Sample records for mm borate ph

  1. Determination of monosaccharides derivatized with 2-aminobenzoic Acid by capillary electrophoresis.

    PubMed

    Abo, Mitsuru; He, Li-Ping; Sato, Kae; Okubo, Akira

    2013-01-01

    Reducing monosaccharides were derivatized with 2-aminobenzoic acid (2-AA) through reductive amination using sodium cyanoborohydride as a reductant, and the derivatives were separated by capillary zone electrophoresis with UV detection using 50 mM sodium phosphate (pH 5.5) or 150 mM sodium borate-50 mM sodium phosphate (pH 7.0) running buffer. The derivatives of monosaccharides, which are major components of various carbohydrate materials, were completely separated within 25 min.

  2. Competitive immunoassay of phenobarbital by microchip electrophoresis with laser induced fluorescence detection.

    PubMed

    Huang, Yong; Zhao, Shulin; Shi, Ming; Liu, Jinwen; Liang, Hong

    2011-05-23

    A microchip electrophoresis method with laser induced fluorescence detection was developed for the immunoassay of phenobarbital. The detection was based on the competitive immunoreaction between analyte phenobarbital and fluorescein isothiocyanate (FITC) labeled phenobarbital with a limited amount of antibody. The assay was developed by varying the borate concentration, buffer pH, separation voltage, and incubation time. A running buffer system containing 35 mM borate and 15 mM sodium dodecyl sulfate (pH 9.5), and 2800 V separation voltage provided analysis conditions for a high-resolution, sensitive, and repeatable assay of phenobarbital. Free FITC-labeled phenobarbital and immunocomplex were separated within 30s. The calibration curve for phenobarbital had a detection limit of 3.4 nM and a range of 8.6-860.0 nM. The assay could be used to determine the phenobarbital plasma concentration in clinical plasma sample. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Ternary borate-nucleoside complex stabilization by Ribonuclease A demonstrates phosphate mimicry

    PubMed Central

    Gabel, Scott A.; London, Robert E.

    2010-01-01

    Phosphate esters play a central role in cellular energetics, biochemical activation, signal transduction and conformational switching. The structural homology of the borate anion with phosphate, combined with its ability to spontaneously esterify hydroxyl groups, suggested that phosphate-ester recognition sites on proteins might exhibit significant affinity for non-enzymatically formed borate esters. 11B NMR studies and activity measurements on ribonuclease A in the presence of borate and several cytidine analogs demonstrate the formation of a stable ternary RNase A•3′-deoxycytidine-2′-borate ternary complex that mimics the complex formed between RNase A and a 2′-cytidine monophosphate (2′-CMP) inhibitor. Alternatively, no slowly exchanging borate resonance is observed for a ternary RNase A, borate, 2′-deoxycytidine mixture, demonstrating the critical importance of the 2′-hydroxyl group for complex formation. Titration of the ternary complex with 2′-CMP shows that it can displace the bound borate ester with a binding constant that is close to the reported inhibition constant of RNase A by 2′CMP. RNase A binding of a cyclic cytidine-2′,3′-borate ester, which is a structural homolog of the cytidine-2′,3′-cyclic phosphate substrate, could also be demonstrated. The apparent dissociation constant for the cytidine-2′,3′-borate•RNase A complex is 0.8 mM, which compares with a Michaelis constant of 11 mM for cCMP at pH 7, indicating considerably stronger binding. However, the value is 1000-fold larger than the reported dissociation constant of the RNase A complex with uridine-vanadate. These results are consistent with recent reports suggesting that in situ formation of borate esters that mimic the corresponding phosphate esters support enzyme catalysis. PMID:17957392

  4. The Regulation of Endogenous Glutamate and GABA Release from In Vitro Preparations of Rat Striatum

    DTIC Science & Technology

    1997-09-19

    polyethylenimine (PEl) in 50 mM sodium borate pH 7.4 overnight. then washed with PBS pH 7.4 twice before 2 m1 of NS-media were added to each well...Celsius in 95% oxygen and 5% CO2 . 2. Fetal striatum dissection and neuron culture preparation Female Sprague-Dawley rats. 18-day pregnant. under 2.5

  5. Separation and determination of epinephrine and dopamine in traditional Chinese medicines by micellar electrokinetic capillary chromatography with laser induced fluorescence detection.

    PubMed

    Dong, Yuming; Chen, Hongli; Chen, Yonglei; Hui, Yang; Chen, Xingguo; Hu, Zhide

    2006-08-01

    A micellar electrokinetic capillary chromatography method with laser-induced fluorescence detection was developed for the analysis of epinephrine and dopamine after derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole. The optimum derivatization conditions were: 30 mM sodium borate (pH adjusted to 8.0 with 1.0 M HCl), reaction time 30 min at 60 degrees C. Baseline separation was achieved within 14 min with a running buffer composed of 10 mM sodium borate + 25 mM sodium dodecyl sulfate (pH adjusted to 9.5 with 0.1 M NaOH) and an applied voltage of 15 kV. Good linearity relationships (correlation coefficients: 0.9991 for epinephrine and 0.9985 for dopamine) between peak areas and concentrations of the analytes were obtained. The detection limits and quantification limits for epinephrine and dopamine were 0.0038 mg/L and 0.013 mg/L, and 0.065 mg/L and 0.020 mg/L, respectively. The method was applied to the analysis of the two compounds in two Chinese medicines with recoveries in the range of 92.6-108.7%.

  6. Direct enantioseparation of catechin and epicatechin in tea drinks by 6-O-alpha-D-glucosyl-beta-cyclodextrin-modified micellar electrokinetic chromatography.

    PubMed

    Kodama, Shuji; Yamamoto, Atsushi; Matsunaga, Akinobu; Yanai, Hiroko

    2004-08-01

    Cyclodextrin-modified micellar electrokinetic chromatography was applied to the enantioseparation of catechin and epicatechin using 6-O-alpha-D-glucosyl-beta-cyclodextrin together with sodium dodecyl sulfate and borate-phosphate buffer. Factors affecting chiral resolution and migration time of catechin and epicatechin were studied. The optimum running conditions were found to be 200 mM borate-20 mM phosphate buffer (pH 6.4) containing 25 mM 6-O-alpha-D-glucosyl-beta-cyclodextrin and 240 mM sodium dodecyl sulfate with an effective voltage of +25 kV at 20 degrees C using direct detection at 210 nm. Under these conditions, the resolution (Rs) of racemic catechin and epicatechin were 4.15 and 1.92, respectively. With this system, catechin and epicatechin enantiomers along with other four catechins ((-)-catechin gallate, (-)-epicatechin gallate, (-)-epigallocatechin, (-)-epigallocatechin gallate) and caffeine in tea samples were analyzed successfully. The difference of migration time between catechin and epicatechin is discussed.

  7. Separation of 2-aminobenzoic acid-derivatized glycosaminoglycans and asparagine-linked glycans by capillary electrophoresis.

    PubMed

    Sato, Kae; Sato, Kiichi; Okubo, Akira; Yamazaki, Sunao

    2005-01-01

    A capillary electrophoresis method was developed for the analysis of oligosaccharides combined with derivatization with 2-aminobenzoic acid. Glycosaminoglycan delta-disaccharides were effectively resolved on a fused-silica capillary tube using 150 mM borate, pH 8.5, as a running electrolyte solution. This analytical method was applied to the identification of glycosaminoglycan in combination with enzymatic digestion. The separation of N-glycans or glucose-oligomers was performed with a phosphate buffer containing polyethylene glycol or borate as an electrolyte solution. This method is expected to be useful in the determination of oligosaccharide structures in a glycoprotein.

  8. Capillary electrophoresis method with UV-detection for analysis of free amino acids concentrations in food.

    PubMed

    Omar, Mei Musa Ali; Elbashir, Abdalla Ahmed; Schmitz, Oliver J

    2017-01-01

    Simple and inexpensive capillary electrophoresis with UV-detection method (CE-UV) was optimized and validated for determination of six amino acids namely (alanine, asparagine, glutamine, proline, serine and valine) for Sudanese food. Amino acids in the samples were derivatized with 4-chloro-7-nitro-2,1,3-benzoxadiazole (NBD-Cl) prior to CE-UV analysis. Labeling reaction conditions (100mM borate buffer at pH 8.5, labeling reaction time 60min, temperature 70°C and NBD-Cl concentration 40mM) were systematically investigated. The optimal conditions for the separation were 100mM borate buffer at pH 9.7 and detected at 475nm. The method was validated in terms of linearity, limit of detection (LOD), limit of quantification (LOQ), precision (repeatability) (RSD%) and accuracy (recovery). Good linearity was achieved for all amino acids (r(2)>0.9981) in the concentration range of 2.5-40mg/L. The LODs in the range of 0.32-0.56mg/L were obtained. Recoveries of amino acids ranging from 85% to 108%, (n=3) were obtained. The validated method was successfully applied for the determination of amino acids for Sudanese food samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Development of Natural Anthocyanin Dye-Doped Silica Nanoparticles for pH and Borate-Sensing Applications

    NASA Astrophysics Data System (ADS)

    Ha, Chu T.; Lien, Nghiem T. Ha; Anh, Nguyen D.; Lam, Nguyen L.

    2017-12-01

    Anthocyanin belongs to a large group of phenolic compounds called flavonoids. It is found primarily in fruits, flowers, roots and other parts of higher plants. Within the black carrot, it has been found that the cyanidin component 1,2 diol was the major anthocyanine. Since the terminal thiols potentially display chemical interactions with borate additives, anthocyanin from the black carrot can act as a sensing material for detecting borate in the environment. As a natural dye, anthocyanin responds to pH change of the medium. Here, we present an application of black carrot dyes for pH sensing and for the detection of borate additives within meats. The dyes were encapsulated within a mesoporous silica (SiO2) matrix in order to prevent the sensing materials from dissolution into the aqueous medium. The encapsulation was done in situ during preparation of silica nanoparticles (size from 100 nm to 500 nm) following an advanced Stöber method. These anthocyanin-encapsulated silica nanoparticles show a clear color change from green in an aqueous solution free of borate to GRAY-red in the presence of borate additive and red (pH 2) to green (pH 10).

  10. Analysis of carbonaceous biomarkers with the Mars Organic Analyzer microchip capillary electrophoresis system: aldehydes and ketones.

    PubMed

    Stockton, Amanda M; Tjin, Caroline Chandra; Huang, Grace L; Benhabib, Merwan; Chiesl, Thomas N; Mathies, Richard A

    2010-11-01

    A microchip CE method is developed for the analysis of two oxidized forms of carbon, aldehydes and ketones, with the Mars Organic Analyzer (MOA). Fluorescent derivitization is achieved in ∼ 15 min by hydrazone formation with Cascade Blue hydrazide in 30 mM borate pH 5-6. The microchip CE separation and analysis method is optimized via separation in 30 mM borate buffer, pH 9.5, at 20°C. A carbonyl standard consisting of ten aldehydes and ketones found in extraterrestrial matter is successfully separated; the resulting LOD depends on the reactivity of the compound and range from 70 pM for formaldehyde to 2 μM for benzophenone. To explore the utility of this method for analyzing complex samples, analyses of several fermented beverages are conducted, identifying ten aldehydes and ketones ranging from 30 nM to 5 mM. A Martian regolith simulant sample, consisting of a basalt matrix spiked with soluble ions and acetone, is designed and analyzed, but acetone is found to have a limited detectable lifetime under simulant Martian conditions. This work establishes the capability of the MOA for studying aldehydes and ketones, a critical class of oxidized organic molecules of interest in planetary and in terrestrial environmental and health studies. Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Boric Acid Corrosion of Concrete Rebar

    NASA Astrophysics Data System (ADS)

    Pabalan, R. T.; Yang, L.; Chiang, K.–T.

    2013-07-01

    Borated water leakage through spent fuel pools (SFPs) at pressurized water reactors is a concern because it could cause corrosion of reinforcement steel in the concrete structure and compromise the integrity of the structure. Because corrosion rate of carbon steel in concrete in the presence of boric acid is lacking in published literature and available data are equivocal on the effect of boric acid on rebar corrosion, corrosion rate measurements were conducted in this study using several test methods. Rebar corrosion rates were measured in (i) borated water flowing in a simulated concrete crack, (ii) borated water flowing over a concrete surface, (iii) borated water that has reacted with concrete, and (iv) 2,400 ppm boric acid solutions with pH adjusted to a range of 6.0 to 7.7. The corrosion rates were measured using coupled multielectrode array sensor (CMAS) and linear polarization resistance (LPR) probes, both made using carbon steel. The results indicate that rebar corrosion rates are low (~1 μm/yr or less)when the solution pH is ~7.1 or higher. Below pH ~7.1, the corrosion rate increases with decreasing pH and can reach ~100 μm/yr in solutions with pH less than ~6.7. The threshold pH for carbon steel corrosion in borated solution is between 6.8 and 7.3.

  12. Solar water oxidation using nickel-borate coupled BiVO4 photoelectrodes.

    PubMed

    Choi, Sung Kyu; Choi, Wonyong; Park, Hyunwoong

    2013-05-07

    A naturally abundant nickel-borate (Ni-Bi) complex is demonstrated to successfully catalyze the photoelectrochemical (PEC) water oxidation of BiVO4 electrodes at 1.23 VRHE with nearly 100% faradaic efficiency for oxygen evolution. Ni-Bi is electrodeposited (ED) and photodeposited (PD) for varying times on BiVO4 electrodes in the 0.1 M borate electrolyte with 1 mM Ni(2+) at pH 9.2. Surprisingly, optimally deposited Ni-Bi films (ED-10 s and PD-30 min) display the same layer thickness of ca. 40 nm. Both Ni-Bi films enhance the photocurrent generation of BiVO4 at 1.23 VRHE by a factor of 3-4 under AM 1.5-light irradiation (100 mW cm(-2)) along with ca. 250% increase in the incident and absorbed photon-to-current efficiencies. Impedance analysis further reveals that the charge transfer resistance at BiVO4 is markedly decreased by Ni-Bi deposits. The primary role of Ni-Bi has been suggested to be a hole-conductor making photogenerated electrons more mobile and catalyzing a four-hole transfer to water through cyclic changes between the lower and higher Ni oxidation states. However, thick Ni-Bi films (>~40 nm) significantly reduce the PEC performance of BiVO4 due to the kinetic bottleneck and charge recombination. Under identical PEC conditions (0.1 M, pH 9.2), the borate electrolyte (good proton acceptor) is found to be better than nitrate (poor proton acceptor), indicative of a proton-coupled electron transfer pathway in PEC water oxidation.

  13. Proline-coated column for the capillary electrochromatographic separation of amino acids by in-column derivatization.

    PubMed

    Lin, Chun-Chi; Liu, Chuen-Ying

    2004-10-01

    With 3-trimethoxysilylpropyl chloride as the spacer, a proline-coated capillary column was prepared for the capillary electrochromatographic (CEC) separation of amino acids by in-column derivatization. Nine standard mixtures, including aspartic acid, glutamic acid, valine, phenylalanine, alanine, isoleucine, leucine, tyrosine, and tryptophan, were injected. o-Phthalaldehyde (OPA), OPA/2-mercaptoethanol (2-ME) and OPA/N-acetylcysteine (NAC) in borate buffer were tested as the derivatizing agent. Among them, OPA (50 mM) in borate buffer (pH 9.5, 50 mM) gave the best performance. The formation of isoindole could be detected by UV detection. The sandwich-type injection was carried out in hydrostatic mode (10 cm) with the program R(10 s)S(10 s) R(10 s)W(10 min) with R, S, and W being the reagent, sample, and waiting times. Mesityl oxide, benzyl alcohol, and acetone showed some interaction with the column. A current monitoring method was used instead of the determination of the electroosmotic flow (EOF). The direction of EOF was from anode to cathode even under acidic condition lower than the pI value (6.31) of the bonded group due to some unreacted silanol groups. Some parameters including pH, nature, and concentration of the mobile phase and the effect of organic modifier with regard to the CEC separation were investigated. With the proline-coated column (75 (50) cm x 75 microm ID) the best separation was performed in phosphate buffer (pH 4.00, 100 mM) with an applied voltage of -15 kV. The established method was also compared with those precolumn derivatized prior to the separation with proline-coated column as well as with in-capillary derivatization and separation with a bare fused-silica column. Copyright 2004 WILEY-VCH Verlag GmbH & Co.

  14. Quality evaluation of Guan-Xin-Ning injection based on fingerprint analysis and simultaneous separation and determination of seven bioactive constituents by capillary electrophoresis.

    PubMed

    Xu, Liying; Chang, Ruimiao; Chen, Meng; Li, Lou; Huang, Yayun; Zhang, Hongfen; Chen, Anjia

    2017-12-01

    The purpose of this study was to develop a comprehensive, rapid and practical capillary electrophoresis (CE) method for quality control (QC) of Guan-Xin-Ning (GXN) injection based on fingerprint analysis and simultaneous separation and determination of seven constituents. In fingerprint analysis, a capillary zone electrophoresis (CZE) method with a running buffer of 30 mM borate solution (pH 9.3) was established. Meanwhile, ten batches of samples were used to establish the fingerprint electropherogram and 34 common peaks were obtained within 20 min. The RSD of relative migration times (RMT) and relative peak areas (RPA) were less than 5%. In order to further evaluate the quality of GXN injection, a micellar electrokinetic chromatography (MEKC) method was developed for simultaneous separation and determination of bioactive constituents. Seven components reached baseline separation with a running buffer containing 35 mM SDS and 45 mM borate solution (pH 9.3). A good linearity was obtained with correlation coefficients from 0.9906 to 0.9997. The LOD and LOQ ranged from 0.12 to 1.50 μg/mL and from 0.40 to 4.90 μg/mL, respectively. The recoveries ranged between 99.0 and 104.4%. Therefore, it was concluded that the proposed method can be used for full-scale quality analysis of GXN injection. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Thermally reversible gels in electrophoresis. I - Matrix characterization

    NASA Technical Reports Server (NTRS)

    Righetti, Pier Giorgio; Snyder, Robert S.

    1988-01-01

    Two series of thermally reversible hydrogen-bonded gels have been characterized: (5 pct) PVA-(4 pct) PEG and (5 pct) PVA-(0.04 pct) borate gels. They both have extremely low melting points (16-17 C) and could be of potential interest for recovery of proteins after preparative electrophoresis. The PVA-borate gels can be exploited in the pH range 7-11 by progressively increasing the borate content in the pH interval 8 to 7 and concomitantly decreasing the borate levels in the pH zone 8 to 11. It is hypothesized that the low melting point of these gels is due to the fact that they are sparingly and sparsely hydrogen bonded along the PVA chain: on the average, 1 OH group out of 3 or 4 OH groups in the PVA polymer should be engaged in H-bond formation.

  16. Identification and characterization of a novel L-arabinose isomerase from Anoxybacillus flavithermus useful in D-tagatose production.

    PubMed

    Li, Yanjun; Zhu, Yueming; Liu, Anjun; Sun, Yuanxia

    2011-05-01

    D-Tagatose is a highly functional rare ketohexose and many attempts have been made to convert D-galactose into the valuable D-tagatose using L-arabinose isomerase (L-AI). In this study, a thermophilic strain possessing L-AI gene was isolated from hot spring sludge and identified as Anoxybacillus flavithermus based on its physio-biochemical characterization and phylogenetic analysis of its 16s rRNA gene. Furthermore, the gene encoding L-AI from A. flavithermus (AFAI) was cloned and expressed at a high level in E. coli BL21(DE3). L-AI had a molecular weight of 55,876 Da, an optimum pH of 10.5 and temperature of 95°C. The results showed that the conversion equilibrium shifted to more D-tagatose from D-galactose by raising the reaction temperatures and adding borate. A 60% conversion of D-galactose to D-tagatose was observed at an isomerization temperature of 95°C with borate. The catalytic efficiency (k (cat) /K (m)) for D-galactose with borate was 9.47 mM(-1) min(-1), twice as much as that without borate. Our results indicate that AFAI is a novel hyperthermophilic and alkaliphilic isomerase with a higher catalytic efficiency for D-galactose, suggesting its great potential for producing D-tagatose.

  17. Tris-borate is a poor counterion for RNA: a cautionary tale for RNA folding studies

    PubMed Central

    Buchmueller, Karen L.; Weeks, Kevin M.

    2004-01-01

    Native polyacrylamide gel electrophoresis is a powerful approach for visualizing RNA folding states and folding intermediates. Tris-borate has a high-buffering capacity and is therefore widely used in electrophoresis-based investigations of RNA structure and folding. However, the effectiveness of Tris-borate as a counterion for RNA has not been systematically investigated. In a recirculated Hepes/KCl buffer, the catalytic core of the bI5 group I intron RNA undergoes a conformational collapse characterized by a bulk transition midpoint, or Mg1/2, of ∼3 mM, consistent with extensive independent biochemical experiments. In contrast, in Tris-borate, RNA collapse has a much smaller apparent Mg1/2, equal to 0.1 mM, because in this buffer the RNA undergoes a different, large amplitude, folding transition at low Mg2+ concentrations. Analysis of structural neighbors using a short-lived, RNA-tethered, photocrosslinker indicates that the global RNA structure eventually converges in the two buffer systems, as the divalent ion concentration approaches ∼1 mM Mg2+. The weak capacity of Tris-borate to stabilize RNA folding may reflect relatively unfavorable interactions between the bulky Tris-borate ion and RNA or partial coordination of RNA functional groups by borate. Under some conditions, Tris-borate is a poor counterion for RNA and its use merits careful evaluation in RNA folding studies. PMID:15601995

  18. Screening and confirmatory methods for the analysis of macrocyclic lactone mycotoxins by CE with amperometric detection.

    PubMed

    Arribas, Alberto Sánchez; Bermejo, Esperanza; Zapardiel, Antonio; Téllez, Helena; Rodríguez-Flores, Juana; Zougagh, Mohammed; Ríos, Angel; Chicharro, Manuel

    2009-02-01

    A simple analytical scheme for the screening and quantification of zearalenone and its metabolites, alpha-zearalenol and beta-zearalenol, is reported. Extracts from maize flour samples were collected by supercritical fluid extraction and afterwards, they were analyzed by CE with amperometric detection. This scheme allowed a rapid and reliable identification of contaminated flour samples according to the reference value established for zearalenone by directive 2005/38/EC (200 microg/kg). The sample screening method was carried out by CZE using 25 mM borate separation buffer at pH 9.2 and 25.0 kV as separation voltage, monitoring the amperometric signal at +700 mV with a carbon paste electrode. In this way, total amount of mycotoxins was determined and samples were processed in 4 min with a detection limit of 12 microg/L, enough to discriminate between positive (more than 200 microg/L total mycotoxins) and negative samples (less than 200 microg/L total mycotoxins). Positive samples were then subjected to CZE separation and quantification of each analyte was done with 50 mM borate running buffer modified with 30% methanol at pH 9.7 and 17.5 kV as separation voltage. Under these conditions, separation was achieved in 15 min with detection limits from 20 to 35 microg/L for each analyte.

  19. Analysis of different beta-lactams antibiotics in pharmaceutical preparations using micellar electrokinetic capillary chromatography.

    PubMed

    Pérez, M I Bailón; Rodríguez, L Cuadros; Cruces-Blanco, C

    2007-01-17

    The potential of micellar electrokinetic capillary chromatography (MEKC) for analyzing nine beta-lactams antibiotics (cloxacillin, dicloxacillin, oxacillin, penicillin G, penicillin V, ampicillin, nafcillin, piperacillin, amoxicillin) in different pharmaceutical preparations, have been demonstrated. An experimental design strategy has been applied to optimize the main variables: pH and buffer concentration, concentration of the micellar medium, separation voltage and capillary temperature. Borate buffer (26mM) at pH 8.5 containing 100mM sodium dodecyl sulphate (SDS) was used as the background electrolyte. The method was validated. Linearity, limit of detection and quantitation and precision were established for each compound. The analysis of some of the beta-lactams in Orbenin capsules, Britapen tables and in Veterin-Micipen injectable, all used in human and veterinary medicine, have demonstrated the applicability of these technique for quality control in the pharmaceutical industry.

  20. Analysis of carbonaceous biomarkers with the Mars Organic Analyzer microchip capillary electrophoresis system: carboxylic acids.

    PubMed

    Stockton, Amanda M; Tjin, Caroline Chandra; Chiesl, Thomas N; Mathies, Richard A

    2011-01-01

    The oxidizing surface chemistry on Mars argues that any comprehensive search for organic compounds indicative of life requires methods to analyze higher oxidation states of carbon with very low limits of detection. To address this goal, microchip capillary electrophoresis (μCE) methods were developed for analysis of carboxylic acids with the Mars Organic Analyzer (MOA). Fluorescent derivatization was achieved by activation with the water soluble 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) followed by reaction with Cascade Blue hydrazide in 30 mM borate, pH 3. A standard containing 12 carboxylic acids found in terrestrial life was successfully labeled and separated in 30 mM borate at pH 9.5, 20 °C by using the MOA CE system. Limits of detection were 5-10 nM for aliphatic monoacids, 20 nM for malic acid (diacid), and 230 nM for citric acid (triacid). Polyacid benzene derivatives containing 2, 3, 4, and 6 carboxyl groups were also analyzed. In particular, mellitic acid was successfully labeled and analyzed with a limit of detection of 300 nM (5 ppb). Analyses of carboxylic acids sampled from a lava tube cave and a hydrothermal area demonstrated the versatility and robustness of our method. This work establishes that the MOA can be used for sensitive analyses of a wide range of carboxylic acids in the search for extraterrestrial organic molecules. © Mary Ann Liebert, Inc.

  1. Nitrate reduction by zerovalent iron: effects of formate, oxalate, citrate, chloride, sulfate, borate, and phosphate.

    PubMed

    Su, Chunming; Puls, Robert W

    2004-05-01

    Recent studies have shown that zerovalent iron (Fe0) may potentially be used as a chemical medium in permeable reactive barriers (PRBs) for groundwater nitrate remediation; however, the effects of commonly found organic and inorganic ligands in soil and sediments on nitrate reduction by Fe0 have not been well understood. A 25.0 mL nitrate solution of 20.0 mg of N L(-1) (1.43 mM nitrate) was reacted with 1.00 g of Peerless Fe0 at 200 rpm on a rotational shaker at 23 degrees C for up to 120 h in the presence of each of the organic acids (3.0 mM formic, 1.5 mM oxalic, and 1.0 mM citric acids) and inorganic acids (3.0 mM HCl, 1.5 mM H2SO4, 3.0 mM H3BO3, and 1.5 mM H3PO4). These acids provided an initial dissociable H+ concentration of 3.0 mM available for nitrate reduction reactions under conditions of final pH < 9.3. Nitrate reduction rates (pseudo-first-order) increased in the order: H3PO4 < citric acid < H3BO3 < oxalic acid < H2SO4 < formic acid < HCl, ranging from 0.00278 to 0.0913 h(-1), corresponding to surface area normalized rates ranging from 0.126 to 4.15 h(-1) m(-2) mL. Correlation analysis showed a negative linear relationship between the nitrate reduction rates for the ligands and the conditional stability constants for the soluble complexes of the ligands with Fe2+ (R2 = 0.701) or Fe3+ (R2 = 0.918) ions. This sequence of reactivity corresponds also to surface adsorption and complexation of the three organic ligands to iron oxides, which increase in the order formate < oxalate < citrate. The results are also consistent with the sequence of strength of surface complexation of the inorganic ligands to iron oxides, which increases in the order: chloride < sulfate < borate < phosphate. The blockage of reactive sites on the surface of Fe0 and its corrosion products by specific adsorption of the inner-sphere complex forming ligands (oxalate, citrate, sulfate, borate, and phosphate) may be responsible for the decreased nitrate reduction by Fe0 relative to the chloride system.

  2. The Role of Newly Discovered Exotoxin (S Toxin) in Pseudomonas aeruginosa Infections

    DTIC Science & Technology

    1979-08-01

    sodium or potassium phosphate 6.0-8.0 N-2-hydroxyethylpiperazine-N’-2-ethanesulfonic acid (HEPES) 6.5-8.5 tris 7.0-9.5 sodium borate 7.5-9.5 sodium...was found to be variable with respect to whether sodium or potassium phosphate buffer was used. With sodium phosphate, virtually all the enzyme...activity bound was eluted between 20-100.2M phosphate at pH 6.8. With the potassium salt, elution occurs at 400-?00mM KP04. Since very little protein was

  3. Mechanism for converting Al2O3-containing borate glass to hydroxyapatite in aqueous phosphate solution.

    PubMed

    Zhao, Di; Huang, Wenhai; Rahaman, Mohamed N; Day, Delbert E; Wang, Deping

    2009-05-01

    The effect of replacing varying amounts (0-2.5 mol.%) of B2O3 with Al2O3 in a borate glass on (1) the conversion of the glass to HA in an aqueous phosphate solution and (2) the compressive strength of the as-formed HA product was investigated. Samples of each glass (10 x 10 x 8 mm) were placed in 0.25 M K2HPO4 solution at 60 degrees C, and the conversion kinetics to HA were determined from the weight loss of the glass and the pH of the solution. The structure and composition of the solid reaction products were characterized using X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. While the conversion rate of the glass to HA decreased considerably with increasing Al2O3 content, the microstructure of the HA product became denser and the compressive strength of the HA product increased. The addition of SiO2 to the Al2O3-containing borate glass reversed the deterioration of the conversion rate, and produced a further improvement in the strength of the HA product. The compressive strength of the HA formed from the borate glass with 2.5 mol.% Al2O3 and 5 mol.% SiO2 was 11.1 +/- 0.2 MPa, which is equal to the highest strengths reported for trabecular bone. The results indicated that simultaneous additions of Al2O3 and SiO2 could be used to control the bioactivity of the borate glass and to enhance the mechanical strength of the HA product. Furthermore, the HA product formed from the glass containing both SiO2 and Al2O3 could be applied to bone repair.

  4. Enantioseparations of amino acids by capillary array electrophoresis with 532 nm laser induced fluorescence detection.

    PubMed

    Liu, Kaiying; Wang, Li

    2013-06-21

    Capillary array electrophoresis (CAE) is a promising technique for multiple enantiomeric separations. Carboxytetramethylrhodamine succinimidyl ester (TAMRA SE), a rhodamine-core fluorescent probe, has rarely been applied as an original precolumn derivatization reagent for chiral amino acid (AA) analysis so far. For these purposes, high-throughput enantiomeric separations of 12 TAMRA SE-AAs by a home-made 532 nm CAE-LIF scanner are presented. The effect of cyclodextrins (CDs) and a variety of organic modifiers was quickly investigated. Baseline separations were achieved in 100 mM Tris-borate buffer (pH 10.0) containing 2 mM β-CD and 10 mM hexamethylenediamine (HDA). Multiple determination of the enantiomeric excess (ee) in non-racemic mixtures of alanine is successfully presented. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Report of the key comparison APMP.QM-K19. APMP comparison on pH measurement of borate buffer

    NASA Astrophysics Data System (ADS)

    Hioki, Akiharu; Asakai, Toshiaki; Maksimov, Igor; Suzuki, Toshihiro; Miura, Tsutomu; Obromsook, Krairerk; Tangpaisarnkul, Nongluck; Rodruangthum, Patumporn; Wong, Siu-Kay; Lam, Wai-Hing; Zakaria, Osman; Anuar Mohd. Amin, Khirul; Thanh, Ngo Huy; Máriássy, Michal; Vyskocil, Leos; Hankova, Zuzana; Fisicaro, Paola; Stoica, Daniela; Singh, Nahar; Soni, Daya; Ticona Canaza, Galia; Kutovoy, Viatcheslav; Barbieri Gonzaga, Fabiano; Dias, Júlio Cesar; Vospelova, Alena; Bakovets, Nickolay; Zhanasbayeva, Bibinur

    2015-01-01

    The APMP.QM-K19 was organised by TCQM of APMP to test the abilities of the national metrology institutes in the APMP region to measure a pH value of a borate buffer. This APMP comparison on pH measurement was proposed by the National Metrology Institute of Japan (NMIJ) and the National Institute of Metrology (Thailand) (NIMT) at the APMP-TCQM meeting held 26-27 November 2012. After approval by TCQM, the comparison has been conducted by NMIJ and NIMT. The comparison is a key comparison following CCQM-K19 and CCQM-K19.1. The comparison material was a borate buffer of pH around 9.2 and the measurement temperatures were 15 °C, 25 °C and 37 °C. This is the second APMP key comparison on pH measurement and the fourth APMP comparison on pH measurement following APMP.QM-P06 (two phosphate buffers) in 2004, APMP.QM-P09 (a phthalate buffer) in 2006 and APMP.QM-K9/APMP.QM-P16 (a phosphate buffer) in 2010-2011. The results can be used further by any participant to support its CMC claim at least for a borate buffer. That claim will concern the pH method employed by the participant during this comparison and will cover the used temperature(s) or the full temperature range between 15°C and 37 °C for the participant which measured pH values at the three temperatures. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

  6. Determination of antibacterial flomoxef in serum by capillary electrophoresis.

    PubMed

    Kitahashi, Toshihiro; Furuta, Itaru

    2003-04-01

    A determination method of flomoxef (FMOX) concentration in serum by capillary electrophoresis is developed. Serum samples are extracted with acetonitrile. After pretreatment, they are separated in a fused-silica capillary tube with a 25 mM borate buffer (pH 10.0) as a running buffer that contains 50mM sodium dodecyl sulfate. The FMOX and acetaminophen (internal standard) are detected by UV absorbance at 200 nm. Linearity (0-200 mg/L) is good, and the minimum limit of detection is 1.0 mg/L (S/N = 3). The relative standard deviations of intra- and interassay variability are 1.60-4.78% and 2.10-3.31%, respectively, and the recovery rate is 84-98%. This method can be used for determination of FMOX concentration in serum.

  7. Mineralogy and sedimentology of the Miocene Göcenoluk borate deposit, Kırka district, western Anatolia, Turkey

    NASA Astrophysics Data System (ADS)

    García-Veigas, Javier; Helvacı, Cahit

    2013-05-01

    The Miocene boratiferous district of Kırka, in western Anatolia (Turkey), is the most important Na-borate (borax) resource in the world. Two separate deposits in the Kırka district are located near the villages of Sarıkaya and Göcenoluk (Eskişehir Province). Borax is intensively exploited in open-pit mines in the Sarıkaya deposit while only small quarries of colemanite are known in the Göcenoluk deposit. Recent exploratory drilling in the Göcenoluk area intersected a thick succession of dolostones, tuffs and three borate-bearing units (Lower, Intermediate and Upper Borate Units). In them, the most abundant borate mineral is ulexite (Ca-Na-borate) passing at depth to probertite. Borax (Na-borate) is only present in the Intermediate Borate Unit. Minor amounts of colemanite (Ca-borate) and hydroboracite (Ca-Mg-borate) occur at the base, and/or top, of each mineralized unit. Pyroclastic layers within the borate units show intense alteration by alkaline, boron-bearing waters and formation of diagenetic clay minerals (smectites), zeolites (analcime) and borosilicates (searlesite). The Göcenoluk succession is interpreted as a shallow, ephemeral, alkaline lake deposit in which carbonates formed as stromatolites and travertines. Borate precipitation in the Göcenoluk area took place interstitially within muddy and carbonate sediments in a lateral progression from marginal Ca-borates towards Na-Ca-borates and rarely to Na-borates in the center of the lake. Authigenic silicate mineral distribution shows parallel changes toward the center of the lake that reflect increasing pH gradient.

  8. Determination of residual cell culture media components by MEKC.

    PubMed

    Zhang, Junge; Chakraborty, Utpal; Foley, Joe P

    2009-11-01

    Folic acid, hypoxanthine, mycophenolic acid, nicotinic acid, riboflavin, and xanthine are widely used as cell culture media components in monoclonal antibody manufacturing. These components are subsequently removed during the downstream purification processes. This article describes a single MEKC method that can simultaneously determine all the listed compounds with acceptable LOD and LOQ. All the analytes were successfully separated by MEKC using running buffer containing 40 mM SDS, 20 mM sodium phosphate, and 20 mM sodium borate at pH 9.0. The MEKC method was compared to the corresponding CZE method using the same running buffer containing no SDS. The effect of SDS concentration on separation, the pH of the running buffer, and the detection wavelength were studied and optimal MEKC conditions were established. Good linearity was obtained with correlation coefficients of more than 0.99 for all analytes. Specificity, accuracy, and precision were also evaluated. The recovery was in the range of 89-112%. The precision results were in the range of 1.7-4.8%. The experimentally determined data demonstrated that the MEKC method is applicable to the determination of the six analytes in in-process samples from monoclonal antibody manufacturing processes.

  9. Separation of dietary omega-3 and omega-6 fatty acids in food by capillary electrophoresis.

    PubMed

    Soliman, Laiel C; Donkor, Kingsley K; Church, John S; Cinel, Bruno; Prema, Dipesh; Dugan, Michael E R

    2013-10-01

    A lower dietary omega-6/omega-3 (n-6/n-3) fatty acid ratio (<4) has been shown to be beneficial in preventing a number of chronic illnesses. Interest exists in developing more rapid and sensitive analytical methods for profiling fatty acid levels in foods. An aqueous CE method was developed for the simultaneous determination of 15 n-3 and n-6 relevant fatty acids. The effect of pH and concentration of buffer, type and concentration of organic modifier, and additive on the separation was investigated in order to determine the best conditions for the analysis. Baseline separations of the 15 fatty acids were achieved using 40 mM borate buffer at pH 9.50 containing 50 mM SDS, 10 mM β-cyclodextrin, and 10% acetonitrile. The developed CE method has LODs of <5 mg/L and good linearity (R(2) > 0.980) for all fatty acids studied. The proposed method was successfully applied to the determination of n-3 and n-6 fatty acids in flax seed, Udo® oils and a selection of grass-fed and grain-fed beef muscle samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Sensitive determination of phenolic acids in extra-virgin olive oil by capillary zone electrophoresis.

    PubMed

    Carrasco Pancorbo, Alegría; Cruces-Blanco, Carmen; Segura Carretero, Antonio; Fernández Gutiérrez, Alberto

    2004-11-03

    A sensitive, rapid, efficient, and reliable method for the separation and determination of phenolic acids by capillary zone electrophoresis has been carried out. A detailed method optimization was carried out to separate 14 different compounds by studying parameters such as pH, type and concentration of buffer, applied voltage, and injection time. The separation was performed within 16 min, using a 25 mM sodium borate buffer (pH 9.6) at 25 kV with 8 s of hydrodynamic injection. With this method and using a liquid-liquid extraction system, with recovery values around 95%, it has been possible to detect small quantities of phenolic acids in olive oil samples. This is apparently the first paper showing the quantification of this specific family of phenolic compounds in virgin olive oil samples.

  11. Quality control of benserazide-levodopa and carbidopa-levodopa tablets by capillary zone electrophoresis.

    PubMed

    Fanali, S; Pucci, V; Sabbioni, C; Raggi, M A

    2000-07-01

    In modern practice, the treatment of Parkinson's disease and syndrome is carried out using pharmaceutical formulations containing a combination of levodopa and a decarboxylation inhibitor (carbidopa or benserazide). Two pharmaceutical formulations were quantified by capillary zone electrophoresis using two procedures which differed only in the kind of background electrolyte used. One procedure used a 25 mM phosphate buffer, pH 2.5, while the second one used a 25 mM borate buffer, pH 8.5. The electrophoretic analysis was carried out using an uncoated fused- silica capillary, a separation voltage of 20 kV with currents typically less than 60 microA, and spectrophotometric detection at 205 nm. Calibration curves were performed for levodopa (concentration range 1-100 microg/mL), for carbidopa and benserazide (1-50 microg/mL), and the plots of the peak area versus concentration were found to be linear with a correlation coefficient better than 0.9990. Satisfactory results were obtained when commercial tablets were analyzed in terms of accuracy (98-102%), repeatability (0.6-2.0%), and intermediate precision (1.1-2.6%).

  12. Chiral separation of benzoporphyrin derivative mono- and diacids by laser induced fluorescence-capillary electrophoresis.

    PubMed

    Peng, Xuejun; Sternberg, Ethan; Dolphin, David

    2002-01-01

    A method for the separation of benzoporphyrin derivative mono- and diacid (BPDMA, BPDDA) enantiomers by laser induced fluorescence-capillary electrophoresis (LIF-CE) has been developed. By using 300 mM borate buffer, pH 9.2, 25 mM sodium cholate and 10% acetronitrile as electrolyte, +10 kV electrokinetic sampling injection of 2 s and an applied +20 kV voltage across the ends of a 37 cm capillary (30 cm to the detector, 50 microm ID), all six BPD stereoisomers were baseline-separated within 20 min. Formation constants, free electrophoretic and complexation mobilities with borate and cholate were determined based on dynamic complexation capillary electrophoresis theory. The BPD enantiomers can be quantitatively determined in the range of 10(-2)-10(-5) mg mL(-1). The correlation coefficients (r2) of the least-squares linear regression analysis of the BPD enantiomers are in the range of 0.9914-0.9997. Their limits of detection are 2.18-3.5 x 10(-3) mg mL(-1). The relative standard deviations for the separation were 2.90-4.64% (n = 10). In comparison with high-performance liquid chromatography (HPLC), CE has better resolution and efficiency. This separation method was successfully applied to the BPD enantiomers obtained from a matrix of bovine serum and from liposomally formulated material as well as from studies with rat, dog and human microsomes.

  13. Borate protection of softwood from Coptotermes acinaciformis (Isoptera: Rhinotermitidae) damage: variation in protection thresholds explained.

    PubMed

    Peters, Brenton C; Fitzgerald, Christopher J

    2006-10-01

    Laboratory and field data reported in the literature are confusing with regard to "adequate" protection thresholds for borate timber preservatives. The confusion is compounded by differences in termite species, timber species and test methodology. Laboratory data indicate a borate retention of 0.5% mass/mass (m/m) boric acid equivalent (BAE) would cause > 90% termite mortality and restrict mass loss in test specimens to < or = 5%. Field data generally suggest that borate retentions appreciably > 0.5% m/m BAE are required. We report two field experiments with varying amounts of untreated feeder material in which Coptotermes acinaciformis (Froggatt) (Isoptera: Rhinotermitidae) responses to borate-treated radiata (Monterey) pine, Pinus radiata D. Don, were measured. The apparently conflicting results between laboratory and field data are explained by the presence or absence of untreated feeder material in the test environment. In the absence of untreated feeder material, wood containing 0.5% BAE provided adequate protection from Coptotermes sp., whereas in the presence of untreated feeder material, increased retentions were required. Furthermore, the retentions required increased with increased amounts of susceptible material present. Some termites, Nasutitermes sp. and Mastotermes darwiniensis Froggatt, for example, are borate-tolerant and borate timber preservatives are not a viable management option with these species. The lack of uniform standards for termite test methodology and assessment criteria for efficacy across the world is recognized as a difficulty with research into the performance of timber preservatives with termites. The many variables in laboratory and field assays make "prescriptive" standards difficult to recommend. The use of "performance" standards to define efficacy criteria ("adequate" protection) is discussed.

  14. Influence of sodium borate on the early age hydration of calcium sulfoaluminate cement

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

    Champenois, Jean-Baptiste; Dhoury, Mélanie; Cau Dit Coumes, Céline, E-mail: celine.cau-dit-coumes@cea.fr

    Calcium sulfoaluminate (CSA) cements are potential candidates for the conditioning of radioactive wastes with high sodium borate concentrations. This work thus investigates early age hydration of two CSA cements with different gypsum contents (0 to 20%) as a function of the mixing solution composition (borate and NaOH concentrations). Gypsum plays a key role in controlling the reactivity of cement. When the mixing solution is pure water, increasing the gypsum concentration accelerates cement hydration. However, the reverse is observed when the mixing solution contains sodium borate. Until gypsum exhaustion, the pore solution pH remains constant at ~ 10.8, and a poorlymore » crystallized borate compound (ulexite) precipitates. A correlation is established between this transient precipitation and the hydration delay. Decreasing the gypsum content in the binder, or increasing the sodium content in the mixing solution, are two ways of reducing the stability of ulexite, thus decreasing the hydration delay.« less

  15. A macrocyclic polyamine as an anion receptor in the capillary electrochromatographic separation of carbohydrates.

    PubMed

    Liu, Chuen-Ying; Chen, Tse-Hsien; Misra, Tarun Kumar

    2007-06-22

    An analytical approach of the 32-membered macrocyclic polyamine, 1,5,9,13,17,21,25,29-octaazacyclodotriacontane ([32]ane-N8) was described for the capillary electrochromatographic (CEC) separation of derivatized mono- and disaccharides. The column displayed reversal electroosmotic flow (EOF) at pH below 7.0, while a cathodic EOF was shown at pH above 7.0. The reductive amination of saccharides was carried out with p-aminobenzoic acid. Some parameters that affect the CEC separations were investigated. Several competitive ligands, such as Tris, EDTA and phosphate were also examined for the effect on the performance. We achieved a complete separation of all compounds as well as the excess derivatizing agent by using borate buffer (pH 9.0) in a mode of concentration gradient (60 mM inlet side and 70 mM outlet side). The relative standard deviation of the retention time measured for each sample was less than 4% in six continuous runs, suggesting that the bonded phase along with the gradient formed inside the column was quite stable. With the mixing modes of anion coordination, anion exchange, and shape discrimination, the interaction adequately accomplishes the separation of carbohydrates which are epimers or have different glycosidic linkage, although the electrophoretic migration is also involved in the separation mechanism.

  16. Capillary Electrophoresis Analysis of Organic Amines and Amino Acids in Saline and Acidic Samples Using the Mars Organic Analyzer

    NASA Astrophysics Data System (ADS)

    Stockton, Amanda M.; Chiesl, Thomas N.; Lowenstein, Tim K.; Amashukeli, Xenia; Grunthaner, Frank; Mathies, Richard A.

    2009-11-01

    The Mars Organic Analyzer (MOA) has enabled the sensitive detection of amino acid and amine biomarkers in laboratory standards and in a variety of field sample tests. However, the MOA is challenged when samples are extremely acidic and saline or contain polyvalent cations. Here, we have optimized the MOA analysis, sample labeling, and sample dilution buffers to handle such challenging samples more robustly. Higher ionic strength buffer systems with pKa values near pH 9 were developed to provide better buffering capacity and salt tolerance. The addition of ethylaminediaminetetraacetic acid (EDTA) ameliorates the negative effects of multivalent cations. The optimized protocol utilizes a 75 mM borate buffer (pH 9.5) for Pacific Blue labeling of amines and amino acids. After labeling, 50 mM (final concentration) EDTA is added to samples containing divalent cations to ameliorate their effects. This optimized protocol was used to successfully analyze amino acids in a saturated brine sample from Saline Valley, California, and a subcritical water extract of a highly acidic sample from the Río Tinto, Spain. This work expands the analytical capabilities of the MOA and increases its sensitivity and robustness for samples from extraterrestrial environments that may exhibit pH and salt extremes as well as metal ions.

  17. Capillary electrophoresis analysis of organic amines and amino acids in saline and acidic samples using the Mars organic analyzer.

    PubMed

    Stockton, Amanda M; Chiesl, Thomas N; Lowenstein, Tim K; Amashukeli, Xenia; Grunthaner, Frank; Mathies, Richard A

    2009-11-01

    The Mars Organic Analyzer (MOA) has enabled the sensitive detection of amino acid and amine biomarkers in laboratory standards and in a variety of field sample tests. However, the MOA is challenged when samples are extremely acidic and saline or contain polyvalent cations. Here, we have optimized the MOA analysis, sample labeling, and sample dilution buffers to handle such challenging samples more robustly. Higher ionic strength buffer systems with pK(a) values near pH 9 were developed to provide better buffering capacity and salt tolerance. The addition of ethylaminediaminetetraacetic acid (EDTA) ameliorates the negative effects of multivalent cations. The optimized protocol utilizes a 75 mM borate buffer (pH 9.5) for Pacific Blue labeling of amines and amino acids. After labeling, 50 mM (final concentration) EDTA is added to samples containing divalent cations to ameliorate their effects. This optimized protocol was used to successfully analyze amino acids in a saturated brine sample from Saline Valley, California, and a subcritical water extract of a highly acidic sample from the Río Tinto, Spain. This work expands the analytical capabilities of the MOA and increases its sensitivity and robustness for samples from extraterrestrial environments that may exhibit pH and salt extremes as well as metal ions.

  18. Experimental Study and Reactive Transport Modeling of Boric Acid Leaching of Concrete

    NASA Astrophysics Data System (ADS)

    Pabalan, R. T.; Chiang, K.-T. K.

    2013-07-01

    Borated water leakage through spent fuel pools (SFPs) at pressurized water reactors is a concern because it could cause corrosion of reinforcement steel in the concrete structure, compromise the integrity of the structure, or cause unmonitored releases of contaminated water to the environment. Experimental data indicate that pH is a critical parameter that determines the corrosion susceptibility of rebar in borated water and the degree of concrete degradation by boric acid leaching. In this study, reactive transport modeling of concrete leaching by borated water was performed to provide information on the solution pH in the concrete crack or matrix and the degree of concrete degradation at different locations of an SFP concrete structure exposed to borated water. Simulations up to 100 years were performed using different boric acid concentrations, crack apertures, and solution flow rates. Concrete cylinders were immersed in boric acid solutions for several months and the mineralogical changes and boric acid penetration in the concrete cylinder were evaluated as a function of time. The depths of concrete leaching by boric acid solution derived from the reactive transport simulations were compared with the measured boric acid penetration depth.

  19. Determination of 1-aminocyclopropane-1-carboxylic acid in apple extracts by capillary electrophoresis with laser-induced fluorescence detection.

    PubMed

    Liu, Xin; Li, Dian-Fan; Wang, Yun; Lu, Ying-Tang

    2004-12-17

    A rapid and sensitive method for the determination of 1-aminocyclopropane-1-carboxylic acid (ACC) in apple tissues has been described. This method is based on the derivatization of ACC with 3-(2-furoyl)quinoline-2-carboxaldehyde (FQ), and separation and quantification of the resulting FQ-ACC derivative by capillary electrophoresis coupled to laser-induced fluorescence detection (CE-LIF). Our results indicated that ACC derivatized with FQ could be well separated from other interfering amino acids using 20 mM borate buffer (pH 9.35) containing 40 mM sodium dodecyl sulfate and 10 mM Brij 35. The linearity of ACC was determined in the range from 0.05 to 5 microM with a correlation of 0.9967. The concentration detection limit for ACC was 10 nM (signal-to-noise = 3). The sensitivity and selectivity of this described method allows the analysis of ACC in crude apple extracts without extra purification and enrichment procedure.

  20. [Determination of glutamic acid in biological material by capillary electrophoresis].

    PubMed

    Narezhnaya, E; Krukier, I; Avrutskaya, V; Degtyareva, A; Igumnova, E A

    2015-01-01

    The conditions for the identification and determination of Glutamic acid by capillary zone electrophoresis without their preliminary derivatization have been optimized. The effect of concentration of buffer electrolyte and pH on determination of Glutamic acid has been investigated. It is shown that the 5 Mm borate buffer concentration and a pH 9.15 are optimal. Quantitative determination of glutamic acid has been carried out using a linear dependence between the concentration of the analyte and the area of the peak. The accuracy and reproducibility of the determination are confirmed by the method "introduced - found". Glutamic acid has been determined in the placenta homogenate. The duration of analysis doesn't exceed 30 minutes. The results showed a decrease in the level of glutamic acid in cases of pregnancy complicated by placental insufficiency compared with the physiological, and this fact allows to consider the level of glutamic acid as a possible marker of complicated pregnancy.

  1. Investigation of folic acid stability in fortified instant noodles by use of capillary electrophoresis and reversed-phase high performance liquid chromatography.

    PubMed

    Hau Fung Cheung, Rodney; Morrison, Paul D; Small, Darryl M; Marriott, Philip J

    2008-12-05

    A single enzyme treatment with alpha-amylase, prior to the quantification of added folic acid (FA) in fortified instant fried Asian noodles with analysis performed by capillary zone electrophoresis (CZE) and reversed-phase high performance liquid chromatography (RP-HPLC) with UV detection, is described. The method was validated and optimized for capillary electrophoresis (CE) with separation achieved using a 8 mM phosphate-12 mM borate run buffer with 5% MeOH at pH 9.5. FA was well separated from matrix components with nicotinic acid (NA) employed as an internal standard. In a comparative study, separation of FA was performed using HPLC with a mobile phase consisting of 27% MeOH (v/v) in aqueous potassium phosphate buffer (3.5 mM KH(2)PO(4) and 3.2 mM K(2)HPO(4)), pH 8.5, and containing 5 mM tetrabutylammonium dihydrogen phosphate as an ion-pairing agent. For both methods, excellent results were obtained for various analytical parameters including linearity, accuracy and precision. The limit of detection was calculated to be 2.2 mg/L for CE without sample stacking and 0.10 mg/L with high performance liquid chromatography (HPLC). Sample extraction involved homogenization and enzymatic extraction with alpha-amylase. Results indicated that FA was stable during four main stages of instant fried noodle manufacturing (dough crumbs, cut sheets, steaming and frying).

  2. [Methods quantitative for determination of water-soluble vitamins in premixes and fortified food products by micellar electrokinetic chromatography on short end of the capillary].

    PubMed

    Bogachuk, M N; Bessonov, V V; Perederiaev, O I

    2011-01-01

    It was purposed new technique by micellar electrokinetic chromatography on short end of the capillary (capillary electrophoresis system Agilent 3D CE, DAD, quartz capillary HPCE stndrd cap 56 cm, 50 microm, 50 mM borate buffer pH=9,3, 100 mM sodium dodecil sulfate) for simultaneous determination of water-soluble vitamins (B1, B2, B6, B12, PP, B5, B9, C, B8) in fortified food products and premixes. It was observed on 6 samples of vitamin premixes and 28 samples of fortified food products using this technique. Our findings are consistent with the results of research on certain vitamins, conducted by other methods. The developed technique can be used in analysis of water-soluble vitamins in premixes and fortified food products.

  3. Electrophoretically mediated microanalysis of a nicotinamide adenine dinucleotide-dependent enzyme and its facile multiplexing using an active pixel sensor UV detector.

    PubMed

    Urban, Pawel L; Goodall, David M; Bergström, Edmund T; Bruce, Neil C

    2007-08-31

    An electrophoretically mediated microanalysis (EMMA) method has been developed for yeast alcohol dehydrogenase and quantification of reactant and product cofactors, NAD and NADH. The enzyme substrate ethanol (1% (v/v)) was added to the buffer (50 mM borate, pH 8.8). Results are presented for parallel capillary electrophoresis with a novel miniature UV area detector, with an active pixel sensor imaging an array of two or six parallel capillaries connected via a manifold to a single output capillary in a commercial CE instrument, allowing conversions with five different yeast alcohol dehydrogenase concentrations to be quantified in a single experiment.

  4. Crystallographic control on the boron isotope paleo-pH proxy

    NASA Astrophysics Data System (ADS)

    Noireaux, J.; Mavromatis, V.; Gaillardet, J.; Schott, J.; Montouillout, V.; Louvat, P.; Rollion-Bard, C.; Neuville, D. R.

    2015-11-01

    When using the boron isotopic composition (δ11B) of marine carbonates as a seawater pH proxy, it is assumed that only the tetrahedral borate ion is incorporated into the growing carbonate crystals and that no boron isotope fractionation occurs during uptake. However, the δ11B of the calcium carbonate from most modern foraminifera shells or corals skeletons is not the same as the δ11B of seawater borate, which depends on pH, an observation commonly attributed to vital effects. In this study, we combined previously published high-field 11B MAS NMR and new δ11B measurements on the same synthetic calcite and aragonite samples precipitated inorganically under controlled environments to avoid vital effects. Our results indicate that the main controlling factors of δ11B are the solution pH and the mineralogy of the precipitated carbonate mineral, whereas the aqueous boron concentration of the solution, CaCO3 precipitation rate and the presence or absence of growth seeds all appear to have negligible influence. In aragonite, the NMR data show that boron coordination is tetrahedral (BO4), in addition, its δ11B is equal to that of aqueous borate, thus confirming the paleo-pH hypothesis. In contrast, both trigonal BO3 and tetrahedral BO4 are present in calcite, and its δ11B values are higher than that of aqueous borate and are less sensitive to solution pH variations compared to δ11B in aragonite. These observations are interpreted in calcite as a reflection of the incorporation of decreasing amounts of boric acid with increasing pH. Moreover, the fraction of BO3 measured by NMR in calcite is higher than that inferred from δ11B which indicates a coordination change from BO4 to BO3 upon boron incorporation in the solid. Overall, this study shows that although the observed differences in δ11B between inorganic and biological aragonite are compatible with a pH increase at calcification sites, the B speciation and isotope composition of biological calcites call for a more complex mechanism of boron incorporation.

  5. Polarized localization and borate-dependent degradation of the Arabidopsis borate transporter BOR1 in tobacco BY-2 cells

    PubMed Central

    Matsuoka, Ken

    2013-01-01

    In Arabidopsis the borate transporter BOR1, which is located in the plasma membrane, is degraded in the presence of excess boron by an endocytosis-mediated mechanism. A similar mechanism was suggested in rice as excess boron decreased rice borate transporter levels, although in this case whether the decrease was dependent on an increase in degradation or a decrease in protein synthesis was not elucidated. To address whether the borate-dependent degradation mechanism is conserved among plant cells, we analyzed the fate of GFP-tagged BOR1 (BOR1-GFP) in transformed tobacco BY-2 cells. Cells expressing BOR1-GFP displayed GFP fluorescence at the plasma membrane, especially at the membrane between two attached cells. The plasma membrane signal was abolished when cells were incubated in medium with a high concentration of borate (3 to 5 mM). This decrease in BOR1-GFP signal was mediated by a specific degradation of the protein after internalization by endocytosis from the plasma membrane. Pharmacological analysis indicated that the decrease in BOR1-GFP largely depends on the increase in degradation rate and that the degradation was mediated by a tyrosine-motif and the actin cytoskeleton. Tyr mutants of BOR1-GFP, which has been shown to inhibit borate-dependent degradation in Arabidopsis root cells, did not show borate-dependent endocytosis in tobacco BY-2 cells. These findings indicate that the borate-dependent degradation machinery of the borate transporter is conserved among plant species. PMID:24715955

  6. Polarized localization and borate-dependent degradation of the Arabidopsis borate transporter BOR1 in tobacco BY-2 cells.

    PubMed

    Yamauchi, Noboru; Gosho, Tadashi; Asatuma, Satoru; Toyooka, Kiminori; Fujiwara, Toru; Matsuoka, Ken

    2013-01-01

    In Arabidopsis the borate transporter BOR1, which is located in the plasma membrane, is degraded in the presence of excess boron by an endocytosis-mediated mechanism. A similar mechanism was suggested in rice as excess boron decreased rice borate transporter levels, although in this case whether the decrease was dependent on an increase in degradation or a decrease in protein synthesis was not elucidated. To address whether the borate-dependent degradation mechanism is conserved among plant cells, we analyzed the fate of GFP-tagged BOR1 (BOR1-GFP) in transformed tobacco BY-2 cells. Cells expressing BOR1-GFP displayed GFP fluorescence at the plasma membrane, especially at the membrane between two attached cells. The plasma membrane signal was abolished when cells were incubated in medium with a high concentration of borate (3 to 5 mM). This decrease in BOR1-GFP signal was mediated by a specific degradation of the protein after internalization by endocytosis from the plasma membrane. Pharmacological analysis indicated that the decrease in BOR1-GFP largely depends on the increase in degradation rate and that the degradation was mediated by a tyrosine-motif and the actin cytoskeleton. Tyr mutants of BOR1-GFP, which has been shown to inhibit borate-dependent degradation in Arabidopsis root cells, did not show borate-dependent endocytosis in tobacco BY-2 cells. These findings indicate that the borate-dependent degradation machinery of the borate transporter is conserved among plant species.

  7. Simultaneous determination of ezetimibe and simvastatin in pharmaceutical preparations by MEKC.

    PubMed

    Yardimci, Ceren; Ozaltin, Nuran

    2010-02-01

    A micellar electrokinetic capillary chromatography method was developed and validated for the simultaneous determination of ezetimibe and simvastatin in pharmaceutical preparations. The influence of buffer concentration, buffer pH, sodium dodecyl sulphate (SDS) concentration, organic modifier, capillary temperature, applied voltage, and injection time was investigated, and the method validation studies were performed. The optimum separation for these analytes was achieved in less than 10 min at 30 degrees C with a fused-silica capillary column (56 cm x 50 microm i.d.) and a 25mM borate buffer at pH 9.0 containing 25mM SDS and 10% (v/v) acetonitrile. The samples were injected hydrodynamically for 3 s at 50 mbar, and the applied voltage was +30.0 kV. Detection wavelength was set at 238 nm. Diflunisal was used as internal standard. The method was suitably validated with respect to stability, specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness. The limits of detection and quantification were 1.0 and 2.0 microg/mL for both ezetimibe and simvastatin, respectively. The method developed was successfully applied to the simultaneous determination of ezetimibe and simvastatin in pharmaceutical preparations.

  8. Overview and Brief History of the Boron Isotope Proxy for Past Seawater pH

    NASA Astrophysics Data System (ADS)

    Hoenisch, B.; Hemming, G.

    2007-05-01

    In 1992 Hemming and Hanson (GCA, vol. 56, p. 537-543) showed that a variety of modern marine carbonates revealed a boron isotopic composition close to the isotopic composition of dissolved borate at modern seawater pH, suggesting this was the boron species preferentially adsorbed and incorporated into marine carbonates. With a constant offset between the trigonal and tetrahedrally coordinated boron species and a pH-dependent variation in their fractions, it appeared that this system would be sensitive to pH changes in the natural range of seawater. Accordingly, it was suggested that the boron isotope composition of marine carbonates is a proxy for past seawater pH. Subsequent culture studies with living planktic foraminifers and corals, as well as synthetic precipitation experiments confirmed that the boron isotopic composition follows the isotopic composition of borate across a wide range of seawater pH. In order to use the proxy with confidence, however, all other controls apart from pH need to be thoroughly understood. Recent laboratory and sediment experiments have demonstrated that vital effects and partial shell dissolution have the potential to modify the primary seawater pH signal recorded in the boron isotopic composition of planktic foraminifers. However it has also been shown that careful sample selection allows for avoiding these potential complications. A record of reconstructed surface seawater pH and estimated aqueous PCO2 shows a remarkable match between boron isotope based atmospheric pCO2 estimates and the Vostok ice core CO2 record. This convincingly demonstrates that boron isotopes in planktic foraminifers allow quantitative estimates of atmospheric pCO2 in the past, and confirms that glacial surface ocean pH was ~0.2 units higher compared to interglacial periods. We are going to review and discuss the achievements generated in Gil Hanson's lab over the past 15 years in the light of recent empirical measurements of the boron isotope fractionation between boric acid and borate in seawater.

  9. THE KINETICS OF SAPONIFICATION OF IODOACETIC ACID BY SODIUM HYDROXIDE AND BY CERTAIN ALKALINE BUFFER SOLUTIONS.

    PubMed

    Brdicka, R

    1936-07-20

    1. The rate of the saponification of iodoacetic acid in sodium hydroxide and alkaline buffer solutions yielding glycollic acid was measured by means of Heyrovský's polarographic method. 2. From the bimolecular velocity constants, increasing with the ionic strength of the solution, the Brönsted factor, F, which characterizes the primary salt effect, was calculated. 3. In the borate buffer solutions the monomolecular constants of the saponification were determined which, at values above the pH of neutralization of boric acid, show a proportionality to the concentration of hydroxyl anions. Below the pH of neutralization of boric acid, they are proportional to the concentration of borate anions.

  10. Pseudotetrahedral manganese complexes supported by the anionic tris(phosphino)borate ligand [PhBPiPr3

    PubMed Central

    Lu, Connie C.; Peters, Jonas C.

    2008-01-01

    This paper presents aspects of the coordination chemistry of mono- and divalent manganese complexes supported by the anionic tris(phosphino)borate ligand, [PhBPiPr3] (where [PhBPiPr3] = [PhB(CH2PiPr2)3]−). The Mn(II) halide complexes, [PhBPiPr3]MnCl (1 and [PhBPiPr3]MnI (2), have been characterized by X-ray diffraction, SQUID magnetometry, and EPR spectroscopy. Compound 2 serves as a precursor to a series of Mn azide, alkyl, and amide species: [PhBPiPr3]Mn(N3) (3), [PhBPiPr3]Mn(CH2Ph) (4), [PhBPiPr3]Mn(Me) (5), [PhBPiPr3]Mn(NH(2,6-iPr2-C6H3)) (6), [PhBPiPr3]Mn(dbabh) (7), and [PhBPiPr3]Mn(1-Ph(isoindolate)) (8). The complexes 2 – 8 feature a divalent-metal center and are pseudotetrahedral. They collectively represent an uncommon structural motif for low-coordinate, polyphosphine-supported Mn complexes. Two Mn(I) species have also been prepared. These include the Tl-Mn adduct, [PhBPiPr3]Tl-MnBr(CO)4 (9), and the octahedral complex [PhBPiPr3]Mn(CNtBu)3 (10). Some of our initial synthetic efforts to generate [PhBPiPr3]Mn≡Nx species are briefly described, as are DFT studies that probe the electronic viability of these types of multiply bonded target structures. PMID:17029370

  11. Uranium(iii) complexes supported by hydrobis(mercaptoimidazolyl)borates: synthesis and oxidation chemistry.

    PubMed

    Maria, Leonor; Santos, Isabel C; Santos, Isabel

    2018-05-23

    The reaction of [UI3(thf)4] with the sodium or lithium salts of hydrobis(2-mercapto-1-methylimidazolyl)borate ligands ([H(R)B(timMe)2]-) in a 1 : 2 ratio, in tetrahydrofuran, gave the U(iii) complexes [UI{κ3-H,S,S'-H(R)B(timMe)2}2(thf)2] (R = H (1), Ph (2)) in good yields. Crystals of [UI{κ3-H,S,S'-H(Ph)B(timMe)2}2(thf)2] (2) were obtained by recrystallization from a tetrahydrofuran/acetonitrile solution, and the ion-separated uranium complex [U{κ3-H,S,S'-H(Ph)B(timMe)2}2(CH3CN)3][I] (3-I) was obtained by dissolution of 2 in acetonitrile followed by recrystallization. One-electron oxidation of 2 with AgBPh4 or I2 resulted in the formation of the cationic U(iv) complexes [U{κ3-H,S,S'-H(Ph)B(timMe)2}3][X] (X = BPh4 (6-BPh4), I (6-I)), due to a ligand redistribution process. These complexes are the first examples of homoleptic poly(azolyl)borate U(iv) complexes. Treatment of complex 2 with azobenzene led to the isolation of crystals of the U(iv) compound [UI{κ3-H(Ph)B(timMe)2}2(κ2-timMe)] (7). Treatment of 2 with pyridine-N oxide (pyNO) led to the formation of the uranyl complex [UO2{κ2-S,S'-H(Ph)B(timMe)2}2] (8) and of complex 6-I, while from the reaction of [U{κ3-H(Ph)B(timMe)2}2(thf)3][BPh4] (5) with pyNO, the oxo-bridged U(iv) complex [{U{κ3-H(Ph)B(timMe)2}2(pyNO)}2(μ-O)][BPh4]2 (9) was also obtained. In the U(iii) and U(iv) complexes, the bis(azolyl)borate ligands bind to the uranium center in a κ3-H,S,S' coordination mode, while in the U(vi) complex the ligands bind to the metal in a κ2-S,S' mode. The presence of UH-B interactions in the solid-state, for the nine-coordinate complexes 1, 2, 3, 6 and 7 and for the eight-coordinate complex 9, was supported by IR spectroscopy and/or X-ray diffraction analysis.

  12. THE KINETICS OF SAPONIFICATION OF IODOACETIC ACID BY SODIUM HYDROXIDE AND BY CERTAIN ALKALINE BUFFER SOLUTIONS

    PubMed Central

    Brdička, R.

    1936-01-01

    1. The rate of the saponification of iodoacetic acid in sodium hydroxide and alkaline buffer solutions yielding glycollic acid was measured by means of Heyrovský's polarographic method. 2. From the bimolecular velocity constants, increasing with the ionic strength of the solution, the Brönsted factor, F, which characterizes the primary salt effect, was calculated. 3. In the borate buffer solutions the monomolecular constants of the saponification were determined which, at values above the pH of neutralization of boric acid, show a proportionality to the concentration of hydroxyl anions. Below the pH of neutralization of boric acid, they are proportional to the concentration of borate anions. PMID:19872968

  13. Development and validation of an MEKC method for determination of nitrogen-containing drugs in pharmaceutical preparations.

