacture of increasingly large composite components is pushing the out-time limits of epoxy/ carbon fiber prepreg. IM7/977-3 is an autoclave processable prepreg material, commonly used in aerospace structures. The out-time limit is reported as 30 days by the manufacturer. The purpose of this work was to evaluate the material processability and composite properties of 977-3 resin and IM7/977-3 prepreg that had been aged at room temperature for up to 60 days. The effects of room temperature aging on the thermal and visco-elastic properties of the materials were investigated. Neat resin was evaluated by differential scanning calorimetry to characterize thermal properties and change in activation energy of cure. Neat resin was also evaluated by rheometry to characterize its processability in composite fabrication. IM7/977-3 prepreg was evaluated by dynamic mechanical analysis to characterize the curing behavior. Prepreg tack was also evaluated over 60 days. The overall test results suggested that IM7/977-3 was a robust material that offered quality laminates throughout this aging process when processed by autoclave.

  17. The influence of ceramic surface treatments on the micro-shear bond strength of composite resin to IPS Empress 2.

    PubMed

    Panah, Faride Gerami; Rezai, Sosan Mir Mohammad; Ahmadian, Leila

    2008-07-01

    An increasing demand for esthetic restorations has resulted in the development of new ceramic systems, but fracture of veneering ceramics still remains the primary cause of failure. Porcelain repair frequently involves replacement with composite resin, but the bond strength between composite resin and all-ceramic coping materials has not been studied extensively. The purpose of this study was to evaluate the influence of different ceramic surface treatments on the micro-shear bond strength of composite resin to IPS Empress 2 coping material. Sixteen 7 x 7 x 1 mm(3) lithia disilicate-based core ceramic plates were fabricated using the lost wax technique. The plates were divided into eight groups, and eight different surface treatments were performed: (1) no treatment (NT); (2) airborne-particle abrasion with 50-mum alumina particles (Al); (3) acid etching with 9.6% hydrofluoric acid for 1 min (HF); (4) silane coating (S); (5) AlHF; (6) AlS; (7) HFS; and (8) AlHFS. Then, ten composite resin cylinders (0.8-mm diameter x 0.5-mm height) were light-polymerized onto the ceramic plates in each group. Each specimen was subjected to a shear load at a crosshead speed of 0.5 mm/min until fracture occurred. The fracture sites were examined with scanning electron microscopy (SEM) to determine the location of failure during debonding and to examine the surface treatment effects. One-way analysis of variance (ANOVA) and multiple comparison (Dunnet T3) tests were used for statistical analysis of data. The mean micro-shear bond strength values (SD) in MPa were--NT: 4.10 (3.06), Al: 7.56 (4.11), HF: 14.04 (2.60), S: 14.58 (2.14), AlHF: 15.56 (3.36), AlS: 23.02 (4.17), HFS: 24.7 (4.43), AlHFS: 26.0 (3.71). ANOVA indicated the influence of surface treatment was significant (p < 0.0001). SEM analysis did not reveal entirely cohesive failure in any composite or ceramic. The micro-shear bond strength of a composite resin to IPS Empress 2 was significantly different depending on the surface treatment method. Among the investigated methods, silane coating after airborne-particle abrasion and etching was the most effective surface treatment in terms of bond strength increase.

  18. Effect of in-office bleaching agents on the color changes of stained ceromers and direct composite resins.

    PubMed

    Xing, Wenzhong; Jiang, Tao; Liang, Shanshan; Sa, Yue; Wang, Zhejun; Chen, Xiaodong; Wang, Yining

    2014-11-01

    To evaluate the effect of two in-office bleaching agents on the color changes of two ceromers (Ceramage and Adoro SR) and one direct composite resin (Gradia Direct Anterior) after staining by tea and coffee. Twenty-four disk-shaped specimens were fabricated for each resin material and randomly divided into three groups (n = 8). The specimens were immersed in tea, coffee or deionized water, respectively, for 7 days. Each group was then equally divided into two sub-groups (n = 4), which were subjected to two in-office bleaching agents (BEYOND and Opalescence Boost), respectively. The color of the specimens was measured by a spectrophotometer at baseline, after staining and after bleaching. The color differences (ΔE values) between baseline and after treatments were calculated. Statistical analysis indicated that the staining solution had significant influence on the color change of resin composites tested (p < 0.001). The discolorations of resin composites were perceptible after immersing in tea or coffee solutions (ΔE>2.0). There was no statistically significant difference between BEYOND and Opalescence Boost in stains removal from discolored resins (p = 0.550). The color changes in ΔE value between baseline and after bleaching were less than 2.0 for all resin composite groups. Tea solution produces severe discoloration of three resin composites tested. The two in-office bleaching agents can effectively remove the stains from two ceromers and one direct composite resin tested in this study.

  19. Flexural properties of denture base polymers reinforced with a glass cloth-urethane polymer composite.

    PubMed

    Kanie, Takahito; Arikawa, Hiroyuki; Fujii, Koichi; Ban, Seiji

    2004-10-01

    A newly designed light-cured reinforcement made from urethanemethacrylate oligomer and woven glass cloth has orthotropic anisotropy. This is produced for incorporation into the outermost position under the greatest tension in denture base resins. In this study, the flexural properties of self-, heat-, and light-curing reinforced resins were determined. The silanized glass cloth was soaked in urethanemethacrylate oligomer containing camphorquinone and 2-(dimethylamino)ethylmethacrylate. It was sandwiched between two pieces of polyethylene film and pressed to form a reinforcement sheet 0.3 mm in thickness, which was light-cured and prepared using four different surface conditions: with or without the polyethylene film and with or without a bonding agent. The reinforcement sheet was fixed in a fluorocarbon resin mold 3 mm in thickness, which was filled with self-, heat-, or light-curing resin and cured. The cured laminated plate was cut for flexural testing (40 x 7 x 3 mm3). A three-point flexural test was carried out at a crosshead speed of 2 mm/min and a span length of 30 mm. In this study, the glass fiber content was measured at percentages by weight because it was not possible to determine accurately the volume of the various polymers. The baseline flexural strengths of the self-, heat-, and light-curing resins were 76.2, 68.6, and 55.6 MPa, respectively, and these values were increased to 271.7, 216.4, and 266.5 MPa by the reinforcement sheet. The baseline flexural moduli of self-, heat-, and light-curing resins were 2.0, 2.4, and 2.1 GPa, respectively. These values were increased to 7.2, 5.1, and 6.6 GPa by the reinforcement sheet. SEM photographs revealed good impregnation of the glass fiber within the polymer matrix. The differences in the flexural strengths and flexural moduli of the control and reinforced specimens were significant (p < 0.01).

  20. Resin rodlets in shale and coal (Lower Cretaceous), Baltimore Canyon Trough

    USGS Publications Warehouse

    Lyons, P.C.; Hatcher, P.G.; Minkin, J.A.; Thompson, C.L.; Larson, R.R.; Brown, Z.A.; Pheifer, R.N.

    1984-01-01

    Rodlets, occurring in shale and coal (uppermost Berriasian to middle Aptian, Lower Cretaceous), were identified from drill cuttings taken from depths between 9330 ft (2844 m) and 11, 460 ft (3493 m) in the Texaco et al., Federal Block 598, No. 2 well, in the Baltimore Canyon Trough. Under the binocular microscope, most of the rodlets appear black, but a few are reddish brown, or brownish and translucent on thin edges. They range in diameter from about 0.4 to 1.7 mm and are commonly flattened. The rodlets break with a conchoidal fracture, and some show an apparent cellular cast on their longitudinal surfaces. When polished and viewed in reflected light, the rodlets appear dark gray and have an average random reflectance of less than 0.1% whereas mean maximum reflectances are 0.48-0.55% for vitrinite in the associated shale and coal. These vitrinite reflectances indicate either subbituminous A or high-volatile C bituminous coal. The rodlets fluoresce dull gray yellow to dull yellow. The scanning electron microscope (SEM) and light microscope reveal the presence of swirl-like features in the rodlet interiors. Minerals associated with the rodlets occur as sand-size grains attached to the outer surface, as finely disseminated interior grains, and as fracture fillings. Electron microprobe and SEM-energy-dispersive X-ray (EDX) anlayses indicate that the minerals are dominantly clays (probably illite and chlorite) and iron disulfide; calcium carbonate, silicon dioxide, potassium aluminum silicate (feldspar), titanium dioxide, zinc sulfide, and iron sulfate minerals have been also identified. The rodlets were analyzed directly for C, H, N, O, and total S and are interpreted as true resins on the basis of C and H contents that range from 75.6 to 80.3 and from 7.4 to 8.7 wt. % (dry, ash-free basis), respectively. Elemental and infrared data support a composition similar to that of resinite from bituminous coal. Elements determined to be organically associated in the rodlets include S (0.2-0.5 wt.%), Cl (0.03-0.1 wt.%), and Si (0.05-0.08 wt.%). The ash content of the resin rodlets ranges from 4 to 24 wt.% and averages 12 wt.%. Total sulfur contents range from 1.7 to 3.6 wt.%. Resins of fossil plants are known to have little or no sulfur and ash; therefore, these data and the presence of minerals in fractures indicate that most of the sulfur and mineral matter were introduced into the resin partly or wholly after the time of brittle fracture of the resin. The probable source of the resin rodlets is fossil pinaceous conifer cones, which are known to have resin canals as much as 2400 ??m in diameter. ?? 1984.

  1. The Effect of Disinfection Techniques on the Flexural Strength of Thermopolymerisable Acrylic Resins With or Without Pigment Addition.

    PubMed

    Goiato, Marcelo Coelho; Zuccolotti, Bruna Carolina Rossatti; Haddad, Marcela Filié; Moreno, Amália; Pesqueira, Aldiéris Alves; Gennari, Humberto Filho; Dos Santos, Daniela Micheline

    2015-12-01

    The aim of this study was to assess the flexural strength of two brands of thermopolymerisable acrylic resins (Onda Cryl, Artigos Odontológicos Clássico Ltda, São Paulo, SP, Brazil; and Lucitone 550, Dentsply, York, PA, USA) with varying concentrations of pigment (Poli-Côr, Artigos Odontológicos Clássico Ltda, São Paulo, SP, Brazil) under the influence of thermocycling, storage and disinfection. A total of 210 samples were manufactured (105 for each acrylic resin brand), with dimensions of 64 x 10 x 3.3 mm. The samples were divided into 30 subgroups (n = 7) according to the proportion of pigment used (without pigment, 3% and 7%), the assessment period (initial or thermocycling for 2000 cycles) and disinfection method (immersion in 1% sodium hypochlorite, (Apothicário, Araçatuba, SP, Brazil), microwave energy or immersion in alkaline peroxide (Efferdent, Pfizer, Morris Plains, NJ, USA). The samples were submitted to the flexural strength test before and after thermocycling, and after storage with disinfection. The disinfection process was performed every 3 days, for 60 days. Data were submitted to analysis of variance (ANOVA) and Tukey test (p < 0.05). The factors that provided statistical alteration in flexural strength values were resin type and assessment period. The Onda Cryl resin and the period after disinfection (126 ± 25 MPa) exhibited the higher values of flexural strength. Following disinfection, Onda-Cryl resin exhibited the highest values of flexural strength. All the samples obtained are considered clinically acceptable.

  2. Argon Ion Laser Polymerized Acrylic Resin: A Comparative Analysis of Mechanical Properties of Laser Cured, Light Cured and Heat Cured Denture Base Resins

    PubMed Central

    Murthy, S Srinivasa; Murthy, Gargi S

    2015-01-01

    Background: Dentistry in general and prosthodontics in particular is evolving at greater pace, but the denture base resins poly methyl methacrylate. There has been vast development in modifying chemically and the polymerization techniques for better manipulation and enhancement of mechanical properties. One such invention was introduction of visible light cure (VLC) denture base resin. Argon ion lasers have been used extensively in dentistry, studies has shown that it can polymerize restorative composite resins. Since composite resin and VLC resin share the same photo initiator, Argon laser is tested as activator for polymerizing VLC resin. In the Phase 1 study, the VLC resin was evaluated for exposure time for optimum polymerization using argon ion laser and in Phase 2; flexural strength, impact strength, surface hardness and surface characteristics of laser cured resin was compared with light cure and conventional heat cure resin. Materials and Methods: Phase 1; In compliance with American Dental Association (ADA) specification no. 12, 80 samples were prepared with 10 each for different curing time using argon laser and evaluated for flexural strength on three point bend test. Results were compared to established performance requirement specified. Phase 2, 10 specimen for each of the mechanical properties (30 specimen) were polymerized using laser, visible light and heat and compared. Surface and fractured surface of laser, light and heat cured resins were examined under scanning electron microscope (SEM). Results: In Phase 1, the specimen cured for 7, 8, 9 and 10 min fulfilled ADA requirement. 8 min was taken as suitable curing time for laser curing. Phase 2 the values of mechanical properties were computed and subjected to statistical analysis using one-way ANOVA and Tukey post-hoc test. The means of three independent groups showed significant differences between any two groups (P < 0.001). Conclusion: Triad VLC resin can be polymerized by argon ion laser with 1 W/mm2 power and exposure time of 8 min to satisfy ADA specification. Impact strength, surface hardness of laser cure was better than light cure and heat cure resin. Flexural strength of light cure was better than laser cure and heat cure resin. The SEM study showed similar density on surface, the fractured surface of heat cure resin was dense and compact. PMID:26124596

  3. Creosote bush (Larrea tridentata) resin increases water demands and reduces energy availability in desert woodrats (Neotoma lepida).

    PubMed

    Mangione, Antonio M; Dearing, M Denise; Karasov, William H

    2004-07-01

    Although many plant secondary compounds are known to have serious consequences for herbivores, the costs of processing them are generally unknown. Two potential costs of ingestion and detoxification of secondary compounds are elevation of the minimum drinking water requirement and excretion of energetically expensive metabolites (i.e., glucuronides) in the urine. To address these impacts, we studied the costs of ingestion of resin from creosote bush (Larrea tridentata) on desert woodrats (Neotoma lepida). The following hypotheses were tested: ingestion of creosote resin by woodrats (1) increases minimum water requirement and (2) reduces energy available by increasing fecal and urinary energy losses. We tested the first hypothesis, by measuring the minimum water requirement of woodrats fed a control diet with and without creosote resin. Drinking water was given in decreasing amounts until woodrats could no longer maintain constant body mass. In two separate experiments, the minimum drinking water requirement of woodrats fed resin was higher than that of controls by 18-30% (about 1-1.7 ml/d). We tested several potential mechanisms of increased water loss associated with the increase in water requirement. The rate of fecal water loss was higher in woodrats consuming resin. Neither urinary water nor evaporative water loss was affected by ingestion of resin. Hypothesis 2 was tested by measuring energy fluxes of woodrats consuming control vs. resin-treated diets. Woodrats on a resin diet had higher urinary energy losses and, thus, metabolized a lower proportion of the dietary energy than did woodrats on control diet. Fecal energy excretion was not affected by resin. The excretion of glucuronic acid represented almost half of the energy lost as a consequence of resin ingestion. The increased water requirement and energy losses of woodrats consuming a diet with resin could have notable ecological consequences.

  4. The in vitro and in vivo influence of 4-META/MMA-TBB resin components on dental pulp tissues.

    PubMed

    Inoue, T; Miyakoshi, S; Shimono, M

    2001-08-01

    The purpose of this study was to qualitate the penetration of the major components of 4-META/MMA-TBB adhesive resin (4-META resin) and to characterize their influence on the in vitro and in vivo wound healing of dental pulp tissues. Fresh 4-META resin was applied to rabbit mesentery; its components penetrated the mesentery to form three of layers, depending on the amounts of monomer components in the tissue. The superficial layer was a soft-tissue hybrid layer (STHL), the intermediate layer contained small particles of polymerized 4-META resin, while the deepest layer contained unpolymerized monomer components including MMA and butanol, which were detected by gas chromatography (GC). To characterize the in vivo effects of the deepest layer, we immersed the pulp tissue in MMA or in 5% 4-META/MMA and autotransplanted it to placement beneath a rabbit kidney capsule. The MMA-immersed pulp was positive for osteocalcin and presented osteodentin formation at 7 days, as did the untreated control pulp tissue. In contrast, the 5% 4-META/MMA-immersed pulp collapsed into the cell-deficient fibrous connective tissue, with slight calcification by 7 days and less osteodentin formation at 14 days. Analysis of these data suggests that MMA does not inhibit osteogenic activity of pulp tissue, while 5% 4-META/MMA does inhibit osteogenic activity to some extent.

  5. Evaluation of an anion exchange resin-based method for concentration of F-RNA coliphages (enteric virus indicators) from water samples.

    PubMed

    Pérez-Méndez, A; Chandler, J C; Bisha, B; Goodridge, L D

    2014-08-01

    Enteric viral contaminants in water represent a public health concern, thus methods for detecting these viruses or their indicator microorganisms are needed. Because enteric viruses and their viral indicators are often found at low concentrations in water, their detection requires upfront concentration methods. In this study, a strong basic anion exchange resin was evaluated as an adsorbent material for the concentration of F-RNA coliphages (MS2, Qβ, GA, and HB-P22). These coliphages are recognized as enteric virus surrogates and fecal indicator organisms. Following adsorption of the coliphages from 50ml water samples, direct RNA isolation and real time RT-PCR detection were performed. In water samples containing 10(5)pfu/ml of the F-RNA coliphages, the anion exchange resin (IRA-900) adsorbed over 96.7% of the coliphages present, improving real time RT-PCR detection by 5-7 cycles compared to direct testing. F-RNA coliphage RNA recovery using the integrated method ranged from 12.6% to 77.1%. Resin-based concentration of samples with low levels of the F-RNA coliphages allowed for 10(0)pfu/ml (MS2 and Qβ) and 10(-1)pfu/ml (GA and HB-P22) to be detected. The resin-based method offers considerable advantages in cost, speed, simplicity and field adaptability. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Characterization of MWCNT/Nanoclay Binary Nanoparticles Modified Composites and Fatigue Performance Evaluation of Nanoclay Modified Fiber Reinforced Composites

    DTIC Science & Technology

    2014-04-21

    modified with binary nanoparticles consist of multi-walled carbon nanotubes (MWCNTs) and nanoclays together. First, epoxy SC-15 resin was reinforced...modified with binary nanoparticles consist of multi-walled carbon nanotubes (MWCNTs) and nanoclays together. First, epoxy SC-15 resin was reinforced with...7 2.2.1 Carbon Nanotube

  7. New phenolic esters from the resinous exudate of Haplopappus taeda.

    PubMed

    Faini, Francesca; Labbé, Cecilia; Torres, René; Rodilla, Jesús M; Silva, Lucía; Delle Monache, Franco

    2007-12-01

    Two new phenolic esters 9-trans-p-coumaroyloxy-alpha-terpineol (1) and 7-trans-p-coumaroyloxy-taedol (2), both endowed with free radical scavenger activity and cleroda-3,13 (E)-dien-15,18-diol (3) for which a cis stereochemistry at the decalin junction was found, were isolated from the resinous exudate from Haplopappus taeda upper parts.

  8. Integral Ramjet Booster Demonstration Program

    DTIC Science & Technology

    1975-02-01

    Table 3-10 THREE-COMPONENT DECOMPOSITION MODEL Component r0 Ibm ;"-3 7ft Ibm ^ft A (Resin) 60.75 B (Resin) 20.24 C (Reinf.) 110.00...Cured Strands Burn rate 1000 psia/ + 70°F, in./sec Pressure exponent o. (-65 to +1600F), %/"F itP , (-65 to tUCF), ü/8» Ballistic Properties, 6

  9. Reaction pH of urea-formaldehyde resins as related to strength properties of southern pine particleboard

    Treesearch

    C. -Y. Hse

    1974-01-01

    Twelve urea-formaldehyde resins were prepared with factorial combinations of 4 alkaline and 3 acidic reaction phases; i. e., the reaction mixture was adjusted to pH 7, 8, 9, or 10 for the first hour and then made weakly acid to pH 5.8, 4.8, or 3.8.

  10. Characteristics of urea-formaldehyde resins as related to glue bond quality of southern pine particleboard

    Treesearch

    C. -Y. Hse

    1974-01-01

    Forty-five urea resins were formulated and replicated by factorial arrangement of three variables: molar ratio of formaldehyde to urea (1.5, 1.7, 1.9, 2.1, and 2.3), reactant concentration (35, 42.5, and 50%), and reaction temperature (75°, 85°, and 95°C).

  11. Arsenic Contaminated Groundwater Treatment Pilot Study at the Sharpe Army Depot (SHAD) Lathrop, California. Task Order 9

    DTIC Science & Technology

    1990-12-01

    I- I IIIIII 11HI ca~ 1- 1.cc III I HHo I H [I I 5-12 December 1990 Revision: 1 in Table 5-6, the performance of F-1 AA, in terms of the equilibrium...required. In treatment of water for boiler makeup, the relative freedom of Amberlite I RA-402 from *. ..IOEAIGCHRCEITC organic fouling insures good...hydroxide form) 1400 F (600 C) medium pressure boilers . This represents a considerable f chloride form) 1700 F (77 0C) saving over the use of deionization

  12. Development of system design information for carbon dioxide using an amine type sorber

    NASA Technical Reports Server (NTRS)

    Rankin, R. L.; Roehlich, F.; Vancheri, F.

    1971-01-01

    Development work on system design information for amine type carbon dioxide sorber is reported. Amberlite IR-45, an aminated styrene divinyl benzene matrix, was investigated to determine the influence of design parameters of sorber particle size, process flow rate, CO2 partial pressure, total pressure, and bed designs. CO2 capacity and energy requirements for a 4-man size system were related mathematically to important operational parameters. Some fundamental studies in CO2 sorber capacity, energy requirements, and process operation were also performed.

  13. Comparison of atmospheric concentrations of currently used pesticides between urban and rural areas during intensive application period in Alsace (France) by using XAD-2® based passive samplers.

    PubMed

    Liaud, Celine; Schwartz, Jean-Jacques; Millet, Maurice

    2017-07-03

    XAD-2® passive samplers (PAS) have been exposed simultaneously for 14 days on two sites, one rural and one urban, situated in Alsace (East of France) during intensive pesticides application in agriculture (between March and September). PAS have been extracted and analyzed for current-used pesticides and lindane with an analytical method coupling accelerated solvent extraction (ASE), solid-phase microextraction (SPME) and GC/MS/MS. Results show the detection of pesticides is linked to the period of application and spatial and temporal variabilities can be observed with these PAS during the selected sampling period. The spatial and temporal variability is comparable to the one previously observed by comparing data obtained with PAS with data from Hi.-Vol. samplers in an urban area. Sampling rates were calculated for some pesticides and values are comparable to the data already available in the literature. From these sampling rates, concentrations in ng m -3 of pesticides in PAS have been calculated and are in the same order of magnitude as those obtained with Hi.Vol. sampling during the same period of time.

  14. Expression of Xylella fastidiosa Fimbrial and Afimbrial Proteins during Biofilm Formation▿

    PubMed Central

    Caserta, R.; Takita, M. A.; Targon, M. L.; Rosselli-Murai, L. K.; de Souza, A. P.; Peroni, L.; Stach-Machado, D. R.; Andrade, A.; Labate, C. A.; Kitajima, E. W.; Machado, M. A.; de Souza, A. A.

    2010-01-01

    Complete sequencing of the Xylella fastidiosa genome revealed characteristics that have not been described previously for a phytopathogen. One characteristic of this genome was the abundance of genes encoding proteins with adhesion functions related to biofilm formation, an essential step for colonization of a plant host or an insect vector. We examined four of the proteins belonging to this class encoded by genes in the genome of X. fastidiosa: the PilA2 and PilC fimbrial proteins, which are components of the type IV pili, and XadA1 and XadA2, which are afimbrial adhesins. Polyclonal antibodies were raised against these four proteins, and their behavior during biofilm development was assessed by Western blotting and immunofluorescence assays. In addition, immunogold electron microscopy was used to detect these proteins in bacteria present in xylem vessels of three different hosts (citrus, periwinkle, and hibiscus). We verified that these proteins are present in X. fastidiosa biofilms but have differential regulation since the amounts varied temporally during biofilm formation, as well as spatially within the biofilms. The proteins were also detected in bacteria colonizing the xylem vessels of infected plants. PMID:20472735

  15. Occupational Exposure to Polycyclic Aromatic Hydrocarbon of Wildland Firefighters at Prescribed and Wildland Fires.

    PubMed

    Navarro, Kathleen M; Cisneros, Ricardo; Noth, Elizabeth M; Balmes, John R; Hammond, S Katharine

    2017-06-06

    Wildland firefighters suppressing wildland fires or conducting prescribed fires work long shifts during which they are exposed to high levels of wood smoke with no respiratory protection. Polycyclic aromatic hydrocarbons (PAHs) are hazardous air pollutants formed during incomplete combustion. Exposure to PAHs was measured for 21 wildland firefighters suppressing two wildland fires and 4 wildland firefighters conducting prescribed burns in California. Personal air samples were actively collected using XAD4-coated quartz fiber filters and XAD2 sorbent tubes. Samples were analyzed for 17 individual PAHs through extraction with dichloromethane and gas chromatograph-mass spectrometer analysis. Naphthalene, retene, and phenanthrene were consistently the highest measured PAHs. PAH concentrations were higher at wildland fires compared to prescribed fires and were highest for firefighters during job tasks that involve the most direct contact with smoke near an actively burning wildland fire. Although concentrations did not exceed current occupational exposure limits, wildland firefighters are exposed to PAHs not only on the fire line at wildland fires, but also while working prescribed burns and while off-duty. Characterization of occupational exposures from wildland firefighting is important to understand better any potential long-term health effects.

  16. Static and cyclic loading of fiber-reinforced dental resin.

    PubMed

    Drummond, James L; Bapna, Mahendra S

    2003-05-01

    The aim of this study was to evaluate the flexure strength of unidirectional fiber-reinforced resins under static and cyclic loading with and without thermal cycling. The fiber-reinforced resin materials chosen for this project were commercially available endodontic posts and commercially procured bar samples. For all materials, controls for flexure strength were tested in air and in water using three-point loading. Specimens were thermal cycled between 7 and 63 degrees C for 6000 cycles. A staircase approach was used to determine the flexure fatigue limit and scanning microscopy was used to examine the microstructure. The carbon/graphite fiber-reinforced resin posts and the glass FiberKor posts were significantly stronger than the ceramic (zirconia) and the other glass-reinforced resin materials. Thermal cycling caused a significant lowering (11-24%) of the flexure strength for each resin based post system. The ceramic post system decreased only by 2%. Further, for standard size glass fiber-reinforced resin bars, no significant differences between testing in air and water was observed, but a significant difference between static and cyclic loading was noted. The decreases in the strength property due to thermal cycling and the cyclic loading of these materials indicates that their utilization in the oral environment enhances their degradation, and potentially shortens their clinical life.

  17. In vitro bond strength and fatigue stress test evaluation of different adhesive cements used for fixed space maintainer cementation

    PubMed Central

    Cantekin, Kenan; Delikan, Ebru; Cetin, Secil

    2014-01-01

    Objective: The purposes of this research were to (1) compare the shear-peel bond strength (SPBS) of a band of a fixed space maintainer (SM) cemented with five different adhesive cements; and (2) compare the survival time of bands of SM with each cement type after simulating mechanical fatigue stress. Materials and Methods: Seventy-five teeth were used to assess retentive strength and another 50 teeth were used to assess the fatigue survival time. SPBS was determined with a universal testing machine. Fatigue testing was conducted in a ball mill device. Results: The mean survival time of bands cemented with R & D series Nova Glass-LC (6.2 h), Transbond Plus (6.7 h), and R & D series Nova Resin (6.8 h) was significantly longer than for bands cemented with Ketac-Cem (5.4 h) and GC Equia (5.2 h) (P < 0.05). Conclusion: Although traditional glass ionomer cement (GIC) cement presented higher retentive strength than resin-based cements (resin, resin modified GIC, and compomer cement), resin based cements, especially dual cure resin cement (nova resin cement) and compomer (Transbond Plus), can be expected to have lower failure rates for band cementation than GIC (Ketac-Cem) in the light of the results of the ball mill test. PMID:25202209

  18. Fabrication and Evaluation of Bis-GMA/TEGDMA Dental Resins/Composites Containing Nano Fibrillar Silicate

    PubMed Central

    Tian, Ming; Gao, Yi; Liu, Yi; Liao, Yiliang; Hedin, Nyle E.; Fong, Hao

    2008-01-01

    Objective To investigate the reinforcement of Bis-GMA/TEGDMA dental resins (without conventional glass filler) and composites (with conventional glass filler) with various mass fractions of nano fibrillar silicate (FS). Methods Three dispersion methods were studied to separate the silanized FS as nano-scaled single crystals and uniformly distribute them into dental matrices. The photo-curing behaviors of the Bis-GMA/TEGDMA/FS resins were monitored in situ by RT-NIR to study the photopolymerization rate and the vinyl double bond conversion. Mechanical properties (flexural strength, elastic modulus and work of fracture) of the nano FS reinforced resins/composites were tested, and Analysis of Variance (ANOVA) was used for the statistical analysis of the acquired data. The morphology of nano FS and the representative fracture surfaces of its reinforced resins/composites were examined by SEM/TEM. Results Impregnation of small mass fractions (1 % and 2.5 %) of nano FS into Bis-GMA/TEGDMA (50/50 mass ratio) dental resins/composites improved the mechanical properties substantially. Larger mass fraction of impregnation (7.5 %), however, did not further improve the mechanical properties (one way ANOVA, P > 0.05) and may even reduce the mechanical properties. The high degree of separation and uniform distribution of nano FS into dental resins/composites was a challenge. Impregnation of nano FS into dental resins/composites could result in two opposite effects: a reinforcing effect due to the highly separated and uniformly distributed nano FS single crystals, or a weakening effect due to the formation of FS agglomerates/particles. Significance Uniform distribution of highly separated nano FS single crystals into dental resins/composites could significantly improve the mechanical properties of the resins/composites. PMID:17572485

  19. Effect of pore structure on the removal of clofibric acid by magnetic anion exchange resin.

    PubMed

    Tan, Liang; Shuang, Chendong; Wang, Yunshu; Wang, Jun; Su, Yihong; Li, Aimin

    2018-01-01

    The effect of pore structure of resin on clofibric acid (CA) adsorption behavior was investigated by using magnetic anion exchange resins (ND-1, ND-2, ND-3) with increasing pore diameter by 11.68, 15.37, 24.94 nm. Resin with larger pores showed faster adsorption rates and a higher adsorption capacity because the more opened tunnels provided by larger pores benefit the CA diffusion into the resin matrix. The ion exchange by the electrostatic interactions between Cl-type resin and CA resulted in chloride releasing to the solution, and the ratio of released chloride to CA adsorption amount decreased from 0.90 to 0.65 for ND-1, ND-2 and ND-3, indicating that non-electrostatic interactions obtain a larger proportional part of the adsorption into the pores. Co-existing inorganic anions and organic acids reduced the CA adsorption amounts by the competition effect of electrostatic interaction, whereas resins with more opened pore structures weakened the negative influence on CA adsorption because of the existence of non-electrostatic interactions. 85.2% and 65.1% adsorption amounts decrease are calculated for resin ND-1 and ND-3 by the negative influence of 1 mmol L -1 NaCl. This weaken effect of organic acid is generally depends on its hydrophobicity (Log Kow) for carboxylic acid and its ionization degree (pKb) for sulfonic acid. The resins could be reused with the slightly decreases by 1.9%, 3.2% and 5.4% after 7 cycles of regeneration, respectively for ND-1, ND-2 and ND-3, suggesting the ion exchange resin with larger pores are against its reuse by the brine solution regeneration. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Effect of organic solvents compared to sandblasting on the repair bond strength of nanohybrid and nanofilled composite resins.

    PubMed

    Brum, Rafael Torres; Vieira, Sergio; Freire, Andrea; Mazur, Rui Fernando; De Souza, Evelise Machado; Rached, Rodrigo Nunes

    2017-01-01

    This study evaluated the effect of different surface treatments on the repair bond strength of nanohybrid (Empress Direct) and nanofilled (Filtek Z350 XT) composite resins. A total of 120 specimens of each material (7.5 x 4.5 x 3 mm) were prepared and polished with SiC paper. Half of the specimens were kept in water for seven days and the other half for six months; they were then divided into six groups according to the type of surface treatment: negative control (no treatment), Al2O3sandblasted, liquid acetone, acetone gel, liquid alcohol and alcohol gel. Following application of the silane coupling agent and the adhesive system, composite resin cylinders were fabricated on the specimens and light cured (20 seconds). The same composite resins were used for the repair. Additionally, ten intact specimens of each composite resin (without repair) were prepared (positive control). The specimens were then loaded to failure in the microshear mode. Three additional specimens were fabricated in each group, and the surface treatments were analyzed by atomic force microscopy, energy-dispersive X-ray spectroscopy (EDS) and scanning electron microscopy (SEM). The nanofilled composite resin showed higher cohesive strength and repair bond strength than the nanohybrid composite resin. The aging process affected the repair bond strength of the nanofilled composite resin. Al2O3sandblasting was more efficient for the nanofilled composite resin and promoted greater surface roughness in both materials. The solvents demonstrated higher efficacy for the nanohybrid composite resin. The strengths resulting from the solvents were material dependent, and Al2O3sandblasting resulted in superior repair bond strength in both materials.

  1. Fabrication and evaluation of Bis-GMA/TEGDMA dental resins/composites containing nano fibrillar silicate.

    PubMed

    Tian, Ming; Gao, Yi; Liu, Yi; Liao, Yiliang; Hedin, Nyle E; Fong, Hao

    2008-02-01

    To investigate the reinforcement of Bis-GMA/TEGDMA dental resins (without conventional glass filler) and composites (with conventional glass filler) with various mass fractions of nano fibrillar silicate (FS). Three dispersion methods were studied to separate the silanized FS as nano-scaled single crystals and uniformly distribute them into dental matrices. The photo-curing behaviors of the Bis-GMA/TEGDMA/FS resins were monitored in situ by RT-NIR to study the photopolymerization rate and the vinyl double bond conversion. Mechanical properties (flexural strength, elastic modulus and work-of-fracture) of the nano FS reinforced resins/composites were tested, and analysis of variance (ANOVA) was used for the statistical analysis of the acquired data. The morphology of nano FS and the representative fracture surfaces of its reinforced resins/composites were examined by SEM/TEM. Impregnation of small mass fractions (1% and 2.5%) of nano FS into Bis-GMA/TEGDMA (50/50 mass ratio) dental resins/composites improved the mechanical properties substantially. Larger mass fraction of impregnation (7.5%), however, did not further improve the mechanical properties (one way ANOVA, P>0.05) and may even reduce the mechanical properties. The high degree of separation and uniform distribution of nano FS into dental resins/composites was a challenge. Impregnation of nano FS into dental resins/composites could result in two opposite effects: a reinforcing effect due to the highly separated and uniformly distributed nano FS single crystals, or a weakening effect due to the formation of FS agglomerates/particles. Uniform distribution of highly separated nano FS single crystals into dental resins/composites could significantly improve the mechanical properties of the resins/composites.

  2. Investigation and Application of a New Passive Sampling Technique for in Situ Monitoring of Illicit Drugs in Waste Waters and Rivers.

    PubMed

    Guo, Changsheng; Zhang, Tingting; Hou, Song; Lv, Jiapei; Zhang, Yuan; Wu, Fengchang; Hua, Zhendong; Meng, Wei; Zhang, Hao; Xu, Jian

    2017-08-15

    Illicit drugs constitute a class of emerging contaminants that has been drawing significant concern due to its potent pharmacological and biological activities. In this study, an in situ passive sampling approach that uses diffusive gradients in thin films (DGT) was successfully tested for measuring ketamine (KET), methamphetamine (METH), and amphetamine (AMP) in water. The diffusion coefficients of KET, METH, and AMP in diffusive gel were (8.13 ± 0.12) × 10 -6 , (8.55 ± 0.14) × 10 -6 , and (7.72 ± 0.18) × 10 -6 cm 2 s -1 at 22 °C, respectively. The capacities of an XAD binding gel for KET, METH, and AMP were 92, 57, and 45 μg per binding gel disc, which were suitable for long-term environmental monitoring. The DGT measurement of these drugs was not influenced by the pH (4 to 9) and the ionic strength (0.001 M - 0.1 M) and unaffected by the water flow, demonstrating the effectiveness of the XAD-based DGT for the in situ monitoring of illicit drugs. DGT samplers were deployed in a WWTP influent and natural rivers in Beijing, China. The ng L -1 levels of the drugs were high in the wastewater influent and low in river waters, with an insignificant fluctuation during the seven-day monitoring. The DGT-measured concentrations were comparable to the average concentrations determined by SPE method, which suggested that the average data measured by DGT could be substituted for high-frequency grab sampling. This study has demonstrated systematically for the first time that DGT is effective and accurate for monitoring illicit drugs in wastewater and surface waters, and provides a powerful tool to investigating the presence, transport, and environmental behaviors of these drugs in the aquatic ecosystem.

  3. Temperature sensitivity of DOC production and transformation in organic soils of the Yukon River Basin, Alaska

    NASA Astrophysics Data System (ADS)

    O'Donnell, J.; Butler, K. D.; Aiken, G.

    2012-12-01

    The flux of dissolved organic carbon (DOC) from terrestrial to aquatic ecosystems represents a critical component of the high-latitude carbon balance. In the Yukon River basin (YRB), DOC fluxes have declined in recent decades, likely in response to regional permafrost thaw and increased groundwater discharge to river flow. Despite improved flux estimates for many arctic rivers, considerable uncertainty exists regarding the potential response of DOC fluxes to projected warming. To improve estimates of future DOC dynamics, it is important to develop a process-based approach whereby empirical constraints are placed on source and sink terms in both soil and river systems. Here, we examine variability in DOC production and microbially mediated transformations as a function of both temperature and organic matter (OM) composition in soils of the YRB. We conducted "tea" experiments by incubating three organic-soil types that vary with depth and decomposition extent (live/dead moss, fibric OM and humic OM) at two temperatures (4 vs. 20 °C). Leachate samples were collected periodically over a 30-day incubation and characterized for DOC concentration, optical properties (specific UV absorbance at 254 nm or SUVA254, fluorescence), and major chemical fractions using XAD8/XAD4 resins. We observed a non-linear increase in DOC production over time, characterized by a rapid initial release of DOC from soils followed by a slower rise in DOC concentration in subsequent weeks. Mean DOC concentration was described by a significant interaction between organic-soil type and temperature, indicating a strong relationship between temperature sensitivity of net DOC production and the decomposition extent of soil OM. On average across all sampling dates, DOC concentrations were highest in leachate from fibric OM (13.4 to 17.8 mgC L-1), and lowest in leachate from humic OM (3.5 to 8.5 mgC L-1). However, the temperature sensitivity of net DOC production was highest in the humic OM treatment, with mean DOC concentrations increasing by 145% between the 4 and 20°C temperature treatments, whereas DOC concentrations in leachate from fibric OM only increased by 33%. We also observed compositional differences in dissolved organic matter (DOM) across experimental treatments and over time, as reflected by UV absorbance and fluorescence measurements. For instance, mean SUVA254 values increased from near-surface soil (live/dead moss = 2.28 ± 0.27 L mgC m-1) to deeper organic horizons (humic OM = 3.86 ± 0.60 L mgC m-1). SUVA254 also increased over time, suggesting selective mineralization of low-molecular weight compounds and enrichment of the aromatic DOM pool. Together, these data help to distinguish vertical differences in DOM origin and composition through soil profiles, and can be used to track the fate of terrestrial DOC under future warming at high latitudes.

  4. What Do We Know about DOM Chemical Composition Based on Its Optical Properties?

    NASA Astrophysics Data System (ADS)

    Aiken, G.

    2016-02-01

    Dissolved organic matter (DOM) optical measurements (UV-Vis light absorbance and fluorescence) provide useful information related to DOM composition and reactivity, and can serve as proxies for DOM concentration and the concentrations of some metals, such as mercury. While these measurements are useful for a range of objectives, they only measure aromatic molecules that absorb UV-Vis light and a smaller subset of these molecules that fluoresce. They provide no information about the substantial fraction of DOM that is non-chromophoric. Based on chromatographic fractionation on XAD resins, DOM optical properties measured on whole water samples strongly correlate with both the concentration and composition of the hydrophobic acid (HPOA) fraction of the DOM. In this presentation the results of DOM optical measurements, DOM fractionation analyses, and 13C-nuclear magnetic resonance (NMR) and ultrahigh-resolution mass spectrometry (FTICR_MS) of HPOA fractions obtained from a wide range a natural waters will be presented to examine the relationships between DOM optical properties and DOM chemical composition. The HPOA fractions within and between rivers exhibit a wide range of optical behaviors reflective of sources and transformations compared to other DOM fractions. While, 13C-NMR and FTICR-MS analyses generally show greater relative concentrations of aromatic molecules for those samples with strong optical signals, they also indicate that the HPOA fractions are mostly composed of a large number of non-chromophoric molecules, such as carbohydrates carboxyl-rich alicyclic molecules (CRAM), and other aliphatic molecules, all of which have implications regarding DOM reactivity, biolability, sources, and age. The utility and short-comings of employing optical data for assessing sources and transformations of DOM in natural waters will be examined using case studies involving organic matter in the Yukon River Basin and riverine export of DOM to the Gulf of Maine.

  5. Calcite growth-rate inhibition by fulvic acids isolated from Big Soda Lake, Nevada, USA, The Suwannee River, Georgia, USA and by polycarboxylic acids

    USGS Publications Warehouse

    Reddy, Michael M.; Leenheer, Jerry

    2011-01-01

    Calcite crystallization rates are characterized using a constant solution composition at 25°C, pH=8.5, and calcite supersaturation (Ω) of 4.5 in the absence and presence of fulvic acids isolated from Big Soda Lake, Nevada (BSLFA), and a fulvic acid from the Suwannee River, Georgia (SRFA). Rates are also measured in the presence and absence of low-molar mass, aliphatic-alicyclic polycarboxylic acids (PCA). BSLFA inhibits calcite crystal-growth rates with increasing BSLFA concentration, suggesting that BSLFA adsorbs at growth sites on the calcite crystal surface. Calcite growth morphology in the presence of BSLFA differed from growth in its absence, supporting an adsorption mechanism of calcite-growth inhibition by BSLFA. Calcite growth-rate inhibition by BSLFA is consistent with a model indicating that polycarboxylic acid molecules present in BSLFA adsorb at growth sites on the calcite crystal surface. In contrast to published results for an unfractionated SRFA, there is dramatic calcite growth inhibition (at a concentration of 1 mg/L) by a SRFA fraction eluted by pH 5 solution from XAD-8 resin, indicating that calcite growth-rate inhibition is related to specific SRFA component fractions. A cyclic PCA, 1, 2, 3, 4, 5, 6-cyclohexane hexacarboxylic acid (CHXHCA) is a strong calcite growth-rate inhibitor at concentrations less than 0.1 mg/L. Two other cyclic PCAs, 1, 1 cyclopentanedicarboxylic acid (CPDCA) and 1, 1 cyclobutanedicarboxylic acid (CBDCA) with the carboxylic acid groups attached to the same ring carbon atom, have no effect on calcite growth rates up to concentrations of 10 mg/L. Organic matter ad-sorbed from the air onto the seed crystals has no effect on the measured calcite crystal-growth rates.

  6. Occurrence of commonly used pesticides in personal air samples and their associated health risk among paddy farmers.

    PubMed

    Hamsan, Hazwanee; Ho, Yu Bin; Zaidon, Siti Zulfa; Hashim, Zailina; Saari, Nazamid; Karami, Ali

    2017-12-15

    Tanjung Karang, Selangor, is widely known for its paddy cultivation activity and hosts the third largest paddy field in Malaysia. Pesticides contamination in agriculture fields has become an unavoidable problem, as pesticides are used to increase paddy productivity and reduce plant disease. Human exposure to agrichemicals is common and could results in both acute and chronic health effects, such as acute and chronic neurotoxicity. This study aims to determine the concentrations of commonly used pesticides (azoxystrobin, buprofezin, chlorantraniliprole, difenoconazole, fipronil, imidacloprid, isoprothiolane, pretilachlor, propiconazole, pymetrozine, tebuconazole, tricyclazole, and trifloxystrobin) in personal air samples and their associated health risks among paddy farmers. Eighty-three farmers from Tangjung Karang, Selangor were involved in this study. A solid sorbent tube was attached to the farmer's breathing zone with a clip, and an air pump was fastened to the belt to collect personal air samples. Pesticides collected in the XAD-2 resin were extracted with acetone, centrifuged, concentrated via nitrogen blowdown and reconstituted with 1mL of 3:1 ultrapure water/HPLC-grade methanol solution. The extract was analyzed using ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The target compounds were detected with a maximum concentration reaching up to 462.5ngm -3 (fipronil). The hazard quotient (HQ) was less than 1 and the hazard index (HI) value was 3.86×10 -3 , indicating that the risk of pesticides related diseases was not significant. The lifetime cancer risk (LCR) for pymetrozine was at an acceptable level (LCR<10 -6 ) with 4.10×10 -8 . The results reported in this study can be beneficial in terms of risk management within the agricultural community. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Development of novel dental adhesive with double benefits of protein-repellent and antibacterial capabilities.