    PubMed

    Buiarelli, Francesca; Coccioli, Franco; Jasionowska, Renata; Terracciano, Alessandro

    2008-09-01

    A fast and accurate micellar electrokinetic capillary chromatography method was developed for quality control of pharmaceutical preparations containing cold remedies as acetaminophen, salicylamide, caffeine, phenylephrine, pseudoephedrine, norephedrine and chlorpheniramine. The method optimization was realized on a Beckman P/ACE System MDQ instrument. The baseline separation of seven analytes was performed in an uncoated fused silica capillary internal diameter (ID)=50 microm using tris-borate (20 mM, pH=8.5) containing sodium dodecyl sulphate 30 mM BGE. On line-UV detection at 214 nm was performed and the applied voltage was 10 kV. The operating temperature was 25 degrees C. After experimental conditions optimization, the proposed method was validated. The evaluated parameters were: precision of migration time and of corrected peak area ratio, linearity range, limit of detection, limit of quantification, accuracy (recovery), ruggedness and applicability. The method was then successfully applied for the analysis of three pharmaceutical preparations containing some of the analytes listed before.

  14. D-Tagatose production in the presence of borate by resting Lactococcus lactis cells harboring Bifidobacterium longum L-arabinose isomerase.

    PubMed

    Salonen, Noora; Salonen, Kalle; Leisola, Matti; Nyyssölä, Antti

    2013-04-01

    Bifidobacterium longum NRRL B-41409 L-arabinose isomerase (L-AI) was overexpressed in Lactococcus lactis using a phosphate depletion inducible expression system. The resting L. lactis cells harboring the B. longum L-AI were used for production of D-tagatose from D-galactose in the presence of borate buffer. Multivariable analysis suggested that high pH, temperature and borate concentration favoured the conversion of D-galactose to D-tagatose. Almost quantitative conversion (92 %) was achieved at 20 g L⁻¹ substrate and at 37.5 °C after 5 days. The D-tagatose production rate of 185 g L⁻¹ day ⁻¹ was obtained at 300 g L⁻¹ galactose, at 1.15 M borate, and at 41 °C during 10 days when the production medium was changed every 24 h. There was no significant loss in productivity during ten sequential 24 h batches. The initial D-tagatose production rate was 290 g L⁻¹ day⁻¹ under these conditions.

  15. Effect of the adsorption of lithium and borate species on the zeta potential of particles of cobalt ferrite, nickel ferrite, and magnetite.

    PubMed

    Barale, M; Lefèvre, G; Carrette, F; Catalette, H; Fédoroff, M; Cote, G

    2008-12-01

    Zetametric measurements on suspensions of oxide particles (cobalt ferrite, nickel ferrite, and magnetite) representative of corrosion products from primary circuits of pressurized water reactors were performed at 25 and 70 degrees C in the presence of lithium and borate species. No effect of lithium ions was observed. Borate species cause a decrease of the isoelectric point (IEP), attributed to the sorption of borate as a negative complex MOB(OH)3(-). A predictive model based on thermodynamic calculations (2-pK and diffuse layer models) of the surface acidity constants from the data of acid-base titrations combined with an empirical relationship between the surface potential Psi 0 and the zeta potential determined by zetametry was developed. A whole set of parameters valid at 25 degrees C, in a range of ionic strength between 10(-4) and 10(-2) molL(-1) and in a range of pH between 4 and 8, was determined for this model. Increase of temperature to 70 degrees C in the presence of borate results in a decrease of IEP for cobalt ferrite and an increase of the IEP for nickel ferrite.

  16. Determination of psilocybin in Psilocybe semilanceata by capillary zone electrophoresis.

    PubMed

    Pedersen-Bjergaard, S; Sannes, E; Rasmussen, K E; Tønnesen, F

    1997-07-04

    A capillary zone electrophoretic (CZE) method was developed for the rapid determination of psilocybin in Psilocybe semilanceata. Following a simple two step extraction with 3.0+2.0 ml methanol, the hallucinogenic compound was effectively separated from matrix components by CZE utilizing a 10 mM borate-phosphate running buffer adjusted to pH 11.5. The identity of psilocybin was confirmed by migration time information and by UV spectra, while quantitation was accomplished utilizing barbital as internal standard. The calibration curve for psilocybin was linear within 0.01-1 mg/ml, while intra-day and inter-day variations of quantitative data were 0.5 and 2.5% R.S.D., respectively. In addition to psilocybin, the method was also suitable for the determination of the structurally related compound baeocystin.

  17. Analysis of sesquiterpenes in Valeriana officinalis by capillary electrophoresis.

    PubMed

    Mikell, J R; Ganzera, M; Khan, I A

    2001-12-01

    A capillary electrophoresis (CE) method permitting the determination of the main sesquiterpenes in Valeriana officinalis has been developed. A separation of valerenic acid and its hydroxy and acetoxy derivatives, three compounds characteristic for the species, was achieved using a 40 mM phosphate-borate buffer at pH 8.5, which contained 10% isopropanol as organic modifier. Applied temperature and voltage were 35 degrees C and 17.5 kV, respectively. This setup allowed a baseline separation of the three compounds within 8 min, with a detection limit of 5.8 micrograms/ml or less. Out of six market products analyzed, only one contained a detectable amount of the marker compounds, with 0.54% of hydroxyvalerenic acid and 0.13% valerenic acid, respectively. The quantitative results were comparable to those obtained by HPLC.

  18. Activation of heteroallenes by coordinatively unsaturated nickel(ii) alkyl complexes supported by the hydrotris(3-phenyl-5-methyl)pyrazolyl borate (Tp(Ph,Me)) ligand.

    PubMed

    Abubekerov, Mark; Eymann, Léonard Y M; Gianetti, Thomas L; Arnold, John

    2016-10-07

    Activation of sulfur containing heteroallenes by nickel(ii) alkyl complexes supported by the bulky hydrotris(3-phenyl-5-methylpyrazolyl)borate (Tp(Ph,Me)) ligand is described. Exposure of Tp(Ph,Me)NiCH2Ph (1a) and Tp(Ph,Me)NiCH2Si(CH3)3 (1b) to CS2 resulted in formation of the insertion products Tp(Ph,Me)Ni(η(2)-CS2)CH2Ph (2a) and Tp(Ph,Me)Ni(η(2)-CS2)CH2Si(CH3)3 (2b) in moderate yields. Reaction of 1a and MeNCS produced two species in a 1 : 1 ratio, identified as Tp(Ph,Me)Ni(η(2)-MeNC)CH2Ph (3) and Tp(Ph,Me)Ni(η(2)-MeNCS)SCH2Ph (4). Isolation of the unexpected insertion product (3) prompted an investigation into the activity of 1a-b in the presence of isocyanides (i.e.(t)BuNC), which resulted in isolation of Tp(Ph,Me)Ni(η(2-t)BuNC)CH2Ph (5a) and Tp(Ph,Me)Ni(η(2-t)BuNC)CH2Si(CH3)3 (5b). Similarly, reaction of 1a with OCS led to the isolation of a rare example of a Ni(i) carbonyl species Tp(Ph,Me)NiCO (6). Alternatively, complex 6 was also formed by exposure of 1a-b to an atmosphere of CO. Isolation of the intermediate species (Tp(Ph,Me)Ni(η(2)-CO)CH2TMS (7b) and Tp(Ph,Me)Ni(CO)(C(O)R, (8a-b) with R = Ph, TMS)) shed light on the formation of such species.

  19. Conversion of borate-based glass scaffold to hydroxyapatite in a dilute phosphate solution.

    PubMed

    Liu, Xin; Pan, Haobo; Fu, Hailuo; Fu, Qiang; Rahaman, Mohamed N; Huang, Wenhai

    2010-02-01

    Porous scaffolds of a borate-based glass (composition in mol%: 6Na2O, 8K2O, 8MgO, 22CaO, 36B2O3, 18SiO2, 2P2O5), with interconnected porosity of approximately 70% and pores of size 200-500 microm, were prepared by a polymer foam replication technique. The degradation of the scaffolds and conversion to a hydroxyapatite-type material in a 0.02 M K2HPO4 solution (starting pH = 7.0) at 37 degrees C were studied by measuring the weight loss of the scaffolds, as well as the pH and the boron concentration of the solution. X-ray diffraction, scanning electronic microscopy and energy dispersive x-ray analysis showed that a hydroxyapatite-type material was formed on the glass surface within 7 days of immersion in the phosphate solution. Cellular response to the scaffolds was assessed using murine MLO-A5 cells, an osteogenic cell line. Scanning electron microscopy showed that the scaffolds supported cell attachment and proliferation during the 6 day incubation. The results indicate that this borate-based glass could provide a promising degradable scaffold material for bone tissue engineering applications.

  20. First Observations of Boron on Mars and Implications for Gale Crater Geochemistry

    NASA Astrophysics Data System (ADS)

    Gasda, P. J.; Haldeman, E. B.; Wiens, R. C.; Rapin, W.; Frydenvang, J.; Maurice, S.; Clegg, S. M.; Delapp, D.; Sanford, V.; McInroy, R.

    2016-12-01

    Borates are potentially important precursor materials for the origin of life on Earth. It has been shown that borates are required to stabilize ribose, a component of RNA, when produced by the formose reaction, a prebiotically plausible mechanism to produce ribose from formaldehyde. Evaporites, including borates, also shed light on the history of aqueous activity on Mars. The ChemCam instrument onboard the NASA Curiosity rover provides quantitative elemental compositions of targets in Gale Crater, Mars, using laser-induced breakdown spectroscopy (LIBS). Laboratory observations of Fe-free targets indicate that a LIBS emission line is visible with as little as 10 ppm B. We have observed B lines in 23 calcium sulfate veins in Gale Crater: 3 in Yellowknife Bay and 20 in the Murray lacustrine mudstone and the Stimson eolian sandstone units since sol 727, as Curiosity arrived at the base of Mt. Sharp, a 5 km sedimentary mound in the center of Gale Crater. To calibrate these observations, samples composed of borates diluted with Hawaiian basalt have been analyzed using the LANL ChemCam engineering model. Preliminary results show that the Gale Crater veins have between 10-100 ppm B. One possible explanation for borates in veins is that Gale Lake evaporated, depositing evaporites, including borates. Later, Gale Crater was partially buried and its lacustrine and overlying eolian units were lithified and fractured. Water flowed through the evaporite-rich layers, partially dissolving them. Fluid moved through the fractures, re-precipitating the borates and sulfates as veins. ChemCam cannot directly determine mineralogy, but B is likely present as borax as the dominate borate phase in these veins, based on previous estimates of vein fluid temperature. Borates forming in this environment tend to precipitate from mildly alkaline fluids. The fluid temperature and pH implies these veins were potentially habitable environments.

  1. Determination of phthalic acid esters in Chinese white spirit using dispersive liquid-liquid microextraction coupled with sweeping β-cyclodextrin-modified micellar electrokinetic chromatography.

    PubMed

    Sun, Jianzhi; He, Hui; Liu, Shuhui

    2014-07-01

    A simple method that consumes low organic solvent is proposed for the analysis of phthalic acid esters in Chinese white spirit using dispersive liquid-liquid microextraction coupled with sweeping-micellar electrokinetic chromatography. Tetrachloromethane and white-spirit-containing ethanol were used as the extraction and dispersing solvents, respectively. The electrophoresis separation buffer was composed of 5 mM β-cyclodextrin, 50 mM sodium dodecyl sulfate and 25 mM borate buffer (pH 9.2) with 9% acetonitrile, enabling the baseline resolution of the analytes within 13 min. Under the optimum conditions, satisfactory linearities (5-1000 ng/mL, r ≥ 0.9909), good reproducibility (RSD ≤ 6.7% for peak area, and RSD ≤ 2.8% for migration time), low detection limits (0.4-0.8 ng/mL) and acceptable recovery rates (89.6-105.7%) were obtained. The proposed method was successfully applied to 22 Chinese white spirits, and the content of dibutyl phthalate in 55% of the samples exceeded the Specific Migration Limit of 0.3 mg/kg established by the domestic and international regulations. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Analysis of some cytokinins in coconut (Cocos nucifera L.) water by micellar electrokinetic capillary chromatography after solid-phase extraction.

    PubMed

    Ge, Liya; Yong, Jean Wan Hong; Tan, Swee Ngin; Yang, Xin Hao; Ong, Eng Shi

    2004-09-03

    Micellar electrokinetic capillary chromatography (MECC) was developed for the separation of cytokinins including trans-zeatin, trans-zeatin-O-glucoside, dihydrozeatin, dihydrozeatin-O-glucoside, meta-topolin riboside, N6-isopentenyladenine and N6-benzylaminopurine. Under the optimum conditions, i.e. a combination of 10 mM phosphate and 10 mM borate as the running buffer containing 50 mM sodium dodecyl sulphate at pH 10.4, the separation of seven cytokinin standards was accomplished within 11 min. The C18 solid-phase extraction (SPE) method was used to pre-concentrate the putative cytokinins present in the coconut water. Following which, the eluate was further purified using mixed mode Oasis MCX SPE columns and this additional step helps to reduce matrix interference during MECC. After the two solid-phase extraction steps, the optimized MECC method was able to screen for certain cytokinins (zeatin-O-glucoside and dihydrozeatin-O-glucoside) present in coconut water. After this screening, the presence of zeatin-O-glucoside and dihydrozeatin-O-glucoside in coconut water was further confirmed by independent high-performance liquid chromatography and liquid chromatography-mass spectrometry experiments.

  3. Geochemical characteristics of Kırka (Sarıkaya) borate deposit, northwestern Anatolia, Turkey

    NASA Astrophysics Data System (ADS)

    Koçak, İ.; Koç, Ş.

    2016-02-01

    The Kırka borate deposit was deposited in a Miocene lacustrine basin which is closely associated with volcanic activity which lasted from Paleogene to the beginning of Quaternary. Borate mineralization alternates with claystone, mudstone, tuff and fine-layered limestone and mostly shows a lenticular structure. The mineral paragenesis is composed of borax, tincalconite, ulexite, kurnakovite, probertite, tunellite, colemanite, dolomite, smectite group minerals, illite and some firstly reported minerals for the Kırka deposit including hydrochloroborite, brianroulstonite, hilgardite-4M and searlesite minerals. In comparison to average values of earth crust, concentrations of Cs, Sr, Li, As and Se were significantly enriched with respective rates of 21, 15, 14, 3 and 188 folds. Regarding KY, KS1 and KS2 locations, there are differences in both element abundances and their geochemical tendencies which are attributed to variations in discharge regime and physico-chemical conditions of the depositional environment. Independent behaviour of B2O3 might indicate that boron is not associated with clays and carbonates and, therefore, most part of boron must be derived from volcanic activity (hydrothermal solutions, gases). REE data indicate that the Kırka borate deposit was formed in a sedimentary environment where highly alkaline (high pH) hydrothermal solutions also took part in borate precipitation process.

  4. Determination of penicillamine in pharmaceuticals and human plasma by capillary electrophoresis with in-column fiber optics light-emitting diode induced fluorescence detection.

    PubMed

    Yang, Xiupei; Yuan, Hongyan; Wang, Chunling; Su, Xiaodong; Hu, Li; Xiao, Dan

    2007-10-18

    In this paper, a capillary electrophoresis (CE) system with in-column fiber optics light-emitting diode (LED) induced fluorescence detection was developed for the determination of penicillamine (PA). The influence of buffer concentration, buffer pH, applied voltage and injection time was systematically investigated. Optimum separation conditions were obtained with 10 mM borate buffer at pH 9.1, applied voltage 20 kV and 8 s hydrodynamic injection at 30 mbar. The detection system displayed linear dynamic range from 3.2 x 10(-7) to 4.8 x 10(-5) mol L(-1) with a correlation coefficient of 0.9991 and good repeatability (R.S.D.=2.46%). The method was applied to the determination of PA in commercial tablets and human plasma, which the recoveries of standard PA added to tablets and human plasma sample were found to be in the range of 96.26-102.68 and 91.10-99.35%, respectively. The proposed method is cheap, rapid, easy, and accurate, and can be successfully applied to the formulation analysis and bioanalysis.

  5. Optical isomer separation of potential analgesic drug candidates by using capillary electrophoresis.

    PubMed

    Ferrara, G; Santagati, N A; Aturki, Z; Fanali, S

    1999-09-01

    Using cyclodextrin capillary zone electrophoresis (CD-CZE), baseline separation of synthetic potential analgesic drug diastereoisomer candidates 6,11-dimethyl-1,2,3,4,5,6-hexahydro-3-[(2'-methoxycarbonyl-2'-phenylc yclopropyl)methyl]-2,6-methano-3-benzazocin-8-ol (MPCB) and 6,11-dimethyl-1,2,3,4,5,6-hexahydro-3-[[2'-methoxycarbonyl-2'(4-chloroph enyl)cyclopropyl]methyl]-2,6-methano-3-benzazocin-8-ol (CCB) was achieved. Among the cyclodextrins tested (hydroxypropyl-, carboxymethyl- and sulfobutyl-beta-cyclodextrin (HP-beta-CD, CM-beta-CD and SBE-beta-CD)) SBE-beta-CD was found to be the most effective complexing agent, allowing good optical isomer separation. Resolution was also influenced by the CD concentration, pH of the buffer and presence of organic modifier in the background electrolyte. The optimum experimental conditions for the separation of studied analgesic drugs were found using 25 mM borate buffer at pH 9 containing 40 mM of SBE-beta-CD and 20% v/v of methanol. Using the above-mentioned background electrolyte, it was also possible to separate, in the same run, the enantiomers of normetazocine (NMZ) as well as the optical isomers of (+/-)-cis-2-chloromethyl-1-phenyl cyclopropancarboxylic acid methyl ester (PCE) or (+/-)-cis-2-chloromethyl-1-(4-chlorophenyl)cyclopropancarboxylic acid methyl ester (CPCE) reagents used in the synthesis of the studied analgesic drugs).

  6. Somatic embryogenesis of carrot in hormone-free medium: external pH control over morphogenesis

    NASA Technical Reports Server (NTRS)

    Smith, D. L.; Krikorian, A. D.

    1990-01-01

    Cultures of preglobular stage proembryos (PGSPs) were initiated from mechanically wounded mature zygotic embryos of carrot, Daucus carota, on a hormone-free, semisolid medium. These PGSPs have been maintained and multiplied for extended periods without their progression into later embryo stages on the same hormone-free medium containing 1 mM NH4+ as the sole nitrogen source. Sustained maintenance of cultures comprised exclusively of PGSPs was dependent on medium pH throughout the culture period. Best growth and multiplication of PGSP cultures occurred when the pH of unbuffered, hormone-free medium fell from 4.5 to 4 over a 2-week period or when buffered medium was titrated to pH 4. If the hormone-free medium was buffered to sustain a pH at or above 4.5, PGSPs developed into later embryo stages. Maintenance with continuous multiplication of PGSPs occurred equally well on medium containing NH4+ or NH4+ and NO3-, but growth was poor with NO3- alone. Additional observations on the effects of medium components such as various nitrogen sources and levels, sucrose concentration, semisolid supports, type of buffer, borate concentration, activated charcoal, and initial pH that permit optimum maintenance of the PGSPs or foster their continued developmental progression into mature embryos and plantlets are reported. The influence of the pH of the hormone-free medium as a determinant in maintaining cultures as PGSPs or allowing their continued embryonic development are unequivocally demonstrated by gross morphology, scanning electron microscopy, and histological preparations.

  7. Intracavity frequency doubling of a continuous-wave, diode-laser-pumped neodymium lanthanum scandium borate laser.

    PubMed

    Meyn, J P; Huber, G

    1994-09-15

    Neodymium-doped lanthanum scandium borate [Nd:LaSc(3)(BO(3))(4)] is a new material for efficient and compact diode-pumped solid-state lasers. A simple plane-plane 3-mm-long resonator is formed by a coated Nd(10%):LaSc(3)(BO(3))(4) crystal and a coated potassium titanyl phosphate (KTP) crystal. The second-harmonic output power at 531 nm is 522 mW at 2.05-W incident pump power of the diode laser. The corresponding optical efficiency is 25%, and the conversion efficiency from the fundamental to the second harmonic is 55%. The wellknown chaotic power fluctuations of intracavity frequency-doubled lasers (green problem) are avoided by use of a short KTP crystal, between 0.5 and 2 mm in length.

  8. Coexpression of β-D-galactosidase and L-arabinose isomerase in the production of D-tagatose: a functional sweetener.

    PubMed

    Zhan, Yijing; Xu, Zheng; Li, Sha; Liu, Xiaoliu; Xu, Lu; Feng, Xiaohai; Xu, Hong

    2014-03-19

    The functional sweetener, d-tagatose, is commonly transformed from galactose by l-arabinose isomerase. To make use of a much cheaper starting material, lactose, hydrolization, and isomerization are required to take place collaboratively. Therefore, a single-step method involving β-d-galactosidase was explored for d-tagatose production. The two vital genes, β-d-galactosidase gene (lacZ) and l-arabinose isomerase mutant gene (araA') were extracted separately from Escherichia coli strains and incorporated into E. coli simultaneously. This gave us E. coli-ZY, a recombinant producing strain capable of coexpressing the two key enzymes. The resulted cells exhibited maximum d-tagatose producing activity at 34 °C and pH 6.5 and in the presence of borate, 10 mM Fe(2+), and 1 mM Mn(2+). Further monitoring showed that the recombinant cells could hydrolyze more than 95% lactose and convert 43% d-galactose into d-tagatose. This research has verified the feasibility of single-step d-tagatose fermentation, thereby laying down the foundation for industrial usage of lactose.

  9. Simultaneous high-throughput determination of clenbuterol, ambroxol and bromhexine in pharmaceutical formulations by HPLC with potentiometric detection.

    PubMed

    Bazylak, Grzegorz; Nagels, Luc J

    2003-08-08

    Potentiometric detection of clenbuterol, ambroxol and bromhexine in marketed pharmaceuticals was described in six isocratic HPLC systems. The podant- and macrocyclic-type neutral ionophores, N,N,N',N'-tetracyclohexyl-oxybis(o-phenyleneoxy)diacetamide (TOPA) and hexakis(2,3,6-tri-O-octyl)-alpha-cyclodextrin (OCD), were applied in poly(vinyl)chloride (PVC)-based liquid membrane electrodes. Both types of neutral ionophores improve the sensitivity for all mentioned drugs when compared with a tetrakis(p-chlorophenyl)borate (BOR)-based electrode as well as with single wavelength UV detection. Detection limits (S/N=3) of 2.6 x 10(-10) mol l(-1) (injected concentration) for the highly hydrophobic bromhexine were achieved with the TOPA-based electrode and a cyano reversed-phase (RP)-HPLC with Uptisphere UP5CN-25QS silica column (250 x 4.6 mm i.d.) eluted with acetonitrile (AcN)-ethanol-perchloric acid (1.66 mM) (60:2:38, v/v/v) (pH* 2.45). Comparable result was obtained with OCD-based electrodes and an XTerra RP18 hybrid silica-polymer column eluted with AcN-phosphoric acid (20 mM) (25:75, v/v) (pH* 2.60). In the mobile phases containing 60-75% v/v AcN or methanol, stable and reproducible response of both types of neutral ionophore-based electrodes was observed for at least 3 days. The results of the validated procedure for reliable simultaneous determination of the drugs in fortified representative samples of pharmaceuticals were also presented.

  10. Offline and online capillary electrophoresis enzyme assays of β-N-acetylhexosaminidase.

    PubMed

    Křížek, Tomáš; Doubnerová, Veronika; Ryšlavá, Helena; Coufal, Pavel; Bosáková, Zuzana

    2013-03-01

    Enzyme assays of β-N-acetylhexosaminidase from Aspergillus oryzae using capillary electrophoresis in the offline and online setup have been developed. The pH value and concentration of the borate-based background electrolyte were optimized in order to achieve baseline separation of N,N',N″-triacetylchitotriose, N,N'-diacetylchitobiose, and N-acetyl-D-glucosamine. The optimized method using 25 mM tetraborate buffer, pH 10.0, was evaluated in terms of repeatability, limits of detection, quantification, and linearity. The method was successfully applied to the offline enzyme assay of β-N-acetylhexosaminidase, which was demonstrated by monitoring the hydrolysis of N,N',N″-triacetylchitotriose. The presented method was also utilized to study the pH dependence of enzyme activity. An online assay with N,N'-diacetylchitobiose as a substrate was developed using the Transverse Diffusion of Laminar Flow Profiles model to optimize the injection sequence and in-capillary mixing of substrate and enzyme plugs. The experimental results were in good agreement with predictions of the model. The online assay was successfully used to observe the inhibition effect of N,N'-dimethylformamide on the activity of β-N-acetylhexosaminidase with nanoliter volumes of reagents used per run and a high degree of automation. After adjustment of background electrolyte pH, an online assay with N,N',N″-triacetylchitotriose as a substrate was also performed.

  11. Amorphous Nickel-Cobalt-Borate Nanosheet Arrays for Efficient and Durable Water Oxidation Electrocatalysis under Near-Neutral Conditions.

    PubMed

    Chen, Lanlan; Ren, Xiang; Teng, Wanqing; Shi, Pengfei

    2017-07-21

    Electrolytic hydrogen generation needs earth-abundant oxygen evolution reaction electrocatalysts that perform efficiently at mild pH. Here, the development of amorphous nickel-cobalt-borate nanosheet arrays on macroporous nickel foam (NiCo-Bi/NF) as a 3D catalyst electrode for high-performance water oxidation in near-neutral media is reported. To drive a current density of 10 mA cm -2 , the resulting NiCo-Bi/NF demands an overpotential of only 430 mV in 0.1 m potassium borate (K-Bi, pH 9.2). Moreover, it also shows long-term electrochemical durability with maintenance of catalytic activity for 20 h, achieving a high turnover frequency of 0.21 s -1 at an overpotential of 550 mV. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Arrested α-hydride migration activates a phosphido ligand for C–H insertion

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

    Hickey, Anne K.; Muñoz, Salvador B.; Lutz, Sean A.

    Bulky tris(carbene)borate ligands provide access to high spin iron(II) phosphido complexes. The complex PhB(MesIm) 3FeP(H)Ph is thermally unstable, and we observed [PPh] group insertion into a C–H bond of the supporting ligand. An arrested α-hydride migration mechanism suggests increased nucleophilicity of the phosphorus atom facilitates [PPh] group transfer reactivity.

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

    Xu, Songchen; Manna, Kuntal; Ellern, Arkady

    In order to facilitate oxidative addition chemistry of fac-coordinated rhodium(I) and iridium(I) compounds, carbene–bis(oxazolinyl)phenylborate proligands have been synthesized and reacted with organometallic precursors. Two proligands, PhB(OxMe2)2(ImtBuH) (H[1]; OxMe2 = 4,4-dimethyl-2-oxazoline; ImtBuH = 1-tert-butylimidazole) and PhB(OxMe2)2(ImMesH) (H[2]; ImMesH = 1-mesitylimidazole), are deprotonated with potassium benzyl to generate K[1] and K[2], and these potassium compounds serve as reagents for the synthesis of a series of rhodium and iridium complexes. Cyclooctadiene and dicarbonyl compounds {PhB(OxMe2)2ImtBu}Rh(η4-C8H12) (3), {PhB(OxMe2)2ImMes}Rh(η4-C8H12) (4), {PhB(OxMe2)2ImMes}Rh(CO)2 (5), {PhB(OxMe2)2ImMes}Ir(η4-C8H12) (6), and {PhB(OxMe2)2ImMes}Ir(CO)2 (7) are synthesized along with ToMM(η4-C8H12) (M = Rh (8); M = Ir (9); ToM = tris(4,4-dimethyl-2-oxazolinyl)phenylborate). The spectroscopicmore » and structural properties and reactivity of this series of compounds show electronic and steric effects of substituents on the imidazole (tert-butyl vs mesityl), effects of replacing an oxazoline in ToM with a carbene donor, and the influence of the donor ligand (CO vs C8H12). The reactions of K[2] and [M(μ-Cl)(η2-C8H14)2]2 (M = Rh, Ir) provide {κ4-PhB(OxMe2)2ImMes'CH2}Rh(μ-H)(μ-Cl)Rh(η2-C8H14)2 (10) and {PhB(OxMe2)2ImMes}IrH(η3-C8H13) (11). In the former compound, a spontaneous oxidative addition of a mesityl ortho-methyl to give a mixed-valent dirhodium species is observed, while the iridium compound forms a monometallic allyl hydride. Photochemical reactions of dicarbonyl compounds 5 and 7 result in C–H bond oxidative addition providing the compounds {κ4-PhB(OxMe2)2ImMes'CH2}RhH(CO) (12) and {PhB(OxMe2)2ImMes}IrH(Ph)CO (13). In 12, oxidative addition results in cyclometalation of the mesityl ortho-methyl similar to 10, whereas the iridium compound reacts with the benzene solvent to give a rare crystallographically characterized cis-[Ir](H)(Ph) complex. Alternatively, the rhodium carbonyl 5 or iridium isocyanide {PhB(OxMe2)2ImMes}Ir(CO)CNtBu (15) reacts with PhSiH3 in the dark to form the silyl compound {PhB(OxMe2)2ImMes}RhH(SiH2Ph)CO (14) or {PhB(OxMe2)2ImMes}IrH(SiH2Ph)CNtBu (17). These examples demonstrate the enhanced thermal reactivity of {PhB(OxMe2)2ImMes}-supported iridium and rhodium carbonyl compounds in comparison to tris(oxazolinyl)borate, tris(pyrazolyl)borate, and cyclopentadienyl-supported compounds.« less

  14. Separation of three water-soluble vitamins by poly(dimethylsiloxane) microchannel electrophoresis with electrochemical detection.

    PubMed

    Li, Xiang-Yun; Zhang, Qian-Li; Lian, Hong-Zhen; Xu, Jing-Juan; Chen, Hong-Yuan

    2007-09-01

    A method for rapid separation and sensitive determination of three water-soluble vitamins, pyridoxine, ascorbic acid (VC), and p-aminobenzoic acid (PABA) has been developed by PDMS microchannel electrophoresis integrated with amperometric detection. After treatment of the microchip with oxygen plasma, the peak shapes of the three analytes were essentially improved. Pyridoxine, VC, and PABA were well separated within only 80 s in a running buffer of 20 mM borate solution (pH 8.5). Good linearity was obtained within the concentration range of 2-200 microM for the three water-soluble vitamins. The detection limits were 1.0 microM for pyridoxine and VC, and 1.5 microM for PABA. The proposed method has been successfully applied to real human urine sample, without solid phase extraction, with recoveries of 80-122% for the three water-soluble vitamins.

  15. Ion Transport Function of SLC4A11 in Corneal Endothelium

    PubMed Central

    Jalimarada, Supriya S.; Ogando, Diego G.; Vithana, Eranga N.; Bonanno, Joseph A.

    2013-01-01

    Purpose. Mutations in SLC4A11, a member of the SLC4 superfamily of bicarbonate transporters, give rise to corneal endothelial cell dystrophies. SLC4A11 is a putative Na+ borate and Na+:OH− transporter. Therefore we ask whether SLC4A11 in corneal endothelium transports borate (B[OH]4−), bicarbonate (HCO3−), or hydroxyl (OH−) anions coupled to Na+. Methods. SLC4A11 expression in cultured primary bovine corneal endothelial cells (BCECs) was determined by semiquantitative PCR, SDS-PAGE/Western blotting, and immunofluorescence staining. Ion transport function was examined by measuring intracellular pH (pHi) or Na+ ([Na+]i) in response to Ringer solutions with/without B(OH)4− or HCO3− after overexpressing or small interfering RNA (siRNA) silencing of SLC4A11. Results. SLC4A11 is localized to the basolateral membrane in BCEC. B(OH)4− (2.5–10 mM) in bicarbonate-free Ringer induced a rapid small acidification (0.01 pH unit) followed by alkalinization (0.05–0.1 pH unit), consistent with diffusion of boric acid into the cell followed by B(OH)4−. However, the rate of B(OH)4−-induced pHi change was unaffected by overexpression of SLC4A11. B(OH)4− did not induce significant changes in resting [Na+i] or the amplitude and rate of acidification caused by Na+ removal. siRNA-mediated knockdown of SLC4A11 (∼70%) did not alter pHi responses to CO2/HCO3−-rich Ringer, Na+-free induced acidification, or the rate of Na+ influx in the presence of bicarbonate. However, in the absence of bicarbonate, siSLC4A11 knockdown significantly decreased the rate (43%) and amplitude (48%) of acidification due to Na+ removal and recovery (53%) upon add-back. Additionally, the rate of acid recovery following NH4+ prepulse was decreased significantly (27%) by SLC4A11 silencing. Conclusions. In corneal endothelium, SLC4A11 displays robust Na+-coupled OH− transport, but does not transport B(OH)4− or HCO3−. PMID:23745003

  16. Kinetic and Mechanistic Study of the pH-Dependent Activation (Epoxidation) of Prodrug Treosulfan Including the Reaction Inhibition in a Borate Buffer.

    PubMed

    Romański, Michał; Ratajczak, Whitney; Główka, Franciszek

    2017-07-01

    A prodrug treosulfan (T) undergoes a pH-dependent activation to epoxide derivatives. The process seems to involve an intramolecular Williamson reaction (IWR) but clear kinetic evidence is lacking. Moreover, a cis-diol system present in the T structure is expected to promote complexation with boric acid. As a result, the prodrug epoxidation would be inhibited; however, this phenomenon has not been investigated. In this article, the effect of pH on the kinetics of T conversion to its monoepoxide was studied from a mechanistic point of view. Also, the influence of boric acid on the reaction kinetics was examined. The rate constants observed for the activation of T (k obs ) in acetate, phosphate, and carbonate buffers satisfied the equation logk obs  = -7.48 + 0.96 pH. The reaction was inhibited in the excess of boric acid over T, and the k obs decreased with increasing borate buffer concentration. The experimental results were consistent with the inhibition model that included the formation of a tetrahedral, anionic T-boric acid monoester. To conclude, in nonborate buffers, the T activation to (2S,3S)-1,2-epoxybutane-3,4-diol 4-methanesulfonate follows IWR mechanism. A borate buffer changes the reaction kinetics and complicates kinetic analysis. Copyright © 2017 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  17. Free Available Chlorine Disinfection Criteria for Fixed Army Installation Primary Drinking Water

    DTIC Science & Technology

    1981-12-01

    Buffered Water with Fuivic Acid (5 C.U.) at pH 9 and 60C ............................................ 6. FAC Disinfection of f 2 Coliphage in Buffered Water ...with and without 250 mg/L -Ca+ at pH 5, 7, and 9 and 6°C ............... 31 10. FAC Disinfection of f 2 Coliphage in Water Containing 5 NTU Bentonite2...rngi L Ca+ 2 at pH- 5, 7, and q and 60C ...... ........................ 34 13. FAC Disinfection of f 2 Coliphage in Borate-Buffered Water with 250 mg

  18. Complexation of Nickel Ions by Boric Acid or (Poly)borates.

    PubMed

    Graff, Anais; Barrez, Etienne; Baranek, Philippe; Bachet, Martin; Bénézeth, Pascale

    2017-01-01

    An experiment based on electrochemical reactions and pH monitoring was performed in which nickel ions were gradually formed by oxidation of a nickel metal electrode in a solution of boric acid. Based on the experimental results and aqueous speciation modeling, the evolution of pH showed the existence of significant nickel-boron complexation. A triborate nickel complex was postulated at high boric acid concentrations when polyborates are present, and the equilibrium constants were determined at 25, 50 and 70 °C. The calculated enthalpy and entropy at 25 °C for the formation of the complex from boric acid and Ni 2+ ions are respectively equal to (65.6 ± 3.1) kJ·mol -1 and (0.5 ± 11.1) J·K -1 ·mol -1 . The results of this study suggest that complexation of nickel ions by borates can significantly enhance the solubility of nickel metal and nickel oxide depending on the concentration of boric acid and pH. First principles calculations were investigated and tend to show that the complex is thermodynamically stable and the nickel cation in solution should interact more strongly with the [Formula: see text] than with boric acid.

  19. Optode Membrane for Determination of Nicotine via Generation of Its Bromoethane Derivative.

    PubMed

    Choi, M M; Wu, X J; Li, Y R

    1999-04-01

    A plasticized poly(vinyl chloride) optode membrane incorporated with a valinomycin ionophore, a H(+)-selective chromoionophore (ETH 5294), and a lipophilic potassium tetrakis(4-chlorophenyl)borate was used as a reversible sensing device for the indirect optical determination of nicotine. Nicotine was extracted from a tobacco product (1-5 g) and converted to its bromoethane derivative (NBD(+)Br(-)) by reacting with a solution of bromoethane in ethanol. NBD(+)Br(-) in a solution of 0.05 M boric acid-Borax buffer and 0.2 mM Triton X-100 was extracted into the bulk of the membrane and subsequently caused changes in optical absorption of the sensing layer. The response slope, dynamic working range, detection limit, sensitivity, selectivity, effects of buffer solution and neutral surfactant Triton X-100, and lifetime were discussed in detail. The response was pH dependent. At pH 8.5, the detection range was extended from 0.4 μM to 1 mM. Typical response times (t(95)) of the samples were 2-4 min. The optode method was successfully used to detect nicotine in a tobacco sample from the market (average content 0.720%; RSD 0.044%; n = 11). The interference of K(+) on the optode method can be prevented by the pre-extraction procedure. Malic acid and citrate showed no interferences. The recovery of nicotine as NBD(+) was 84-119% in the range 0.035-5% nicotine. The result was satisfactory compared with an AOAC UV standard method.

  20. Observation of sum-frequency-generation-induced cascaded four-wave mixing using two crossing femtosecond laser pulses in a 0.1 mm beta-barium-borate crystal.

    PubMed

    Liu, Weimin; Zhu, Liangdong; Fang, Chong

    2012-09-15

    We demonstrate the simultaneous generation of multicolor femtosecond laser pulses spanning the wavelength range from UV to near IR in a 0.1 mm Type I beta-barium borate crystal from 800 nm fundamental and weak IR super-continuum white light (SCWL) pulses. The multicolor broadband laser pulses observed are attributed to two concomitant cascaded four-wave mixing (CFWM) processes as corroborated by calculation: (1) directly from the two incident laser pulses; (2) by the sum-frequency generation (SFG) induced CFWM process (SFGFWM). The latter signal arises from the interaction between the frequency-doubled fundamental pulse (400 nm) and the SFG pulse generated in between the fundamental and IR-SCWL pulses. The versatility and simplicity of this spatially dispersed multicolor self-compressed laser pulse generation offer compact and attractive methods to conduct femtosecond stimulated Raman spectroscopy and time-resolved multicolor spectroscopy.

  1. Separation of plant hormones from biofertilizer by capillary electrophoresis using a capillary coated dynamically with polycationic polymers.

    PubMed

    Jiang, Ting-Fu; Lv, Zhi-Hua; Wang, Yuan-Hong; Yue, Mei-E

    2006-06-01

    A new, simple and rapid capillary electrophoresis (CE) method, using hexadimethrine bromide (HDB) as electroosmotic flow (EOF) modifier, was developed for the identification and quantitative determination of four plant hormones, including gibberellin A3 (GA3), indole-3-acetic acid (IAA), alpha-naphthaleneacetic acid (NAA) and 4-chlorophenoxyacetic acid (4-CA). The optimum separation was achieved with 20 mM borate buffer at pH 10.00 containing 0.005% (w/v) of HDB. The applied voltage was -25 kV and the capillary temperature was kept constant at 25 degrees C. Salicylic acid was used as internal standard for quantification. The calibration dependencies exhibited good linearity within the ratios of the concentrations of standard samples and internal standard and the ratios of the peak areas of samples and internal standard. The correlation coefficients were from 0.9952 to 0.9997. The relative standard deviations of migration times and peak areas were < 1.93 and 6.84%, respectively. The effects of buffer pH, the concentration of HDB and the voltage on the resolution were studied systematically. By this method, the contents of plant hormone in biofertilizer were successfully determined within 7 min, with satisfactory repeatability and recovery.

  2. Microwave assisted synthesis of metal-organic framework MIL-101 nanocrystals as sorbent and pseudostationary phase in capillary electrophoresis for the separation of anthraquinones in environmental water samples.

    PubMed

    Liu, Yue; Hu, Jia; Li, Yan; Shang, Yun-Tao; Wang, Jia-Qi; Zhang, Ye; Wang, Zhong-Liang

    2017-10-01

    In this work, a CE method was developed to separate five anthraquinones: aloe-emodin, rhein, emodin, chrysophanol, and physcion. The CE method used a nano-sized metal organic framework MIL-101 (nMIL-101) as pseudostationary phase (PSP) and sorbent for dispersed particle extraction (DPE). The nMIL-101 was synthesized by microwave technique and was characterized by UV-vis, TEM, Zeta potential, X-ray diffraction spectrometry and micropore physisorption. In this method, anthraquinones were adsorbed by nMIL-101 of a fast kinetics within 10 min and then separated by CE. The CE conditions were optimized considering time, pH, buffer ionic strength, and nanoparticles concentration. The optimal CE condition is using 20 mM sodium borate buffer (pH 9.1) containing 15% methanol (v/v) and 400 mg/L nMIL-101 as additives within 8 min. The LODs varied from 24 to 57 μg/L, which were lower than those previously reported. Our method has been successfully applied to determine trace anthraquinones in environmental water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Crystal structure of a new polar borate Na{sub 2}Ce{sub 2}[BO{sub 2}(OH)][BO{sub 3}]{sub 2} · H{sub 2}O with isolated boron triangles

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

    Topnikova, A. P.; Belokoneva, E. L., E-mail: elbel@geol.msu.ru; Dimitrova, O. V.

    2016-11-15

    Crystals of a new polar borate Na{sub 2}Ce{sub 2}[BO{sub 2}(OH)][BO{sub 3}]{sub 2} · H{sub 2}O were prepared by hydrothermal synthesis. The crystals are orthorhombic, a = 7.2295(7) Å, b = 11.2523(8) Å, c = 5.1285(6) Å, Z = 2, sp. gr. C2mm (Amm2), R = 0.0253. The formula of the compound was derived from the structure determination. The Ce and Na atoms are coordinated by nine and six O atoms, respectively. The Ce position is split, and a small amount of Ce is incorporated into the Na1 site with the isomorphous substitution for Na. The anionic moieties exist as isolatedmore » BO{sub 3} and BO{sub 2}(OH) triangles. The planes of the BO{sub 2}(OH) triangles with mm2 symmetry are parallel to the ab plane. The planes of the BO{sub 3} triangles with m symmetry are perpendicular to the ab plane and are rotated in a diagonal way. The splitting of the Ce positions and the polar arrangement of the BO{sub 2}(OH) triangles, water molecules, and Na atoms are observed along the polar a axis. The new structure is most similar to the new borate NaCa{sub 4}[BO{sub 3}]{sub 3} (sp. gr. Ama2), in which triangles of one type are arranged in a polar fashion along the c axis. Weak nonlinear-optical properties of both polar borates are attributed to the quenching of the second-harmonic generation due to the mutually opposite orientation of two-thirds of B triangles in the unit cell.« less

  4. Capillary electrophoresis for caffeine and pyroglutamate determination in coffees study of the in vivo effect on learning and locomotor activity in mice.

    PubMed

    Maeso, N; del Castillo, C; Cornejo, L; García-Acicollar, M; Alguacil, L F; Barbas, C

    2006-06-16

    In a preliminary study pyroglutamate showed to be over 10 times increased in some lyophilised coffees with respect to brewed or filtered coffees, and probably that increase is related to some stage of the industrial process. Pyroglutamate is known to have a number of remarkable cognitive enhancing effects, which could be also related to the properties of coffee traditionally associated to caffeine. Pyroglutamate improves memory and learning and has anti-anxiety effects in rats. Therefore, a method has been developed and validated for the simultaneous determination of caffeine and pyroglutamate in coffee by capillary electrophoresis. Separation conditions employed MECK conditions with 50 mM borate buffer at pH 9.5 with 130 mM SDS. The applied potential was 10 kV and detection was performed at 200 nm. Afterwards, 10 soluble coffees from the market were measured and caffeine and pyroglutamate levels were compared. Those coffees with higher pyroglutamate with or without caffeine were preliminarily tested for sedative/stimulant properties and cognition enhancing effects in mice. The most relevant finding was a partial reversal of scopolamine-induced amnesia in the passive avoidance paradigm after oral administration of one coffee.

  5. Steric and electronic effects on arylthiolate coordination in the pseudotetrahedral complexes [(Tp(Ph,Me))Ni-SAr] (Tp(Ph,Me) = hydrotris{3-phenyl-5-methyl-1-pyrazolyl}borate).

    PubMed

    Deb, Tapash; Anderson, Caitlin M; Chattopadhyay, Swarup; Ma, Huaibo; Young, Victor G; Jensen, Michael P

    2014-12-14

    Synthesis and characterization of several new pseudotetrahedral arylthiolate complexes [(Tp(Ph,Me))Ni-SAr] (Tp(Ph,Me) = hydrotris{3-phenyl-5-methyl-1-pyrazolyl}borate; Ar = Ph, 2,4,6-(i)Pr3C6H2, C6H4-4-Cl, C6H4-4-Me, C6H4-4-OMe) are reported, including X-ray crystal structures of the first two complexes. With prior results, two series of complexes are spanned, [(Tp(Ph,Me))Ni-S-2,4,6-RC6H2] (R'' = H, Me, (i)Pr) plus the xylyl analogue [(Tp(Ph,Me))Ni-S-2,6-Me2C6H3], as well as [(Tp(Ph,Me))Ni-S-C6H4-4-Y] (Y = Cl, H, Me, OMe), intended to elucidate steric and/or electronic effects on arylthiolate coordination. In contrast to [(Tp(Me,Me))Ni-SAr] analogues that adopt a sawhorse conformation, the ortho-disubstituted complexes show enhanced trigonal and Ni-S-Ar bending, reflecting the size of the 3-pyrazole substituents. Moreover, weakened scorpionate ligation is implied by spectroscopic data. Little spectroscopic effect is observed in the series of para-substituted complexes, suggesting the observed effects are primarily steric in origin. The relatively electron-rich and encumbered complex [(Tp(Ph,Me))Ni-S-2,4,6-(i)Pr3C6H2] behaves uniquely when dissolved in CH3CN, forming a square planar solvent adduct with a bidentate scorpionate ligand, [(κ(2)-Tp(Ph,Me))Ni(NCMe)(S-2,4,6-(i)Pr3C6H2)]. This adduct was isolated and characterized by X-ray crystallography. Single-point DFT and TD-DFT calculations on a simplified [(κ(2)-Tp)Ni(NCMe)(SPh)] model were used to clarify the electronic spectrum of the adduct, and to elucidate differences between Ni-SAr bonding and spectroscopy between pseudotetrahedral and square planar geometries.

  6. Ytterbium-doped borate fluoride laser crystals and lasers

    DOEpatents

    Schaffers, Kathleen I.; DeLoach, Laura D.; Payne, Stephen A.; Keszler, Douglas A.

    1997-01-01

    A new class of solid state laser crystals and lasers are formed from Yb-doped borate fluoride host crystals. The general formula for the host crystals is MM'(BO.sub.3)F, where M, M' are monovalent, divalent aria trivalent metal cations. A particular embodiment of the invention is Yb-doped BaCaBO.sub.3 F (Yb:BCBF). BCBF and some of the related derivative crystals are capable of nonlinear frequency conversion, whereby the fundamental of the laser is converted to a longer or shorter wavelength. In this way, these new crystals can simultaneously serve as self-frequency doubling crystals and laser materials within the laser resonator.

  7. Investigations on Mg-borate kinetics and mechanisms during evaporation, dilution and crystallization by Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Peng, Jiaoyu; Chen, Jing; Dong, Yaping; Li, Wu

    2018-06-01

    Raman spectra of boron-concentrated, diluted, and corresponding mother solutions of brine were recorded at 298.15 K. The main polyborate anions present and their interactions in brine during evaporation and dilution were proposed according to the Raman spectra. The polyborate anions B(OH)3, B3O3(OH)4-, B5O6(OH)4-, and B6O7(OH)62- were found to be the main forms in boron-concentrated brine with B3O3(OH)4- ion being the principal form. Diluting brines with water accelerated depolymerization of B5O6(OH)4- and B6O7(OH)62- anions into B(OH)3 and B3O3(OH)4- ions and generated OH- ions, causing the pH of the solutions to increase from 4.2 to almost 8.0. Mg-borates precipitated from all diluted solutions could be classified as either hexaborates or triborates. A mechanism of solid phase transformation was also proposed and discussed based on Raman spectra analysis and solid species and solution pH data.

  8. Optimizing high-performance liquid chromatography method for quantification of glucosamine using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate derivatization in rat plasma: application to a pharmacokinetic study.

    PubMed

    Wang, Xianhuo; Chen, Xiang; Chen, Lijuan; Wang, Biqin; Peng, Cheng; He, Chunmei; Tang, Minghai; Zhang, Fan; Hu, Jia; Li, Rui; Zhao, Xia; Wei, Yuquan

    2008-11-01

    A sensitive and reliable HPLC method with fluorescence detection based on the precolumn derivatization of glucosamine with 6-aminoquinolyl-N-hydroxylsuccinimidyl carbamate (AQC) was established for the quantitative determination of glucosamine in rat plasma. The plasma protein was precipitated by acetonitrile, followed by vortex mixing and centrifugation. The supernatant was divided into the organic layer and aqueous layer by adding sodium chloride, and then the aqueous layer was derivatized with AQC in 0.2 M borate buffer of pH 8.8 before the HPLC analysis. An amino acid analysis column (3.9 x 150 mm, 4 microm) was applied, with 140 mM sodium acetate buffer (pH = 5.25) and acetonitrile as mobile phase at a flow rate of 1 mL/min. A linear correlation coefficient of 0.9987 was calculated within the range of 0.1-30 microg/mL of the standard curve for glucosamine. The limit of detection was 30 ng/mL. The intra- and inter-day precisions (as RSD) were less than 7.38 and 12.72%, respectively. The intra- and inter-day accuracy ranged from 91.8 to 110.0%. Extraction recoveries of glucosamine in plasma were more than 90%. The validated method was successfully applied for the quantitative determination of glucosamine in rat plasma and evaluation for pharmacokinetic study of glucosamine. It was also possible to be applied for the quantitative determination of other compounds containing amino group in biological samples.

  9. Ion-pair vortex assisted liquid-liquid microextraction with back extraction coupled with high performance liquid chromatography-UV for the determination of metformin in plasma.

    PubMed

    Alshishani, Anas; Makahleh, Ahmad; Yap, Hui Fang; Gubartallah, Elbaleeq Adam; Salhimi, Salizawati Muhamad; Saad, Bahruddin

    2016-12-01

    A new sample preparation method, ion-pair vortex assisted liquid-liquid microextraction (VALLME-BE), for the determination of a highly polar anti-diabetic drug (metformin) in plasma sample was developed. The VALLME-BE was performed by diluting the plasma in borate buffer and extracted to 150µL 1-octanol containing 0.2M di-(2-ethylhexyl)phosphoric acid as intermediate phase. The drug was next back-extracted into 20µL of 0.075M HCl solution. The effects of pH, ion-pair concentration, type of organic solvent, volume of extraction phases, ionic strength, vortexing and centrifugation times on the extraction efficiency were investigated. The optimum conditions were at pH 9.3, 60s vortexing and 2min centrifugation. The microextract, contained metformin and buformin (internal standard), was directly injected into a HPLC unit using C1 column (250mm×4.6mm×10µm) and detected at 235nm. The method was validated and calibration curve was linear with r 2 >0.99 over the range of 20-2000µgL -1 . The limits of detection and quantitation were 1.4 and 4.1µgL -1 , respectively. The accuracy was within 94.8-108% of the nominal concentration. The relative standard deviation for inter- and intra-day precision was less than 10.8%. The method was conveniently applied for the determination of metformin in plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Succinimidyl Ester Surface Chemistry: Implications of the Competition between Aminolysis and Hydrolysis on Covalent Protein Immobilization

    PubMed Central

    2015-01-01

    N-Hydroxysuccinimide (NHS) ester terminal groups are commonly used to covalently couple amine-containing biomolecules (e.g., proteins and peptides) to surfaces via amide linkages. This one-step aminolysis is often performed in buffered aqueous solutions near physiological pH (pH 6 to pH 9). Under these conditions, the hydrolysis of the ester group competes with the amidization process, potentially degrading the efficiency of the coupling chemistry. The work herein examines the efficiency of covalent protein immobilization in borate buffer (50 mM, pH 8.50) using the thiolate monolayer formed by the chemisorption of dithiobis (succinimidyl propionate) (DSP) on gold films. The structure and reactivity of these adlayers are assessed via infrared spectroscopy (IR), X-ray photoelectron spectroscopy (XPS), electrochemical reductive desorption, and contact angle measurements. The hydrolysis of the DSP-based monolayer is proposed to follow a reaction mechanism with an initial nucleation step, in contrast to a simple pseudo first-order reaction rate law for the entire reaction, indicating a strong dependence of the interfacial reaction on the packing and presence of defects in the adlayer. This interpretation is used in the subsequent analysis of IR-ERS kinetic plots which give a heterogeneous aminolysis rate constant, ka, that is over 3 orders of magnitude lower than that of the heterogeneous hydrolysis rate constant, kh. More importantly, a projection of these heterogeneous kinetic rates to protein immobilization suggests that under coupling conditions in which low protein concentrations and buffers of near physiological pH are used, proteins are more likely physically adsorbed rather than covalently linked. This result is paramount for biosensors that use NHS chemistry for protein immobilization due to effects that may arise from noncovalently linked proteins. PMID:25317495

  11. Modern bioanalysis of proteins by electrophoretic techniques.

    PubMed

    Krizkova, Sona; Ryvolova, Marketa; Masarik, Michal; Zitka, Ondrej; Adam, Vojtech; Hubalek, Jaromir; Eckschlager, Tomas; Kizek, Rene

    2014-01-01

    In 1957, protein rich in cysteine able to bind cadmium was isolated from horse kidney and named as metallothionein according to its structural properties. Further, this protein and metallothionein-like proteins have been found in tissues of other animal species, yeasts, fungi and plants. MT is as a potential cancer marker in the focus of interest, and its properties, functions, and behavior under various conditions are intensively studied. Our protocol describes separation of two major mammalian isoforms of MT (MT-1 and MT-2) using capillary electrophoresis (CE) coupled with UV detector. This protocol enables separation of MT isoforms and studying of their basic behavior as well as their quantification with detection limit in units of ng per μL. Sodium borate buffer (20 mM, pH 9.5) was optimized as a background electrolyte, and the separation was carried out in fused silica capillary with internal diameter of 75 μm and electric field intensity of 350 V/cm. Optimal detection wavelength was 254 nm.

  12. Ytterbium-doped borate fluoride laser crystals and lasers

    DOEpatents

    Schaffers, K.I.; DeLoach, L.D.; Payne, S.A.; Keszler, D.A.

    1997-10-14

    A new class of solid state laser crystals and lasers are formed from Yb-doped borate fluoride host crystals. The general formula for the host crystals is MM{prime}(BO{sub 3})F, where M, M{prime} are monovalent, divalent aria trivalent metal cations. A particular embodiment of the invention is Yb-doped BaCaBO{sub 3}F (Yb:BCBF). BCBF and some of the related derivative crystals are capable of nonlinear frequency conversion, whereby the fundamental of the laser is converted to a longer or shorter wavelength. In this way, these new crystals can simultaneously serve as self-frequency doubling crystals and laser materials within the laser resonator. 6 figs.

  13. Experimental Evaluation of pH and Temperature Effects on the Adsorption of Boron onto Clay Minerals

    NASA Astrophysics Data System (ADS)

    Hoenisch, B.; Marone, D.; Ruprecht, J.

    2017-12-01

    Modeling the secular evolution of the concentration [B] and isotopic composition (δ11B) of boron in seawater is hampered by limited constraints on the relative sources (i.e. riverine input of weathering products, hydrothermal convection at mid-ocean ridges and fluids expelled from accretionary prisms) and sinks (i.e. alteration of the oceanic crust, adsorption onto clays, and co-precipitation in carbonates) of boron to and from the ocean. Clays remove approximately 28% of total boron from the ocean and quantification of this sink thus represents a major factor for reconstructing the secular evolution of seawater [B] and δ11B over the Cenozoic. However, the relative strength of the clay sink could have been much smaller in the early Cenozoic compared to today, because borate ion as the charged species is preferentially adsorbed onto detrital clays over boric acid, and because the relative abundance of borate in seawater should have been lower under the more acidic conditions of the early Cenozoic. In addition, different clay minerals tend to fractionate boron isotopes differentially, and the relative composition of clay minerals has varied in the past with the dominant climate and weathering patterns on the continents. We have conducted a range of pH (7.5-8.4) and temperature (3-32°C) experiments with four clay minerals (Kaolinite, Illite, Montmorillonite and Chlorite), to build on previously published but limited experimental data. Similar to a previous study and as expected based on the relative abundance of borate ion in seawater, boron adsorption onto these clays increases at higher pH and lower temperatures, but whereas Montmorillonite and Illite absorb similar quantities of boron, Kaolinite is most and Chlorite least efficient in this process. We are now in the process of characterizing the boron isotope fractionation associated with these adsorption experiments.

  14. Ferromagnetic resonance in a single crystal of iron borate and magnetic field tuning of hybrid oscillations in a composite structure with a dielectric: Experiment and theory

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

    Popov, M. A.; Zavislyak, I. V.; Chumak, H. L.

    2015-07-07

    The high-frequency properties of a composite resonator comprised single crystal iron borate (FeBO{sub 3}), a canted antiferromagnet with a weak ferromagnetic moment, and a polycrystalline dielectric were investigated at 9–10 GHz. Ferromagnetic resonance in this frequency range was observed in FeBO{sub 3} for bias magnetic fields of ∼250 Oe. In the composite resonator, the magnetic mode in iron borate and dielectric mode are found to hybridize strongly. It is shown that the hybrid mode can be tuned with a static magnetic field. Our studies indicate that coupling between the magnetic mode and the dielectric resonance can be altered from maximum hybridization tomore » a minimum by adjusting the position of resonator inside the waveguide. Magnetic field tuning of the resonance frequency by a maximum of 145 MHz and a change in the transmitted microwave power by as much as 16 dB have been observed for a bias field of 250 Oe. A model is discussed for the magnetic field tuning of the composite resonator and theoretical estimates are in reasonable agreement with the data. The composite resonator with a weak ferromagnet and a dielectric is of interest for application in frequency agile devices with electronically tunable electrodynamic characteristics for the mm and sub-mm wave bands.« less

  15. Catalytic copolymerization of CO and ethylene with a charge neutral palladium(II) zwitterion.

    PubMed

    Lu, Connie C; Peters, Jonas C

    2002-05-15

    The synthesis of a zwitterionic Pd(II) complex supported by an anionic bis(phosphino)borate ligand, Ph(2)B(CH(2)PPh(2))(2) (abbreviated as [Ph(2)BP(2)]), is reported. The new complex, [Ph(2)BP(2)]PdMe(THF), is active for CO and ethylene copolymerization. The copolymerization activity and polyketone molecular weight for the neutral, zwitterionic system are compared with those for the cationic systems [R(2)E(CH(2)PPh(2))(2)PdMe(THF)][B(C(6)F(5))(4)] where ER(2) = SiPh(2) and CH(2). Surprisingly, the more electron rich zwitterionic system is a catalyst of activity comparable to that of the more conventional cationic systems.

  16. Characterization of the Terminal Iron(IV) Imides {[PhBPtBu2(pz’)]FeIV≡NAd}+

    PubMed Central

    Thomas, Christine M.; Mankad, Neal P.; Peters, Jonas C.

    2008-01-01

    New hybrid bis(phosphine)(pyrazole)borate tripodal ligands ([PhBPtBu2(pz’)]−) are reported that support pseudotetrahedral iron in the oxidation states +1, +2, +3, and +4. The higher oxidation states are stabilized by a terminal Fe≡NR linkage. Of particular interest is the generation and thorough characterization of an S = 1 FeIV≡NR+ imide cation using this new ligand system. The latter species can be observed electrochemically and spectroscopically, and its solid-state crystal structure is reported. PMID:16608321

  17. Effect of Gamma Radiation on Absorption of Light in Potassium-Aluminoborate Glasses with Additions of Iron Oxide

    NASA Astrophysics Data System (ADS)

    Ibragimova, E. M.; Salakhitdinov, A. N.; Salakhitdinova, M. K.; Yusupov, A. A.

    2018-05-01

    The effect of radiation on the absorption of light by potassium-alumina-borate glasses with various concentrations of iron additions and various thicknesses was investigated. It was shown that in contrast to samples of small thickness (1 mm) a bleaching effect was observed in the samples with a thickness of 8 mm. A possible mechanism involving the formation of nanostructured units is proposed for the observed effect.

  18. Simple luminescence detectors using a light-emitting diode or a Xe lamp, optical fiber and charge-coupled device, or photomultiplier for determining proteins in capillary electrophoresis: a critical comparison.

    PubMed

    Casado-Terrones, Silvia; Fernández-Sánchez, Jorge F; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto

    2007-06-01

    The performance of two homemade fluorescence-induced capillary electrophoresis detectors, one based on light-emitting diode (LED) as the excitation source and a charge-coupled device (CCD) photodetector and the other based on a commercial luminescence spectrometer (Xe lamp) as the excitation source and a photomultiplier tube as a detector, were compared for the determination of fluorescent proteins R-phycoerythrin and B-phycoerythrin. Both devices use commercially available, reasonably priced optical components that can be used by nonexperts. After fine optimization of several optical and separation parameters in both devices, a zone capillary electrophoresis methodology was achieved with 50mM borate buffer (pH 8.4) and 10mM phytic acid for the determination of two phycobiliproteins. Detection limits of 0.50 and 0.64microg/ml for R-phycoerythrin and B-phycoerythrin, respectively, were achieved by using the LED-induced fluorescence capillary electrophoresis (LED-IF-CE) system, and corresponding detection limits of 2.73 and 2.16microg/ml were achieved by using the Xe lamp-IF-CE system. Analytical performance and other parameters, such as cost and potential to miniaturization, are compared for both devices.

  19. Evaluation of a molecularly imprinted polymer for determination of steroids in goat milk by matrix solid phase dispersion.

    PubMed

    Gañán, Judith; Morante-Zarcero, Sonia; Gallego-Picó, Alejandrina; Garcinuño, Rosa María; Fernández-Hernando, Pilar; Sierra, Isabel

    2014-08-01

    A molecularly imprinted polymer-matrix solid-phase dispersion methodology for simultaneous determination of five steroids in goat milk samples was proposed. Factors affecting the extraction recovery such as sample/dispersant ratio and washing and elution solvents were investigated. The molecularly imprinted polymer used as dispersant in the matrix solid-phase dispersion procedure showed high affinity to steroids, and the obtained extracts were sufficiently cleaned to be directly analyzed. Analytical separation was performed by micellar electrokinetic chromatography using a capillary electrophoresis system equipped with a diode array detector. A background electrolyte composed of borate buffer (25mM, pH 9.3), sodium dodecyl sulfate (10mM) and acetonitrile (20%) was used. The developed MIP-MSPD methodology was applied for direct determination of testosterone (T), estrone (E1), 17β-estradiol (17β-E2), 17α-ethinylestradiol (EE2) and progesterone (P) in different goat milk samples. Mean recoveries obtained ranged from 81% to 110%, with relative standard deviations (RSD)≤12%. The molecularly imprinted polymer-matrix solid-phase dispersion method is fast, selective, cost-effective and environment-friendly compared with other pretreatment methods used for extraction of steroids in milk. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Micellar electrokinetic capillary chromatographic method for the quantitative analysis of uricosuric and antigout drugs in pharmaceutical preparations.

    PubMed

    Kou, Hwang-Shang; Lin, Tsai-Pei; Chung, Tang-Chia; Wu, Hsin-Lung

    2006-06-01

    A simple MEKC method is described for the separation and quantification of seven widely used uricosuric and antigout drugs, including allopurinol (AP), benzbromarone (BZB), colchicine (COL), orotic acid (OA), oxypurinol (OP), probenecid (PB), and sulfinpyrazone (SPZ). The drugs were separated in a BGE of borate buffer (45 mM; pH 9.00) with SDS (20 mM) as the micellar source and the separated drugs were directly monitored with a UV detector (214 nm). Several parameters affecting the separation and analysis of the drugs were studied. Based on the normalized peak-area ratios of the drugs to an internal standard versus the concentration of the drugs, the method is applicable to quantify BZB, COL, and SPZ (each 5-200 microM), AP, OA, OP, and PB (each 10-200 microM) with detection limits (S/N = 3, 0.5 psi, 5 s injection) in the range of 0.6-4.0 microM. The precision (RSD; n = 5) and accuracy (relative error; n = 5) of the method for intraday and interday analyses of the analytes at three levels (30, 120, and 180 microM) are below 4% (n = 3). The method was demonstrated to be suitable for the analysis of AP and COL in commercial tablets with speed and simplicity.

  1. Investigation of inorganic nonlinear optical potassium penta borate tetra hydrate (PPBTH) single crystals grown by slow evaporation method

    NASA Astrophysics Data System (ADS)

    Arivuselvi, R.; Babu, P. Ramesh

    2018-03-01

    Borates family crystals were plays vital role in the field of non linear optics (NLO) due to needs of wide range of applications. In this report, NLO crystals (potassium penta borate tetra hydrate (KB5H8O12) are grown by slow evaporation method at room temperature (28° C) and studied their physical properties. The harvested single crystals are transparent with the dimension of 12 × 10 × 6 mm3 and colourless. X-ray diffraction of single crystals reveals that the grown crystal belongs to orthorhombic system with non-centrosymmetric space group Pba2. All the absorbed functional groups are present in the order of inorganic compounds expect 1688 cm-1 because of water (Osbnd H sbnd O blending) molecule present in the pristine. Crystals show transparent in the entire visible region with 5.9 eV optical band gap and also it shows excellence in both second and third order nonlinear optical properties. Crystals can withstand upto 154 °C without any phase changes which is observed using thermal (TGA/DTA) analysis.

  2. Striking Effects of Storage Buffers on Apparent Half-Lives of the Activity of Pseudomonas aeruginosa Arylsulfatase.

    PubMed

    Li, Yuwei; Yang, Xiaolan; Wang, Deqiang; Hu, Xiaolei; Yuan, Mei; Pu, Jun; Zhan, Chang-Guo; Yang, Zhaoyong; Liao, Fei

    2016-08-01

    To obtain the label enzyme for enzyme-linked-immunoabsorbent-assay of two components each time in one well with conventional microplate readers, molecular engineering of Pseudomonas aeruginosa arylsulfatase (PAAS) is needed. To compare thermostability of PAAS/mutants of limited purity, effects of buffers on the half-activity time (t 0.5) at 37 °C were tested. At pH 7.4, PAAS showed non-exponential decreases of activity, with the apparent t 0.5 of ~6.0 days in 50 mM HEPES, but ~42 days in 10 mM sodium borate with >85 % activity after 15 days; protein concentrations in both buffers decreased at slower rates after there were significant decreases of activities. Additionally, the apparent t 0.5 of PAAS was ~14 days in 50 mM Tris-HCl, and ~21 days in 10 mM sodium phosphate. By sodium dodecyl-polyacrylamide gel electrophoresis, the purified PAAS gave single polypeptide; after storage for 14 days at 37 °C, there were many soluble and insoluble fragmented polypeptides in the HEPES buffer, but just one principal insoluble while negligible soluble fragmented polypeptides in the borate buffer. Of tested mutants in the neutral borate buffer, rates for activity decreases and polypeptide degradation were slower than in the HEPES buffer. Hence, dilute neutral borate buffers were favorable for examining thermostability of PAAS/mutants.

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

    Esswein, AJ; Surendranath, Y; Reece, SY

    A high surface area electrode is functionalized with cobalt-based oxygen evolving catalysts (Co-OEC = electrodeposited from pH 7 phosphate, Pi, pH 8.5 methylphosphonate, MePi, and pH 9.2 borate electrolyte, Bi). Co-OEC prepared from MePi and operated in Pi and Bi achieves a current density of 100 mA cm(-2) for water oxidation at 442 and 363 mV overpotential, respectively. The catalyst retains activity in near-neutral pH buffered electrolyte in natural waters such as those from the Charles River (Cambridge, MA) and seawater (Woods Hole, MA). The efficacy and ease of operation of anodes functionalized with Co-OEC at appreciable current density togethermore » with its ability to operate in near neutral pH buffered natural water sources bodes well for the translation of this catalyst to a viable renewable energy storage technology.« less

  4. Functional magnetic microspheres

    NASA Technical Reports Server (NTRS)

    Rembaum, Alan (Inventor); Landel, Robert F. (Inventor); Yen, Shiao-Ping S. (Inventor)

    1981-01-01

    Functional magnetic particles are formed by dissolving a mucopolysaccharide such as chitosan in acidified aqueous solution containing a mixture of ferrous chloride and ferric chloride. As the pH of the solution is raised magnetite is formed in situ in the solution by raising the pH. The dissolved chitosan is a polyelectrolyte and forms micelles surrounding the granules at pH of 8-9. The chitosan precipitates on the granules to form microspheres containing the magnetic granules. On addition of the microspheres to waste aqueous streams containing dissolved ions, the hydroxyl and amine functionality of the chitosan forms chelates binding heavy metal cations such as lead, copper, and mercury and the chelates in turn bind anions such as nitrate, fluoride, phosphate and borate.