    PubMed

    Zhang, Ning; Weir, Michael D; Romberg, Elaine; Bai, Yuxing; Xu, Hockin H K

    2015-07-01

    Secondary caries at the tooth-restoration margins remains a main reason for restoration failure. The objectives of this study were to: (1) combine protein-repellent 2-methacryloyloxyethyl phosphorylcholine (MPC) with quaternary ammonium dimethylaminohexadecyl methacrylate (DMAHDM) to develop a new dental adhesive with double benefits of protein-repellent and antibacterial capabilities for the first time; and (2) investigate the effects on protein adsorption, anti-biofilm activity, and dentin bond strength. MPC and DMAHDM were incorporated into Scotchbond Multi-Purpose (SBMP) primer and adhesive. Dentin shear bond strengths were measured using extracted human molars. Protein adsorption onto the adhesive resin surfaces was determined by the micro bicinchoninic acid (BCA) method. A dental plaque microcosm biofilm model with human saliva as inoculum was used to investigate biofilm metabolic activity, colony-forming unit (CFU) counts, lactic acid production and live/dead staining of biofilms on resins. Incorporation of 7.5% MPC and 5% DMAHDM into primer and adhesive did not adversely affect the dentin shear bond strength (p>0.1). The resin with 7.5% MPC+5% DMAHDM had protein adsorption that was nearly 20-fold less than SBMP control (p<0.05). The resin with 7.5% MPC+5% DMAHDM had much stronger antibacterial effects than using MPC or DMAHDM alone (p<0.05). Biofilm CFU counts on the resin with 7.5% MPC+5% DMAHDM were reduced by more than 4 orders of magnitude, compared to SBMP control. The use of double agents (protein-repellent MPC+antibacterial DMAHDM) in dental adhesive achieved much stronger inhibition of biofilms than using each agent alone. The novel protein-repellent and antibacterial bonding agent is promising to reduce biofilm/plaque buildup and reduce recurrent caries at the tooth-restoration margins. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  8. Color stability and marginal integrity of interim crowns: An in vitro study

    PubMed Central

    Elagra, Marwa I.; Rayyan, Mohammad R.; Alhomaidhi, Maisam M.; Alanaziy, Areej A.; Alnefaie, Mona O.

    2017-01-01

    Objective: Many commercial dental materials are used to fabricate interim restorations. This study aimed to compare the color stability and the marginal integrity of four different interim crown materials. Materials and Methods: An ivorine right maxillary central incisor was prepared for a full coverage all-ceramic restoration. A total of 36 specimens in the form of crowns were fabricated on the master die using four different materials (n = 9); Polymethyl methacrylate (PMMA) resin (TrimPLUS), PMMA computer-aided design, and computer-aided manufacturing (CAD-CAM) blocks (Ceramill TEMP), cold cure bis-acryl resin (Success CD), and bis-acryl resin dual-cure composite (TempSpan). Color change ΔE for each sample was calculated by measuring its color as Commission Internationale de l’Eclairage L* a* b* with a spectrophotometer before and after immersing in a concentrated tea solution for 7 days. Marginal gap was measured at four reference points using stereomicroscope at ×40. One-way ANOVA and the Tukey multiple comparisons test were used to determine any statistically significant difference between the four groups, (α = 0.05). Results: Success CD showed significantly the greatest color change (7.7) among all the tested materials, while no significant difference was found between the other three materials. TempSpan showed significantly the highest marginal gap formation (430.15 μm), while no significant difference was found between the three other materials. Conclusions: Bis-acryl resin composite materials demonstrated clinically noticeable change in color while PMMA materials demonstrated superior color stability. Dual cure interim materials exhibited significantly higher marginal discrepancy in comparison to PMMA and cold cure bis-acrylic resin materials. CAD-CAM PMMA material exhibited the best color stability and marginal integrity. PMID:28932142

  9. Flavylium chromophores as species markers for dragon's blood resins from Dracaena and Daemonorops trees.

    PubMed

    Sousa, Micaela M; Melo, Maria J; Parola, A Jorge; Seixas de Melo, J Sérgio; Catarino, Fernando; Pina, Fernando; Cook, Frances E M; Simmonds, Monique S J; Lopes, João A

    2008-10-31

    A simple and rapid liquid chromatographic method with diode-array UV-vis spectrophotometric detection has been developed for the authentication of dragon's blood resins from Dracaena and Daemonorops trees. Using this method it was discovered that the flavylium chromophores, which contribute to the red colour of these resins, differ among the species and could be used as markers to differentiate among species. A study of parameters, such as time of extraction, proportion of MeOH and pH, was undertaken to optimise the extraction of the flavyliums. This method was then used to make extracts from samples of dragon's blood resin obtained from material of known provenance. From the samples analysed 7,6-dihydroxy-5-methoxyflavylium (dracorhodin), 7,4'-dihydroxy-5-methoxyflavylium (dracoflavylium) and 7,4'-dihydroxyflavylium were selected as species markers for Daemonorops spp., Dracaena draco and Dracaena cinnabari, respectively. The chromatograms from these samples were used to build an HPLC-DAD database. The ability to discriminate among species of dragon's blood using the single marker compounds was compared with a principal components analysis of the chromatograms in the HPLC-DAD database. The results from the HPLC-DAD method based on the presence of these flavylium markers was unequivocal. The HPLC-DAD method was subsequently applied to 37 samples of dragon blood resins from the historical samples in the Economic Botany Collection, Royal Botanic Gardens, Kew. The method identified anomalies in how samples in this collection had been labelled. It is clear that the method can be used to evaluate the provenance of samples used in different areas of cultural heritage. It also could be used to monitor the trade of endangered species of dragon's blood and the species being used in complex formulations of traditional Chinese medicine.

  10. Epoxy Resins Toughened with Surface Modified Epoxidized Natural Rubber Fibers by One-Step Electrospinning.

    PubMed

    Kim, Joo Ran; Kim, Jung J

    2017-04-27

    Epoxidized natural rubber fibers (ERFs) are developed through one-step electrospinning and directly deposited into epoxy resins without collecting and distributing of fibers. The shape of ERFs shows rough surface due to different evaporation rate of solvent mixture consisting of chloroform and dichloromethane and the average diameter of ERFs is 6.2 µm. The increase of ERFs loading from 0 to 20 wt % into the epoxy resin increases the fracture strain significantly from 1.2% to 13% and toughness from 0.3 MPa to 1.9 MPa by a factor of 7. However, the tensile strength and Young's modulus decrease about 34% from 58 MPa to 34 MPa and from 1.4 GPa to 0.9 GPa, respectively. Due to the crosslinking reactions between oxirane groups of ERFs and amine groups in the resin, surface roughness and the high aspect ratio of ERFs, ERFs result in more effective toughening effect with the minimum loss of tensile properties in epoxy resins.

  11. Effect of ultraviolet light irradiation period on bond strengths between fiber-reinforced composite post and core build-up composite resin.

    PubMed

    Asakawa, Yuya; Takahashi, Hidekazu; Iwasaki, Naohiko; Kobayashi, Masahiro

    2014-01-01

    The aim of the present study was to characterize the effects of the ultraviolet light (UV) irradiation period on the bond strength of fiber-reinforced composite (FRC) posts to core build-up resin. Three types of FRC posts were prepared using polymethyl methacrylate, urethane dimethacrylate, and epoxy resin. The surfaces of these posts were treated using UV irradiation at a distance of 15 mm for 0 to 600 s. The pull-out bond strength was measured and analyzed with the Dunnett's comparison test (α=0.05). The bond strengths of the post surfaces without irradiation were 6.9 to 7.4 MPa; those after irradiation were 4.2 to 26.1 MPa. The bond strengths significantly increased after 15 to 120-s irradiation. UV irradiation on the FRC posts improved the bond strengths between the FRC posts and core build-up resin regardless of the type of matrix resin.

  12. Epoxy Resins Toughened with Surface Modified Epoxidized Natural Rubber Fibers by One-Step Electrospinning

    PubMed Central

    Kim, Joo Ran; Kim, Jung J.

    2017-01-01

    Epoxidized natural rubber fibers (ERFs) are developed through one-step electrospinning and directly deposited into epoxy resins without collecting and distributing of fibers. The shape of ERFs shows rough surface due to different evaporation rate of solvent mixture consisting of chloroform and dichloromethane and the average diameter of ERFs is 6.2 µm. The increase of ERFs loading from 0 to 20 wt % into the epoxy resin increases the fracture strain significantly from 1.2% to 13% and toughness from 0.3 MPa to 1.9 MPa by a factor of 7. However, the tensile strength and Young’s modulus decrease about 34% from 58 MPa to 34 MPa and from 1.4 GPa to 0.9 GPa, respectively. Due to the crosslinking reactions between oxirane groups of ERFs and amine groups in the resin, surface roughness and the high aspect ratio of ERFs, ERFs result in more effective toughening effect with the minimum loss of tensile properties in epoxy resins. PMID:28772822

  13. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Nash, C.; Williams, M.; Restivo, M.

    All prior testing with SuperLig® 639 has been done with the aqueous concentration of LAW at ~5 M [Na+], where the resin sinks, and can be used in a conventional down-flow column orientation. However, the aqueous LAW stream from the Waste Treatment Plant is expected to be ~8 M [Na+]. The resin would float in this higher density liquid, potentially disrupting the ability to achieve a good decontamination due to poor packing of the resin that leads to channeling. Testing was completed with a higher salt concentration in the feed simulant (7.8 M [Na+]) in an engineering-scale apparatus with twomore » columns, each containing ~0.9 L of resin. Testing of this system used a simulant of the LAW solution, and substituted ReO4 - as a surrogate for TcO4 -. Results were then compared using computer modeling. Bench-scale testing was also performed, and examined an unconstrained resin bed, while engineering-scale tests used both constrained and unconstrained beds in a two-column, lead and lag sequential arrangement.« less

  14. Surface discoloration of composite resins: Effects of staining and bleaching.

    PubMed

    Poggio, Claudio; Beltrami, Riccardo; Scribante, Andrea; Colombo, Marco; Chiesa, Marco

    2012-09-01

    The purpose of this in vitro study was to evaluate surface discoloration of three microhybrid composite resins (Esthet•X HD, Clearfil AP-X, Gradia Direct) and five nanohybrid composite resins (Ceram•X, GC Kalore, G-aenial, Grandio, GrandioSO), after staining and bleaching procedures. The composite resins were polymerized with a curing light (Celalux II, Voco, Cuxhaven, Germany) into 160 silicon molds (6,4 mm in diameter and 2 mm in thickness) to obtain identical specimens. Twenty samples for each composite resin were prepared. The specimens were polished using an automated polishing machine with the sequence of 600-, 800-, 1000-grit abrasive paper under water irrigation. The specimens were immersed in tea and distilled water: the specimens were dipped for 20 min, once a day (every 24 h), for 14 days into the drinks. The specimens were then bleached with carbamide peroxide at 17% (Perfect Bleach-Voco). The color of specimens was measured with a spectrophotometer according to the CIE L(*)a(*)b(*) system after light-polymerization of composite resin specimens, after 7 days, after 14 days, and after bleaching. The color difference h index (DEab(*)) between each measurement was calculated. Statistical analysis was made using analysis of variance (ANOVA). All specimens showed a significant increase in staining with a similar trend and no significant differences between microhybrid and nanohybrid composite resins. After whitening procedures, materials tested showed both significant and unsignificant differences of the h index. Microhybrid and nanohybrid composite resins had similar in vitro surface discoloration in tea. After bleaching, discoloration was removed from some composite resins tested.

  15. Surface discoloration of composite resins: Effects of staining and bleaching

    PubMed Central

    Poggio, Claudio; Beltrami, Riccardo; Scribante, Andrea; Colombo, Marco; Chiesa, Marco

    2012-01-01

    Background: The purpose of this in vitro study was to evaluate surface discoloration of three microhybrid composite resins (Esthet•X HD, Clearfil AP-X, Gradia Direct) and five nanohybrid composite resins (Ceram•X, GC Kalore, G-aenial, Grandio, GrandioSO), after staining and bleaching procedures. Materials and Methods: The composite resins were polymerized with a curing light (Celalux II, Voco, Cuxhaven, Germany) into 160 silicon molds (6,4 mm in diameter and 2 mm in thickness) to obtain identical specimens. Twenty samples for each composite resin were prepared. The specimens were polished using an automated polishing machine with the sequence of 600-, 800-, 1000-grit abrasive paper under water irrigation. The specimens were immersed in tea and distilled water: the specimens were dipped for 20 min, once a day (every 24 h), for 14 days into the drinks. The specimens were then bleached with carbamide peroxide at 17% (Perfect Bleach-Voco). The color of specimens was measured with a spectrophotometer according to the CIE L*a*b* system after light-polymerization of composite resin specimens, after 7 days, after 14 days, and after bleaching. The color difference h index (DEab*) between each measurement was calculated. Statistical analysis was made using analysis of variance (ANOVA). Results: All specimens showed a significant increase in staining with a similar trend and no significant differences between microhybrid and nanohybrid composite resins. After whitening procedures, materials tested showed both significant and unsignificant differences of the h index. Conclusions: Microhybrid and nanohybrid composite resins had similar in vitro surface discoloration in tea. After bleaching, discoloration was removed from some composite resins tested. PMID:23559921

  16. Novel protein-repellent dental adhesive containing 2-methacryloyloxyethyl phosphorylcholine

    PubMed Central

    Zhang, Ning; Melo, Mary Anne S.; Bai, Yuxing; Xu, Hockin H. K.

    2015-01-01

    Objectives Biofilms at tooth-restoration margins can produce acids and cause secondary caries. A protein-repellent adhesive resin can potentially inhibition bacteria attachment and biofilm growth. However, there has been no report on protein-repellent dental resins. The objectives of this study were to develop a protein-repellent bonding agent incorporating 2-methacryloyloxyethyl phosphorylcholine (MPC), and to investigate its resistance to protein adsorption and biofilm growth for the first time. Methods MPC was incorporated into Scotchbond Multi-Purpose (SBMP) at 0%, 3.75%, 7.5%, 11.25%, and 15% by mass. Extracted human teeth were used to measure dentin shear bond strengths. Protein adsorption onto resins was determined by a micro bicinchoninic acid (BCA) method. A dental plaque microcosm biofilm model with human saliva as inoculum was used to measure biofilm metabolic activity and colony-forming unit (CFU) counts. Results Adding 7.5% MPC into primer and adhesive did not decrease the dentin bond strength, compared to control (p > 0.1). Incorporation of 7.5% of MPC achieved the lowest protein adsorption, which was 20-fold less than that of control. Incorporation of 7.5% of MPC greatly reduced bacterial adhesion, yielding biofilm total microorganism, total streptococci, and mutans streptococci CFU that were an order of magnitude less than control. Conclusions A protein-repellent dental adhesive resin was developed for the first time. Incorporation of MPC into primer and adhesive at 7.5% by mass greatly reduced the protein adsorption and bacterial adhesion, without compromising the dentin bond strength. The novel protein-repellent primer and adhesive are promising to inhibit biofilm formation and acid production, to protect the tooth-restoration margins and prevent secondary caries. PMID:25234652

  17. Nanostructured polymer-titanium composites and titanium oxide through polymer swelling in titania precursor.

    PubMed

    Kierys, A; Zaleski, R; Buda, W; Pikus, S; Dziadosz, M; Goworek, J

    2013-06-01

    Polymer (XAD7HP)/Ti 4+ nanocomposites were prepared through the swelling of polymer in titanium (IV) ethoxide as a titanium dioxide precursor. The nanocomposite beads exhibit relatively high porosity different than the porosity of the initial polymer. Thermal treatment of composite particles up to 200 °C in vacuum causes the change of their internal structure. At higher temperature, the components of composite become more tightly packed. Calcination at 600 °C and total removal of polymer produce spherically shaped TiO 2 condensed phase as determined by XRD. Thermally treated composites show the substantial change of pore dimensions within micro- and mesopores. The presence of micropores and their transformation during thermal processing was studied successfully by positron annihilation lifetime spectroscopy (PALS). The results derived from PALS experiment were compared with those obtaining from low-temperature nitrogen adsorption data.

  18. In-office bleaching efficacy on stain removal from CAD/CAM and direct resin composite materials.

    PubMed

    Alharbi, Amal; Ardu, Stefano; Bortolotto, Tissiana; Krejci, Ivo

    2018-01-01

    To evaluate the efficacy of in-office bleaching on stain removal from stained resin composite and ceramic computer-assisted design/computer-assisted manufacturing (CAD/CAM) blocks and direct resin composites. Forty disk-shaped samples were fabricated from each of nine materials: six CAD/CAM (VITABLOCS Mark II, Paradigm MZ100, Exp Vita Hybrid Ceramic, VITA ENAMIC, Exp Kerr, and LAVA Ultimate) and three direct resin composites (Filtek Supreme, Venus Diamond, and Filtek Silorane). Samples were randomly divided into five groups (n = 8), each stained with a particular staining solution. Using a calibrated spectrophotometer and a black background, L*a*b* values were assessed before and after 120 days of staining. Samples were subjected to in-office bleaching using 40% hydrogen peroxide gel for one hour. At subsequent assessment, color change (ΔE) was calculated as the difference between L*a*b* values. Both ANOVA and the Duncan test were used to identify differences between groups (α = 0.05). Bleaching resulted in significant differences in ΔE values for all materials (P < .001). Bleaching efficacy was highly influenced by material composition and staining solution. Residual color values after bleaching for ceramic and hybrid ceramics ranged from -0.49 to 2.35, within the clinically acceptable maximum of 3.3. Values after bleaching for resin-based CAD/CAM ranged from -0.7 to 7.08 while direct resin composites values ranged from -1.47 to 25.13. Coffee left the greatest residual color on all materials. Based on material nature, 40% hydrogen peroxide bleaching can remove staining. The new resin-based CAD/CAM blocks showed promising results in terms of color stability. Bleaching using 40% hydrogen peroxide can be an effective method to remove stains from dental restorations. In this way, restoration replacement as a result of discoloration may no longer be necessary. © 2017 Wiley Periodicals, Inc.

  19. A 15-year randomized controlled study of a reduced shrinkage stress resin composite.

    PubMed

    van Dijken, Jan W V; Lindberg, Anders

    2015-09-01

    The aim of this randomized controlled study was to evaluate the long term effectiveness of a reduced shrinkage stress resin composite in Class II restorations. The material was compared intra-individually with a microhybrid resin composite. Each of 50 patients with at least one pair of two similar sized Class II cavities participated (22 female, 28 male, mean age 43 years, range 18-64). Each participant received in each pair, in a randomized way, one Class II restoration performed with a reduced shrinkage stress resin composite (InTen-S) and the other restoration with a microhybrid resin composite restoration (Point 4). Both restorations were placed with an etch-and-rinse bonding system and an oblique layering technique. A total of 106 restorations, 33 premolar and 73 molars, were placed. The restorations were evaluated blindly each year using modified USPHS criteria. The overall performance of the experimental restorations was tested after intra-individual comparison using the Friedmańs two-way analysis of variance test. The hypothesis was rejected at the 5% level. At 15 years, 91 restorations were evaluated. The drop out frequency was 15 restorations (5 male, 3 female participants; 2 premolar and 13 molar restorations). Except for 2 participants, who reported slight symptoms during a few weeks after placement, no post-operative sensitivity was observed at the recalls. The overall success rate at 15 years was 77%. Twenty-one non acceptable restorations were observed during the 15 years follow up, 10 InTen-S (21.7%) and 11 Point 4 (24.4%) restorations (p>0.05). Annual failure rates for the resin composites were 1.5% and 1.6%, respectively. The main reasons for failure were secondary caries (8) and resin composite fracture (7). The differences between premolar vs. molar restorations and between restorations in male vs. female participants were not significant. Significant differences were observed between 2-surface vs. 3-surface restorations. During the 15-year follow up, the reduced shrinkage stress resin composite showed a good clinical durability in Class II cavities, but not significantly better than the control microhybrid resin composite. Secondary caries and material fracture were the main reasons of failure. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  20. Cast metal, resin-bonded prostheses: a 10-year retrospective study.

    PubMed

    Williams, V D; Thayer, K E; Denehy, G E; Boyer, D B

    1989-04-01

    A sample of 99 resin-bonded prostheses placed over a 10-year period were examined by four clinicians using a standardized criteria sheet. Areas examined included hard tissues, periodontium, retainer and pontic design, retention, the effect of occlusion on framework design and retention rate, and bonding media. The data from 7- and 10-year retrospective studies were compared for meaningful trends. Results showed (1) caries on retainer teeth was 3%, (2) gingival index of the retainer teeth was less than the gingival index of the rest of the mouth (0.7 +/- 0.5 versus 0.9 +/- 0.6), (3) the respective mean probing depths of retainer teeth of 34 patients in the 7- and 10-year studies were 2.2 +/- 0.4 mm and 1.9 +/- 0.7 mm, (4) the debond rate of all the prostheses from all causes was 31%, (5) the debond rate comparing etched metal and perforated retainers from all causes was 32% and 31% [corrected], respectively, and (6) 83% liked the prosthesis; 17% were noncommittal. The authors concluded that the resin-bonded prosthesis may be considered a permanent restoration and a valuable asset in the clinician's armamentarium.

  1. 40 CFR 63.99 - Delegated Federal authorities.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... (stage 1) R X 9 Pulp & Paper I S X 10 Halogenated Solvent Cleaning T X 11 Polymer & Resins 1 U X 12... Sterilization O X 7 Chromium Cooling Towers Q X 8 Gasoline Distribution (stage 1) R X 9 Pulp & Paper I S X 10... R Gasoline Distribution X S Pulp & Paper MACT I X T Halogenated Solvent X U Polymers & Resins/Group...

  2. Failure behavior of glass ionomer cement under Hertzian indentation.

    PubMed

    Wang, Yan; Darvell, B W

    2008-09-01

    To investigate the load-bearing capacity and failure mode of various types of glass ionomer cement (GIC) under Hertzian indentation, exploring the relationship between the failure behavior and formulation, and examining claims of filler-reinforcement of GIC. Discs 2mm thick, 10mm diameter, 8-18 replicates, were fabricated for two filler-reinforced GICs, four unmodified and unreinforced GICs, and four resin-modified GICs, with a dental silver amalgam and a filled-resin restorative material for comparison. Testing was at 23 degrees C, wet, after 7d storage at 37 degrees C in artificial saliva at pH 6, using a 20mm diameter hard steel ball and filled-nylon substrate (E: 10GPa). First failure was detected acoustically; mode was determined visually. At least 1/3 of specimens in each case were examined under scanning electronic microscope for corroboration. Reinforced and unmodified-unreinforced GICs were indistinguishable by failure load (one-way analysis of variance, P=0.425, overall 260+/-70N) and mode. Failure loads for resin-modified GICs were 360-1150N, amalgam approximately 680N, and filled resin approximately 1200N. Resin-modified GICs tended to be tougher (incomplete fracture), all others gave complete fracture (radial cracking). The stronger materials (two resin-modified GICs and filled resin) showed some cone cracking. While resin-modified GICs showed various extents of increase of failure load over that of the plain GICs, consistent with the hybrid chemistry, filler-reinforcement was not evident for the two claimed products, consistent with structural and theoretical expectations.

  3. Bisphenol A Release: Survey of the Composition of Dental Composite Resins

    PubMed Central

    Dursun, Elisabeth; Fron-Chabouis, Hélène; Attal, Jean-Pierre; Raskin, Anne

    2016-01-01

    Background: Bisphenol A (BPA) is an endocrine disruptor with potential toxicity. Composite resins may not contain pure BPA, but its derivatives are widely used. Several studies found doses of BPA or its derivatives in saliva or urine of patients after composite resin placement. Objective: The aims of this study were to establish an exhaustive list of composite resins marketed in Europe and their composition, and to assess the extent of BPA derivatives used. Methods: A research on manufacturers' websites was performed to reference all composite resins marketed in Europe, then their composition was determined from both material safety data sheets and a standardized questionnaire sent to manufacturers. Manufacturers had to indicate whether their product contained the monomers listed, add other monomers if necessary, or indicate “not disclosed”. Results: 160 composite resins were identified from 31 manufacturers and 23 manufacturers (74.2%) responded to the survey. From the survey and websites, the composition of 130 composite resins (81.2%) was: 112 (86.2%) based on BPA derivatives, 97 (74.7%) on bis-GMA, 17 (13.1%) without monomer derived from BPA (UDMA, sometimes with TEGDMA) and 6 (4.6%) with UDMA (only); 1 (0.8%) did not contain a BPA derivative or UDMA or TEGDMA. Pure BPA was never reported. Conclusion: This work has established a list of 18 composite resins that contain no BPA derivative. Manufacturers should be required to report the exact composition of their products as it often remains unclear or incomplete. PMID:27708726

  4. Bisphenol A Release: Survey of the Composition of Dental Composite Resins.

    PubMed

    Dursun, Elisabeth; Fron-Chabouis, Hélène; Attal, Jean-Pierre; Raskin, Anne

    2016-01-01

    Bisphenol A (BPA) is an endocrine disruptor with potential toxicity. Composite resins may not contain pure BPA, but its derivatives are widely used. Several studies found doses of BPA or its derivatives in saliva or urine of patients after composite resin placement. The aims of this study were to establish an exhaustive list of composite resins marketed in Europe and their composition, and to assess the extent of BPA derivatives used. A research on manufacturers' websites was performed to reference all composite resins marketed in Europe, then their composition was determined from both material safety data sheets and a standardized questionnaire sent to manufacturers. Manufacturers had to indicate whether their product contained the monomers listed, add other monomers if necessary, or indicate "not disclosed". 160 composite resins were identified from 31 manufacturers and 23 manufacturers (74.2%) responded to the survey. From the survey and websites, the composition of 130 composite resins (81.2%) was: 112 (86.2%) based on BPA derivatives, 97 (74.7%) on bis-GMA, 17 (13.1%) without monomer derived from BPA (UDMA, sometimes with TEGDMA) and 6 (4.6%) with UDMA (only); 1 (0.8%) did not contain a BPA derivative or UDMA or TEGDMA. Pure BPA was never reported. This work has established a list of 18 composite resins that contain no BPA derivative. Manufacturers should be required to report the exact composition of their products as it often remains unclear or incomplete.

  5. Extractive scintillating polymer sensors for trace-level detection of uranium in contaminated ground water.

    PubMed

    Duval, Christine E; DeVol, Timothy A; Husson, Scott M

    2016-12-01

    This contribution describes the synthesis of robust extractive scintillating resin and its use in a flow-cell detector for the direct detection of uranium in environmental waters. The base poly[(4-methyl styrene)-co-(4-vinylbenzyl chloride)-co-(divinylbenzene)-co-(2-(1-napthyl)-4-vinyl-5-phenyloxazole)] resin contains covalently bound fluorophores. Uranium-binding functionality was added to the resin by an Arbuzov reaction followed by hydrolysis via strong acid or trimethylsilyl bromide (TMSBr)-mediated methanolysis. The resin was characterized by Fourier-transform infrared spectroscopy and spectrofluorometry. Fluorophore degradation was observed in the resin hydrolyzed by strong acid, while the resin hydrolyzed by TMSBr-mediated methanolysis maintained luminosity and showed hydrogen bonding-induced Stokes' shift of ∼100 nm. The flow cell detection efficiency for uranium of the TMSBr-mediated methanolysis resin was evaluated at pH 4, 5 and 6 in DI water containing 500 Bq L -1 uranium-233 and demonstrated flow cell detection efficiencies of 23%, 16% and 7%. Experiments with pH 4, synthetic groundwater with 50 Bq L -1 uranium-233 exhibited a flow cell detection efficiency of 17%. The groundwater measurements show that the resins can concentrate the uranyl cation from waters with high concentrations of competitor ions at near-neutral pH. Findings from this research will lay the groundwork for development of materials for real-time environmental sensing of alpha- and beta-emitting radionuclides. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Silanated Surface Treatment: Effects on the Bond Strength to Lithium Disilicate Glass-Ceramic.

    PubMed

    Baratto, Samantha Schaffer Pugsley; Spina, Denis Roberto Falcão; Gonzaga, Carla Castiglia; Cunha, Leonardo Fernandes da; Furuse, Adilson Yoshio; Baratto Filho, Flares; Correr, Gisele Maria

    2015-10-01

    The aim of this study was to evaluate the effect of silanization protocols on the bond strength of two resin cements to a lithium disilicate glass-ceramic. Thirty-two ceramic discs were assigned to 2 groups (n=16): G1 - dual-cured resin cement and G2 - light-cured resin cement. Four subgroups were evaluated according to the used silanization protocol. The glass-ceramic was etched with 10% hydrofluoric acid for 20 s and silane was applied for 1 min, as follows: CTL - according to the manufacturer's instructions; HA - dried with hot air; NWA - washed and dried with water and air at room temperature; HWA - washed and dried with hot water and hot air. Thereafter, adhesive was applied and light-cured for 20 s. Silicon molds were used to prepare resin cement cylinders (1x1 mm) on the ceramic surface. The specimens were stored in deionized water at 37 °C for 48 h and subjected to a micro-shear test. The data were submitted to statistical analysis (?#61537;=0.05). Group G1 showed higher bond strengths than G2, except for the CTL and NWA subgroups. Differences as function of the silanization protocol were only observed in G1: HWA (25.13±6.83)≥HA (22.95±7.78)≥CTL(17.44±7.24) ≥NWA(14.63±8.76). For G2 there was no difference among the subgroups. In conclusion, the silanization protocol affected the resin cement/ceramic bond strengths, depending on the material. Washing/drying with hot water and/or hot air increased only the bond strength of the dual-cured resin cement.

  7. Color stability and flexural strength of poly (methyl methacrylate) and bis-acrylic composite based provisional crown and bridge auto-polymerizing resins exposed to beverages and food dye: an in vitro study.

    PubMed

    Gujjari, Anil K; Bhatnagar, Vishrut M; Basavaraju, Ravi M

    2013-01-01

    To evaluate the color stability and flexural strength of poly (methyl methacrylate) (PMMA) and bis-acrylic composite based provisional crown and bridge auto-polymerizing resins exposed to tea, coffee, cola, and food dye. Two provisional crown and bridge resins, one DPI self-cure tooth molding powder (PMMA) (Group A), and one Protemp 4 Temporization Material (bis-acrylic composite) (Group B) were used. Disk-shaped specimens for color stability testing (n = 30 for each material) and bar-shaped specimens for flexural strength testing (n = 30 for each material) were fabricated using a metal mold. The specimens were immersed in artificial saliva, artificial saliva + tea, artificial saliva + coffee, artificial saliva + cola, and artificial saliva + food dye solutions and stored in an incubator at 37°C. Color measurements were taken before immersion, and then after 3 and 7 days of immersion. Flexural strength was evaluated after 7 days of immersion. Group A showed significantly higher color stability as compared to Group B, and artificial saliva + coffee solution had the most staining capacity for the resins. Test solutions had no effect on the flexural strength of Group A, but Group B specimens immersed in artificial saliva + cola showed significantly lower flexural strength values as compared to the control group. The findings of the study showed that for materials used in the study, PMMA was more color stable than bis-acrylic composite based resin. Also, material based on PMMA was more resistant to damage from dietary beverages as compared to bis-acrylic composite based provisional crown and bridge resin.

  8. Arsenic and fluoride removal from contaminated drinking water with Haix-Fe-Zr and Haix-Zr resin beads.

    PubMed

    Phillips, Debra H; Sen Gupta, Bhaskar; Mukhopadhyay, Soumyadeep; Sen Gupta, Arup K

    2018-06-01

    The objective of the study was to carry-out batch tests to examine the effectiveness of Haix-Fe-Zr and Haix-Zr resin beads in the removal of As(III), As(V) and F - from groundwater with a similar geochemistry to a site where a community-based drinking water plant has been installed in West Bengal, India. The groundwater was spiked separately with ∼200 μg/L As(III) and As(V) and 5 mg/L F - . Haix-Zr resin beads were more effective than Haix-Fe-Zr resin beads in removing As(III) and As(V). Haix-Zr resin beads showed higher removal of As(V) compared to As(III). Haix-Zr resin beads removed As(V) below the WHO (10 μg/L) drinking water standards at 8.79 μg/L after 4 h of shaking, while As(III) was reduced to 7.72 μg/L after 8 h of shaking. Haix-Fe-Zr resin beads were more effective in removing F - from the spiked groundwater compared to Haix-Zr resin beads. Concentrations of F - decreased from 6.27 mg/L to 1.26 mg/L, which is below the WHO drinking water standards (1.5 mg/L) for F - , after 15 min of shaking with Haix-Fe-Zr resin beads. After 20 min of shaking in groundwater treated with Haix-Zr resin beads, F - concentrations decreased from 6.27 mg/L to 1.43 mg/L. In the removal of As(III), As(V), and F - from the groundwater, Haix-Fe-Zr and Haix-Zr resin beads fit the parabolic diffusion equation (PDE) suggesting that adsorption of these contaminants was consistent with inter-particle diffusion. Copyright © 2018 Elsevier Ltd. All rights reserved.

  9. Color change of CAD-CAM materials and composite resin cements after thermocycling.

    PubMed

    Gürdal, Isil; Atay, Ayse; Eichberger, Marlis; Cal, Ebru; Üsümez, Aslihan; Stawarczyk, Bogna

    2018-04-24

    The color of resin cements and computer-aided-design and computer-aided-manufacturing (CAD-CAM) restorations may change with aging. The purpose of this in vitro study was to analyze the influence of thermocycling on the color of CAD-CAM materials with underlying resin cement. Seven different CAD-CAM materials, composite resins and glass-ceramics were cut into 0.7-mm and 1.2-mm thicknesses (n=10) and cemented with a dual-polymerizing resin cement, a light-polymerizing resin cement, and a preheated composite resin (N=420). Color values were measured by using spectrophotometry. Specimens were subjected to thermocycling (5°C and 55°C; 5000 cycles). The measured color difference (ΔE) data were analyzed by using descriptive statistics. Normality of data distribution was tested by using the Kolmogorov-Smirnov test. Three-way and 1-way ANOVA followed by the Scheffé post-hoc test and unpaired 2-sample Student t test were computed to determine the significant differences among the tested parameters (α=.05). ΔE values were significantly influenced by the CAD-CAM material (η p 2 =0.85, P<.001) and the resin composite cement (η P 2 =0.03, P=.003) but were not influenced by thickness (P=.179). Significant interactions were present among thickness, cement, and CAD-CAM materials (P<.001). Vita Suprinity and GC Cerasmart showed significantly the lowest ΔE values (P<.001). The highest ΔE values were observed for IPS Empress CAD. The dual-polymerizing resin cement showed significantly lower ΔE values than the preheated composite resin (P=.003). Restoration materials and composite resin cement types used for cementation influence the amount of color change due to aging. Copyright © 2018 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  10. The Effect of Resin and Monoterpenes on Spore Germination and Growth in Fusarium circinatum.

    PubMed

    Slinski, S L; Zakharov, F; Gordon, T R

    2015-01-01

    Resin obtained from Pinus radiata and five monoterpene components of resin (limonene, α-pinene, β-pinene, camphene, and myrcene) were tested to determine their effects on mycelial growth and germination and survival of spores of Fusarium circinatum, the cause of pitch canker in pine, and F. temperatum, which is interfertile with F. circinatum but not pathogenic to pine. Averaged across all treatments, F. temperatum sustained the greatest reduction in radial growth (16.9±0.02% of control). The greatest reduction in dry weight also occurred in F. temperatum (11.7±0.01% of control), and all isolates of F. circinatum were significantly less affected (P<0.05). Spore germination rates in a saturated atmosphere of monoterpenes were relatively high for all tested isolates but, when placed in direct contact with resin, spore survival was significantly greater for F. circinatum than for F. temperatum. Our results are consistent with the hypothesis that greater tolerance of resin is one factor distinguishing F. circinatum from the nonpathogenic F. temperatum. However, differential tolerance of monoterpene components of resin is not sufficient to explain the observed variation in virulence to pine in F. circinatum.

  11. [Study on adsorption of tea polyphenol and caffine with polyamide resin].

    PubMed

    Tang, Ke-wen; Zhou, Chun-shan; Zhong, Shi-an; Zhu, Jie-ding

    2003-02-01

    The performance of adsorption of tea polyphenol and caffine with polyamide resin was investigated. The results obtained by spectrophotometry and HPLC show that the ability of adsorption of tea polyphenol with polyamide is stronger than that of caffine, in which hydrogen bond plays a very important role. The adsorption amount of caffine is 2.65 mg.g-1 with 7.5% adsorption ratio when 100 mL of 0.71 g.L-1 caffine is adsorbed on polyamide resine, but the adsorption amount of tea polyphenol is up to 148.13 mg.g-1 with 85% adsorption ratio when 700 mL of 1.98 g.L-1 tea polyphenol is adsorbed on polyamide resine. The dilution ratios of caffine and tea polyphenol are 74% and 90%, respectively, when they are diluted by 85% alcohol. The static adsorptions of caffine and tea polyphenol on polyamide resine reach equilibrium quickly in 80 min, and the plots of adsorption kinetics are nearly linear. Tea polyphenol and caffine are successfully separated on polyamide resine, and the obtained product contains more than 96% of tea polyphenol and 80% of EGCC with caffine less than 2.8%.

  12. Rechargeable infection-responsive antifungal denture materials.

    PubMed

    Cao, Z; Sun, X; Yeh, C-K; Sun, Y

    2010-12-01

    Candida-associated denture stomatitis (CADS) is a significant clinical concern. We developed rechargeable infection-responsive antifungal denture materials for potentially managing the disease. Polymethacrylic acid (PMAA) was covalently bound onto diurethane dimethacrylate denture resins in the curing step. The PMAA resins bound cationic antifungal drugs such as miconazole and chlorhexidine digluconate (CG) through ionic interactions. The anticandidal activities of the drug-containing PMAA-resin discs were sustained for a prolonged period of time (weeks and months). Drug release was much faster at acidic conditions (pH 5) than at pH 7. Drugs bound to the denture materials could be "washed out" by treatment with EDTA, and the drug-depleted resins could be recharged with the same or a different class of anticandidal drugs. These results suggest clinical potential of the newly developed antifungal denture materials in the management of CADS and other infectious conditions.

  13. Estrogenicity of resin-based composites and sealants used in dentistry.

    PubMed Central

    Olea, N; Pulgar, R; Pérez, P; Olea-Serrano, F; Rivas, A; Novillo-Fertrell, A; Pedraza, V; Soto, A M; Sonnenschein, C

    1996-01-01

    We tested some resin-based composites used in dentistry for their estrogenic activity. A sealant based on bisphenol-A diglycidylether methacrylate (bis-GMA) increased cell yields, progesterone receptor expression, and pS2 secretion in human estrogen-target, serum-sensitive MCF7 breast cancer cells. Estrogenicity was due to bisphenol-A and bisphenol-A dimethacrylate, monomers found in the base paste of the dental sealant and identified by mass spectrometry. Samples of saliva from 18 subjects treated with 50 mg of a bis-GMA-based sealant applied on their molars were collected 1 hr before and after treatment. Bisphenol-A (range 90-931 micrograms) was identified only in saliva collected during a 1-hr period after treatment. The use of bis-GMA-based resins in dentistry, and particularly the use of sealants in children, appears to contribute to human exposure to xenoestrogens. Images Figure 1. A Figure 1. B Figure 2. Figure 3. A Figure 3. B Figure 4. A Figure 4. B Figure 5. A Figure 5. B Figure 6. A Figure 6. B Figure 7. A Figure 7. B Figure 8. Figure 9. Figure 10. PMID:8919768

  14. Mechanical testing of a steel-reinforced epoxy resin bar and clamp for external skeletal fixation of long-bone fractures in cats.

    PubMed

    Leitch, B J; Worth, A J

    2018-05-01

    To provide veterinarians with confidence when using a commercially available epoxy resin in external skeletal fixators (ESF), testing was conducted to determine exothermia during curing of the epoxy resin compared to polymethylmethacrylate (PMMA), the hardness of the epoxy resin as a bar over 16 weeks, and the strength of the epoxy resin bar compared with metal clamps in similarly constructed Type 1a ESF constructs simulating the repair of feline long bone fractures. Exothermia of the epoxy resin during curing was tested against PMMA with surface temperatures recorded over the first 15 minutes of curing, using four samples of each product. The hardness of 90 identical epoxy resin bars was tested by subjecting them to cyclic loads (1,000 cycles of 20.5 N, every 7 days) over a 16-week period and impact testing 10 bars every 2 weeks. Ten bars that were not subjected to cyclic loads were impact tested at 0 weeks and another 10 at 16 weeks. Strength of the epoxy resin product, as a bar and clamp composite, was tested against metal SK and Kirschner-Ehmer (KE) clamps and bars in Type 1a, tied-in intramedullary pin, ESF constructs with either 90° or 75° pin placement, subjected to compressive and bending loads to 75 N. The maximum temperature during curing of the epoxy resin (min 39.8, max 43.0)°C was less than the PMMA (min 85.2, max 98.5)°C (p<0.001). There was no change in hardness of the epoxy resin bars over the 16 weeks of cyclic loading (p=0.58). There were no differences between the median strength of the epoxy resin, SK or KE ESF constructs in compression or bending when tested to 75 N (p>0.05). Stiffness of constructs with 75° pin placement was greater for SK than epoxy resin constructs in compression (p=0.046), and was greater for KE than epoxy resin constructs in bending (p=0.033). The epoxy resin tested was found to be less exothermic than PMMA; bars made from the epoxy resin showed durability over an expected fracture healing timeframe and had mechanical strength characteristics comparable to metal bar and clamp ESF constructs. The epoxy resin ESF construct tested in this study can be considered a suitable replacement for SK or KE ESF constructs in the treatment of feline long-bone fractures, in terms of mechanical strength.

  15. NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF AIR SAMPLES FOR GC/MS ANALYSIS OF PESTICIDE AND PAH (BCO-L-27.0)

    EPA Science Inventory

    The purpose of this SOP is to describe methods for extracting and preparing an air sample consisting of a quartz fiber filter (Pallflex) and an XAD-2 cartridge for analysis of pesticides and polyaromatic hydrocarbons (PAHs). It covers the preparation of samples that are to be an...

  16. Effect of sealant agents on the color stability and surface roughness of nanohybrid composite resins.

    PubMed

    Dede, Doğu Ömür; Şahin, Onur; Koroglu, Aysegül; Yilmaz, Burak

    2016-07-01

    The effect of sealant agents on the surface roughness and color stability of nanohybrid composite resins is unknown. The purpose of this in vitro study was to evaluate the effect of sealant agents on the surface roughness and color stability of 4 nanohybrid composite resin materials. Forty disks (10×2 mm) were fabricated for each nanohybrid composite resin material (Z-550, Tetric EvoCeram, Clearfill Majesty, Ice) (N=160) and divided into 4 surface treatment groups: 1 conventional polishing (control) and 3 different sealant agent (Palaseal, Optiglaze, BisCover) coupling groups (n=10). The specimens were thermocycled, and surface roughness (Ra) values were obtained with a profilometer. Scanning electron microscope images were also recorded. CIELab color parameters of each specimen were measured with a spectrophotometer before and after 7 days of storage in a coffee solution. Color differences were calculated by the CIEDE 2000 (ΔE00) formula. The data were statistically analyzed by 2-way ANOVA and by the Tukey HSD test (α=.05). The surface treatment technique significantly affected the Ra values of the composite resins tested (P<.001). The interaction between the surface treatment technique and composite resin material was also significant for ΔE00 values (P<.05). Within the composite resin groups, significant decreases in Ra were observed only for the Palaseal agent coupled composite resin groups (except Ice) compared with the control groups (P<.05). Scanning electron microscope images revealed rougher surfaces with conventionally polished groups compared with test groups. Conventionally polished groups had the highest ΔE00 (3.09 to 3.49) values for each composite resin group, except for BisCover applied Clearfill Majesty (P<.05). Within the composite resin groups, significant differences were observed between the color change seen with BisCover and other sealants for Clearfill Majesty composite resin (P<.05). Using Palaseal agent on all tested composite resins except for Ice produced smoother surfaces. All surface sealant agents provided less discoloration of nanohybrid composite resins after coffee staining compared with conventional polishing except for BisCover applied Clearfill Majesty composite resin. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  17. Parallel solid-phase synthesis and high-throughput 1H NMR evaluation of a 96-member 1,2,4-trisubstituted-pyrimidin-6-one-5-carboxylic acid library.

    PubMed

    Hamper, Bruce C; Kesselring, Allen S; Chott, Robert C; Yang, Shengtian

    2009-01-01

    A solid-phase organic synthesis method has been developed for the preparation of trisubstituted pyrimidin-6-one carboxylic acids 12, which allows elaboration to a 3-dimensional combinatorial library. Three substituents are introduced by initial Knoevenagel condensation of an aldehyde and malonate ester resin 7 to give resin bound 1. Cyclization of 1 with an N-substituted amidine 10, oxidation, and cleavage afforded pyrimidinone 12. The initial solid-phase reaction sequence was followed by gel-phase (19)FNMR and direct-cleavage (1)H NMR of intermediate resins to determine the optimal conditions. The scope of the method for library production was determined by investigation of a 3 x 4 pilot library of twelve compounds. Cyclocondensation of N-methylamidines and 7 followed by CAN oxidation gave mixtures of the resin bound pyrimidin-6-one 11 and the regioisomeric pyrimidin-4-one 15, which after cleavage from the resin afforded a nearly 1:1 mixture of pyrimidin-6-one and pyrimidin-4-one carboxylic acids 12 and 16, respectively. The regiochemical assignment was confirmed by ROESY1D and gHMBC NMR experiments. A library was prepared using 8 aldehydes, 3 nitriles, and 4 amines to give a full combinatorial set of 96 pyrimidinones 12. Confirmation of structural identity and purity was carried out by LCMS using coupled ELS detection and by high-throughput flow (1)H NMR.

  18. Change in surface roughness of esthetic restorative materials after exposure to different immersion regimes in a cola drink.

    PubMed

    Bajwa, Navroop Kaur; Pathak, Anuradha

    2014-01-01

    Context. An in vitro study carried out to evaluate and compare the effect of Cola drink on surface roughness of esthetic restorative materials. Purpose. To compare the effect of different immersion regimes in a Cola drink on surface roughness of esthetic restorative materials. Method. Two hundred samples were grouped into 4 equal groups of 50 samples each: Group I: conventional glass ionomer, Group II: resin modified glass ionomer, Group III: polyacid-modified resin composite, Group IV: Composite resin. Each group was further subdivided into 5 subgroups of 10 samples each. Subgroup A (Control Subgroup). Samples were kept immersed in artificial saliva. Subgroup B. Samples were immersed in Cola drink once a day. Subgroup C. Samples were immersed in Cola drink, 3 times a day. Subgroup D. Samples were immersed in Cola drink 5 times a day. Subgroup E. Samples were immersed in Cola drink 10 times a day. Each immersion lasted 5 minutes. The immersion protocol was repeated for 7 days. Results. Maximum surface roughness was seen in Group I conventional glass ionomer cement, followed by Group II resin modified glass ionomer, Group III polyacid modified resin composite, and Group IV composite resin samples. Conclusion. Resistance to change in surface roughness is more in resin based restorative materials as compared to glass ionomer based materials.