  5. Interfacing Capillary-Based Separations to Mass Spectrometry Using Desorption Electrospray Ionization

    PubMed Central

    Barbula, Griffin K.; Safi, Samir; Chingin, Konstantin; Perry, Richard H.; Zare, Richard N.

    2014-01-01

    The powerful hybrid analysis method of capillary-based separations followed by mass spectrometric analysis gives substantial chemical identity and structural information. It is usually carried out using electrospray ionization. However, the salts and detergents used in the mobile phase for electrokinetic separations suppress ionization efficiencies and contaminate the inlet of the mass spectrometer. This report describes a new method that uses desorption electrospray ionization (DESI) to overcome these limitations. Effluent from capillary columns is deposited on a rotating Teflon disk that is covered with paper. As the surface rotates, the temporal separation of the eluting analytes (i.e., the electropherogram) is spatially encoded on the surface. Then, using DESI, surface-deposited analytes are preferentially ionized, reducing the effects of ion suppression and inlet contamination on signal. With the use of this novel approach, two capillary-based separations were performed: a mixture of the rhodamine dyes at milligram/milliliter levels in a 10 mM sodium borate solution was separated by capillary electrophoresis, and a mixture of three cardiac drugs at milligram/milliliter levels in a 12.5 mM sodium borate and 12.5 mM sodium dodecyl sulfate solution was separated by micellar electrokinetic chromatography. In both experiments, the negative effects of detergents and salts on the MS analyses were minimized. PMID:21319740

  6. Host responses to a strontium releasing high boron glass using a rabbit bilateral femoral defect model.

    PubMed

    O'Connell, Kathleen; Pierlot, Caitlin; O'Shea, Helen; Beaudry, Diane; Chagnon, Madeleine; Assad, Michel; Boyd, Daniel

    2017-10-01

    Borate glasses have shown promising potential as bioactive materials. With recent research demonstrating that glass properties may be modulated by appropriate compositional design. This may provide for indication specific material characteristics and controlled release of therapeutic inorganic ions (i.e., strontium); controlling such release is critical in order to harness the therapeutic potential. Within this sub-chronic pilot study, a rabbit long-bone model was utilized to explore the safety and efficacy of a high borate glass (LB102: 70B 2 O 3 -20SrO-6Na 2 O-4La 2 O 3 ) particulate (90 - 710 μm) for bone regeneration. Six bilateral full-thickness defects (Ø = 3.5 mm; L = 8 mm) were created in three white New Zealand rabbits. Longitudinal non-decalcified sections of each defect site were produced and stained with Goldner's Trichrome. Histopathological examination revealed that LB102 demonstrated osteoconductive and osseointegrative properties with greater new bone being formed within and surrounding LB102 particles, when compared to the sham control. The inflammatory cell infiltration was observed to be slightly higher in the control when compared to LB102 defect sites, while no significant difference in fibrosis and neovascularization was determined, indicating that healing was occurring in a normal fashion. These data further suggest the possible utility of high borate glasses with appropriate compositional design for medical applications, such as bone augmentation. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 1818-1827, 2017. © 2016 Wiley Periodicals, Inc.

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

    Paajanen, A.; Lehto, J.; Santapakka, T.

    The efficiencies of 15 commercially available activated carbons were tested for the separation of trace cobalt ({sup 60}Co) in buffer solutions at pH 5.0, 6.7, and 9.1. On the basis of the results four carbon products, Diahope-006, Eurocarb TN5, Hydraffin DG47, and Norit ROW Supra, were selected for further study. These carbons represented varying (low, medium and high) cobalt removal efficiencies and were prepared of three typical raw materials: peat, coconut shell, or coal. Study was made of the effects on sorption efficiencies of factors of interest in metal/radionuclide-bearing waste effluents. These factors were pH, sodium ions, borate, and citrate.

  8. A novel high sensitivity HPLC assay for topiramate, using 4-chloro-7-nitrobenzofurazan as pre-column fluorescence derivatizing agent.

    PubMed

    Bahrami, Gholamreza; Mohammadi, Bahareh

    2007-05-01

    A new, sensitive and simple high-performance liquid chromatographic method for analysis of topiramate, an antiepileptic agent, using 4-chloro-7-nitrobenzofurazan as pre-column derivatization agent is described. Following liquid-liquid extraction of topiramate and an internal standard (amlodipine) from human serum, derivatization of the drugs was performed by the labeling agent in the presence of dichloromethane, methanol, acetonitrile and borate buffer (0.05 M; pH 10.6). A mixture of sodium phosphate buffer (0.05 M; pH 2.4): methanol (35:65 v/v) was eluted as mobile phase and chromatographic separation was achieved using a Shimpack CLC-C18 (150 x 4.6 mm) column. In this method the limit of quantification of 0.01 microg/mL was obtained and the procedure was validated over the concentration range of 0.01 to 12.8 microg/mL. No interferences were found from commonly co-administrated antiepileptic drugs including phenytoin, phenobarbital carbamazepine, lamotrigine, zonisamide, primidone, gabapentin, vigabatrin, and ethosuximide. The analysis performance was carried-out in terms of specificity, sensitivity, linearity, precision, accuracy and stability and the method was shown to be accurate, with intra-day and inter-day accuracy from -3.4 to 10% and precise, with intra-day and inter-day precision from 1.1 to 18%.

  9. Photon Interaction Parameters for Some Borate Glasses

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

    Mann, Nisha; Kaur, Updesh; Singh, Tejbir

    2010-11-06

    Some photon interaction parameters of dosimetric interest such as mass attenuation coefficients, effective atomic number, electron density and KERMA relative to air have been computed in the wide energy range from 1 keV to 100 GeV for some borate glasses viz. barium-lead borate, bismuth-borate, calcium-strontium borate, lead borate and zinc-borate glass. It has been observed that lead borate glass and barium-lead borate glass have maximum values of mass attenuation coefficient, effective atomic number and KERMA relative to air. Hence, these borate glasses are suitable as gamma ray shielding material, packing of radioactive sources etc.

  10. Factors Affecting the Tunneling Behavior of the Western Subterranean Termite, Reticulitermes Hesperus Banks

    Treesearch

    James L. Smith; Michael K. Rust

    1991-01-01

    Laboratory studies were conducted to determine factors that affect the tunneling behavior of the western subterranean termite (Reticulitermes hesperus Banks). Soil particle sizes between 2.36 and 0.84 mm prevented tunneling. Exposure to solid layers of calcium, magnesium, or zinc borate did not repel workers, but produced >87 percent kill...

  11. Carbon nanotube/poly(ethylene-co-vinyl acetate) composite electrode for capillary electrophoretic determination of esculin and esculetin in Cortex Fraxini.

    PubMed

    Chen, Zhi; Zhang, Luyan; Chen, Gang

    2009-10-01

    In this report, a novel carbon nanotube/poly(ethylene-co-vinyl acetate) (CNT/EVA) composite electrode was developed for the amperometric detection in CE. The composite electrode was fabricated by packing a mixture of CNTs and melted EVA in a piece of fused-silica capillary under heat. It was coupled with CE for the separation and detection of esculin and esculetin in Cortex Fraxini, a traditional Chinese medicine, to demonstrate its feasibility and performance. Esculin and esculetin have been well separated within 9 min in a 40 cm long capillary at a separation voltage of 12 kV using a 50 mM borate buffer (pH 9.2). The new CNT-based CE detector offered significantly lower detection potentials, yielded enhanced S/N characteristics, and exhibited high resistance to surface fouling and enhanced stability. It showed long-term stability and reproducibility with relative standard deviations of less than 5% for the peak current (n=15) and should also find a wide range of applications in other microfluidic analysis systems.

  12. Analysis of compositional monosaccharides in fungus polysaccharides by capillary zone electrophoresis.

    PubMed

    Hu, Yuanyuan; Wang, Tong; Yang, Xingbin; Zhao, Yan

    2014-02-15

    A rapid analytical method of capillary zone electrophoresis (CZE) was established for the simultaneous separation and determination of 10 monosaccharides (aldoses and uronic acids). The monosaccharides were labeled with 1-phenyl-3-methyl-5-pyrazolone (PMP), and subsequently separated using an uncoated capillary (50 μm i.d. × 58.5 cm) and detected by UV at 245 nm with pH 11.0, 175 mM borate buffer at voltage 20 kV and capillary temperature 25 °C by CZE. The 10 PMP-labeled monosaccharides were rapidly baseline separated within 20 min. The optimized CZE method was successfully applied to the simultaneous separation and identification of the monosaccharide composition in Termitomyces albuminosus polysaccharides (TAPs) and Panus giganteus polysaccharides (PGPs). The quantitative recovery of the component monosaccharides in the fungus polysaccharides was in the range of 92.0-101.0% and the CV value was lower than 3.5%. The results demonstrate that the proposed CZE method is precise and practical for the monosaccharide analysis of fungus polysaccharides. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Rapid sample screening method for authenticity controlling vanilla flavors using a CE microchip approach with electrochemical detection.

    PubMed

    Avila, Mónica; González, María Cristina; Zougagh, Mohammed; Escarpa, Alberto; Ríos, Angel

    2007-11-01

    Five vanilla-related flavors of food significance, vanillic alcohol (VOH), ethyl maltol (EMA), maltol (MAL), ethyl vanillin (EVA) and vanillin (VAN), were separated using CE microchips with electrochemical detection (CE-ED microchips). A +2 kV driving voltage for both injection and separation operation steps, using a borate buffer (pH 9.5, 20 mM) and 1 M nitric acid in the detection reservoir allowed the selective and sensitive detection of the target analytes in less than 200 s with reproducible control of EOF (RSD(migration times)<3%). The analysis in selected real vanilla samples was focusing on VAN and EVA because VAN is a basic fragrance compound of the vanilla aroma, whereas EVA is an unequivocal proof of adulteration of vanilla flavors. Fast detection of all relevant flavors (200 s) with an acceptable resolution (R(s) >1.5) and a high accuracy (recoveries higher than 90%) were obtained with independence of the matrices and samples examined. These results showed the reliability of the method and the potential use of CE microchips in the food control field for fraudulent purposes.

  14. Fast and simultaneous detection of prominent natural antioxidants using analytical microsystems for capillary electrophoresis with a glassy carbon electrode: a new gateway to food environments.

    PubMed

    Blasco, Antonio Javier; Barrigas, Inés; González, María Cristina; Escarpa, Alberto

    2005-12-01

    This paper examines for the first time the analytical possibilities of fast and simultaneous detection of prominent natural antioxidants including examples of flavonoids and vitamins using a CE microchip with electrochemical detection (ED). Unpinched injection conditions, zone electrophoretic separation and amperometric detection were carefully assayed and optimised. Analysis involved the zone electrophoretic separation of arbutin, (+)-catechin and ascorbic acid in less than 4 min using a borate buffer (pH 9.0, 50 mM), employing 2 kV as the separation voltage and +1.0 V as the detection potential. In addition, the separation of different 'couples' of natural antioxidants of food significance including (+)-catechin and ascorbic acid, (+)-catechin and rutin, as well as arbutin and phlorizdin is proposed. To demonstrate the potential and future role of CE microsystems, analytical possibilities and a new route in the raw sample analysis are presented. The preliminary results obtained allow the proposal of CE-ED microchips as a real gateway to microanalysis in foods.

  15. Elution characteristics of teicoplanin-loaded biodegradable borate glass/chitosan composite.

    PubMed

    Jia, Wei-Tao; Zhang, Xin; Zhang, Chang-Qing; Liu, Xin; Huang, Wen-Hai; Rahaman, Mohamed N; Day, Delbert E

    2010-03-15

    Local antibiotic delivery system has an advantage over systemic antibiotic for osteomyelitis treatment due to the delivery of high local antibiotic concentration while avoiding potential systemic toxicity. Composite biomaterials with multifunctional roles, consisting of a controlled antibiotic release, a mechanical (load-bearing) function, and the ability to promote bone regeneration, gradually become the most active area of investigation and development of local antibiotic delivery vehicles. In the present study, a composite of borate glass and chitosan (designated BG/C) was developed as teicoplanin delivery vehicle. The in vitro elution kinetics and antibacterial activity of teicoplanin released from BG/C composite as a function of immersion time were determined. Moreover, the pH changes of eluents and the bioactivity of the composite were characterized using scanning electron microscopy coupled with energy-dispersive spectroscopy and X-ray diffraction analysis. 2009 Elsevier B.V. All rights reserved.

  16. Development of a microchip-pulsed electrochemical method for rapid determination of L-DOPA and tyrosine in Mucuna pruriens.

    PubMed

    Li, Xinchun; Chen, Zuanguang; Yang, Fan; Pan, Jianbin; Li, Yinbao

    2013-05-01

    L-3,4-dihydroxyphenylalanine (L-DOPA) is a well-recognized therapeutic compound to Parkinson's disease. Tyrosine is a precursor for the biosynthesis of L-DOPA, both of which are widely found in traditional medicinal material, Mucuna pruriens. In this paper, we described a validated novel analytical method based on microchip capillary electrophoresis with pulsed electrochemical detection for the simultaneous measurement of L-DOPA and tyrosine in M. pruriens. This protocol adopted end-channel amperometric detection using platinum disk electrode on a homemade glass/polydimethylsiloxane electrophoresis microchip. The background buffer consisted of 10 mM borate (pH 9.5) and 0.02 mM cetyltrimethylammonium bromide, which can produce an effective resolution for the two analytes. In the optimal condition, sufficient electrophoretic separation and sensitive detection for the target analytes can be realized within 60 s. Both tyrosine and L-DOPA yielded linear response in the concentration range of 5.0-400 μM (R(2) > 0.99), and the LOD were 0.79 and 1.1 μM, respectively. The accuracy and precision of the established method were favorable. The present method shows several merits such as facile apparatus, high speed, low cost and minimal pollution, and provides a means for the pharmacologically active ingredients assay in M. pruriens. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Quantitative and qualitative optimization of allergen extraction from peanut and selected tree nuts. Part 2. Optimization of buffer and ionic strength using a full factorial experimental design.

    PubMed

    L'Hocine, Lamia; Pitre, Mélanie

    2016-03-01

    A full factorial design was used to assess the single and interactive effects of three non-denaturing aqueous (phosphate, borate, and carbonate) buffers at various ionic strengths (I) on allergen extractability from and immunoglobulin E (IgE) immunoreactivity of peanut, almond, hazelnut, and pistachio. The results indicated that the type and ionic strength of the buffer had different effects on protein recovery from the nuts under study. Substantial differences in protein profiles, abundance, and IgE-binding intensity with different combinations of pH and ionic strength were found. A significant interaction between pH and ionic strength was observed for pistachio and almond. The optimal buffer system conditions, which maximized the IgE-binding efficiency of allergens and provided satisfactory to superior protein recovery yield and profiles, were carbonate buffer at an ionic strength of I=0.075 for peanut, carbonate buffer at I=0.15 for almond, phosphate buffer at I=0.5 for hazelnut, and borate at I=0.15 for pistachio. The buffer type and its ionic strength could be manipulated to achieve the selective solubility of desired allergens. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

  18. Kinetics and mechanisms of the conversion of silicate (45S5), borate, and borosilicate glasses to hydroxyapatite in dilute phosphate solutions.

    PubMed

    Huang, Wenhai; Day, Delbert E; Kittiratanapiboon, Kanisa; Rahaman, Mohamed N

    2006-07-01

    Bioactive glasses with controllable conversion rates to hydroxyapatite (HA) may provide a novel class of scaffold materials for bone tissue engineering. The objective of the present work was to comprehensively characterize the conversion of a silicate bioactive glass (45S5), a borate glass, and two intermediate borosilicate glass compositions to HA in a dilute phosphate solution at 37 degrees Celsius. The borate glass and the borosilicate glasses were derived from the 45S5 glass by fully or partially replacing the SiO(2) with B(2)O(3). Higher B(2)O(3) content produced a more rapid conversion of the glass to HA and a lower pH value of the phosphate solution. Whereas the borate glass was fully converted to HA in less than 4 days, the silicate (45S5) and borosilicate compositions were only partially converted even after 70 days, and contained residual SiO(2) in a Na-depleted core. The concentration of Na(+) in the phosphate solution increased with reaction time whereas the PO(4) (3-) concentration decreased, both reaching final limiting values at a rate that increased with the B(2)O(3) content of the glass. However, the Ca(2+) concentration in the solution remained low, below the detection limit of atomic absorption, throughout the reaction. Immersion of the glasses in a mixed solution of K(2)HPO(4) and K(2)CO(3) produced a carbonate-substituted HA but the presence of the K(2)CO(3) had little effect on the kinetics of conversion to HA. The kinetics and mechanisms of the conversion process of the four glasses to HA are compared and used to develop a model for the process.

  19. Synthesis and evaluation of borates derived from boric acid and diols for the protection of wood against fungal decay and thermal degradation

    Treesearch

    George C. Chen

    2004-01-01

    N,N-dimethyl amino carbinol catechol borate(1). N,N-dimethyl amino carbinol-4-methyl catechol borate(2), N,N-dimethyl amino carbinol-4-t- butyl catechol borate(3). N,N-dimethyl amino carbinol-2,3-naphthyl borate 4) were synthesized by refluxing boric acid and diol in DMF(N,N-dimethyl formamide). The borates were characterized by NMR. Wood impregnated with borate 1,2 or...

  20. Simultaneous determination of anthraquinones, their 8-beta-D-glucosides, and sennosides of Rhei Rhizoma by capillary electrophoresis.

    PubMed

    Koyama, Junko; Morita, Izumi; Fujiyoshi, Hirotaka; Kobayashi, Norihiro

    2005-05-01

    The simultaneous separation and determination of major anthraquinones (emodin, chrysophanol, rhein and their glucosides, aloe-emodin, sennoside A, and sennoside B) of Rhei Rhizoma were achieved by cyclodextrin modified capillary zone electrophoresis. The running electrolyte used in this method was 0.005 M alpha-cyclodextrin in 0.03 M borate buffer (pH 10.0) containing 20% acetonitrile, with an applied voltage of 20 kV.

  1. Separation of 20 coumarin derivatives using the capillary electrophoresis method optimized by a series of Doehlert experimental designs.

    PubMed

    Woźniakiewicz, Michał; Gładysz, Marta; Nowak, Paweł M; Kędzior, Justyna; Kościelniak, Paweł

    2017-05-15

    The aim of this study was to develop the first CE-based method enabling separation of 20 structurally similar coumarin derivatives. To facilitate method optimization a series of three consequent Doehlert experimental designs with the response surface methodology was employed, using number of peaks and the adjusted time of analysis as the selected responses. Initially, three variables were examined: buffer pH, ionic strength and temperature (No. 1 Doehlert design). The optimal conditions provided only partial separation, on that account, several buffer additives were examined at the next step: organic cosolvents and cyclodextrin (No. 2 Doehlert design). The optimal cyclodextrin type was also selected experimentally. The most promising results were obtained for the buffers fortified with methanol, acetonitrile and heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin. Since these additives may potentially affect acid-base equilibrium and ionization state of analytes, the third Doehlert design (No. 3) was used to reconcile concentration of these additives with optimal pH. Ultimately, the total separation of all 20 compounds was achieved using the borate buffer at basic pH 9.5 in the presence of 10mM cyclodextrin, 9% (v/v) acetonitrile and 36% (v/v) methanol. Identity of all compounds was confirmed using the in-lab build UV-VIS spectra library. The developed method succeeded in identification of coumarin derivatives in three real samples. It demonstrates a huge resolving power of CE assisted by addition of cyclodextrins and organic cosolvents. Our unique optimization approach, based on the three Doehlert designs, seems to be prospective for future applications of this technique. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Effect of pH on the rheological properties of borate crosslinked hydroxypropyl guar gum hydrogel and hydroxypropyl guar gum.

    PubMed

    Wang, Shibin; Tang, Hongbiao; Guo, Jianchun; Wang, Kunjie

    2016-08-20

    pH is an important factor affecting the performance of polymer fluid. The rheological properties of hydroxypropyl guar gum (HPG) base fluid and the structural strength, rheological properties, viscoelastic properties and thixotropy properties of HPG gel depend largely on the pH values. For the base fluid, an apparent viscosity-increasing effect was observed over the pH range from 7 to 11, and the apparent viscosity gradually decreased at pH 11.5-14, exhibiting electrostatic repulsion behavior and steric effects. For the HPG gel, at pH 7-12.5, the gel possessed higher apparent viscosity, higher elastic modulus (G'), lower tanδ (the ratio of the viscous modulus to the elastic modulus) and an "8"-shaped hysteresis loop, indicating stronger gel structure strength and the elastic dominant property. At pH 13-13.5, the gel samples exhibited the transition from a pseudoplastic fluid to a Newtonian fluid, and their viscosity, elastic modulus decreased but tanδ increased with the increase in pH values, exhibiting gradually weakened elastic properties. When the pH was 14, the gel mainly exhibited viscous characteristics. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. Preparation and properties of porous microspheres made from borate glass.

    PubMed

    Conzone, Samuel D; Day, Delbert E

    2009-02-01

    Dysprosium lithium-borate glass microspheres and particles, ranging from 45 to 150 microm in diameter, were reacted with a 0.25 M phosphate solution at 37 degrees C, whose pH was either 3 or 8.8. The glass reacted nonuniformly and was converted into a porous, amorphous, hydrated, dysprosium phosphate reaction product. The amorphous product had the same volume and shape (pseudomorphic) as the unreacted glass, and could be dried without cracking. After heating at 300 degrees C for 1 h, the amorphous reaction product had a specific surface area of approximately 200 m(2)/g, a pore size of approximately 30 nm, and nominal crushing strength of approximately 10 MPa. When the reaction product was heated to 600 degrees C for 15 min, the specific surface area decreased to approximately 90 m(2)/g and the nominal crushing strength increased to 35 MPa. Heating above 615 degrees C converted the amorphous dysprosium phosphate product into crystalline DyPO(4), which contained open porosity until heated above 800 degrees C for 15 min. Highly porous materials of different chemical composition can be prepared by chemically reacting a borate-based glass with an aqueous solution at low-temperature (<100 degrees C). These highly porous materials are easy to process, and are considered candidates for controlled drug delivery, catalysis, chromatographic separation, filtration, and as bioactive materials.

  4. Synthesis and formation mechanism of pinnoite by the phase transition process

    NASA Astrophysics Data System (ADS)

    Lin, Feng; Dong, Yaping; Peng, Jiaoyu; Wang, Liping; Li, Wu

    2016-06-01

    Pinnoite (MgB2O(OH)6) for the first time was synthesized using the solid-liquid-solid conversion method. The effects of reaction time, pH value and concentrations of magnesium and borate were investigated. Pinnoite was synthesized under the optimum condition of 8 mmol hungtsaoite and 1% boric acid solution at 80 °C. The products were determined using X-ray diffraction, Fourier-transform infrared spectroscopy, TG-DSC and a UV-vis spectrometer. The change processes of the surface morphology of pinnoite were investigated using scanning electron microscopy. In addition, the formation mechanism of pinnoite was discussed according to the changes in the content of precipitation and pH value.

  5. Mg- and K-bearing borates and associated evaporites at Eagle Borax spring, Death Valley, California: A spectroscopic exploration

    USGS Publications Warehouse

    Crowley, J.K.

    1996-01-01

    Efflorescent crusts at the Eagle Borax spring in Death Valley, California, contain an array of rare Mg and K borate minerals, several of which are only known from one or two other localities. The Mg- and/or K-bearing borates include aristarainite, hydroboracite, kaliborite, mcallisterite, pinnoite, rivadavite, and santite. Ulexite and probertite also occur in the area, although their distribution is different from that of the Mg and K borates. Other evaporite minerals in the spring vicinity include halite, thenardite, eugsterite, gypsum-anhydrite, hexahydrite, and bloedite. Whereas the first five of these minerals are found throughout Death Valley, the last two Mg sulfates are more restricted in occurrence and are indicative of Mg-enriched ground water. Mineral associations observed at the Eagle Borax spring, and at many other borate deposits worldwide, can be explained by the chemical fractionation of borate-precipitating waters during the course of evaporative concentration. The Mg sulfate and Mg borate minerals in the Eagle Borax efflorescent crusts point to the fractionation of Ca by the operation of a chemical divide involving Ca carbonate and Na-Ca borate precipitation in the subsurface sediments. At many other borate mining localities, the occurrence of ulexite in both Na borate (borax-kernite) and Ca borate (ulexite-colemanite) deposits similarly reflects ulexite's coprecipitation with Ca carbonate at an early concentration stage. Such ulexite may perhaps be converted to colemanite by later reaction with the coexisting Ca carbonate - the latter providing the additional Ca2+ ions needed for the conversion. Mg and Ca-Mg borates are the expected late-stage concentration products of waters forming ulexite-colemanite deposits and are therefore most likely to occur in the marginal zones or nearby mud facies of ulexite-colemanite orebodies. Under some circumstances, Mg and Ca-Mg borates might provide a useful prospecting guide for ulexite-colemanite deposits, although the high solubility of Mg borate minerals may prevent their formation in lacustrine settings and certainly inhibits their geologic preservation. The occurrence of Mg borates in borax-kernite deposits is also related to fractionation processes and points to the operation of an Mg borate chemical divide, characterized by Mg borate precipitation ahead of Mg carbonate. All of these considerations imply that Mg is a significant chemical component of many borate-depositing ground waters, even though Mg borate minerals may not be strongly evident in borate orebodies. The Eagle Borax spring borates and other evaporite minerals were studied using spectroscopic and X-ray powder diffraction methods, which were found to be highly complementary. Spectral reflectance measurements provide a sensitive means for detecting borates present in mixtures with other evaporites and can be used to screen samples rapidly for X-ray diffraction analysis. The apparently limited occurrence of Mg and K borate minerals compared to Ca and Na borates may stem partly from the inefficiency of X-ray diffraction methods for delineating the mineralogy of large and complex deposits. Spectral reflectance measurements can be made in the laboratory, in the field, on the mine face, and even remotely. Reflectance data should have an important role in studies of existing deposit mineralogy and related chemical fractionation processes, and perhaps in the discovery of new borate mineral resources.

  6. Intra-Shell boron isotope ratios in benthic foraminifera: Implications for paleo-pH reconstructions

    NASA Astrophysics Data System (ADS)

    Rollion-Bard, C.; Erez, J.

    2009-12-01

    The boron isotope composition of marine carbonates is considered to be a seawater pH proxy. Nevertheless, the use of δ11B has some limitations: 1) the knowledge of fractionation factor (α4-3) between the two boron dissolved species (boric acid and borate ion), 2) the δ11B of seawater may have varied with time and 3) the amplitude of the "vital effects" of this proxy. Using secondary ion mass spectrometry (SIMS), we looked at the internal variability in the boron isotope ratio of the shallow water, symbionts bearing foraminiferan Amphistegina lobifera. Specimens were cultured at constant temperature (24±0.1 °C) in seawater with pH ranging between 7.90 and 8.45. We performed 6 to 8 measurements of δ11B in each foraminifera. Intra-shell boron isotopes show large variability with an upper threshold value of pH ~ 9. The ranges of the skeletal calculated pH values in different cultured foraminifera, show strong correlation with the culture pH values and may thus serve as proxy for pH in the past ocean.

  7. Development and Validation of a Micellar Capillary Electrophoresis Method for Determination of IFNβ-1b in Lyophilized Formulation of a Biosimilar Product

    PubMed Central

    Dadgarnejad, Manuchehr; Rastegar, Hosein; Ilka, Hooshmand; Shekarchi, Maryam; Adib, Nooshin; Alebouyeh, Mahmood; Keypour, Nadia; Shoeibi, Shahram; Kobarfard, Farzad; Fazeli, Mohammad Reza

    2015-01-01

    Human interferons (IFNs) are key cytokines secreted by immune system. They have several effects such as antiviral and anti tumors activity, activating immune cells and healing of multiple sclerosis. The type IFNs present in humans are α ,β and Υ. IFN β is a polypeptide, normally produced by fibroblasts and seems to be more species-specific than IFN. Structural properties of IFNs are important for their biologic effects. There are a few analytical techniques for separation, identification and determination of IFNs in its formulations such as mass spectroscopy, RP-HPLC and capillary electrophoresis (CE). In this study we used Micellar Electrokinetic Chromatography (MEKC) as a unique mode of CE because of its capability to separate neutral as well as charged solutes. We used sodium tetraborate (Borax) as buffer without any modifier and sodium dodecyl sulfate (SDS) as surfactant. The optimum MECK running buffer consisted of Borate 50 Mm; SDS 20 mM pH =9.6. The validated method was used for determination of the IFN β-1b formulation which is manufactured in Iran. From 9 collected different batches, all of them had acceptable potency as claimed on their label with average 102.25 ±10.030 %. This is the first time that a MEKC method is introduced for quantification of IFN β-1b in its pharmaceutical dosage forms. The method is reliable safe, rapid and accurate. PMID:26330863

  8. Development and Validation of a Micellar Capillary Electrophoresis Method for Determination of IFNβ-1b in Lyophilized Formulation of a Biosimilar Product.

    PubMed

    Dadgarnejad, Manuchehr; Rastegar, Hosein; Ilka, Hooshmand; Shekarchi, Maryam; Adib, Nooshin; Alebouyeh, Mahmood; Keypour, Nadia; Shoeibi, Shahram; Kobarfard, Farzad; Fazeli, Mohammad Reza

    2015-01-01

    Human interferons (IFNs) are key cytokines secreted by immune system. They have several effects such as antiviral and anti tumors activity, activating immune cells and healing of multiple sclerosis. The type IFNs present in humans are α ,β and Υ. IFN β is a polypeptide, normally produced by fibroblasts and seems to be more species-specific than IFN. Structural properties of IFNs are important for their biologic effects. There are a few analytical techniques for separation, identification and determination of IFNs in its formulations such as mass spectroscopy, RP-HPLC and capillary electrophoresis (CE). In this study we used Micellar Electrokinetic Chromatography (MEKC) as a unique mode of CE because of its capability to separate neutral as well as charged solutes. We used sodium tetraborate (Borax) as buffer without any modifier and sodium dodecyl sulfate (SDS) as surfactant. The optimum MECK running buffer consisted of Borate 50 Mm; SDS 20 mM pH =9.6. The validated method was used for determination of the IFN β-1b formulation which is manufactured in Iran. From 9 collected different batches, all of them had acceptable potency as claimed on their label with average 102.25 ±10.030 %. This is the first time that a MEKC method is introduced for quantification of IFN β-1b in its pharmaceutical dosage forms. The method is reliable safe, rapid and accurate.

  9. Method development for the determination of coumarin compounds by capillary electrophoresis with indirect laser-induced fluorescence detection.

    PubMed

    Wang, Weiping; Tang, Jianghong; Wang, Shumin; Zhou, Lei; Hu, Zhide

    2007-04-27

    A capillary zone electrophoresis (CZE) with indirect laser-induced fluorescence detection (ILIFD) method is described for the simultaneous determination of esculin, esculetin, isofraxidin, genistein, naringin and sophoricoside. The baseline separation was achieved within 5 min with running buffer (pH 9.4) composed of 5mM borate, 20% methanol (v/v) as organic modifier, 10(-7)M fluorescein sodium as background fluorophore and 20 kV of applied voltage at 30 degrees C of cartridge temperature. Good linearity relationships (correlation coefficients >0.9900) between the second-order derivative peak-heights (RFU) and concentrations of the analytes (mol L(-1)) were obtained. The detection limits for all analytes in second-order derivative electrophoregrams were in the range of 3.8-15 microM. The RSD data of intra-day for migration times and second-order derivative peak-height were less than 0.95 and 5.02%, respectively. This developed method was applied to the analysis of the courmin compounds in herb plants with recoveries in the range of 94.7-102.1%. In this work, although the detection sensitivity was lower than that of direct LIF, yet the method would extend the application range of LIF detection.

  10. Determination of arbutin and bergenin in Bergeniae Rhizoma by capillary electrophoresis with a carbon nanotube-epoxy composite electrode.

    PubMed

    Zhang, Luyan; Zhang, Wei; Chen, Gang

    2015-11-10

    This report describes the fabrication and the application of a novel carbon nanotube (CNT)-epoxy composite electrode as a sensitive amperometric detector for the capillary electrophoresis (CE). The composite electrode was fabricated on the basis of the in situ polycondensation of a mixture of CNTs and 1,2-ethanediamine-containing bisphenol A epoxy resin in the inner bore of a piece of fused silica capillary under heat. It was coupled with CE for the separation and detection of arbutin and bergenin in Bergeniae Rhizoma, a traditional Chinese medicine, to demonstrate its feasibility and performance. The two phenolic constituents were well separated within 10min in a 45cm capillary length at a separation voltage of 12kV using a 50mM borate buffer (pH 9.2). The CNT-based detector offered higher sensitivity, significantly lower operating potential, satisfactory resistance to surface fouling, and lower expense of operation, indicating great promise for a wide range of analytical applications. It showed long-term stability and reproducibility with relative standard deviations of less than 5% for the peak current (n=15). Copyright © 2015 Elsevier B.V. All rights reserved.

  11. A rapid quantitative determination of phenolic acids in Brassica oleracea by capillary zone electrophoresis.

    PubMed

    Lee, Iris S L; Boyce, Mary C; Breadmore, Michael C

    2011-07-15

    A simple and rapid capillary zone electrophoresis method to quantitatively determine the phenolic acid contents in brassica vegetables is described. Phenolic compounds were extracted from broccoli, broccolini, Brussels sprouts, cabbage and cauliflower and the main hydroxycinnamic acids (sinapic, ferulic, p-coumaric and caffeic acids) were isolated by solid phase extraction with C18 cartridges. Using an optimised method, the four analytes were separated in less than 7min in a 50μm×60cm capillary with a 15mM borate buffer (pH=9.13) and a separation voltage of 30kV at 30°C. A linear relationship was observed for the method (r=0.9997-0.9999) with detection limits ranging from 1.1 to 2.3mg/kg of vegetables for the analytes. This method demonstrated good reproducibility with coefficients of variation of less than 5% for peak area and less than 1% for migration time (n=7). The method was successfully applied to quantitatively determine the phenolic acid contents in a range of brassica vegetables and the results were in good agreement when compared to those from high performance liquid chromatography analysis. Crown Copyright © 2011. Published by Elsevier Ltd. All rights reserved.

  12. Capillary electrophoresis fingerprinting and spectrophotometric determination of antioxidant potential for classification of Mentha products.

    PubMed

    Roblová, Vendula; Bittová, Miroslava; Kubáň, Petr; Kubáň, Vlastimil

    2016-07-01

    In this work aqueous infusions from ten Mentha herbal samples (four different Mentha species and six hybrids of Mentha x piperita) and 20 different peppermint teas were screened by capillary electrophoresis with UV detection. The fingerprint separation was accomplished in a 25 mM borate background electrolyte with 10% methanol at pH 9.3. The total polyphenolic content in the extracts was determined spectrophotometrically at 765 nm by a Folin-Ciocalteu phenol assay. Total antioxidant activity was determined by scavenging of 2,2-diphenyl-1-picrylhydrazyl radical at 515 nm. The peak areas of 12 dominant peaks from CE analysis, present in all samples, and the value of total polyphenolic content and total antioxidant activity obtained by spectrophotometry was combined into a single data matrix and principal component analysis was applied. The obtained principal component analysis model resulted in distinct clusters of Mentha and peppermint tea samples distinguishing the samples according to their potential protective antioxidant effect. Principal component analysis, using a non-targeted approach with no need for compound identification, was found as a new promising tool for the screening of herbal tea products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Validation of a rapid micellar electrokinetic capillary chromatographic method for the simultaneous determination of isoniazid and pyridoxine hydrochloride in pharmaceutical formulation.

    PubMed

    Nemutlu, E; Celebier, M; Uyar, B; Altinöz, S

    2007-07-01

    An efficient and reliable micellar electrokinetic capillary chromatography (MEKC) method has been developed for the simultaneous determination of isoniazid (ISO) and pyridoxine hydrochloride (PYR) in pharmaceutical formulations. A chemometric two level full factorial design approach was used to search for the optimum conditions of separation. Three parameters were selected for this study: the buffer pH, the buffer concentration and sodium dodecyl sulphate (SDS) concentrations. Resolution, peak symmetry and analysis time were established as response. The two analytes were separated within 6 min with the optimized conditions: 50 mM borate buffer, 25 mM SDS pH 7.8, 35 degrees C, at 50 mbar 4s injection and 30 kV by using a fused silica capillary (72 cm effective length, 50 microm i.d.). The detection wavelength was set to 205 nm. Meloxicam was used as internal standard. The method was validated with respect to stability, linearity range, limit of quantitation and detection, precision, accuracy, specificity and robustness. The detection limits of the method were 1.0 microg mL(-1) for ISO and 0.40 microg mL(-1) for PYR and the method was linear at least in the range of 3.0-100 microg mL(-1) for ISO and 1.0-100 microg mL(-1) for PYR with excellent correlation coefficients (0.9995 for ISO and 0.9998 for PYR). Relative standard deviations (R.S.D.s) of the described method ranged between 0.54 and 2.27% for intra-day precision and between 0.65 and 2.69% for inter-day precision. The developed method was applied to the tablet form of ISO and PYR-containing the pharmaceutical preparations and the data were compared with obtained from the standard addition method. No statistically significant difference was found.

  14. Penetration of boron from topically applied borate solutions

    Treesearch

    Stan T. Lebow; Patricia K. Lebow; Steven A. Halverson

    2010-01-01

    Borate penetration relies on diffusion when borate and glycol-borate preservatives are applied to the surface of wood. This study evaluated the extent of borate penetration in framing lumber as a function of preservative formulation, wood moisture content, and diffusion time after treatment. In Phase I of the study, end-matched specimens were conditioned to target...

  15. Comparison of classical fenton, nitrilotriacetic acid (NTA)-Fenton, UV-Fenton, UV photolysis of Fe-NTA, UV-NTA-Fenton, and UV-H2O2 for the degradation of cyclohexanoic acid.

    PubMed

    Zhang, Ying; Klamerth, Nikolaus; Chelme-Ayala, Pamela; Gamal El-Din, Mohamed

    2017-05-01

    The treatment of a naphthenic acid model compound, cyclohexanoic acid, with classical Fenton, UV-H 2 O 2 , UV-Fenton, nitrilotriacetic acid (NTA)-Fenton, UV-NTA-Fenton, and UV photolysis of Fe-NTA processes at pHs 3 and 8 was investigated. At 1.47 mM H 2 O 2 , 0.089 mM Fe, and 0.18 mM NTA, the UV-NTA-Fenton process at pH 3 exhibited the highest H 2 O 2 decomposition (100% in 25 min), CHA removal (100% in 12 min) with a rate constant of 0.27 ± 0.025 min -1 , and NTA degradation (100% in 6 min). Due to the formation of H 2 O 2 -Fe(III)NTA adduct, the total Fe concentration in the UV-NTA-Fenton system (0.063 mM at the end of the reaction) at pH 8 was much higher than that in the UV photolysis of Fe(III)NTA process (0.024 mM). The co-complexing effect of borate buffer helped to keep iron soluble; however, it imposed a negative influence on the CHA degradation in the UV-NTA-Fenton process (68% CHA removal in 60 min in the borate buffer compared to 92% in MilliQ water). The results demonstrated that the most efficient process for the CHA degradation under the experimental conditions was the UV-NTA-Fenton process at pH 3. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. Haloacyl complexes of boron, [(CF3)3BC(O)Hal]- (Hal=F, Cl, Br, I).

    PubMed

    Finze, Maik; Bernhardt, Eduard; Willner, Helge; Lehmann, Christian W

    2005-11-04

    The haloacyltris(trifluoromethyl)borate anions [(CF3)3BC(O)Hal]- (Hal=F, Cl, Br, I) have been synthesized by reacting (CF3)3BCO with either MHal (M=K, Cs; Hal=F) in SO2 or MHal (M=[nBu4N]+, [Et4N]+, [Ph4P]+; Hal=Cl, Br, I) in dichloromethane. Metathesis reactions of the fluoroacyl complex with Me3SiHal (Hal=Cl, Br, I) led to the formation of its higher homologues. The thermal stabilities of the haloacyltris(trifluoromethyl)borates decrease from the fluorine to the iodine derivative. The chemical reactivities decrease in the same order as demonstrated by a series of selected reactions. The new [(CF3)3BC(O)Hal]- (Hal=F, Cl, Br) salts are used as starting materials in the syntheses of novel compounds that contain the (CF3)3B-C fragment. All borate anions [(CF3)3BC(O)Hal]- (Hal=F, Cl, Br, I) have been characterized by multinuclear NMR spectroscopy (11B, 13C, 17O, 19F) and vibrational spectroscopy. [PPh4][(CF3)3BC(O)Br] crystallizes in the monoclinic space group P2/c (no. 13) and the bond parameters are compared with those of (CF3)3BCO and K[(CF3)3BC(O)F]. The interpretation of the spectroscopic and structural data are supported by DFT calculations [B3LYP/6-311+G(d)].

  17. Amount of leachant and water absorption levels of wood treated with borates and water repellents.

    PubMed

    Baysal, Ergun; Sonmez, Abdullah; Colak, Mehmet; Toker, Hilmi

    2006-12-01

    Wood protection efficacy of borates against biological agents, flame retardancy, and suitability to the environment is well known. Since borates can be applied to timber as water based solutions, they are preferred economically as well. Even though they are highly mobile in wood, boron compounds are widely used in timber preservation. Borates migrate in liquid and increase the hygroscopicity of wood in damp conditions. This study deals with the physical restriction of water access in wood by impregnating water repellent agents into wood to limit amount of leachant and water absorption levels of wood after boron treatment. Borates were incorporated with polyethylene glycol-400 (PEG-400) their bulking effect in wood was considered. Results indicated that the amount of leachates from wood treated with borates in PEG-400 was remarkably higher compared to those of wood treated with the aqueous solutions of borates. Water absorption (WA) levels of wood treated with aqueous solutions of borates were higher than those of their treated samples with the solutions in PEG-400. Secondary treatments of wood with the water repellent (WR) chemicals following borate impregnation reduced the leaching of chemicals from wood in water and also WA of the specimens were less than those of the wood treated with only borates from aqueous and PEG solutions. Styrene (St) was the most effective monomer among the other agents used in terms of immobility effect on borates and WA.

  18. Combined effects of lithium and borate ions on the hydration of calcium sulfoaluminate cement

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

    Cau Dit Coumes, Céline, E-mail: celine.cau-dit-coumes@cea.fr; Dhoury, Mélanie; Champenois, Jean-Baptiste

    This work investigates the combined influence of borate and lithium ions on the hydration of two calcium sulfoaluminate (CSA) cements containing 0 or 10 wt% gypsum. On the one hand, borates are known to retard CSA cement hydration due to the rapid precipitation of ulexite. On the other hand, lithium ions accelerate CSA cement hydration thanks to the fast precipitation of Li-containing aluminum hydroxide. When borates and lithium are present simultaneously, these two mechanisms are superimposed. With a gypsum-free cement, a third process is additionally observed: lithium promotes the initial precipitation of a borated AFm phase which is later convertedmore » into a borated AFt phase when hydration accelerates. Lithium salts can counteract the retardation by sodium borate. However, their influence is limited once a sufficient amount of Li-containing Al(OH){sub 3} seeds is formed. For the CSA cements under investigation, the threshold lithium concentration is close to 0.03 mmol/g of cement and similar with or without borate.« less

  19. Borates

    USGS Publications Warehouse

    Crangle, R.D.

    2013-01-01

    Four minerals represent 90 percent of the borates used by industry worldwide — the sodium borates (tincal and kernite), calcium borate (colemanite) and the sodium-calcium borate (ulexite). Borax is a white crystalline substance, chemically known as sodium tetraborate decahydrate, and is found naturally as the mineral tincal. Boric acid is a colorless crystalline solid sold in technical, national formulary and special quality grades as granules or powder and marketed most often as anhydrous boric acid. Deposits of borates are associated with volcanic activity and arid climates, with the largest economically viable deposits located in the Mojave Desert of the United States near Boron, CA, the Alpide belt in southern Asia and the Andean belt of South America.

  20. Li{sub 2}Sr{sub 4}B{sub 12}O{sub 23}: A new alkali and alkaline-earth metal mixed borate with [B{sub 10}O{sub 18}]{sup 6-} network and isolated [B{sub 2}O{sub 5}]{sup 4-} unit

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

    Zhang Min; Graduate University of Chinese Academy of Sciences, Beijing 100049; Pan Shilie, E-mail: slpan@ms.xjb.ac.cn

    2012-06-15

    A novel ternary lithium strontium borate Li{sub 2}Sr{sub 4}B{sub 12}O{sub 23} crystal with size up to 20 mm Multiplication-Sign 10 mm Multiplication-Sign 4 mm has been grown via the top-seeded solution growth method below 730 Degree-Sign C. Single-crystal XRD analyses showed that Li{sub 2}Sr{sub 4}B{sub 12}O{sub 23} crystallizes in the monoclinic space group P2{sub 1}/c with a=6.4664(4) A, b=8.4878(4) A, c=15.3337(8) A, {beta}=102.02(3) Degree-Sign , Z=2. The crystal structure is composed of [B{sub 10}O{sub 18}]{sup 6-} network and isolated [B{sub 2}O{sub 5}]{sup 4-} unit. The IR spectrum further confirmed the presence of both BO{sub 3} and BO{sub 4} groups. TG-DSCmore » and Transmission spectrum were reported. Band structures and density of states were calculated. - Graphical abstract: A new phase, Li{sub 2}Sr{sub 4}B{sub 12}O{sub 23}, has been discovered in the ternary M{sub 2}O-M Prime O-B{sub 2}O{sub 3} (M=alkali-metal, M Prime =alkalineearth metal) system. The crystal structure consists of [B{sub 10}O{sub 18}]{sup 6-} network and isolated [B{sub 2}O{sub 5}]{sup 4-} unit. Highlights: Black-Right-Pointing-Pointer Li{sub 2}Sr{sub 4}B{sub 12}O{sub 23} is a a novel borate discovered in the M{sub 2}O-M Prime O-B{sub 2}O{sub 3} (M=alkali-metal, M Prime =alkaline-earth metal) system. Black-Right-Pointing-Pointer Li{sub 2}Sr{sub 4}B{sub 12}O{sub 23} crystal structure has a three-dimensional crystal structure with [B{sub 10}O{sub 18}]{sup 6-} network and isolated [B{sub 2}O{sub 5}]{sup 4-} unit. Black-Right-Pointing-Pointer Sr{sub 1} and Sr{sub 2} are located in two different channels constructed by {sup 3}{sub {infinity}}[B{sub 10}O{sub 18}] network.« less

  1. Method of recycling lithium borate to lithium borohydride through methyl borate

    DOEpatents

    Filby, Evan E.

    1977-01-01

    This invention provides a method for the recycling of lithium borate to lithium borohydride which can be reacted with water to generate hydrogen for utilization as a fuel. The lithium borate by-product of the hydrogen generation reaction is reacted with hydrogen chloride and water to produce boric acid and lithium chloride. The boric acid and lithium chloride are converted to lithium borohydride through a methyl borate intermediate to complete the recycle scheme.

  2. The response of Serratia marcescens JG to environmental changes by quorum sensing system.

    PubMed

    Sun, Shu-Jing; Liu, Hui-Jun; Weng, Cai-Hong; Lai, Chun-Fen; Ai, Liu-Ying; Liu, Yu-Chen; Zhu, Hu

    2016-08-01

    Many bacterial cells are known to regulate their cooperative behaviors and physiological processes through a molecular mechanism called quorum sensing. Quorum sensing in Serratia marcescens JG is mediated by the synthesis of autoinducer 2 (AI-2) which is a furanosyl borate diester. In this study, the response of quorum sensing in S. marcescens JG to environment changes such as the initial pH, carbon sources and boracic acid was investigated by a bioreporter and real-time PCR analysis. The results show that glucose can affect AI-2 synthesis to the greatest extent, and 2.0 % glucose can stimulate S. marcescens JG to produce more AI-2, with a 3.5-fold increase in activity compared with control culture. Furthermore, the response of quorum sensing to changes in glucose concentration was performed by changing the amount of luxS RNA transcripts. A maximum of luxS transcription appeared during the exponential growth phase when the glucose concentration was 20.0 g/L. AI-2 production was also slightly impacted by the low initial pH. It is significant for us that the addition of boracic acid at microdosage (0.1-0.2 g/L) can also induce AI-2 synthesis, which probably demonstrated the feasible fact that the 4,5-dihydroxy-2, 3-pentanedione cyclizes by the addition of borate and the loss of water, is hydrated and is converted to the final AI-2 in S. marcescens JG.

  3. 40 CFR 721.10631 - Mixed metal borate (generic).

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Mixed metal borate (generic). 721... Substances § 721.10631 Mixed metal borate (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified generically as mixed metal borate (PMN P-12-64...

  4. 40 CFR 721.10631 - Mixed metal borate (generic).

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Mixed metal borate (generic). 721... Substances § 721.10631 Mixed metal borate (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified generically as mixed metal borate (PMN P-12-64...

  5. Theoretical isotopic fractionation between structural boron in carbonates and aqueous boric acid and borate ion

    NASA Astrophysics Data System (ADS)

    Balan, Etienne; Noireaux, Johanna; Mavromatis, Vasileios; Saldi, Giuseppe D.; Montouillout, Valérie; Blanchard, Marc; Pietrucci, Fabio; Gervais, Christel; Rustad, James R.; Schott, Jacques; Gaillardet, Jérôme

    2018-02-01

    The 11B/10B ratio in calcite and aragonite is an important proxy of oceanic water pH. However, the physico-chemical mechanisms underpinning this approach are still poorly known. In the present study, we theoretically determine the equilibrium isotopic fractionation properties of structural boron species in calcium carbonates, BO33-, BO2(OH)2- and B(OH)4- anions substituted for carbonate groups, as well as those of B(OH)4- and B(OH)3 species in vacuum. Significant variability of equilibrium isotopic fractionation properties is observed among these structural species which is related to their contrasted coordination state, Bsbnd O bond lengths and atomic-scale environment. The isotopic composition of structural boron does not only depend on its coordination number but also on its medium range environment, i.e. farther than its first coordination shell. The isotopic fractionation between aqueous species and their counterparts in vacuum are assessed using previous investigations based on similar quantum-mechanical modeling approaches. At 300 K, the equilibrium isotope composition of structural trigonal species is 7-15‰ lighter than that of aqueous boric acid molecules, whereas substituted tetrahedral borate ions are heavier than their aqueous counterparts by 10-13‰. Although significant uncertainties are known to affect the theoretical prediction of fractionation factors between solids and solutions, the usually assumed lack of isotopic fractionation during borate incorporation in carbonates is challenged by these theoretical results. The present theoretical equilibrium fractionation factors between structural boron and aqueous species differ from those inferred from experiments which may indicate that isotopic equilibrium, unlike chemical equilibrium, was not reached in most experiments. Further research into the isotopic fractionation processes at the interface between calcium carbonates and aqueous solution as well as long duration experiments aimed at investigating the kinetics of equilibration of boron environment and isotopic composition are therefore required to refine our understanding of boron coprecipitation in carbonates and thus the theory behind the use of boron isotopes as an ocean pH proxy.

  6. Acidic and basic solutions dissolve protein plugs made of lithostathine complicating choledochal cyst/pancreaticobiliary maljunction.

    PubMed

    Kaneko, Kenitiro; Ono, Yasuyuki; Tainaka, Takahisa; Sumida, Wataru; Ando, Hisami

    2009-07-01

    Symptoms of choledochal cysts are caused by protein plugs made of lithostathine, which block the long common channel and increase pancreaticobiliary ductal pressure. Agents that dissolve protein plugs can provide relief from or prevent symptoms. In the present study, drugs reportedly effective for pancreatic and biliary stones were used in dissolution tests. Protein plugs were obtained from choledochal cysts during surgery in two children (5- and 6-year-old girls). Plugs approximately 2 mm in diameter were immersed in citric acid, tartaric acid, dimethadione, bromhexine, dehydrocholic acid, sodium citrate, hydrochloric acid, and sodium hydroxide solutions under observation with a digital microscope. The pH of each solution was measured using a pH meter. Plugs dissolved in citric acid (5.2 mM; pH 2.64), tartaric acid (6.7 mM; pH 2.51), dimethadione (75 mM; pH 3.70), hydrochloric acid (0.5 mM; pH 3.13), and sodium hydroxide (75 mM; pH 12.75) solutions. Plugs did not dissolve in dimethadione (7.5 mM; pH 4.31), bromhexine (0.1%; pH 4.68), dehydrocholic acid (5%; pH 7.45), and sodium citrate (75 mM; pH 7.23) solutions. Protein plugs in choledochal cysts are dissolved in acidic and basic solutions, which may eliminate longitudinal electrostatic interactions of the lithostathine protofibrils.

  7. 21 CFR 872.3400 - Karaya and sodium borate with or without acacia denture adhesive.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... denture adhesive. 872.3400 Section 872.3400 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF... and sodium borate with or without acacia denture adhesive. (a) Identification. A karaya and sodium borate with or without acacia denture adhesive is a device composed of karaya and sodium borate with or...

  8. Hydrodesulfurization reactions of atmospheric gas oil over CoMo/alumina-aluminum borate catalysts

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

    Chiuping Li; Jungchung Wu; Yuwen Chen

    1993-08-01

    A precipitation technique at constant pH value was used to prepare a series of alumina-aluminum borates (AABs) with various Al/B atomic ratios. These materials were used as the supports of Co-Mo catalysts. Hydrodesulfurization (HDS) of Kuwait atmospheric gas (AGO) oil was carried out over these presulfided catalysts in a bench-scale trickle bed reactor at 400 psi and 340 C. All CoMo/AAB catalysts are much more active than the conventional CoMo/Al[sub 2]O[sub 3] catalyst on HDS reactions. A correlation exists between the acidity and the HDS activity of the catalysts. The high activities of the CoMo/AAB catalysts can be rationalized onmore » the presence of boron. On one hand, it can increase the metal dispersions and hydrogenation capabilities. On the other hand, it can enhance the acidities and cracking abilities of the catalysts. The desulfurization data can be fitted with a pseudo-second-order rate equation. The activation energy for desulfurization is found to be 26 kcal/mol.« less

  9. Appearance of small polaron hopping conduction in iron modified cobalt lithium bismuth borate glasses

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

    Dahiya, M. S.; Khasa, S., E-mail: skhasa@yahoo.com; Yadav, Arti

    2016-05-23

    Lithium bismuth borate glasses containing different amounts of cobalt and iron oxides having chemical composition xFe{sub 2}O{sub 3}•(20-x)CoO•30Li{sub 2}O•10Bi{sub 2}O{sub 3}•40B{sub 2}O{sub 3} (x = 0, 5, 10, 15 and 20 mol% abbreviated as CFLBB1-5 respectively) prepared via melt quench technique have been investigated for their dc electrical conductivity. The amorphous nature of prepared glasses has been confirmed through X-ray diffraction measurements. The dc electrical conductivity has been analyzed by applying Mott’s small polaron hopping model. Activation energies corresponding to lower and higher temperature region have been evaluated. The iron ion concentration (N), mean spacing between iron ions (R) and polaronmore » radius (R{sub p}) has been evaluated using the values of phonon radius (R{sub ph}) and Debye temperature (θ{sub D}). The glass sample without iron (CFLBB1) shows ionic conductivity but the incorporation of iron in the glass matrix results in the appearance of electronic conductivity.« less

  10. Corrosion Behavior of Ultra-fine Grained 1050 Aluminum Alloy Fabricated by ARB Process in a Buffer Borate Solution

    NASA Astrophysics Data System (ADS)

    Fattah-alhosseini, A.; Gashti, S. O.

    2015-09-01

    Accumulative roll bonding (ARB) has been used as a severe plastic deformation process for the industrial production of ultra-fine grained (UFG) and nano-crystalline sheets with excellent mechanical properties. In the present study, the effect of the ARB process on the corrosion behavior of UFG and nano-crystalline 1050 aluminum alloy in a buffer borate solution (pH 5.5) has been investigated. The result of microhardness tests revealed that microhardness values increase with an increasing number of ARB cycles. A sharp increase in microhardness is seen after three ARB cycles, whereas moderate additional increases are observed afterward for up to nine cycles. Also, the XRD results showed that the mean crystallite size decreased to about 91 nm after nine cycles. The potentiodynamic plots show that as a result of ARB, the corrosion behavior of the UFG and nano-crystalline specimens improves, compared to the annealed 1050 aluminum alloy. Moreover, electrochemical impedance spectroscopy measurements showed that the polarization resistance increases with an increasing number of ARB cycles.

  11. Determination of neonicotinoid insecticides in environmental samples by micellar electrokinetic chromatography using solid-phase treatments.

    PubMed

    Ettiene, Gretty; Bauza, Roberto; Plata, María R; Contento, Ana M; Ríos, Angel

    2012-10-01

    A sensitive and reliable method based on MEKC has been developed and validated for trace determination of neonicotinoid insecticides (thiamethoxam, acetamiprid, and imidacloprid) and the metabolite 6-chloronicotinic acid in water and soil matrices. Optimum separation of the neonicotinoid insecticides was obtained on a 58 cm long capillary (75 μm id) using as the running electrolyte 40 mM SDS, 5 mM borate (pH 10.4), and 5% (v/v) methanol at a temperature of 25°C, a voltage of 25 kV and with hydrodynamic injection (10 s). The analysis time was less than 7 min. Prior to MEKC determination, the samples were purified and enriched by carrying out extraction-preconcentration steps. For aqueous samples, off-line SPE with a sorptive material such as Strata-X (polymeric hydrophobic sorbent) and octadecylsilane (C₁₈) was carried out to clean up and preconcentrate the insecticides. However, for soil samples, matrix solid-phase dispersion (MSPD) was applied with C₁₈ used as the dispersant. Good linearity, accuracy, and precision were obtained and the detection limits were in the range between 0.01 and 0.07 μg mL⁻¹ for river water and 0.17 and 0.37 μg g⁻¹ for soil samples. Recovery levels reached greater than 92% for all of the assayed neonicotinoids in river water samples with Strata-X. In soil matrices, the best recoveries (63-99%) were obtained with MSPD. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Controls on the pH of hyper-saline lakes - A lesson from the Dead Sea

    NASA Astrophysics Data System (ADS)

    Golan, Rotem; Gavrieli, Ittai; Ganor, Jiwchar; Lazar, Boaz

    2016-01-01

    The pH of aqueous environments is determined by the dominant buffer systems of the water, defined operationally as total alkalinity (TA). The major buffer systems in the modern ocean are carbonic and boric acids of which the species bicarbonate, carbonate and borate make up about 77%, 19% and 4% of the TA, respectively. During the course of seawater evaporation (e.g. lagoons) the residual brine loses considerable portion of the dissolved inorganic carbon (DIC) and carbonate alkalinity (CA) already at the early stages of evaporation. DIC and CA decrease due to massive precipitation of CaCO3, while total boron (TB) increases conservatively, turning borate to the dominant alkalinity species in marine derived brines. In the present work we assess the apparent dissociation constant value of boric acid (KB‧) in saline and hypersaline waters, using the Dead Sea (DS) as a case study. We explain the DS low pH (∼6.3) and the effect of the boric and carbonic acid pK‧-s on the behavior of the brine's buffer system, including the pH increase that results from brine dilution. The KB‧ in DS was estimated from TB, TA, DIC and pH data measured in this study and early empirical data on artificial DS brines containing just carbonic acid. The KB‧ value was corroborated by Pitzer ion interaction model calculations using PHREEQC thermodynamic code applied to the chemical composition of the DS. Our results show that KB‧ increases considerably with the brine's ionic strength, reaching in the DS to a factor of 100 higher than in ;mean; seawater. Based on theoretical calculations and analyses of other natural brines it is suggested that brines' composition is a major factor in determining the KB‧ value and in turn the pH of such brines. We show that the higher the proportion of divalent cations in the brine the higher the dissociation constants of the weak acids (presumably due to formation of complexes). The low pH of the Dead Sea is accordingly explained by its extremely high ionic strength (TDS = 348 g/L) and the dominance of the divalent cation, Mg2+. Other natural hyper-saline brines with high concentration of divalent cations such as Kunteyi Lake in China and Don-Juan Pond in Antarctica follow the same general pattern. In contrast, the high pH of soda lakes results not only from their high TA but also by the dominance of the monovalent cation, Na+. Our study emphasizes the strong control of brine composition on pKB‧ and pH. These factors should be taken into consideration when reconstructing past and present environmental evaporitic environments.

  13. Purification of the Alpha Glycerophosphate Oxidase from African Trypanosomes

    DTIC Science & Technology

    1988-02-02

    remo~val of all unattached enzymes , the GPO would be eluted with a buffer containing the substrate a- GP. Cyancqen bromide activated Sepharose 4B was...released upon eluticn with a buffer cm-xtaining 100 rm of a-GP. Unfortunately, in these experiments, trypan blue was eluted from the colmn and the enzyme ...borate buffer (pH 8.0), there was no leakage of the ligand but the GPO was not released fram the colun when eluted with 10aM c-GP. Enzyme assays of the

  14. Separation of flavonol-2-O-glycosides from Calendula officinalis and Sambucus nigra by high-performance liquid and micellar electrokinetic capillary chromatography.

    PubMed

    Pietta, P; Bruno, A; Mauri, P; Rava, A

    1992-02-28

    Calendula officinalis and Sambucus nigra flowers were analysed by reversed-phase high-performance liquid chromatography (RP-HPLC) and micellar electrokinetic capillary chromatography (MECC). RP-HPLC was performed on C8 Aquapore RP 300 columns with eluents containing 2-propanol and tetrahydrofuran. MECC was carried out on a 72-cm fused-silica capillary using sodium dodecyl sulphate and sodium borate (pH 8.3) as the running buffer. The results obtained by these techniques are compared.

  15. Effective binding of perhalogenated closo-borates to serum albumins revealed by spectroscopic and ITC studies

    NASA Astrophysics Data System (ADS)

    Kuperman, Marina V.; Losytskyy, Mykhaylo Yu.; Bykov, Alexander Yu.; Yarmoluk, Sergiy M.; Zhizhin, Konstantin Yu.; Kuznetsov, Nikolay T.; Varzatskii, Oleg A.; Gumienna-Kontecka, Elzbieta; Kovalska, Vladyslava B.

    2017-08-01

    The interactions of boron cluster compounds closo-borates with biomolecules are widely studied due to their efficiency as agents for boron neutron capture therapy of cancer. In present work the binding abilities of anionic halogen closo-borates [B10Hal10]2- (Hal = Cl, Br, I) and [B12Hal12]2- (Hal = Cl, I) towards bovine and human serum albumins were investigated by spectroscopic and isothermal titration calorimetry (ITC) methods. The protein fluorescence quenching method and ITC studies confirmed the complex formation. The degree of protein fluorescence quenching increased from chlorine to iodine boron derivatives that is attributed to external heavy atom effect. The ITC data point on the existence in the protein structure of two types of binding sites: with higher and lower affinity to closo-borates. Albumin-closo-borate complex binding ratio, n (4-5 anions per protein molecule) is higher than for the parent hydrogen closo-borates (2 anions per protein molecule). Binding constants estimated by fluorescent and ITC methods indicate higher affinity of halogen closo-borates to albumins (K in the range of 104-106 M-1) comparing to that of the hydrogen closo-borate (K about 103 M-1). Due to their high affinity and high binding ratio to albumins halogen closo-borates are proposed for further studies as agents for boron neutron capture therapy.

  16. Visual test of subparts per billion-level mercuric ion with a gold nanoparticle probe after preconcentration by hollow fiber supported liquid membrane.

    PubMed

    Tan, Zhi-qiang; Liu, Jing-fu

    2010-05-15

    With the combination of the gold nanoparticle (AuNP)-based visual test with hollow fiber supported liquid membrane (HFSLM) extraction, a highly sensitive and selective method was developed for field detection of mercuric ion (Hg(2+)) in environmental waters. Hg(2+) in water samples was extracted through HFSLM and trapped in the aqueous acceptor and then visually detected based on the red-to-blue color change of 3-mercaptopropionic acid-functionalized AuNP (MPA-AuNP) probe. The highest extraction efficiency of Hg(2+) was obtained by using a 600 mL sample (pH 8.0, 2.0% (w/v) NaCl), approximately 35 microL of acceptor (10 mM of 2,6-pyridinedicarboxylic acid, pH 4.0) filled in the lumen of a polypropylene hollow fiber tubing (55 cm in length, 50 microm wall thickness, 280 microm inner diameter), a liquid membrane of 2.0% (w/v) trioctycphosphine oxide in undecane, and a shaking rate of 250 rpm. The chromegenic reaction was conducted by incubating the mixture of MPA-AuNP stock solution (12 microL, 15 nM), Tris-borate buffer solution (18 microL, 0.2 M, pH 9.5), and acceptor (30 microL) at 30 degrees C for 1 h. The detection limit can be adjusted to 0.8 microg/L Hg(2+) (corresponding to an enrichment factor of approximately 1000 in the HFSLM) and 2.0 microg/L Hg(2+) (the U.S. Environmental Protection Agency limit of [Hg(2+)] for drinkable water) by using extraction times of 3 and 1 h, respectively. The proposed method is extremely specific for Hg(2+) with tolerance to at least 1000-fold of other environmentally relevant heavy and transition metal ions and was successfully applied to detect Hg(2+) in a certified reference water sample, as well as real river, lake, and tap water samples.

  17. The hydrothermolysis of the picrate anion: Kinetics and mechanism

    USGS Publications Warehouse

    Ross, D.S.; Jayaweera, I.

    2002-01-01

    The hydrothermolysis of the picrate anion in aqueous solution has been studied at 260-325??C in liquid water. At starting pH values above 12, the disappearance of picrate begins immediately and is first order in OH-. At lower pH, there is an induction period preceding the disappearance, and over the pH range 6.7-11.9 there is no pH dependence in the developed reaction phase. Added borate and silicate salts promote the reaction, suggesting their acting as nucleophiles at hydrothermal conditions. Nitrite is an initial product, while acetate is a final product and reflective of a vigorous oxidative sequence consuming the intermediate products. A reaction sequence consistent with the results at the lower pH includes initiation of a chain process by displacement of nitrite by water, followed by nucleophilic displacement of nitrite by nitrite such that a nitro group is replaced by an O-N=O group. The ester then rapidly hydrolyzes, and the net reaction is the production of an additional nitrite with each cycle. A simple modeling of this system satisfactorily fits the experimental findings. ?? 2002 Elsevier Science B.V. All rights reserved.

  18. Sequential antimicrobial therapy: comparison of the views of microbiologists and pharmacists.

    PubMed

    Smyth, E T; Tillotson, G S

    1998-07-01

    Sequential antimicrobial therapy (SAT) is arousing keen interest in microbiologists and pharmacists. In an attempt to obtain information from these groups regarding the use of SAT in hospitals, an anonymized postal survey was carried out. A SAT questionnaire was circulated to consultant medical microbiologists, clinical microbiologists, and heads of pharmacy departments within the British Isles. Four hundred and forty-seven microbiologists and pharmacists returned completed questionnaires, giving a response rate of 29%. Just over half of medical microbiologists (MM) and pharmacists (PH) indicated that SAT was used in their institution in respiratory medicine, geriatrics, surgery and, significantly, to a lesser degree in paediatrics. The most common infections treated were pneumonia, bronchitis and wound infection. However, there were significant differences between MM and PH, with MM favouring greater use of SAT in peritonitis (P=0.03), septicaemia (P<0.01), bone infection (P<0.01), pyelonephritis (UTI) (P<0.01), and PH favouring use in bronchitis (P<0.01). The ability to take oral fluids or a recognition of no potential absorption problems were key criteria in the decision process leading to the institution of SAT by MM and PH. Significantly more MM favoured employing criteria such as temperature <38 degrees C (P<0.01), no requirement for high tissue concentrations (P=0.02) and evidence of response to i.v. antimicrobial therapy (P<0.01) than PH. The most frequently "switched" antimicrobials were metronidazole, ciprofloxacin and co-amoxiclav. There were more than five times as many MM reporting the use of clindamycin than PH (P<0.01), whereas nearly twice as many PH cited use of cefuroxime (P<0.01). Of those hospitals not employing SAT, most MM and PH concurred that the commonest reason to institute SAT was financial, followed by convenience to patients and staff. However, more PH than MM indicated that protocols (P<0.01) and a reduction in i.v. complications (P<0.01) were important to them. In promoting SAT, MM and PH felt they had the major role. Significantly, each profession felt that the other had a lesser role to play; MM as judged by the PH (P<0.01) and PH as judged by MM (P<0.01). When promoting SAT, both MM and PH felt that "education for clinicians" followed by regular audit was the best way to ensure implementation. However, significant differences arose with PH regarding nurse education (P<0.01), SAT posters (P=0.02), regular review of patients (P=0.04) and patient's notes SAT stickers (P<0.01) as more important to them than MM. Significantly, less MM than PH (P<0.01) insisted that either the i.v. and PO antimicrobials were identical or were from the same group or class when "switching". This survey highlights interesting comparisons between the approaches of MM and PH towards SAT and may indicate ways in which both groups may work together to bring about change.