  19. Change in Surface Roughness of Esthetic Restorative Materials after Exposure to Different Immersion Regimes in a Cola Drink

    PubMed Central

    Bajwa, Navroop Kaur; Pathak, Anuradha

    2014-01-01

    Context. An in vitro study carried out to evaluate and compare the effect of Cola drink on surface roughness of esthetic restorative materials. Purpose. To compare the effect of different immersion regimes in a Cola drink on surface roughness of esthetic restorative materials. Method. Two hundred samples were grouped into 4 equal groups of 50 samples each: Group I: conventional glass ionomer, Group II: resin modified glass ionomer, Group III: polyacid-modified resin composite, Group IV: Composite resin. Each group was further subdivided into 5 subgroups of 10 samples each. Subgroup A (Control Subgroup). Samples were kept immersed in artificial saliva. Subgroup B. Samples were immersed in Cola drink once a day. Subgroup C. Samples were immersed in Cola drink, 3 times a day. Subgroup D. Samples were immersed in Cola drink 5 times a day. Subgroup E. Samples were immersed in Cola drink 10 times a day. Each immersion lasted 5 minutes. The immersion protocol was repeated for 7 days. Results. Maximum surface roughness was seen in Group I conventional glass ionomer cement, followed by Group II resin modified glass ionomer, Group III polyacid modified resin composite, and Group IV composite resin samples. Conclusion. Resistance to change in surface roughness is more in resin based restorative materials as compared to glass ionomer based materials. PMID:25006464

  20. Multi-podant diglycolamides and room temperature ionic liquid impregnated resins: An excellent combination for extraction chromatography of actinides.

    PubMed

    Gujar, R B; Ansari, S A; Verboom, W; Mohapatra, P K

    2016-05-27

    Extraction chromatography resins, prepared by impregnating two multi-podant diglycolamide ligands, viz. diglycolamide-functionalized calix[4]arene (C4DGA) and tripodal diglycolamide (T-DGA) dissolved in the room temperature ionic liquid 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide (RTIL: C4mimTf2N) on Chromosorb-W (an inert solid support), gave excellent results for the removal of trivalent actinides from acidic waste solutions. Distribution coefficient measurements on several metal ions showed selective sorption of Am(III) over hexavalent uranyl ions and other fission product elements such as strontium and cesium. The sorbed metal ions could be efficiently desorbed with a complexing solution containing guanidine carbonate and EDTA buffer. The sorption of Am(III) on both resins followed pseudo-second order rate kinetics with rate constants of 1.37×10(-6) and 6.88×10(-7)g/cpmmin for T-DGA and C4DGA resins, respectively. The metal sorption on both resins indicated the Langmuir monolayer chemisorption phenomenon with Eu(III) sorption capacities of 4.83±0.21 and 0.52±0.05mg per g of T-DGA and C4DGA resins, respectively. The results of column studies show that these resins are of interest for a possible application for the recovery of hazardous trivalent actinides from dilute aqueous solutions. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Immobilization and characterization of tannase from a metagenomic library and its use for removal of tannins from green tea infusion.

    PubMed

    Yao, Jian; Chen, Qinglong; Zhong, Guoxiang; Cao, Wen; Yu, An; Liu, Yuhuan

    2014-01-01

    Tannase (Tan410) from a soil metagenomic library was immobilized on different supports, including mesoporous silica SBA-15, chitosan, calcium alginate, and amberlite IRC 50. Entrapment in calcium alginate beads was comparatively found to be the best method and was further characterized. The optimum pH of the immobilized Tan410 was shifted toward neutrality compared with the free enzyme (from pH 6.4 to pH 7.0). The optimum temperature was determined to be 45°C for the immobilized enzyme and 30°C for the free enzyme, respectively. The immobilized enzyme had no loss of activity after 10 cycles, and retained more than 90% of its original activity after storage for 30 days. After immobilization, the enzyme activity was only slightly affected by Hg(2+), which completely inhibited the activity of the free enzyme. The immobilized tannase was used to remove 80% of tannins from a green tea infusion on the first treatment. The beads were used for six successive runs resulting in overall hydrolysis of 56% of the tannins.

  2. Effect of Imaging Powders on the Bond Strength of Resin Cement

    DTIC Science & Technology

    2016-09-19

    Jordan Advanced Education in General Dentistry Residency Uniformed Services University Date: 6 June 2013 INITIATOR Uniformed Services...Title: Resident , Advanced Education in General Dentistry Residency (AEGD-2) 3. School/DepartmenUCenter: Air Force Postgraduate Dental School (AFPDS) 4...Strength of Resin Cement 7. Intended publication/meeting: General Dentistry (the journal of the Academy of General Dentistry ) 8. "Required by" date

  3. The effect of polishing technique on 3-D surface roughness and gloss of dental restorative resin composites.

    PubMed

    Ereifej, N S; Oweis, Y G; Eliades, G

    2013-01-01

    The aim of this study was to compare surface roughness and gloss of resin composites polished using different polishing systems. Five resin composites were investigated: Filtek Silorane (FS), IPS Empress Direct (IP), Clearfil Majesty Posterior (CM), Premise (PM), and Estelite Sigma (ES). Twenty-five disk specimens were prepared from each material, divided into five groups, each polished with one of the following methods: Opti1Step (OS), OptiDisc (OD), Kenda CGI (KD), Pogo (PG), or metallurgical polishing (ML). Gloss and roughness parameters (Sa, Sz, Sq, and St) were evaluated by 60°-angle glossimetry and white-light interferometric profilometry. Two-way analysis of variance was used to detect differences in different materials and polishing techniques. Regression and correlation analyses were performed to examine correlations between roughness and gloss. Significant differences in roughness parameters and gloss were found according to the material, type of polishing, and material/polishing technique (p< 0.05). The highest roughness was recorded when KD was used (Sa: 581.8 [62.1] for FS/KD, Sq: 748.7 [55.6] for FS/KD, Sz: 17.7 [2.7] for CM/KD, and St: 24.6 [6.8] for FS/KD), while the lowest was recorded after ML (Sa: 133.6 [68.9] for PM/ML, Sq: 256.5 [53.5] for ES/ML, Sz: 4.0 [1.3] for ES/ML, and St: 7.1 [0.7] for ES/ML). The highest gloss was recorded for PM/ML (88.4 [2.3]) and lowest for FS/KD (30.3 [5.7]). All roughness parameters were significantly correlated with gloss (r= 0.871, 0.846, 0.713, and 0.707 for Sa, Sq, Sz, St, and gloss, respectively). It was concluded that the polishing procedure and the type of composite can have significant impacts on surface roughness and gloss of resin composites.

  4. Silver distribution and release from an antimicrobial denture base resin containing silver colloidal nanoparticles.

    PubMed

    Monteiro, Douglas Roberto; Gorup, Luiz Fernando; Takamiya, Aline Satie; de Camargo, Emerson Rodrigues; Filho, Adhemar Colla Ruvolo; Barbosa, Debora Barros

    2012-01-01

    The aim of this study was to evaluate a denture base resin containing silver colloidal nanoparticles through morphological analysis to check the distribution and dispersion of these particles in the polymer and by testing the silver release in deionized water at different time periods. A Lucitone 550 denture resin was used, and silver nanoparticles were synthesized by reduction of silver nitrate with sodium citrate. The acrylic resin was prepared in accordance with the manufacturers' instructions, and silver nanoparticle suspension was added to the acrylic resin monomer in different concentrations (0.05, 0.5, and 5 vol% silver colloidal). Controls devoid of silver nanoparticles were included. The specimens were stored in deionized water at 37°C for 7, 15, 30, 60, and 120 days, and each solution was analyzed using atomic absorption spectroscopy. Silver was not detected in deionized water regardless of the silver nanoparticles added to the resin and of the storage period. Micrographs showed that with lower concentrations, the distribution of silver nanoparticles was reduced, whereas their dispersion was improved in the polymer. Moreover, after 120 days of storage, nanoparticles were mainly located on the surface of the nanocomposite specimens. Incorporation of silver nanoparticles in the acrylic resin was evidenced. Moreover, silver was not detected by the detection limit of the atomic absorption spectrophotometer used in this study, even after 120 days of storage in deionized water. Silver nanoparticles are incorporated in the PMMA denture resin to attain an effective antimicrobial material to help control common infections involving oral mucosal tissues in complete denture wearers. © 2011 by the American College of Prosthodontists.

  5. Light transmittance of zirconia as a function of thickness and microhardness of resin cements under different thicknesses of zirconia

    PubMed Central

    Egilmez, Ferhan; Ergun, Gulfem; Kaya, Bekir M.

    2013-01-01

    Objective: The objective of this study was to compare microhardness of resin cements under different thicknesses of zirconia and the light transmittance of zirconia as a function of thickness. Study design: A total of 126 disc-shaped specimens (2 mm in height and 5 mm in diameter) were prepared from dual-cured resin cements (RelyX Unicem, Panavia F and Clearfil SA cement). Photoactivation was performed by using quartz tungsten halogen and light emitting diode light curing units under different thicknesses of zirconia. Then the specimens (n=7/per group) were stored in dry conditions in total dark at 37°C for 24 h. The Vicker’s hardness test was performed on the resin cement layer with a microhardness tester. Statistical significance was determined using multifactorial analysis of variance (ANOVA) (alpha=.05). Light transmittance of different thicknesses of zirconia (0.3, 0.5 and 0.8 mm) was measured using a hand-held radiometer (Demetron, Kerr). Data were analyzed using one-way ANOVA test (alpha=.05). Results: ANOVA revealed that resin cement and light curing unit had significant effects on microhardness (p < 0.001). Additionally, greater zirconia thickness resulted in lower transmittance. There was no correlation between the amount of light transmitted and microhardness of dual-cured resin cements (r = 0.073, p = 0.295). Conclusion: Although different zirconia thicknesses might result in insufficient light transmission, dual-cured resin cements under zirconia restorations could have adequate microhardness. Key words:Zirconia, microhardness, light transmittance, resin cement. PMID:23385497

  6. Dental Resin Cements-The Influence of Water Sorption on Contraction Stress Changes and Hydroscopic Expansion.

    PubMed

    Sokolowski, Grzegorz; Szczesio, Agata; Bociong, Kinga; Kaluzinska, Karolina; Lapinska, Barbara; Sokolowski, Jerzy; Domarecka, Monika; Lukomska-Szymanska, Monika

    2018-06-08

    Resin matrix dental materials undergo contraction and expansion changes due to polymerization and water absorption. Both phenomena deform resin-dentin bonding and influence the stress state in restored tooth structure in two opposite directions. The study tested three composite resin cements (Cement-It, NX3, Variolink Esthetic DC), three adhesive resin cements (Estecem, Multilink Automix, Panavia 2.0), and seven self-adhesive resin cements (Breeze, Calibra Universal, MaxCem Elite Chroma, Panavia SA Cement Plus, RelyX U200, SmartCem 2, and SpeedCEM Plus). The stress generated at the restoration-tooth interface during water immersion was evaluated. The shrinkage stress was measured immediately after curing and after 0.5 h, 24 h, 72 h, 96 h, 168 h, 240 h, 336 h, 504 h, 672 h, and 1344 h by means of photoelastic study. Water sorption and solubility were also studied. All tested materials during polymerization generated shrinkage stress ranging from 4.8 MPa up to 15.1 MPa. The decrease in shrinkage strain (not less than 57%) was observed after water storage (56 days). Self-adhesive cements, i.e., MaxCem Elite Chroma, SpeedCem Plus, Panavia SA Plus, and Breeze exhibited high values of water expansion stress (from 0 up to almost 7 MPa). Among other tested materials only composite resin cement Cement It and adhesive resin cement Panavia 2.0 showed water expansion stress (1.6 and 4.8, respectively). The changes in stress value (decrease in contraction stress or built up of hydroscopic expansion) in time were material-dependent.

  7. Separation and purification of both tea seed polysaccharide and saponin from camellia cake extract using macroporous resin.

    PubMed

    Yang, Pengjie; Zhou, Mingda; Zhou, Chengyun; Wang, Qian; Zhang, Fangfang; Chen, Jian

    2015-02-01

    A novel method to separate and purify tea seed polysaccharide and tea seed saponin from camellia cake extract by macroporous resin was developed. Among four kinds of resins (AB-8, NKA-9, XDA-6, and D4020) tested, AB-8 macroporous resin possessed optimal separating capacity for the two substances and thus was selected for the separation, in which deionized water was used to elute tea seed polysaccharide, 0.25% NaOH solution to remove the undesired pigments, and 90% ethanol to elute tea seed saponin. Further dynamic adsorption/desorption experiments on AB-8 resin-based column chromatography were conducted to obtain the optimal parameters. Under optimal dynamic adsorption and desorption conditions, 18.7 and 11.8% yield of tea seed polysaccharide and tea seed saponin were obtained with purities of 89.2 and 96.0%, respectively. The developed method provides a potential approach for the large-scale production of tea seed polysaccharide and tea seed saponin from camellia cake. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Microshear bond strength of preheated silorane- and methacrylate-based composite resins to dentin.

    PubMed

    Demirbuga, Sezer; Ucar, Faruk Izzet; Cayabatmaz, Muhammed; Zorba, Yahya Orcun; Cantekin, Kenan; Topçuoğlu, Hüseyin Sinan; Kilinc, Halil Ibrahim

    2016-01-01

    The aim of this study was to investigate the effect of preheating on microshear bond strength (MSBS) of silorane and methacrylate-based composite resins to human dentin. The teeth were randomly divided into three main groups: (1) composite resins were heated upto 68 °C; (2) cooled to 4 °C; and (3) control [room temperature (RT)]. Each group was then randomly subdivided into four subgroups according to adhesive system used [Solobond M (Voco), All Bond SE (Bisco), Clearfil SE Bond (CSE) (Kuraray), Silorane adhesive system (SAS) (3M ESPE)]. Resin composite cylinders were formed (0.9 mm diameter × 0.7 mm length) and MSBS of each specimen was tested. The preheated groups exhibited the highest MSBS (p < 0.001) and the groups cooled to 4 °C exhibited the lowest MSBS (p < 0.001). The CSE showed higher MSBS than the other adhesives (p < 0.001). This study concludes that preheating of composite resins may be an alternative way to increase the MSBS of composites on dentin. © Wiley Periodicals, Inc.

  9. Synthesis of improved phenolic resins

    NASA Technical Reports Server (NTRS)

    Delano, C. B.; Mcleod, A. H.

    1979-01-01

    Twenty seven addition cured phenolic resin compositions were prepared and tested for their ability to give char residues comparable to state-of-the-art phenolic resins. Cyanate, epoxy, allyl, acrylate, methacrylate and ethynyl derivatized phenolic oligomers were investigated. The novolac-cyanate and propargyl-novolac resins provided anaerobic char yields at 800 C of 58 percent. A 59 percent char yield was obtained from modified epoxy novolacs. A phosphonitrilic derivative was found to be effective as an additive for increasing char yields. The novolac-cyanate, epoxy-novolac and methacrylate-epoxy-novolac systems were investigated as composite matrices with Thornel 300 graphite fiber. All three resins showed good potential as composite matrices. The free radical cured methacrylate-epoxy-novolac graphite composite provided short beam shear strengths at room temperature of 93.3 MPa (13.5 ksi). The novolac-cyanate graphite composite produced a short beam shear strength of 74 MPa (10.7 ksi) and flexural strength of 1302 MPa (189 ksi) at 177 C. Air heat aging of the novolac-cyanate and epoxy novolac based composites for 12 weeks at 204 C showed good property retention.

  10. Identification of genotoxic compounds in crude oil using fractionation according to distillation, polarity and Kow.

    PubMed

    Park, Shin Yeong; Lee, Hyo Jin; Khim, Jong Seong; Kim, Gi Beum

    2017-01-30

    We examined the degree of DNA damage caused by fractions of crude oil in accordance with the boiling points, polarity and log K ow . Relatively high DNA damage was observed in the aromatic fraction (290-330°C) and resin and polar fraction (350-400°C). The resin and polar fraction showed relatively high genotoxicity compared with the aliphatic and aromatic fraction at the 1-4 log K ow range. At the 6-7 log K ow range, the aromatic fraction showed relatively high DNA damage compared with the aliphatic and resin and polar fraction. In particular, every detailed fraction in accordance with the log K ow values (aliphatic and aromatic (310-320°C) and resins and polar fractions (370-380°C)) showed one or less than one DNA damage. However, the fractions before separation in accordance with log K ow values (aliphatic and aromatic (310-320°C) and resin and polar (370-380°C) fractions) showed high DNA damage. Thus, we confirm the synergistic action between the detailed compounds. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. Embedding and Chemical Reactivation of Green Fluorescent Protein in the Whole Mouse Brain for Optical Micro-Imaging

    PubMed Central

    Gang, Yadong; Zhou, Hongfu; Jia, Yao; Liu, Ling; Liu, Xiuli; Rao, Gong; Li, Longhui; Wang, Xiaojun; Lv, Xiaohua; Xiong, Hanqing; Yang, Zhongqin; Luo, Qingming; Gong, Hui; Zeng, Shaoqun

    2017-01-01

    Resin embedding has been widely applied to fixing biological tissues for sectioning and imaging, but has long been regarded as incompatible with green fluorescent protein (GFP) labeled sample because it reduces fluorescence. Recently, it has been reported that resin-embedded GFP-labeled brain tissue can be imaged with high resolution. In this protocol, we describe an optimized protocol for resin embedding and chemical reactivation of fluorescent protein labeled mouse brain, we have used mice as experiment model, but the protocol should be applied to other species. This method involves whole brain embedding and chemical reactivation of the fluorescent signal in resin-embedded tissue. The whole brain embedding process takes a total of 7 days. The duration of chemical reactivation is ~2 min for penetrating 4 μm below the surface in the resin-embedded brain. This protocol provides an efficient way to prepare fluorescent protein labeled sample for high-resolution optical imaging. This kind of sample was demonstrated to be imaged by various optical micro-imaging methods. Fine structures labeled with GFP across a whole brain can be detected. PMID:28352214

  12. Zinc Chloride Influence on The Resins Furan Polymerization to Foundry Moulds

    NASA Astrophysics Data System (ADS)

    de Miranda, Leila Figueiredo; Vale, Marcus; Júnior, Antonio Hortêncio Munhoz; Masson, Terezinha Jocelen; de Andrade e Silva, Leonardo Gondin

    The resins used in foundry molds developed for the automotive market has led to major changes in the manufacturing method of foundry molds. The polymerization of these resins and a subsequent curing are used to connect to the foundry sand in a rigid structure capable of receiving and holding liquid metal. It is essential to know the process of polymerization of these resins and their impact on the final properties of the obtained molds, especially in the mechanical characteristics. In this work it was studied the influence of the addition of zinc chloride (in solution) in the sand-furan resin mixture, with the aim of reducing the relation between the extraction time intervals and time bench life. The results showed that addition of percentages of the order of 5.0wt% to 7.5wt% zinc chloride solution reduces this ratio between 10% and 17%; this means that the casting model may be extracted from the sand mass in a smaller time interval increasing the productivity of manufacturing molds. It was also observed that there was also an increase of 9% to 18% in bench life intervals.

  13. Associations of symptoms related to isocyanate, ureaformol, and formophenolic exposures with respiratory symptoms and lung function in coal miners

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Bertrand, J.P.; Simon, V.; Chau, N.

    The respiratory effects of diphenylmethane diisocyanate (MDI)-based resins and ureaformol- and formophenolic-based resins, used in coal mining, are unknown. This cross-sectional study of 354 miners evaluated respiratory health in miners with MDI-related symptoms (IS) and ureaformol/formophenolic-related symptoms (UFS). The protocol included clinical examination, chest radiograph, questionnaire on respiratory symptoms, smoking habit, job history, resin handling, and spirometry. Resin handling concerned 27.7% of the miners. IS affected 5.6%, and 1.4% also after work. UFS affected 22.6%, and 2.3% also after work. Wheezing affected 35.6%; chronic cough, expectoration, or bronchitis about 10%; dyspnea 5.4%; and asthma 2.8%. The miners with UFS hadmore » significantly more frequent chronic cough, expectoration, chronic bronchitis, dyspnea, and wheezing, whereas those with IS at and after work had markedly lower FVC, FEV1, MMEF, FEF50% and FEF25%. These findings raise the possibility of deleterious effects of exposures to MDI and ureaformol/ ormophenolic resins on respiratory health and lung function in coal miners during their working life.« less

  14. Chemical analysis of the resinous exudate isolated from Heliotropium taltalense and evaluation of the antioxidant activity of the phenolics components and the resin in homogeneous and heterogeneous systems.

    PubMed

    Modak, Brenda; Rojas, Macarena; Torres, René

    2009-06-02

    H. taltalense (Phil.) Johnst. (Heliotropiaceae) is an endemic species of the northern coast of Chile that produces a resinous exudate that covers its foliar surface and stems. Its chemical composition was analyzed for the first time, and two aromatic geranyl derivatives: filifolinol and filifolinyl senecionate and three flavonoids - naringenin, 3-O-methylgalangin and 7-O-methyleriodictiol - were isolated. The antioxidant activity of the flavonoids and the resinous exudates was carried out by measuring the 1,1-diphenyl-2-picrylhydrazyl (DPPH) bleaching effect in ethanolic solution and in sodium dodecyl sulfate (SDS) micelles. The influence of the reaction medium was analyzed. The initial velocity reactions for the pure compounds and for the extract were higher in SDS media than in ethanolic solution. The velocity of reaction observed was interpreted in terms of the reaction medium environment in the micelle.

  15. Rechargeable Infection-responsive Antifungal Denture Materials

    PubMed Central

    Cao, Z.; Sun, X.; Yeh, C.-K.; Sun, Y.

    2010-01-01

    Candida-associated denture stomatitis (CADS) is a significant clinical concern. We developed rechargeable infection-responsive antifungal denture materials for potentially managing the disease. Polymethacrylic acid (PMAA) was covalently bound onto diurethane dimethacrylate denture resins in the curing step. The PMAA resins bound cationic antifungal drugs such as miconazole and chlorhexidine digluconate (CG) through ionic interactions. The anticandidal activities of the drug-containing PMAA-resin discs were sustained for a prolonged period of time (weeks and months). Drug release was much faster at acidic conditions (pH 5) than at pH 7. Drugs bound to the denture materials could be “washed out” by treatment with EDTA, and the drug-depleted resins could be recharged with the same or a different class of anticandidal drugs. These results suggest clinical potential of the newly developed antifungal denture materials in the management of CADS and other infectious conditions. PMID:20940361

  16. Effects of solvent on solution prepregging of the resin system LaRC{trademark}-IAX-2

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Cano, R.J.; Massey, C.P.; St. Clair, T.L.

    1996-12-31

    This work assesses the feasibility of using an alternative solvent for the production of composites from polyimide resin systems via solution prepregging. Previous work on solution prepregging of polyimide systems at NASA Langley Research Center has concentrated on the use of the solvent N-methylpyrrolidinone. An alternative solvent with a similar boiling point, -{gamma}-Butyrolactone, was used to prepare the poly(amide acid) version of LaRC{trademark}-IAX-2. These solutions were subsequently used to prepare prepreg and graphite-reinforced composites. Mechanical properties are presented for the resin system LaRC{trademark}-IAX-2 (4% and 5% offset in stoichiometry and endcapped with phthalic anhydride) impregnated onto Hercules IM7 carbon fiber.more » Results from this work were compared to data obtained on the same resin system which had been solution prepregged with the solvent N-methylpyrrolidinone.« less

  17. Mechanical properties, water sorption characteristics, and compound release of grape seed extract-incorporated resins

    PubMed Central

    EPASINGHE, Don Jeevanie; YIU, Cynthia Kar Yung; BURROW, Michael Francis

    2017-01-01

    Abstract Objective This study evaluated the effect of grape seed extract (GSE) incorporation on the mechanical properties, water sorption, solubility, and GSE release from the experimental adhesive resins. Material and Methods An experimental comonomer mixture, consisting of 40% Bis-GMA, 30% Bis MP, 28% HEMA, 0.26% camphorquinone and 1% EDMAB, was used to prepare four GSE-incorporated adhesive resins at concentrations of 0.5, 1, 1.5, and 2 wt%. The neat resin without GSE was used as the control. Six resin beams (25 mm x 2 mm x 2 mm) per group were prepared for flexural strength and modulus of elasticity evaluations using a universal testing machine at a crosshead speed of 1 mm/min. Five disks (6 mm in diameter and 2 mm in thickness) per group were used for microhardness measurements using a Leitz micro-hardness tester with Leica Qgo software. Five disks (7 mm in diameter and 2 mm in thickness) per group were prepared and stored in deionized water for 28 days. Water sorption, solubility, and GSE release in deionized water were calculated for each GSE-incorporated adhesive at the end of 28th day. Data was evaluated using one-way ANOVA and Tukey multiple comparisons. Results Flexural strength, modulus of elasticity and microhardness of GSE-incorporated adhesive decreased significantly with incorporation of 1.5% of GSE (p<0.05). Addition of GSE had no effect on the water sorption of the adhesive resins (p=0.33). The solubility of the resin also increased significantly with incorporation of 1.5% of GSE (p<0.05). Quantities of GSE release increased with increased concentration of GSE in the adhesive resin. Conclusion Up to 1% of GSE can be incorporated into a dental adhesive resin without interfering with the mechanical properties or solubility of the resins. PMID:28877280

  18. Effect of Glass Fiber Incorporation on Flexural Properties of Experimental Composites

    PubMed Central

    Fonseca, Rodrigo Borges; Marques, Aline Silva; Bernades, Karina de Oliveira; Carlo, Hugo Lemes; Naves, Lucas Zago

    2014-01-01

    This study evaluated the effect of fiber addiction in flexural properties of 30 wt% silica filled BisGMA resin (FR) or unfilled Bis-GMA (UR). Ten groups were created (N = 10) varying the resin (FR or UR) and quantity of glass fibers (wt%: 0, 10, 15, 20, and 30). Samples (10 × 2 × 1 mm) were submitted to flexural strength test following SEM examination. Data were analyzed by two-way ANOVA, Tukey, and Student t-test (α = 0.05). Results for flexural strength (MPa) were FR-groups: 0% (442.7 ± 140.6)C, 10% (772.8 ± 446.3)ABC, 15% (854.7 ± 297.3)AB, 20% (863.4 ± 418.0)A, 30% (459.5 ± 140.5)BC; UR-groups: 0% (187.7 ± 120.3)B, 10% (795.4 ± 688.1)B, 15% (1999.9 ± 1258.6)A, 20% (1911.5 ± 596.8)A, and 30% (2090.6 ± 656.7)A, and for flexural modulus (GPa) FR-groups: 0% (2065.63 ± 882.15)B, 10% (4479.06 ± 3019.82)AB, 15% (5694.89 ± 2790.3)A, 20% (6042.11 ± 3392.13)A, and 30% (2495.67 ± 1345.86)B; UR-groups: 0% (1090.08 ± 708.81)C, 10% (7032.13 ± 7864.53)BC, 15% (19331.57 ± 16759.12)AB, 20% (15726.03 ± 8035.09)AB, and 30% (29364.37 ± 13928.96)A. Fiber addiction in BisGMA resin increases flexural properties, and the interaction between resin and fibers seems better in the absence of inorganic fillers increasing flexural properties. PMID:25136595

  19. Effect of glass fiber incorporation on flexural properties of experimental composites.

    PubMed

    Fonseca, Rodrigo Borges; Marques, Aline Silva; Bernades, Karina de Oliveira; Carlo, Hugo Lemes; Naves, Lucas Zago

    2014-01-01

    This study evaluated the effect of fiber addiction in flexural properties of 30 wt% silica filled BisGMA resin (FR) or unfilled Bis-GMA (UR). Ten groups were created (N = 10) varying the resin (FR or UR) and quantity of glass fibers (wt%: 0, 10, 15, 20, and 30). Samples (10 × 2 × 1 mm) were submitted to flexural strength test following SEM examination. Data were analyzed by two-way ANOVA, Tukey, and Student t-test (α = 0.05). Results for flexural strength (MPa) were FR-groups: 0% (442.7 ± 140.6)(C), 10% (772.8 ± 446.3)(ABC), 15% (854.7 ± 297.3)(AB), 20% (863.4 ± 418.0)(A), 30% (459.5 ± 140.5)(BC); UR-groups: 0% (187.7 ± 120.3)(B), 10% (795.4 ± 688.1)(B), 15% (1999.9 ± 1258.6)(A), 20% (1911.5 ± 596.8)(A), and 30% (2090.6 ± 656.7)(A), and for flexural modulus (GPa) FR-groups: 0% (2065.63 ± 882.15)(B), 10% (4479.06 ± 3019.82)(AB), 15% (5694.89 ± 2790.3)(A), 20% (6042.11 ± 3392.13)(A), and 30% (2495.67 ± 1345.86)(B); UR-groups: 0% (1090.08 ± 708.81)(C), 10% (7032.13 ± 7864.53)(BC), 15% (19331.57 ± 16759.12)(AB), 20% (15726.03 ± 8035.09)(AB), and 30% (29364.37 ± 13928.96)(A). Fiber addiction in BisGMA resin increases flexural properties, and the interaction between resin and fibers seems better in the absence of inorganic fillers increasing flexural properties.

  20. [Comparative evaluation of the marginal accuracy of single crowns fabricated computer using aided design/computer aided manufacturing methods, self-curing resin and Luxatemp].

    PubMed

    Jianming, Yuan; Ying, Tang; Feng, Pan; Weixing, Xu

    2016-12-01

    This study aims to compare the marginal accuracy of single crowns fabricated using self-curing resin, Luxatemp, and computer aided design/computer aided manufacturing (CAD/CAM) methods in clinical application. A total of 30 working dies, which were obtained from 30 clinical teeth prepared with full crown as standard, were created and made into 30 self-curing resin, Luxatemp, and CAD/CAM single crowns. The restorations were seated on the working dies, and stereomicroscope was used to observe and measure the thickness of reference points. One-way analysis of variance, which was performed using SPSS 19.0 software package, compared the marginal gap widths of self-curing resin, Luxatemp, and CAD/CAM provisional crowns. The mean marginal gap widths of the fabricated self-curing resin, Luxatemp, and CAD/CAM were (179.06±33.24), (88.83±9.56), and (43.61±7.27) μm, respectively. A significant difference was observed among the three provisional crowns (P<0.05). The marginal gap width of CAD/CAM provisional crown was lower than that of the self-curing resin and Luxatemp. Thus, the CAD/CAM provisional crown offers a better remediation effect in clinical application.

  1. Comparison of temperature change among different adhesive resin cement during polymerization process.

    PubMed

    Alkurt, Murat; Duymus, Zeynep Yesil; Gundogdu, Mustafa; Karadas, Muhammet

    2017-01-01

    The aim of this study was to assess the intra-pulpal temperature changes in adhesive resin cements during polymerization. Dentin surface was prepared with extracted human mandibular third molars. Adhesive resin cements (Panavia F 2.0, Panavia SA, and RelyX U200) were applied to the dentin surface and polymerized under IPS e.max Press restoration. K-type thermocouple wire was positioned in the pulpal chamber to measure temperature change ( n = 7). The temperature data were recorded (0.0001 sensible) and stored on a computer every 0.1 second for sixteen minutes. Differences between the baseline temperature and temperatures of various time points (2, 4, 6, 8, 10, 12, 14, and 16 minute) were determined and mean temperature changes were calculated. At various time intervals, the differences in temperature values among the adhesive resin cements were analyzed by two-way ANOVA and post-hoc Tukey honestly test (α = 0.05). Significant differences were found among the time points and resin cements ( P < 0.05). Temperature values of the Pan SA group were significantly higher than Pan F and RelyX ( P < 0.05). Result of the study on self-adhesive and self-etch adhesive resin cements exhibited a safety intra-pulpal temperature change.

  2. The Effect of Irradiation Distance on Microhardness of Resin Composites Cured with Different Light Curing Units

    PubMed Central

    Cekic-Nagas, Isil; Egilmez, Ferhan; Ergun, Gulfem

    2010-01-01

    Objectives: The aim of this study was to compare the microhardness of five different resin composites at different irradiation distances (2 mm and 9 mm) by using three light curing units (quartz tungsten halogen, light emitting diodes and plasma arc). Methods: A total of 210 disc-shaped samples (2 mm height and 6 mm diameter) were prepared from different resin composites (Simile, Aelite Aesthetic Enamel, Clearfil AP-X, Grandio caps and Filtek Z250). Photoactivation was performed by using quartz tungsten halogen, light emitting diode and plasma arc curing units at two irradiation distances (2 mm and 9 mm). Then the samples (n=7/per group) were stored dry in dark at 37°C for 24 h. The Vickers hardness test was performed on the resin composite layer with a microhardness tester (Shimadzu HMV). Data were statistically analyzed using nonparametric Kruskal Wallis and Mann-Whitney U tests. Results: Statistical analysis revealed that the resin composite groups, the type of the light curing units and the irradiation distances have significant effects on the microhardness values (P<.05). Conclusions: Light curing unit and irradiation distance are important factors to be considered for obtaining adequate microhardness of different resin composite groups. PMID:20922164

  3. Assessment of the biological and chemical availability of the freshly spiked and aged DDE in soil.

    PubMed

    Škulcová, L; Neuwirthová, N; Hofman, J; Bielská, L

    2016-05-01

    The study compared the ability of various chemical methods (XAD, β-hydroxypropylcyclodextrin - HPCD) and solid phase micro-extraction (SPME)) to mimic earthworm uptake from two similar soils containing either spiked or aged p,p´-DDE, thus representing two extreme scenarios with regard to the length of pollutant-soil contact time and the way of contamination. The extent of bioaccumulation was assessed at fixed exposure periods (10 and 21 days) and at equilibrium derived from uptake curves by multiple-point comparison or kinetic modeling. The decision on the best chemical predictor of biological uptake differed. The degree of bioaccumulation at equilibrium was best predicted by XAD while HPCD rather reflected the extent of accumulation derived after 21 days when, however, steady-state was not reached for spiked p,p´-DDE. SPME seemed to underestimate the uptake of aged p,p´-DDE, probably of the fraction taken up via soil particles. Thus, the degree of predictability seems to be associated with the capability of the chemical method to mimic the complex earthworm uptake via skin and intestinal tract as well as with the quality of biological data where the insufficient length of exposure period appears to be the major concern. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. Evaluation of solid sorbents for the determination of fenhexamid, metalaxyl-M, pyrimethanil, malathion and myclobutanil residues in air samples: application to monitoring malathion and fenhexamid dissipation in greenhouse air using C-18 or Supelpak-2 for sampling.

    PubMed

    Tsiropoulos, Nikolaos G; Bakeas, Evangelos B; Raptis, Vasilios; Batistatou, Stavroula S

    2006-07-28

    A methodology is described for greenhouse air analysis by sampling fenhexamid, pyrimethanil, malathion, metalaxyl-M and myclobutanil in solid sorbents. Pesticides were determined by gas chromatography with NP Detector. The trapping efficiency of XAD-2, XAD-4, Supelpak-2, Florisil and C-18 at different sampling conditions (rate, time and air humidity) and pesticides concentration levels has been evaluated. No breakthrough was observed in the range of concentration studied (0.10-75 microg of each pesticide). In almost all the cases good stability results were obtained. Personal pumps have been used with selected sorbents (Supelpak-2 and C-18) in order to sample malathion and fenhexamid in air of experimental greenhouse after their application in a tomato crop. The dissipation process of the analytes in various time periods after application has been studied. Malathion concentrations varied between 20.1 microg m(-3) just after application and 1.06 microg m(-3) 3 days later. Fenhexamid concentrations, determined by high performance liquid chromatography with UV detection, fall rapidly; after 12 h post-application being below 0.50 microg m(-3).

  5. Structure/Property Relationships of Cyanate Ester Resins from Renewable Sources

    DTIC Science & Technology

    2013-04-11

    derived from lignin . These materials possess favorable thermal and water uptake properties with dry glass transition temperatures above 200°C and wet...distribution is unlimited. Creosol as a Monomer Source 7 • Input material cost is an important consideration for cyanate ester resins • Lignin is...from lignin • Oxidative and reductive coupling reactions lead to precursor phenols, which are then treated with cyanogen bromide to generate cyanate

  6. Glass ionomer ART sealant and fluoride-releasing resin sealant in fissure caries prevention – results from a randomized clinical trial

    PubMed Central

    2014-01-01

    Background The relative performance of ART sealant and fluoride-releasing resin sealant in preventing fissure caries in permanent molars was compared in a randomized clinical trial conducted in southern China (ClinicalTrials.gov NCT01829334). Methods After obtaining ethical approval, healthy schoolchildren who had permanent first molars with occlusal fissures which were sound but deep or presented with only incipient caries were recruited for the study. Included molars were randomly allocated into one of four parallel study groups in units of left/right teeth per mouth. Two of the four groups adopted the methods of ART or fluoride-releasing resin sealant placement while the other two groups adopted the topical fluoride application methods. Fissure status of the molars in each group was evaluated every 6 months. Development of dentine caries and sealant retention over 24 months in the molars in the two sealant-using groups was compared in this report. Outcome on cost-effectiveness of all four groups over 36 months will be reported elsewhere. Results At baseline, a total of 280 children (383 molars) with mean age 7.8 years were involved for the two sealant groups. After 24 months, 261 children (357 molars) were followed. Proportions of molars with dentine caries were 7.3% and 3.9% in the ART sealant and fluoride-releasing resin sealant groups, respectively (chi-square test, p = 0.171). Life-table survival analysis showed that sealant retention (full and partial) rate over 24 months for the resin sealant (73%) was significantly higher than that (50%) for the ART sealant (p < 0.001). Molar survival (no development of dentine caries) rates in the ART sealant (93%) and fluoride-releasing resin sealant (96%) groups were not significantly different (p = 0.169). Multilevel logistic regression (GEE modeling) accounting for the effects of data clustering and confounding factors confirmed this finding. Conclusions Though the retention of fluoride-releasing resin sealant was better than that of the ART sealant, their effectiveness in preventing fissure caries in permanent molars did not differ significantly over 24 months. ART sealants could be a good alternative when and where resources for resin sealant placement are not readily available. PMID:24886444

  7. Reinforcing effects of different fibers on denture base resin based on the fiber type, concentration, and combination.

    PubMed

    Yu, Sang-Hui; Lee, Yoon; Oh, Seunghan; Cho, Hye-Won; Oda, Yutaka; Bae, Ji-Myung

    2012-01-01

    The aim of this study was to evaluate the reinforcing effects of three types of fibers at various concentrations and in different combinations on flexural properties of denture base resin. Glass (GL), polyaromatic polyamide (PA) and ultra-high molecular weight polyethylene (PE) fibers were added to heat-polymerized denture base resin with volume concentrations of 2.6%, 5.3%, and 7.9%, respectively. In addition, hybrid fiber-reinforced composite (FRC) combined with either two or three types of fibers were fabricated. The flexural strength, modulus and toughness of each group were measured with a universal testing machine at a crosshead speed of 5 mm/min. In the single fiber-reinforced composite groups, the 5.3% GL and 7.9% GL had the highest flexural strength and modulus; 5.3% PE was had the highest toughness. Hybrid FRC such as GL/PE, which showed the highest toughness and the flexural strength, was considered to be useful in preventing denture fractures clinically.

  8. Microbial desalination cells packed with ion-exchange resin to enhance water desalination rate.

    PubMed

    Morel, Alexandre; Zuo, Kuichang; Xia, Xue; Wei, Jincheng; Luo, Xi; Liang, Peng; Huang, Xia

    2012-08-01

    A novel configuration of microbial desalination cell (MDC) packed with ion-exchange resin (R-MDC) was proposed to enhance water desalination rate. Compared with classic MDC (C-MDC), an obvious increase in desalination rate (DR) was obtained by R-MDC. With relatively low concentration (10-2 g/L NaCl) influents, the DR values of R-MDC were about 1.5-8 times those of C-MDC. Ion-exchange resins packed in the desalination chamber worked as conductor and thus counteracted the increase in ohmic resistance during treatment of low concentration salt water. Ohmic resistances of R-MDC stabilized at 3.0-4.7 Ω. By contrast, the ohmic resistances of C-MDC ranged from 5.5 to 12.7 Ω, which were 55-272% higher than those of R-MDC. Remarkable improvement in desalination rate helped improve charge efficiency for desalination in R-MDC. The results first showed the potential of R-MDC in the desalination of water with low salinity. Copyright © 2012 Elsevier Ltd. All rights reserved.

  9. Combined Detoxification and In-situ Product Removal by a Single Resin During Lignocellulosic Butanol Production

    PubMed Central

    Gao, Kai; Rehmann, Lars

    2016-01-01

    Phragmites australis (an invasive plant in North America) was used as feedstock for ABE (acetone-butanol-ethanol) fermentation by Clostridium saccharobutylicum. Sulphuric acid pretreated phragmites hydrolysate (SAEH) without detoxification inhibited butanol production (0.73 g/L butanol from 30 g/L sugars). The treatment of SAEH with resin L-493 prior the fermentation resulted in no inhibitory effects and an ABE titer of 14.44 g/L, including 5.49 g/L butanol was obtained, corresponding to an ABE yield and productivity of 0.49 g/g and 0.60 g/L/h, respectively. Dual functionality of the resin was realized by also using it as an in-situ product removal agent. Integrating in-situ product removal allowed for the use of high substrate concentrations without the typical product inhibition. Resin-detoxified SAEH was supplemented with neat glucose and an effective ABE titer of 33 g/L (including 13.7 g/L acetone, 16.4 g/L butanol and 1.9 g/L ethanol) was achieved with resin-based in-situ product removal, corresponding to an ABE yield and productivity of 0.41 g/g and 0.69 g/L/h, respectively. Both detoxification of the substrate and the products was achieved by the same resin, which was added prior the fermentation. Integrating hydrolysate detoxification and in-situ butanol removal in a batch process through single resin can potentially simplify cellulosic butanol production. PMID:27459906

  10. Lignin model compounds as bio-based reactive diluents for liquid molding resins.

    PubMed

    Stanzione, Joseph F; Sadler, Joshua M; La Scala, John J; Wool, Richard P

    2012-07-01

    Lignin is a copious paper and pulping waste product that has the potential to yield valuable, low molecular weight, single aromatic chemicals when strategically depolymerized. The single aromatic lignin model compounds, vanillin, guaiacol, and eugenol, were methacrylated by esterification with methacrylic anhydride and a catalytic amount of 4-dimethylaminopyridine. Methacrylated guaiacol (MG) and methacrylated eugenol (ME) exhibited low viscosities at room temperature (MG: 17 cP and ME: 28 cP). When used as reactive diluents in vinyl ester resins, they produced resin viscosities higher than that of vinyl ester-styrene blends. The relative volatilities of MG (1.05 wt% loss in 18 h) and ME (0.96 wt% loss in 18 h) measured by means of thermogravimetric analysis (TGA) were considerably lower than that of styrene (93.7 wt% loss in 3 h) indicating the potential of these chemicals to be environmentally friendly reactive diluents. Bulk polymerization of MG and ME generated homopolymers with glass transition temperatures (T(g)s) of 92 and 103 °C, respectively. Blends of a standard vinyl ester resin with MG and ME (50 wt % reactive diluent) produced thermosets with T(g)s of 127 and 153 °C, respectively, which are comparable to vinyl ester-styrene resins, thus demonstrating the ability of MG and ME to completely replace styrene as reactive diluents in liquid molding resins without sacrificing cured-resin thermal performance. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Simultaneous separation and purification of flavonoids and oleuropein from Olea europaea L. (olive) leaves using macroporous resin.

    PubMed

    Li, Chen; Zheng, Yuanyuan; Wang, Xiaofei; Feng, Shilan; Di, Duolong

    2011-12-01

    This study developed a feasible process to simultaneously separate and purify polyphenols, including flavonoids and oleuropein, from the leaves of Olea europaea L. Macroporous resins were used as the separation and purification materials. The performance and separation capabilities of eight resins (D101, DM130, HPD450, LSA-21, LSA-40, 07C, LSD001 and HPD600) were systematically evaluated. The contents of target polyphenols in different extracts were determined using ultraviolet (for flavonoids) and high-performance liquid chromatographic (for oleuropein) methods. The static adsorption and desorption results showed that resin LSA-21 had better adsorption properties among the eight resins. Influential factors such as extraction method, pH value of feeding solution, desorption solution, adsorption kinetics and adsorption isotherm, etc. to the extraction and purification of these polyphenols were successively investigated on resin LSA-21. The target flavonoids and oleuropein were selectively purified using resin LSA-21. Compared with the contents in raw leaves, the contents of total flavonoids and oleuropein in the final purified products were increased 13.2-fold (from 16 to 211 g kg(-1) ) and 7.5-fold (from 120 to 902 g kg(-1) ) with recovery yields of 87.9% and 85.6%, respectively. This extraction and purification method could be used in the large-scale enrichment or purification of flavonoids, oleuropein and other polyphenols from O. europaea L. leaves or other herbal materials in industrial, food processing and medical manufacture. Copyright © 2011 Society of Chemical Industry.