  19. A crystal-chemical classification of borate structures with emphasis on hydrated borates

    USGS Publications Warehouse

    Christ, C.L.; Clark, J.R.

    1977-01-01

    The rules governing formation of hydrated borate polyanions that were proposed by C.L. Christ in 1960 are critically reviewed and new rules added on the basis of recent crystal structure determinations. Principles and classifications previously published by others are also critically reviewed briefly. The fundamental building blocks from which borate polyanions can be constructed are defined on the basis of the number n of boron atoms, and the fully hydrated polyanions are illustrated. Known structures are grouped accordingly, and a shorthand notation using n and symbols ?? = triangle, T = tetrahedron is introduced so that the polyanions can be easily characterized. For example, 3:??+2T describes [B3O3(OH)5]2-. Correct structural formulas are assigned borates with known structures whereas borates of unknown structure are grouped separately. ?? 1977 Springer-Verlag.

  20. Simultaneous immobilization of borate, arsenate, and silicate from geothermal water derived from mining activity by co-precipitation with hydroxyapatite.

    PubMed

    Sasaki, Keiko; Hayashi, Yoshikazu; Toshiyuki, Kenta; Guo, Binglin

    2018-09-01

    The treatment of the geothermal water discharged through mining activity is a critical issue because the rate of discharge is 12,000 m 3 per day and the discharge contains high concentrations of borate (>20 mg/L) and arsenate (ca. 0.4 mg/L) as well as silicate and carbonate. The simultaneous reduction of borate and arsenate concentrations to acceptable levels was successfully performed by co-precipitation with hydroxyapatite (HAp). Although the coexisting high concentrations of carbonate act as a disturbing element, the co-precipitation equilibrium of borate was shifted to lower values by adjusting the P/Ca molar ratio, and the removal rate of borate was accelerated by using Al 3+ additives, resulting in the efficient reduction of borate within 1 h. The initially immobilized boron in HAp is in the tetragonal form, which probably occupies the hydroxyl sites in HAp, gradually transforming into the trigonal form in the solid state, as interpreted by 1 H NMR and 11 B-NMR. The coexisting silicate was also immobilized in an ellestadite form, as confirmed by 29 Si-NMR measurements. Arsenate and silicate were immobilized before borate in geothermal water. A dissolution assay of borate in the solid residues after co-precipitation with HAp verified the acceptable stability of borate, which is independent of the amount of added Al 3+ . Copyright © 2018 Elsevier Ltd. All rights reserved.

  1. Borates

    USGS Publications Warehouse

    Angulo, M.A.

    2011-01-01

    The article discusses the latest developments in the borates industry, particularly in the U.S., as of June 2011. It claims that the biggest economically feasible deposits of borates are seen in the U.S.' Mojave Desert, the Alpide belt in southern Asia and the Andean belt of South America. Turkish state-owned mining firm Eti Maden AS reported that borates were mainly used in the manufacture of glass, ceramics, fertilizer and detergent in 2009.

  2. Anti-prelog reduction of prochiral carbonyl compounds by Oenococcus oeni in a biphasic system.

    PubMed

    Hu, Jian; Xu, Yan

    2006-07-01

    An aqueous-organic biphasic system was established and used with whole cells of Oenococcus oeni to reduce 2-octanone to (R)-2-octanol. The conversion reached 99% when the Tris/borate buffer was increased from 50 mM to 300 mM in the aqueous phase. In addition, the conversion increased as the log P value of the organic solvent changed from 0.5 to 6.6. Under optimized conditions, the conversion of (R)-2-octanol reached 99% from 0.5 M 2-octanone with an optical purity of 99% e.e. The biphasic system allows the anti-Prelog reduction of aliphatic and aromatic ketones to furnish (R)-configurated alcohols in high optical purity as well.

  3. Development of a novel oxirane-acrylate composite restorative resin material

    NASA Astrophysics Data System (ADS)

    Sripathi Panditaradhyula, Anuhya

    The need for resin with a long clinical life can be satiated through the novel formulation of varying concentrations of oxirane and acrylate monomers with an increase in filler loading in the sample, which will allow the creation of a resin that is less susceptible to chemical degradation along with improved mechanical properties. Various concentrations of oxirane and acrylate monomers with a three-component photoinitiation system, which is capable of both free radical (acrylate) and cationic (oxirane) initiation, are used. The resin composites were placed in the Speedmixer for 30 seconds and gravitation convection oven for one minute, repeated 5-7 times. The resin composites were used to create a 9.525 mm diameter * 1.5875 mm thick resin mold. The mold was then photocured for twenty seconds on both sides using VALO blue LED light. The Rockwell hardness and shore D durometer hardness served as relative measures of bonding between the monomers. The ideal formulation of oxirane and acrylate concentrations were used to perform the Instron 3 point bend test, as well as contact angle determination. The goal is to identify a resin with a clinical life twice that of the resins being used in practice. Potential findings include ideal oxirane and acrylate concentrations with the highest shore D durometer hardness, Rockwell hardness, contact angle values, and Instron 3 point bend test values. Ideal color, transparency and properties of the resin are taken into account. Optimization of oxirane and acrylate monomers, impact while using various filler components (salination, number of fillers), filler particle size variations and variations in using different filler concentrations are observed. Results of using micro and nano-sized monomers are also studied. Addition of fluorinated acrylate monomer to the micro and nano composite was the next goal. A comparison of all the above stated compositions to the control group 70/30 BisTEG was done. A study on the degradation behavior of these specimens were done by placing the respective specimens in distilled water, ascorbic acid (pH=1.5) and NaOH (pH=13). These resins were not fully cured with filler apart from filled 25:75 oxirane: acrylate cured best. Replacing 4-(Octyloxy) phenyl] phenyl iodonium SbF6 (OPPI) with 4-Isopropyl-4'- methyldiphenyl iodonium Tetrakis (pentafluorophenyl borate (Borate) initiator enhanced 24hr oxirane cure. Formulations had greater hardness compared with the controls. The increase in hardness was due to Increase in oxirane functionality, Increase in filler loading and use of acrylate-salinated filler. Modulus and ultimate transverse strength are greater than controls, but did not have statistically significance energy to break. Thus, these composites are as tough as controls and less brittle. They have the higher hydrophobicity than BisGMA: TEGDMA controls. Furthermore, other means of increasing hydrophobicity was explored, because higher the hydrophobicity, higher the resistance to hydrolytic degradation. Further research observations, such as dynamic mechanical analysis, should be carried out in order to determine the molecular interactions and usage of multi-walled, white carbon nanotubes as filler material.

  4. SLC4A11 is an EIPA-sensitive Na+ permeable pHi regulator

    PubMed Central

    Ogando, Diego G.; Jalimarada, Supriya S.; Zhang, Wenlin; Vithana, Eranga N.

    2013-01-01

    Slc4a11, a member of the solute linked cotransporter 4 family that is comprised predominantly of bicarbonate transporters, was described as an electrogenic 2Na+-B(OH)4− (borate) cotransporter and a Na+-2OH− cotransporter. The goal of the current study was to confirm and/or clarify the function of SLC4A11. In HEK293 cells transfected with SLC4A11 we tested if SLC4A11 is a: 1) Na+-HCO3− cotransporter, 2) Na+-OH−(H+) transporter, and/or 3) Na+-B(OH)4− cotransporter. CO2/HCO3− perfusion yielded no significant differences in rate or extent of pHi changes or Na+ flux in SLC4A11-transfected compared with control cells. Similarly, in CO2/HCO3−, acidification on removal of Na+ and alkalinization on Na+ add back were not significantly different between control and transfected indicating that SLC4A11 does not have Na+-HCO3− cotransport activity. In the absence of CO2/HCO3−, SLC4A11-transfected cells showed higher resting intracelllular Na+ concentration ([Na+]i; 25 vs. 17 mM), increased NH4+-induced acidification and increased acid recovery rate (160%) after an NH4 pulse. Na+ efflux and influx were faster (80%) following Na+ removal and add back, respectively, indicative of Na+-OH−(H+) transport by SLC4A11. The increased alkalinization recovery was confirmed in NHE-deficient PS120 cells demonstrating that SLC4A11 is a bonafide Na+-OH−(H+) transporter and not an activator of NHEs. SLC4A11-mediated H+ efflux is inhibited by 5-(N-ethyl-N-isopropyl) amiloride (EIPA; EC50: 0.1 μM). The presence of 10 mM borate did not alter dpHi/dt or ΔpH during a Na+-free pulse in SLC4A11-transfected cells. In summary our results show that SLC4A11 is not a bicarbonate or borate-linked transporter but has significant EIPA-sensitive Na+-OH−(H+) and NH4+ permeability. PMID:23864606

  5. Determination of water-soluble vitamins in multivitamin dietary supplements and in artichokes by micellar electrokinetic chromatography.

    PubMed

    Serni, Enrico; Audino, Valeria; Del Carlo, Sara; Manera, Clementina; Saccomanni, Giuseppe; Macchia, Marco

    2013-01-01

    Several procedures of extraction with solvents for the simultaneous determination of vitamin C and some vitamins belonging to the B group (thiamine, riboflavine, nicotinic acid and nicotinamide) in multivitamin preparations and in artichokes (Cynara cardunculus subsp. scolymus [L.] Hegi) were developed. Different experimental conditions were used, in terms of heat treatment, composition and pH of the extraction mixture, with particular attention to high-temperature steps; purification of the extracts with solid phase extraction and stabilisation through lyophilisation were discussed. Analyses of the extracts were conducted by capillary electrophoresis in micellar electrokinetic chromatography modality. Borate buffer at pH 8.2 was used, and sodium dodecyl sulphate was added to the background electrolyte as surfactant. A range of linearity was determined and calibration curves were plotted for all the analytes.

  6. Synthesis and evaluation of aminoborates derived from boric acid and diols for protecting wood against fungal and thermal degradation

    Treesearch

    George C. Chen

    2008-01-01

    N-methyl amino catechol borate (1), N-methyl amino-4-methyl catechol borate (2), N-methyl amino-4-t-butyl catechol borate (3), and N-methyl amino-2, 3-naphthyl borate (4) were synthesized by reflux of boric acid with a diol in solvent N,N-dimethyl formamide. The aminoborates were characterized by proton nuclear magnetic resonance spectroscopy, FTIR spectroscopy and...

  7. Recent advances in rare earth doped alkali-alkaline earth borates for solid state lighting applications

    NASA Astrophysics Data System (ADS)

    Verma, Shefali; Verma, Kartikey; Kumar, Deepak; Chaudhary, Babulal; Som, Sudipta; Sharma, Vishal; Kumar, Vijay; Swart, Hendrik C.

    2018-04-01

    As a novel class of inorganic phosphor, the alkali-alkaline earth borate phosphors have gained huge attention due to their charming applications in solid-state lighting (SSL) and display devices. The current research drive shows that phosphors based on the alkali-alkaline earth borates have transformed the science and technology due to their high transparency over a broad spectral range, their flexibility in structure and durability for mechanical and high-laser applications. Recent advances in various aspects of rare-earth (RE) doped borate based phosphors and their utilizations in SSL and light emitting diodes are summarized in this review article. Moreover, the present status and upcoming scenario of RE-doped borate phosphors were reviewed in general along with the proper credential from the existing literature. It is believed that this review is a sole compilation of crucial information about the RE-doped borate phosphors in a single platform.

  8. Use of ion-pairing reagent for improving iodine speciation analysis in seaweed by pressure-driven capillary electrophoresis and ultraviolet detection.

    PubMed

    Sun, Jiannan; Wang, Dan; Cheng, Heyong; Liu, Jinhua; Wang, Yuanchao; Xu, Zigang

    2015-01-30

    This study achieved resolution improvement for iodine speciation in the presence of an ion-pairing reagent by a pressure-driven capillary electrophoresis (CE) system. Addition of 0.01mM tetrabutyl ammonium hydroxide (TBAH) as the ion-pairing reagent into the electrophoretic buffer resulted in the complete separation of four iodine species (I(-), IO3(-), mono-iodothyrosine-MIT and di-iodothyrosine-DIT), because of the electrostatic interaction between TBAH and the negatively charged analytes. A +16kV separation voltage was applied along the separation capillary (50μm i.d., 80cm total and 60cm effective) with the inlet grounded. The detection wavelength was fixed at 210nm, and the pressure-driven flow rate was set at 0.12mLmin(-1) with an injected volume of 2μL. The optimal electrolyte consisted of 2mM borate, 2mM TBAH and 80% methanol with pH adjusted to 8.5. Baseline separation of iodine species was achieved within 7min. The detection limits for I(-), IO3(-), MIT and DIT were 0.052, 0.040, 0.032 and 0.025mgL(-1), respectively. The relative standard deviations of peak heights and areas were all below 3% for 5mgL(-1) and 5% for 1mgL(-1). Application of the proposed method was demonstrated by speciation analysis of iodine in two seaweed samples. The developed method offered satisfactory recoveries in the 91-99% range and good precisions (<5%). Good agreement between the determined values by the proposed CE method and the HPLC-ICP-MS method was also obtained. All results proved its great potential in routine analysis of iodine speciation in environmental, food and biological samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Comparative reactivity of TpRu(L)(NCMe)Ph (L = CO or PMe3): impact of ancillary ligand l on activation of carbon-hydrogen bonds including catalytic hydroarylation and hydrovinylation/oligomerization of ethylene.

    PubMed

    Foley, Nicholas A; Lail, Marty; Lee, John P; Gunnoe, T Brent; Cundari, Thomas R; Petersen, Jeffrey L

    2007-05-30

    Complexes of the type TpRu(L)(NCMe)R [L = CO or PMe3; R = Ph or Me; Tp = hydridotris(pyrazolyl)borate] initiate C-H activation of benzene. Kinetic studies, isotopic labeling, and other experimental evidence suggest that the mechanism of benzene C-H activation involves reversible dissociation of acetonitrile, reversible benzene coordination, and rate-determining C-H activation of coordinated benzene. TpRu(PMe3)(NCMe)Ph initiates C-D activation of C6D6 at rates that are approximately 2-3 times more rapid than that for TpRu(CO)(NCMe)Ph (depending on substrate concentration); however, the catalytic hydrophenylation of ethylene using TpRu(PMe3)(NCMe)Ph is substantially less efficient than catalysis with TpRu(CO)(NCMe)Ph. For TpRu(PMe3)(NCMe)Ph, C-H activation of ethylene, to ultimately produce TpRu(PMe3)(eta3-C4H7), is found to kinetically compete with catalytic ethylene hydrophenylation. In THF solutions containing ethylene, TpRu(PMe3)(NCMe)Ph and TpRu(CO)(NCMe)Ph separately convert to TpRu(L)(eta3-C4H7) (L = PMe3 or CO, respectively) via initial Ru-mediated ethylene C-H activation. Heating mesitylene solutions of TpRu(L)(eta3-C4H7) under ethylene pressure results in the catalytic production of butenes (i.e., ethylene hydrovinylation) and hexenes.

  10. Transition and post-transition metal ions in borate glasses: Borate ligand speciation, cluster formation, and their effect on glass transition and mechanical properties.

    PubMed

    Möncke, D; Kamitsos, E I; Palles, D; Limbach, R; Winterstein-Beckmann, A; Honma, T; Yao, Z; Rouxel, T; Wondraczek, L

    2016-09-28

    A series of transition and post-transition metal ion (Mn, Cu, Zn, Pb, Bi) binary borate glasses was studied with special consideration of the cations impact on the borate structure, the cations cross-linking capacity, and more generally, structure-property correlations. Infrared (IR) and Raman spectroscopies were used for the structural characterization. These complementary techniques are sensitive to the short-range order as in the differentiation of tetrahedral and trigonal borate units or regarding the number of non-bridging oxygen ions per unit. Moreover, vibrational spectroscopy is also sensitive to the intermediate-range order and to the presence of superstructural units, such as rings and chains, or the combination of rings. In order to clarify band assignments for the various borate entities, examples are given from pure vitreous B 2 O 3 to meta-, pyro-, ortho-, and even overmodified borate glass compositions. For binary metaborate glasses, the impact of the modifier cation on the borate speciation is shown. High field strength cations such as Zn 2+ enhance the disproportionation of metaborate to polyborate and pyroborate units. Pb 2+ and Bi 3+ induce cluster formation, resulting in PbO n - and BiO n -pseudophases. Both lead and bismuth borate glasses show also a tendency to stabilize very large superstructural units in the form of diborate polyanions. Far-IR spectra reflect on the bonding states of modifier cations in glasses. The frequency of the measured cation-site vibration band was used to obtain the average force constant for the metal-oxygen bonding, F M-O . A linear correlation between glass transition temperature (T g ) and F M-O was shown for the metaborate glass series. The mechanical properties of the glasses also correlate with the force constant F M-O , though for cations of similar force constant the fraction of tetrahedral borate units (N 4 ) strongly affects the thermal and mechanical properties. For paramagnetic Cu- and Mn-borate glasses, N 4 was determined from the IR spectra after deducing the relative absorption coefficient of boron tetrahedral versus boron trigonal units, α = α 4 /α 3 , using NMR literature data of the diamagnetic glasses.

  11. Production of o-diphenols by immobilized mushroom tyrosinase.

    PubMed

    Marín-Zamora, María Elisa; Rojas-Melgarejo, Francisco; García-Cánovas, Francisco; García-Ruiz, Pedro Antonio

    2009-01-15

    The o-diphenols 4-tert-butyl-catechol, 4-methyl-catechol, 4-methoxy-catechol, 3,4-dihydroxyphenylpropionic acid and 3,4-dihydroxyphenylacetic acid were produced from the corresponding monophenols (4-tert-butyl-phenol, 4-methyl-phenol, 4-methoxy-phenol, p-hydroxyphenylpropionic acid and p-hydroxyphenylacetic acid) using immobilized mushroom tyrosinase from Agaricus bisporus. In all cases the yield was R(diphenol)> or =88-96%, which, according to the literature, is the highest yield so far, obtained using tyrosinase. The reaction was carried out in 0.5M borate buffer pH 9.0 which was used to minimize the diphenolase activity of tyrosinase by complexing the o-diphenols generated. Hydroxylamine and ascorbic acid were also present in the reaction medium, the former being used to reduce mettyrosinase to deoxytyrosinase, closing the catalytic cycle, and the latter to reduce the o-quinone produced to o-diphenol. Inactivation of the tyrosinase by ascorbic acid was also minimized due to the formation of an ascorbic acid-borate complex. Concentrations of the o-diphenolic compounds obtained at several reaction times were determined by gas chromatography-mass spectrometry (GC-MS) and UV-vis spectroscopy. The experimental results are discussed.

  12. Substituted benzotriazoles as inhibitors of copper corrosion in borate buffer solutions

    NASA Astrophysics Data System (ADS)

    Agafonkina, M. O.; Andreeva, N. P.; Kuznetsov, Yu. I.; Timashev, S. F.

    2017-08-01

    The adsorption of substituted 1,2,3-benzotriazoles (R-BTAs) onto copper is measured via ellipsometry in a pure borate buffer (pH 7.4) and satisfactorily described by Temkin's isotherm. The adsorption free energy (-Δ G a 0 ) values of these azoles are determined. The (-Δ G a 0 ) values are found to rise as their hydrophobicity, characterized by the logarithm of the partition coefficient of a substituted BTA in a model octanol-water system (log P), grows. The minimum concentration sufficient for the spontaneous passivation of copper ( C min) and a shift in the potential of local copper depassivation with chlorides ( E pt) after an azole is added to the solution (i.e., Δ E = E pt in - E pt backgr characterizing the ability of its adsorption to stabilize passivation) are determined in the same solution containing a corrosion additive (0.01M NaCl) for each azole under study. Both criteria of the passivating properties of azoles (log C min and Δ E) are shown to correlate linearly with log P, testifying to the role played by surface activity of this family of organic inhibitors in protecting copper in an aqueous solution.

  13. Self-assembled 3D zinc borate florets via surfactant assisted synthesis under moderate pressures: Process temperature dependent morphology study

    NASA Astrophysics Data System (ADS)

    Mahajan, Dhiraj S.; Deshpande, Tushar; Bari, Mahendra L.; Patil, Ujwal D.; Narkhede, Jitendra S.

    2018-04-01

    In the present study, we prepared zinc borates using aqueous phase synthesis under moderate pressures (MP) (<150 psi) with ethanol as a co-solvent in the presence of a quaternary ammonium surfactant-Cetyltrimethylammonium bromide (CTAB). 3D morphologies of self-assembled zinc borate (Zn(H2O)B2O4 · 0.12 H2O, Zn3B6O12 · 3.5H2O, ZnB2O4) resembling flower-like structures were obtained by varying temperature under moderate pressure conditions. Synthesized zinc borates’ florets were morphologically characterized by Field Emission Scanning Electron Microscopy. The x-ray diffractions of borate species reveal rhombohydra, monoclinic and cubic phases of zinc borate crystals as a function of process temperature. Additionally, thermal analysis confirms excellent dehydration/degradation behavior for the zinc borate crystals synthesized at moderate pressures and elevated temperatures and could be utilized as potential flame retardant fillers in the polymer matrices.

  14. Bioactive borate glass coatings for titanium alloys.

    PubMed

    Peddi, Laxmikanth; Brow, Richard K; Brown, Roger F

    2008-09-01

    Bioactive borate glass coatings have been developed for titanium and titanium alloys. Glasses from the Na(2)O-CaO-B(2)O(3) system, modified by additions of SiO(2), Al(2)O(3), and P(2)O(5), were characterized and compositions with thermal expansion matches to titanium were identified. Infrared and X-ray diffraction analyses indicate that a hydroxyapatite surface layer forms on the borate glasses after exposure to a simulated body fluid for 2 weeks at 37 degrees C; similar layers form on 45S5 Bioglass((R)) exposed to the same conditions. Assays with MC3T3-E1 pre-osteoblastic cells show the borate glasses exhibit in vitro biocompatibility similar to that of the 45S5 Bioglass((R)). An enameling technique was developed to form adherent borate glass coatings on Ti6Al4V alloy, with adhesive strengths of 36 +/- 2 MPa on polished substrates. The results show these new borate glasses to be promising candidates for forming bioactive coatings on titanium substrates.

  15. Functionalization of carbon dioxide and carbon disulfide using a stable uranium(III) alkyl complex.

    PubMed

    Matson, Ellen M; Forrest, William P; Fanwick, Phillip E; Bart, Suzanne C

    2011-04-06

    A rare uranium(III) alkyl complex, Tp*(2)U(CH(2)Ph) (2) (Tp* = hydrotris(3,5-dimethylpyrazolyl)borate), was synthesized by salt metathesis from Tp*(2)UI (1) and KCH(2)Ph and fully characterized using (1)H NMR, infrared, and electronic absorption spectroscopies as well as X-ray crystallography. This complex has a uranium-carbon distance of 2.57(2) Å, which is comparable to other uranium alkyls reported. Treating this compound with either carbon dioxide or carbon disulfide results in insertion into the uranium-carbon bond to generate Tp*(2)U(κ(2)-O(2)CCH(2)Ph) (3) and Tp*(2)U(SC(S)CH(2)Ph) (4), respectively. These species, characterized spectroscopically and by X-ray crystallography, feature new carboxylate and dithiocarboxylate ligands. Analysis by electronic absorption spectroscopy supports the trivalent oxidation state of the uranium center in both of these derivatives. Addition of trimethylsilylhalides (Me(3)SiX; X = Cl, I) to 3 results in the release of the free silyl ester, Me(3)SiOC(O)CH(2)Ph, forming the initial uranium monohalide species, Tp*(2)UX, which can then be used over multiple cycles for the functionalization of carbon dioxide. © 2011 American Chemical Society

  16. Evolution of Spatial pH Distribution in Aqueous Solution induced by Atmospheric Pressure Plasma

    NASA Astrophysics Data System (ADS)

    Takahashi, Shigenori; Mano, Kakeru; Hayashi, Yui; Takada, Noriharu; Kanda, Hideki; Goto, Motonobu

    2016-09-01

    Discharge plasma at gas-liquid interface produces some active species, and then they affect chemical reactions in aqueous solution, where pH of aqueous solution is changed due to redox species. The pH change of aqueous solution is an important factor for chemical reactions. However, spatial pH distribution in a reactor during the discharge has not been clarified yet. Thus, this work focused on spatial pH distribution of aqueous solution when pulsed discharge plasma was generated from a copper electrode in gas phase to aqueous solution in a reactor. Experiments were conducted using positive unipolar pulsed power. The unipolar pulsed voltage at +8.0 kV was applied to the copper electrode and the bottom of the reactor was grounded. The size of the reactor was 80 mm wide, 10 mm deep, and 40 mm high. The electrode was set at distance of 2 mm from the solution surface. Anthocyanins were contained in the aqueous solution as a pH indicator. The change pH solution spread horizontally, and low pH region of 10 mm in depth was formed. After discharge for 10 minutes, the low pH region was diffused toward the bottom of the reactor. After discharge for 60 minutes, the pH of the whole solution decreased.

  17. 40 CFR 180.1121 - Boric acid and its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 24 2014-07-01 2014-07-01 false Boric acid and its salts, borax... salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric anhydride... its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric...

  18. 40 CFR 180.1121 - Boric acid and its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 24 2011-07-01 2011-07-01 false Boric acid and its salts, borax... salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric anhydride... its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric...

  19. 40 CFR 180.1121 - Boric acid and its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 25 2012-07-01 2012-07-01 false Boric acid and its salts, borax... salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric anhydride... its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric...

  20. 40 CFR 180.1121 - Boric acid and its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 25 2013-07-01 2013-07-01 false Boric acid and its salts, borax... salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric anhydride... its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric...

  1. 76 FR 74831 - Aging Management of Stainless Steel Structures and Components in Treated Borated Water

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-12-01

    ... exposed to treated borated water. In response to a request from the Nuclear Energy Institute (NEI), the... NUCLEAR REGULATORY COMMISSION [NRC-2011-0256] Aging Management of Stainless Steel Structures and Components in Treated Borated Water AGENCY: Nuclear Regulatory Commission. ACTION: Draft interim staff...

  2. Structure and luminescence spectra of lutetium and yttrium borates synthesized from ammonium nitrate melt

    NASA Astrophysics Data System (ADS)

    Klassen, Nikolay V.; Shmurak, Semion Z.; Shmyt'ko, Ivan M.; Strukova, Galina K.; Derenzo, Stephen E.; Weber, Marvin J.

    2005-01-01

    Lutetium and yttrium borates doped with europium, terbium, gadolinium, etc. have been synthesized by dissolving initial oxides and nitrates in ammonium nitrate melt and thermal decomposition of the solvent. Annealings in the range of 500-1100°C modified the dimensions of the grains from 2 to 3 nm to more than 100 nm. Significant dependence of the structure of lutetium borate on slight doping with rare earth ions has been found: terbium makes high-temperature vaterite phase preferential at room temperature, whereas europium stabilizes low-temperature calcite phase. Influence of the structure of the borates on the pattern of the luminescence spectra of europium dopant was observed. Possibilities for manufacturing of scintillating lutetium borate ceramics by means of this method of synthesis are discussed.

  3. Angiogenic effects of borate glass microfibers in a rodent model.

    PubMed

    Lin, Yinan; Brown, Roger F; Jung, Steven B; Day, Delbert E

    2014-12-01

    The primary objective of this research was to evaluate the use of bioactive borate-based glass microfibers for angiogenesis in soft tissue repair applications. The effect of these fibers on growth of capillaries and small blood vessels was compared to that of 45S5 silica glass microfibers and sham implant controls. Compressed mats of three types of glass microfibers were implanted subcutaneously in rats and tissues surrounding the implant sites histologically evaluated 2-4 weeks post surgery. Bioactive borate glass 13-93B3 supplemented with 0.4 wt % copper promoted extensive angiogenesis as compared to silica glass microfibers and sham control tissues. The angiogenic responses suggest the copper-containing 13-93B3 microfibers may be effective for treating chronic soft tissue wounds. A second objective was to assess the possible systemic cytotoxicity of dissolved borate ions and other materials released from implanted borate glass microfibers. Cytotoxicity was assessed via histological evaluation of kidney tissue collected from animals 4 weeks after subcutaneously implanting high amounts of the borate glass microfibers. The evaluation of the kidney tissue from these animals showed no evidence of chronic histopathological changes in the kidney. The overall results indicate the borate glass microfibers are safe and effective for soft tissue applications. © 2014 Wiley Periodicals, Inc.

  4. Analysis of Soft Drinks: UV Spectrophotometry, Liquid Chromatography, and Capillary Electrophoresis

    NASA Astrophysics Data System (ADS)

    McDevitt, Valerie L.; Rodriguez, Alejandra; Williams, Kathryn R.

    1998-05-01

    Instrumental analysis students analyze commercial soft drinks in three successive laboratory experiments. First, UV multicomponent analysis is used to determine caffeine and benzoic acid in Mello YelloTM using the spectrophotometer's software and manually by the simultaneous equations method. The following week, caffeine, benzoic acid and aspartame are determined in a variety of soft drinks by reversed-phase liquid chromatography using 45% methanol/55% aqueous phosphate, pH 3.0, as the mobile phase. In the third experiment, the same samples are analyzed by capillary electrophoresis using a pH 9.4 borate buffer. Students also determine the minimum detection limits for all three compounds by both LC and CE. The experiments demonstrate the analytical use and limitations of the three instruments. The reports and prelab quizzes also stress the importance of the chemistry of the three compounds, especially the relationships of acid/base behavior and polarity to the LC and CE separations.

  5. Determination of phenolic constituents of biological interest in red wine by capillary electrophoresis with electrochemical detection.

    PubMed

    Peng, Youyuan; Chu, Qingcui; Liu, Fanghua; Ye, Jiannong

    2004-01-28

    A simultaneous determination of trans-resveratrol, (-)-epicatechin, and (+)-catechin in red wine by capillary electrophoresis with electrochemical detection (CE-ED) is reported. The effects of the potential of the working electrode, pH and concentration of running buffer, separation voltage, and injection time on CE-ED were investigated. Under the optimum conditions, the analytes could be separated in a 100 mmol/L borate buffer (pH 9.2) within 20 min. A 300 microm diameter carbon disk electrode has a good response at +0.85 V (vs SCE) for all analytes. The response was linear over 3 orders of magnitude with detection limit (S/N = 3) ranging from 2 x 10(-7) to 5 x 10(-7) g/mL for all analytes. This method has been used for the determination of these analytes in red wine without enrichment, and the assay result was satisfactory.

  6. Activation of carbon-hydrogen bonds via 1,2-addition across M-X (X = OH or NH(2)) bonds of d(6) transition metals as a potential key step in hydrocarbon functionalization: a computational study.

    PubMed

    Cundari, Thomas R; Grimes, Thomas V; Gunnoe, T Brent

    2007-10-31

    Recent reports of 1,2-addition of C-H bonds across Ru-X (X = amido, hydroxo) bonds of TpRu(PMe3)X fragments {Tp = hydridotris(pyrazolyl)borate} suggest opportunities for the development of new catalytic cycles for hydrocarbon functionalization. In order to enhance understanding of these transformations, computational examinations of the efficacy of model d6 transition metal complexes of the form [(Tab)M(PH3)2X]q (Tab = tris-azo-borate; X = OH, NH2; q = -1 to +2; M = TcI, Re(I), Ru(II), Co(III), Ir(III), Ni(IV), Pt(IV)) for the activation of benzene C-H bonds, as well as the potential for their incorporation into catalytic functionalization cycles, are presented. For the benzene C-H activation reaction steps, kite-shaped transition states were located and found to have relatively little metal-hydrogen interaction. The C-H activation process is best described as a metal-mediated proton transfer in which the metal center and ligand X function as an activating electrophile and intramolecular base, respectively. While the metal plays a primary role in controlling the kinetics and thermodynamics of the reaction coordinate for C-H activation/functionalization, the ligand X also influences the energetics. On the basis of three thermodynamic criteria characterizing salient energetic aspects of the proposed catalytic cycle and the detailed computational studies reported herein, late transition metal complexes (e.g., Pt, Co, etc.) in the d6 electron configuration {especially the TabCo(PH3)2(OH)+ complex and related Co(III) systems} are predicted to be the most promising for further catalyst investigation.

  7. Influence of calcium, iron and pH on phosphate availability for microbial mineralization of organic chemicals

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

    Robertson, B.K.; Alexander, M.

    1992-01-01

    A study was conducted to determine some of the factors affecting the P requirement for the biodegradation of p-nitrophenol, phenol, and glucose by Pseudomonas and Corynebacterium strains. Mineralization of glucose was rapid and the Pseudomonas sp. grew extensively in solutions with 5 and 10 mM phosphate, but the rate and extent of degradation were low and the bacterial population never became abundant in media with 0.2 mM phosphate. Similar results were obtained with the Corynebacterium sp. growing in media containing p-nitrophenol or phenol and in solutions with a purified phosphate salt. The extent of growth of the Corynebacterium sp. wasmore » reduced with 2 or 10 mM phosphate in media containing high Fe concentrations. Ca at 5 mM but not 0.5 mM inhibited p-nitrophenol mineralization by the Corynebacterium sp. with phosphate concentrations from 0.2 to 5.0 mM. Phenol mineralization by the Pseudomonas sp. in medium with 0.2 mM phosphate was rapid at pH 5.2, but the bacteria had little or no activity at pH 8.0. In contrast, the activity was greater at pH 8.0 than at pH 5.2 when the culture contained 10 mM phosphate. These effects of pH were similar in media with 5 mM Ca or no added Ca. The authors conclude that the effect of P on bacterial degradation can be influenced by the pH and the concentrations of Fe and Ca.« less

  8. Determination of Conjugation Efficiency of Antibodies and Proteins to the Superparamagnetic Iron Oxide Nanoparticles by Capillary Electrophoresis with Laser-Induced Fluorescence Detection

    NASA Astrophysics Data System (ADS)

    Wang, Fu-Hua; Yoshitake, Takashi; Kim, Do-Kyung; Muhammed, Mamoun; Bjelke, Börje; Kehr, Jan

    2003-04-01

    The method based on capillary electrophoresis with laser-induced fluorescence detection (CE/LIF) was developed for determination of magnetic iron oxide nanoparticles (hydrodynamic diameters of 100 nm) functionalized with molecules containing primary amino groups. The magnetic nanoparticles with carboxylic or aminopropyl-trimethoxysilane groups at their surface were conjugated to the model proteins (bovine serum albumin, BSA; streptavidin or goat anti-rabbit immunoglobulin G, IgG) using carbodiimide as a zero-length cross-linker. The nanoparticle-protein conjugates (hydrodynamic diameter 163-194 nm) were derivatized with naphthalene-2,3-dicarboxaldehyde reagent and separated by CE/LIF with a helium-cadmium laser (excitation at 442 nm, emission at 488 nm). The separations were carried out by using a fused-silica capillary (effective length 48 cm, inner diameter 75 um) and 100 mM sodium borate buffer (pH 9.2), the potential was 30 kV. The detection limit for BSA-conjugate was 1.3 pg/10 nl, i.e. about 20 amol. The present method provides an efficient and fast tool for sensitive determination of the efficacy of biomolecular functionalization of magnetic nanoparticles. The CE/LIF technique requires only negligible sample volumes for analysis, which is especially suitable for controlling the process of preparation of functionalized nanoparticles with unique properties aimed to be used for diagnostic or therapeutic purposes.

  9. Stability evaluation of tramadol enantiomers using a chiral stability-indicating capillary electrophoresis method and its application to pharmaceutical analysis.

    PubMed

    Mohammadi, Ali; Nojavan, Saeed; Rouini, Mohammadreza; Fakhari, Ali Reza

    2011-07-01

    In this study, a chiral stability-indicating CE assay was developed for the stability evaluation of tramadol (TR) enantiomers in commercial tablets using maltodextrin as chiral selector. To investigate the stability-indicating power of the analytical method as well as stability evaluation of TR enantiomers, active pharmaceutical ingredient and TR tablets were subjected to photolysis, heat, oxidation and hydrolysis to conduct stress testing. Best separation for the TR enantiomers was achieved on an uncoated fused-silica capillary at 20 °C using borate buffer (50 mM, pH 10.2) containing 10% m/v maltodextrin. All determinations were performed by a UV detector at 214 nm. A constant voltage of 20 kV was applied to obtain the separation. The range of quantitation for both enantiomers was 5-100 μg/mL (R>0.996). Intra- and inter-day RSD (n=6) were less than 10%. The percent relevant errors were obtained to be less than 4.0 for both enantiomers. The limits of quantitation and detection for both enantiomers were 5 and 1.5 μg/mL, respectively. Degradation products resulting from the stress studies were the same for both enantiomers and did not interfere with the detection of the enantiomers. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Capillary zone electrophoresis method to assay tipranavir capsules and identification of oxidation product and organic impurity by quadrupole-time of flight mass spectrometry.

    PubMed

    Lago, Matheus Wagner; Friedrich, Mariane Lago; Iop, Gabrielle Dineck; de Souza, Thiago Belarmino; de Azevedo Mello, Paola; Adams, Andréa Inês Horn

    2018-05-01

    Tipranavir (TPV) is one of the most recently developed protease inhibitors (PI) and it is specially recommended for treatment-experienced patients who are resistant to other PI drugs. In this work, a simple and friendly environmental CZE stability-indicating method to assay TPV capsules was developed and two TPV organic impurities were identified by high resolution mass spectrometry (HRMS). The optimized analytical conditions were: background electrolyte composed of sodium borate 50mM, pH 9.0 and 5% of methanol; voltage + 28kV; hydrodynamic injection of 5s (100mbar), detection wavelength 240nm, at 25°C. The separation was achieved in a fused silica capillary with 50µm × 40cm (inner diameter × effective length), using furosemide as internal standard. All the validation parameters were met and the method was specific, even in the presence of degradation products and impurities. Oxidation was indicated as the main degradation pathway among those evaluated in this study (acidic, alkaline, thermal, photolytic and oxidative) and it showed a second order degradation kinetic, under the conditions used in this study. The main oxidation product and an organic impurity detected in the standard were characterized by Q-TOF, and both of them correspond to oxidation products of TPV. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Analysis of polyphenols in white wine by CZE with amperometric detection using carbon nanotube-modified electrodes.

    PubMed

    Moreno, Mónica; Arribas, Alberto Sánchez; Bermejo, Esperanza; Zapardiel, Antonio; Chicharro, Manuel

    2011-04-01

    A method for the simultaneous detection of five polyphenols (caffeic, chlorogenic, ferulic and gallic acids and (+)-catechin) by CZE with electrochemical detection was developed. Separation of these polyphenols was performed in a 100 mM borate buffer (pH 9.2) within 15 min. Under optimized separation conditions, the performance of glassy carbon (GC) electrodes modified with multiwalled carbon nanotube layer obtained from different dispersions was examined. GC electrode modified with a dispersion of multi-walled carbon nanotubes (CNT) in polyethylenimine has proven to be the most suitable CNT-based electrode for its application as amperometric detector for the CZE separation of the studied compounds. The excellent electrochemical properties of this electrode allowed the detection of the selected polyphenols at +200 mV and improved the efficiency and the resolution of their CZE separation. Limits of detection below 3.1 μM were obtained with linear ranges covering the 10⁻⁵ to 10⁻⁴  M range. The proposed method has been successfully applied for the detection (ferulic, caffeic and gallic acids and (+)-catechin) and the quantification (gallic acid and (+)-catechin) of polyphenols in two different white wines without any preconcentration step. A remarkable signal stability was observed on the electrode performance despite the presence of potential fouling substances in wine. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Effect of borate glass composition on its conversion to hydroxyapatite and on the proliferation of MC3T3-E1 cells.

    PubMed

    Brown, Roger F; Rahaman, Mohamed N; Dwilewicz, Agatha B; Huang, Wenhai; Day, Delbert E; Li, Yadong; Bal, B Sonny

    2009-02-01

    Glasses containing varying amounts of B(2)O(3) were prepared by partially or fully replacing the SiO(2) in silicate 45S5 bioactive glass with B(2)O(3). The effects of the B(2)O(3) content of the glass on its conversion to hydroxyapatite (HA) and on the proliferation of MC3T3-E1 cells were investigated in vitro. Conversion of the glasses to HA in dilute (20 mM) K(2)HPO(4) solution was monitored using weight loss and pH measurements. Proliferation of MC3T3-E1 cells was determined qualitatively by assay of cell density at the glass interface after incubation for 1 day and 3 days, and quantitatively by fluorescent measurements of total DNA in cultures incubated for 4 days. Higher B(2)O(3) content of the glass increased the conversion rate to HA, but also resulted in a greater inhibition of cell proliferation under static culture conditions. For a given mass of glass in the culture medium, the inhibition of cell proliferation was alleviated by using glasses with lower B(2)O(3) content, by incubating the cell cultures under dynamic rather than static conditions, or by partially converting the glass to HA prior to cell culture.

  13. Method for producing a borohydride

    DOEpatents

    Kong, Peter C [Idaho Falls, ID

    2008-09-02

    A method for producing a borohydride is described and which includes the steps of providing a source of borate; providing a material which chemically reduces the source of the borate to produce a borohydride; and reacting the source of borate and the material by supplying heat at a temperature which substantially effects the production of the borohydride.

  14. Method for producing a borohydride

    DOEpatents

    Kong, Peter C.

    2010-06-22

    A method for producing a borohydride is described that includes the steps of providing a source of borate; providing a material that chemically reduces the source of the borate to produce a borohydride; and reacting the source of the borate and the material by supplying heat at a temperature that substantially effects the production of the borohydride.

  15. The allergens of Schistosoma mansoni

    PubMed Central

    Harris, W. G.

    1973-01-01

    Ten antigen fractions were prepared from adult Schistosoma mansoni by extraction into borate-buffered saline, precipitation at pH 4.6 and separation on Sephadex G-100. The allergic activity of these antigens was assayed by a modified Prausnitz—Kustner type reaction in rats; this test system was found to be sensitive and consistent, allowing differences in allergenicity between antigens to be accurately assessed. Skin-reactivity was detected in both acid-soluble and acid-insoluble fractions. Specific allergenicity was located in peak 3 of a G-100 separation of the acid-soluble fraction and in peaks 1 and 2 of a G-100 separation of the acid-insoluble fraction suggesting that the allergens of S. mansoni were of at least two types: (1) a protein of mol. wt above 150,000 precipitated at pH 4.6, and (2) a protein of mol. wt 20–30,000 remaining in solution at this pH. It is suggested that both these allergens are glycoproteins. Non-specific histamine-releasing agents were found in peak 1 of the G-100 separation of the acid-soluble material. ImagesFIG. 1 PMID:4122335

  16. Improved synthesis of fine zinc borate particles using seed crystals

    NASA Astrophysics Data System (ADS)

    Gürhan, Deniz; Çakal, Gaye Ö.; Eroğlu, İnci; Özkar, Saim

    2009-03-01

    Zinc borate is a flame retardant additive used in polymers, wood applications and textile products. There are different types of zinc borate having different chemical compositions and structures. In this study, the production of zinc borate having the molecular formula of 2ZnO·3B 2O 3·3.5H 2O was reexamined by studying the effects of reaction parameters on the properties of product as well as the reaction kinetics. Production of zinc borate from the reaction of boric acid and zinc oxide in the presence of seed crystals was performed in a continuously stirred, temperature-controlled batch reactor having a volume of 1.5 L. Samples taken in regular time intervals during the experiments were analyzed for the concentration of zinc oxide and boron oxide in the solid as well as for the conversion of zinc oxide to zinc borate versus time. The zinc borate production reaction was fit to the logistic model. The reaction rate, reaction completion time, composition and particle size distribution of zinc borate product were determined by varying the following parameters: the boric acid to zinc oxide ratio (H 3BO 3:ZnO=3:1, 3.5:1, 5:1 and 7:1), the particle size of zinc oxide (10 and 25 μm), stirring rate (275, 400, 800 and 1600 rpm), temperature (75, 85 and 95 °C) and the size of seed crystals (10 and 2 μm). The products were also analyzed for particle size distribution. The experimental results showed that the reaction rate increases with the increase in H 3BO 3:ZnO ratio, particle size of zinc oxide, stirring rate and temperature. Concomitantly, the reaction completion time is decreased by increasing the H 3BO 3:ZnO ratio, stirring rate and temperature. The average particle sizes of the zinc borate products are in the range 4.3-16.6 μm (wet dispersion analysis).

  17. 40 CFR 721.1880 - Borate(1-), tris(acetato-.kappa.O)hydro-, sodium, (T-4)-.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...)hydro-, sodium, (T-4)-. 721.1880 Section 721.1880 Protection of Environment ENVIRONMENTAL PROTECTION... New Uses for Specific Chemical Substances § 721.1880 Borate(1-), tris(acetato-.kappa.O)hydro-, sodium... substance identified as borate(1-), tris(acetato-.kappa.O)hydro-, sodium, (T-4)- (PMN P-00-0922; CAS No...

  18. 40 CFR 721.1880 - Borate(1-), tris(acetato-.kappa.O)hydro-, sodium, (T-4)-.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...)hydro-, sodium, (T-4)-. 721.1880 Section 721.1880 Protection of Environment ENVIRONMENTAL PROTECTION... New Uses for Specific Chemical Substances § 721.1880 Borate(1-), tris(acetato-.kappa.O)hydro-, sodium... substance identified as borate(1-), tris(acetato-.kappa.O)hydro-, sodium, (T-4)- (PMN P-00-0922; CAS No...

  19. 40 CFR 180.1121 - Boric acid and its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Boric acid and its salts, borax (sodium borate decahydrate), disodium octaborate tetrahydrate, boric oxide (boric anhydride), sodium borate and sodium metaborate; exemptions from the requirement of a tolerance. 180.1121 Section 180.1121 Protection of Environment ENVIRONMENTAL PROTECTION...

  20. Preservation of tissue specimens during transport to mycobacteriology laboratories.

    PubMed Central

    Richards, W D; Wright, H S

    1983-01-01

    Chloramine-T and sodium borate solutions were evaluated for their effectiveness in preserving Mycobacterium bovis and controlling the growth of non-mycobacterial contaminants on tissue specimens during transport to laboratories. The number of culturable M. bovis cells in suspension was reduced by 5.1 log10 upon exposure to chloramine-T solution and by less than 1 log10 upon exposure to sodium borate solution for 7 days. Reinoculation of laboratory media (because of overgrowth by non-mycobacterial contaminants) was required for 52.6% of 190 routine bovine tissue specimens shipped refrigerated in chloramine-T solution and for 6.1% of 520 specimens shipped unrefrigerated in sodium borate solution. M. bovis was isolated from bovine tissue stored in sodium borate solution at 23 degrees C for 17 weeks and at 4 degrees C for 25 weeks. Unrefrigerated sodium borate solution has been used successfully to ship tissue specimens to our laboratory for the past 11 years. PMID:6341397

  1. Ultrabright femtosecond source of biphotons based on a spatial mode inverter.

    PubMed

    Jarutis, Vygandas; Juodkazis, Saulius; Mizeikis, Vygantas; Sasaki, Keiji; Misawa, Hiroaki

    2005-02-01

    A method of enhancing the efficiency of entangled biphoton sources based on a type II femtosecond spontaneous parametric downconversion (SPDC) process is proposed and implemented experimentally. Enhancement is obtained by mode inversion of one of the SPDC output beams, which allows the beams to overlap completely, thus maximizing the number of SPDC photon pairs with optimum spatiotemporal overlap. By use of this method, biphoton count rates as high as 16 kHz from a single 0.5-mm-long beta-barium borate crystal pumped by second-harmonic radiation from a Ti:sapphire laser were obtained.

  2. Laboratory evaluation of borate:amine:copper derivatives In wood for fungal decay protection

    Treesearch

    George Chen

    2011-01-01

    This study aimed to evaluate borate:amine:copper derivatives in wood for fungal decay protection as well as the permanence of copper and boron in wood. Each of four derivatives of borate:amine:copper prevented fungal decay in wood. Disodium tetraborate decahydrate (borax):amine:copper derivatives with 0.61-0.63% retention after water leaching prevented decay by...

  3. Corrosion studies of titanium in borated water for TPX

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

    Wilson, D.F.; Pawel, S.J.; DeVan, J.H.

    1995-12-31

    Corrosion testing was performed to demonstrate the compatibility of the titanium vacuum vessel with borated water. Borated water is proposed to fill the annulus of the double wall vacuum vessel to provide effective radiation shielding. Borating the water with 110 grams of boric acid per liter is sufficient to reduce the nuclear heating in the Toroidal Field Coil set and limit the activation of components external to the vacuum vessel. Constant extension rate tensile (CERT) and electrochemical potentiodynamic tests were performed. Results of the CERT tests confirm that stress corrosion cracking is not significant for Ti-6Al4V or Ti-3AI-2.5V. Welded andmore » unwelded specimens were tested in air and in borated water at 150{degree}C. Strength, elongation, and time to failure were nearly identical for all test conditions, and all the samples exhibited ductile failure. Potentiodynamic tests on Ti-6A1-4V and Ti in borated water as a function of temperature showed low corrosion rates over a wide passive potential range. Further, this passivity appeared stable to anodic potentials substantially greater than those expected from MHD effects.« less

  4. Effect of modifying agents on the hydrophobicity and yield of zinc borate synthesized by zinc oxide

    NASA Astrophysics Data System (ADS)

    Acarali, Nil Baran; Bardakci, Melek; Tugrul, Nurcan; Derun, Emek Moroydor; Piskin, Sabriye

    2013-06-01

    The aim of this study was to synthesize zinc borate using zinc oxide, reference boric acid, and reference zinc borate (reference ZB) as the seed, and to investigate the effects of modifying agents and reaction parameters on the hydrophobicity and yield, respectively. The reaction parameters include reaction time (1-5 h), reactant ratio (H3BO3/ZnO by mass: 2-5), seed ratio (seed crystal/(H3BO3+ZnO) by mass: 0-2wt%), reaction temperature (50-120°C), cooling temperature (10-80°C), and stirring rate (400-700 r/min); the modifying agents involve propylene glycol (PG, 0-6wt%), kerosene (1wt%-6wt%), and oleic acid (OA, 1wt%-6wt%) with solvents (isopropyl alcohol (IPA), ethanol, and methanol). The results of reaction yield obtained from either magnetically or mechanically stirred systems were compared. Zinc borate produced was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and contact angle tests to identify the hydrophobicity. In conclusion, zinc borate is synthesized successfully under the optimized reaction conditions, and the different modifying agents with various solvents affect the hydrophobicity of zinc borate.

  5. Novel method for early investigation of bioactivity in different borate bio-glasses

    NASA Astrophysics Data System (ADS)

    Abdelghany, A. M.

    Some ternary borate glasses were prepared and corrosion behavior of such ternary borate glasses after immersion in aqueous dilute phosphate solution was studied using different immersion times. Fourier transform infrared (FTIR) absorption spectral measurements were done before and after immersion in the mentioned solution for extended times up to 2 days to justify the appearance of the characteristic FTIR bands due to calcium phosphate (hydroxyapatite (HA)) which is considered as the potential indication of bioactivity. Experimental IR data confirm the beginning of the appearance of FTIR bands at about 580 and 620 cm-1 after 3 days and the complete resolution with its characteristic split form after 1 week and more. Deconvolution analysis technique (DAT) of the FTIR spectrum was employed to investigate the bioactivity of such ternary borate system after a short period of immersion. The corrosion behavior of such glasses is explained in relation to a suggested hydrolysis followed by direct dissolution mechanism. The ease of dissolution of all the borate glasses constituents explains the formation of calcium phosphate and conversion to crystalline hydroxyapatite within the borate glass matrix. X-ray diffraction may be used to retrace the structural changes and degree of crystallinity of the prepared glasses.

  6. A medium range order structural connection to the configurational heat capacity of borate-silicate mixed glasses.

    PubMed

    Liu, Hao; Smedskjaer, Morten M; Tao, Haizheng; Jensen, Lars R; Zhao, Xiujian; Yue, Yuanzheng

    2016-04-28

    It has been reported that the configurational heat capacity (C(p,conf)) first increases and then becomes saturated with increasing B2O3/SiO2 ratio in borate-silicate mixed glasses. Through Raman spectroscopy measurements, we have, in this work, found an implication for the intermediate range order (IRO) structural connection to the composition dependence of the C(p,conf) of borate-silicate mixed glasses. In the silica-rich compositions, the C(p,conf) rapidly increases with increasing B2O3 content. This is attributed to the increase of the content of the B-O-Si network units ([B2Si2O8](2-)) and 6-membered borate rings with 1 or 2 B(4). In the boron-rich compositions, the C(p,conf) is almost constant, independent of the increase in the B2O3/SiO2 ratio. This is likely attributed to the counteraction between the decrease of the fraction of two types of metaborate groups and the increase of the fraction of other borate superstructural units (particularly 6-membered borate rings). The overall results suggest that the glasses containing more types of superstructural units have a larger C(p,conf).

  7. Investigation of impact of water type on borate ore flotation.

    PubMed

    Ozkan, S G; Acar, A

    2004-04-01

    In this work, the impact of water type on borate ore flotation was investigated, while various physical parameters during flotation were considered in order to compare the results. Two different colemanite samples from Emet deposits of Turkey, named as Emet-A and Emet-B contained 44% B(2)O(3) and 40% B(2)O(3), respectively. The flotation tests were performed at feed particle size range of -210 +20 microm. Optimal consumption values for the reagents were determined as 2000 gt(-1) for AeroPromoter R825 from Cytec Company, a sulphonate type collector, 1500 gt(-1) for Procol CA927 from Allied Colloids Company, a sulphosuccinamate type collector and 100 gt(-1) for AeroFrother 70 from Cytec Company, an alcohol-type frother. In the tests, the impeller speed of the Denver-type flotation machine was set to 1200 rpm and the samples were fed into a litre cell at 25% solid/liquid ratio and at natural pH value of the slurry at room temperature. The flotation results obtained from the tests with use of tap water, demineralised water and the artificial water prepared with Ca(2+) and Mg(2+) cations deliberately added into demineralised water were compared to each other in optimal flotation conditions.

  8. Association of Borderline Pulmonary Hypertension With Mortality and Hospitalization in a Large Patient Cohort: Insights From the Veterans Affairs Clinical Assessment, Reporting, and Tracking Program.

    PubMed

    Maron, Bradley A; Hess, Edward; Maddox, Thomas M; Opotowsky, Alexander R; Tedford, Ryan J; Lahm, Tim; Joynt, Karen E; Kass, Daniel J; Stephens, Thomas; Stanislawski, Maggie A; Swenson, Erik R; Goldstein, Ronald H; Leopold, Jane A; Zamanian, Roham T; Elwing, Jean M; Plomondon, Mary E; Grunwald, Gary K; Barón, Anna E; Rumsfeld, John S; Choudhary, Gaurav

    2016-03-29

    Pulmonary hypertension (PH) is associated with increased morbidity across the cardiopulmonary disease spectrum. Based primarily on expert consensus opinion, PH is defined by a mean pulmonary artery pressure (mPAP) ≥25 mm Hg. Although mPAP levels below this threshold are common among populations at risk for PH, the relevance of mPAP <25 mm Hg to clinical outcome is unknown. We analyzed retrospectively all US veterans undergoing right heart catheterization (2007-2012) in the Veterans Affairs healthcare system (n=21,727; 908-day median follow-up). Cox proportional hazards models were used to evaluate the association between mPAP and outcomes of all-cause mortality and hospitalization, adjusted for clinical covariates. When treating mPAP as a continuous variable, the mortality hazard increased beginning at 19 mm Hg (hazard ratio [HR]=1.183; 95% confidence interval [CI], 1.004-1.393) relative to 10 mm Hg. Therefore, patients were stratified into 3 groups: (1) referent (≤18 mm Hg; n=4,207); (2) borderline PH (19-24 mm Hg; n=5,030); and (3) PH (≥25 mm Hg; n=12,490). The adjusted mortality hazard was increased for borderline PH (HR=1.23; 95% CI, 1.12-1.36; P<0.0001) and PH (HR=2.16; 95% CI, 1.96-2.38; P<0.0001) compared with the referent group. The adjusted hazard for hospitalization was also increased in borderline PH (HR=1.07; 95% CI, 1.01-1.12; P=0.0149) and PH (HR=1.15; 95% CI, 1.09-1.22; P<0.0001). The borderline PH cohort remained at increased risk for mortality after excluding the following high-risk subgroups: (1) patients with pulmonary artery wedge pressure >15 mm Hg; (2) pulmonary vascular resistance ≥3.0 Wood units; or (3) inpatient status at the time of right heart catheterization. These data illustrate a continuum of risk according to mPAP level and that borderline PH is associated with increased mortality and hospitalization. Future investigations are needed to test the generalizability of our findings to other populations and study the effect of treatment on outcome in borderline PH. © 2016 American Heart Association, Inc.

  9. Borate minerals and origin of the RNA world.

    PubMed

    Grew, Edward S; Bada, Jeffrey L; Hazen, Robert M

    2011-08-01

    The RNA World is generally thought to have been an important link between purely prebiotic (>3.7 Ga) chemistry and modern DNA/protein biochemistry. One concern about the RNA World hypothesis is the geochemical stability of ribose, the sugar moiety of RNA. Prebiotic stabilization of ribose by solutions associated with borate minerals, notably colemanite, ulexite, and kernite, has been proposed as one resolution to this difficulty. However, a critical unresolved issue is whether borate minerals existed in sufficient quantities on the primitive Earth, especially in the period when prebiotic synthesis processes leading to RNA took place. Although the oldest reported colemanite and ulexite are 330 Ma, and the oldest reported kernite, 19 Ma, boron isotope data and geologic context are consistent with an evaporitic borate precursor to 2400-2100 Ma borate deposits in the Liaoning and Jilin Provinces, China, as well as to tourmaline-group minerals at 3300-3450 Ma in the Barberton belt, South Africa. The oldest boron minerals for which the age of crystallization could be determined are the metamorphic tourmaline species schorl and dravite in the Isua complex (metamorphism between ca. 3650 and ca. 3600 Ma). Whether borates such as colemanite, ulexite and kernite were present in the Hadean (>4000 Ma) at the critical juncture when prebiotic molecules such as ribose required stabilization depends on whether a granitic continental crust had yet differentiated, because in its absence we see no means for boron to be sufficiently concentrated for borates to be precipitated.

  10. Longitudinal meta-analysis of NIST pH Standard Reference Materials(®): a complement to pH key comparisons.

    PubMed

    Pratt, Kenneth W

    2015-04-01

    This meta-analysis assesses the long-term (up to 70 years) within-laboratory variation of the NIST pH Standard Reference Material® (SRM) tetroxalate, phthalate, phosphate, borate, and carbonate buffers. Values of ΔpH(S), the difference between the certified pH value, pH(S), of each SRM issue and the mean of all pH(S) values for the given SRM at that Celsius temperature, t, are graphed as a function of the SRM issue and t. In most cases, |ΔpH(S)| < 0.004. Deviations from the nominal base:acid amount (mole) ratio of a buffer yield t-independent, constant shifts in ΔpH(S). The mean ΔpH(S) characterizes such deviations. The corresponding mole fraction of impurity in the conjugate buffer component is generally <0.3 %. Changes in the equipment, personnel, materials, and methodology of the pH(S) measurement yield t-dependent variations. The standard deviation of ΔpH(S) characterizes such changes. Standard deviations of ΔpH(S) are generally 0.0015 or less. The results provide a long-term, single-institution complement to the time-specific, multi-institution results of pH key comparisons administered by the Consultative Committee for Metrology in Chemistry and Biology (CCQM).

  11. Mild partial deoxygenation of esters catalyzed by an oxazolinylborate-coordinated rhodium silylene

    DOE PAGES

    Xu, Songchen; Boschen, Jeffery S.; Biswas, Abhranil; ...

    2015-08-17

    An electrophilic, coordinatively unsaturated rhodium complex supported by borate-linked oxazoline, oxazoline-coordinated silylene, and N-heterocyclic carbene donors [{κ³-N,Si,C-PhB(Ox Me²)(Ox Me²SiHPh)Im Mes}Rh(H)CO][HB(C₆F₅)₃] (2, Ox Me² = 4,4-dimethyl-2-oxazoline; Im Mes = 1-mesitylimidazole) is synthesized from the neutral rhodium silyl {PhB(Ox Me²)₂Im Mes}RhH(SiH 2Ph)CO (1) and B(C 6F 5) 3. The unusual oxazoline-coordinated silylene structure in 2 is proposed to form by rearrangement of an unobserved isomeric cationic rhodium silylene species [{PhB(Ox Me²)₂Im Mes}RhH(SiHPh)CO][HB(C₆F₅)₃] generated by H abstraction. Complex 2 catalyzes reductions of organic carbonyl compounds with silanes to give hydrosilylation products or deoxygenation products. The pathway to these reactions is primarily influenced bymore » the degree of substitution of the organosilane. Reactions with primary silanes give deoxygenation of esters to ethers, amides to amines, and ketones and aldehydes to hydrocarbons, whereas tertiary silanes react to give 1,2-hydrosilylation of the carbonyl functionality. In contrast, the strong Lewis acid B(C₆F₅)₃ catalyzes the complete deoxygenation of carbonyl compounds to hydrocarbons with PhSiH₃ as the reducing agent.« less

  12. Mild partial deoxygenation of esters catalyzed by an oxazolinylborate-coordinated rhodium silylene

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

    Xu, Songchen; Boschen, Jeffery S.; Biswas, Abhranil

    An electrophilic, coordinatively unsaturated rhodium complex supported by borate-linked oxazoline, oxazoline-coordinated silylene, and N-heterocyclic carbene donors [{κ³-N,Si,C-PhB(Ox Me²)(Ox Me²SiHPh)Im Mes}Rh(H)CO][HB(C₆F₅)₃] (2, Ox Me² = 4,4-dimethyl-2-oxazoline; Im Mes = 1-mesitylimidazole) is synthesized from the neutral rhodium silyl {PhB(Ox Me²)₂Im Mes}RhH(SiH 2Ph)CO (1) and B(C 6F 5) 3. The unusual oxazoline-coordinated silylene structure in 2 is proposed to form by rearrangement of an unobserved isomeric cationic rhodium silylene species [{PhB(Ox Me²)₂Im Mes}RhH(SiHPh)CO][HB(C₆F₅)₃] generated by H abstraction. Complex 2 catalyzes reductions of organic carbonyl compounds with silanes to give hydrosilylation products or deoxygenation products. The pathway to these reactions is primarily influenced bymore » the degree of substitution of the organosilane. Reactions with primary silanes give deoxygenation of esters to ethers, amides to amines, and ketones and aldehydes to hydrocarbons, whereas tertiary silanes react to give 1,2-hydrosilylation of the carbonyl functionality. In contrast, the strong Lewis acid B(C₆F₅)₃ catalyzes the complete deoxygenation of carbonyl compounds to hydrocarbons with PhSiH₃ as the reducing agent.« less

  13. Laboratory evaluation of borate/amine/zinc formulations for fungal decay protection

    Treesearch

    George C. Chen; Rebecca E. Ibach

    2010-01-01

    The goals of this study were to evaluate borate/amine/zinc formulations in wood for fungal decay protection as well as the permanence of zinc and boron in wood. Wood treated with each of four formulations of borate/amine/zinc prevented or decreased fungal degradation after a 12-week AWPA Standard soil-block test. For non-leached specimens, wood treated with borax/amine...

  14. A mechanistic study of the interaction of water-soluble borate glass with apatite-bound heterocyclic nitrogen-containing bisphosphonates.

    PubMed

    Pramanik, Chandrani; Sood, Parveen; Niu, Li-Na; Yuan, He; Ghoshal, Sushanta; Henderson, Walter; Liu, Yaodong; Jang, Seung Soon; Kumar, Satish; Pashley, David H; Tay, Franklin R

    2016-02-01

    Long-term oral and intravenous use of nitrogen-containing bisphosphonates (N-BPs) is associated with osteonecrosis of the jaw. Although N-BPs bind strongly to bone surfaces via non-covalent bonds, it is possible for extrinsic ions to dissociate bound N-BPs from mineralized bone by competitive desorption. Here, we investigate the effects and mechanism of using an ionic cocktail derived from borate bioactive glass for sequestration of heterocyclic N-BPs bound to apatite. By employing solid-state and solution-state analytical techniques, we confirmed that sequestration of N-BPs from bisphosphonate-bound apatite occurs in the presence of the borate-containing ionic cocktail. Simulations by density functional theory computations indicate that magnesium cation and borate anion are well within the extent of the risedronate or zoledronate anion to form precipitate complexes. The sequestration mechanism is due to the borate anion competing with bisphosphonates for similar electron-deficient sites on the apatite surface for binding. Thus, application of the borate-containing ionic cocktail represents a new topical lavage approach for removing apatite-bound heterocyclic N-BPs from exposed necrotic bone in bisphosphonate-related osteonecrosis of the jaw. Long-term oral consumption and injections of nitrogen-containing bisphosphonates (N-BPs) may result in death of the jaw bone when there is traumatic injury to the bone tissues. To date, there is no effective treatment for such a condition. This work reported the use of an ionic cocktail derived from water-soluble borate glass microfibers to displace the most potent type of N-BPs that are bound strongly to the mineral component on bone surfaces. The mechanism responsible for such an effect has been identified to be cation-mediated complexation of borate anions with negatively-charged N-BPs, allowing them to be released from the mineral surface. This borate-containing cocktail may be developed into a novel topical rinse for removing mineral-bound N-BPs from exposed dead bone. Copyright © 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  15. Stability of cefozopran hydrochloride in aqueous solutions.

    PubMed

    Zalewski, Przemysław; Skibiński, Robert; Paczkowska, Magdalena; Garbacki, Piotr; Talaczyńska, Alicja; Cielecka-Piontek, Judyta; Jelińska, Anna

    2016-01-01

    The influence of pH on the stability of cefozopran hydrochloride (CZH) was investigated in the pH range of 0.44-13.00. Six degradation products were identified with a hybrid ESI-Q-TOF mass spectrometer. The degradation of CZH as a result of hydrolysis was a pseudo-first-order reaction. As general acid-base hydrolysis of CZH was not occurred in the solutions of hydrochloric acid, sodium hydroxide, acetate, borate and phosphate buffers, kobs = kpH because specific acid-base catalysis was observed. Specific acid-base catalysis of CZH consisted of the following reactions: hydrolysis of CZH catalyzed by hydrogen ions (kH+), hydrolysis of dications (k1H2O), monocations (k2H2O) and zwitter ions (k3H2O) and hydrolysis of zwitter ions (k1OH-) and monoanions (k2OH-) of CZH catalyzed by hydroxide ions. The total rate of the reaction was equal to the sum of partial reactions: [Formula: see text]. CZH similarly like other fourth generation cephalosporin was most stable at slightly acidic and neutral pH and less stable in alkaline pH. The cleavage of the β-lactam ring resulting from a nucleophilic attack on the carbonyl carbon in the β-lactam moiety is the preferred degradation pathway of β-lactam antibiotics in aqueous solutions.

  16. The pH-dependent local anesthetic activity of diethylaminoethanol, a procaine metabolite.

    PubMed

    Butterworth, J F; Lief, P A; Strichartz, G R

    1988-04-01

    To test whether the products of procaine hydrolysis have local anesthetic actions resembling those of procaine, the authors compared the ability of procaine and its metabolites diethylaminoethanol (DEAE) and para-aminobenzoic acid (PABA) to block compound action potentials in excised, desheathed frog and rat sciatic nerves. Studies were performed in solutions of impermeant buffers at pH 7.4 (corresponding to mammalian physiologic pH) and at pH 9.2 (close to the pKa of procaine and DEAE) to test for extracellular pH-dependent increases in drug permeation and potency. Both procaine and DEAE inhibited compound action potentials at pH 7.4 and 9.2 in a reversible and dose-dependent manner, and both were approximately ten-fold more potent at pH 9.2 than at pH 7.4, procaine inhibiting the action potential height by 50% at 0.15 mM (pH 9.2) and 1.1 mM (pH 7.4), DEAE at 4 mM (pH 9.2) and 70 mM (pH 7.4). In contrast, PABA at concentrations up to 25 mM and at either pH failed to inhibit compound action potentials, and did not modify the effects of DEAE when both drugs were given together. Procaine produced greater use-dependent block at the higher pH and at higher stimulation rates (100 Hz vs. 40 Hz); DEAE produced almost no use-dependent block. These observations suggest: 1) that DEAE might account for some of the neuropharmacologic activity of procaine in techniques that favor the accumulation of metabolites (such as those requiring large doses or prolonged infusions); and 2) that alkalinization of procaine and DEAE solutions appears to increase their potency for both resting and use-dependent block of action potentials.