  12. Adsorptive removal of antibiotics from water using magnetic ion exchange resin.

    PubMed

    Wang, Tianyue; Pan, Xun; Ben, Weiwei; Wang, Jianbing; Hou, Pin; Qiang, Zhimin

    2017-02-01

    The occurrence of antibiotics in the environment has recently raised serious concern regarding their potential threat to aquatic ecosystem and human health. In this study, the magnetic ion exchange (MIEX) resin was applied for removing three commonly-used antibiotics, sulfamethoxazole (SMX), tetracycline (TCN) and amoxicillin (AMX) from water. The results of batch experiments show that the maximum adsorption capacities on the MIEX resin for SMX, TCN and AMX were 789.32, 443.18 and 155.15μg/mL at 25°C, respectively, which were 2-7 times that for the powdered activated carbon. The adsorption kinetics of antibiotics on the MIEX resin could be simulated by the pseudo-second-order model (R 2 =0.99), and the adsorption isotherm data were well described by the Langmuir model (R 2 =0.97). Solution pH exhibited a remarkable impact on the adsorption process and the absorbed concentrations of the tested antibiotics were obtained around the neutral pH. The MIEX resin could be easily regenerated by 2mol/L NaCl solution and maintained high adsorption removal for the tested antibiotics after regeneration. Anion exchange mechanism mainly controlled the adsorption of antibiotic and the formation of hydrogen binding between the antibiotic and resin can also result in the increase of adsorption capacity. The high adsorption capacity, fast adsorption rate and prominent reusability make the MIEX resin a potential adsorbent in the application for removing antibiotics from water. Copyright © 2016. Published by Elsevier B.V.

  13. Biological activity of some naturally occurring resins, gums and pigments against in vitro LDL oxidation.

    PubMed

    Andrikopoulos, Nikolaos K; Kaliora, Andriana C; Assimopoulou, Andreana N; Papapeorgiou, Vassilios P

    2003-05-01

    Naturally occurring gums and resins with beneficial pharmaceutical and nutraceutical properties were tested for their possible protective effect against copper-induced LDL oxidation in vitro. Chiosmastic gum (CMG) (Pistacia lentiscus var. Chia resin) was the most effective in protecting human LDL from oxidation. The minimum and maximum doses for the saturation phenomena of inhibition of LDL oxidation were 2.5 mg and 50 mg CMG (75.3% and 99.9%, respectively). The methanol/water extract of CMG was the most effective compared with other solvent combinations. CMG when fractionated in order to determine a structure-activity relationship showed that the total mastic essential oil, collofonium-like residue and acidic fractions of CMG exhibited a high protective activity ranging from 65.0% to 77.8%. The other natural gums and resins (CMG resin 'liquid collection', P. terebinthus var. Chia resin, dammar resin, acacia gum, tragacanth gum, storax gum) also tested as above, showed 27.0%-78.8% of the maximum LDL protection. The other naturally occurring substances, i.e. triterpenes (amyrin, oleanolic acid, ursolic acid, lupeol, 18-a-glycyrrhetinic acid) and hydroxynaphthoquinones (naphthazarin, shikonin and alkannin) showed 53.5%-78.8% and 27.0%-64.1% LDL protective activity, respectively. The combination effects (68.7%-76.2% LDL protection) of ursolic-, oleanolic- and ursodeoxycholic- acids were almost equal to the effect (75.3%) of the CMG extract in comparable doses. Copyright 2003 John Wiley & Sons, Ltd.

  14. Combined Detoxification and In-situ Product Removal by a Single Resin During Lignocellulosic Butanol Production

    NASA Astrophysics Data System (ADS)

    Gao, Kai; Rehmann, Lars

    2016-07-01

    Phragmites australis (an invasive plant in North America) was used as feedstock for ABE (acetone-butanol-ethanol) fermentation by Clostridium saccharobutylicum. Sulphuric acid pretreated phragmites hydrolysate (SAEH) without detoxification inhibited butanol production (0.73 g/L butanol from 30 g/L sugars). The treatment of SAEH with resin L-493 prior the fermentation resulted in no inhibitory effects and an ABE titer of 14.44 g/L, including 5.49 g/L butanol was obtained, corresponding to an ABE yield and productivity of 0.49 g/g and 0.60 g/L/h, respectively. Dual functionality of the resin was realized by also using it as an in-situ product removal agent. Integrating in-situ product removal allowed for the use of high substrate concentrations without the typical product inhibition. Resin-detoxified SAEH was supplemented with neat glucose and an effective ABE titer of 33 g/L (including 13.7 g/L acetone, 16.4 g/L butanol and 1.9 g/L ethanol) was achieved with resin-based in-situ product removal, corresponding to an ABE yield and productivity of 0.41 g/g and 0.69 g/L/h, respectively. Both detoxification of the substrate and the products was achieved by the same resin, which was added prior the fermentation. Integrating hydrolysate detoxification and in-situ butanol removal in a batch process through single resin can potentially simplify cellulosic butanol production.

  15. Influence of different adhesive systems on the pull-out bond strength of glass fiber posts.

    PubMed

    da Silva, Luciana Mendonça; Andrade, Andréa Mello de; Machuca, Melissa Fernanda Garcia; da Silva, Paulo Maurício Batista; da Silva, Ricardo Virgolino C; Veronezi, Maria Cecília

    2008-01-01

    This in vitro study evaluated the tensile bond strength of glass fiber posts (Reforpost - Angelus-Brazil) cemented to root dentin with a resin cement (RelyX ARC - 3M/ESPE) associated with two different adhesive systems (Adper Single Bond - 3M/ESPE and Adper Scotchbond Multi Purpose (MP) Plus - 3M/ESPE), using the pull-out test. Twenty single-rooted human teeth with standardized root canals were randomly assigned to 2 groups (n=10): G1- etching with 37% phosphoric acid gel (3M/ESPE) + Adper Single Bond + #1 post (Reforpost - Angelus) + four #1 accessory posts (Reforpin - Angelus) + resin cement; G2- etching with 37% phosphoric acid gel + Adper Scotchbond MP Plus + #1 post + four #1 accessory posts + resin cement. The specimens were stored in distilled water at 37 degrees C for 7 days and submitted to the pull-out test in a universal testing machine (EMIC) at a crosshead speed of 0.5 mm/min. The mean values of bond strength (kgf) and standard deviation were: G1- 29.163 +/- 7.123; G2- 37.752 +/-13.054. Statistical analysis (Student's t-test; a=0.05 showed no statistically significant difference (p<0.05) between the groups. Adhesive bonding failures between resin cement and root canal dentin surface were observed in both groups, with non-polymerized resin cement in the apical portion of the post space when Single Bond was used (G1). The type of adhesive system employed on the fiber post cementation did not influence the pull-out bond strength.

  16. Polymerization contraction stress in thin resin composite layers as a function of layer thickness.

    PubMed

    Alster, D; Feilzer, A J; de Gee, A J; Davidson, C L

    1997-05-01

    In the present study, the effect of layer thickness on the curing stress in thin resin composite layers was investigated. Since the value of the contraction stress is dependent on the compliance of the measuring equipment (especially for thin films), a method to determine the compliance of the test apparatus was tested. A chemically initiated resin composite (Clearfil F2, Kuraray) was inserted between two sandblasted and silane-coated stainless steel discs in a tensilometer. The curing contraction of the cylindrical samples was continuously counteracted by feedback displacement of the tensilometer crosshead, and the curing stress development was registered. After 20 min, the samples were loaded in tension until fracture. The curing stress was determined for layer thicknesses of 50, 100, 200, 300, 400, 500, 600, 700 microns, 1.4 mm and 2.7 mm. The compliance of the apparatus was calculated with the aid of a non-linear regression analysis, using an equation derived from Hooke's Law as the model. None of the samples fractured due to contraction stress prior to tensile loading. The contraction stress after 20 min decreased from 23.3 +/- 5.3 MPa for the 50 microns layer to 5.5 +/- 0.6 MPa for the 2.7 mm layer. The compliance on the apparatus was 0.029 mm/MPa. A measuring method was developed which was found to be suitable for the determination of axial polymerization contraction stress in this films of chemically initiated resin composites. The method makes it possible to estimate the stress levels that occur in resin composite films in the clinical situation.

  17. [Effect of hydrofluoric acid etching time on the resin bond durability of glass ceramic].

    PubMed

    Meng, Xiang-feng; Zhou, Xiao-lu; Luo, Xiao-ping

    2010-05-01

    To analyze the effect of hydrofluoric acid (HFA) etching time on the resin bond durability of glass ceramic. Three groups of samples of machinable glass ceramic (ProCAD) were etched by 4.8% HFA for 0, 30 and 60 s respectively. The roughness parameters (Ra, Sm, S) and surface area of the samples, were measured with a 3D-laser scanning microscope. Then the ceramic surfaces were bonded with four resin cements (silane coupler/resin cement), which were Monobond S/Variolink II, Clearfil Ceramic Primer/Clearfil Esthetic Cement, GC Ceramic Primer/Linkmax HV, and Porcelain Liner M/SuperBond. The micro-bond strengths between the ceramic and the resin were tested at baseline and after the samples had been treated in 30000 thermal cycles. The Ra [(3.89+/-1.94), (12.53+/-0.80), (13.58+/-1.10) microm] and surface area [(7.81+/-2.96), (30.18+/-2.05), (34.16+/-1.97) mm2] of ceramic increased with the increase of HFA etching time. The thermal cycling test reduced the bond strength of all test groups. The bond strength of Monobond S/Variolink II group [(3.59+/-3.51), (16.18+/-2.62), (20.33+/-2.45) MPa] and Clearfil Ceramic Primer/Clearfil Esthetic Cement group [(4.74+/-2.08), (7.77+/-1.55), (13.45+/-3.75) MPa] increased with the increase of HFA etching time; 30 s HFA etching group of Porcelain Liner M/SuperBond had higher bond strength [(22.00+/-1.64) MPa] than its 0 s HFA etching group [(12.96+/-4.17) MPa], and no significant difference was found between the 30 s and 60 s HFA etching groups of Porcelain Liner M/SuperBond [(20.42+/-3.01) MPa]. HFA etching time had no effect on the bond strength of GC Ceramic Primer/Linkmax HV. HFA etching can improve the resin bond durability of glass ceramic, and the etching time is not only related to the change of ceramic surface roughness and area, but also to the characteristics of resins.

  18. Retention of metal-ceramic crowns with contemporary dental cements.

    PubMed

    Johnson, Glen H; Lepe, Xavier; Zhang, Hai; Wataha, John C

    2009-09-01

    New types of crown and bridge cement are in use by practitioners, and independent studies are needed to assess their effectiveness. The authors conducted a study in three parts (study A, study B, and study C) and to determine how well these new cements retain metal-ceramic crowns. The authors prepared teeth with a 20-degree taper and a 4-millimeter length. They cast high-noble metal-ceramic copings, then fitted and cemented them with a force of 196 newtons. The types of cements they used were zinc phosphate, resin-modified glass ionomer, conventional resin and self-adhesive modified resin. They thermally cycled the cemented copings, then removed them. They recorded the removal force and calculated the stress of dislodgment by using the surface area of each preparation. They used a single-factor analysis of variance to analyze the data (alpha = .05). The mean stresses necessary to remove crowns, in megapascals, were 8.0 for RelyX Luting (3M ESPE, St. Paul, Minn.), 7.3 for RelyX Unicem (3M ESPE), 5.7 for Panavia F (Kuraray America, New York) and 4.0 for Fuji Plus (GC America, Alsip, Ill.) in study A; 8.1 for RelyX Luting, 2.6 for RelyX Luting Plus (3M ESPE) and 2.8 for Fuji CEM (GC America) in study B; and 4.9 for Maxcem (Kerr, Orange, Calif.), 4.0 for BisCem (Bisco, Schaumburg, Ill.), 3.7 for RelyX Unicem Clicker (3M ESPE), 2.9 for iCEM (Heraeus Kulzer, Armonk, N.Y.) and 2.3 for Fleck's Zinc Cement (Keystone Industries, Cherry Hill, N.J.) in study C. Powder-liquid versions of new cements were significantly more retentive than were paste-paste versions of the same cements. The mean value of crown removal stress for the new self-adhesive modified-resin cements varied appreciably among the four cements tested. All cements retained castings as well as or better than did zinc phosphate cement. Powder-liquid versions of cements, although less convenient to mix, may be a better clinical choice when crown retention is an issue. All cements tested will retain castings adequately on ideal preparations because the corresponding removal stresses are comparable with or higher than those associated with zinc phosphate. Powder-liquid resin-modified glass ionomer cement, selected self-adhesive modified-resin cements and conventional resin cements provide additional retention when desired.

  19. Characterization of an anti-tuberculosis resin glycoside from the prairie medicinal plant Ipomoea leptophylla.

    PubMed

    Barnes, Curtis C; Smalley, Mary K; Manfredi, Kirk P; Kindscher, Kelly; Loring, Hillary; Sheeley, Douglas M

    2003-11-01

    The organic soluble extract from the leaves of the native North American prairie plant Ipomoea leptophylla (big root morning glory) showed in vitro activity against M. tuberculosis. Bioassay-guided fractionation of this extract resulted in the identification of two new resin glycosides (6, 7). Base-catalyzed hydrolysis of these glycosides gave operculinic acid (1) as the glycosidic acid component as well as trans-cinnamic acid, propanoic acid, and lauric acid. The complete structure elucidation was accomplished through derivatization, 1D and 2D NMR spectroscopy (TOCSY, ROESY, HSQC, HMBC), and MS/MS experiments on 6 and 7 as well as the permethylated derivative 8.

  20. Effects of Macroporous Resin Size on Candida antarctica Lipase B Adsorption, Fraction of Active Molecules, and Catalytic Activity for Polyester Synthesis

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chen,B.; Miller, E.; Miller, L.

    2007-01-01

    Methyl methacrylate resins with identical average pore diameter (250 {angstrom}) and surface area (500 m{sup 2}/g) but with varied particle size (35 to 560-710 {mu}m) were employed to study how immobilization resin particle size influences Candida antarctica Lipase B (CALB) loading, fraction of active sites, and catalytic properties for polyester synthesis. CALB adsorbed more rapidly on smaller beads. Saturation occurred in less than 30 s and 48 h for beads with diameters 35 and 560-710 {mu}m, respectively. Linearization of adsorption isotherm data by the Scatchard analysis showed for the 35 {mu}m resin that: (1) CALB loading at saturation was wellmore » below that required to form a monolayer and fully cover the support surface and (2) CALB has a high affinity for this resin surface. Infrared microspectroscopy showed that CALB forms protein loading fronts for resins with particle sizes 560-710 and 120 {mu}m. In contrast, CALB appears evenly distributed throughout 35 {mu}m resins. By titration with p-nitrophenyl n-hexyl phosphate (MNPHP), the fraction of active CALB molecules adsorbed onto resins was <50% which was not influenced by particle size. The fraction of active CALB molecules on the 35 {mu}m support increased from 30 to 43% as enzyme loading was increased from 0.9 to 5.7% (w/w) leading to increased activity for {epsilon}-caprolactone ({epsilon}-CL) ring-opening polymerization. At about 5% w/w CALB loading, by decreasing the immobilization support diameter from 560-710 to 120, 75, and 35 {mu}m, conversion of {epsilon}-CL % to polyester increased (20 to 36, 42, and 61%, respectively, at 80 min). Similar trends were observed for condensation polymerizations between 1,8-octanediol and adipic acid.« less

  1. Verification of a three-dimensional resin transfer molding process simulation model

    NASA Technical Reports Server (NTRS)

    Fingerson, John C.; Loos, Alfred C.; Dexter, H. Benson

    1995-01-01

    Experimental evidence was obtained to complete the verification of the parameters needed for input to a three-dimensional finite element model simulating the resin flow and cure through an orthotropic fabric preform. The material characterizations completed include resin kinetics and viscosity models, as well as preform permeability and compaction models. The steady-state and advancing front permeability measurement methods are compared. The results indicate that both methods yield similar permeabilities for a plain weave, bi-axial fiberglass fabric. Also, a method to determine principal directions and permeabilities is discussed and results are shown for a multi-axial warp knit preform. The flow of resin through a blade-stiffened preform was modeled and experiments were completed to verify the results. The predicted inlet pressure was approximately 65% of the measured value. A parametric study was performed to explain differences in measured and predicted flow front advancement and inlet pressures. Furthermore, PR-500 epoxy resin/IM7 8HS carbon fabric flat panels were fabricated by the Resin Transfer Molding process. Tests were completed utilizing both perimeter injection and center-port injection as resin inlet boundary conditions. The mold was instrumented with FDEMS sensors, pressure transducers, and thermocouples to monitor the process conditions. Results include a comparison of predicted and measured inlet pressures and flow front position. For the perimeter injection case, the measured inlet pressure and flow front results compared well to the predicted results. The results of the center-port injection case showed that the predicted inlet pressure was approximately 50% of the measured inlet pressure. Also, measured flow front position data did not agree well with the predicted results. Possible reasons for error include fiber deformation at the resin inlet and a lag in FDEMS sensor wet-out due to low mold pressures.

  2. Bond Strength of Resin Cements to Zirconia Ceramic Using Adhesive Primers.

    PubMed

    Stefani, Ariovaldo; Brito, Rui Barbosa; Kina, Sidney; Andrade, Oswaldo Scopin; Ambrosano, Gláucia Maria Bovi; Carvalho, Andreia Assis; Giannini, Marcelo

    2016-07-01

    To evaluate the influence of adhesive primers on the microshear bond strength of resin cements to zirconia ceramic. Fifty zirconia plates (12 mm × 5 mm × 1.5 mm thick) of a commercially available zirconium oxide ceramic (ZirCad) were sintered, sandblasted with aluminum oxide particles, and cleaned ultrasonically before bonding. The plates were randomly divided into five groups of 10. Three resin cements were selected (RelyX ARC, Multilink Automix, Clearfil SA Cement self-adhesive resin cement), along with two primers (Metal-Zirconia Primer, Alloy Primer) and one control group. The primers and resin cements were used according to manufacturers' recommendations. The control group comprised the conventional resin cement (RelyX ARC) without adhesive primer. Test cylinders (0.75 mm diameter × 1 mm high) were formed on zirconia surfaces by filling cylindrical Tygon tube molds with resin cement. The specimens were stored in distilled water for 24 hours at 37°C, then tested for shear strength on a Shimadzu EZ Test testing machine at 0.5 mm/min. Bond strength data were analyzed statistically by two-way ANOVA and Dunnett's test (5%). The bond strength means in MPa (± s.d.) were: RelyX ARC: 28.1 (6.6); Multilink Automix: 37.6 (4.5); Multilink Automix + Metal-Zirconia Primer: 55.7 (4.0); Clearfil SA Cement: 46.2 (3.3); and Clearfil SA Cement + Alloy Primer: 47.0 (4.1). Metal-Zirconia Primer increased the bond strength of Multilink Automix resin cement to zirconia, but no effect was observed for Alloy Primer using Clearfil SA Cement. RelyX ARC showed the lowest bond strength to zirconia. © 2015 by the American College of Prosthodontists.

  3. A Continuous Procedure Based on Column Chromatography to Purify Anthocyanins from Schisandra chinensis by a Macroporous Resin plus Gel Filtration Chromatography.

    PubMed

    Yue, Daran; Yang, Lei; Liu, Shouxin; Li, Jian; Li, Wei; Ma, Chunhui

    2016-02-06

    In our previous study, as natural food colorants and antioxidants, the color and content stabilities of Schisandra chinensis (S. chinensis) anthocyanins were investigated. In this work, the purification process parameters of S. chinensis anthocyanins using a macroporous resin and gel filtration chromatography were evaluated. The optimized parameters of static adsorption and desorption were as follows. The selected resin is HPD-300 (nonpolar copolymer styrene type resin), and the anthocyanins adsorption saturation capacity of HPD-300 resin was 0.475 mg/g dry resin. Adsorption time was 4 h, and 0.517 mg/mL of S. chinensis anthocyanins was adsorbed on the resin column with a flow rate of 39 mL/h (3 BV/h). After adsorption, the anthocyanins were completely desorpted with 2.5 BV of 90% (v/v) ethanol solution, and the desorption flow rate was 13 mL/h (1 BV/h). After purification by dynamic adsorption and desorption, the anthocyanins content in the effluent increased from 47.6 mg/g to 128.4 mg/g, the purity of anthocyanins increased six-fold from 5.08% to 30.43%, and the anthocyanins recovery was 96.5%. The major constituent of S. chinensis anthocyanins was isolated with Bio-Gel P2 gel filtration chromatography, and it was detected by liquid chromatography electrospray ionisation tandem mass spectrometry (LC-ESI-MS) as cyanidin-3-O-xylosylrutinoside. Moreover, the antioxidant activities of S. chinensis anthocyanins were investigated. After purification using the HPD-300 resin, the antioxidant activities of anthocyanins were increased 1.2-fold (FRAP) and 1.7-fold (ABTS).

  4. Fundamental aspects related to batch and fixed-bed sulfate sorption by the macroporous type 1 strong base ion exchange resin Purolite A500.

    PubMed

    Guimarães, Damaris; Leão, Versiane A

    2014-12-01

    Acid mine drainage is a natural process occurring when sulfide minerals such as pyrite are exposed to water and oxygen. The bacterially catalyzed oxidation of pyrite is particularly common in coal mining operations and usually results in a low-pH water polluted with toxic metals and sulfate. Although high sulfate concentrations can be reduced by gypsum precipitation, removing lower concentrations (below 1200 mg/L) remains a challenge. Therefore, this work sought to investigate the application of ion exchange resins for sulfate sorption. The macroporous type 1 strong base IX resin Purolite A500 was selected for bath and fixed-bed sorption experiments using synthetic sulfate solutions. Equilibrium experiments showed that sulfate loading on the resin can be described by the Langmuir isotherm with a maximum uptake of 59 mg mL-resin(-1). The enthalpy of sorption was determined as +2.83 kJ mol(-1), implying an endothermic physisorption process that occurred with decreasing entropy (-15.5 J mol(-1).K(-1)). Fixed-bed experiments were performed at different bed depths, flow rates, and initial sulfate concentrations. The Miura and Hashimoto model predicted a maximum bed loading of 25-30 g L-bed(-1) and indicated that both film diffusion (3.2 × 10(-3) cm s(-1) to 22.6 × 10(-3) cm s(-1)) and surface diffusion (1.46 × 10(-7) cm(2) s(-1) to 5.64 × 10(-7) cm(2) s(-1)) resistances control the sorption process. It was shown that IX resins are an alternative for the removal of sulfate from mine waters; they ensure very low residual concentrations, particularly in effluents where the sulfate concentration is below the gypsum solubility threshold. Copyright © 2014 Elsevier Ltd. All rights reserved.

  5. Biosorption of mercury by the inactivated cells of Pseudomonas aeruginosa PU21 (Rip64)

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chang, J.S.; Hong, J.