  17. Low-energy collisionally activated dissociation of pentose-borate complexes

    NASA Astrophysics Data System (ADS)

    Pepi, Federico; Garzoli, Stefania; Tata, Alessandra; Giacomello, Pierluigi

    2010-01-01

    Pentose-borate 1:1 complexes were generated in the ESI source of a triple quadrupole and ion trap mass spectrometer by electrospray ionization of Na2B4O7 and pentose (arabinose, lyxose, ribose, xylose) 2:1 solution in CH3CN/H2O. The study of their low-energy collisionally activated dissociation (CAD) demonstrated that ribose and lyxose are preferentially complexed at the C2-C3 cis-diol function whereas arabinose and xylose are esterified at the C1-C2 hydroxyl groups. No evidence was found of the stronger affinity for ribose to borate. The ribose probiotic rule can be explained by considering its peculiar capability, among the investigated pentoses, to almost totally complex the borate anion at the C2-C3 hydroxyl group, thus enabling the subsequent stages of nucleotide assembly, such as phosphorylation and linkage to the nucleobases. Finally, the differences observed in the pentose-borate complex CAD spectra can be used for the mass spectrometric discrimination of isomeric pentoses in complex mixtures.

  18. Study on Microstructure and Electrochemical Corrosion Behavior of PEO Coatings Formed on Aluminum Alloy

    NASA Astrophysics Data System (ADS)

    Xiang, N.; Song, R. G.; Li, H.; Wang, C.; Mao, Q. Z.; Xiong, Y.

    2015-12-01

    Plasma electrolytic oxidation (PEO) treated 6063 aluminum alloy was applied in a silicate- and borate-based alkaline solution. The microstructure and electrochemical corrosion behavior were studied by scanning electron microscopy, electrochemical impedance spectroscopy (EIS), and potentiodynamic polarization techniques. The results showed that the silicate-based PEO coating was of a denser structure compared with that of borate-based PEO coating. In addition, the silicate-based PEO coating was composed of more phased (Al9Si) than borate-based PEO coating. The results of corrosion test indicated that the silicate-based PEO coating provided a superior protection to 6063 aluminum alloy substrate, while borate-based PEO coating with a porous structure showed an inferior conservancy against corrosive electrolyte. Furthermore, the EIS tests proved that both coatings were capable to resist the aggressive erosion in 0.5 M NaCl solution after 72 h of immersion. However, the borate-based PEO coating could not provide sufficient protection to the substrate after 72-h immersion in 1 M NaCl solution.

  19. Synthesis of hydrophobic zinc borate nanoflakes and its effect on flame retardant properties of polyethylene

    NASA Astrophysics Data System (ADS)

    Li, Shengli; Long, Beihong; Wang, Zichen; Tian, Yumei; Zheng, Yunhui; Zhang, Qian

    2010-04-01

    Zinc borate (2ZnO·3B 2O 3·3.5H 2O) has relatively high dehydration on-set temperature which property permits processing in a wide range of polymer system. But zinc borate particles are hardly dispersed in a polymer matrix so that they prevent their using in industry. To address this problem, we synthesized hydrophobic zinc borate (2ZnO·3B 2O 3·3.5H 2O) nanoflakes by employing solid-liquid reaction of zinc oxide (ZnO) and boric acid (H 3BO 3) in the presence of oleic acid. This method does not bring pollution. By conducting morphological and microscopic analyses, we found that this compound displayed nanoflake morphology with particle size of around 100-200 nm, thickness less than 100 nm and there were uniform mesopores with the diameter about 10 nm within the particles. Furthermore, our products had an effect on flame retardant of polyethylene, especially when the zinc borate was modified by oleic acid.

  20. Boron

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

    Cozen, L.F.

    1991-05-01

    This paper reports that borate minerals and refined borates are used extensively for the manufacture of vitreous materials such as insulation and textile fiberglasses, borosilicate glass, and porcelain enamels and frits. In North America, these applications are estimated to account for over 54% of the borate consumption. Other substantial uses are in soaps and detergents, metallurgy, fire retardants, industrial biocides, agriculture, and various miscellaneous applications. Reported domestic borate consumption in 1990 was estimated by the U.S. Bureau of Mines to be 320 000 metric tons B{sub 2}O{sub 3} versus 354 000 metric tons B{sub 2}O{sub 3} in 1989. Consumption ismore » projected to remain essentially static in 1991. Imports were estimated by the Bureau to be 50 000 metric tons B{sub 2}O{sub 3} in 1990. Exports of boric acid and refined borates were approximately 650 000 metric tons of product, a 15 000 metric ton increase from the 1989 level. This increase partially offsets the drop in the 1990 consumption level.« less

  1. Effects of oxyanions, natural organic matter, and bacterial cell numbers on the bioreduction of lepidocrocite ({gamma}-FeOOH) and the formation of secondary mineralization products.

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

    O'Loughlin, E. J.; Gorski, C. A.; Scherer, M. M.

    Microbial reduction of Fe(III) oxides results in the production of Fe(II) and may lead to the subsequent formation of Fe(II)-bearing secondary mineralization products including magnetite, siderite, vivianite, chukanovite (ferrous hydroxy carbonate (FHC)), and green rust; however, the factors controlling the formation of specific Fe(II) phases are often not well-defined. This study examined effects of (i) a range of inorganic oxyanions (arsenate, borate, molybdate, phosphate, silicate, and tungstate), (ii) natural organic matter (citrate, oxalate, microbial extracellular polymeric substances [EPS], and humic substances), and (iii) the type and number of dissimilatory iron-reducing bacteria on the bioreduction of lepidocrocite and formation of Fe(II)-bearingmore » secondary mineralization products. The bioreduction kinetics clustered into two distinct Fe(II) production profiles. 'Fast' Fe(II) production kinetics [19-24 mM Fe(II) d-1] were accompanied by formation of magnetite and FHC in the unamended control and in systems amended with borate, oxalate, gellan EPS, or Pony Lake fulvic acid or having 'low' cell numbers. Systems amended with arsenate, citrate, molybdate, phosphate, silicate, tungstate, EPS from Shewanella putrefaciens CN32, or humic substances derived from terrestrial plant material or with 'high' cell numbers exhibited comparatively slow Fe(II) production kinetics [1.8-4.0 mM Fe(II) d-1] and the formation of green rust. The results are consistent with a conceptual model whereby competitive sorption of more strongly bound anions blocks access of bacterial cells and reduced electron-shuttling compounds to sites on the iron oxide surface, thereby limiting the rate of bioreduction.« less

  2. In vitro stimulation of vascular endothelial growth factor by borate-based glass fibers under dynamic flow conditions.

    PubMed

    Chen, Sisi; Yang, Qingbo; Brow, Richard K; Liu, Kun; Brow, Katherine A; Ma, Yinfa; Shi, Honglan

    2017-04-01

    Bioactive borate glass has been recognized to have both hard and soft tissue repair and regeneration capabilities through stimulating both osteogenesis and angiogenesis. However, the underlying biochemical and cellular mechanisms remain unclear. In this study, dynamic flow culturing modules were designed to simulate the micro-environment near the vascular depletion and hyperplasia area in wound-healing regions, thus to better investigate the mechanisms underlying the biocompatibility and functionality of borate-based glass materials. Glass fibers were dosed either upstream or in contact with the pre-seeded cells in the dynamic flow module. Two types of borate glasses, doped with (1605) or without (13-93B3) CuO and ZnO, were studied along with the silicate-based glass, 45S5. Substantial fiber dissolution in cell culture medium was observed, leading to the release of ions (boron, sodium and potassium) and the deposition of a calcium phosphate phase. Different levels of vascular endothelial growth factor secretion were observed from cells exposed to these three glass fibers, and the copper/zinc containing borate 1605 fibers exhibited the most positive influence. These results indicate that dynamic studies of in vitro bioactivity provide useful information to understand the in vivo response to bioactive borate glasses. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Novel method for early investigation of bioactivity in different borate bio-glasses.

    PubMed

    Abdelghany, A M

    2013-01-01

    Some ternary borate glasses were prepared and corrosion behavior of such ternary borate glasses after immersion in aqueous dilute phosphate solution was studied using different immersion times. Fourier transform infrared (FTIR) absorption spectral measurements were done before and after immersion in the mentioned solution for extended times up to 2 days to justify the appearance of the characteristic FTIR bands due to calcium phosphate (hydroxyapatite (HA)) which is considered as the potential indication of bioactivity. Experimental IR data confirm the beginning of the appearance of FTIR bands at about 580 and 620 cm(-1) after 3 days and the complete resolution with its characteristic split form after 1 week and more. Deconvolution analysis technique (DAT) of the FTIR spectrum was employed to investigate the bioactivity of such ternary borate system after a short period of immersion. The corrosion behavior of such glasses is explained in relation to a suggested hydrolysis followed by direct dissolution mechanism. The ease of dissolution of all the borate glasses constituents explains the formation of calcium phosphate and conversion to crystalline hydroxyapatite within the borate glass matrix. X-ray diffraction may be used to retrace the structural changes and degree of crystallinity of the prepared glasses. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Application of quartz crystal microbalance to study the impact of pH and ionic strength on protein-silicone oil interactions.

    PubMed

    Dixit, Nitin; Maloney, Kevin M; Kalonia, Devendra S

    2011-06-30

    In this study, we have used quartz crystal microbalance (QCM) to quantitate the adsorption of a protein on silicone oil coated surfaces as a function of protein concentration, pH and ionic strength using a 5 MHz quartz crystal. Protein adsorption isotherms were generated at different solution pH and ionic strengths. Surface saturation concentrations were selected from adsorption isotherms and used to generate adsorption profiles from pH 3.0 to 9.0, and at ionic strengths of 10 mM and 150 mM. At low ionic strength (10mM) and pH 5.0 (close to the isoelectric point of the protein), maximum adsorption of protein to the silicone oil surface was observed. At higher ionic strength (150 mM), no significant pH influence on adsorption was observed. QCM could be used as a reliable technique to study the binding of proteins to silicone oil coated surfaces. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Effect of individual SCFA on the epithelial barrier of sheep rumen under physiological and acidotic luminal pH conditions.

    PubMed

    Greco, Gabriele; Hagen, Franziska; Meißner, Svenja; Shen, Zanming; Lu, Zhongyan; Amasheh, Salah; Aschenbach, Jörg R

    2018-02-15

    The objective of this study was to investigate whether individual short-chain fatty acids (SCFA) have a different potential to either regulate the formation of the ruminal epithelial barrier (REB) at physiological pH or to damage the REB at acidotic ruminal pH. Ruminal epithelia of sheep were incubated in Ussing chambers on their mucosal side in buffered solutions (pH 6.1 or 5.1) containing no SCFA (control), 30 mM of either acetate, propionate or butyrate, or 100 mM acetate. Epithelial conductance (Gt), short-circuit current (Isc), and fluorescein flux rates were measured over 7 h. Thereafter, mRNA and protein abundance, as well as localization of the tight junction proteins claudin (Cldn)-1, -4, -7, and occludin were analyzed. At pH 6.1, butyrate increased Gt and decreased Isc, with additional decreases in claudin-7 mRNA and protein abundance (each P < 0.05) and disappearance of Cldn-7 immunosignals from the stratum corneum. By contrast, the mRNA abundance of Cldn-1 and/or Cldn-4 were upregulated by 30 mM propionate, 30 mM butyrate, or 100 mM acetate (P < 0.05), however, without coordinated changes in protein abundance. At luminal pH 5.1, neither Gt, Isc, nor TJ protein abundance was altered in the absence of SCFA; only fluorescein flux rates were slightly increased (P < 0.05) and fluorescein signals were no longer restricted to the stratum corneum. The presence of acetate, propionate, or butyrate at pH 5.1 increased fluorescein flux rates and Gt, and decreased Isc (each P < 0.05). Protein abundance of Cldn-1 was decreased in all SCFA treatments but 30 mM butyrate; abundance of Cldn -4 and -7 was decreased in all SCFA treatments but 30 mM acetate; and abundance of occludin was decreased in all SCFA treatments but 30 mM propionate (each P < 0.05). Immunofluorescence staining of SCFA-treated tissues at pH 5.1 showed disappearance of Cldn-7, discontinuous pattern for Cldn-4 and blurring of occludin and Cldn-1 signals in tight junction complexes. The fluorescein dye appeared to freely diffuse into deeper cell layers. The strongest increase in Gt and consistent decreases in the abundance and immunosignals of tight junction proteins were observed with 100 mM acetate at pH 5.1. We conclude that SCFA may contribute differently to the REB formation at luminal pH 6.1 with possible detrimental effects of butyrate at 30 mM concentration. At luminal pH 5.1, all SCFA elicited REB damage with concentration appearing more critical than SCFA species.

  6. In vitro effects of bicarbonate and bicarbonate-lactate buffered peritoneal dialysis solutions on mesothelial and neutrophil function.

    PubMed

    Topley, N; Kaur, D; Petersen, M M; Jörres, A; Williams, J D; Faict, D; Holmes, C J

    1996-02-01

    The inclusion of bicarbonate in the formulation of peritoneal dialysis solutions may avoid the in vitro impairment of certain cell functions seen with acidic lactate-based fluids. The supranormal physiological levels of HCO3- and PCO2 inherent in such formulations may, however, not be biocompatible. This study compared the in vitro biocompatibility of a pH 5.2 lactate-based formulation with formulations containing either 40 mM lactate at pH 7.4, 38 mM HCO3- at pH 6.8 (PCO2 at approximately 240 mm Hg) or 7.4 (PCO2 at approximately 60 mm Hg), and 25 mM HCO3- plus 15 mM lactate at pH 6.8 (PCO2 at approximately 160 mm Hg) or 7.4 (PCO2 at approximately 40 mm Hg). Significant release of lactate dehydrogenase or decreases in ATP content by human peritoneal mesothelial cells (HPMC) and human peripheral polymorphonuclear leukocytes (PMN) after a 30-min exposure to each test solution was only seen with the pH 5.2 lactate-based fluid. The ATP content of HPMC exposed to this fluid returned to control levels after 30 min of recovery in M199 control medium but showed a trend toward decreasing ATP content at 240 min. Similarly, interleukin (IL)-1 beta-induced IL-6 synthesis by HPMC was also only significantly reduced by the pH 5.2 lactate solution. PMN chemiluminescence was unaffected by 30-min exposure to all test solutions except for the pH 5.2 lactate formulation. Staphylococcus epidermidis phagocytosis was reduced to between 46 to 57% of control with all test solutions except the pH 5.2 lactate solution, which further suppressed the chemiluminescence response to 17% of control. These data suggest that short exposure to supranormal physiological levels of HCO3- and PCO2 does not impair HPMC or PMN viability and function. Furthermore, neutral pH lactate-containing solutions show equivalent biocompatibility to bicarbonate-based ones.

  7. Transition metal complexes of oxazolinylboranes and cyclopentadienyl-bis(oxazolinyl)borates: Catalysts for asymmetric olefin hydroamination and acceptorless alcohol decarbonylation

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

    Manna, Kuntal

    The research presented and discussed in this dissertation involves the synthesis of transition metal complexes of oxazolinylboranes and cyclopentadienyl-bis(oxazolinyl)borates, and their application in catalytic enantioselective olefin hydroamination and acceptorless alcohol decarbonylation. Neutral oxazolinylboranes are excellent synthetic intermediates for preparing new borate ligands and also developing organometallic complexes. Achiral and optically active bis(oxazolinyl)phenylboranes are synthesized by reaction of 2-lithio-2-oxazolide and 0.50 equiv of dichlorophenylborane. These bis(oxazolinyl)phenylboranes are oligomeric species in solid state resulting from the coordination of an oxazoline to the boron center of another borane monomer. The treatment of chiral bis(oxazolinyl)phenylboranes with sodium cyclopentadienide provide optically active cyclopentadienyl-bis(oxazolinyl)borates H[PhB(C 5Hmore » 5)(Ox R) 2] [Ox R = Ox 4S-iPr,Me2, Ox 4R-iPr,Me2, Ox 4S-tBu]. These optically active proligands react with an equivalent of M(NMe 2) 4 (M = Ti, Zr, Hf) to afford corresponding cyclopentadienyl-bis(oxazolinyl)borato group 4 complexes {PhB(C 5H 4)(Ox R) 2}M(NMe 2) 2 in high yields. These group 4 compounds catalyze cyclization of aminoalkenes at room temperature or below, providing pyrrolidine, piperidine, and azepane with enantiomeric excesses up to 99%. Our mechanistic investigations suggest a non-insertive mechanism involving concerted C-N/C-H bond formation in the turnover limiting step of the catalytic cycle. Among cyclopentadienyl-bis(oxazolinyl)borato group 4 catalysts, the zirconium complex {PhB(C 5H 4)(Ox4 S-iPr,Me2) 2}Zr(NMe 2) 2 ({S-2}Zr(NMe 2) 2) displays highest activity and enantioselectivity. Interestingly, S-2Zr(NMe 2) 2 also desymmetrizes olefin moieties of achiral non-conjugated aminodienes and aminodiynes during cyclization. The cyclization of aminodienes catalyzed by S-2Zr(NMe 2) 2 affords diastereomeric mixture of cis and trans cylic amines with high diasteromeric ratios and excellent enantiomeric excesses. Similarly, the desymmetrization of alkyne moieties in S-2Zr(NMe 2) 2-catalyzed cyclization of aminodiynes provides corresponding cyclic imines bearing quaternary stereocenters with enantiomeric excesses up to 93%. These stereoselective desymmetrization reactions are significantly affected by concentration of the substrate, temperature, and the presence of a noncyclizable primary amine. In addition, both the diastereomeric ratios and enantiomeric excesses of the products are markedly enhanced by N-deuteration of the substrates. Notably, the cationic zirconium-monoamide complex [ S-2Zr(NMe 2)][B(C 6F 5) 4] obtained from neutral S-2Zr(NMe 2) 2 cyclizes primary aminopentenes providing pyrrolidines with S-configuration; whereas S-2Zr(NMe 2) 2 provides R-configured pyrrolidines. The yttrium complex S-2YCH 2SiMe 3 also affords S-configured pyrrolidines by cyclization of aminopentenes, however the enantiomeric excesses of products are low. An alternative optically active yttrium complex {PhB(C 5H 4)(Ox 4S-tBu) 2}YCH 2SiMe 3 ({S-3}YCH 2SiMe 3) is synthesized, which displays highly enantioselective in the cyclization of aminoalkenes at room temperature affording S-configured cyclic amines with enantiomeric excesses up to 96%. A noninsertive mechanism involving a six-membered transition state by a concerted C-N bond formation and N-H bond cleavage is proposed for {S-3}YCH 2SiMe 3 system based on the kinetic, spectroscopic, and stereochemical features. In the end, a series of bis- and tris(oxazolinyl)borato iridium and rhodium complexes are synthesized with bis(oxazolinyl)phenylborane [PhB(Ox Me2) 2] n, tris(oxazolinyl)borane [B(Ox M) 3]n, and tris(4,4-dimethyl-2-oxazolinyl)phenylborate [To M] -. All these new and other known rhodium and iridium complexes were examined in acceptorless dehydrogenative decarbonylation of primary alcohols. The catalysts survey shows that the compound To MIr(η 4- C 8H 12) is the most active for the conversion of primary alcohols into alkane, H 2, and CO at 180 °C in toluene. Several aliphatic and aromatic primary alcohols are decarbonylated in the catalytic conditions. Furthermore, To MIr(η 4-C 8H 12) is also able to decarbonylate polyols such as ethylene glycol and glycerol to syngas (H 2 and CO) at 180 °C.« less

  8. Method of recycling lithium borate to lithium borohydride through diborane

    DOEpatents

    Filby, Evan E.

    1976-01-01

    This invention provides a method for the recycling of lithium borate to lithium borohydride which can be reacted with water to generate hydrogen for utilization as a fuel. The lithium borate by-product of the hydrogen generation reaction is reacted with hydrogen chloride and water to produce boric acid and lithium chloride. The boric acid and lithium chloride are converted to lithium borohydride through a diborane intermediate to complete the recycle scheme.

  9. Low-energy vibrational dynamics of cesium borate glasses.

    PubMed

    Crupi, C; D'Angelo, G; Vasi, C

    2012-06-07

    Low-temperature specific heat and inelastic light scattering experiments have been performed on a series of cesium borate glasses and on a cesium borate crystal. Raman measurements on the crystalline sample have revealed the existence of cesium rattling modes in the same frequency region where glasses exhibit the boson peak (BP). These localized modes are supposed to overlap with the BP in cesium borate glasses affecting its magnitude. Their influence on the low frequency vibrational dynamics in glassy samples has been considered, and their contribution to the specific heat has been estimated. Evidence for a relation between the changes of the BP induced by the increased amount of metallic oxide and the variations of the elastic medium has been provided.

  10. A Low Spin Manganese(IV) Nitride Single Molecule Magnet

    PubMed Central

    Ding, Mei; Cutsail, George E.; Aravena, Daniel; Amoza, Martín; Rouzières, Mathieu; Dechambenoit, Pierre; Losovyj, Yaroslav; Pink, Maren

    2016-01-01

    Structural, spectroscopic and magnetic methods have been used to characterize the tris(carbene)borate compound PhB(MesIm)3Mn≡N as a four-coordinate manganese(IV) complex with a low spin (S = 1/2) configuration. The slow relaxation of the magnetization in this complex, i.e. its single-molecule magnet (SMM) properties, is revealed under an applied dc field. Multireference quantum mechanical calculations indicate that this SMM behavior originates from an anisotropic ground doublet stabilized by spin-orbit coupling. Consistent theoretical and experiment data show that the resulting magnetization dynamics in this system is dominated by ground state quantum tunneling, while its temperature dependence is influenced by Raman relaxation. PMID:27746891

  11. Catalytic and inhibiting effect of amino acids on the porphyrin metallation reactions

    NASA Astrophysics Data System (ADS)

    Mamardashvili, Galina M.; Zhdanova, Daria Yu.; Mamardashvili, Nugzar Zh.; Koifman, Oskar I.; Dehaen, Wim

    In the present work, using the interaction of tetra-(4-sulfophenyl)porphyrin with copper(II) chloride as an example, it has been shown how different amino acid additives (glycine, valine, leucine and tryptophan) catalyze or inhibit the formation of Cu-porphyrin as a function of the chemical environment (borate buffer (pH7.4), DMSO) and the concentration of the additive. It has been demonstrated that the type of amino acid affects the complexation reaction rate. Possible mechanisms of metalloporphyrin formation and the ways of their acceleration are discussed. Ways in which different amino acid additives catalyze or inhibit the interaction of tetra-(4-sulfophenyl)porphyrin with copper(II) chloride are examined.

  12. Root-zone acidity affects relative uptake of nitrate and ammonium from mixed nitrogen sources

    NASA Technical Reports Server (NTRS)

    Vessey, J. K.; Henry, L. T.; Chaillou, S.; Raper, C. D. Jr; Raper CD, J. r. (Principal Investigator)

    1990-01-01

    Soybean plants (Glycine max [L.] Merr. cv Ransom) were grown for 21 days on 4 sources of N (1.0 mM NO3-, 0.67 mM NO3- plus 0.33 mM NH4+, 0.33 mM NO3- plus 0.67 mM NH4+, and 1.0 mM NH4+) in hydroponic culture with the acidity of the nutrient solution controlled at pH 6.0, 5.5, 5.0, and 4.5. Dry matter and total N accumulation of the plants was not significantly affected by N-source at any of the pH levels except for decreases in these parameters in plants supplied solely with NH4+ at pH 4.5. Shoot-to-root ratios increased in plants which had an increased proportion [correction of proporiton] of NH4(+)-N in their nutrient solutions at all levels of root-zone pH. Uptake of NO3- and NH4+ was monitored daily by ion chromatography as depletion of these ions from the replenished hydroponic solutions. At all pH levels the proportion of either ion that was absorbed increased as the ratio of that ion increased in the nutrient solution. In plants which were supplied with sources of NO3- plus NH4+, NH4+ was absorbed at a ratio of 2:1 over NO3- at pH 6.0. As the pH of the root-zone declined, however, NH4+ uptake decreased and NO3- uptake increased. Thus, the NH4+ to NO3- uptake ratio declined with decreases in root-zone pH. The data indicate a negative effect of declining root-zone pH on NH4+ uptake and supports a hypothesis that the inhibition of growth of plants dependent on NH4(+)-N at low pH is due to a decline in NH4+ uptake and a consequential limitation of growth by N stress.

  13. [Ru(dpp)(3)][(4-Clph)(4)B](2) nanoislands directly assembled on an ITO electrode surface and its electrogenerated chemiluminescence.

    PubMed

    Chen, Ying; Mao, Jianfei; Liu, Chunhua; Yuan, Hongyan; Xiao, Dan; Choi, Martin M F

    2009-01-20

    In this work, solid-state tris(4,7-diphenyl-1,10-phenanthroline) ruthenium(II) ditetrakis(4-chlorophenyl)borate ([Ru(dpp)(3)][(4-Clph)(4)B](2)) nanoislands are assembled spontaneously and simultaneously on an indium-doped tin oxide (ITO) glass electrode surface via a facile dewetting procedure. The fabrication process is very simple and also amenable to mass production. The as-prepared ruthenium complex nanoislands exhibit useful properties. The electrode is more electrochemically active and can produce strong, stable, reproducible solid-state electrochemiluminescence (ECL) signals using oxalate as the coreactant. The self-assembled nanoislands exhibit semiconductor-like broad, red-shift ECL spectrum. More importantly, they extend the application of the ruthenium complex ECL system from the usual alkaline to acidic conditions. The pH turn-off behavior of the ECL is observed for the first time and can serve as an ultrasensitive pH sensor around physiological pH 7.0. The solid-state [Ru(dpp)(3)][(4-Clph)(4)B](2) ECL signal is efficiently inhibited by phenol even at a very low concentration (i.e., 20 nM), thus providing the potential for the determination of phenolic compounds in practical applications.

  14. INVESTIGATION OF ARSENIC SPECIATION ON DRINKING WATER TREATMENT MEDIA UTILIZING AUTOMATED SEQUENTIAL CONTINUOUS FLOW EXTRACTION WITH IC-ICP-MS DETECTION

    EPA Science Inventory

    Three treatment media, used for the removal of arsenic from drinking water, were sequentially extracted using 10mM MgCl2 (pH 8), 10mM NaH2PO4 (pH 7) followed by 10mM (NH4)2C2O4 (pH 3). The media were extracted using an on-line automated continuous extraction system which allowed...

  15. Functional Analysis of Human NF1 in Drosophila

    DTIC Science & Technology

    2007-01-01

    adjusted to 1 mg/ml. Fifty microlitres of 2 assay buffer (50 mM Tris– acetate buffer at pH 7.5, 20 mM MgCl2, 2 mM dithiothreitol, 10 mM creatine phosphate...200 units/ml creatinine kinase, 0.1 mM cAMP at pH 7.5, 0.2 mg/ml bovine serum albumin, 0.02 mg/ml aprotinin, 0.02 mg/ml pepstatin and fresh 0.2 mg

  16. Optimization of pH, temperature and CaCl2 concentrations for Ricotta cheese production from Buffalo cheese whey using Response Surface Methodology.

    PubMed

    Rashid, Abdul Ahid; Huma, Nuzhat; Zahoor, Tahir; Asgher, Muhammad

    2017-02-01

    The recovery of milk constituents from cheese whey is affected by various processing conditions followed during production of Ricotta cheese. The objective of the present investigation was to optimize the temperature (60-90 °C), pH (3-7) and CaCl2 concentration (2·0-6·0 mm) for maximum yield/recovery of milk constituents. The research work was carried out in two phases. In 1st phase, the influence of these processing conditions was evaluated through 20 experiments formulated by central composite design (CCD) keeping the yield as response factor. The results obtained from these experiments were used to optimize processing conditions for maximum yield using response surface methodology (RSM). The three best combinations of processing conditions (90 °C, pH 7, CaCl2 6 mm), (100 °C, pH 5, CaCl2 4 mm) and (75 °C, pH 8·4, CaCl2 4 mm) were exploited in the next phase for Ricotta cheese production from a mixture of Buffalo cheese whey and skim milk (9 : 1) to determine the influence of optimized conditions on the cheese composition. Ricotta cheeses were analyzed for various physicochemical (moisture, fat, protein, lactose, total solids, pH and acidity indicated) parameters during storage of 60 d at 4 ± 2 °C after every 15 d interval. Ricotta cheese prepared at 90 °C, pH 7 and CaCl2 6 mm exhibited the highest cheese yield, proteins and total solids, while high fat content was recorded for cheese processed at 100 °C, pH 5 and 4 mm CaCl2 concentration. A significant storage-related increase in acidity and NPN was recorded for all cheese samples.

  17. Prognostic Effect and Longitudinal Hemodynamic Assessment of Borderline Pulmonary Hypertension.

    PubMed

    Assad, Tufik R; Maron, Bradley A; Robbins, Ivan M; Xu, Meng; Huang, Shi; Harrell, Frank E; Farber-Eger, Eric H; Wells, Quinn S; Choudhary, Gaurav; Hemnes, Anna R; Brittain, Evan L

    2017-12-01

    Pulmonary hypertension (PH) is diagnosed by a mean pulmonary arterial pressure (mPAP) value of at least 25 mm Hg during right heart catheterization (RHC). While several studies have demonstrated increased mortality in patients with mPAP less than that threshold, little is known about the natural history of borderline PH. To test the hypothesis that patients with borderline PH have decreased survival compared with patients with lower mPAP and frequently develop overt PH and to identify clinical correlates of borderline PH. Retrospective cohort study from 1998 to 2014 at Vanderbilt University Medical Center, comprising all patients undergoing routine RHC for clinical indication. We extracted demographics, clinical data, invasive hemodynamics, echocardiography, and vital status for all patients. Patients with mPAP values of 18 mm Hg or less, 19 to 24 mm Hg, and at least 25 mm Hg were classified as reference, borderline PH, and PH, respectively. Mean pulmonary arterial pressure. Our primary outcome was all-cause mortality after adjusting for clinically relevant covariates in a Cox proportional hazards model. Our secondary outcome was the diagnosis of overt PH in patients initially diagnosed with borderline PH. Both outcomes were determined prior to data analysis. We identified 4343 patients (mean [SD] age, 59 [15] years, 51% women, and 86% white) among whom the prevalence of PH and borderline PH was 62% and 18%, respectively. Advanced age, features of the metabolic syndrome, and chronic heart and lung disease were independently associated with a higher likelihood of borderline PH compared with reference patients in a logistic regression model. After adjusting for 34 covariates in a Cox proportional hazards model, borderline PH was associated with increased mortality compared with reference patients (hazard ratio, 1.31; 95% CI, 1.04-1.65; P = .001). The hazard of death increased incrementally with higher mPAP, without an observed threshold. In the 70 patients with borderline PH who underwent a repeated RHC, 43 (61%) had developed overt PH, with a median increase in mPAP of 5 mm Hg (interquartile range, -1 to 11 mm Hg; P < .001). Borderline PH is common in patients undergoing RHC and is associated with significant comorbidities, progression to overt PH, and decreased survival. Small increases in mPAP, even at values currently considered normal, are independently associated with increased mortality. Prospective studies are warranted to determine whether early intervention or closer monitoring improves clinical outcomes in these patients.

  18. Analysis of plant hormones by microemulsion electrokinetic capillary chromatography coupled with on-line large volume sample stacking.

    PubMed

    Chen, Zongbao; Lin, Zian; Zhang, Lin; Cai, Yan; Zhang, Lan

    2012-04-07

    A novel method of microemulsion electrokinetic capillary chromatography (MEEKC) coupled with on-line large volume sample stacking was developed for the analysis of six plant hormones including indole-3-acetic acid, indole-3-butyric acid, indole-3-propionic acid, 1-naphthaleneacetic acid, abscisic acid and salicylic acid. Baseline separation of six plant hormones was achieved within 10 min by using the microemulsion background electrolyte containing a 97.2% (w/w) 10 mM borate buffer at pH 9.2, 1.0% (w/w) ethyl acetate as oil droplets, 0.6% (w/w) sodium dodecyl sulphate as surfactant and 1.2% (w/w) 1-butanol as cosurfactant. In addition, an on-line concentration method based on a large volume sample stacking technique and multiple wavelength detection was adopted for improving the detection sensitivity in order to determine trace level hormones in a real sample. The optimal method provided about 50-100 fold increase in detection sensitivity compared with a single MEEKC method, and the detection limits (S/N = 3) were between 0.005 and 0.02 μg mL(-1). The proposed method was simple, rapid and sensitive and could be applied to the determination of six plant hormones in spiked water samples, tobacco leaves and 1-naphthylacetic acid in leaf fertilizer. The recoveries ranged from 76.0% to 119.1%, and good reproducibilities were obtained with relative standard deviations (RSDs) less than 6.6%.

  19. Sensitive fluorescence HPLC assay for AQ-13, a candidate aminoquinoline antimalarial, that also detects chloroquine and N-dealkylated metabolites.

    PubMed

    Deng, Haiyan; Liu, Huayin; Krogstad, Frances M; Krogstad, Donald J

    2006-04-03

    A sensitive, specific and reproducible fluorescence high performance liquid chromatography (HPLC) assay has been developed for the separate or simultaneous measurement of AQ-13 (a candidate 4-aminoquinoline antimalarial), chloroquine (CQ), and their metabolites in whole blood. After liquid-solid extraction using commercially available extraction cartridges, these two aminoquinolines (AQs) and their metabolites were separated on C18 (Xterra RP18) columns using a mobile phase containing 60% borate buffer (20 mM, pH 9.0) and 40% acetonitrile with isocratic elution at a flow-rate of 1.0 ml/min. The assay uses a biologically inactive 8-chloro-4-aminoquinoline (AQ-18) as its internal standard (IS). There is a linear relationship between the concentrations of these AQs and the peak area ratio (ratio between the peak area of the AQ or metabolite and the peak area of the IS) on the chromatogram. Linear calibration curves with correlation coefficients > or = 0.997 (r2 > or = 0.995, p < 0.001) were obtained for AQ-13, CQ and their N-dealkylated metabolites. Reproducibility of the assay was excellent with coefficients of variation (CVs) < or = 3.8% for AQ-13 and its metabolites, and < or =2.5% for CQ and its metabolites. The sensitivity of the assay is 5 nM using 1.0 ml of blood and a 20 microl injection volume, and can be increased by using 5.0 ml of blood with an injection volume of 40 microl.

  20. Classification of Spanish white wines using their electrophoretic profiles obtained by capillary zone electrophoresis with amperometric detection.

    PubMed

    Arribas, Alberto Sánchez; Martínez-Fernández, Marta; Moreno, Mónica; Bermejo, Esperanza; Zapardiel, Antonio; Chicharro, Manuel

    2014-06-01

    A method was developed for the simultaneous detection of eight polyphenols (t-resveratrol, (+)-catechin, quercetin and p-coumaric, caffeic, sinapic, ferulic, and gallic acids) by CZE with electrochemical detection. Separation of these polyphenols was achieved within 25 min using a 200 mM borate buffer (pH 9.4) containing 10% methanol as separation electrolyte. Amperometric detection of polyphenols was carried out with a glassy carbon electrode (GCE) modified with a multiwalled carbon nanotubes (CNT) layer obtained from a dispersion of CNT in polyethylenimine. The excellent electrochemical properties of this modified electrode allowed the detection and quantification of the selected polyphenols in white wines without any pretreatment step, showing remarkable signal stability despite the presence of potential fouling substances in wine. The electrophoretic profiles of white wines, obtained using this methodology, have proven to be useful for the classification of these wines by means of chemometric multivariate techniques. Principal component analysis and discriminant analysis allowed accurate classification of wine samples on the basis of their grape varietal (verdejo and airén) using the information contained in selected zones of the electropherogram. The utility of the proposed CZE methodology based on the electrochemical response of CNT-modified electrodes appears to be promising in the field of wine industry and it is expected to be successfully extended to classification of a wider range of wines made of other grape varietals. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Evaluation to the effect of B2O3-La2O3-SrO-Na2O-Al2O3 bonding agent on Ti6Al4V-porcelain bonding.

    PubMed

    Zhao, C Q; Wu, S Q; Lu, Y J; Gan, Y L; Guo, S; Lin, J J; Huang, T T; Lin, J X

    2016-10-01

    Low-fusing bonding agents have been widely applied in Ti-ceramics restorations. As an important category, borate bonding agents have great potentials in increasing Ti-porcelain bonding. The purpose of this study is to evaluate the effect of borate bonding agent with addition of Na2O and Al2O3 on Ti6Al4V-porcelain bonding. The thermal properties of borate bonding agent, such as glass transition temperature (Tg) and crystallization peak temperature (Tp), were investigated to establish the sintering process. And the coefficient of thermal expansion (CTE) was to evaluate the matching effect of porcelain to Ti6Al4V. The bond strength was analyzed by the three point bending test. The microscopic morphology of the borate bonding agent surface after sintering, the interface of Ti-borate bonding agent-porcelain, and the fracture mode after porcelains fracture, were studied to assess the influence of borate bonding agent on Ti6Al4V-ceramics. With the addition of Na2O and Al2O3, the porcelain residues were observed increased indication on the Ti6Al4V surface after porcelain fracture and the bond strength was acquired the maximum (49.45MPa) in the bonding agent composition of 75.70B2O3-5.92La2O3-11.84SrO-4.67Na2O-1.87Al2O3. Those results suggest that borate bonding agent is an effective way to improve the Ti6Al4V-ceramics bond strength. And the addition of Na2O and Al2O3 strengthen this effect. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. The Mechanism of Boron Mobility in Wheat and Canola Phloem1[C][OA

    PubMed Central

    Stangoulis, James; Tate, Max; Graham, Robin; Bucknall, Martin; Palmer, Lachlan; Boughton, Berin; Reid, Robert

    2010-01-01

    Low-molecular-weight borate complexes were isolated from canola (Brassica napus) and wheat (Triticum aestivum) phloem exudates, as well as the cytoplasm of the fresh-water alga Chara corallina, and identified using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Phloem exudate was collected from field-grown canola inflorescence stalks by shallow incision, while wheat phloem exudate was collected by aphid stylectomy. Chara cytoplasm was collected by careful manual separation of the cell wall, vacuole, and cytosolic compartments. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry showed the presence of isotopic borate complexes, at mass-to-charge ratio of 690.22/691.22 in the canola and wheat phloem and at 300.11/301.11 in canola phloem and Chara cytoplasm. Using reference compounds, the borate complexes with mass-to-charge ratio 690.22/691.22 was identified as a bis-sucrose (Suc) borate complex in which the 4,6-hydroxyl pairs from the two α-glucopyranoside moieties formed an [L2B]−1 complex. Further investigation using liquid chromatography electrospray ionization triple quadrupole mass spectrometry analysis confirmed the presence of the bis-Suc borate complex in wheat phloem with a concentration up to 220 μm. The 300.11/301.11 complex was putatively identified as a bis-N-acetyl-serine borate complex but its concentration was below the detection limits of the liquid chromatography electrospray ionization triple quadrupole mass spectrometer so could not be quantified. The presence of borate complexes in the phloem provides a mechanistic explanation for the observed phloem boron mobility in canola and wheat and other species that transport Suc as their primary photoassimilate. PMID:20413647

  3. Determination of phosphate concentration and pH in artificial tear drops.

    PubMed

    de Frutos-Lezaun, M; Martínez-Soroa, I; Ostra Beldarrain, M; Egia Zurutuza, A; Irastorza Larburu, M B; Fernandez Iriarte, A; Bachiller Cacho, M P

    2016-08-01

    To determine phosphate concentration and pH in artificial tear eye drops commercially available in Spain. A total of 71 examples of artificial tear preparations were identified in a search of Vademecum 2014 and the Spanish Medicines Agency website. In the 24 artificial tear products containing phosphates, quantification of these was performed by ultraviolet molecular absorption spectrophotometry, and the determination of pH was performed using scan image analysis algorithms of pH strips. Of the 71 artificial tears tested, 24 contained phosphate among their excipients in the data sheet, three of which had a concentration level below detection limit (<0.1mM). The mean phosphate concentration was 17.91±23.87mM. The artificial tear sample containing a higher concentration was Colircusi Humectante (87.1mM). Lubricants based on hypromellose showed the highest phosphate concentration (41.59±32.1mM), showing statistically significant differences compared to povidone (P=.0196) and hyaluronate (P=.0067). Statistically significant differences were found between products containing preservatives (32.39±20.91mM), and preservative free ones (8.49±11.98mM) (P=.0498). However, no difference was found between multidose (20.21±26.91mM) and unidose (9.31±14.39mM) samples, or between brand name (15.44±23.3mM) and generic eye drops (20.81mM). The mean pH was 6.93±0.26 (6.2-7.22). No statistical correlation was detected between phosphate concentration and pH (Spearman's Rho -0.1089 and P=.6125). A total of 24 (33.8%) of the 71 artificial tears contained phosphate. We believe identifying the phosphate concentration of artificial tears is useful information in order to avoid complications in high-risk patients. Copyright © 2016. Published by Elsevier España, S.L.U.

  4. Geochemical characteristics of The Emet (Espey-Hisarcik) borate deposits, Kütahya, Turkey

    NASA Astrophysics Data System (ADS)

    Koçak, İ.; Koç, Ş.

    2018-06-01

    Nearly 72% world's borate reserves are in western part of Turkey. The Emet (Kütahya) deposit is one of these deposits. The Emet borate deposit, like other deposits in western Anatolia, was deposited in Miocene lacustrine environment whose formation coincides with volcanic activity started in Paleogene and lasted to the beginning of Quaternary. The borate ore displaying lenticular structure is alternated with claystone, marl, tuff and thin bedded limestone. The mineral paragenesis is composed of colemanite, hydroboracite, Veatchite, dolomite, calcite, montmorillonite and illite. The Emet borate deposit has been the subject of various geologic and mineralogical studies. In the present study major and trace element contents of 60 borate samples from this deposit are discussed. Among the trace elements, significant enrichment was found in As, Se, Sr, Cs, Sb and Li. Element correlations indicate volcanic source for boron (exhalations and hydrothermal solutions) whilst other elements are found to be derived from a terrestrial source. According to REE data, high Ce concentrations and anomalies are generally indicative of oxygenated depositional environment whilst low Ce contents facilitated the lake waters to be low oxygenated as a result of H2S-rich hydrothermal solutions. The weak negative anomaly detected only in the Hisarcık region is attributed to lacking of Eu contribution to the lake due to insufficient alteration on the continent.

  5. Strontium borate glass: potential biomaterial for bone regeneration

    PubMed Central

    Pan, H. B.; Zhao, X. L.; Zhang, X.; Zhang, K. B.; Li, L. C.; Li, Z. Y.; Lam, W. M.; Lu, W. W.; Wang, D. P.; Huang, W. H.; Lin, K. L.; Chang, J.

    2010-01-01

    Boron plays important roles in many life processes including embryogenesis, bone growth and maintenance, immune function and psychomotor skills. Thus, the delivery of boron by the degradation of borate glass is of special interest in biomedical applications. However, the cytotoxicity of borate glass which arises with the rapid release of boron has to be carefully considered. In this study, it was found that the incorporation of strontium into borate glass can not only moderate the rapid release of boron, but also induce the adhesion of osteoblast-like cells, SaOS-2, thus significantly increasing the cyto-compatibility of borate glass. The formation of multilayers of apatite with porous structure indicates that complete degradation is optimistic, and the spread of SaOS-2 covered by apatite to form a sandwich structure may induce bone-like tissue formation at earlier stages. Therefore, such novel strontium-incorporated borosilicate may act as a new generation of biomaterial for bone regeneration, which not only renders boron as a nutritious element for bone health, but also delivers strontium to stimulate formation of new bones. PMID:20031984

  6. Is Boron a Prebiotic Element? A Mini-review of the Essentiality of Boron for the Appearance of Life on Earth

    NASA Astrophysics Data System (ADS)

    Scorei, Romulus

    2012-02-01

    Boron is probably a prebiotic element with special importance in the so-called "sugars world". Boron is not present on Earth in its elemental form. It is found only in compounds, e.g., borax, boric acid, kernite, ulexite, colemanite and other borates. Volcanic spring waters sometimes contain boron-based acids (e.g., boric, metaboric, tetraboric and pyroboric acid). Borates influence the formation of ribofuranose from formaldehyde that feeds the "prebiotic metabolic cycle". The importance of boron in the living world is strongly related to its implications in the prebiotic origins of genetic material; consequently, we believe that throughout the evolution of life, the primary role of boron has been to provide thermal and chemical stability in hostile environments. The complexation of boric acid and borates with organic cis-diols remains the most probable chemical mechanism for the role of this element in the evolution of the living world. Because borates can stabilize ribose and form borate ester nucleotides, boron may have provided an essential contribution to the "pre-RNA world".

  7. Synthesis and characterization of cerium- and gallium-containing borate bioactive glass scaffolds for bone tissue engineering.

    PubMed

    Deliormanlı, Aylin M

    2015-02-01

    Bioactive glasses are widely used in biomedical applications due to their ability to bond to bone and even to soft tissues. In this study, borate based (13-93B3) bioactive glass powders containing up to 5 wt% Ce2O3 and Ga2O3 were prepared by the melt quench technique. Cerium (Ce+3) and gallium (Ga+3) were chosen because of their low toxicity associated with bacteriostatic properties. Bioactive glass scaffolds were fabricated using the polymer foam replication method. In vitro degradation and bioactivity of the scaffolds were evaluated in SBF under static conditions. Results revealed that the cerium- and gallium-containing borate glasses have much lower degradation rates compared to the bare borate glass 13-93B3. In spite of the increased chemical durability, substituted glasses exhibited a good in vitro bioactive response except when the Ce2O3 content was 5 wt%. Taking into account the high in vitro hydroxyapatite forming ability, borate glass scaffolds containing Ce+3 and Ga+3 therapeutic ions are promising candidates for bone tissue engineering applications.

  8. Thermoluminescence response of rare earth activated zinc lithium borate glass

    NASA Astrophysics Data System (ADS)

    Saidu, A.; Wagiran, H.; Saeed, M. A.; Obayes, H. K.; Bala, A.; Usman, F.

    2018-03-01

    New glasses of zinc lithium borate doped with terbium oxide were synthesized by high temperature solid-state reaction. The amorphous nature of the glasses was confirmed using x-ray diffraction analysis (XRD). Thermoluminescence (TL) response of pure zinc lithium borate (ZLB) and zinc lithium borate doped with terbium (ZLB: Tb) exposed to gamma radiation was measured and compared. There is significant enhancement in the TL yields of ZLB: Tb compared to that of pure ZLB. Effect of varying concentration of dopant (Tb4O7) on the TL response of zinc lithium borate was investigated. 0.3 mol% concentration of Tb exhibited strongest TL intensity. Thermoluminescence curve of the phosphor consist of single isolated peak. The TL response of the new materials to the exposed radiation is linear within 0.5-100 Gy range of dose with sublinearity at the lower region of the curve. High sensitivity was exhibited by the new amorphous materials. Reproducibility, thermal fading and energy response of the proposed TLD were investigated and shows remarkable result that made the phosphor suitable for radiation dosimetry.

  9. Strontium borate glass: potential biomaterial for bone regeneration.

    PubMed

    Pan, H B; Zhao, X L; Zhang, X; Zhang, K B; Li, L C; Li, Z Y; Lam, W M; Lu, W W; Wang, D P; Huang, W H; Lin, K L; Chang, J

    2010-07-06

    Boron plays important roles in many life processes including embryogenesis, bone growth and maintenance, immune function and psychomotor skills. Thus, the delivery of boron by the degradation of borate glass is of special interest in biomedical applications. However, the cytotoxicity of borate glass which arises with the rapid release of boron has to be carefully considered. In this study, it was found that the incorporation of strontium into borate glass can not only moderate the rapid release of boron, but also induce the adhesion of osteoblast-like cells, SaOS-2, thus significantly increasing the cyto-compatibility of borate glass. The formation of multilayers of apatite with porous structure indicates that complete degradation is optimistic, and the spread of SaOS-2 covered by apatite to form a sandwich structure may induce bone-like tissue formation at earlier stages. Therefore, such novel strontium-incorporated borosilicate may act as a new generation of biomaterial for bone regeneration, which not only renders boron as a nutritious element for bone health, but also delivers strontium to stimulate formation of new bones.

  10. Secondary relaxations in supercooled and glassy sucrose-borate aqueous solutions.

    PubMed

    Longinotti, M Paula; Corti, Horacio R; Pablo, Juan J de

    2008-10-13

    The dielectric relaxation spectra of concentrated aqueous solutions of sucrose-borate mixtures have been measured in the supercooled and glassy regions in the frequency range of 40Hz to 2MHz. The secondary (beta) relaxation process was analyzed in the temperature range 183-233K at water contents between 20 and 30wt%. The relaxation times were obtained, and the activation energy of that process was calculated. In order to assess the effect of borate on the relaxation of disaccharide-water mixtures, we also studied the dielectric behavior of sucrose aqueous solutions in the same range of temperatures and water contents. Our findings support the view that, beyond a water content of approximately 20wt%, the secondary relaxation of water-sucrose and water-sucrose-borate mixtures adopts a universal character that can be explained in terms of a simple exponential function of the temperature scaled by the glass transition temperature (T(g)). The behavior observed for water-sucrose and water-sucrose-borate mixtures is compared with previous results obtained in other water-carbohydrate systems.

  11. Medial extrusion of the posterior segment of medial meniscus is a sensitive sign for posterior horn tears.

    PubMed

    Ohishi, Tsuyoshi; Suzuki, Daisuke; Yamamoto, Kazufumi; Banno, Tomohiro; Shimizu, Yuta; Matsuyama, Yukihiro

    2014-01-01

    To evaluate medial extrusion of the posterior segment of the medial meniscus in posterior horn tears. This study enrolled 72 patients without medial meniscal tears (group N), 72 patients with medial meniscal tears without posterior horn tears (group PH-), 44 patients with posterior horn tears of the medial meniscus (group PH+). All meniscal tears were confirmed by arthroscopy. Medial extrusion of the middle segment and the posterior segment was measured on coronal MRIs. Extrusions of both middle and posterior segments in groups PH- and PH+ (middle segment; 2.94±1.51 mm for group PH- and 3.75±1.69 mm for group PH+, posterior segment; 1.85±1.82 mm for group PH- and 4.59±2.74 mm for group PH+) were significantly larger than those in group N (middle segment; 2.04±1.20, posterior segment; 1.21±1.86). Both indicators of extrusion in group PH+ were larger than those in group PH-. In the early OA category, neither middle nor posterior segment in group PH- extruded more than in group N. However, only the posterior segment in group PH+ extruded significantly more than in group N. Multiple lineal regression analyses revealed that posterior segment extrusion was strongly correlated with the posterior horn tears (p<0.001) among groups PH- and PH+. The newly presented indicator for extrusion of the posterior segment of the medial meniscus is associated with posterior horn tears in comparison with the extrusion of the middle segment, especially in the early stages of osteoarthritis. Level II--Diagnostic Study. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. The molecular structure of the borate mineral rhodizite (K, Cs)Al4Be4(B, Be)12O28 - A vibrational spectroscopic study

    NASA Astrophysics Data System (ADS)

    Frost, Ray L.; López, Andrés; Xi, Yunfei; Scholz, Ricardo; Souza, Larissa; Lana, Cristiano

    2014-07-01

    We have studied the borate mineral rhodizite (K, Cs)Al4Be4(B, Be)12O28 using a combination of DEM with EDX and vibrational spectroscopic techniques. The mineral occurs as colorless, gray, yellow to white crystals in the triclinic crystal system. The studied sample is from the Antandrokomby Mine, Sahatany valley, Madagascar. The mineral is prized as a semi-precious jewel. Semi-quantitative chemical composition shows a Al, Ca, borate with minor amounts of K, Mg and Cs. The mineral has a characteristic borate Raman spectrum and bands are assigned to the stretching and bending modes of B, Be and Al. No Raman bands in the OH stretching region were observed.

  13. Effects of starvation on the transport of Escherichia coli K12 in saturated porous media are dependent on pH and ionic strength

    NASA Astrophysics Data System (ADS)

    Xu, S.; Walczak, J. J.; Wang, L.; Bardy, S. L.; Li, J.

    2010-12-01

    In this research, we investigate the effects of starvation on the transport of E. coli K12 in saturated porous media. Particularly, we examine the relationship between such effects and the pH and ionic strength of the electrolyte solutions that were used to suspend bacterial cells. E. coli K12 (ATCC 10798) cells were cultured using either Luria-Bertani Miller (LB-Miller) broth (10 g trypton, 5 g yeast extract and 10 g NaCl in 1 L of deionized water) or LB-Luria broth (10 g tryptone, 5 g yeast extract and 0.5 g NaCl in 1 L of deionized water). Both broths had similar pH (~7.1) but differed in ionic strength (LB-Miller: ~170 mM, LB-Luria: ~ 8 mM). The bacterial cells were then harvested and suspended using one of the following electrolyte solutions: phosphate buffered saline (PBS) (pH ~7.2; ionic strength ~170 mM), 168 mM NaCl (pH ~5.7), 5% of PBS (pH ~ 7.2; ionic strength ~ 8 mM) and 8 mM NaCl (pH ~ 5.7). Column transport experiments were performed at 0, 21 and 48 hours following cell harvesting to evaluate the change in cell mobility over time under “starvation” conditions. Our results showed that 1) starvation increased the mobility of E. coli K12 cells; 2) the most significant change in mobility occurred when bacterial cells were suspended in an electrolyte solution that had different pH and ionic strength (i.e., LB-Miller culture suspended in 8 mM NaCl and LB-Luria culture suspended in 168 mM Nacl); and 3) the change in cell mobility primarily occurred within the first 21 hours. The size of the bacterial cells was measured and the surface properties (e.g., zeta potential, hydrophobicity, cell-bound protein, LPS sugar content, outer membrane protein profiles) of the bacterial cells were characterized. We found that the measured cell surface properties could not fully explain the observed changes in cell mobility caused by starvation.

  14. Potassium extrusion by the moderately halophilic and alkaliphilic methanogen methanolobus taylorii GS-16 and homeostasis of cytosolic pH.

    PubMed Central

    Ni, S; Boone, J E; Boone, D R

    1994-01-01

    Methanolobus taylorii GS-16, a moderately halophilic and alkaliphilic methanogen, grows over a wide pH range, from 6.8 to 9.0. Cells suspended in medium with a pH above 8.2 reversed their transmembrane pH gradient (delta pH), making their cytosol more acidic than the medium. The decreased energy in the proton motive force due to the reversed delta pH was partly compensated by an increased electric membrane potential (delta psi). The cytosolic acidification by M. taylorii at alkaline pH values was accompanied by K+ extrusion. The cytosolic K+ concentration was 110 mM in cells suspended at pH 8.7, but it was 320 mM in cells suspended at neutral pH values. High external K+ concentrations (210 mM or higher) inhibited the growth of M. taylorii at alkaline pH values, perhaps by preventing K+ extrusion. Cells suspended at pH 8.5 and 300 mM external K+ failed to acidify their cytosol. The key observation indicative of the involvement of K+ transport in cytosolic acidification was that valinomycin (0.8 microM), a K+ uniporter, inhibited the growth of M. taylorii only at alkaline pH values. Experiments with resting cells indicated that at alkaline pH values valinomycin uncoupled catabolic reactions from ATP synthesis. Thus, K+/H+ antiport activity was proposed to account for the K+ extrusion and the uncoupling effect of valinomycin at alkaline pH values. Such antiport activity was demonstrated by the sharp drop in pH of the bulk medium of the cell suspension upon the addition of 0.1 M KCl. The antiporter appeared to be active only at alkaline pH values, which was in accordance with a possible role in pH homeostasis by M. taylorii growing at alkaline pH values. PMID:7961499

  15. The internal consistency of the North Sea carbonate system

    NASA Astrophysics Data System (ADS)

    Salt, Lesley A.; Thomas, Helmuth; Bozec, Yann; Borges, Alberto V.; de Baar, Hein J. W.

    2016-05-01

    In 2002 (February) and 2005 (August), the full suite of carbonate system parameters (total alkalinity (AT), dissolved inorganic carbon (DIC), pH, and partial pressure of CO2 (pCO2) were measured on two re-occupations of the entire North Sea basin, with three parameters (AT, DIC, pCO2) measured on four additional re-occupations, covering all four seasons, allowing an assessment of the internal consistency of the carbonate system. For most of the year, there is a similar level of internal consistency, with AT being calculated to within ± 6 μmol kg- 1 using DIC and pH, DIC to ± 6 μmol kg- 1 using AT and pH, pH to ± 0.008 using AT and pCO2, and pCO2 to ± 8 μatm using DIC and pH, with the dissociation constants of Millero et al. (2006). In spring, however, we observe a significant decline in the ability to accurately calculate the carbonate system. Lower consistency is observed with an increasing fraction of Baltic Sea water, caused by the high contribution of organic alkalinity in this water mass, not accounted for in the carbonate system calculations. Attempts to improve the internal consistency by accounting for the unconventional salinity-borate relationships in freshwater and the Baltic Sea, and through application of the new North Atlantic salinity-boron relationship (Lee et al., 2010), resulted in no significant difference in the internal consistency.

  16. Structural and Luminescent property of Holmium doped Borate Glasses

    NASA Astrophysics Data System (ADS)

    Usharani, V. L.; Eraiah, B.

    2018-02-01

    Holmium doped Lithium Lead Borate glasses of different compositions were prepared by melt quenching technique. Fourier transform infrared investigations on lithium lead borate glasses have been made to study the local order and vibrations of atoms in the glass network and it contains mainly BO3 and BO4 structural units. Photoluminescence techniques were employed to investigate the luminescent property of these glasses excited at 451nm. Blue emission have been observed from the transition 495 (5F3 → 5I8).

  17. Mineral resource of the month: boron

    USGS Publications Warehouse

    Crangle, Robert D.

    2012-01-01

    The article offers information on the mineral, boron. Boron compounds, particularly borates, have more commercial applications than its elemental relative which is a metalloid. Making up the 90% of the borates that are used worldwide are colemanite, kernite, tincal, and ulexite. The main borate deposits are located in the Mojave Desert of the U.S., the Tethyan belt in southern Asia, and the Andean belt of South America. Underground and surface mining are being used in gathering boron compounds. INSETS: Fun facts;Boron production and consumption.

  18. Thermal property of holmium doped lithium lead borate glasses

    NASA Astrophysics Data System (ADS)

    Usharani, V. L.; Eraiah, B.

    2018-04-01

    The new glass system of holmium doped lithium lead borate glasses were prepared by conventional melt quenching technique. The thermal stability of the different compositions of Ho3+ ions doped lithium lead borate glasses were studied by using TG-DTA. The Tg values are ranging from 439 to 444 °C with respect to the holmium concentration. Physical parameters like polaron radius(rp), inter-nuclear distance (ri), field strength (F) and polarizability (αm) of oxide ions were calculated using appropriate formulae.

  19. Fabrication and characterization of poly (bisphenol A borate) with high thermal stability

    NASA Astrophysics Data System (ADS)

    Wang, Shujuan; Wang, Xiao; Jia, Beibei; Jing, Xinli

    2017-01-01

    In this work, poly (bisphenol A borate) (PBAB), which has excellent thermal resistance and a high char yield, was synthesized via a convenient A2 + B3 strategy by using bisphenol A (BPA) and boric acid (BA). The chemical reaction between BPA and BA and the chemical structure of PBAB were investigated. The results demonstrate that PBAB consists of aromatic, Ph-O-B and B-O-B structures, as well as a small number of boron hydroxyl groups and phenolic hydroxyl groups. The thermal properties of PBAB were studied by DMA and TGA. The results indicate that the glass transition temperature and char yield are gradually enhanced by increasing the boron content, where the char yield of PBAB at 800 °C in nitrogen (N2) reaches up to 71.3%. It is of particular importance that PBAB show excellent thermal resistance in N2 and air atmospheres. By analysing the pyrolysis of PBAB, the high char yield of PBAB can be attributed to the formation of boron oxide and boron carbide at high temperatures, which reduced the release of volatile carbon dioxide and improved the thermal stability of the carbonization products. This study provides a new perspective on the design of novel boron-containing polymers and possesses significant potential for the improvement of the comprehensive performance of thermosetting resins to broaden their applicability in the field of advanced composites.

  20. High-pressure synthesis and characterization of the first cerium fluoride borate CeB{sub 2}O{sub 4}F

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

    Hinteregger, Ernst; Wurst, Klaus; Tribus, Martina

    2013-08-15

    CeB{sub 2}O{sub 4}F is the first cerium fluoride borate, which is exclusively built up of one-dimensional, infinite chains of condensed trigonal-planar [BO{sub 3}]{sup 3−} groups. This new cerium fluoride borate was synthesized under high-pressure/high-temperature conditions of 0.9 GPa and 1450 °C in a Walker-type multianvil apparatus. The compound crystallizes in the orthorhombic space group Pbca (No. 61) with eight formula units and the lattice parameters a=821.63(5), b=1257.50(9), c=726.71(6) pm, V=750.84(9) Å{sup 3}, R{sub 1}=0.0698, and wR{sub 2}=0.0682 (all data). The structure exhibits a 9+1 coordinated cerium ion, one three-fold coordinated fluoride ion and a one-dimensional chain of [BO{sub 3}]{sup 3−}more » groups. Furthermore, IR spectroscopy, Electron Micro Probe Analysis and temperature-dependent X-ray powder diffraction measurements were performed. - Graphical abstract: A new rare-earth fluoride borate CeB{sub 2}O{sub 4}F could be synthesized under high-pressure/high-temperature conditions of 0.9 °GPa and 1450 °Cin a Walker-type multianvil apparatus. The crystal structure represents a new structure type in the class of rare-earth fluoride borates. The structure exhibits a 9+1 coordinated cerium ion, one three-fold coordinated fluoride ion and a one-dimensional chain of [BO{sub 3}]{sup 3−} groups. A closer view on the ac-plane shows an interesting wave-like modulation of the borate chains. Highlights: • CeB{sub 2}O{sub 4}F is the first fluoride borate exclusively built up of one-dimensional, infinite chains of condensed trigonal-planar [BO{sub 3}]{sup 3−} groups. • CeB{sub 2}O{sub 4}F is the first cerium fluoride borate. • High-pressure conditions were necessary to synthesize CeB{sub 2}O{sub 4}F.« less

  1. On-line focusing of flavin derivatives using Dynamic pH junction-sweeping capillary electrophoresis with laser-induced fluorescence detection.

    PubMed

    Britz-McKibbin, Philip; Otsuka, Koji; Terabe, Shigeru

    2002-08-01

    Simple yet effective methods to enhance concentration sensitivity is needed for capillary electrophoresis (CE) to become a practical method to analyze trace levels of analytes in real samples. In this report, the development of a novel on-line preconcentration technique combining dynamic pH junction and sweeping modes of focusing is applied to the sensitive and selective analysis of three flavin derivatives: riboflavin, flavin mononucleotide (FMN) and flavin adenine dinucleotide (FAD). Picomolar (pM) detectability of flavins by CE with laser-induced fluorescence (LIF) detection is demonstrated through effective focusing of large sample volumes (up to 22% capillary length) using a dual pH junction-sweeping focusing mode. This results in greater than a 1,200-fold improvement in sensitivity relative to conventional injection methods, giving a limit of detection (S/N = 3) of approximately 4.0 pM for FAD and FMN. Flavin focusing is examined in terms of analyte mobility dependence on buffer pH, borate complexation and SDS interaction. Dynamic pH junction-sweeping extends on-line focusing to both neutral (hydrophobic) and weakly acidic (hydrophilic) species and is considered useful in cases when either conventional sweeping or dynamic pH junction techniques used alone are less effective for certain classes of analytes. Enhanced focusing performance by this hyphenated method was demonstrated by greater than a 4-fold reduction in flavin bandwidth, as compared to either sweeping or dynamic pH junction, reflected by analyte detector bandwidths <0.20 cm. Novel on-line focusing strategies are required to improve sensitivity in CE, which may be applied toward more effective biochemical analysis methods for diverse types of analytes.

  2. Autoinducer-2 detection among commensal oral streptococci is dependent on pH and boric acid.

    PubMed

    Cuadra, Giancarlo A; Frantellizzi, Ashley J; Gaesser, Kimberly M; Tammariello, Steven P; Ahmed, Anika

    2016-07-01

    Autoinducer-2, considered a universal signaling molecule, is produced by many species of bacteria; including oral strains. Structurally, autoinducer-2 can exist bound to boron (borated autoinducer-2). Functionally, autoinducer-2 has been linked to important bacterial processes such as virulence and biofilm formation. In order to test production of autoinducer-2 by a given bacterial strain, a bioassay using marine bioluminescent bacteria Vibrio harveyi as a reporter for autoinducer-2 has been designed. We hypothesize that pH adjustment and addition of boron are required for optimal bioluminescence and accurate autoinducer-2 detection. Using this reporter strain we tested autoinducer-2 activity from two oral commensal species, Streptococcus gordonii DL1 and Streptococcus oralis 34. Spent broth was collected and adjusted to pH 7.5 and supplemented with boric acid prior to measuring autoinducer- 2 activity. Results show that low pH inhibits bioluminescence of the reporter strain, but pH 7.5 allows for bioluminescence induction and proper readings of autoinducer-2 activity. Addition of boric acid also has a positive effect on bioluminescence allowing for a more sensitive detection of autoinducer-2 activity. Our data suggests that although autoinducer-2 is present in spent broth, low pH and/or low levels of boric acid become an obstacle for proper autoinducer-2 detection. For proper autoinducer-2 detection, we propose a protocol using this bioassay to include pH adjustment and boric acid addition to spent broth. Studies on autoinducer-2 activity in several bacteria species represent an important area of study as this universal signaling molecule is involved in critical bacterial phenotypes such as virulence and biofilm formation.

  3. Green colorants based on energetic azole borates.

    PubMed

    Glück, Johann; Klapötke, Thomas M; Rusan, Magdalena; Stierstorfer, Jörg

    2014-11-24

    The investigation of green-burning boron-based compounds as colorants in pyrotechnic formulations as alternative for barium nitrate, which is a hazard to health and to the environment, is reported. Metal-free and nitrogen-rich dihydrobis(5-aminotetrazolyl)borate salts and dihydrobis(1,3,4-triazolyl)borate salts have been synthesized and characterized by NMR spectroscopy, elemental analysis, mass spectrometry, and vibrational spectroscopy. Their thermal and energetic properties have been determined as well. Several pyrotechnic compositions using selected azolyl borate salts as green colorants were investigated. Formulations with ammonium dinitramide and ammonium nitrate as oxidizers and boron and magnesium as fuels were tested. The burn time, dominant wavelength, spectral purity, luminous intensity, and luminous efficiency as well as the thermal and energetic properties of these compositions were measured. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. The molecular structure of the borate mineral rhodizite (K, Cs)Al4Be4(B, Be)12O28--a vibrational spectroscopic study.

    PubMed

    Frost, Ray L; López, Andrés; Xi, Yunfei; Scholz, Ricardo; Souza, Larissa; Lana, Cristiano

    2014-07-15

    We have studied the borate mineral rhodizite (K, Cs)Al4Be4(B, Be)12O28 using a combination of DEM with EDX and vibrational spectroscopic techniques. The mineral occurs as colorless, gray, yellow to white crystals in the triclinic crystal system. The studied sample is from the Antandrokomby Mine, Sahatany valley, Madagascar. The mineral is prized as a semi-precious jewel. Semi-quantitative chemical composition shows a Al, Ca, borate with minor amounts of K, Mg and Cs. The mineral has a characteristic borate Raman spectrum and bands are assigned to the stretching and bending modes of B, Be and Al. No Raman bands in the OH stretching region were observed. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. The effect of pH and buffer concentration on anode biofilms of Thermincola ferriacetica.