    1994-10-01

    Biomass of a mercury-resistance strain Pseudomonas aeruginosa PU21 (Rip64) and hydrogen-form cation exchange resin (AG 50W-X8) were investigated for their ability to adsorb mercury. The maximum adsorption capacity was approximately 180 mg Hg/g dry cell in deionized water and 400 mg Hg/g dry cell in sodium phosphate solution of pH 7.4, higher than the maximum mercury uptake capacity in the cation exchange resin. The mercury selectivity of the biomass over sodium ions was evaluated when 50 mM and 150 mM of Na[sup +] were present. Biosorption of mercury was also examined in sodium phosphate solution and phosphate-buffered saline solution containingmore » 50 mM and 150 mM of Na[sup +], respectively. It was found that the presence of Na[sup +] did not severely affect the biosorption of Hg[sup 2+], indicating a high mercury selectivity of the biomass over sodium ions. In contrast, the mercury uptake by the ion exchange resin was strongly inhibited by high sodium concentrations. The mercury biosorption was most favorable in sodium phosphate solution (pH 7.4), with a more than twofold increase in the maximum mercury uptake capacity. The pH was found to affect the adsorption of Hg[sup 2+] by the biomass and the optimal pH value was approximately 7.4. The adsorption of mercury on the biomass and the ion exchange resin appeared to follow the Langmuir or Freundlich adsorption isotherms.« less

  6. Wound healing activity of extracts derived from Shorea robusta resin.

    PubMed

    Yaseen Khan, Mohammad; Ali, Saleh Abbas; Pundarikakshudu, Kilambi

    2016-01-01

    Shorea robusta Gaertn.f. (Dipterocarpaceae) resin is used for treating infected wounds and burns by tribals in India. The objective of this study was to investigate wound-healing activity of S. robusta resin extracts and essential oil in rats. Methanol extract (SRME), petroleum ether, benzene insoluble fraction of methanol extract (SRPEBIME), and essential oil (SREO) of S. robusta resin were incorporated in soft yellow paraffin (10% w/w) and applied once daily on incision and excision wounds of Wistar rats. Framycetin ointment (1.0% w/w) was applied to the standard group. Tensile strength (on the 10th day), wound contraction, and scar area (on the 14th day) were recorded. On the 15th day, granulation tissues of excision wounds were analyzed for total protein, hydroxyproline, and hexosamine contents and activities of lipid peroxidation and super oxide dismutase (SOD). Histopathology of the wounds was also studied. SRPEBIME and SREO healed incision and excision wounds faster than plain ointment base and framycetin. Tensile strength of SRPEBIME-treated incision wounds was 53% higher than that of control animals. In excision wounds, wound contraction and scar areas were found to be 99% and 7.7 mm(2) (SRPEBIME) and 71.7% and 21 mm(2) (control). Protein and hydroxyproline contents were higher in SRPEBIME (20.8 and 3.5% w/w) and SREO (17.4 and 2.8% w/w) groups as against 9.95 and 1.48% w/w in control groups. Histopathology revealed complete epithelization and new blood vessel formation in SRPEBIME groups. SRPEBIME and SREO have significant wound-healing activities on incision and excision wounds.

  7. Industrial Hygiene Air Sampling and Bulk Sampling Instructions

    DTIC Science & Technology

    1990-12-01

    registered trademark of Johns - Manville Products Corp., Denver, CO. "Cellosolve is a registered trademark of Union Carbide Corp., 270 Park Ave, New...registered trademark of Johns - Manville Products Corp., Denver, CO. 0 &Florisil is a registered trademark of Floridin Company, ITT System, Pittsburgh, PA. C...Thermosorb is a registered trademark of Johns - Manville Products Corp., Denver, CO. ®XAD-2 is a registered trademark of Rohm and Haas, Philadelphia, PA. C

  8. Chemical analysis of monomers in epoxy resins based on bisphenols F and A.

    PubMed

    Pontén, A; Zimerson, E; Sörensen, O; Bruze, M

    2004-05-01

    Diglycidyl ether of bisphenol A (DGEBA) is the monomer and most important contact allergen in epoxy resin(s) based on bisphenol A (DGEBA-R). Both thin-layer chromatography (TLC) and high-pressure liquid chromatography (HPLC) methods are available for the analysis of products containing DGEBA-R. With respect to detection and quantification, epoxy resins of the bisphenol F-type, i.e. epoxy resins containing the isomers of diglycidyl ethers of bisphenol F (DGEBF), are not as well investigated as DGEBA-R. The isomers of DGEBF are p,p'-DGEBF, o,p'-DGEBF and o,o'-DGEBF. Both p,p'-DGEBF and o,p'-DGEBF have been shown to be contact allergens in humans, and all 3 isomers are sensitizers in the guinea pig maximization test. We aimed (i). to develop HPLC methods for separation and purification of the individual DGEBF isomers, (ii). to detect and quantify the DGEBF isomers in epoxy resins of the bisphenol F-type and (iii). to evaluate and develop the TLC as a method for the detection of the DGEBF monomers. We found the total content of the DGEBF isomers in the investigated epoxy resins of the bisphenol F-type to vary from 17.0 to 81.7% w/w. Some of them also contained 0.1-2.4% w/w DGEBA. The HPLC method showed a sensitivity that was 2000-20 000x higher than that obtained with the TLC method for the DGEBF monomers. We concluded that the range of the DGEBF isomer content in epoxy resins of the bisphenol F-type is approximately the same as the monomer content in liquid compared to solid DGEBA-R. The relevance of contact allergy to DGEBA-R can remain unrecognized if the suspected product is an epoxy resin of the bisphenol F-type, which is analysed with the TLC method.

  9. Color stainability of CAD/CAM and nanocomposite resin materials.

    PubMed

    Acar, Ozlem; Yilmaz, Burak; Altintas, Subutay Han; Chandrasekaran, Indumathi; Johnston, William M

    2016-01-01

    The color stainability of recently introduced computer-assisted design/computer-assisted manufacturing (CAD/CAM) hybrid ceramic and resin nanoceramic is unknown. The purpose of this in vitro study was to compare the effect of coffee staining on the color of 3 different CAD/CAM restorative materials and a nanocomposite resin. Specimens from a hybrid dental ceramic (VITA Enamic), a resin nanoceramic (Lava Ultimate), a lithium disilicate glass ceramic (IPS e.max CAD), and a nanocomposite resin (Filtek Supreme Ultra Universal) were evaluated for color change due to thermocycling in coffee (n=5). Specimens 0.5 to 0.7 mm and 1 to 1.2 mm in thickness were thermocycled for 5000 cycles. CIEDE2000 color differences (ΔE00) due to thermocycling in coffee were calculated using the color coordinates obtained from a spectroradiometer. ANCOVA was used to analyze the color differences among the materials with thickness as the covariate. Significant differences at average thickness were analyzed with the Tukey-Kramer test. For color difference due to staining, thickness was a significant covariate (P<.001). Regarding the analysis of color differences, every pair of the tested materials was significantly different (P<.001). Least squares means of color differences (ΔE00) at mean thickness were 4.34 for the nanohybrid composite resin, 3.66 for the resin nanoceramic, 1.35 for the hybrid ceramic, and 0.43 for the lithium disilicate ceramic. When exposed to hot and cold coffee, the color change was beyond clinical acceptability for the tested resin nanoceramic and nanocomposite resin materials. The average color change of the hybrid ceramic was clinically perceivable over the tested thickness values. The color change of lithium disilicate ceramic was not clinically perceivable at any tested thickness. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  10. Resin purification from Dragons Blood by using sub critical solvent extraction method

    NASA Astrophysics Data System (ADS)

    Saifuddin; Nahar

    2018-04-01

    Jernang resin (dragon blood) is the world's most expensive sap. The resin obtained from jernang that grows only on the islands of Sumatra and Borneo. Jernang resin is in demand by the State of China, Hong Kong, and Singapore since they contain compounds that have the potential dracohordin as a medicinal ingredient in the biological and pharmacological activity such as antimicrobial, antiviral, antitumor and cytotoxic activity. The resin extracting process has conventionally been done by drizzly with maceration method as one way of processing jernang, which is done by people in Bireuen, Aceh. However, there are still significant obstacles, namely the quality of the yield that obtained lower than the jernang resin. The technological innovation carried out by forceful extraction process maceration by using methanol produced a yield that is higher than the extraction process maceration method carried out in Bireuen. Nevertheless, the use of methanol as a solvent would raise the production costs due to the price, which is relatively more expensive and non-environmentally friendly. To overcome the problem, this research proposed a process, which is known as subcritical solvent method. This process is cheap, and also abundant and environmentally friendly. The results show that the quality of jernang resins is better than the one that obtained by the processing group in Bireuen. The quality of the obtained jernang by maceration method is a class-A quality based on the quality specification requirements of jernang (SNI 1671: 2010) that has resin (b/b) 73%, water (w/w) of 6.8%, ash (w/b) 7%, impurity (w/w) 32%, the melting point of 88°C and red colours. While the two-stage treatment obtained a class between class-A and super quality, with the resin (b/b) 0.86%, water (w/w) of 6.5%, ash (w/w) of 2.8%, levels of impurities (w/w) of 9%, the melting point of 88 °C and dark-red colours.

  11. Enhanced DOC removal using anion and cation ion exchange resins.

    PubMed

    Arias-Paic, Miguel; Cawley, Kaelin M; Byg, Steve; Rosario-Ortiz, Fernando L

    2016-01-01

    Hardness and DOC removal in a single ion exchange unit operation allows for less infrastructure, is advantageous for process operation and depending on the water source, could enhance anion exchange resin removal of dissolved organic carbon (DOC). Simultaneous application of cationic (Plus) and anionic (MIEX) ion exchange resin in a single contact vessel was tested at pilot and bench scales, under multiple regeneration cycles. Hardness removal correlated with theoretical predictions; where measured hardness was between 88 and 98% of the predicted value. Comparing bench scale DOC removal of solely treating water with MIEX compared to Plus and MIEX treated water showed an enhanced DOC removal, where removal was increased from 0.5 to 1.25 mg/L for the simultaneous resin application compared to solely applying MIEX resin. A full scale MIEX treatment plant (14.5 MGD) reduced raw water DOC from 13.7 mg/L to 4.90 mg/L in the treated effluent at a bed volume (BV) treatment rate of 800, where a parallel operation of a simultaneous MIEX and Plus resin pilot (10 gpm) measured effluent DOC concentrations of no greater than 3.4 mg/L, even at bed volumes of treatment 37.5% greater than the full scale plant. MIEX effluent compared to simultaneous Plus and MIEX effluent resulted in differences in fluorescence intensity that correlated to decreases in DOC concentration. The simultaneous treatment of Plus and MIEX resin produced water with predominantly microbial character, indicating the enhanced DOC removal was principally due to increased removal of terrestrially derived organic matter. The addition of Plus resin to a process train with MIEX resin allows for one treatment process to remove both DOC and hardness, where a single brine waste stream can be sent to sewer at a full-scale plant, completely removing lime chemical addition and sludge waste disposal for precipitative softening processes. Published by Elsevier Ltd.

  12. Novel 1,3-dioxanes from apple juice and cider.

    PubMed

    Kavvadias, D; Beuerle, T; Wein, M; Boss, B; König, T; Schwab, W

    1999-12-01

    Extracts obtained by XAD solid-phase extraction of apple juice and cider were separated by liquid chromatography on silica gel. Several new 1,3-dioxanes including the known 2-methyl-4-pentyl-1,3-dioxane and 2-methyl-4-[2'(Z)-pentenyl]-1,3-dioxane, were identified in the nonpolar fractions by GC/MS analysis and confirmed by chemical synthesis. The enantioselective synthesis of the stereoisomers of the 1,3-dioxanes was performed using (R)- and (R,S)-octane-1,3-diol and (R)- and (R,S)-5(Z)-octene-1,3-diol as starting material. Comparison with the isolated products indicated that the natural products consisted of a mixture of (2S,4R) and (2R,4R) stereoisomers in the ratio of approximately 10:1, except for 1,3-dioxanes generated from acetone and 2-butanone. It is assumed that the 1, 3-dioxanes are chemically formed in the apples and cider from the natural apple ingredients (R)-octane-1,3-diol, (R)-5(Z)-octene-1, 3-diol, (3R,7R)- and (3R,7S)-octane-1,3,7-triol, and the appropriate aldehydes and ketones, which are produced either by the apples or by yeast during fermentation of the apple juice.

  13. An Efficient Protocol for Preparation of Gallic Acid from Terminalia bellirica (Gaertn.) Roxb by Combination of Macroporous Resin and Preparative High-Performance Liquid Chromatography.

    PubMed

    Zou, Denglang; Chen, Tao; Chen, Chen; Li, Hongmei; Liu, Yongling; Li, Yulin

    2016-08-01

    In this article, macroporous resin column chromatography and preparative high-performance liquid chromatography were applied for preparation of gallic acid from Terminalia bellirica (Gaertn.) Roxb. In the first step, six kinds of resins were investigated by adsorption and desorption tests and AB-8 macroporous resin was selected for the enrichment of gallic acid. As a result, 20 g of gallic acid at a purity of 71% could be separated from 100 g of crude extract in which the content of gallic acid was 16.7% and the recovery of gallic acid reached 85.0%. In the second step, preparative high-performance liquid chromatography was selected to purify gallic acid. As a result, 640 mg of gallic acid at a purity of 99.1% was obtained from 1 g of sample in 35 min. The results demonstrated that macroporous resin coupled with preparative high-performance liquid chromatography was suitable for preparation of gallic acid from T. bellirica (Gaertn.) Roxb. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  14. Combining Through-Thickness Reinforcement and Self-Healing for Improved Damage Tolerance and Durability of Composites

    NASA Technical Reports Server (NTRS)

    O'Brien, T. Kevin; Czabaj, Michael W.; Hinkley, Jeffrey A.; Tsampas, Spiros; Greenhalgh, Emile S.; McCombe, Gregory; Bond, Ian P.; Trask, Richard

    2013-01-01

    A study was undertaken to develop a prototype method for adding through-thickness hollow glass tubes infused with uncured resin and hardener in a carbon Z-pin through-thickness reinforcement field embedded in a composite laminate. Two types of tube insertion techniques were attempted in an effort to ensure the glass tubes survived the panel manufacturing process. A self-healing resin was chosen with a very low viscosity, two component, liquid epoxy resin system designed to be mixed at a 2-to-1 ratio of epoxy to hardener. IM7/8552 carbon epoxy double cantilever beam (DCB) specimens were cut from the hybrid Z-pin and glass tube reinforced panels and tested. In-situ injection of resin and hardener directly into glass tubes, in a staggered pattern to allow for 2-to-1 ratio mixing, resulted in partial healing of the fracture plane, but only if the injection was performed while the specimen was held at maximum load after initial fracture. Hence, there is some potential for healing delamination via resin and hardener delivered through a network of through-thickness glass tubes, but only if the tubes are connected to a reservoir where additional material may be injected as needed.

  15. Influence of different materials and techniques to transfer molding in multiple implants.

    PubMed

    Faria, Júlio C B; Cruz, Fernando L G; Silva-Concílio, Laís R; Neves, Ana C C

    2012-01-01

    The aim of this study was to compare different materials and techniques used in transfer molding of multiple implants, by evaluating the space between implants and superstructure. Four external hexagon implants were fixed in a master template and the same on a superstructure. Transfer molding of implants were done using the direct and indirect techniques, with transfers united or not, using the union chemically activated acrylic resin (QA) and other groups polymerized acrylic resin (FT), and sectioned and not split. The casts were made with polyether and models divided into 8 groups (n = 5). The space between the superstructure and the master implants was measured with a microscope and the data was analyzed statistically by Student's t test (p < 0.05). For the material of union there was no significant difference, except when the groups were compared with the resin Duralay QA (G4) and the resin Duolay FT (G8) and groups using resins Duolay QA (G5) and Duolay FT (G7) for the union of the transfers. When comparing the groups who had the union between the transfers and sectioned again united with those in which the union was not severed there was no statistically significant difference. QA resin was superior to the FT with respect to the union of transfers. Techniques with united transfers or not were similar.

  16. Radiopacity of conventional, resin-modified glass ionomer, and resin-based luting materials.

    PubMed

    Tsuge, Takuma

    2009-06-01

    The purpose of the present study was to evaluate the radiopacity of currently available dental luting materials. Five conventional cements, six resin-modified glass ionomers (RMGIs), two methyl methacrylate (MMA)-based acrylic resins (eight shades), and nine composite luting materials were evaluated. Radiographs of the specimens were taken together with tooth slices and aluminum step wedges. The density of the specimens was determined with a densitometer and was expressed in terms of the equivalent thickness of aluminum per 2.0-mm unit thickness of specimen. The radiopacity values for human enamel and dentin were 4.3 and 2.3 mm Al/2.0 mm specimen, respectively. The values for materials ranged from 5.1 to 12.9 for conventional luting materials, from 3.4 to 6.3 for RMGIs, from less than 0.5 to 7.3 for MMA resins, and from 2.3 to 9.9 for the composite luting materials. A zinc phosphate cement showed the highest value (12.9), whereas five shades of MMA resin resulted in the lowest value (less than 0.5). Two RMGIs and three composite luting materials exhibited radiopacity values between those of enamel (4.3) and dentin (2.3). It can be concluded that the radiopacity value of luting materials varies considerably, and that care must be taken when selecting luting materials, considering the material composition of restorations.

  17. The Effect of Al2O3 Addition on the Thermal Diffusivity of Heat Activated Acrylic Resin.

    PubMed

    Atla, Jyothi; Manne, Prakash; Gopinadh, A; Sampath, Anche; Muvva, Suresh Babu; Kishore, Krishna; Sandeep, Chiramana; Chittamsetty, Harika

    2013-08-01

    This study aimed at investigating the effect of adding 5% to 20% by weight aluminium oxide powder (Al2O3) on thermal diffusivity of heat-polymerized acrylic resin. Twenty five cylindrical test specimens with an embedded thermocouple were used to determine thermal diffusivity over a physiologic temperature range (0 to 70°C). The specimens were divided into five groups (5 specimens/group) which were coded A to E. Group A was the control group (unmodified acrylic resin specimens). The specimens of the remaining four groups were reinforced with 5%, 10%, 15%, and 20% Al2O3 by weight. RESULTS were analysed by using one-way analysis of variance (ANOVA). Test specimens which belonged to Group E showed the highest mean thermal diffusivity value of 10.7mm(2)/sec, followed by D (9.09mm(2)/sec), C (8.49mm(2)/sec), B(8.28mm(2)/sec) and A(6.48mm(2)/sec) groups respectively. Thermal diffusivities of the reinforced acrylic resins were found to be significantly higher than that of the unmodified acrylic resin. Thermal diffusivity was found to increase in proportion to the weight percentage of alumina filler. Al2O3 fillers have potential to provide increased thermal diffusivity. Increasing the heat transfer characteristics of the acrylic resin base material could lead to more patient satisfaction.

  18. Bonding efficacy of new self-etching, self-adhesive dual-curing resin cements to dental enamel.

    PubMed

    Benetti, Paula; Fernandes, Virgílio Vilas; Torres, Carlos Rocha; Pagani, Clovis

    2011-06-01

    This study evaluated the efficacy of the union between two new self-etching self-adhesive resin cements and enamel using the microtensile bond strength test. Buccal enamel of 80 bovine teeth was submitted to finishing and polishing with metallographic paper to a refinement of #600, in order to obtain a 5-mm2 flat area. Blocks (2 x 4 x 4 mm) of laboratory composite resin were cemented to enamel according to different protocols: (1) untreated enamel + RelyX Unicem cement (RX group); (2) untreated enamel + Bifix SE cement (BF group); (3) enamel acid etching and application of resin adhesive Single Bond + RelyX Unicem (RXA group); (4) enamel acid etching and application of resin adhesive Solobond M + Bifix SE (BFA group). After 7 days of storage in distillated water at 37°C, the blocks were sectioned for obtaining microbar specimens with an adhesive area of 1 mm2 (n = 120). Specimens were submitted to the microtensile bond strength test at a crosshead speed of 0.5 mm/min. The results (in MPa) were analyzed statistically by ANOVA and Tukey's test. Enamel pre-treatment with phosphoric acid and resin adhesive (27.9 and 30.3 for RXA and BFA groups) significantly improved (p ≤ 0.05) the adhesion of both cements to enamel compared to the union achieved with as-polished enamel (9.9 and 6.0 for RX and BF). Enamel pre-treatment with acid etching and the application of resin adhesive significantly improved the bond efficacy of both luting agents compared to the union achieved with as-polished enamel.

  19. Effect of autoclave postpolymerization treatments on the fracture toughness of autopolymerizing dental acrylic resins.

    PubMed

    Durkan, Rukiye; Gürbüz, Ayhan; Yilmaz, Burak; Özel, M Birol; Bağış, Bora

    2012-06-26

    Microwave and water bath postpolymerization have been suggested as methods to improve the mechanical properties of heat and autopolymerizing acrylic resins. However, the effects of autoclave heating on the fracture properties of autopolymerizing acrylic resins have not been investigated. The aim of this study was to assess the effectiveness of various autoclave postpolymerization methods on the fracture properties of 3 different autopolymerizing acrylic resins. Forty-two specimens of 3 different autopolymerizing acrylic resins (Orthocryl, Paladent RR and Futurajet) were fabricated (40x8x4mm), and each group was further divided into 6 subgroups (n=7). Control group specimens remained as processed (Group 1). The first test group was postpolymerized in a cassette autoclave at 135°C for 6 minutes and the other groups were postpolymerized in a conventional autoclave at 130°C using different time settings (5, 10, 20 or 30 minutes). Fracture toughness was then measured with a three-point bending test. Data were analyzed by ANOVA followed by the Duncan test (α=0.05). The fracture toughness of Orthocryl and Paladent-RR acrylic resins significantly increased following conventional autoclave postpolymerization at 130°C for 10 minutes (P<.05). However, the fracture toughness of autoclave postpolymerized Futurajet was not significantly different than its control specimens (P<.05). The fracture toughness of Futurajet was significantly less than Paladent RR and Orthocryl specimens when autoclaved at 130°C for 10 minutes. Within the limitations of this study, it can be suggested that autoclave postpolymerization is an effective method for increasing the fracture toughness of tested autoploymerized acrylic resins.

  20. Synthesis and characterization of novel halloysite-incorporated adhesive resins.

    PubMed

    Feitosa, Sabrina A; Münchow, Eliseu A; Al-Zain, Afnan O; Kamocki, Krzysztof; Platt, Jeffrey A; Bottino, Marco C

    2015-11-01

    To investigate the effects of Halloysite® aluminosilicate clay nanotubes (HNTs) addition on selected physical, mechanical, and biological properties of experimental adhesive resins. Experimental dentin adhesive resins were prepared by mixing Bis-GMA, TEGDMA, HEMA (50/25/25wt.%), and photo-initiators. As-received HNTs were then incorporated into the resin mixture at distinct concentrations: 0 (HNT-free, control), 1, 2.5, 5, 7.5, 10, and 20wt.%. The degree of conversion (DC), radiopacity (RP), Knoop hardness (KHN), flexural strength (FS), and cytotoxicity analyses were carried out for each adhesive formulation. The adhesive resin of Adper Scotchbond Multi-Purpose (SBMP) was used as the commercially available reference for both the RP and cytotoxicity tests. Data were statistically analyzed using One-Way ANOVA and Tukey's test (p≤0.05). All adhesives exhibited similar DC (p=0.1931). The RP of adhesives was improved with the addition of up to 5wt.% of HNTs (p<0.001). Adhesives containing 5-10wt.% of HNTs led to greater KHN when compared to the control (p<0.001). The FS was reduced only when 20wt.% of HNTs was added (p≤0.001). None of the prepared adhesives was cytotoxic. The incorporation of up to 10wt.% of HNTs into the adhesive resins did not jeopardize the tested physical and biological properties. When using HNTs as carriers of drugs/bioactive compounds, the amount of the former added into adhesive resin materials should not exceed 10wt.%; otherwise, a significant reduction in physicomechanical properties may be expected. Copyright © 2015 Elsevier Ltd. All rights reserved.

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