    PubMed

    Lusk, Bradley G; Parameswaran, Prathap; Popat, Sudeep C; Rittmann, Bruce E; Torres, Cesar I

    2016-12-01

    We assessed the effects of pH and buffer concentration on current production and growth of biofilms of Thermincola ferriacetica - a thermophilic, Gram-positive, anode-respiring bacterium (ARB) - grown on anodes poised at a potential of -0.06V vs. SHE in microbial electrolysis cells (MECs) at 60°C. T. ferriacetica generated current in the pH range of 5.2 to 8.3 with acetate as the electron donor and 50mM bicarbonate buffer. Maximum current density was reduced by ~80% at pH5.2 and ~14% at 7.0 compared to pH8.3. Increasing bicarbonate buffer concentrations from 10mM to 100mM resulted in an increase in the current density by 40±6%, from 6.8±1.1 to 11.2±2.7Am(-2), supporting that more buffer alleviated pH depression within T. ferriacetica biofilms. Confocal laser scanning microscopy (CLSM) images indicated that higher bicarbonate buffer concentrations resulted in larger live biofilm thicknesses: from 68±20μm at 10mM bicarbonate to >150μm at 100mM, supporting that buffer availability was a strong influence on biofilm thickness. In comparison to mesophilic Geobacter sulfurreducens biofilms, the faster transport rates at higher temperature and the ability to grow at relatively lower pH allowed T. ferriacetica to produce higher current densities with lower buffer concentrations. Published by Elsevier B.V.

  6. Kinetic evidence for the interactive inhibition of laccase from Trametes versicolor by pH and chloride.

    PubMed

    Raseda, Nasrin; Hong, Soonho; Kwon, O Yul; Ryu, Keungarp

    2014-12-28

    The interactive inhibitory effects of pH and chloride on the catalysis of laccase from Trametes versicolor were investigated by studying the alteration of inhibition characteristics of sodium chloride at different pHs for the oxidation of 2,2'-azino-bis (3-ethylbenzthiazoline-6-sulfonic acid). At pH 3.0, the addition of sodium chloride (50 mM) brought about a 40-fold increase in Km(app) and a 4-fold decrease in Vmax(app). As the pH increased to 7.0, the inhibitory effects of sodium chloride became significantly weakened. The mixed-inhibition mechanism was successfully used to quantitatively estimate the competitive and uncompetitive inhibition strengths by chloride at two different pHs (pH 3.0 and 6.0). At pH 3.0, the competitive inhibition constant, Ki, was 0.35 mM, whereas the uncompetitive inhibition constant, Ki', was 18.1 mM, indicating that the major cause of the laccase inhibition by chloride is due to the competitive inhibition step. At a higher pH of 6.0, where the inhibition of the laccase by hydroxide ions takes effect, the inhibition of the laccase by chloride diminished to a great extent, showing increased values of both the competitive inhibition constant (Ki= 23.7 mM) and uncompetitive inhibition constant (Ki' = 324 mM). These kinetic results evidenced that the hydroxide anion and chloride share a common mechanism to inhibit the laccase activity.

  7. Influence of solution chemistry on the inactivation of particle-associated viruses by UV irradiation.

    PubMed

    Feng, Zhe; Lu, Ruiqing; Yuan, Baoling; Zhou, Zhenming; Wu, Qingqing; Nguyen, Thanh H

    2016-12-01

    MS2 inactivation by UV irradiance was investigated with the focus on how the disinfection efficacy is influenced by bacteriophage MS2 aggregation and adsorption to particles in solutions with different compositions. Kaolinite and Microcystis aeruginosa were used as model inorganic and organic particles, respectively. In the absence of model particles, MS2 aggregates formed in either 1mM NaCl at pH=3 or 50-200mM ionic strength CaCl 2 solutions at pH=7 led to a decrease in the MS2 inactivation efficacy because the virions located inside the aggregate were protected from the UV irradiation. In the presence of kaolinite and Microcystis aeruginosa, MS2 adsorbed onto the particles in either 1mM NaCl at pH=3 or 50-200mM CaCl 2 solutions at pH=7. In contrast to MS2 aggregates formed without the presence of particles, more MS2 virions adsorbed on these particles were exposed to UV irradiation to allow an increase in MS2 inactivation. In either 1mM NaCl at pH from 4 to 8 or 2-200mM NaCl solutions at pH=7, the absence of MS2 aggregation and adsorption onto the model particles explained why MS2 inactivation was not influenced by pH, ionic strength, and the presence of model particles in these conditions. The influence of virus adsorption and aggregation on the UV disinfection efficiency found in this research suggests the necessity of accounting for particles and cation composition in virus inactivation for drinking water. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Optical and physical properties of samarium doped lithium diborate glasses

    NASA Astrophysics Data System (ADS)

    Hanumantharaju, N.; Sardarpasha, K. R.; Gowda, V. C. Veeranna

    2018-05-01

    Sm3+ doped lithium di-borate glasses with composition 30Li2O-60B2O3-(10-x) PbO, (where 0 < x < 2 mole. %) were prepared by melt quenching method. The addition of modifier oxide to vitreous B2O3 modifies the glass network by converting three coordinated trigonal boron units (BO3) to weaker anionic four coordinated tetrahedral borons (BO4). The decrease in density and increase in molar volume with samarium ion content indicates the openness of the glass structure. The gradual increase in average separation of boron-boron atoms with VmB clearly indicates deterioration of borate glass network, which in turn leads to decrease in the oxygen packing density. The replacements of Sm2O3 for PbO depolymerise the chain structure and that would increase the concentration of non-bridging oxygens. The marginal increase of optical band gap energy after 1.0 mol.% of Sm2O3 is explained by considering the structural modification in lead-borate. The influence of Sm3+ ion on physical and optical properties in lithium-lead-borate glasses is investigated and the results were discussed in view of the structure of borate glass network.

  9. Zirconocene mediated acetylboron chemistry.

    PubMed

    Jian, Zhongbao; Daniliuc, Constantin G; Kehr, Gerald; Erker, Gerhard

    2018-05-31

    The methyl zirconocene complex Cp*2Zr(Me)OMes reacts with H3C-B(C6F5)2 and CO to give the respective acetyl(methyl)borate Zr complex. Cp*2Zr(H)OMes reacts with H3C-B(C6F5)2 and CO to give the respective acetyl(hydrido)borate Zr product, admixed with a minor amount of the formyl(methyl)borate Zr complex isomer. Prolonged exposure to CO under close to ambient conditions results in the uptake of another CO equivalent to yield the corresponding borata-β-lactone zirconocene product.

  10. The effects of borate minerals on the synthesis of nucleic acid bases, amino acids and biogenic carboxylic acids from formamide.

    PubMed

    Saladino, Raffaele; Barontini, Maurizio; Cossetti, Cristina; Di Mauro, Ernesto; Crestini, Claudia

    2011-08-01

    The thermal condensation of formamide in the presence of mineral borates is reported. The products afforded are precursors of nucleic acids, amino acids derivatives and carboxylic acids. The efficiency and the selectivity of the reaction was studied in relation to the elemental composition of the 18 minerals analyzed. The possibility of synthesizing at the same time building blocks of both genetic and metabolic apparatuses, along with the production of amino acids, highlights the interest of the formamide/borate system in prebiotic chemistry.

  11. Copper-induced ammonia N-H functionalization.

    PubMed

    Álvarez, María; Álvarez, Eleuterio; Fructos, Manuel R; Urbano, Juan; Pérez, Pedro J

    2016-10-07

    The activation of ammonia has been achieved with the aid of the Tp(Ms)Cu core (Tp(Ms) = hydrotris(3-mesityl-pyrazolyl)borate). Complexes of the general composition Tp(Ms)Cu(amine) (1-4) including the ammonia adduct Tp(Ms)Cu(NH3) (1) have been synthesized and fully spectroscopical- and structurally characterized. Coordinated ammonia in 1 has been reacted with Ph3CPF6 yielding Tp(Ms)Cu(NH2CPh3) (5) as a result of N-H cleavage and N-C bond formation. In a parallel manner the catalytic functionalization of ammonia with ethyl diazoacetate leading to glycinate derivatives has been developed with Tp(Ms)Cu(THF) as the catalyst, in the first example of this transformation with ammonia and a copper-based system.

  12. Cytoplasmic Acidification and the Benzoate Transcriptome in Bacillus subtilis

    PubMed Central

    Kitko, Ryan D.; Cleeton, Rebecca L.; Armentrout, Erin I.; Lee, Grace E.; Noguchi, Ken; Berkmen, Melanie B.; Jones, Brian D.; Slonczewski, Joan L.

    2009-01-01

    Background Bacillus subtilis encounters a wide range of environmental pH. The bacteria maintain cytoplasmic pH within a narrow range. Response to acid stress is a poorly understood function of external pH and of permeant acids that conduct protons into the cytoplasm. Methods and Principal Findings Cytoplasmic acidification and the benzoate transcriptome were observed in Bacillus subtilis. Cytoplasmic pH was measured with 4-s time resolution using GFPmut3b fluorimetry. Rapid external acidification (pH 7.5 to 6.0) acidified the B. subtilis cytoplasm, followed by partial recovery. Benzoate addition up to 60 mM at external pH 7 depressed cytoplasmic pH but left a transmembrane ΔpH permitting growth; this robust adaptation to benzoate exceeds that seen in E. coli. Cytoplasmic pH was depressed by 0.3 units during growth with 30 mM benzoate. The transcriptome of benzoate-adapted cells was determined by comparing 4,095 gene expression indices following growth at pH 7, +/− 30 mM benzoate. 164 ORFs showed ≥2-fold up-regulation by benzoate (30 mM benzoate/0 mM), and 102 ORFs showed ≥2-fold down-regulation. 42% of benzoate-dependent genes are regulated up or down, respectively, at pH 6 versus pH 7; they are candidates for cytoplasmic pH response. Acid-stress genes up-regulated by benzoate included drug resistance genes (yhbI, yhcA, yuxJ, ywoGH); an oligopeptide transporter (opp); glycine catabolism (gcvPA-PB); acetate degradation (acsA); dehydrogenases (ald, fdhD, serA, yrhEFG, yjgCD); the TCA cycle (citZ, icd, mdh, sucD); and oxidative stress (OYE-family yqjM, ohrB). Base-stress genes down-regulated by benzoate included malate metabolism (maeN), sporulation control (spo0M, spo0E), and the SigW alkali shock regulon. Cytoplasmic pH could mediate alkali-shock induction of SigW. Conclusions B. subtilis maintains partial pH homeostasis during growth, and withstands high concentrations of permeant acid stress, higher than for gram-negative neutralophile E. coli. The benzoate adaptation transcriptome substantially overlaps that of external acid, contributing to a cytoplasmic pH transcriptome. PMID:20011599

  13. Factors affecting calcium oxalate dihydrate fragmented calculi regrowth

    PubMed Central

    Costa-Bauzá, A; Perelló, J; Isern, B; Sanchis, P; Grases, F

    2006-01-01

    Background The use of extracorporeal shock wave lithotripsy (ESWL) to treat calcium oxalate dihydrate (COD) renal calculi gives excellent fragmentation results. However, the retention of post-ESWL fragments within the kidney remains an important health problem. This study examined the effect of various urinary conditions and crystallization inhibitors on the regrowth of spontaneously-passed post-ESWL COD calculi fragments. Methods Post-ESWL COD calculi fragments were incubated in chambers containing synthetic urine varying in pH and calcium concentration: pH = 5.5 normocalciuria (3.75 mM), pH = 5.5 hypercalciuria (6.25 mM), pH = 6.5 normocalciuria (3.75 mM) or pH = 6.5 hypercalciuria (6.25 mM). Fragment growth was evaluated by measuring increases in weight. Fragment growth was standardized by calculating the relative mass increase. Results Calcium oxalate monohydrate (COM) crystals formed on COD renal calculi fragments under all conditions. Under pH = 5.5 normocalciuria conditions, only COM crystals formed (growth rate = 0.22 ± 0.04 μg/mg·h). Under pH = 5.5 hypercalciuria and under pH = 6.5 normocalciuria conditions, COM crystals and a small number of new COD crystals formed (growth rate = 0.32 ± 0.03 μg/mg·h and 0.35 ± 0.05 μg/mg·h, respectively). Under pH = 6.5 hypercalciuria conditions, large amounts of COD, COM, hydroxyapatite and brushite crystals formed (growth rate = 3.87 ± 0. 34 μg/mg·h). A study of three crystallization inhibitors demonstrated that phytate completely inhibited fragment growth (2.27 μM at pH = 5.5 and 4.55 μM at pH = 6.5, both under hypercalciuria conditions), while 69.0 μM pyrophosphate caused an 87% reduction in mass under pH = 6.5 hypercalciuria conditions. In contrast, 5.29 mM citrate did not inhibit fragment mass increase under pH = 6.5 hypercalciuria conditions. Conclusion The growth rate of COD calculi fragments under pH = 6.5 hypercalciuria conditions was approximately ten times that observed under the other three conditions. This observation suggests COD calculi residual fragments in the kidneys together with hypercalciuria and high urinary pH values may be a risk factor for stone growth. The study also showed the effectiveness of specific crystallization inhibitors in slowing calculi fragment growth. PMID:16822299

  14. Chemical composition and mineralogy of borate from Rio Grande deposit, Uyuni (Bolivia) as raw materials for industrial applications

    NASA Astrophysics Data System (ADS)

    Guillen Vargas, Julio; Arancibia, Jony Roger Hans; Alfonso, Pura; Garcia-Valles, Maite; Parcerisa, David; Martinez, Salvador

    2014-05-01

    Bolivia has large tailings as a result of the historic and present-day Sn mining activity developed extensively in that country. Tailings produced in these mining activities have an appropriate composition to reprocess them and make silicate glass and glass-ceramics, obtaining the valorization of wastes and reducing the visual and chemical impact. Reprocessing the wastes to make glass and glass-ceramics prevents the leaching of heavy metals from those wastes because they are retained in the structure of the glass. Furthermore, an option to increase the economic value of these glasses is the introduction of boron and other additives to produce borosilicate glass. In this study a characterization of the Rio Grande borate deposit for its use in the manufacture of borosilicate glass is presented. Mineralogy was determined by X-ray diffraction (XRD), and Fourier transforms infrared spectroscopy (FTIR); textures were observed by scanning electron microscopy (SEM) and chemical composition was determined by inductively coupled plasma mass spectrometry (ICP-MS). The Rio Grande borate deposit is located in an area of about 50 km2 close to the south of the Salar of Uyuni, in the Río Grande de Lípez Delta. Borates occur in the contact between fluvio-deltaic and lacustrine sediments from water raising the surface by capillarity. The borates crop out in an extent area but towards the west they are covered by fluvio-deltaic sediments, which can be up to 2 m thick. These borates occur as lenses 50-100 m in diameter and layers up to 1 m thick. They usually form brittle nodules with a cotton-ball texture. Chemical composition of the Rio Grande borates is CaO, 11.82-13.83 wt%; Na2O, 13.50-19.35 wt%; K2O, 0.05- 1.04 wt%; MgO, 0.42-1.46 wt%; B2O3, 36.21-42.60 wt%; SiO2, up to 0.53 wt% and SO2, up to 0.60 wt%. Trace elements are low: Sr content is between 151-786 ppm, Al 12-676 ppm, Mn between 1-17 ppm, As 2-10 ppm and Fe between 9-376 ppm. The most abundant borate mineral in this deposit is ulexite (NaCaB5.5H20), halite can reach up to 17 wt% and gypsum up to 1.2 wt.%. Calcite occurs in minor contents. Ulexite exhibits a fibrous morphology with fibers oriented parallel each other. Purity of borates from the Rio Grande deposits makes them suitable for the most restrictive applications. Chemistry of these borates is in accordance with the necessary composition for obtaining borosilicate glasses. Acknowledgements: This work was partly financed by the project AECID: A3/042750/11, and the SGR 2009SGR-00444.

  15. Supramolecular assembly of borate with quaternary ammonium: Crystal structure and tunable luminescent properties

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

    Liang, Jie; Wang, Yong-gang; Wang, Ying-xia, E-mail: wangyx@pku.edu.cn

    2013-04-15

    A new borate [C{sub 6}H{sub 16}N][B{sub 5}O{sub 6}(OH){sub 4}] (1) is synthesized hydrothermally by the reaction of isopropyltrimethylammonium hydroxide with boric acid. It crystallizes in the triclinic space group P-1 with the parameters a=9.1578(10) Å, b=9.372(9) Å, c=9.9812(10) Å, α=66.508(2)°, β=74.751(2)°, γ=81.893(2)°. The [B{sub 5}O{sub 6}(OH){sub 4}]{sup −} anions are interlinked via hydrogen bonding forming a 3D supramolecular network containing large cavities, where reside the (CH{sub 3}){sub 3}(i-C{sub 3}H{sub 7}) N{sup +} cations. This borate shows tunable luminescent properties with temperature, heating-treatment, exciting-light, and solvents. The fluorescent intensity of 1 enhances 6-fold with decreasing the temperature from 25 K tomore » 78 K. By treatment under different temperatures, the luminescence of 1 shifted from blue to white and the sample treated at 230 °C emits bright white light to naked eyes. The hybrid borate can disperse in different solvents, and shows a red-shifted and intense emission in polar solvents. - Graphical abstract: The new quaternary ammonium borate [C{sub 6}H{sub 17}N][B{sub 5}O{sub 6}(OH){sub 4}] contains a 3D supramolecular network formed by hydrogen bond linked [B{sub 5}O{sub 6}(OH){sub 4}]{sup −} anions and shows tunable luminescent properties with temperature, excitation light, and solvents. Highlights: ► A novel quaternary ammonium borate was synthesized. ► It possesses a supramolecular network fomed by H-bonded [B{sub 5}O{sub 6}(OH){sub 4}]{sup −} anions. ► This borate shows tunable luminescent properties with temperature, heating treatment, excitation light, and solvents.« less

  16. Comparison of four advanced oxidation processes for the removal of naphthenic acids from model oil sands process water.

    PubMed

    Liang, Xiaoming; Zhu, Xingdong; Butler, Elizabeth C

    2011-06-15

    Four advanced oxidation processes (UV/TiO(2), UV/IO(4)(-), UV/S(2)O(8)(2-), and UV/H(2)O(2)) were tested for their ability to mineralize naphthenic acids to inorganic carbon in a model oil sands process water containing high dissolved and suspended solids at pH values ranging from 8 to 12. A medium pressure mercury (Hg) lamp was used, and a Quartz immersion well surrounded the lamp. The treatment goal of 5mg/L naphthenic acids (3.4 mg/L total organic carbon (TOC)) was achieved under four conditions: UV/S(2)O(8)(2-) (20mM) at pH 8 and 10, and UV/H(2)O(2) (50mM) at pH 8 (all with the Quartz immersion well). Values of electrical energy required to meet the treatment goal were about equal for UV/S(2)O(8)(2-) (20mM) and UV/H(2)O(2) (50mM) at pH 8, but three to four times larger for treatment by UV/S(2)O(8)(2-) (20mM) at pH 10. The treatment goal was also achieved using UV/S(2)O(8)(2-) (20mM) at pH 10 when using a Vycor filter that transmits light primarily in the mid and near UV, suggesting that that treatment of naphthenic acids by UV/S(2)O(8)(2-) using low pressure Hg lamps may be feasible. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Pulmonary Hypertension in Patients With Severe Aortic Stenosis: Prognostic Impact After Transcatheter Aortic Valve Replacement: Pulmonary Hypertension in Patients Undergoing TAVR.

    PubMed

    Alushi, Brunilda; Beckhoff, Frederik; Leistner, David; Franz, Marcus; Reinthaler, Markus; Stähli, Barbara E; Morguet, Andreas; Figulla, Hans R; Doenst, Torsten; Maisano, Francesco; Falk, Volkmar; Landmesser, Ulf; Lauten, Alexander

    2018-04-13

    The authors investigated the development of pulmonary hypertension (PH), predictors of PH regression, and its prognostic impact on short, mid-, and long-term outcomes in patients undergoing transcatheter aortic valve replacement (TAVR) for severe aortic stenosis (AS). PH represents a common finding in patients with AS. Although TAVR is frequently associated with regression of PH, the predictors of reversible PH and its prognostic significance remain uncertain. In this study, 617 consecutive patients undergoing TAVR between 2009 and 2015 were stratified per baseline tertiles of pulmonary artery systolic pressure (PASP) as follows: normal (PASP <34 mm Hg), mild-to-moderate (34 mm Hg ≤ PASP <46 mm Hg), and severe PASP elevation (PASP ≥46 mm Hg). After TAVR, 520 patients with PH at discharge were stratified according to the presence or absence of PASP reduction. Primary outcome was all-cause mortality at 30 days, 1 year, and long-term follow-up at a maximum of 5.9 years. In patients with both mild-to-moderate and severe PH at baseline, PASP decreased significantly at discharge (ΔPASP 3.0 ± 9.3 mm Hg and 12.0 ± 10.0 mm Hg, respectively) and 1 year (ΔPASP 5.0 ± 9.7 mm Hg and 18.0 ± 14.0 mm Hg, respectively). At a median follow-up of 370 days (interquartile range [IQR]: 84 to 500 days), the risk of all-cause mortality was similar among baseline PASP groups at all time intervals evaluated. After TAVR, a significant regression of PH was observed in 46% of patients. Contrarily, patients with residual PH had a higher risk of all-cause mortality at 30 days (hazard ratio [HR]: 3.49, 95% confidence interval [CI]: 1.74 to 6.99; p < 0.001), 1 year (HR: 3.12, 95% CI: 2.06 to 4.72; p < 0.001), and long-term (HR: 2.47, 95% CI: 1.74 to 3.49; p < 0.001). Left ventricular ejection fraction (LVEF) >40% (odds ratio [OR]: 3.56, 95% CI: 2.24 to 5.65; p < 0.001), baseline PASP ≥46 mm Hg (OR: 3.26, 95% CI: 2.07 to 5.12; p < 0.001), absence of concomitant tricuspid regurgitation (TR) ≥ moderate (OR: 0.53, 95% CI: 0.34 to 0.84; p < 0.001), and logistic EuroSCORE <25% (OR: 1.59, 95% CI: 1.04 to 2.45; p = 0.03) were independent predictors of PASP reduction. In most patients with PH and AS, TAVR is associated with a significant early and late reduction of PASP. Patients with reversible PH after TAVR are at lower risk of all-cause mortality at early, mid-, and long-term follow-up. Therefore, the presence of PH should not preclude treatment with TAVR. Copyright © 2018 American College of Cardiology Foundation. Published by Elsevier Inc. All rights reserved.

  18. The Antemortem Detection and Conformational Switches of Prion Proteins

    DTIC Science & Technology

    2006-07-01

    distribution of di-, mono-, and unglycosylated PrPC molecules (Fig. 7B, lane 2). Subsequent elution of the column with N-acetyl glucosamine yielded...pellet was washed in 50 mM Tris, pH 8.0, 150 mM NaCl, and then solubilized in 6 M guanidinium hydrochloride , 50 mM Tris pH 8.0, 150 mM NaCl. The...and 150mM sodium chloride (TCl) containing 6M guanidinium hydrochloride . The supernatant was centrifuged for 30min at 18,000g. The protein was

  19. Impact of vanadium ions in barium borate glass

    NASA Astrophysics Data System (ADS)

    Abdelghany, A. M.; Hammad, Ahmed H.

    2015-02-01

    Combined optical and infrared spectral measurements of prepared barium borate glasses containing different concentrations of V2O5 were carried out. Vanadium containing glasses exhibit extended UV-visible (UV/Vis.) bands when compared with base binary borate glass. UV/Vis. spectrum shows the presence of an unsymmetrical strong UV broad band centered at 214 nm attributed to the presence of unavoidable trace iron impurities within the raw materials used for the preparation of such glass. The calculated direct and indirect optical band gaps are found to decrease with increasing the vanadium content (2.9:137 for indirect and 3.99:2.01 for direct transition). This change was discussed in terms of structural changes in the glass network. Infrared absorption spectra of the glasses reveal the appearance of both triangular and tetrahedral borate units. Electron spin resonance analyses indicate the presence of unpaired species in sufficient quantity to be identified and to confirm the spectral data.

  20. Tetraarylborate polymer networks as single-ion conducting solid electrolytes

    DOE PAGES

    Van Humbeck, Jeffrey F.; Aubrey, Michael L.; Alsbaiee, Alaaeddin; ...

    2015-06-23

    A new family of solid polymer electrolytes based upon anionic tetrakis(phenyl)borate tetrahedral nodes and linear bis-alkyne linkers is reported. Sonogashira polymerizations using tetrakis(4-iodophenyl)borate, tetrakis(4-iodo-2,3,5,6-tetrafluorophenyl)borate and tetrakis(4-bromo-2,3,5,6-tetrafluorophenyl)borate delivered highly cross-linked polymer networks with both 1,4-diethynylbeznene and a tri(ethylene glycol) substituted derivative. Promising initial conductivity metrics have been observed, including high room temperature conductivities (up to 2.7 × 10 -4 S cm -1), moderate activation energies (0.25–0.28 eV), and high lithium ion transport numbers (up to t Li+ = 0.93). Initial investigations into the effects of important materials parameters such as bulk morphology, porosity, fluorination, and other chemical modification, provide starting designmore » parameters for further development of this new class of solid electrolytes.« less

  1. Effect of Borates and Silicates on Wearing Properties of Mao Coatings

    NASA Astrophysics Data System (ADS)

    Zhang, Yu; Zhao, Yan-Wei; Xiang, Nan; Song, Ren-Guo

    In the present study, microarc oxidation (MAO) coatings were formed on ZL101A aluminum alloy in an electrolytic bath containing 3g/L KOH + 2g/L Na2WO4+ 4g/L KF. The morphology and wearing behavior were investigated. In both electrolytes, the additives were borates (Na2B4O718g/L) and silicates (Na2SiO3 18g/L), respectively. It was found that the coating formed in borates-containing electrolyte was of compact and smooth structure than that of the one formed in silicates-containing electrolyte at the optimum treatment time. It was found that all the coatings were composed of á-Al2O3 and ã-Al2O3. The microhardness and wear tests proved that the coating formed in borates-containing electrolyte was having better mechanical properties than those of the coating formed in silicates-containing electrolyte.

  2. Effect of glycine on pH changes and protein stability during freeze-thawing in phosphate buffer systems.

    PubMed

    Pikal-Cleland, Katherine A; Cleland, Jeffrey L; Anchordoquy, Thomas J; Carpenter, John F

    2002-09-01

    Previous studies have established that the selective precipitation of a less soluble buffer component during freezing can induce a significant pH shift in the freeze concentrate. During freezing of sodium phosphate solutions, crystallization of the disodium salt can produce a pH decrease as great as 3 pH units which can dramatically affect protein stability. The objective of our study was to determine how the presence of glycine (0-500 mM), a commonly used bulking agent in pharmaceutical protein formulations, affects the pH changes normally observed during freezing in sodium phosphate buffer solutions and to determine whether these pH changes contribute to instability of model proteins in glycine/phosphate formulations. During freezing in sodium phosphate buffers, the presence of glycine significantly influenced the pH. Glycine at the lower concentrations (< or = 50 mM) suppressed the pH decrease normally observed during freezing in 10 and 100 mM sodium phosphate buffer, possibly by reducing the nucleation rate of salt and thereby decreasing the extent of buffer salt crystallization. The presence of glycine at higher concentration (> 100 mM) in the sodium phosphate buffer resulted in a more complete crystallization of the disodium salt as indicated by the frozen pH values closer to the equilibrium value (pH 3.6). Although high concentrations of glycine can facilitate more buffer salt crystallization and these pH shifts may prove to be potentially damaging to the protein, glycine, in its amorphous state, can also act to stabilize a protein via the preferential exclusion mechanism. Copyright 2002 Wiley-Liss Inc.

  3. Structural, Spectroscopic, and Electrochemical Properties of Nonheme Fe(II)-Hydroquinonate Complexes: Synthetic Models of Hydroquinone Dioxygenases

    PubMed Central

    Baum, Amanda E.; Park, Heaweon; Wang, Denan; Lindeman, Sergey V.; Fiedler, Adam T.

    2012-01-01

    Using the tris(3,5-diphenylpyrazol-1-yl)borate (Ph2Tp) supporting ligand, a series of mono- and dinuclear ferrous complexes containing hydroquinonate (HQate) ligands have been prepared and structurally characterized with X-ray crystallography. The monoiron(II) complexes serve as faithful mimics of the substrate-bound form of hydroquinone dioxygenases (HQDOs) – a family of nonheme Fe enzymes that catalyze the oxidative cleavage of 1,4-dihydroxybenzene units. Reflecting the variety of HQDO substrates, the synthetic complexes feature both mono- and bidentate HQate ligands. The bidentate HQates cleanly provide five-coordinate, high-spin Fe(II) complexes with the general formula [Fe(Ph2Tp)(HLX)] (1X), where HLX is a HQate(1-) ligand substituted at the 2-position with a benzimidazolyl (1A), acetyl (1B and 1C), or methoxy (1D) group. In contrast, the monodentate ligand 2,6-dimethylhydroquinone (H2LF) exhibited a greater tendency to bridge between two Fe(II) centers, resulting in formation of [Fe2(Ph2Tp)2(μ-LF)(MeCN)] [2F(MeCN)]. However, addition of one equivalent of “free” pyrazole (Ph2pz) ligand provided the mononuclear complex, [Fe(Ph2Tp)(HLF)(Ph2pz)] [1F(Ph2pz)], which is stabilized by an intramolecular hydrogen bond between the HLF and Ph2pz donors. Complex 1F(Ph2pz) represents the first crystallographically-characterized example of a monoiron complex bound to an untethered HQate ligand. The geometric and electronic structures of the Fe/HQate complexes were further probed with spectroscopic (UV-vis absorption, 1H NMR) and electrochemical methods. Cyclic voltammograms of complexes in the 1X series revealed an Fe-based oxidation between 0 and −300 mV (vs. Fc+/0), in addition to irreversible oxidation(s) of the HQate ligand at higher potentials. The one-electron oxidized species (1Xox) were examined with UV-vis absorption and electron paramagnetic resonance (EPR) spectroscopies. PMID:22930005

  4. Magnesium and zinc borate enhance osteoblastic differentiation of stem cells from human exfoliated deciduous teeth in vitro.

    PubMed

    Liu, Yao-Jen; Su, Wen-Ta; Chen, Po-Hung

    2018-01-01

    Various biocompatible and biodegradable scaffolds blended with biochemical signal molecules with adequate osteoinductive and osteoconductive properties have attracted significant interest in hard tissue engineering regeneration. We evaluated the distinct effects of magnesium borate, zinc borate, and boric acid blended into chitosan scaffold for osteogenic differentiation of stem cells from exfoliated deciduous teeth. Stem cells from exfoliated deciduous teeth cells are a potential source of functional osteoblasts for applications in bone tissue engineering, but the efficiency of osteoblastic differentiation is low, thereby significantly limiting their clinical applications. Divalent metal borates have potential function in bone remodeling because they can simulate bone formation and decrease bone resorption. These magnesium, zinc, and B ions can gradually be released into the culture medium from the scaffold and induce advanced osteoblastic differentiation from stem cells from exfoliated deciduous teeth. Stem cells from exfoliated deciduous teeth with magnesium borate or zinc borate as inducer demonstrated more osteoblastic differentiation after 21 days of culture. Differentiated cells exhibited activity of alkaline phosphatase, bone-related gene expression of collagen type I, runt-related transcription factor 2, osteopontin, osteocalcin, vascular endothelial growth factor, and angiopoietin-1, as noted via real-time polymerase chain reaction analysis, as well as significant deposits of calcium minerals. Divalent mental magnesium and zinc and nonmetal boron can be an effective inducer of osteogenesis for stem cells from exfoliated deciduous teeth. This experiment might provide useful inducers for osteoblastic differentiation of stem cells from exfoliated deciduous teeth for tissue engineering and bone repair.

  5. Effect of zinc-borate glass addition on the thermal properties of the cordierite/Al2O3 composites containing nano-sized spinel crystal.

    PubMed

    Jo, Sinae; Kang, Seunggu

    2013-11-01

    Low-melting zinc-borate glass was added to the cordierite/Al2O3 composite in order to improve the sintering facility of Al2O3 and formation of nano-sized spinel crystal of high thermal conductivity. Increasing the ZnO/B2O3 ratio in the zinc-borate glass increased the ZnAl2O4 spinel and decreased the Al4B2O9 crystal peak intensities in X-ray diffraction pattern. The XRD peak intensities of the ZnAl2O4 spinel and Al4B2O9 crystals in the specimen containing 10 wt% zinc-borate glass (10G series) are higher than that of the specimen containing 5 wt% zinc-borate glass (5G series). The microstructures of most 10G series specimens had the flower-shaped crystal which was composed of 50 nm wide and 250 nm long needle-like crystals and identified as ZnAl2O4 spinel phase. The thermal conductivity of the 10G series specimen was higher than that of the 5G series in any ZnO/B2O3 ratio due to the formation of plenty of nano-sized ZnAl2O4 spinel of high thermal conductivity. Particularly, the thermal conductivity of the cordierite/Al2O3 composite containing 10 wt% zinc-borate glass of ZnO/B2O3 weight ratio = 1.5 was 3.8 W/Km which is much higher than that of the published value (3.0 W/Km).

  6. Comparison of intracanal EndoSequence Root Repair Material and ProRoot MTA to induce pH changes in simulated root resorption defects over 4 weeks in matched pairs of human teeth.

    PubMed

    Hansen, Stephen W; Marshall, J Gordon; Sedgley, Christine M

    2011-04-01

    Intracanal mineral trioxide aggregate (MTA) may provide an alternative to calcium hydroxide in the treatment of external inflammatory root resorption. This in vitro study using human matched pairs of teeth compared white ProRoot MTA (WMTA; (Dentsply Tulsa Dental Specialties, Tulsa, OK) and an alternative material with purportedly improved handling properties, EndoSequence Root Repair Material (ES; Brasseler USA, Savannah, GA), by measuring pH in simulated root surface resorptive defects after intracanal placement. The null hypothesis tested was that there is no difference between WMTA and ES. Bilaterally matched pairs (n = 24) of extracted, human, single-rooted teeth were instrumented to apical size 50/.06, and root surface cavities were prepared at 5 mm and 2 mm from the apex. Root canals of experimental matched pairs (n = 20) were filled with WMTA or ES; control pairs (n = 4) were filled with calcium hydroxide (positive control [POS]) or saline (negative control [NEG]). Teeth were sealed coronally and apically and immersed in saline. The pH in root surface cavities was measured at 20 minutes, 3 hours, 24 hours, 1 week, 2 weeks, 3 weeks, and 4 weeks. The pH at 5 mm when compared with the 2-mm level was significantly higher for the WMTA, ES, and POS groups (P < .05, paired t tests); therefore, each level was analyzed separately. At both the 2-mm and 5-mm levels, significant pH changes occurred over time in the WMTA, ES (both P < .0001, repeated-measures analysis of variance), and POS (P < .0001, Friedman test) groups and not in the NEG group (mean pH = 7.32 ± 0.04, P > .05). There were no differences between WMTA and ES at 20 minutes and 3 hours at both levels or at 24 hours at 5mm. The pH of WMTA was higher than ES by 24 hours at the 2-mm level (8.79 vs 8.56, P < .05, paired t test) and after 1 week at the 5-mm level (8.91 vs 8.05, P < .0001) and was thereafter always significantly higher in WMTA compared with ES (P < .0001). The null hypothesis was rejected. In matched pairs of teeth, intracanal placement of WMTA compared with ES resulted in a higher pH in simulated root resorption defects that was time and root level dependent. Copyright © 2011 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

  7. Hydrothermal synthesis and structural analysis of new mixed oxyanion borates: Ba{sub 11}B{sub 26}O{sub 44}(PO{sub 4}){sub 2}(OH){sub 6}, Li{sub 9}BaB{sub 15}O{sub 27}(CO{sub 3}) and Ba{sub 3}Si{sub 2}B{sub 6}O{sub 16}

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

    Heyward, Carla, E-mail: cheywar@clemson.edu; McMillen, Colin D., E-mail: cmcmill@clemson.edu; Kolis, Joseph, E-mail: kjoseph@clemson.edu

    2013-07-15

    Several new borate compounds, Ba{sub 11}B{sub 26}O{sub 44}(PO{sub 4}){sub 2}(OH){sub 6} (1), Li{sub 9}BaB{sub 15}O{sub 27}(CO{sub 3}) (2), and Ba{sub 3}Si{sub 2}B{sub 6}O{sub 16} (3) were synthesized containing other hetero-oxyanion building blocks in addition to the borate frameworks. They were all prepared under hydrothermal conditions and characterized by single crystal and powder X-ray diffraction, and IR spectroscopy. Crystal data: For 1; space group P2{sub 1}/c, a=6.8909 (14) Å, b=13.629 (3) Å, c=25.851 (5) Å, β=90.04 (3)°; For 2; space group P-31c, a=8.8599 (13) Å, c=15.148 (3) Å; For 3; space group P-1, a=5.0414 (10) Å, b=7.5602 (15) Å, c=8.5374 (17)more » Å, α=77.15 (3)°, β=77.84 (3)°, γ=87.41 (3)° for 3. Compounds 1 and 2 contain isolated oxyanions [PO{sub 4}]{sup 3−} and [CO{sub 3}]{sup 2−} respectively, sitting in channels created by the borate framework, while structure 3 has the [SiO{sub 4}]{sup 4−} groups directly bonded to the borate groups creating a B–O–Si framework. - Highlights: • Hydrothermal syntheses of three new mixed oxyanion borates are presented. • Ba{sub 11}B{sub 26}O{sub 44}(PO{sub 4}){sub 2}(OH){sub 6} contains isolated [PO{sub 4}]{sup 3−} in voids of the borate framework. • Li{sub 9}BaB{sub 15}O{sub 27}(CO{sub 3}) contains isolated [CO{sub 3}]{sup 2−} in channels created by the framework. • Ba{sub 3}Si{sub 2}B{sub 6}O{sub 16} has direct bonding of [SiO{sub 4}]{sup 4−} and borates creating a B–O–Si framework.« less

  8. Corneal epithelial cell biocompatibility to silicone hydrogel and conventional hydrogel contact lens packaging solutions

    PubMed Central

    Tanti, N.C.; Jones, L.; Sheardown, H.

    2010-01-01

    Purpose Although all contact lenses (CLs) are applied initially to the eye directly from a packaging solution, little is known about the effects of these solutions on human corneal epithelial cells (HCECs). Due to the porous nature of CL materials, they have the potential to sorb components of the packaging solution during storage, which could then be subsequently released upon insertion of the CL on the eye. The purpose of this study was to investigate the effect of various packaging solutions on HCECs, using an in vitro model. Methods An in vitro assay was developed whereby various silicone hydrogels and conventional, poly-2-hydroxyethylmethacrylate  (polyHEMA)-based lens materials were removed directly from their packaging and then incubated for up to 24 h with HCECs. The effect of the retained and released packaging solution components on HCECs was assessed by measuring cell viability, adhesion phenotype, and apoptosis. Results Incubation of HCECs with CLs stored in borate-buffered packaging solutions resulted in a significant reduction in cell viability. Adherent cells incubated with these CLs also exhibited reduced levels of β1 and α3 integrin. Soaking borate-buffered packaged CLs in PBS before cell incubation resolved viability and integrin expression in all cases, with the exception of galyfilcon A and balafilcon A, from which a 20% reduction in cell viability was still observed. In comparison, CLs stored in phosphate-buffered packaging solutions had cellular viability and expression of integrins similar to control cells (cells incubated in the absence of a lens). When incubated with cells at a 10% concentration in serum-free medium, borate-buffered packaging solutions and borate-containing saline (Unisol 4) significantly reduced cell viability and integrin expression. Neither caspase activation nor annexin V binding was observed on cells following exposure to borate buffer solution. However, a significant decrease in reactive oxygen species was observed at 24 h. These latter results suggest that in vitro exposure to low concentration of borate/boric acid results in cell dysfunction, leading to necrosis rather than apoptosis. Conclusions Borate-buffered packaging solutions were shown to adversely affect the viability and integrin expression of HCECs in vitro. When used in ophthalmic packaging solutions, the antimicrobial properties of borate buffer may be outweighed by its relatively cytotoxic effects on cells. PMID:20169012

  9. Corneal epithelial cell biocompatibility to silicone hydrogel and conventional hydrogel contact lens packaging solutions.

    PubMed

    Gorbet, M B; Tanti, N C; Jones, L; Sheardown, H

    2010-02-19

    Although all contact lenses (CLs) are applied initially to the eye directly from a packaging solution, little is known about the effects of these solutions on human corneal epithelial cells (HCECs). Due to the porous nature of CL materials, they have the potential to sorb components of the packaging solution during storage, which could then be subsequently released upon insertion of the CL on the eye. The purpose of this study was to investigate the effect of various packaging solutions on HCECs, using an in vitro model. An in vitro assay was developed whereby various silicone hydrogels and conventional, poly-2-hydroxyethylmethacrylate (polyHEMA)-based lens materials were removed directly from their packaging and then incubated for up to 24 h with HCECs. The effect of the retained and released packaging solution components on HCECs was assessed by measuring cell viability, adhesion phenotype, and apoptosis. Incubation of HCECs with CLs stored in borate-buffered packaging solutions resulted in a significant reduction in cell viability. Adherent cells incubated with these CLs also exhibited reduced levels of beta(1) and alpha(3) integrin. Soaking borate-buffered packaged CLs in PBS before cell incubation resolved viability and integrin expression in all cases, with the exception of galyfilcon A and balafilcon A, from which a 20% reduction in cell viability was still observed. In comparison, CLs stored in phosphate-buffered packaging solutions had cellular viability and expression of integrins similar to control cells (cells incubated in the absence of a lens). When incubated with cells at a 10% concentration in serum-free medium, borate-buffered packaging solutions and borate-containing saline (Unisol 4) significantly reduced cell viability and integrin expression. Neither caspase activation nor annexin V binding was observed on cells following exposure to borate buffer solution. However, a significant decrease in reactive oxygen species was observed at 24 h. These latter results suggest that in vitro exposure to low concentration of borate/boric acid results in cell dysfunction, leading to necrosis rather than apoptosis. Borate-buffered packaging solutions were shown to adversely affect the viability and integrin expression of HCECs in vitro. When used in ophthalmic packaging solutions, the antimicrobial properties of borate buffer may be outweighed by its relatively cytotoxic effects on cells.

  10. A Non-Invasive Assessment of Cardiopulmonary Hemodynamics with MRI in Pulmonary Hypertension

    PubMed Central

    Bane, Octavia; Shah, Sanjiv J.; Cuttica, Michael J.; Collins, Jeremy D.; Selvaraj, Senthil; Chatterjee, Neil R.; Guetter, Christoph; Carr, James C.; Carroll, Timothy J.

    2015-01-01

    Purpose We propose a method for non-invasive quantification of hemodynamic changes in the pulmonary arteries resulting from pulmonary hypertension (PH). Methods Using a two-element windkessel model, and input parameters derived from standard MRI evaluation of flow, cardiac function and valvular motion, we derive: pulmonary artery compliance (C), mean pulmonary artery pressure (mPAP), pulmonary vascular resistance (PVR), pulmonary capillary wedge pressure (PCWP), time-averaged intra-pulmonary pressure waveforms and pulmonary artery pressures (systolic (sPAP) and diastolic (dPAP)). MRI results were compared directly to reference standard values from right heart catheterization (RHC) obtained in a series of patients with suspected pulmonary hypertension (PH). Results In 7 patients with suspected PH undergoing RHC, MRI and echocardiography, there was no statistically significant difference (p<0.05) between parameters measured by MRI and RHC. Using standard clinical cutoffs to define PH (mPAP ≥ 25 mmHg), MRI was able to correctly identify all patients as having pulmonary hypertension, and to correctly distinguish between pulmonary arterial (mPAP≥ 25 mmHg, PCWP<15 mmHg) and venous hypertension (mPAP ≥ 25 mmHg, PCWP ≥ 15 mmHg) in 5 of 7 cases. Conclusions We have developed a mathematical model capable of quantifying physiological parameters that reflect the severity of PH. PMID:26283577

  11. Passive safety injection system using borated water

    DOEpatents

    Conway, Lawrence E.; Schulz, Terry L.

    1993-01-01

    A passive safety injection system relies on differences in water density to induce natural circulatory flow patterns which help maintain prescribed concentrations of boric acid in borated water, and prevents boron from accumulating in the reactor vessel and possibly preventing heat transfer.

  12. Treatment of cells with alkaline borate buffer extends the capability of interphase FISH mapping.

    PubMed

    Yokota, H; van den Engh, G; Mostert, M; Trask, B J

    1995-01-20

    Interphase fluorescence in situ hybridization (FISH) has been shown to be a means to map DNA sequences relative to each other in the 100 kb to 1-2 Mb genomic-separation range. At distances below 0.1 Mb, probe sites are infrequently resolved in interphase chromatin. In the 0.1- to 1-Mb range, interphase chromatin can be modeled as a freely flexible chain. The mean square interphase distance between two probes is proportional to the genomic separation between the probes on the linear DNA molecule. Above 1-2 Mb, the relationship between interphase distance and genomic separation changes abruptly and appears to level off. We have used alkaline-borate treatment to expand the capability of interphase FISH mapping. We show here that alkaline-borate treatment increases nuclear diameter, the interphase distance between probes on homologous chromosomes, and the distance between probes on the same chromosome. We also show that the mean square distance between hybridization sites in borate-treated nuclei is proportional to genomic separation up to 4 Mb. Thus, alkaline-borate treatment enhances the capability of interphase FISH mapping by increasing the absolute distance between probes and extending the range of the simple relationship between interphase distance and genomic separation.

  13. Treatment of cells with alkaline borate buffer extends the capability of interphase FISH mapping

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

    Yokota, H.; Van Den Engh, G.; Mostert, M.

    1995-01-20

    Interphase fluorescence in situ hybridization (FISH) has been shown to be a means to map DNA sequences relative to each other in the 100 kb to 1-2 Mb genomic-separation range. At distances below 0.1 Mb, probe sites are infrequently resolved in interphase chromatin. In the 0.1- to 1-Mb range, interphase chromatin can be modeled as a freely flexible chain. The mean square interphase distance between two probes is proportional to the genomic separation between the probes on the linear DNA molecule. Above 1-2 Mb, the relationship between interphase distance and genomic separation changes abruptly and appears to level off. Wemore » have used alkaline-borate treatment to expand the capability of interphase FISH mapping. We show here that alkaline-borate treatment increases nuclear diameter, the interphase distance between probes on homologous chromosomes, and the distance between probes on the same chromosome. We also show that the mean square distance between hybridization sites in borate-treated nuclei is proportional to genomic separation up to 4 Mb. Thus, alkaline-borate treatment enhances the capability of interphase FISH mapping by increasing the absolute distance between probes and extending the range of the simple relationship between interphase distance and genomic separation. 31 refs., 5 figs.« less

  14. A novel injectable borate bioactive glass cement for local delivery of vancomycin to cure osteomyelitis and regenerate bone.

    PubMed

    Cui, Xu; Zhao, Cunju; Gu, Yifei; Li, Le; Wang, Hui; Huang, Wenhai; Zhou, Nai; Wang, Deping; Zhu, Yi; Xu, Jun; Luo, Shihua; Zhang, Changqing; Rahaman, Mohamed N

    2014-03-01

    Osteomyelitis (bone infection) is often difficult to cure. The commonly-used treatment of surgical debridement to remove the infected bone combined with prolonged systemic and local antibiotic treatment has limitations. In the present study, an injectable borate bioactive glass cement was developed as a carrier for the antibiotic vancomycin, characterized in vitro, and evaluated for its capacity to cure osteomyelitis in a rabbit tibial model. The cement (initial setting time = 5.8 ± 0.6 min; compressive strength = 25.6 ± 0.3 MPa) released vancomycin over ~25 days in phosphate-buffered saline, during which time the borate glass converted to hydroxyapatite (HA). When implanted in rabbit tibial defects infected with methicillin-resistant Staphylococcus aureus (MRSA)-induced osteomyelitis, the vancomycin-loaded cement converted to HA and supported new bone formation in the defects within 8 weeks. Osteomyelitis was cured in 87 % of the defects implanted with the vancomycin-loaded borate glass cement, compared to 71 % for the defects implanted with vancomycin-loaded calcium sulfate cement. The injectable borate bioactive glass cement developed in this study is a promising treatment for curing osteomyelitis and for regenerating bone in the defects following cure of the infection.

  15. In vitro bioactivity, cytocompatibility, and antibiotic release profile of gentamicin sulfate-loaded borate bioactive glass/chitosan composites.

    PubMed

    Cui, Xu; Gu, Yifei; Li, Le; Wang, Hui; Xie, Zhongping; Luo, Shihua; Zhou, Nai; Huang, Wenhai; Rahaman, Mohamed N

    2013-10-01

    Borate bioactive glass-based composites have been attracting interest recently as an osteoconductive carrier material for local antibiotic delivery. In the present study, composites composed of borate bioactive glass particles bonded with a chitosan matrix were prepared and evaluated in vitro as a carrier for gentamicin sulfate. The bioactivity, degradation, drug release profile, and compressive strength of the composite carrier system were studied as a function of immersion time in phosphate-buffered saline at 37 °C. The cytocompatibility of the gentamicin sulfate-loaded composite carrier was evaluated using assays of cell proliferation and alkaline phosphatase activity of osteogenic MC3T3-E1 cells. Sustained release of gentamicin sulfate occurred over ~28 days in PBS, while the bioactive glass converted continuously to hydroxyapatite. The compressive strength of the composite loaded with gentamicin sulfate decreased from the as-fabricated value of 24 ± 3 MPa to ~8 MPa after immersion for 14 days in PBS. Extracts of the soluble ionic products of the borate glass/chitosan composites enhanced the proliferation and alkaline phosphatase activity of MC3T3-E1 cells. These results indicate that the gentamicin sulfate-loaded composite composed of chitosan-bonded borate bioactive glass particles could be useful clinically as an osteoconductive carrier material for treating bone infection.

  16. Synthesis and study on the luminescence properties of cadmium borate phosphors

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

    Annalakshmi, O.; Jose, M.T., E-mail: mtjosein@yahoo.co.in; Venkatraman, B.

    2014-02-01

    Highlights: • Cadmium borate synthesized by solid state sintering technique. • Neutron sensitivity of the material ten times that of TLD-600. • Gamma sensitivity is found to be twice that of TLD-100. • Gamma response is linear from 0.1 to 10{sup 3} mGy. - Abstract: Cadmium borate compound prepared through wet chemical reaction from the starting chemicals followed by high temperature solid state synthesis below the melting point to get the final TL phosphor powder. Phase purity and bond details of cadmium borate crystals are characterized using X-ray diffraction technique and infrared spectroscopy. Feasibility of these materials for radiation dosimetrymore » applications was studied after gamma and neutron irradiation. Gamma irradiation of undoped phosphors show a single peak around 185 °C whereas doping with gadolinium and silver, new more intense peak observed at 290 °C. Irradiation to thermal neutrons revealed single peak around 170 °C for all the phosphors. TL emission spectra and photoluminescence (PL) studies were also carried out on the phosphors. These borate materials are found to be highly sensitive to neutrons and hence can be used for neutron detection. Neutron sensitivity of the material is about ten times that of TLD-600.« less

  17. Basolateral membrane Na/base cotransport is dependent on CO2/HCO3 in the proximal convoluted tubule

    PubMed Central

    1987-01-01

    The mechanism of basolateral membrane base transport was examined in the in vitro microperfused rabbit proximal convoluted tubule (PCT) in the absence and presence of ambient CO2/HCO3- by means of the microfluorometric measurement of cell pH. The buffer capacity of the cells measured using rapid NH3 washout was 42.8 +/- 5.6 mmol.liter-1.pH unit-1 in the absence and 84.6 +/- 7.3 mmol.liter-1.pH unit-1 in the presence of CO2/HCO3-. In the presence of CO2/HCO3-, lowering peritubular pH from 7.4 to 6.8 acidified the cell by 0.30 pH units and lowering peritubular Na from 147 to 0 mM acidified the cell by 0.25 pH units. Both effects were inhibited by peritubular 4-acetamido-4'- isothiocyanostilbene-2,2'-disulfonate (SITS). In the absence of exogenous CO2/HCO3-, lowering peritubular pH from 7.4 to 6.8 acidified the cell by 0.25 pH units and lowering peritubular Na from 147 to 0 mM decreased cell pH by 0.20 pH units. Lowering bath pH from 7.4 to 6.8 induced a proton flux of 643 +/- 51 pmol.mm-1.min-1 in the presence of exogenous CO2/HCO3- and 223 +/- 27 pmol.mm-1.min-1 in its absence. Lowering bath Na from 147 to 0 mM induced proton fluxes of 596 +/- 77 pmol.mm-1.min-1 in its absence. The cell acidification induced by lowering bath pH or bath Na in the absence of CO2/HCO3- was inhibited by peritubular SITS or by acetazolamide, whereas peritubular amiloride had no effect. In the absence of exogenous CO2/HCO3-, cyanide blocked the cell acidification induced by bath Na removal, but was without effect in the presence of exogenous CO2/HCO3-. We reached the following conclusions. (a) The basolateral Na/base n greater than 1 cotransporter in the rabbit PCT has an absolute requirement for CO2/HCO3-. (b) In spite of this CO2 dependence, in the absence of exogenous CO2/HCO3-, metabolically produced CO2/HCO3- is sufficient to keep the transporter running at 30% of its control rate in the presence of ambient CO2/HCO3- . (c) There is no apparent amiloride-sensitive Na/H antiporter on the basolateral membrane of the rabbit PCT. PMID:2831294

  18. Intra-shell boron isotope ratios in the symbiont-bearing benthic foraminiferan Amphistegina lobifera: Implications for δ 11B vital effects and paleo-pH reconstructions

    NASA Astrophysics Data System (ADS)

    Rollion-Bard, C.; Erez, J.

    2010-03-01

    The boron isotope composition of marine carbonates is considered to be a seawater pH proxy. Nevertheless, the use of δ 11B has some limitations such as the knowledge of the fractionation factor ( α4-3) between boric acid and the borate ion and the amplitude of "vital effects" on this proxy that are not well constrained. Using secondary ion mass spectrometry (SIMS) we have examined the internal variability of the boron isotope ratio in the shallow water, symbionts bearing foraminiferan Amphistegina lobifera. Specimens were cultured at constant temperature (24 ± 0.1 °C) in seawater with pH ranging between 7.90 and 8.45. Intra-shell boron isotopes showed large variability with an upper limit value of ≈30‰. Our results suggest that the fractionation factor α4-3 of 0.97352 ( Klochko et al., 2006) is in better agreement with our experiments and with direct pH measurements in seawater vacuoles associated with the biomineralization process in these foraminifera. Despite the large variability of the skeletal pH values in each cultured specimen, it is possible to link the lowest calculated pH values to the experimental culture pH values while the upper pH limit is slightly below 9. This variability can be interpreted as follows: foraminifera variably increase the pH at the biomineralization site to about 9. This increase above ambient seawater pH leads to a range in δ 11B (Δ 11B) for each seawater pH. This Δ 11B is linearly correlated with the culture seawater pH with a slope of -13.1 per pH unit, and is independent of the fractionation factor α4-3, or the δ 11B sw through time. It may also be independent of the p KB (the dissociation constant of boric acid) value. Therefore, Δ 11B in foraminifera can potentially reconstruct paleo-pH of seawater.

  19. Spectral-luminescent and laser properties of the (Y1-x,Ybx)2O3-Al2O3-B2O3 glasses

    NASA Astrophysics Data System (ADS)

    Malashkevich, G. E.; Kouhar, V. V.; Pestryakov, E. V.; Sigaev, V. N.; Golubev, N. V.; Ziyatdinova, M. Z.; Sukhodola, A. A.

    2018-02-01

    Yttrium-alumina-borate glasses activated by the Yb3+ ions with compositions close to the huntite-like (Y1-xLnx)Al3(BO3)4 crystals have been synthesized by conventional melt-quenching technique in a platinum crucible, and their spectral-luminescent and laser properties have been investigated. It is established that this activator forms in the given glass one type of optical centers having the radiation decay time of 870 ± 40 μs. The limiting quantum yield of its luminescence in the case of complete dehydration of the glass will amount to ≈94%. The main laser parameters have been calculated and the nonlinearity of the refractive index and the threshold of laser-induced destruction of the glass surface have been determined. The lasing has been obtained on the glass plate of 2.1 mm thickness with a threshold of ≈60 W/mm2 estimated by specific absorbed power.

  20. Global patterns of changes in underwater sound transmission caused by ocean acidification

    NASA Astrophysics Data System (ADS)

    Ilyina, T.; Zeebe, R. E.; Brewer, P. G.

    2009-04-01

    Oceanic uptake of man-made CO2 leads to a decrease in the ocean pH and carbonate saturation state. This processes, known as ocean acidification is expected to have adverse effects on a variety of marine organisms. A surprising consequence of ocean acidification, which has gone widely unrecognized, is its effect on underwater sound transmission. Low-frequency sound absorption in the ocean occurs due to chemical relaxation of the pH-dependent boric acid-borate ion reaction. As ocean pH drops, sound absorption in the audible range decreases. The decreased sound absorption will amplify ambient noise levels, and enhance long distance sound transmission, although its exact environmental impact is uncertain. Changes in the underwater sound absorption will affect the operation of scientific, commercial, and naval applications that are based on ocean acoustics, with yet unknown consequences for marine life. We project these changes using a global biogeochemical model (HAMOCC), which is forced by the anthropogenic CO2 emissions during the years 1800-2300. Based on model projections, we quantify when and where in the ocean these ocean chemistry induced perturbations in sound absorption will occur.

  1. Cyclic variations in nitrogen uptake rate of soybean plants: effects of pH and mixed nitrogen sources

    NASA Technical Reports Server (NTRS)

    Raper, C. D. Jr; Vessey, J. K.; Henry, L. T.; Chaillou, S.

    1991-01-01

    To determine if the daily pattern of NO3- and NH4+ uptake is affected by acidity or NO3- : NH4+ ratio of the nutrient solution, non-nodulated soybean plants (Glycine max) were exposed for 21 days to replenished, complete nutrient solutions at pH 6.0, 5.5, 5.0, and 4.5 which contained either 1.0 mM NH4+, 1.0 mM NO3- [correction of NO3+], 0.67 mM NH4+ plus 0.33 mM NO3- (2:1 NH4+ : NO3-) [correction of (2:1 NH3+ : NO4-)], or 0.33 mM NH4+ plus 0.67 mM NO3- (1:2 NH4+ : NO3-). Net uptake rates of NH4+ and NO3- were measured daily by ion chromatography as depletion from the replenished solutions. When NH4+ and NO3- were supplied together, cumulative uptake of total nitrogen was not affected by pH or solution NH4+ : NO3- ratio. The cumulative proportion of nitrogen absorbed as NH4+ decreased with increasing acidity; however, the proportional uptake of NH4+ and NO3- was not constant, but varied day-to-day. This day-to-day variation in relative proportions of NH4+ and NO3- absorbed when NH4+ : NO3- ratio and pH of solution were constant indicates that the regulatory mechanism is not directly competitive. Regardless of the effect of pH on cumulative uptake of NH4+, the specific nitrogen uptake rates from mixed and from individual NH4+ and NO3- sources oscillated between maxima and minima at each pH with average periodicities similar to the expected interval of leaf emergence.

  2. Purification and characterization of polyphenol oxidase from cauliflower (Brassica oleracea L.).

    PubMed

    Rahman, Andi Nur Faidah; Ohta, Mayumi; Nakatani, Kazuya; Hayashi, Nobuyuki; Fujita, Shuji

    2012-04-11

    Polyphenol oxidase (PPO) of cauliflower was purified to 282-fold with a recovery rate of 8.1%, using phloroglucinol as a substrate. The enzyme appeared as a single band on sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). The estimated molecular weight of the enzyme was 60 and 54 kDa by SDS-PAGE and gel filtration, respectively. The purified enzyme, called phloroglucinol oxidase (PhO), oxidized phloroglucinol (K(m) = 3.3 mM) and phloroglucinolcarboxylic acid. The enzyme also had peroxidase (POD) activity. At the final step, the activity of purified cauliflower POD was 110-fold with a recovery rate of 3.2%. The PhO and POD showed the highest activity at pH 8.0 and 4.0 and were stable in the pH range of 3.0-11.0 and 5.0-8.0 at 5 °C for 20 h, respectively. The optimum temperature was 55 °C for PhO and 20 °C for POD. The most effective inhibitor for PhO was sodium diethyldithiocarbamate at 10 mM (IC(50) = 0.64 and K(i) = 0.15 mM), and the most effective inhibitor for POD was potassium cyanide at 1.0 mM (IC(50) = 0.03 and K(i) = 29 μM).

  3. Resilience of cold-water scleractinian corals to ocean acidification: Boron isotopic systematics of pH and saturation state up-regulation

    NASA Astrophysics Data System (ADS)

    McCulloch, Malcolm; Trotter, Julie; Montagna, Paolo; Falter, Jim; Dunbar, Robert; Freiwald, André; Försterra, Günter; López Correa, Matthias; Maier, Cornelia; Rüggeberg, Andres; Taviani, Marco

    2012-06-01

    The boron isotope systematics has been determined for azooxanthellate scleractinian corals from a wide range of both deep-sea and shallow-water environments. The aragonitic coral species, Caryophyllia smithii, Desmophyllum dianthus, Enallopsammia rostrata, Lophelia pertusa, and Madrepora oculata, are all found to have relatively high δ11B compositions ranging from 23.2‰ to 28.7‰. These values lie substantially above the pH-dependent inorganic seawater borate equilibrium curve, indicative of strong up-regulation of pH of the internal calcifying fluid (pHcf), being elevated by ˜0.6-0.8 units (ΔpH) relative to ambient seawater. In contrast, the deep-sea calcitic coral Corallium sp. has a significantly lower δ11B composition of 15.5‰, with a corresponding lower ΔpH value of ˜0.3 units, reflecting the importance of mineralogical control on biological pH up-regulation. The solitary coral D. dianthus was sampled over a wide range of seawater pHT and shows an approximate linear correlation with ΔpHDesmo = 6.43 - 0.71pHT (r2 = 0.79). An improved correlation is however found with the closely related parameter of seawater aragonite saturation state, where ΔpHDesmo = 1.09 - 0.14Ωarag (r2 = 0.95), indicating the important control that carbonate saturation state has on calcification. The ability to up-regulate internal pHcf, and consequently Ωcf, of the calcifying fluid is therefore a process present in both azooxanthellate and zooxanthellate aragonitic corals, and is attributed to the action of Ca2+-ATPase in modulating the proton gradient between seawater and the site of calcification. These findings also show that the boron isotopic compositions (δ11Bcarb) of aragonitic corals are highly systematic and consistent with direct uptake of the borate species within the biologically controlled extracellular calcifying medium. We also show that the relatively strong up-regulation of pH and consequent elevation of the internal carbonate saturation state (Ωcf ˜8.5 to ˜13) at the site of calcification by cold-water corals, facilitates calcification at or in some cases below the aragonite saturation horizon, providing a greater ability to adapt to the already low and now decreasing carbonate ion concentrations. Although providing greater resilience to the effects of ocean acidification and enhancing rates of calcification with increasing temperature, the process of internal pHcf up-regulation has an associated energetic cost, and therefore growth-rate cost, of ˜10% per 0.1 pH unit decrease in seawater pHT. Furthermore, as the aragonite saturation horizon shoals with rapidly increasing pCO2 and Ωarag < 1, increased dissolution of the exposed skeleton will ultimately limit their survival in the deep oceans.

  4. An automated method of on-line extraction coupled with flow injection and capillary electrophoresis for phytochemical analysis.

    PubMed

    Chen, Hongli; Ding, Xiuping; Wang, Min; Chen, Xingguo

    2010-11-01

    In this study, an automated system for phytochemical analysis was successfully fabricated for the first time in our laboratory. The system included on-line decocting, filtering, cooling, sample introducing, separation, and detection, which greatly simplified the sample preparation and shortened the analysis time. Samples from the decoction extract were drawn every 5 min through an on-line filter and a condenser pipe to the sample loop from which 20-μL samples were injected into the running buffer and transported into a split-flow interface coupling the flow injection and capillary electrophoresis systems. The separation of glycyrrhetinic acid (GTA) and glycyrrhizic acid (GA) took less than 5 min by using a 10 mM borate buffer (adjusted pH to 8.8) and +10 kV voltage. Calibration curves showed good linearity with correlation coefficients (R) more than 0.9991. The intra-day repeatabilities (n = 5, expressed as relative standard deviation) of the proposed system, obtained using GTA and GA standards, were 1.1% and 0.8% for migration time and 0.7% and 0.9% for peak area, respectively. The mean recoveries of GTA and GA in the off-line extract of Glycyrrhiza uralensis Fisch root were better than 99.0%. The limits of detection (signal-to-noise ratio = 3) of the proposed method were 6.2 μg/mL and 6.9 μg/mL for GTA and GA, respectively. The dynamic changes of GTA and GA on the decoction time were obtained during the on-line decoction process of Glycyrrhiza uralensis Fisch root.

  5. Glutamate cysteine ligase (GCL) in the freshwater bivalve Unio tumidus: impact of storage conditions and seasons on activity and identification of partial coding sequence of the catalytic subunit.

    PubMed

    Coffinet, Stéphanie; Cossu-Leguille, Carole; Rodius, François; Vasseur, Paule

    2008-09-01

    Glutamate cysteine ligase (GCL; EC 6.3.2.2) is the first enzyme involved in the synthesis of glutathione. A HPLC method with fluorimetric detection was used to measure GCL activity in the gills and the digestive gland of the freshwater bivalve, Unio tumidus. Storage conditions were optimized in order to prevent decrease of GCL activity and consisted in freezing the cytosolic fraction in the presence of protease (1 mM phenylmethylsulfonic fluoric acid) and gamma-glutamyltranspeptidase (1 mM L-serine borate mixture and 0.5 mM acivicin) inhibitors. Seasonal variations of activity in the digestive gland and to a lesser extent in the gills were found with activity increasing in spring compared to winter. No sex differences were revealed. The GCL coding sequence was identified using degenerated primers designed in the highly conserved regions of the catalytic subunit of GCL. The partial sequence identified encoded for 121 amino acids. The comparison of the identified partial coding sequence of U. tumidus with those available from vertebrates and invertebrates indicated that GCL sequence was highly conserved.

  6. Unusual stoichiometry control in the atomic layer deposition of manganese borate films from manganese bis(tris(pyrazolyl)borate) and ozone

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

    Klesko, Joseph P.; Bellow, James A.; Saly, Mark J.

    The atomic layer deposition (ALD) of films with the approximate compositions Mn{sub 3}(BO{sub 3}){sub 2} and CoB{sub 2}O{sub 4} is described using MnTp{sub 2} or CoTp{sub 2} [Tp = tris(pyrazolyl)borate] with ozone. The solid state decomposition temperatures of MnTp{sub 2} and CoTp{sub 2} are ∼370 and ∼340 °C, respectively. Preparative-scale sublimations of MnTp{sub 2} and CoTp{sub 2} at 210 °C/0.05 Torr afforded >99% recoveries with <0.1% nonvolatile residues. Self-limited ALD growth was demonstrated at 325 °C for MnTp{sub 2} or CoTp{sub 2} with ozone as the coreactant. The growth rate for the manganese borate process was 0.19 Å/cycle within the ALD window of 300–350 °C. The growth ratemore » for the cobalt borate process was 0.39–0.42 Å/cycle at 325 °C. X-ray diffraction of the as-deposited films indicated that they were amorphous. Atomic force microscopy of 35–36 nm thick manganese borate films grown within the 300–350 °C ALD window showed root mean square surface roughnesses of 0.4–0.6 nm. Film stoichiometries were assessed by x-ray photoelectron spectroscopy and time of flight-elastic recoil detection analysis. The differing film stoichiometries obtained from the very similar precursors MnTp{sub 2} and CoTp{sub 2} are proposed to arise from the oxidizing ability of the intermediate high valent manganese oxide layers and lack thereof for cobalt.« less

  7. Optical absorption and photoluminescence properties of Er3+ doped mixed alkali borate glasses.

    PubMed

    Ratnakaram, Y C; Kumar, A Vijaya; Naidu, D Tirupathi; Rao, J L

    2005-07-01

    An investigations of the optical absorption and fluorescence spectra of 0.2 mol% Er2O3 in mixed alkali borate glasses of the type 67.8B2O3 x xLi2O(32-x)Na2O, 67.8B2O3 x xLi2O(32-x)K2O and 67.8B2O3 x xNa2O(32-x)K2O (where x = 8, 12, 16, 20 and 24) are presented. The glasses were obtained by quenching melts consisting of H3BO3, Li2CO3, Na2CO3, K2CO3 and Er2O3 (950-1100 degrees C, 1.5-2 h) between two brass plates. Spectroscopic parameters like Racah (E1, E2 and E3), spin-orbit (xi(4f)) and configuration interaction (alpha) parameters are deduced as function of x. Using Judd-Ofelt theory, Judd-Ofelt intensity parameters (omega2, omega4 and omega6) are obtained. Radiative and non-radiative transition rates (A(T) and W(MPR)), radiative lifetimes (tauR), branching ratios (beta) and integrated absorption cross-sections (sigma) have been computed for certain excited states of Er3+ in these mixed alkali borate glasses. Emission spectra have been studied for all the three Er3+ doped mixed alkali borate glasses. The present paper throws light on the trends observed in the intensity parameters, radiative lifetimes, branching ratios and emission cross-sections as a function of x in these borate glasses, keeping in view the effect of mixed alkalies in borate glasses.

  8. Final report of the key comparison APMP.QM-K91: APMP comparison on pH measurement of phthalate buffer

    NASA Astrophysics Data System (ADS)

    Hioki, Akiharu; Asakai, Toshiaki; Maksimov, Igor; Suzuki, Toshihiro; Miura, Tsutomu; Ketrin, Rosi; Nuryatini; Thanh, Ngo Huy; Truong Chinh, Nguyen; Vospelova, Alena; Bastkowski, Frank; Sander, Beatrice; Matzke, Jessica; Prokunin, Sergey; Frolov, Dmitry; Aprelev, Alexey; Dobrovolskiy, Vladimir; Uysal, Emrah; Liv, Lokman; Velina Lara-Manzano, Judith; Montero-Ruiz, Jazmin; Ortiz-Aparicio, JosÉ Luis; Ticona Canaza, Galia; Anuar Mohd Amin, Khirul; Abd Kadir, Haslina; Bakovets, Nickolay; Wong, Siu-Kay; Lam, Wai-Hing

    2017-01-01

    The APMP.QM-K91 was organised by TCQM of APMP to test the abilities of the national metrology institutes in the APMP region to measure a pH value of a phthalate buffer. This APMP comparison on pH measurement was proposed by the National Metrology Institute of Japan at the APMP-TCQM meeting held September 22-23, 2014. After approval by TCQM, the comparison has been conducted by NMIJ. The comparison is a key comparison following CCQM-K91. The comparison material was a phthalate buffer of pH around 4.0 and the measurement temperatures were 15 °C, 25 °C and 37 °C. This is the third APMP key comparison on pH measurement and the fifth APMP comparison on pH measurement following APMP.QM-P06 (two phosphate buffers) in 2004, APMP.QM-P09 (a phthalate buffer) in 2006, APMP.QM-K9/APMP.QM-P16 (a phosphate buffer) in 2010-2011 and APMP.QM-K19/APMP.QM-P25 (a borate buffer) in 2013-2014. The results can be used further by any participant to support its CMC claim at least for a phthalate buffer. That claim will concern the pH method employed by the participant during this comparison and will cover the used temperature(s) or the full temperature range between 15°C and 37 °C for the participant which measured pH values at the three temperatures. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

  9. Sex-based differences in veterans with pulmonary hypertension: Results from the veterans affairs-clinical assessment reporting and tracking database.

    PubMed

    Ventetuolo, Corey E; Hess, Edward; Austin, Eric D; Barón, Anna E; Klinger, James R; Lahm, Tim; Maddox, Thomas M; Plomondon, Mary E; Thompson, Lauren; Zamanian, Roham T; Choudhary, Gaurav; Maron, Bradley A

    2017-01-01

    Women have an increased risk of pulmonary hypertension (PH) but better survival compared to men. Few studies have explored sex-based differences in population-based cohorts with PH. We sought to determine whether sex was associated with hemodynamics and survival in US veterans with PH (mean pulmonary artery pressure [mPAP] ≥ 25 mm Hg) from the Veterans Affairs Clinical Assessment, Reporting, and Tracking database. The relationship between sex and hemodynamics was assessed with multivariable linear mixed modeling. Cox proportional hazards models were used to compare survival by sex for those with PH and precapillary PH (mPAP ≥ 25 mm Hg, pulmonary artery wedge pressure [PAWP] ≤ 15 mm Hg and pulmonary vascular resistance [PVR] > 3 Wood units) respectively. The study population included 15,464 veterans with PH, 516 (3%) of whom were women; 1,942 patients (13%) had precapillary PH, of whom 120 (6%) were women. Among those with PH, women had higher PVR and pulmonary artery pulse pressure, and lower right atrial pressure and PAWP (all p <0.001) compared with men. There were no significant differences in hemodynamics according to sex in veterans with precapillary PH. Women with PH had 18% greater survival compared to men with PH (adjusted HR 0.82, 95% CI 0.69-0.97, p = 0.020). Similarly, women with precapillary PH were 29% more likely to survive as compared to men with PH (adjusted HR 0.71, 95% CI 0.52-0.98, p = 0.040). In conclusion, female veterans with PH have better survival than males despite higher pulmonary afterload.

  10. Development of a calibration for the B isotope paleo-pH proxy in the deep sea coral Desmophyllum dianthus

    NASA Astrophysics Data System (ADS)

    Anagnostou, E.; Huang, K.; You, C.; Sherrell, R. M.

    2011-12-01

    The boron isotope ratio (δ11B) of foraminifera and coral carbonate has been proposed to record seawater pH. Here we test this pH proxy in the deep sea coral Desmophyllum dianthus (D. dianthus ). This coral species is cosmopolitan in geographic distribution and tolerates a wide temperature and depth range. Previous studies have shown that fossil D. dianthus skeletons can be dated precisely with U/Th measurements. Additionally, skeletal mass is sufficient for multiple elemental, isotopic, and radiocarbon measurements per sample making it a powerful candidate for paleoceanographic reconstructions. Ten modern corals from a depth range of 274-1470m in the Atlantic, Pacific, and Southern Oceans were analyzed using the sublimation method and multi-collector ICP-MS (Neptune), and the measured δ11B was regressed against ambient pH taken from hydrographic data sets (range pH 7.6 to 8.1). Replicate skeletal subsamples from a single coral agree within 0.35% (2SD). The array of δ11B values for these corals plots above the seawater borate δ11B vs. pH curve (Klochko et al., 2006) by an apparently constant value of 11.7 ± 1.2%, well above the range of values seen in foraminifera and surface corals. This offset is attributed to either partial incorporation of boric acid from seawater or, more likely, to physiological manipulation of the calcifying fluid to pH 8.7-9.0. The uncertainty in calculation of seawater pH from δ11B, dominated by the uncertainty in the offset value, currently limits the precision of absolute pH reconstructions to ±0.09pH units. However, the empirical calibration could be used to examine relative pH changes, thereby overcoming contributions to the uncertainty in the offset that result from the calculation of the empirical fractionation factor α and from sampling bias and variable vital effects among individuals, reducing the reconstruction error envelope. This study provides the first evidence that δ11B in D. dianthus has the potential to record ambient seawater pH.

  11. Dosimetric properties of dysprosium doped lithium borate glass irradiated by 6 MV photons

    NASA Astrophysics Data System (ADS)

    Ab Rasid, A.; Wagiran, H.; Hashim, S.; Ibrahim, Z.; Ali, H.

    2015-07-01

    Undoped and dysprosium doped lithium borate glass system with empirical formula (70-x) B2O3-30 Li2O-(x) Dy2O3 (x=0.1, 0.3, 0.5, 0.7, 1.0 mol%) were prepared using the melt-quenching technique. The dosimetric measurements were performed by irradiating the samples to 6 MV photon beam using linear accelerator (LINAC) over a dose range of 0.5-5.0 Gy. The glass series of dysprosium doped lithium borate glass produced the best thermoluminescence (TL) glow curve with the highest intensity peak from sample with 1.0 mol% Dy2O3 concentration. Minimum detectable dose was detected at 2.24 mGy, good linearity of regression coefficient, high reproducibility and high sensitivity compared to the undoped glass are from 1.0 mol% dysprosium doped lithium borate glass. The results indicated that the series of dysprosium doped lithium glasses have a great potential to be considered as a thermoluminescence dosimetry (TLD).

  12. Impact of vanadium ions in barium borate glass.

    PubMed

    Abdelghany, A M; Hammad, Ahmed H

    2015-02-25

    Combined optical and infrared spectral measurements of prepared barium borate glasses containing different concentrations of V2O5 were carried out. Vanadium containing glasses exhibit extended UV-visible (UV/Vis.) bands when compared with base binary borate glass. UV/Vis. spectrum shows the presence of an unsymmetrical strong UV broad band centered at 214 nm attributed to the presence of unavoidable trace iron impurities within the raw materials used for the preparation of such glass. The calculated direct and indirect optical band gaps are found to decrease with increasing the vanadium content (2.9:137 for indirect and 3.99:2.01 for direct transition). This change was discussed in terms of structural changes in the glass network. Infrared absorption spectra of the glasses reveal the appearance of both triangular and tetrahedral borate units. Electron spin resonance analyses indicate the presence of unpaired species in sufficient quantity to be identified and to confirm the spectral data. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Reliability of Monte Carlo simulations in modeling neutron yields from a shielded fission source

    NASA Astrophysics Data System (ADS)

    McArthur, Matthew S.; Rees, Lawrence B.; Czirr, J. Bart

    2016-08-01

    Using the combination of a neutron-sensitive 6Li glass scintillator detector with a neutron-insensitive 7Li glass scintillator detector, we are able to make an accurate measurement of the capture rate of fission neutrons on 6Li. We used this detector with a 252Cf neutron source to measure the effects of both non-borated polyethylene and 5% borated polyethylene shielding on detection rates over a range of shielding thicknesses. Both of these measurements were compared with MCNP calculations to determine how well the calculations reproduced the measurements. When the source is highly shielded, the number of interactions experienced by each neutron prior to arriving at the detector is large, so it is important to compare Monte Carlo modeling with actual experimental measurements. MCNP reproduces the data fairly well, but it does generally underestimate detector efficiency both with and without polyethylene shielding. For non-borated polyethylene it underestimates the measured value by an average of 8%. This increases to an average of 11% for borated polyethylene.

  14. Borate cross-linking chitosan/graphene oxide films: Toward the simultaneous enhancement of gases barrier and mechanical properties

    NASA Astrophysics Data System (ADS)

    Yan, Ning; Capezzuto, Filomena; Buonocore, Giovanna G.; Tescione, Fabiana; Lavorgna, Marino; Xia, Hesheng; Ambrosio, Luigi

    2015-12-01

    Borate adducts, originated from hydrolysis of sodium tetraborate decahydrate (borax), have been used to crosslink chitosan (CS) and graphene oxide (GO) nanosheets for the production of innovative composite sustainable materials. CS/GO film consisting of 10wt% borax and 1wt% GO exhibits a significant improvement of both toughness and oxygen barrier properties in comparison to pristine chitosan. In particular the tensile strength increases by about 100% and 150% after thermal annealing of samples at 90°C for 50min whereas the oxygen permeability reduces of about 90% compared to pristine chitosan. The enhancement of both mechanical and barrier properties is ascribed to the formation of a resistant network due to the chemical crosslinking, including borate orthoester bonds and hydroxyl moieties complexes, formed among borate ions, chitosan, and GO nanoplatelets. The crosslinked graphene-based chitosan material with its enhanced mechanical and barrier properties may significantly broad the range of applications of chitosan based-materials which presently are very limited and addressed only to packaging.

  15. Vibrational spectroscopy of the borate mineral kotoite Mg₃(BO₃)₂.

    PubMed

    Frost, Ray L; Xi, Yunfei

    2013-02-15

    Vibrational spectroscopy has been used to assess the structure of kotoite a borate mineral of magnesium which is isostructural with jimboite. The mineral is orthorhombic with point group: 2/m 2/m 2/m. The mineral has the potential as a new memory insulator material. The mineral has been characterised by a combination of Raman and infrared spectroscopy. The Raman spectrum is dominated by a very intense band at 835 cm(-1), assigned to the symmetric stretching mode of tetrahedral boron. Raman bands at 919, 985 and 1015 cm(-1) are attributed to the antisymmetric stretching modes of tetrahedral boron. Kotoite is strictly an hydrous borate mineral. An intense Raman band observed at 3559 cm(-1) is attributed to the stretching vibration of hydroxyl units, more likely to be associated with the borate mineral hydroxyborate. The lack of observation of water bending modes proves the absence of water in the kotoite structure. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. New insight in the nature of surface magnetic anisotropy in iron borate

    NASA Astrophysics Data System (ADS)

    Strugatsky, M.; Seleznyova, K.; Zubov, V.; Kliava, J.

    2018-02-01

    The theory of surface magnetism of iron borate, FeBO3, has been extended by taking into consideration a crystal field contribution to the surface magnetic anisotropy energy. For this purpose, a model of distortion of the six-fold oxygen environment of iron ions in the near-surface layer of iron borate has been put forward. The spin Hamiltonian parameters for isolated Fe3+ ions in the distorted environment of the near-surface layer have been calculated using the Newman's superposition model. The crystal field contribution to the surface magnetic anisotropy energy has been calculated in the framework of the perturbation theory. The model developed allows concluding that the distortions of the iron environment produce a significant crystal field contribution to the surface magnetic anisotropy constant. The results of experimental studies of the surface magnetic anisotropy in iron borate can be described assuming the existence of relative contractions in the near-surface layer of the order of 1 %.

  17. Mechanism of Action of Ribavirin: An Antiviral Drug of Military Importance,

    DTIC Science & Technology

    1980-06-01

    was suspended in 120 mM Tris, 60 mM sodium ace- tate, 3 mM EDTA (pH 7.4) plus 10% glycerol and 0.1% bromophenol blue. Following electrophoresis, gels ... polyacryl - amide gels . J. Mol. Biol. 26:373-387. 2. Browne, M. J. 1979. Mechanism and specificity of action of ri- bavirin. Antimicrob. Agents...of 10 mM EDTA, 1% sodi- um dodecylsulfate (SDS) and 0.4 N sodium acetate (pH 5.2) then ex- tracted twice with a mixture of 50% phenol, 49% chloroform

  18. Crystallization and preliminary crystallographic study of 3 alpha, 20 beta-hydroxysteroid dehydrogenase from Streptomyces hydrogenans.

    PubMed

    Fitzgerald, P M; Duax, W L; Punzi, J S; Orr, J C

    1984-05-15

    3 alpha, 20 beta-Hydroxysteroid dehydrogenase, an NADH-dependent oxidoreductase isolated from Streptomyces hydrogenans , is a tetramer containing four subunits each of Mr 25,000. The enzyme has been crystallized by the vapor diffusion technique using either phosphate or borate buffered ammonium sulfate (pH between 6.0 and 8.7) as the precipitant. The crystals are hexagonal bipyramids ; they have the symmetry of space group P6(4)22 (or P6(2)22), with unit cell dimensions a = 127.3 A, c = 112.2 A. Volume and density considerations imply that the crystallographic asymmetric unit contains two monomers, and therefore that the tetramer possesses a 2-fold axis of symmetry that is coincident with a crystallographic 2-fold symmetry element.

  19. Investigation of passive films formed on the surface of alloy 690 in borate buffer solution

    NASA Astrophysics Data System (ADS)

    Jinlong, Lv; Tongxiang, Liang; Chen, Wang; Wenli, Guo

    2015-10-01

    The passive film formed on the surface of the alloy 690 in borate buffer solution was studied by potentiodynamic curves and electrochemical impedance spectroscopy. With the increasing of the passivation potential, the corrosion resistance of the alloy 690 reduced. Moreover, the corrosion resistance of the passive film was the lowest in the vicinity of 0.6 VSCE. These results were supported by XPS and Mott-Schottky analyses. The corrosion resistance of the alloy 690 increased with the increasing of passivated potential in borate buffer solution with chloride ion. The chloride ion decreased corrosion resistance of the alloy 690 according to point defect model.

  20. [Investigations of the efficacy and bio-availability of different pilocarpine eye drops].

    PubMed

    Tapasztó, I; Boross, F

    1982-01-01

    The efficacy of three pilocarpine preparations in different concentrations (pilocarpine borate 0.5%, 1%, 2%; pilocarpine hydrochloride 0.5%, 1%, 2%; pilocarpine nitrate 1%, 2%) was investigated in 57 glaucomatous patients. Pilocarpine borate reduced intraocular pressure more effectively than either of the other pilocarpine solutions. The 2% concentration had a particularly prolonged effect. This finding corresponded well with pilocarpine levels in the aqueous humour of rabbits, as determined by spectrophotometric analysis. Pilocarpine borate 2% revealed an almost two-fold amount of drug compared to the 2% hydrochloride and nitrate solutions, and a detectable pilocarpine level was present for a longer period as well.

  1. The preparation and characterization of a lithium borate glass prepared by the gel technique

    NASA Technical Reports Server (NTRS)

    Weinberg, M. C.; Neilson, G. F.; Smith, G. L.; Dunn, B.; Moore, G. S.; Mackenzie, J. D.

    1985-01-01

    The preparation of an amorphous lithium borate gel by the metal organic procedure is described. In addition, a preliminary evaluation of the behavior of the gel upon heating is given. In particular the crystallization tendency of the gel is studied with the aid of DTA and X-ray diffraction, and the structural changes in the gel are monitored with the aid of IR spectroscopy. The glass produced from the lithium borate gel is compared to both the gel precursor material and a glass of similar composition prepared by conventional techniques. Specifically, the relevant water contents, crystallization behavior, and structural features are contrasted.

  2. Fracturing fluid cleanup by controlled release of enzymes from polyelectrolyte complex nanoparticles

    NASA Astrophysics Data System (ADS)

    Barati Ghahfarokhi, Reza

    Guar-based polymer gels are used in the oil and gas industry to viscosify fluids used in hydraulic fracturing of production wells, in order to reduce leak-off of fluids and pressure, and improve the transport of proppants. After fracturing, the gel and associated filter cake must be degraded to very low viscosities using breakers to recover the hydraulic conductivity of the well. Enzymes are widely used to achieve this but injecting high concentrations of enzyme may result in premature degradation, or failure to gel; denaturation of enzymes at alkaline pH and high temperature conditions can also limit their applicability. In this study, application of polyelectrolyte nanoparticles for entrapping, carrying, releasing and protecting enzymes for fracturing fluids was examined. The objective of this research is to develop nano-sized carriers capable of carrying the enzymes to the filter cake, delaying the release of enzyme and protecting the enzyme against pH and temperature conditions inhospitable to native enzyme. Polyethylenimine-dextran sulfate (PEI-DS) polyelectrolyte complexes (PECs) were used to entrap two enzymes commonly used in the oil industry in order to obtain delayed release and to protect the enzyme from conditions inhospitable to native enzyme. Stability and reproducibility of PEC nanoparticles was assured over time. An activity measurement method was used to measure the entrapment efficiency of enzyme using PEC nanoparticles. This method was confirmed using a concentration measurement method (SDS-PAGE). Entrapment efficiencies of pectinase and a commercial high-temperature enzyme mixture in polyelectrolyte complex nanoparticles were maximized. Degradation, as revealed by reduction in viscoelastic moduli of borate-crosslinked hydroxypropyl guar (HPG) gel by commercial enzyme loaded in polyelectrolyte nanoparticles, was delayed, compared to equivalent systems where the enzyme mixture was not entrapped. This indicates that PEC nanoparticles delay the activity of enzymes by entrapping them. It was also observed that control PEC nanoparticles decreased both viscoelastic moduli, but with a slower rate compared to the PEC nanoparticles loaded with enzyme. Preparation shear and applied shear showed no significant effect on activity of enzyme-loaded PEC nanoparticles mixed with HPG solutions. However, fast addition of chemicals during the preparations showed smaller particle size compared to the drop-wise method. PEC nanoparticles (PECNPs) also protected both enzymes from denaturation at elevated temperature and pH. Following preparation, enzyme-loaded PEC nanoparticles were mixed with borate crosslinked HPG and the mixture was injected through a shear loop. Pectinase-loaded nanoparticles mixed with gelled HPG showed no sensitivity to shear applied along the shear loop at 25 °C. However, EL2X-loaded PEC nanoparticles showed sensitivity to shear applied along the shear loop at 40 °C. Filter cake was formed and degraded in a fluid loss cell for borate crosslinked HPG solutions mixed with either enzymes or enzyme-loaded PEC nanoparticles. Cleanup slopes of filter cake degraded using enzyme-loaded PEC nanoparticles and systems with enzymes mixed with HPG gel were significantly higher than for the filter cake formed with HPG gel mixed with no enzyme. In a different application, enzyme-loaded PEC nanoparticles showed significantly slower reduction in viscosity of HPG solution over time compared to the HPG systems mixed with enzyme. Increasing the viscosity of low concentration HPG, used as slick-water, decreases the proppant settling velocity. This is of specific interest in fracturing fluids used for unconventional reservoirs.

  3. A method for determining the composition of methanol-trimethyl borate mixtures

    NASA Technical Reports Server (NTRS)

    Kaye, Samuel; Sordyl, Frank

    1955-01-01

    A study of mixtures of pure methanol and trimethyl borate showed that the composition can be accurately obtained by a simple density determination. The refractive-index determination gives the composition with much less accuracy. The potentiometric titration of boric acid is also discussed.

  4. INFLUENCE OF BORATE BUFFERS ON THE ELECTROPHORETIC BEHAVIOR OF HUMIC SUBSTANCES IN CAPILLARY ZONE ELECTROPHORESIS

    EPA Science Inventory

    The influence of tetrahydroxyborate ions on the electrophoretic mobility of humic acids was evaluated by capillary electrophoresis (CE). Depending on the molarity of borate ions in the separation buffer, the humic acids exhibit electropherograms with sharp peaks consistently exte...

  5. Isolation of Active Mitochondria From Tomato Fruit 1

    PubMed Central

    Ku, Han San; Pratt, Harlan K.; Spurr, Arthur R.; Harris, William M.

    1968-01-01

    An improved method for isolating mitochondria from tomato fruit (Lycopersicon esculentum Mill.) is described. The fruit is chilled, and the tissue of the fruit wall cut by hand into very thin slices with a razor blade while immersed in a buffer containing 0.4 m sucrose, 2 mm MgCl2, 8 mm EDTA, 4 mm cysteine, 10 mm KCl, 0.5 mg per ml bovine serum albumin 50 mm tris-HCl, pH 7.6. The pH is monitored and kept within the range of 7.0 to 7.2 by dropwise addition of 1 n KOH during cutting. The tissue is strained through 8 layers of cheesecloth and centrifuged at 2000 × g for 15 minutes. The supernatant is then centrifuged at 11,000 × g for 20 minutes, and the sediment is washed once with a medium containing 0.4 m sucrose, 10 mm KCl, 1 mm MgCl2, 10 mm tris-HCl, 10 mm KH2PO4 and bovine serum albumin (0.5 mg per ml), pH 7.2. Electron microscope studies show that this method gives homogeneous, relatively intact mitochondria; they have a higher respiratory control ratio than those reported by other workers. The method was also tested successfully on fruits of cantaloupe and `Honey Dew' melon. Images PMID:16656857

  6. Hydrothermal synthesis and structural analysis of new mixed oxyanion borates: Ba11B26O44(PO4)2(OH)6, Li9BaB15O27(CO3) and Ba3Si2B6O16

    NASA Astrophysics Data System (ADS)

    Heyward, Carla; McMillen, Colin D.; Kolis, Joseph

    2013-07-01

    Several new borate compounds, Ba11B26O44(PO4)2(OH)6 (1), Li9BaB15O27(CO3) (2), and Ba3Si2B6O16 (3) were synthesized containing other hetero-oxyanion building blocks in addition to the borate frameworks. They were all prepared under hydrothermal conditions and characterized by single crystal and powder X-ray diffraction, and IR spectroscopy. Crystal data: For 1; space group P21/c, a=6.8909 (14) Å, b=13.629 (3) Å, c=25.851 (5) Å, β=90.04 (3)°; For 2; space group P-31c, a=8.8599 (13) Å, c=15.148 (3) Å; For 3; space group P-1, a=5.0414 (10) Å, b=7.5602 (15) Å, c=8.5374 (17) Å, α=77.15 (3)°, β=77.84 (3)°, γ=87.41 (3)° for 3. Compounds 1 and 2 contain isolated oxyanions [PO4]3- and [CO3]2- respectively, sitting in channels created by the borate framework, while structure 3 has the [SiO4]4- groups directly bonded to the borate groups creating a B-O-Si framework.

  7. Effects of chronic Akt/mTOR inhibition by rapamycin on mechanical overload-induced hypertrophy and myosin heavy chain transition in masseter muscle.

    PubMed

    Umeki, Daisuke; Ohnuki, Yoshiki; Mototani, Yasumasa; Shiozawa, Kouichi; Fujita, Takayuki; Nakamura, Yoshiki; Saeki, Yasutake; Okumura, Satoshi

    2013-01-01

    To examine the effects of the Akt/mammalian target of rapamycin (mTOR) pathway on masseter muscle hypertrophy and myosin heavy chain (MHC) transition in response to mechanical overload, we analyzed the effects of bite-opening (BO) on the hypertrophy and MHC composition of masseter muscle of BO-rats treated or not treated with rapamycin (RAPA), a selective mTOR inhibitor. The masseter muscle weight in BO-rats was significantly greater than that in controls, and this increase was attenuated by RAPA treatment. Expression of slow-twitch MHC isoforms was significantly increased in BO-rats with/without RAPA treatment, compared with controls, but the magnitude of the increase was much smaller in RAPA-treated BO-rats. Phosphorylation of p44/42 MAPK (ERK1/2), which preserves fast-twitch MHC isoforms in skeletal muscle, was significantly decreased in BO-rats, but the decrease was abrogated by RAPA treatment. Calcineurin signaling is known to be important for masseter muscle hypertrophy and fast-to-slow MHC isoform transition, but expression of known calcineurin activity modulators was unaffected by RAPA treatment. Taken together, these results indicate that the Akt/mTOR pathway is involved in both development of masseter muscle hypertrophy and fast-to-slow MHC isoform transition in response to mechanical overload with inhibition of the ERK1/2 pathway and operates independently of the calcineurin pathway.

  8. Degradable borate glass polyalkenoate cements.

    PubMed

    Shen, L; Coughlan, A; Towler, M; Hall, M

    2014-04-01

    Glass polyalkenoate cements (GPCs) containing aluminum-free borate glasses having the general composition Ag2O-Na2O-CaO-SrO-ZnO-TiO2-B2O3 were evaluated in this work. An initial screening study of sixteen compositions was used to identify regions of glass formation and cement compositions with promising rheological properties. The results of the screening study were used to develop four model borate glass compositions for further study. A second round of rheological experiments was used to identify a preferred GPC formulation for each model glass composition. The model borate glasses containing higher levels of TiO2 (7.5 mol %) tended to have longer working times and shorter setting times. Dissolution behavior of the four model GPC formulations was evaluated by measuring ion release profiles as a function of time. All four GPC formulations showed evidence of incongruent dissolution behavior when considering the relative release profiles of sodium and boron, although the exact dissolution profile of the glass was presumably obscured by the polymeric cement matrix. Compression testing was undertaken to evaluate cement strength over time during immersion in water. The cements containing the borate glass with 7.5 mol % TiO2 had the highest initial compressive strength, ranging between 20 and 30 MPa. No beneficial aging effect was observed-instead, the strength of all four model GPC formulations was found to degrade with time.

  9. Forces of interactions between bare and polymer-coated iron and silica: effect of pH, ionic strength, and humic acids.

    PubMed

    Pensini, Erica; Sleep, Brent E; Yip, Christopher M; O'Carroll, Denis

    2012-12-18

    The interactions between a silica substrate and iron particles were investigated using atomic force microscopy-based force spectroscopy (AFM). The micrometer- and nanosized iron particles employed were either bare or coated with carboxymethyl cellulose (CMC), a polymer utilized to stabilize iron particle suspensions. The effect of water chemistry on the forces of interaction was probed by varying ionic strength (with 100 mM NaCl and 100 mM CaCl₂) or pH (4, 5.5, and 8) or by introducing 10 mg/L of humic acids (HA). When particles were uncoated, the forces upon approach between silica and iron were attractive at pH 4 and 5.5 and in 100 mM CaCl₂ at pH 8, but they were negligible in 100 mM NaCl buffered to pH 8 and repulsive in water buffered to pH 8 and in HA solutions. HA produced electrosteric repulsion between iron particles and silica, likely due to its sorption to iron particles. HA sorption to silica was excluded on the basis of experiments conducted with a quartz-crystal microbalance with dissipation monitoring. Repulsion with CMC-coated iron was attributed to electrosteric forces, which were damped at high ionic strength. An extended DLVO model and a modified version of Ohshima's theory were successfully utilized to model AFM data.

  10. 77 FR 27815 - Aging Management of Stainless Steel Structures and Components in Treated Borated Water

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-05-11

    ... NUCLEAR REGULATORY COMMISSION [NRC-2011-0256] Aging Management of Stainless Steel Structures and... Guidance (LR-ISG), LR-ISG-2011-01, ``Aging Management of Stainless Steel Structures and Components in...) Report for the aging management of stainless steel structures and components exposed to treated borated...

  11. 76 FR 69292 - Aging Management of Stainless Steel Structures and Components in Treated Borated Water

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-11-08

    ... NUCLEAR REGULATORY COMMISSION [NRC-2011-0256] Aging Management of Stainless Steel Structures and... Stainless Steel Structures and Components in Treated Borated Water.'' This LR-ISG revises the guidance in...) and Generic Aging Lessons Learned (GALL) Report for the aging management of stainless steel structures...

  12. 77 FR 74883 - Aging Management of Stainless Steel Structures and Components in Treated Borated Water; Revision 1

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-12-18

    ... NUCLEAR REGULATORY COMMISSION [NRC-2011-0256] Aging Management of Stainless Steel Structures and..., ``Aging Management of Stainless Steel Structures and Components in Treated Borated Water,'' which was... Staff Guidance LR-ISG-2011-01, ``Aging Management of Stainless Steel Structures and Components in...

  13. Could borate have played a role in the RNA World?

    NASA Astrophysics Data System (ADS)

    Grew, E. S.; Bada, J. L.; Hazen, R. M.

    2012-12-01

    Two scenarios have been proposed for boron to play a critical role in the stabilization of ribose and other sugars in the ribonucleic acid (RNA) World, >3.8 Ga ago. One scenario envisages oligomeric RNA being synthesized in subaerial intermountane desert valleys in which groundwater was enriched in borate from breakdown of tourmaline (Benner et al. 2012 doi: 10.1021/ar200332w). In the alternative scenario, borates are enriched in hydrothermal environments (<150°C) in oceanic crust where ferromagnesian minerals are altered to brucite, serpentine and other minerals that can extract borate from the circulating seawater (Holm et al. 2006 doi:10.1186/1467-4866-7-7). Both scenarios presume that (1) B concentrations in non-marine water or sea water were about the same at >3.8 Ma as they are today and (2) plate tectonics was the prevailing regime. The postulated non-marine borate deposits would have been associated with continental collision and subduction with volcanism releasing B, whereas in the second scenario, ocean floor caught up in an early phase of subduction is considered a favorable site for borate formation. Because borate deposits are typically ephemeral and poorly preserved, the lack of evidence in the geologic record for these scenarios does not invalidate them. For example, the oldest reported non-marine borate deposits analogous to the type postulated in first scenario are only 20 Ma, but metamorphosed borates of Precambrian age have been interpreted to have non-marine evaporite precursors, the oldest being 2.4-2.1 Ga in the Liaoning-Jilin area, China. The first B minerals so far reported in the geologic record are metamorphic dravite-schorl tourmalines in the 3.7-3.8 Ga Isua supracrustal belt (southern West Greenland), where there is good evidence for seafloor spreading and subduction. The precursors to the Isua tourmalines are reported to include B-bearing marine clay minerals and detrital tourmaline. The relatively high Li contents in zircon from Jack Hills, Australia, have been cited as evidence for the presence of granitic (s. l.) "protocontinental" crust by 4.3 Ga (Ushikuba et al. 2008 doi:10.1016/j.epsl.2008.05.032; Valley et al. 2010 Rec Geol Surv W Aust, 5-7), but the existence of conventional plate tectonics prior to 3.8 Ga remains controversial. Chaussidon & Appel (1997 Chem Geol 136, 171-180) concluded that boron isotope compositions (δ11B) of tourmaline from Isua volcaniclastic rocks provide no evidence for changes of δ11B in the mantle or continental crust between now and 3.8 Ga, whereas the very light B (δ11B = -20‰) in tourmaline from Isua metachert could indicate that seawater δ11B was at least 10‰ less at 3.8 Ga than now and that there was proportionally less B in sediments at 3.8 Ga, i.e., fractionation of B between depleted mantle, oceans, continental crust and oceanic crust was still in progress (Chaussidon & Albarède 1992, EPSL 108, 229-241). If fractionation and outgassing of boron had not proceeded very far during the RNA World, neither of the proposed scenarios of borate enrichment is plausible, particularly in the absence of a conventional plate tectonics regime.

  14. Pulmonary hypertension in chronic obstructive pulmonary disease.

    PubMed

    Weitzenblum, Emmanuel; Chaouat, Ari; Kessler, Romain

    2013-01-01

    Pulmonary hypertension (PH) is a common complication of advanced chronic obstructive pulmonary disease (COPD) and is defined by a mean pulmonary artery pressure (PAP) ≥ 25 mm Hg at rest in the supine position. Owing to its frequency, COPD is a common cause of PH; in fact, it is the second most frequent cause of PH, just after left heart diseases. PH is due to the elevation of pulmonary vascular resistance, which is caused by functional and morphological factors, chronic alveolar hypoxia being the most important. In COPD PH is generally mild to moderate, PAP usually ranging between 25 and 35 mm Hg in a stable state of the disease. A small proportion of COPD patients may present a severe or "disproportionate" PH with a resting PAP > 35-40 mm Hg. The prognosis is particularly poor in these patients. In COPD PH worsens during exercise, sleep and severe exacerbations of the disease, and these acute increases in afterload may favour the development of right heart failure. The diagnosis of PH relies on Doppler echocardiography, and right heart catheterization is needed in a minority of patients. Treatment of PH in COPD relies on long-term oxygen therapy (≥ 16h/day) which generally stabilizes or at least attenuates the progression of PH. Vasodilator drugs, which are commonly used in idiopathic pulmonary arterial hypertension, have rarely been used in COPD, and we lack studies in this field. Patients with severe PH should be referred to a specialist PH centre where the possibility of inclusion in a controlled clinical trial should be considered.

  15. Note: Detector collimators for the nanoscale ordered materials diffractometer instrument at the Spallation Neutron Source

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

    Tamalonis, A.; Weber, J. K. R.; Neuefeind, J. C.

    2015-09-01

    Five neutron collimator designs were constructed and tested at the nanoscale ordered materials diffractometer (NOMAD) instrument. Collimators were made from High Density PolyEthylene (HDPE) or 5% borated HDPE. In all cases, collimators improved the signal to background ratio and reduced detection of secondary scattering. In the Q-range 10-20 (angstrom) -1, signal to background ratio improved by factors of approximately 1.6 and 2.0 for 50 and 100 mm deep collimators, respectively. In the Q-range 40-50 angstrom -1, the improvement factors were 1.8 and 2.7. Secondary scattering as measured at Q similar to 9.5 angstrom -1 was significantly decreased when the collimatorsmore » were installed.« less

  16. Growth of crystals for synchrotron radiation Mössbauer investigation

    NASA Astrophysics Data System (ADS)

    Kotrbova, M.; Hejduk, J.; Malnev, V. V.; Seleznev, V. N.; Yagupov, S. V.; Andronova, N. V.; Chechin, A. I.; Mikhailov, A. Yu.

    1991-10-01

    Iron borate crystals (FeBO 3) were flux grown at the Physical Institute (Prague) and at Simferopol State University. During the crystal growth procedure the temperature regime was held constant to 0.1°C accuracy. Crystals were investigated with the help of a double crystal X-ray diffractometer DRON-2 (SiO 2(30 overline33)FeBO 3(444), MoK α 1 radiation). The rocking curve measurements were carried out in a constant magnetic field of 1kG. Most of the crystal surface has a rocking curve 10″-15″ wide. Some parts of some crystals with the area 1 × 1 mm 2 have rocking curves of 3″-4″ width and can be considered ideal.

  17. Note: Detector collimators for the nanoscale ordered materials diffractometer instrument at the Spallation Neutron Source

    DOE PAGES

    Tamalonis, A.; Weber, J. K. R.; Neuefeind, J. C.; ...

    2015-09-09

    We constructed and tested five neutron collimator designs using the nanoscale ordered materials diffractometer (NOMAD) instrument. Collimators were made from High Density PolyEthylene (HDPE) or 5% borated HDPE. In all cases, collimators improved the signal to background ratio and reduced detection of secondary scattering. Moreover, in the Q-range 10-20 Å -1, signal to background ratio improved by factors of approximately 1.6 and 2.0 for 50 and 100 mm deep collimators, respectively. In the Q-range 40-50 Å -1, the improvement factors were 1.8 and 2.7. Secondary scattering as measured at Q similar to 9.5 Å -1 was significantly decreased when themore » collimators were installed.« less

  18. DNase 1 Retains Endodeoxyribonuclease Activity Following Gold Nanocluster Synthesis

    DTIC Science & Technology

    2014-07-04

    mM) was added to 2 mL of protein solution under vigorous stirring at 37 °C (Table 1). After 5 min, 200 μL of NaOH (1 M) was added to raise the pH to...12 for the 1, 5, and 10 mM HAuCl4 samples whereas 400 μL of NaOH (1M) was required to obtain a pH of 12 for the 20 mM HAuCl4 sample due to the... magnesium sulfate pH 5.0), containing 2 μg of dsDNA. The reaction was incubated at room temperature for 20 min followed by the addition of 2 units of

  19. Influence of pH and ionic strength (NaCl/Na2SO4) on the reaction HO Cl/ClO- + NO2-

    NASA Astrophysics Data System (ADS)

    Marcellos da Rosa, M.; Zetzsch, C.

    2003-04-01

    Equilibria such as HOCl + NO_2^- leftrightarrow ClNO_2 + OH^- and ClNO_2 + H_2O leftrightarrow NO_3^- + 2H^+ + Cl^- play an important role in halogen activation in the troposphere. We studied the oxidation of NO_2^- by HOCl/ClO^- in aqueous phase by stopped-flow measurements at different ionic strengths (bidestilled water, 0.1M NaCl, 1.0M NaCl and 1.0M Na_2SO^4) at various pH values (4.0, 5.5, 6.2 and 10.0) at 293K. The experiments were performed using a SX.18MV Applied Photophysics spectrophotometer, observing the exponential decay of HOCl/ClO^- at λ = 290nm between 10ms and 100s. HOCl (pK_a= 7.50) was obtained by bubbling N_2 with 1% Cl_2 through bidestilled water. The pH of the aqueous solutions of HOCl was determined by a pH meter (CG820, Schott) with a glass electrode N6180 (calibrated with standard buffer solutions at pH = 3.0, 4.0, 7.0 and 10.0), and the pH values were adjusted by dropwise addition of HClO_4 or NaOH. The concentrations of HOCl (ɛHOCl (230nm) = 100M-1cm-1) ([HOCl] = 1.3mM - 10mM) and ClO- (ɛClO- (292nm) = 350 M-1cm-1) ([ClO^-] = 1.3mM - 5mM) were determined by UV spectrometry (Kontron UVIKON 860) at a resolution of 2 nm in 1 cm cells at various pH values. The concentration range of NO_2^- was between 5mM and 50mM. The following second-order rate constant kII were obtained at 293K at various pH values (in units of M-1s-1) in H_2O: pH 4.0, (5.6±0.3)\\cdot 10^3; pH 5.5, (5.0±0.4)\\cdot 10^3; pH 10.0, 3.9±0.4; in 0.1M NaCl: pH 5.5, (4.3±0.4)\\cdot 10^3; pH 10.0, 2.6±0.4; in 1.0M NaCl: pH 5.5, (4.0±0.3); pH 10.0, 0.7±0.2 and in 1.0M Na_2SO_4: pH 5.5, (3.0±0.3)\\cdot 10^3; pH 10.0, 1.9±0.4. There is a strong effect of the pH on the reaction HOCl/ClO^- + NO_2^-, as reflected in the ratio kII_a(pH 5.5, HOCl)/kII_b(pH 10.0, ClO^-): in H_2O (kII_a ˜ 1200 \\cdot kII_b), in 0.1M NaCl (kII_a ˜ 1900 \\cdot kII_b), in 1.0M NaCl (kII_a ˜ 5700 \\cdot kII_b) and in 1.0 M Na_2SO_4 (kII_a ˜ 1500 \\cdot kII_b). A mechanism for the oxidation of NO_2^- by HOCl/ClO^- will be presented and compared with previous work.

  20. Purification of α-glucosidase from mouse intestine by countercurrent chromatography coupled with a reverse micelle solvent system.

    PubMed

    He, Kai; Zou, Zongyao; Hu, Yinran; Yang, Yong; Xiao, Yubo; Gao, Pincao; Li, Xuegang; Ye, Xiaoli

    2016-02-01

    Countercurrent chromatography coupled with a reverse micelle solvent was applied to separate α-glucosidase, which is stable at pH 6.0-8.8, 15-50°C. The separation conditions are as follows: stationary phase: pH 4.0 Tris-HCl buffer phase containing 50 mM Tris-HCl and 50 mM KCl; mobile phase A: isooctane containing 50 mM anionic surfactant sodium di(2-ethylhexyl)sulfosuccinate; mobile phase B: 50 mM Tris-HCl buffer containing 500 mM KCl (pH 8.0); In total, 25 mL (23.9 mg) crude enzyme was injected through the injection valve, the enzymatic reaction and sodium dodecylsulfate polyacrylamide gel electrophoresis results imply that the activity of purified α-glucosidase is 6.63-fold higher than that of the crude enzyme. Therefore, countercurrent chromatography coupled with a reverse micelle solvent is capable for protein separation and enrichment. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Influence of leaching conditions for ecotoxicological classification of ash.

    PubMed

    Stiernström, S; Enell, A; Wik, O; Hemström, K; Breitholtz, M

    2014-02-01

    The Waste Framework Directive (WFD; 2008/98/EC) states that classification of hazardous ecotoxicological properties of wastes (i.e. criteria H-14), should be based on the Community legislation on chemicals (i.e. CLP Regulation 1272/2008). However, harmonizing the waste and chemical classification may involve drastic changes related to choice of leaching tests as compared to e.g. the current European standard for ecotoxic characterization of waste (CEN 14735). The primary aim of the present study was therefore to evaluate the influence of leaching conditions, i.e. pH (inherent pH (∼10), and 7), liquid to solid (L/S) ratio (10 and 1000 L/kg) and particle size (<4 mm, <1 mm, and <0.125 mm), for subsequent chemical analysis and ecotoxicity testing in relation to classification of municipal waste incineration bottom ash. The hazard potential, based on either comparisons between element levels in leachate and literature toxicity data or ecotoxicity testing of the leachates, was overall significantly higher at low particle size (<0.125 mm) as compared to particle fractions <1mm and <4mm, at pH 10 as compared to pH 7, and at L/S 10 as compared to L/S 1000. These results show that the choice of leaching conditions is crucial for H-14 classification of ash and must be carefully considered in deciding on future guidance procedures in Europe. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. Basal buffer systems for a newly glycosylated recombinant human interferon-β with biophysical stability and DoE approaches.

    PubMed

    Kim, Nam Ah; Song, Kyoung; Lim, Dae Gon; Hada, Shavron; Shin, Young Kee; Shin, Sangmun; Jeong, Seong Hoon

    2015-10-12

    The purpose of this study was to develop a basal buffer system for a biobetter version of recombinant human interferon-β 1a (rhIFN-β 1a), termed R27T, to optimize its biophysical stability. The protein was pre-screened in solution as a function of pH (2-11) using differential scanning calorimetry (DSC) and dynamic light scattering (DLS). According to the result, its experimental pI and optimal pH range were 5.8 and 3.6-4.4, respectively. Design of experiment (DoE) approach was developed as a practical tool to aid formulation studies as a function of pH (2.9-5.7), buffer (phosphate, acetate, citrate, and histidine), and buffer concentration (20 mM and 50 mM). This method employed a weight-based procedure to interpret complex data sets and to investigate critical key factors representing protein stability. The factors used were Tm, enthalpy, and relative helix contents which were obtained by DSC and Fourier Transform Infrared spectroscopy (FT-IR). Although the weights changed by three responses, objective functions from a set of experimental designs based on four buffers were highest in 20 mM acetate buffer at pH 3.6 among all 19 scenarios tested. Size exclusion chromatography (SEC) was adopted to investigate accelerated storage stability in order to optimize the pH value with susceptible stability since the low pH was not patient-compliant. Interestingly, relative helix contents and storage stability (monomer remaining) increased with pH and was the highest at pH 4.0. On the other hand, relative helix contents and thermodynamic stability decreased at pH 4.2 and 4.4, suggesting protein aggregation issues. Therefore, the optimized basal buffer system for the novel biobetter was proposed to be 20 mM acetate buffer at pH 3.8±0.2. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Training Program in the Molecular Basis of Breast Cancer Research

    DTIC Science & Technology

    2000-08-01

    BRCA1 protein and the product was purified by electrophoresis on a 15% polyacryl - interact with the importin-a subunit of the nuclear transport signal...40 mM potassium phos- the 2.0-kb DNA fragment containing the complete ORF of scHEC] was inserted phate [pH 6.5] containing 0.5 M MgC12 and 4...with a mM potassium HEPES [pH 7.7], 0.1 M KCI, 10% glycerol, 2 mM MgC12, 5 mM number of proteins important for GV/M progression and chro- EGTA), 0.5 ml

  4. Functional photoacoustic microscopy of pH

    NASA Astrophysics Data System (ADS)

    Chatni, M. Rameez; Yao, Junjie; Danielli, Amos; Favazza, Christopher P.; Maslov, Konstantin I.; Wang, Lihong V.

    2012-02-01

    pH is a tightly regulated indicator of metabolic activity. In mammalian systems, imbalance of pH regulation may result from or result in serious illness. Even though the regulation system of pH is very robust, tissue pH can be altered in many diseases such as cancer, osteoporosis and diabetes mellitus. Traditional high-resolution optical imaging techniques, such as confocal microscopy, routinely image pH in cells and tissues using pH sensitive fluorescent dyes, which change their fluorescence properties with the surrounding pH. Since strong optical scattering in biological tissue blurs images at greater depths, high-resolution pH imaging is limited to penetration depths of 1mm. Here, we report photoacoustic microscopy (PAM) of commercially available pH-sensitive fluorescent dye in tissue phantoms. Using both opticalresolution photoacoustic microscopy (OR-PAM), and acoustic resolution photoacoustic microscopy (AR-PAM), we explored the possibility of recovering the pH values in tissue phantoms. In this paper, we demonstrate that PAM was capable of recovering pH values up to a depth of 2 mm, greater than possible with other forms of optical microscopy.

  5. Boiling water neutronic reactor incorporating a process inherent safety design

    DOEpatents

    Forsberg, Charles W.

    1987-01-01

    A boiling-water reactor core is positioned within a prestressed concrete reactor vessel of a size which will hold a supply of coolant water sufficient to submerge and cool the reactor core by boiling for a period of at least one week after shutdown. Separate volumes of hot, clean (non-borated) water for cooling during normal operation and cool highly borated water for emergency cooling and reactor shutdown are separated by an insulated wall during normal reactor operation with contact between the two water volumes being maintained at interfaces near the top and bottom ends of the reactor vessel. Means are provided for balancing the pressure of the two volumes at the lower interface zone during normal operation to prevent entry of the cool borated water into the reactor core region, for detecting the onset of excessive power to coolant flow conditions in the reactor core and for detecting low water levels of reactor coolant. Cool borated water is permitted to flow into the reactor core when low reactor coolant levels or excessive power to coolant flow conditions are encountered.

  6. Preparation and characterization of magnesium borate for special glass

    NASA Astrophysics Data System (ADS)

    Dou, Lishuang; Zhong, Jianchu; Wang, Hongzhi

    2010-05-01

    Magnesium borate with a variety of B2O3/MgO molar ratios, which can be applied for special glass, has been prepared through the reaction of light-burned magnesia with boric acid by a hydrothermal method. The effects of the B2O3/MgO molar ratio of raw materials, reaction time, temperature and liquid to solid ratio (ml g-1) on the synthetic product are investigated. The XRD and TG-DTG analyses indicate that the prepared magnesium borate is a mixture of magnesium hexaborate hydrate and ascharite. The results show that high B2O3/MgO molar ratios of raw materials and low reaction liquid-solid ratios favour the product with a high B2O3/MgO molar ratio and vice versa. There exists free MgO in the product when the reaction temperature is below 140 °C or the reaction time is not enough, because of the incomplete reaction of magnesium oxide with boric acid. The process of fractional crystallization for the magnesium borate mixture is also discussed.

  7. Advanced shield development for a fission surface power system for the lunar surface

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

    A. E. Craft; I. J. Silver; C. M. Clark

    A nuclear reactor power system such as the affordable fission surface power system enables a potential outpostonthemoon.Aradiation shieldmustbe included in the reactor system to reduce the otherwise excessive dose to the astronauts and other vital system components. The radiation shield is typically the most massive component of a space reactor system, and thus must be optimized to reduce mass asmuchas possible while still providing the required protection.Various shield options for an on-lander reactor system are examined for outpost distances of 400m and 1 kmfromthe reactor. Also investigated is the resulting mass savings from the use of a high performance cermetmore » fuel. A thermal analysis is performed to determine the thermal behaviours of radiation shields using borated water. For an outpost located 1000m from the core, a tetramethylammonium borohydride shield is the lightest (5148.4 kg), followed by a trilayer shield (boron carbide–tungsten–borated water; 5832.3 kg), and finally a borated water shield (6020.7 kg). In all of the final design cases, the temperature of the borated water remains below 400 K.« less

  8. Silica-Based and Borate-Based, Titania-Containing Bioactive Coatings Characterization: Critical Strain Energy Release Rate, Residual Stresses, Hardness, and Thermal Expansion.

    PubMed

    Rodriguez, Omar; Matinmanesh, Ali; Phull, Sunjeev; Schemitsch, Emil H; Zalzal, Paul; Clarkin, Owen M; Papini, Marcello; Towler, Mark R

    2016-12-01

    Silica-based and borate-based glass series, with increasing amounts of TiO₂ incorporated, are characterized in terms of their mechanical properties relevant to their use as metallic coating materials. It is observed that borate-based glasses exhibit CTE (Coefficient of Thermal Expansion) closer to the substrate's (Ti6Al4V) CTE, translating into higher mode I critical strain energy release rates of glasses and compressive residual stresses and strains at the coating/substrate interface, outperforming the silica-based glasses counterparts. An increase in the content of TiO₂ in the glasses results in an increase in the mode I critical strain energy release rate for both the bulk glass and for the coating/substrate system, proving that the addition of TiO₂ to the glass structure enhances its toughness, while decreasing its bulk hardness. Borate-based glass BRT3, with 15 mol % TiO₂ incorporated, exhibits superior properties overall compared to the other proposed glasses in this work, as well as 45S5 Bioglass ® and Pyrex.

  9. Silica-Based and Borate-Based, Titania-Containing Bioactive Coatings Characterization: Critical Strain Energy Release Rate, Residual Stresses, Hardness, and Thermal Expansion

    PubMed Central

    Rodriguez, Omar; Matinmanesh, Ali; Phull, Sunjeev; Schemitsch, Emil H.; Zalzal, Paul; Clarkin, Owen M.; Papini, Marcello; Towler, Mark R.

    2016-01-01

    Silica-based and borate-based glass series, with increasing amounts of TiO2 incorporated, are characterized in terms of their mechanical properties relevant to their use as metallic coating materials. It is observed that borate-based glasses exhibit CTE (Coefficient of Thermal Expansion) closer to the substrate’s (Ti6Al4V) CTE, translating into higher mode I critical strain energy release rates of glasses and compressive residual stresses and strains at the coating/substrate interface, outperforming the silica-based glasses counterparts. An increase in the content of TiO2 in the glasses results in an increase in the mode I critical strain energy release rate for both the bulk glass and for the coating/substrate system, proving that the addition of TiO2 to the glass structure enhances its toughness, while decreasing its bulk hardness. Borate-based glass BRT3, with 15 mol % TiO2 incorporated, exhibits superior properties overall compared to the other proposed glasses in this work, as well as 45S5 Bioglass® and Pyrex. PMID:27916951

  10. Benzoate- and Salicylate-Tolerant Strains of Escherichia coli K-12 Lose Antibiotic Resistance during Laboratory Evolution

    PubMed Central

    Creamer, Kaitlin E.; Ditmars, Frederick S.; Basting, Preston J.; Kunka, Karina S.; Hamdallah, Issam N.; Bush, Sean P.; Scott, Zachary; He, Amanda; Penix, Stephanie R.; Gonzales, Alexandra S.; Eder, Elizabeth K.; Camperchioli, Dominic W.; Berndt, Adama; Clark, Michelle W.; Rouhier, Kerry A.

    2016-01-01

    ABSTRACT Escherichia coli K-12 W3110 grows in the presence of membrane-permeant organic acids that can depress cytoplasmic pH and accumulate in the cytoplasm. We conducted experimental evolution by daily diluting cultures in increasing concentrations of benzoic acid (up to 20 mM) buffered at external pH 6.5, a pH at which permeant acids concentrate in the cytoplasm. By 2,000 generations, clones isolated from evolving populations showed increasing tolerance to benzoate but were sensitive to chloramphenicol and tetracycline. Sixteen clones grew to stationary phase in 20 mM benzoate, whereas the ancestral strain W3110 peaked and declined. Similar growth occurred in 10 mM salicylate. Benzoate-evolved strains grew like W3110 in the absence of benzoate, in media buffered at pH 4.8, pH 7.0, or pH 9.0, or in 20 mM acetate or sorbate at pH 6.5. Genomes of 16 strains revealed over 100 mutations, including single-nucleotide polymorphisms (SNPs), large deletions, and insertion knockouts. Most strains acquired deletions in the benzoate-induced multiple antibiotic resistance (Mar) regulon or in associated regulators such as rob and cpxA, as well as the multidrug resistance (MDR) efflux pumps emrA, emrY, and mdtA. Strains also lost or downregulated the Gad acid fitness regulon. In 5 mM benzoate or in 2 mM salicylate (2-hydroxybenzoate), most strains showed increased sensitivity to the antibiotics chloramphenicol and tetracycline; some strains were more sensitive than a marA knockout strain. Thus, our benzoate-evolved strains may reveal additional unknown drug resistance components. Benzoate or salicylate selection pressure may cause general loss of MDR genes and regulators. IMPORTANCE Benzoate is a common food preservative, and salicylate is the primary active metabolite of aspirin. In the gut microbiome, genetic adaptation to salicylate may involve loss or downregulation of inducible multidrug resistance systems. This discovery implies that aspirin therapy may modulate the human gut microbiome to favor salicylate tolerance at the expense of drug resistance. Similar aspirin-associated loss of drug resistance might occur in bacterial pathogens found in arterial plaques. PMID:27793830

  11. Total chemical synthesis of human matrix Gla protein

    PubMed Central

    Hackeng, Tilman M.; Rosing, Jan; Spronk, Henri M.H.; Vermeer, Cees

    2001-01-01

    Human matrix Gla protein (MGP) is a vitamin K–dependent extracellular matrix protein that binds Ca2+ ions and that is involved in the prevention of vascular calcification. MGP is a 10.6-kD protein (84 amino acids) containing five γ-carboxyglutamic acid (Gla) residues and one disulfide bond. Studies of the mechanism by which MGP prevents calcification of the arterial media are hampered by the low solubility of the protein (<10 μg/mL). Because of solubility problems, processing of a recombinantly expressed MGP-fusion protein chimera to obtain MGP was unsuccessful. Here we describe the total chemical synthesis of MGP by tBoc solid-phase peptide synthesis (SPPS) and native chemical ligation. Peptide Tyr1-Ala53 was synthesized on a derivatized resin yielding a C-terminal thioester group. Peptide Cys54-Lys84 was synthesized on Lys-PAM resin yielding a C-terminal carboxylic acid. Subsequent native chemical ligation of the two peptides resulted in the formation of a native peptide bond between Ala53 and Cys54. Folding of the 1–84-polypeptide chain in 3 M guanidine (pH 8) resulted in a decrease of molecular mass from 10,605 to 10,603 (ESI-MS), representing the loss of two protons because of the formation of the Cys54-Cys60 internal disulfide bond. Like native MGP, synthetic MGP had the same low solubility when brought into aqueous buffer solutions with physiological salt concentrations, confirming its native like structure. However, the solubility of MGP markedly increased in borate buffer at pH 7.4 in the absence of sodium chloride. Ca2+-binding to MGP was confirmed by analytical HPLC, on which the retention time of MGP was reduced in the presence of CaCl2. Circular dichroism studies revealed a sharp increase in α-helicity at 0.2 mM CaCl2 that may explain the Ca2+-dependent shift in high-pressure liquid chromatography (HPLC)-retention time of MGP. In conclusion, facile and efficient chemical synthesis in combination with native chemical ligation yielded MGP preparations that can aid in unraveling the mechanism by which MGP prevents vascular calcification. PMID:11274477

  12. Increased rate of adenine incorporation into adenine nucleotide pool in erythrocytes of patients with chronic renal failure.

    PubMed

    Marlewski, M; Smolenski, R T; Szolkiewicz, M; Aleksandrowicz, Z; Rutkowski, B; Swierczynski, J

    2000-11-01

    Elevated purine nucleotide pool (mainly ATP) in erythrocytes of patients with chronic renal failure (CRF) is a known phenomenon, however the mechanism responsible for this abnormality is far from being clear. We hypothesize that the increased rate of adenine incorporation into adenine nucleotide pool is responsible for the elevated level of ATP in uremic erythrocytes. In chronically uremic patients we evaluated using HPLC technique: (a) plasma adenine concentration; (b) the rate of adenine incorporation into adenine nucleotide pool in uremic erythrocytes. Additionally, the effect of higher than physiological phosphate concentration (2.4 mM) and lower than physiological pH (7.1) on adenine incorporation into erythrocytes adenine nucleotide pool was investigated. Healthy volunteers with normal renal function served as control. The concentration of adenine in plasma of CRF patients was found to be significantly higher than in plasma of healthy subjects. In contrast, adenosine concentration was similar both in healthy humans and in CRF patients. In isolated erythrocytes of uremic patients (incubated in the medium pH 7.4, containing 1.2 mM inorganic phosphate) adenine was incorporated into adenine nucleotide pool at a rate approximately 2-fold higher than in erythrocytes from healthy subjects. The rate of adenosine incorporation into adenine nucleotide pool was similar in erythrocytes of both studied groups. Incubation of erythrocytes obtained from healthy subjects in the medium pH 7.4, containing 2.4 mM inorganic phosphate, caused the increase of adenine incorporation into adenine nucleotide pool by about 60%. Incubation of the cells in the pH 7.1 buffer containing 2. 4 mM inorganic phosphate increased the rate of adenine incorporation into adenylate approximately 2-fold as compared to erythrocytes incubated in the medium pH 7.4 containing 1.2 mM inorganic phosphate. Erythrocytes obtained from uremic patients and incubated in the pH 7.1 medium containing 2.4 mM phosphate incorporated adenine into adenine nucleotide pool at a rate similar to erythrocytes incubated in the medium pH 7.4 containing 1.2 mM phosphate. Erythrocytes obtained from either healthy subjects or from patients with CRF and incubated in the presence of higher than physiological concentration of inorganic phosphate (2.4 mM) and lower than physiological pH (7. 1) did not exhibit any increase in the rate of adenisine incorporation into adenine nucleotide pool. These results suggest that the increased rate of adenine incorporation into adenine nucleotide pool could be partially responsible for the increased concentration of ATP in uremic erythrocytes. Copyright 2000 S. Karger AG, Basel

  13. Buffer salt effects in off-line coupling of capillary electrophoresis and mass spectrometry.

    PubMed

    Marák, Jozef; Stanová, Andrea

    2014-05-01

    In this work, the impact of buffer salts/matrix effects on the signal in direct injection MS with an electrospray interface (DI-ESI-MS) following pITP fractionation of the sample was studied. A range of buffers frequently used in CE analyses (pH 3-10) was prepared containing 10, 50, and 90% v/v of ACN, respectively. The sets of calibration solutions of cetirizine (an antihistaminic drug with an amphiprotic character) within a 0.05-2.0 mg/L concentration range were prepared in different buffers. The greatest enhancements in the MS signal (in terms of change in the slope of the calibration line) were obtained for the beta-alanine buffer (pH 3.5) in positive ionization and for the borate buffer (pH 9.2) in negative ionization, respectively. The procedure was successfully applied to the analysis of buserelin (a peptidic drug). The slope of the calibration line for solutions containing the beta-alanine buffer with 50% of ACN was 4 times higher than for water or urine, respectively. This study clearly demonstrates that the buffer salt/matrix effects in an offline combination of pITP and DI-ESI-MS can also play a positive role, as they can enhance the signal in MS. A similar influence of the above effects can also be presumed in the CE techniques combined on-line with ESI-MS.

  14. The Use of a Fractional Factorial Design to Determine the Factors That Impact 1,3-Propanediol Production from Glycerol by Halanaerobium hydrogeniformans.

    PubMed

    Kalia, Shivani; Trager, Jordan; Sitton, Oliver C; Mormile, Melanie R

    2016-08-20

    In recent years, biodiesel, a substitute for fossil fuels, has led to the excessive production of crude glycerol. The resulting crude glycerol can possess a high concentration of salts and an alkaline pH. Moreover, current crude glycerol purification methods are expensive, rendering this former commodity a waste product. However, Halanaerobium hydrogeniformans, a haloalkaliphilic bacterium, possesses the metabolic capability to convert glycerol into 1,3-propanediol, a valuable commodity compound, without the need for salt dilution or adjusting pH when grown on this waste. Experiments were performed with different combinations of 24 medium components to determine their impact on the production of 1,3-propanediol by using a fractional factorial design. Tested medium components were selected based on data from the organism's genome. Analysis of HPLC data revealed enhanced production of 1,3-propanediol with additional glycerol, pH, vitamin B12, ammonium ions, sodium sulfide, cysteine, iron, and cobalt. However, other selected components; nitrate ions, phosphate ions, sulfate ions, sodium:potassium ratio, chloride, calcium, magnesium, silicon, manganese, zinc, borate, nickel, molybdenum, tungstate, copper and aluminum, did not enhance 1,3-propanediol production. The use of a fractional factorial design enabled the quick and efficient assessment of the impact of 24 different medium components on 1,3-propanediol production from glycerol from a haloalkaliphilic bacterium.

  15. Assessment of Salivary Flow Rate and pH Among Areca Nut Chewers and Oral Submucous Fibrosis Subjects: A Comparative Study.

    PubMed

    Abdul Khader, Nishat Fatima; Dyasanoor, Sujatha

    2015-09-01

    To assess and compare the salivary flow rate (SFR) and salivary pH among areca nut chewers, oral submucous fibrosis (OSMF) patients and apparently healthy individuals. A comparative study was conducted to assess and compare the SFR and pH among 135 outpatients (45 areca nut chewers + 45 OSMF + 45 control) at The Oxford Dental College and Research Hospital, Bangalore, India. Subjects were interviewed using structural proforma and Modified Schirmer strips and pH paper were implemented for assessing SFR and pH respectively. Statistical analysis was done using IBM SPSS ver. 21.0 software. A statistically significant increase in SFR (35.7 mm at 3rd minutes) among areca nut group and a decrease in SFR among OSMF group (23.4 mm at 3rd minutes) when compared to apparently healthy subjects (30.7 mm at 3rd minutes). The mean pH among areca nut, OSMF and control groups was 6.76, 6.82, and 6.74 respectively with no statistical significance. The observation and findings of the study clearly showed hypersalivation among areca nut group and hyposalivation among OSMF group, with no significant change in salivary pH when compared to healthy subjects.

  16. Extracellular acidosis and very low [Na+ ] inhibit NBCn1- and NHE1-mediated net acid extrusion from mouse vascular smooth muscle cells.

    PubMed

    Bonde, L; Boedtkjer, E

    2017-10-01

    The electroneutral Na + , HCO3- cotransporter NBCn1 and Na + /H + exchanger NHE1 regulate acid-base balance in vascular smooth muscle cells (VSMCs) and modify artery function and structure. Pathological conditions - notably ischaemia - can dramatically perturb intracellular (i) and extracellular (o) pH and [Na + ]. We examined effects of low [Na + ] o and pH o on NBCn1 and NHE1 activity in VSMCs of small arteries. We measured pH i by 2',7'-bis-(2-carboxyethyl)-5-(and-6)-carboxyfluorescein-based fluorescence microscopy of mouse mesenteric arteries and induced intracellular acidification by NH4+ prepulse technique. NBCn1 activity - defined as Na + -dependent, amiloride-insensitive net base uptake with CO 2 /HCO3- present - was inhibited equally when pH o decreased from 7.4 (22 mm HCO3-/5% CO 2 ) by metabolic (pH o 7.1/11 mm HCO3-: 22 ± 8%; pH o 6.8/5.5 mm HCO3-: 61 ± 7%) or respiratory (pH o 7.1/10% CO 2 : 35 ± 11%; pH o 6.8/20% CO 2 : 56 ± 7%) acidosis. Extracellular acidosis more prominently inhibited NHE1 activity - defined as Na + -dependent net acid extrusion without CO 2 /HCO3- present - at both pH o 7.1 (45 ± 9%) and 6.8 (85 ± 5%). Independently of pH o , lowering [Na + ] o from 140 to 70 mm reduced NBCn1 and NHE1 activity <20% whereas transport activities declined markedly (25-50%) when [Na + ] o was reduced to 35 mm. Steady-state pH i decreased more during respiratory (ΔpH i /ΔpH o  = 71 ± 4%) than metabolic (ΔpH i /ΔpH o  = 30 ± 7%) acidosis. Extracellular acidification inhibits NBCn1 and NHE1 activity in VSMCs. NBCn1 is equivalently inhibited when pCO 2 is raised or [HCO3-] o decreased. Lowering [Na + ] o inhibits NBCn1 and NHE1 markedly only below the typical physiological and pathophysiological range. We propose that inhibition of Na + -dependent net acid extrusion at low pH o protects against cellular Na + overload at the cost of intracellular acidification. © 2017 Scandinavian Physiological Society. Published by John Wiley & Sons Ltd.

  17. Solution and particle effects on the biosorption of heavy metals by seaweed biomass

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

    Leusch, A.; Holan, Z.R.; Volesky, B.

    Biosorption of cadmium (Cd), cobalt (Co), copper (Cu), nickel (Ni), lead (Pb), and zinc (Zn) by six fractions of particle sizes, ranging from 0.063 to 1.4 mm of dry marine algal biomass of Sargassum fluitans and Ascophyllum nodosum, is examined. Equilibrium metal uptake by larger particles was higher than that by smaller particles in the order of Pb > Cd > Cu > Co > Zn > Ni for both biomass types, with S. fluitans sorbing slightly more than A. nodosum. Uptakes of metals ranged from the highest, q{sub max} = 369 mg Pb/g (particle size 0.84-1.00 mm), to themore » low Zn and Ni uptakes, q{sub max} = 77 mg/g (size 0.84-1.00 mm) for S. fluitans. A. nodosum adsorbed metals in the range from q{sub max} = 287 mg Pg/g (particle size 0.84-1.00 mm) to q{sub max} = 73 mg Zn/g (particle size 0.84-1.00mm). Harder stipe fractions of S. fluitans demonstrated generally higher metal uptakes than the softer fractions derived from its blades (leaves). The pH dependence of the Zn uptake by S. fluitans exhibited an S-shaped curve between pH 1.5 and pH 7, with 50% of the maximum (pH 7.0) uptake at pH 3.5. Monovalent Na and K ions at higher concentrations inhibited the biosorption of Zn by S. fluitans. A significant inhibition started at 50 mM potassium chloride or sodium acetate, and at 1M the biosorption was completely blocked. 40 refs., 8 figs., 3 tabs.« less

  18. Reactivity of cyclopentadienyl transition metal(ii) complexes with borate ligands: structural characterization of the toluene-activated molybdenum complex [Cp*Mo(CO)2(η3-CH2C6H5)].

    PubMed

    Ramalakshmi, Rongala; Maheswari, K; Sharmila, Dudekula; Paul, Anamika; Roisnel, Thierry; Halet, Jean-François; Ghosh, Sundargopal

    2016-10-18

    Reactions of cyclopentadienyl transition-metal halide complexes [Cp*Mo(CO) 3 Cl], 1, and [CpFe(CO) 2 I], 2, (Cp = C 5 H 5 ; Cp* = η 5 -C 5 Me 5 ) with borate ligands are reported. Treatment of 1 with [NaBt 2 ] (Bt 2 = dihydrobis(2-mercapto-benzothiazolyl)borate) in toluene yielded [Cp*Mo(CO) 2 (C 7 H 4 S 2 N)], 3, and [Cp*Mo(CO) 2 (η 3 -CH 2 C 6 H 5 )], 4, with a selective binding of toluene through C-H activation followed by orthometallation. Note that compound 4 is a structurally characterized toluene-activated molecule in which the metal is in η 3 -coordination mode. Under similar reaction conditions, [NaPy 2 ] (Py 2 = dihydrobis(2-mercaptopyridyl)borate) produced only the mercaptopyridyl molybdenum complex [Cp*Mo(CO) 2 (C 5 H 4 SN)], 5, in good yield. On the other hand, when compound 2 was treated individually with [NaBt] (Bt = trihydro(2-mercapto-benzothiazolyl)borate) and [NaPy 2 ] in THF, formation of the η 1 -coordinated complexes [CpFe(CO) 2 (C 7 H 4 S 2 N)], 6, and [CpFe(CO) 2 (C 5 H 4 SN)], 7, was observed. The solid-state molecular structures of compounds 3, 4, 6, and 7 have been established by single-crystal X-ray crystallographic analyses.

  19. Influence of pH, benzoic acid, glutathione, EDTA, 4-hexylresorcinol, and sodium chloride on the pressure inactivation kinetics of mushroom polyphenol oxidase.

    PubMed

    Weemaes, C A; Ludikhuyze, L R; Van den Broeck, I; Hendrickx, M E

    1999-09-01

    Pressure inactivation of mushroom PPO was studied for pH values ranging from 4 to 8, and the effect of some antibrowning agents on the pressure stability of mushroom PPO at pH 6.5 was evaluated. pH reduction below 6.5 resulted in a lowered inactivation threshold pressure and an increase of the absolute value of the activation volume (or a decrease of the z(p) value), the latter two parameters reflecting the pressure dependency of the inactivation rate constant. An increase in pH from 6.5 to 8, on the other hand, did only marginally affect the pressure stability of the enzyme. Mushroom PPO at pH 6.5 was markedly sensitized toward pressure by the presence of 2.5 mM 4-hexylresorcinol and slightly stabilized by the presence of 5 mM EDTA. The presence of 5 mM glutathione, sodium chloride, or benzoic acid caused no significant alteration of the enzyme pressure stability. Only in the presence of 4-hexylresorcinol, significant changes of the activation volume and z(p) value were noticed.

  20. Relationship between Eu{sup 3+} reduction and glass polymeric structure in Al{sub 2}O{sub 3}-modified borate glasses under air atmosphere

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

    Jiao, Qing; Yu, Xue; Xu, Xuhui

    2013-06-15

    The reduction of Eu{sup 3+} to Eu{sup 2+} is realized efficiently in Eu{sub 2}O{sub 3}-doped borate glasses prepared under air condition by melting-quenching method. Luminescent spectra show an increasing tendency of Eu{sup 2+} emission with increasing Al{sub 2}O{sub 3} concentration in B{sub 2}O{sub 3}–Na{sub 2}O glasses. It is interesting that significant enhancement appeared of Eu{sup 2+} luminescence in the Al{sub 2}O{sub 3}-rich sample comparing to the samples of Al{sub 2}O{sub 3} less than 6 mol%. FTIR and Raman scattering measurements indicated that some new vibration modes assigned to the low-polymerized structure groups decomposed from the slight Al{sub 2}O{sub 3} dopantmore » samples. These results demonstrated that the polymerization of the glass structure decreased with increasing incorporation of Al{sub 2}O{sub 3} into the borate glasses, linking to the efficiency of Eu{sup 3+} self-reduction in air at high temperature. - graphical abstract: A novel europium valence reduction phenomenon occurred in Al{sub 2}O{sub 3} modified borate glasses, FTIR and Raman measurements revealed that high polymeric groups were destroyed to low polymery structures with Al{sub 2}O{sub 3} addition. - Highlights: • The efficient reduction of Eu{sup 3+} to Eu{sup 2+} is observed in the B{sub 2}O{sub 3}–Na{sub 2}O glasses. • Eu{sup 2+} luminescence is significant enhanced in the Al{sub 2}O{sub 3}-rich glasses. • The introduction of Al{sub 2}O{sub 3} changed the network structure of the borate glasses. • High polymeric borate groups in the glass matrix may be destroyed to the lower ones.« less

  1. Borate cross-linked graphene oxide-chitosan as robust and high gas barrier films

    NASA Astrophysics Data System (ADS)

    Yan, Ning; Capezzuto, Filomena; Lavorgna, Marino; Buonocore, Giovanna G.; Tescione, Fabiana; Xia, Hesheng; Ambrosio, Luigi

    2016-05-01

    Chitosan (CS) is one of the most promising polymers due to its biocompatibility, biodegradability, and natural abundance. However, its poor mechanical and barrier properties make it difficult to satisfy a wide range of applications. Herein, borate ions, originating from the hydrolysis of sodium tetraborate decahydrate (borax), have been used to crosslink chitosan and graphene oxide (GO) nanocomposites. Chitosan films consisting of 1.0 wt% boron and 1.0 wt% GO exhibit a significant improvement in both the toughness and oxygen barrier properties compared to pristine chitosan. In particular the tensile strength of the samples after thermal treatment increases by ~160% compared to pristine chitosan, whereas their oxygen permeability reduces by ~90%. This is ascribed to the chemical crosslinking between chitosan and GO nanoplatelets through borate ions, as well as the formation of a layered morphology with graphene nanoplatelets oriented parallel to the sample surface. The exceptional robust and high gas barrier film has promising application in the packaging industry. The borate-crosslinking chemistry represents the potential strategy for improving properties of other polymer nanocomposites.Chitosan (CS) is one of the most promising polymers due to its biocompatibility, biodegradability, and natural abundance. However, its poor mechanical and barrier properties make it difficult to satisfy a wide range of applications. Herein, borate ions, originating from the hydrolysis of sodium tetraborate decahydrate (borax), have been used to crosslink chitosan and graphene oxide (GO) nanocomposites. Chitosan films consisting of 1.0 wt% boron and 1.0 wt% GO exhibit a significant improvement in both the toughness and oxygen barrier properties compared to pristine chitosan. In particular the tensile strength of the samples after thermal treatment increases by ~160% compared to pristine chitosan, whereas their oxygen permeability reduces by ~90%. This is ascribed to the chemical crosslinking between chitosan and GO nanoplatelets through borate ions, as well as the formation of a layered morphology with graphene nanoplatelets oriented parallel to the sample surface. The exceptional robust and high gas barrier film has promising application in the packaging industry. The borate-crosslinking chemistry represents the potential strategy for improving properties of other polymer nanocomposites. Electronic supplementary information (ESI) available: Detailed characterization methods and survey XPS spectra. See DOI: 10.1039/c6nr00377j

  2. Barium recovery by crystallization in a fluidized-bed reactor: effects of pH, Ba/P molar ratio and seed.

    PubMed

    Su, Chia-Chi; Reano, Resmond L; Dalida, Maria Lourdes P; Lu, Ming-Chun

    2014-06-01

    The effects of process conditions, including upward velocity inside the column, the amount of added seed and seed size, the pH value of the precipitant or the phosphate stream and the Ba/P molar ratio in a fluidized-bed reactor (FBR) were studied with a view to producing BaHPO₄ crystals of significant size and maximize the removal of barium. XRD were used to identify the products that were collected from the FBR. Experimental results show that an upward velocity of 48 cmmin(-1) produced the largest BaHPO₄ crystals with a size of around 0.84-1.0mm. The addition of seed crystals has no effect on barium removal. The use of a seed of a size in the ranges unseeded<0.149-0.29 mm<0.149 mm<0.29-0.42 mm produced increasing amounts of increasingly large crystals. The largest BaHPO₄ crystals were obtained at pH 8.4-8.8 with a Ba/P molar ratio of 1.0. In the homogeneous and heterogeneous processes, around 98% of barium was removed at pH 8.4-8.6 and [Ba]/[P]=1.0. The XRD results show that a significant amount of barium phosphate (Ba₃(PO₄)₂) was obtained at pH 11. The compounds BaHPO₄ and BaO were present at a pH of below 10. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Matching phosphate and maleate buffer systems for dissolution of weak acids: Equivalence in terms of buffer capacity of bulk solution or surface pH?

    PubMed

    Cristofoletti, Rodrigo; Dressman, Jennifer B

    2016-06-01

    The development of in vitro dissolution tests able to anticipate the in vivo fate of drug products has challenged pharmaceutical scientists over time, especially in the case of ionizable compounds. In the seminal model proposed by Mooney et al. thirty-five years ago, the pH at the solid-liquid interface (pH0) was identified as a key parameter in predicting dissolution rate. In the current work it is demonstrated that the in vitro dissolution of the weak acid ibuprofen in maleate and phosphate buffer systems is a function of the pH0, which in turn is affected by properties of the drug and the medium. The reported pH0 for ibuprofen dissolution in bicarbonate buffer, the predominant buffer species in the human small intestine under fasting conditions, can be achieved by reducing the phosphate buffer concentration to 5.0mM or the maleate buffer concentration to 2.2mM. Using this approach to identify the appropriate buffer/buffer capacity combination for in vitro experiments in FaSSIF-type media, it would be possible to increase the physiological relevance of this important biopharmaceutics tool. However, the necessity of monitoring and adjusting the bulk pH during the experiments carried out in 5.0mM phosphate or 2.2mM maleate buffers must also be taken into consideration. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. A water-soluble and water-coordinated Mn(II) complex: synthesis, characterization and phantom MRI image study.

    PubMed

    Phukan, Bedika; Patel, Anant B; Mukherjee, Chandan

    2015-08-07

    Ligand H4bedik was reacted with MnCl2·4H2O at pH ∼ 6.5 to give a highly water-soluble and water-coordinated Mn(ii) complex (). The complex was found to show r1 = 3.11 mM(-1) s(-1) per Mn(ii) at 1.4 T and 6.26 mM(-1) s(-1) per Mn(ii) at 14.1 T at 25 °C, pH = 7.4. In addition to r1, the r2 at 14.1 T was found to be 132.78 mM(-1) s(-1) per Mn(ii) at 25 °C, pH = 7.4.

  5. The impact of concomitant pulmonary hypertension on early and late outcomes following surgery for mitral stenosis.

    PubMed

    Yang, Bo; DeBenedictus, Christina; Watt, Tessa; Farley, Sean; Salita, Alona; Hornsby, Whitney; Wu, Xiaoting; Herbert, Morley; Likosky, Donald; Bolling, Steven F

    2016-08-01

    To provide initial evidence on the management of mitral stenosis and pulmonary hypertension (PH) based on short-term and long-term outcomes following mitral valve surgery. Consecutive patients with mitral stenosis (n = 317) who had undergone mitral valve surgery between 1992 and 2014 with recorded pulmonary artery pressure (PAP) data were reviewed. PH severity, based on systolic PAP, was categorized as mild (35 to 44 mm Hg), moderate (45 to 59 mm Hg), or severe (>60 mm Hg). Primary outcomes were 30-day mortality and long-term survival. There were no significant between-group differences in age or preoperative comorbidities. Mitral valve surgery included mitral valve replacement (78%) and repair (22%). The severe PH group had more mitral valve replacement (81%; P = .04), severe tricuspid valve regurgitation (31%; P = .003), right heart failure (17%; P = .02), and concomitant tricuspid valve procedures (46%; P < .001). For severe PH, 30-day mortality was 9%, with no significant group differences. Ten- and 12-year survival were significantly worse in the moderate-severe PH group (58% and 51%, respectively) compared with the normal PAP-mild PH group (83% and 79%, respectively) with a hazard ratio of 2.98 (95% confidence interval, 1.55-5.75; P = .001). Ten-year survival after mitral valve surgery for mitral stenosis was inversely associated with preoperative PAP. Mitral valve surgery can be performed with acceptable 30-day mortality for patients with mitral stenosis and moderate to severe PH, but long-term survival is impaired by moderate to severe PH. Patients with mitral stenosis and mild PH (systolic PAP 35-44 mm Hg) should be considered for mitral valve surgery. Copyright © 2016 The American Association for Thoracic Surgery. Published by Elsevier Inc. All rights reserved.

  6. Pulmonary hypertensive vasculopathy in parenchymal lung diseases and/or hypoxia: Number 1 in the Series "Pathology for the clinician" Edited by Peter Dorfmüller and Alberto Cavazza.

    PubMed

    Ghigna, Maria Rosa; Mooi, Wolter J; Grünberg, Katrien

    2017-06-30

    Pulmonary hypertension (PH) with complicating chronic lung diseases and/or hypoxia falls into group 3 of the updated classification of PH. Patients with chronic obstructive lung disease (COPD), diffuse lung disease (such as idiopathic pulmonary fibrosis (IPF)) and with sleep disordered breathing are particularly exposed to the risk of developing PH. Although PH in such a context is usually mild, a minority of patients exhibit severe haemodynamic impairment, defined by a mean pulmonary arterial pressure (mPAP) of ≥35 mmHg or mPAP values ranging between 25 mmHg and 35 mmHg with a low cardiac index (<2 L·min -1 ·m -2 ). The overlap between lung parenchymal disease and PH heavily affects life expectancy in such a patient population and complicates their therapeutic management. In this review we illustrate the pathological features and the underlying pathophysiological mechanisms of pulmonary circulation in chronic lung diseases, with an emphasis on COPD, IPF and obstructive sleep apnoea syndrome. Copyright ©ERS 2017.

  7. Human SLC4A11 Is a Novel NH3/H+ Co-transporter*

    PubMed Central

    Zhang, Wenlin; Ogando, Diego G.; Bonanno, Joseph A.; Obukhov, Alexander G.

    2015-01-01

    SLC4A11 has been proposed to be an electrogenic membrane transporter, permeable to Na+, H+ (OH−), bicarbonate, borate, and NH4+. Recent studies indicate, however, that neither bicarbonate or borate is a substrate. Here, we examined potential NH4+, Na+, and H+ contributions to electrogenic ion transport through SLC4A11 stably expressed in Na+/H+ exchanger-deficient PS120 fibroblasts. Inward currents observed during exposure to NH4Cl were determined by the [NH3]o, not [NH4+]o, and current amplitudes varied with the [H+] gradient. These currents were relatively unaffected by removal of Na+, K+, or Cl− from the bath but could be reduced by inclusion of NH4Cl in the pipette solution. Bath pH changes alone did not generate significant currents through SLC4A11, except immediately following exposure to NH4Cl. Reversal potential shifts in response to changing [NH3]o and pHo suggested an NH3/H+-coupled transport mode for SLC4A11. Proton flux through SLC4A11 in the absence of ammonia was relatively small, suggesting that ammonia transport is of more physiological relevance. Methylammonia produced currents similar to NH3 but with reduced amplitude. Estimated stoichiometry of SLC4A11 transport was 1:2 (NH3/H+). NH3-dependent currents were insensitive to 10 μm ethyl-isopropyl amiloride or 100 μm 4,4′- diisothiocyanatostilbene-2,2′-disulfonic acid. We propose that SLC4A11 is an NH3/2H+ co-transporter exhibiting unique characteristics. PMID:26018076

  8. Prevalence of Pulmonary Hypertension and its Influence on Survival in Patients With Advanced Chronic Obstructive Pulmonary Disease Prior to Lung Transplantation.

    PubMed

    Hayes, Don; Black, Sylvester M; Tobias, Joseph D; Mansour, Heidi M; Whitson, Bryan A

    2016-01-01

    Prevalence of pulmonary hypertension (PH) and its influence on survival in chronic obstructive pulmonary disease (COPD) are not well studied in the lung allocation score (LAS) era. The UNOS database was queried from 2005 to 2013 to identify first-time adult lung transplant candidates with COPD who were tracked from wait list entry date until death or censoring to determine both prevalence and influence of PH. Using right heart catheterization measurements, mild PH was defined as mean pulmonary artery pressure (mPAP) ≥ 25 mmHg and severe ≥ 35 mmHg. Of 1315 COPD candidates not transplanted, 1243 were used for survival analysis using Cox proportional hazards models, and 1010 (mild PH) and 244 (severe PH) were used for propensity score matching, respectively. A total of 52% (652) of subjects had PH mPAP ≥ 25 mmHg. Univariate analysis revealed significant differences in survival for mild PH (HR = 1.769; 95% CI: 1.331, 2.351; p < 0.001) and severe PH (HR = 3.271; 95% CI: 2.311, 4.630; p < 0.001). Kaplan-Meier survival function demonstrated significant disparities for mild PH (Log-rank test: Chi-square1: 15.87, p < 0.0001) and severe PH (Log-rank test: Chi-square1: 50.13, p < 0.0001). Multivariate Cox models identified significant risk for death for mild PH (HR = 1.987; 95% CI: 1.484, 2.662; p < 0.001) and severe PH (HR = 3.432; 95% CI: 2.410, 4.888; p < 0.001). Propensity score matching confirmed increased mortality hazard associated with mild PH (HR = 2.280; 95% CI: 1.425, 3.649; p = 0.001) and severe PH (HR = 7.000; 95% CI: 2.455, 19.957; p < 0.001). PH is highly prevalent in advanced COPD and associated with a significantly higher risk for mortality.

  9. Solid-phase extraction-fluorimetric high performance liquid chromatographic determination of domoic acid in natural seawater mediated by an amorphous titania sorbent.

    PubMed

    Chan, Ivy O M; Tsang, Vic W H; Chu, K K; Leung, S K; Lam, Michael H W; Lau, T C; Lam, Paul K S; Wu, Rudolf S S

    2007-01-30

    The feasibility of using sol-gel amorphous titania (TiO2) as a solid-phase sorbent for the pre-concentration of domoic acid (DA), a potent amnesic shellfish poisoning (ASP) toxin, directly from seawater was explored. The sol-gel titania material is able to adsorb DA from seawater, via the formation of ester-linkage between the carboxylic moieties of DA and the Ti-OH groups on the sorbent surface, at low pH and desorb it at high pH. The chemisorption process is not significantly interfered by the seawater matrix. The optimum pH values for the adsorption and desorption of DA were found to be pH 4 and 11, respectively. The optimal sorbent loading for the batch-type solid-phase extraction of DA was 0.67 mg-TiO2 ng-DA(-1) and adsorption equilibrium was achieved in 2 h at room temperature. The desorbed DA in 500 microL of 0.1 M alkaline borate buffer can be directly derviatized by 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) in aqueous media for fluorimetric HPLC quantification. Analyte recovery, repeatability and detection limit of this titania SPE-fluorimetric HPLC determination are 89%, 6.2% and 120 pg-DA mL(-1) (n=7, P<0.05), respectively, for a sample volume of 30 mL. This titania SPE technique should also be applicable to the pre-concentration of other polar carboxylate- and phosphonate-containing biomolecules and pharmaceuticals in complex and interfering environmental sample matrices.

  10. Boron removal by electrocoagulation and recovery.

    PubMed

    Isa, Mohamed Hasnain; Ezechi, Ezerie Henry; Ahmed, Zubair; Magram, Saleh Faraj; Kutty, Shamsul Rahman Mohamed

    2014-03-15

    This work investigated the removal of boron from wastewater and its recovery by electrocoagulation and hydrothermal mineralization methods respectively. The experimental design was developed using Box-Behnken Model. An initial study was performed based on four preselected variables (pH, current density, concentration and time) using synthetic wastewater. Response surface methodology (RSM) was used to evaluate the effect of process variables and their interaction on boron removal. The optimum conditions were obtained as pH 6.3, current density 17.4 mA/cm(2), and time 89 min. At these applied optimum conditions, 99.7% boron removal from an initial concentration of 10.4 mg/L was achieved. The process was effectively optimized by RSM with a desirability value of 1.0. The results showed that boron removal efficiency enhanced with increase in current density and treatment time. Removal efficiency also increased when pH was increased from 4 to 7 and subsequently decreased at pH 10. Adsorption kinetics study revealed that the reaction followed pseudo second order kinetic model; evidenced by high correlation and goodness of fit. Thermodynamics study showed that mechanism of boron adsorption was chemisorption and the reaction was endothermic in nature. Furthermore, the adsorption process was spontaneous as indicated by negative values of the adsorption free energy. Treatment of real produced water using electrocoagulation resulted in 98% boron removal. The hydrothermal mineralization study showed that borate minerals (Inyoite, Takadaite and Nifontovite) can be recovered as recyclable precipitate from electrocoagulation flocs of produced water. Copyright © 2013 Elsevier Ltd. All rights reserved.

  11. Spectroscopic properties of some borate glasses containg uranium

    NASA Astrophysics Data System (ADS)

    Culea, E.; Milea, I.; Bratu, I.

    1993-03-01

    Spectroscopic properties of some borate glasses containing 1-5%UO 3 have been studied in the fields of 700-1200 cm -1 and 10,000-30,000 cm -1 Absorption bands specific for U 6+ and U 4+ ions were observed. The increase of the melting time produces the reduction of U 6+ ions to U 4+.

  12. CADMIUM-RARE EARTH BORATE GLASS AS REACTOR CONTROL MATERIAL

    DOEpatents

    Ploetz, G.L.; Ray, W.E.

    1958-11-01

    A reactor control rod fabricated from a cadmiumrare earth-borate glass is presented. The rare earth component of this glass is selected from among those rare earths having large neutron capture cross sections, such as samarium, gadolinium or europium. Partlcles of this glass are then dispersed in a metal matrix by standard powder metallurgy techniques.

  13. N-Alkyl-N-methylpyrrolidinium Difluoro(oxalato)borate Ionic Liquids: Physical/Electrochemical Properties and Al Corrosion

    DTIC Science & Technology

    2013-01-01

    U.S. Army Research Laboratory, Adelphi, MD 20783, USA The synthesis and physical properties of difluoro(oxalato) borate (DFOB-)-based ionic...have a melting point (Tm) of -5°C and 31°C, respectively, whereas the PY15DFOB salt does not crystallize. Instead, this salt has a glass transition

  14. Infrared-to-visible conversion luminescence of Er 3+ ions in lead borate transparent glass-ceramics

    NASA Astrophysics Data System (ADS)

    Pisarski, Wojciech A.; Pisarska, Joanna; Lisiecki, Radosław; Grobelny, Łukasz; Dominiak-Dzik, Grażyna; Ryba-Romanowski, Witold

    2009-10-01

    Transparent glass-ceramics were successfully prepared during controlled heat treatment of lead borate glasses. The PbF 2 particles were dispersed into a borate glass matrix which was evidenced by X-ray diffraction analysis. The phase identification revealed that crystalline peaks can be related to the orthorhombic PbF 2 phase. Green up-conversion luminescence due to the 4S 3/2- 4I 15/2 transition of Er 3+ ions was registered. In comparison to the precursor glass the luminescence intensity was considerably higher, whereas the luminescence linewidth slightly decreased in the studied oxyfluoride transparent glass-ceramics. It indicated that a part of the trivalent erbium was incorporated into the PbF 2 crystalline phase.

  15. Framework influence of erbium doped oxyfluoride glasses on their optical properties

    NASA Astrophysics Data System (ADS)

    Środa, Marcin; Cholewa-Kowalska, Katarzyna; Różański, Marek; Nocuń, Marek

    2011-01-01

    Glasses of different matrix (phosphate, borate, silicate and lead-silicate) were studied for their optical properties. The effect of Er dopant on transmittance and luminescence properties was presented. The significant “red shift” and “blue shift” of UV edge absorption were discussed based on the changes in the framework of the borate and phosphate glasses, respectively. It was showed that the integral intensity of the two main optical absorption transitions monotonically increases with the order: phosphate < borate < silicate < lead-silicate. Ellipsometric measurement was applied to obtain the refractive index of the glasses. The correlation between the shift of edge absorption and the change of refractive index was presented. Effect of glassy matrix on luminescence of Er3+ was discussed.

  16. Acoustic diagnosis of pulmonary hypertension: automated speech- recognition-inspired classification algorithm outperforms physicians

    NASA Astrophysics Data System (ADS)

    Kaddoura, Tarek; Vadlamudi, Karunakar; Kumar, Shine; Bobhate, Prashant; Guo, Long; Jain, Shreepal; Elgendi, Mohamed; Coe, James Y.; Kim, Daniel; Taylor, Dylan; Tymchak, Wayne; Schuurmans, Dale; Zemp, Roger J.; Adatia, Ian

    2016-09-01

    We hypothesized that an automated speech- recognition-inspired classification algorithm could differentiate between the heart sounds in subjects with and without pulmonary hypertension (PH) and outperform physicians. Heart sounds, electrocardiograms, and mean pulmonary artery pressures (mPAp) were recorded simultaneously. Heart sound recordings were digitized to train and test speech-recognition-inspired classification algorithms. We used mel-frequency cepstral coefficients to extract features from the heart sounds. Gaussian-mixture models classified the features as PH (mPAp ≥ 25 mmHg) or normal (mPAp < 25 mmHg). Physicians blinded to patient data listened to the same heart sound recordings and attempted a diagnosis. We studied 164 subjects: 86 with mPAp ≥ 25 mmHg (mPAp 41 ± 12 mmHg) and 78 with mPAp < 25 mmHg (mPAp 17 ± 5 mmHg) (p  < 0.005). The correct diagnostic rate of the automated speech-recognition-inspired algorithm was 74% compared to 56% by physicians (p = 0.005). The false positive rate for the algorithm was 34% versus 50% (p = 0.04) for clinicians. The false negative rate for the algorithm was 23% and 68% (p = 0.0002) for physicians. We developed an automated speech-recognition-inspired classification algorithm for the acoustic diagnosis of PH that outperforms physicians that could be used to screen for PH and encourage earlier specialist referral.

  17. Performance of an alkalophilic and halotolerant laccase from gamma-proteobacterium JB in the presence of industrial pollutants.

    PubMed

    Singh, Gursharan; Sharma, Prince; Capalash, Neena

    2009-08-01

    An alkalophilic and halotolerant laccase from gamma-proteobacterium JB catalyzed in high concentrations of organic solvents and various salts. The enzyme retained 80-100% activity in 10% concentration of dimethylsulfoxide (DMSO), ethanol, acetone or methanol; 100, 85 and 50% activity in 20 mM MgCl(2), 5.0 mM MnCl(2) and 0.1 mM CuCl(2); 140, 120 and 110% activity in 5.0 mM MnSO(4), 10 mM MgSO(4) and 1mM CaSO(4), respectively. Sodium halides inhibited the enzyme in the order: F(-)> Br(-)> I(-)> Cl(-). In 0.5 M NaCl, pH 6.0, laccase was approximately 60% active. Decolorization of indigo carmine by laccase at pH 9.0 was not inhibited even in the presence of 0.5 M NaCl. Release of chromophoric, reducing and hydrophobic compounds during biobleaching of straw rich-soda pulp by laccase was not inhibited when the enzyme was applied in the presence of 1 M NaCl at pH 8.0. Laccase retained 50% residual activity even when incubated with 5% calcium hypochlorite for 30 min.

  18. Low pH affects survival, growth, size distribution, and carapace quality of the postlarvae and early juveniles of the freshwater prawn Macrobrachium rosenbergii de Man

    NASA Astrophysics Data System (ADS)

    Kawamura, Gunzo; Bagarinao, Teodora; Yong, Annita Seok Kian; Chen, Chiau Yu; Noor, Siti Norasidah Mat; Lim, Leong Seng

    2015-06-01

    Acidification of rain water caused by air pollutants is now recognized as a serious threat to aquatic ecosystems. We examined the effects of low pH (control pH 7.5, pH 6, pH 5, pH 4) on the survival, growth, and shell quality of Macrobrachium rosenbergii postlarvae and early juveniles in the laboratory. Hatcheryproduced postlarvae (PL 5) were stocked at 250 PL per aquarium, acclimated over 7 d to experimental pH adjusted with hydrochloric acid, and reared for 30 d. Dead specimens were removed and counted twice a day. After 27 d rearing, all specimens were measured for total length and body weight. Carapace quality was assessed by spectrophotometry. Survival of juveniles was highest at pH 6 (binomial 95% confidence interval 79 - 89%) followed by control pH 7.5 (56 - 68%) and pH 5 (50 - 60%) and was lowest for unmetamorphosed postlarvae and juveniles at pH 4 (43 - 49%). The final median total length and body weight of juveniles were similar at control pH 7.5 (18.2 TL, 50.2 mg BW) and pH 6 (17.7 mm TL, 45.0 mg BW) but significantly less at pH 5 (16.7 mm TL, 38.2 mg BW); at pH 4, the postlarvae did not metamorphose and measured only 9.8 mm TL, 29.3 mg BW. Length frequency distribution showed homogeneous growth at pH 6, positive skew at control pH 7.5 and pH 5, and extreme heterogeneity at pH 4. The carapace showed different transmittance spectra and lower total transmittance (i.e. thicker carapace) in juveniles at pH 7.5, pH 6, and pH 5 than in unmetamorphosed postlarvae and juveniles with thinner carapace at pH 4. Thus, survival, growth, size distribution, and carapace quality of M. rosenbergii postlarvae and early juveniles were negatively affected by pH 5 and especially pH 4. The thinner carapace of the survivors at pH 4 was mostly due to their small size and failure to metamorphose. Natural waters affected by acid rain could decimate M. rosenbergii populations in the wild.

  19. Core-shell CoFe2O4@Co-Fe-Bi nanoarray: a surface-amorphization water oxidation catalyst operating at near-neutral pH.

    PubMed

    Ji, Xuqiang; Hao, Shuai; Qu, Fengli; Liu, Jingquan; Du, Gu; Asiri, Abdullah M; Chen, Liang; Sun, Xuping

    2017-06-14

    The exploration of high-performance and earth-abundant water oxidation catalysts operating under mild conditions is highly attractive and challenging. In this communication, core-shell CoFe 2 O 4 @Co-Fe-Bi nanoarray on carbon cloth (CoFe 2 O 4 @Co-Fe-Bi/CC) was successfully fabricated by in situ surface amorphization of CoFe 2 O 4 nanoarray on CC (CoFe 2 O 4 /CC). As a 3D water oxidation electrode, CoFe 2 O 4 @Co-Fe-Bi/CC shows outstanding activity with an overpotential of 460 mV to drive a geometrical catalytic current density of 10 mA cm -2 in 0.1 M potassium borate (pH 9.2). Notably, it also demonstrates superior long-term durability for at least 20 h with 96% Faradic efficiency. Density functional theory calculations indicate that the conversion from OOH* to O 2 is the rate-limiting step and the high water oxidation activity of CoFe 2 O 4 @Co-Fe-Bi/CC is associated with the lower free energy of 1.84 eV on a Co-Fe-Bi shell.

  20. Association of three putative periodontal pathogens with chronic periodontitis in Brazilian subjects

    PubMed Central

    GONÇALVES, Cristiane; SOARES, Geisla Mary S.; FAVERI, Marcelo; PÉREZ-CHAPARRO, Paula Juliana; LOBÃO, Eduardo; FIGUEIREDO, Luciene Cristina; BACCELLI, Gustavo Titonele; FERES, Magda

    2016-01-01

    ABSTRACT Objective The aim of this study was to evaluate the association of Porphyromonas endodontalis, Filifactor alocis and Dialister pneumosintes with the occurrence of periodontitis. Material and Methods Thirty subjects with chronic periodontitis (ChP) and 10 with periodontal health (PH) were included in the study. Nine subgingival biofilm samples were collected as follows: i) PH group - from the mesial/buccal aspect of each tooth in two randomly chosen contralateral quadrants; ii) ChP group - from three sites in each of the following probing depth (PD) categories: shallow (≤3 mm), moderate (4-6 mm) and deep (≥7 mm). Checkerboard DNA-DNA hybridization was used to analyze the samples. Results We found the three species evaluated in a higher percentage of sites and at higher levels in the group with ChP than in the PH group (p<0.05, Mann-Whitney test). We also observed these differences when the samples from sites with PD≤4 mm or ≥5 mm of subjects with ChP were compared with those from subjects with PH (p<0.05, Mann-Whitney test). In addition, the prevalence and levels of D. pneumosintes, and especially of F. alocis were very low in healthy subjects (0.12x105 and 0.01x105, respectively). Conclusion F. alocis and D. pneumosintes might be associated with the etiology of ChP, and their role in the onset and progression of this infection should be further investigated. The role of P. endodontalis was less evident, since this species was found in relatively high levels and prevalence in the PH group. PMID:27119767

  1. Association of three putative periodontal pathogens with chronic periodontitis in Brazilian subjects.

    PubMed

    Gonçalves, Cristiane; Soares, Geisla Mary S; Faveri, Marcelo; Pérez-Chaparro, Paula Juliana; Lobão, Eduardo; Figueiredo, Luciene Cristina; Baccelli, Gustavo Titonele; Feres, Magda

    2016-04-01

    Objective The aim of this study was to evaluate the association of Porphyromonas endodontalis, Filifactor alocis and Dialister pneumosintes with the occurrence of periodontitis. Material and Methods Thirty subjects with chronic periodontitis (ChP) and 10 with periodontal health (PH) were included in the study. Nine subgingival biofilm samples were collected as follows: i) PH group - from the mesial/buccal aspect of each tooth in two randomly chosen contralateral quadrants; ii) ChP group - from three sites in each of the following probing depth (PD) categories: shallow (≤3 mm), moderate (4-6 mm) and deep (≥7 mm). Checkerboard DNA-DNA hybridization was used to analyze the samples. Results We found the three species evaluated in a higher percentage of sites and at higher levels in the group with ChP than in the PH group (p<0.05, Mann-Whitney test). We also observed these differences when the samples from sites with PD≤4 mm or ≥5 mm of subjects with ChP were compared with those from subjects with PH (p<0.05, Mann-Whitney test). In addition, the prevalence and levels of D. pneumosintes, and especially of F. alocis were very low in healthy subjects (0.12x105 and 0.01x105, respectively). Conclusion F. alocis and D. pneumosintes might be associated with the etiology of ChP, and their role in the onset and progression of this infection should be further investigated. The role of P. endodontalis was less evident, since this species was found in relatively high levels and prevalence in the PH group.

  2. Buffer capacity of biologics--from buffer salts to buffering by antibodies.

    PubMed

    Karow, Anne R; Bahrenburg, Sven; Garidel, Patrick

    2013-01-01

    Controlling pH is essential for a variety of biopharmaceutical process steps. The chemical stability of biologics such as monoclonal antibodies is pH-dependent and slightly acidic conditions are favorable for stability in a number of cases. Since control of pH is widely provided by added buffer salts, the current study summarizes the buffer characteristics of acetate, citrate, histidine, succinate, and phosphate buffers. Experimentally derived values largely coincide with values calculated from a model that had been proposed in 1922 by van Slyke. As high concentrated protein formulations become more and more prevalent for biologics, the self-buffering potential of proteins becomes of relevance. The current study provides information on buffer characteristics for pH ranges down to 4.0 and up to 8.0 and shows that a monoclonal antibody at 50 mg/mL exhibits similar buffer capacity as 6 mM citrate or 14 mM histidine (pH 5.0-6.0). Buffer capacity of antibody solutions scales linearly with protein concentration up to more than 200 mg/mL. At a protein concentration of 220 mg/mL, the buffer capacity resembles the buffer capacity of 30 mM citrate or 50 mM histidine (pH 5.0-6.0). The buffer capacity of monoclonal antibodies is practically identical at the process relevant temperatures 5, 25, and 40°C. Changes in ionic strength of ΔI=0.15, in contrast, can alter the buffer capacity up to 35%. In conclusion, due to efficient self-buffering by antibodies in the pH range of favored chemical stability, conventional buffer excipients could be dispensable for pH stabilization of high concentrated protein solutions. Copyright © 2013 American Institute of Chemical Engineers.

  3. Minimally invasive wireless motility capsule to study canine gastrointestinal motility and pH.

    PubMed

    Warrit, K; Boscan, P; Ferguson, L E; Bradley, A M; Dowers, K L; Rao, S; Twedt, D C

    2017-09-01

    The aim of this study was to describe the feasibility of using a gastrointestinal tract wireless motility capsule (WMC) that measured intraluminal pressure, pH and transit time through the gastrointestinal tract, in dogs in their home environment. Forty-four adult healthy dogs, eating a standard diet, were prospectively enrolled. The WMC was well tolerated by all dogs and provided data from the different sections of the gastrointestinal tract. Median gastric emptying time was 20h (range, 6.3-119h), demonstrating a large range. The gastric pressure pattern and pH depended on the phase of food consumption. The small bowel transit time was 3.1h (range, 1.6-5.4h) with average contraction pressures of 6.5mmHg (range, 1.1-21.4mmHg) and pH 7.8 (range, 7-8.9). The large bowel transit time was 21h (range, 1-69h) with average contractions pressures of 0.9mmHg (range, 0.3-2.7mmHg) and pH 6.4 (range, 5.3-8.2). There was considerable individual variation in motility patterns and transit times between dogs. No difference was observed between the sexes. No relationships between any transit time, bowel pH or pressure pattern and bodyweights were identified. The WMC likely represents movement of a large non-digestible particle rather than normal ingesta. Due to its large size, the WMC should not be use in smaller dogs. The WMC is a promising minimally invasive tool to assess GIT solid phase transit times, pressures and pH. However, further studies are necessary due to the current limitations observed. Published by Elsevier Ltd.

  4. A new amperometric enzyme electrode for alcohol determination.

    PubMed

    Gülce, H; Gülce, A; Kavanoz, M; Coşkun, H; Yildiz, A

    2002-06-01

    A new enzyme electrode for the determination of alcohols was developed by immobilizing alcohol oxidase in polvinylferrocenium matrix coated on a Pt electrode surface. The amperometric response due to the electrooxidation of enzymatically generated H(2)O(2) was measured at a constant potential of +0.70 V versus SCE. The effects of substrate, buffer and enzyme concentrations, pH and temperature on the response of the electrode were investigated. The optimum pH was found to be pH 8.0 at 30 degrees C. The steady-state current of this enzyme electrode was reproducible within +/-5.0% of the relative error. The sensitivity of the enzyme electrode decreased in the following order: methanol>ethanol>n-butanol>benzyl alcohol. The linear response was observed up to 3.7 mM for methanol, 3.0 mM for ethanol, 6.2 mM for n-butanol, and 5.2 mM for benzyl alcohol. The apparent Michaelis-Menten constant (K(Mapp)) value and the activation energy, E(a), of this immobilized enzyme system were found to be 5.78 mM and 38.07 kJ/mol for methanol, respectively.

  5. Determination of the R(-) and S(+)-enantiomers of vigabatrin in human plasma by ultra-high-performance liquid chromatography and tandem mass-spectrometry.

    PubMed

    Duhamel, Paul; Ounissi, Marwa; Le Saux, Thomas; Bienayme, Hugues; Chiron, Catherine; Jullien, Vincent

    2017-12-01

    An analytical method was developed for the quantification in plasma of the R and S enantiomers of vigabatrin (VGB), a drug used for the treatment of some refractory pediatric epileptic syndromes. After adding 50μL of the internal standard, which consisted of a 15mg/L solution of deuterated racemic VGB, and 100μL of water to 100μL of plasma samples, a protein precipitation was performed by adding 600μL of methanol. The supernatant was evaporated to dryness under a stream of nitrogen and the dry residue was reconstituted with 500μL of water. Then, 100μL of 0.01M o-phthaldialdehyde and 0.01M N-acetyl-l-cysteine in borate buffer (0.1M, pH=9.5) were added for pre-column derivatization of the enantiomers as diastereomeric isoindoles. One microliter of the resulting mixture was injected in the chromatographic system. The chromatographic separation was performed in gradient elution mode at a flow rate of 400μL/min using a phenomenex EVO C-18 column with a mobile phase composed of 5mM ammonium acetate and a methanol:acetonitrile (63:37v/v) mixture. Detection was performed by mass spectrometry in selected reaction monitoring mode using heated electrospray ionization in positive mode as the ion source. Intra- and inter-day precision and accuracy were lower than 15% over the calibration range (0.2-50mg/L for each enantiomer) and the method was successfully used to assess plasma concentrations of VGB in epileptic children. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Characterization of a novel particle into liquid sampler for analysis of single fluorescent aerosol particles through capillary electrophoresis.

    PubMed

    Tang, Hao; Hiemstra, Scott; Thompson, Jonathan E

    2011-09-19

    An approach to sample and analyze single aerosolized droplets (<10 nL) of solutions containing fluorescein isothiocyanate (FITC) labeled glycine (GLY) and glutamic acid (GLU) is demonstrated. The sampling approach is based on inertial impaction in which the sample particle is accelerated through a nozzle and directly into a small drop of buffered solution (20 mM borate, pH=10) suspended at the end of a coaxial tube of stainless steel and a fused silica capillary. A spherical light scattering cell and laser (λ=532 nm) is used to detect the arrival of particles at the buffered droplet. Upon dissolution and/or mixing, a portion of the sample is injected onto the fused silica capillary for subsequent chemical analysis by capillary electrophoresis (CE) and detection by laser-induced fluorescence (LIF). It was found that the inertial impaction approach sampled particles >1 μm diameter with an efficiency of 80% or greater. At 15 kV applied potential, the FITC conjugates of GLY and GLU could be resolved in less than 120 s allowing qualitative analysis of the contents of single dispersed particles. However, the extent to which the sample is diluted into the buffer droplet varied significantly on a per-particle basis that caused >80% R.S.D. in fluorescence peak heights. This aspect of the method would necessitate the use of internal standards for quantitative analysis of materials present within the particles. It is envisaged that further improvements to the device described may ultimately lead to analysis of the contents of single particles dispersed in earth's atmosphere. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Structural and Biochemical Studies of the Ovarian Tumor Domain

    DTIC Science & Technology

    2007-05-01

    solution containing Bis-Tris pH 5.5-6.5, 16-20% PEG 3350 , and 100-200 mM of a magnesium cation. These crystals belong to spacegroup P64 with unit...drop method using a reservoir solution containing Bis-Tris pH 5.5-6.5, 16-20% PEG 3350 , and 50-200 mM ammonium acetate . Orthorhombic crystals

  8. Cerebral interstitial tissue oxygen tension, pH, HCO3, CO2.

    PubMed

    Charbel, F T; Hoffman, W E; Misra, M; Hannigan, K; Ausman, J I

    1997-10-01

    There are many techniques for monitoring the injured brain following trauma, subarachnoid hemorrhage, or surgery. It is thought that the major determinants for recovery of injured cerebral tissue are oxygen, glucose delivery, and the clearance of metabolites. These factors, at optimal levels, are probably responsible for the regaining of neuronal functions. These parameters are in turn dependent on the tissue's blood flow and metabolism. We have been using a single, compact, polyethylene sensor, the Paratrend 7 for the measurement of cerebral oxygen tension, CO2, pH, and temperature. This sensor is designed for continuous blood gas analysis to aid in monitoring neurosurgical patients, both during surgery and in the intensive care unit. Using the Paratrend 7 sensor, we found the normal range of values to be: PO2 33 +/- 11 mm Hg; PCO2 48 +/- 7 mm Hg; pH 7.19 +/- 0.11. Critical measurements are considered to be tissue PO2 < 10 mm Hg; PCO2 > 60 mm Hg, and pH < 6.8. We have had no complications with this device; the risks are similar to those of placing a parenchymal intracranial pressure monitor. We believe that assessment of interstitial cerebral oxygen saturation can be of great value both intraoperatively and postoperatively. In our experience, the Paratrend 7 system is an effective method of measuring tissue cerebral oxygen tension, along with carbon dioxide levels, pH, and temperature.

  9. Group 2 Pulmonary Hypertension: Pulmonary Venous Hypertension: Epidemiology and Pathophysiology.

    PubMed

    Clark, Craig B; Horn, Evelyn M

    2016-08-01

    Pulmonary hypertension from left heart disease (PH-LHD) is the most common form of PH, defined as mean pulmonary artery pressure ≥25 mm Hg and pulmonary artery wedge pressure ≥15 mm Hg. PH-LHD development is associated with more severe left-sided disease and its presence portends a poor prognosis, particularly once right ventricular failure develops. Treatment remains focused on the underlying LHD and despite initial enthusiasm for PH-specific therapies, most studies have been disappointing and their routine clinical use cannot be recommended. More work is urgently needed to better understand the pathophysiology underlying this disease and to develop effective therapeutic strategies. Copyright © 2016 Elsevier Inc. All rights reserved.

  10. Structure-Function Relationship of Hydrophiidae Postsynaptic Neurotoxins

    DTIC Science & Technology

    1990-09-18

    24 hr. Buffer F consisted of 10 mM sodium phosphate, pH 7.5. containing 0.02% (w/v) lauryl sulfate (SDS), and 0.04% (w/v) sodium cholate. The...subjected to gel filtration on Sephadex G-50-50 using 10 mM sodium phosphate buffer (pH 6.5) containing 0.1 M NaCl. Samples were dissolved in 3.5 ml buffer...sequencing. Isolation of Cobrotoxin. The venom from NaJa naia atra was subjected to Sephadex G50-50 gel filtration pre-equilibrated with 10 mM sodium

  11. Safety of regadenoson stress testing in patients with pulmonary hypertension.

    PubMed

    Moles, Victor M; Cascino, Thomas; Saleh, Ashraf; Mikhova, Krasimira; Lazarus, John J; Ghannam, Michael; Yun, Hong J; Konerman, Matthew; Weinberg, Richard L; Ficaro, Edward P; Corbett, James R; McLaughlin, Vallerie V; Murthy, Venkatesh L

    2018-06-01

    We sought to determine the safety of regadenoson stress testing in patients with PH. PH is increasingly recognized at more advanced ages. As many as one-third of patients with PH have coronary artery disease. Because of their physical limitations, patients with PH are unable to adequately exercise. Regadenoson can potentially have an adverse impact due to their tenuous hemodynamics. Current guidelines suggest performing a coronary angiography in patients with PH who have angina or multiple coronary risk factors. We identified 67 consecutive patients with confirmed PH by catheterization (mean PA > 25 mmHg not due to left heart disease) who underwent MPI with regadenoson stress. Medical records were reviewed to determine hemodynamic and ECG response to regadenoson. No serious events occurred. Common side effects related to regadenoson were observed, dyspnea being the most common (70.6%). No syncope occurred. Heart rate increased from 74.6 ± 14 to 96.3 ± 18.3 bpm, systolic blood pressure increased from 129.8 ± 20.9 to 131.8 ± 31 mmHg, and diastolic blood pressure decreased from 77.1 ± 11.4 to 72.9 ± 15.3 mmHg. There was no ventricular tachycardia, ventricular fibrillation, or second- or third-degree atrioventricular block. Regadenoson stress MPI appears to be well tolerated and safe in patients with PH.

  12. Hemodynamic profile of pulmonary hypertension (PH) in ARDS

    PubMed Central

    Calcaianu, Mihaela; Gschwend, Anthony; Canuet, Matthieu; Meziani, Ferhat; Kessler, Romain

    2017-01-01

    Acute respiratory distress syndrome (ARDS) is a diffuse lung injury that leads to a severe acute respiratory failure. Traditional diagnostic criteria for pulmonary hypertension (PH), in this situation, may be unreliable due to the effects of positive pressure ventilation and vasoactive agents. The aim of this study is to describe the hemodynamic characteristics of PH secondary to ARDS, in relation with respiratory parameters. We assessed the hemodynamic, respiratory function, and ventilator parameters in a cohort of 38 individuals with ARDS-associated PH defined by mean pulmonary arterial pressure (mPAP) ≥ 25 mmHg. Individual characteristics: PaO2/FiO2 = 110 ± 60 mmHg, alveolar-arterial oxygen gradient (A-aO2) = 549 ± 148.9 mmHg, positive end-expiratory pressure (PEEP) = 8.7 ± 3.5 cmH2O, pulmonary static compliance (Cstat) = 30 ± 12.1 L*cmH2O-1, mPAP = 35.4 ±6.6 mmHg, pulmonary artery wedge pressure (PAWP) = 15.6 ± 5.5 mmHg, cardiac index (CI) = 3.4 ± 1.2 L/min/m2, pulmonary vascular resistance (PVR) = 3.3 ± 1.6 Wood units (WU), right atrial pressure (RAP) = 13.4 ± 5.4 mmHg, diastolic pulmonary gradient (DPG) = 12.6 ± 6.5 mmHg, and trans-pulmonary gradient (TPG) = 19.7 ± 7.7 mmHg. The composite marker—DPG >7 mmHg and PVR > 3 WU—is associated with lower CI (P = 0.016), higher mPAP (P = 0.003), and lower pulmonary static compliance (P = 0.028). We confirmed a poor prognosis of ARDS associated with PH, with a 50% survival rate after 17 days. We observed that the survival rate at 28 days was better in the case of improvement in the PaO2/FiO2 ratio in the first 24 h (log rank P = 0.003). ARDS associated with PH is a severe condition with a very poor survival rate. The composite marker DPG > 7 mmHg and PVR > 3 WU seemed to better describe the hemodynamic and respiratory dysfunction. The improvement in PaO2/FiO2 ratio in the first 24 h defined a better survival in our cohort of patients. PMID:29283029

  13. Hemodynamic profile of pulmonary hypertension (PH) in ARDS.

    PubMed

    Calcaianu, George; Calcaianu, Mihaela; Gschwend, Anthony; Canuet, Matthieu; Meziani, Ferhat; Kessler, Romain

    2018-01-01

    Acute respiratory distress syndrome (ARDS) is a diffuse lung injury that leads to a severe acute respiratory failure. Traditional diagnostic criteria for pulmonary hypertension (PH), in this situation, may be unreliable due to the effects of positive pressure ventilation and vasoactive agents. The aim of this study is to describe the hemodynamic characteristics of PH secondary to ARDS, in relation with respiratory parameters. We assessed the hemodynamic, respiratory function, and ventilator parameters in a cohort of 38 individuals with ARDS-associated PH defined by mean pulmonary arterial pressure (mPAP) ≥ 25 mmHg. Individual characteristics: PaO2/FiO2 = 110 ± 60 mmHg, alveolar-arterial oxygen gradient (A-aO2) = 549 ± 148.9 mmHg, positive end-expiratory pressure (PEEP) = 8.7 ± 3.5 cmH 2 O, pulmonary static compliance (Cstat) = 30 ± 12.1 L*cmH 2 O-1, mPAP = 35.4 ±6.6 mmHg, pulmonary artery wedge pressure (PAWP) = 15.6 ± 5.5 mmHg, cardiac index (CI) = 3.4 ± 1.2 L/min/m 2 , pulmonary vascular resistance (PVR) = 3.3 ± 1.6 Wood units (WU), right atrial pressure (RAP) = 13.4 ± 5.4 mmHg, diastolic pulmonary gradient (DPG) = 12.6 ± 6.5 mmHg, and trans-pulmonary gradient (TPG) = 19.7 ± 7.7 mmHg. The composite marker-DPG >7 mmHg and PVR > 3 WU-is associated with lower CI ( P = 0.016), higher mPAP ( P = 0.003), and lower pulmonary static compliance ( P = 0.028). We confirmed a poor prognosis of ARDS associated with PH, with a 50% survival rate after 17 days. We observed that the survival rate at 28 days was better in the case of improvement in the PaO2/FiO2 ratio in the first 24 h (log rank P = 0.003). ARDS associated with PH is a severe condition with a very poor survival rate. The composite marker DPG > 7 mmHg and PVR > 3 WU seemed to better describe the hemodynamic and respiratory dysfunction. The improvement in PaO2/FiO2 ratio in the first 24 h defined a better survival in our cohort of patients.

  14. Dosimetric properties of dysprosium doped calcium magnesium borate glass subjected to Co-60 gamma ray

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

    Omar, R. S., E-mail: ratnasuffhiyanni@gmail.com; Wagiran, H., E-mail: husin@utm.my; Saeed, M. A.

    Thermoluminescence (TL) dosimetric properties of dysprosium doped calcium magnesium borate (CMB:Dy) glass are presented. This study is deemed to understand the application of calcium as the modifier in magnesium borate glass with the presence of dysprosium as the activator to be performed as TL dosimeter (TLD). The study provides fundamental knowledge of a glass system that may lead to perform new TL glass dosimetry application in future research. Calcium magnesium borate glass systems of (70-y) B{sub 2}O{sub 3} − 20 CaO – 10 MgO-(y) Dy{sub 2}O{sub 3} with 0.05  mol % ≤ y ≤ 0.7  mol % of dyprosium weremore » prepared by melt-quenching technique. The amorphous structure and TL properties of the prepared samples were determined using powder X-ray diffraction (XRD) and TL reader; model Harshaw 4500 respectively. The samples were irradiated to Co-60 gamma source at a dose of 50 Gy. Dosimetric properties such as annealing procedure, time temperature profile (TTP) setting, optimization of Dy{sub 2}O{sub 3} concentration of 0.5 mol % were determined for thermoluminescence dosimeter (TLD) reader used.« less

  15. Thermoluminescent properties of rare earth doped lithium strontium borate phosphors

    NASA Astrophysics Data System (ADS)

    Jakathamani, S.; Annalakshmi, O.; Jose, M. T.

    2018-04-01

    Thermoluminescence (TL) of borates is remarkable in the field of radiation dosimetry because they can detect both neutron and gamma radiations. Usually, the TL efficiency of pure borates is low and hence dopants have to be added to increase their TL output. Their sensitivity and thermal stability vary widely and depend strongly on the preparation method. In this study polycrystalline powders of different rare earth doped thermoluminescent phosphors of Lithium Strontium borate (LSB) were synthesized by solid state sintering technique. Among the different rare earth dopants, the phosphor doped with cerium was found to have a simple glow curve structure with a dosimetric peak at around 265°C for a heating rate of 5°C/s. In order to study the effect of dopant on the TL characteristics, LSB phosphor with different concentrations of Ce dopant was synthesized and the TL intensity was found to be maximum for a dopant concentration of 0.7 mol%. All other important dosimetric characteristics like dose response and fading were carried out for the LSB:Ce (0.7 mol%) phosphor. Kinetic parameters like trap depth and frequency factor were determined using Peak shape method from Chen's equation.

  16. Evaluation of borate bioactive glass scaffolds with different pore sizes in a rat subcutaneous implantation model.

    PubMed

    Deliormanli, Aylin M; Liu, Xin; Rahaman, Mohamed N

    2014-01-01

    Borate bioactive glass has been shown to convert faster and more completely to hydroxyapatite and enhance new bone formation in vivo when compared to silicate bioactive glass (such as 45S5 and 13-93 bioactive glass). In this work, the effects of the borate glass microstructure on its conversion to hydroxyapatite (HA) in vitro and its ability to support tissue ingrowth in a rat subcutaneous implantation model were investigated. Bioactive borate glass scaffolds, designated 13-93B3, with a grid-like microstructure and pore widths of 300, 600, and 900 µm were prepared by a robocasting technique. The scaffolds were implanted subcutaneously for 4 weeks in Sprague Dawley rats. Silicate 13-93 glass scaffolds with the same microstructure were used as the control. The conversion of the scaffolds to HA was studied as a function of immersion time in a simulated body fluid. Histology and scanning electron microscopy were used to evaluate conversion of the bioactive glass implants to hydroxyapatite, as well as tissue ingrowth and blood vessel formation in the implants. The pore size of the scaffolds was found to have little effect on tissue infiltration and angiogenesis after the 4-week implantation.

  17. Titanium addition influences antibacterial activity of bioactive glass coatings on metallic implants.

    PubMed

    Rodriguez, Omar; Stone, Wendy; Schemitsch, Emil H; Zalzal, Paul; Waldman, Stephen; Papini, Marcello; Towler, Mark R

    2017-10-01

    In an attempt to combat the possibility of bacterial infection and insufficient bone growth around metallic, surgical implants, bioactive glasses may be employed as coatings. In this work, silica-based and borate-based glass series were synthesized for this purpose and subsequently characterized in terms of antibacterial behavior, solubility and cytotoxicity. Borate-based glasses were found to exhibit significantly superior antibacterial properties and increased solubility compared to their silica-based counterparts, with BRT0 and BRT3 (borate-based glasses with 0 and 15 mol% of titanium dioxide incorporated, respectively) outperforming the remainder of the glasses, both borate and silicate based, in these respects. Atomic Absorption Spectroscopy confirmed the release of zinc ions (Zn 2+ ), which has been linked to the antibacterial abilities of glasses SRT0, BRT0 and BRT3, with inhibition effectively achieved at concentrations lower than 0.7 ppm. In vitro cytotoxicity studies using MC3T3-E1 osteoblasts confirmed that cell proliferation was affected by all glasses in this study, with decreased proliferation attributed to a faster release of sodium ions over calcium ions in both glass series, factor known to slow cell proliferation in vitro .

  18. Diagnostic accuracy of echocardiography combined with chest CT in pulmonary hypertension.

    PubMed

    Shujaat, Adil; Bajwa, Abubakr A; Al-Saffar, Farah; Bellardini, Jason; Jones, Lisa; Cury, James D

    2018-03-01

    Transthoracic echocardiography (TTE) and computerized axial tomography (CT) are complementary imaging techniques. It is possible that a combination of the two may offer a better way of identifying pulmonary hypertension (PH) than either one alone. To determine the diagnostic accuracy of TTE combined with chest CT in pulmonary hypertension. We performed a retrospective review of consecutive patients who had undergone TTE, CT and right heart catheterization (RHC) between 7/1/2008 and 6/30/2012. PH was defined as systolic pulmonary artery pressure >40 mm Hg or tricuspid regurgitant (TR) jet velocity >2.8m/s on TTE, ratio of diameter of pulmonary artery to ascending aorta (rPA) >1 or diameter of PA (dPA) >30 mm on CT, and mean PAP (mPAP) >25 mm Hg on RHC. There was a total of 87 patients. The mean ± SD age was 54.3 ± 15.9 years and 69 (79%) were female. The prevalence of PH was 75%. The mean ± SD mPAP was 35.8 ± 14.2 mm Hg. The majority of the patients belonged to World Health Organization group I PH. Fifty per cent of the CT scans were done with intravenous contrast dye. The combination of TR jet velocity and rPA provided the best combination of sensitivity (98%) and specificity (70%) with an ROC area under the curve of 0.84. The combination of TTE and chest CT is better than either imaging technique alone in identifying patients with PH in a heterogeneous population and may exclude PH. © 2017 John Wiley & Sons Ltd.

  19. Mechanism of basolateral membrane H+/OH-/HCO-3 transport in the rat proximal convoluted tubule. A sodium-coupled electrogenic process

    PubMed Central

    1985-01-01

    In order to examine the mechanism of basolateral membrane H+/OH-/HCO-3 transport, a method was developed for the measurement of cell pH in the vivo doubly microperfused rat proximal convoluted tubule. A pH- sensitive fluorescein derivative, (2',7')-bis(carboxyethyl)-(5,6)- carboxyfluorescein, was loaded into cells and relative changes in fluorescence at two excitation wavelengths were followed. Calibration was accomplished using nigericin with high extracellular potassium concentrations. When luminal and peritubular fluids were pH 7.32, cell pH was 7.14 +/- 0.01. Decreasing peritubular pH from 7.32 to 6.63 caused cell pH to decrease from 7.16 +/- 0.02 to 6.90 +/- 0.03. This effect occurred at an initial rate of 2.4 +/- 0.3 pH units/min, and was inhibited by 0.5 mM SITS. Lowering the peritubular sodium concentration from 147 to 25 meq/liter caused cell pH to decrease from 7.20 +/- 0.03 to 6.99 +/- 0.01. The effect of peritubular sodium concentration on cell pH was inhibited by 0.5 mM SITS, but was unaffected by 1 mM amiloride. In addition, when peritubular pH was decreased in the total absence of luminal and peritubular sodium, the rate of cell acidification was 0.2 +/- 0.1 pH units/min, a greater than 90% decrease from that in the presence of sodium. Cell depolarization achieved by increasing the peritubular potassium concentration caused cell pH to increase, an effect that was blocked by peritubular barium or luminal and peritubular sodium removal. Lowering the peritubular chloride concentration from 128 to 0 meq/liter did not affect cell pH. These results suggest the existence of an electrogenic, sodium-coupled H+/OH- /HCO-3 transport mechanism on the basolateral membrane of the rat proximal convoluted tubule. PMID:2999293

  20. The role of pH in determining the species composition of the human colonic microbiota.

    PubMed

    Duncan, Sylvia H; Louis, Petra; Thomson, John M; Flint, Harry J

    2009-08-01

    The pH of the colonic lumen varies with anatomical site and microbial fermentation of dietary residue. We have investigated the impact of mildly acidic pH, which occurs in the proximal colon, on the growth of different species of human colonic bacteria in pure culture and in the complete microbial community. Growth was determined for 33 representative human colonic bacteria at three initial pH values (approximately 5.5, 6.2 and 6.7) in anaerobic YCFA medium, which includes a mixture of short-chain fatty acids (SCFA) with 0.2% glucose as energy source. Representatives of all eight Bacteroides species tested grew poorly at pH 5.5, as did Escherichia coli, whereas 19 of the 23 gram-positive anaerobes tested gave growth rates at pH 5.5 that were at least 50% of those at pH 6.7. Growth inhibition of B. thetaiotaomicron at pH 5.5 was increased by the presence of the SCFA mix (33 mM acetate, 9 mM propionate and 1 mM each of iso-valerate, valerate and iso-butyrate). Analysis of amplified 16S rRNA sequences demonstrated a major pH-driven shift within a human faecal bacterial community in a continuous flow fermentor. Bacteroides spp. accounted for 27% of 16S rRNA sequences detected at pH 5.5, but 86% of sequences at pH 6.7. Conversely, butyrate-producing gram-positive bacteria related to Eubacterium rectale represented 50% of all 16S rRNA sequences at pH 5.5, but were not detected at pH 6.7. Inhibition of the growth of a major group of gram-negative bacteria at mildly acidic pH apparently creates niches that can be exploited by more low pH-tolerant microorganisms.

  1. Experimental Determination of Solubilities of Sodium Polyborates In MgCl 2 Solutions: Solubility Constant of Di-Sodium Hexaborate Tetrahydrate, and Implications For the Diagenetic Formation of Ameghinite

    DOE PAGES

    Xiong, Yongliang; Kirkes, Leslie; KNOX, Jandi; ...

    2017-11-01

    In this paper, solubility measurements were conducted for sodium polyborates in MgCl 2 solutions at 22.5 ± 0.5 °C. According to solution chemistry and XRD patterns, di-sodium tetraborate decahydrate (borax) dissolves congruently, and is the sole solubility-controlling phase, in a 0.01 mol/kg MgCl 2 solution: Na 2B 4O 7•10H 2O(cr) ⇌ 2Na + + 4B(OH) 4 + 2H + + H 2O(l). However, in a 0.1 mol/kg MgCl 2 solution borax dissolves incongruently and is in equilibrium with di-sodium hexaborate tetrahydrate: 2Na 2B 6O 10•4H 2O(cr) + 2Na + + 23H 2O(l) ⇌ 3Na 2B 4O 7•10H 2O(cr) + 2Hmore » +. In this study, the equilibrium constant (log K 0) for Reaction 2 at 25 °C and infinite dilution was determined to be –16.44 ± 0.13 (2σ) based on the experimental data and the Pitzer model for calculations of activity coefficients of aqueous species. In accordance with the log K 0 for Reaction 1 from a previous publication from this research group, and log K 0 for Reaction 2 from this study, the equilibrium constant for dissolution of di-sodium hexaborate tetrahydrate at 25 °C and at infinite dilution, Na 2B 6O 10•4H 2O(cr) + 10H 2O(l) ⇌ 2Na + + 6B(OH) 4 - + 4H + was derived to be –45.42 ± 0.16 (2σ). The equilibrium constants determined in this study can find applications in many fields. For example, in the field of nuclear waste management, the formation of di-sodium hexaborate tetrahydrate in brines containing magnesium will decrease borate concentrations, making less borate available for interactions with Am(III). In the field of experimental investigations, based on the equilibrium constant for Reaction 2, the experimental systems can be controlled in terms of acidity around neutral pH by using the equilibrium assemblage of borax and di-sodium hexaborate tetrahydrate at 25 °C. As salt lakes and natural brines contain both borate and magnesium as well as sodium, the formation of sodium hexaborate tetrahydrate may influence the chemical evolution of salt lakes and natural brines. Di-sodium hexaborate tetrahydrate is a polymorph of the mineral ameghinite [chemical formula Na 2B 6O 10•4H 2O; structural formula NaB 3O 3(OH) 4 or Na 2B 6O 6(OH) 8]. Finally, di-sodium hexaborate tetrahydrate could be a precursor of ameghinite and could be transformed when borate deposits are subject to diagenesis.« less

  2. Experimental Determination of Solubilities of Sodium Polyborates In MgCl 2 Solutions: Solubility Constant of Di-Sodium Hexaborate Tetrahydrate, and Implications For the Diagenetic Formation of Ameghinite

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

    Xiong, Yongliang; Kirkes, Leslie; KNOX, Jandi

    In this paper, solubility measurements were conducted for sodium polyborates in MgCl 2 solutions at 22.5 ± 0.5 °C. According to solution chemistry and XRD patterns, di-sodium tetraborate decahydrate (borax) dissolves congruently, and is the sole solubility-controlling phase, in a 0.01 mol/kg MgCl 2 solution: Na 2B 4O 7•10H 2O(cr) ⇌ 2Na + + 4B(OH) 4 + 2H + + H 2O(l). However, in a 0.1 mol/kg MgCl 2 solution borax dissolves incongruently and is in equilibrium with di-sodium hexaborate tetrahydrate: 2Na 2B 6O 10•4H 2O(cr) + 2Na + + 23H 2O(l) ⇌ 3Na 2B 4O 7•10H 2O(cr) + 2Hmore » +. In this study, the equilibrium constant (log K 0) for Reaction 2 at 25 °C and infinite dilution was determined to be –16.44 ± 0.13 (2σ) based on the experimental data and the Pitzer model for calculations of activity coefficients of aqueous species. In accordance with the log K 0 for Reaction 1 from a previous publication from this research group, and log K 0 for Reaction 2 from this study, the equilibrium constant for dissolution of di-sodium hexaborate tetrahydrate at 25 °C and at infinite dilution, Na 2B 6O 10•4H 2O(cr) + 10H 2O(l) ⇌ 2Na + + 6B(OH) 4 - + 4H + was derived to be –45.42 ± 0.16 (2σ). The equilibrium constants determined in this study can find applications in many fields. For example, in the field of nuclear waste management, the formation of di-sodium hexaborate tetrahydrate in brines containing magnesium will decrease borate concentrations, making less borate available for interactions with Am(III). In the field of experimental investigations, based on the equilibrium constant for Reaction 2, the experimental systems can be controlled in terms of acidity around neutral pH by using the equilibrium assemblage of borax and di-sodium hexaborate tetrahydrate at 25 °C. As salt lakes and natural brines contain both borate and magnesium as well as sodium, the formation of sodium hexaborate tetrahydrate may influence the chemical evolution of salt lakes and natural brines. Di-sodium hexaborate tetrahydrate is a polymorph of the mineral ameghinite [chemical formula Na 2B 6O 10•4H 2O; structural formula NaB 3O 3(OH) 4 or Na 2B 6O 6(OH) 8]. Finally, di-sodium hexaborate tetrahydrate could be a precursor of ameghinite and could be transformed when borate deposits are subject to diagenesis.« less

  3. Uranium Hydridoborates: Synthesis, Magnetism, and X-ray/Neutron Diffraction Structures.

    PubMed

    Braunschweig, H; Gackstatter, A; Kupfer, T; Radacki, K; Franke, S; Meyer, K; Fucke, K; Lemée-Cailleau, M-H

    2015-08-17

    While uranium hydridoborate complexes containing the [BH4](-) moiety have been well-known in the literature for many years, species with functionalized borate centers remained considerably rare. We were now able to prepare several uranium hydridoborates (1-4) with amino-substituted borate moieties with high selectivity by smooth reaction of [Cp*2UMe2] (Cp* = C5Me5) and [Cp'2UMe2] (Cp' = 1,2,4-tBu3C5H2) with the aminoborane H2BN(SiMe3)2. A combination of nuclear magnetic resonance spectroscopy, deuteration experiments, magnetic SQUID measurements, and X-ray/neutron diffraction studies was used to verify the anticipated molecular structures and oxidation states of 1-4 and helped to establish a linear tridentate coordination mode of the borate anions.

  4. Investigation of Mechanistic Pathway for Trimethyl Borate Mediated Amidation of (R)-Mandelic Acid for the Synthesis of Mirabegron, an Antimuscarinic Agent.

    PubMed

    Deshmukh, Dattatray G; Bangal, Mukund N; Patekar, Mukunda R; Medhane, Vijay J; Mathad, Vijayavitthal Thippannachar

    2018-03-01

    The present work describes investigation of mechanistic pathway for trimethyl borate mediated amidation of (R)-mandelic acid (3) with 4-nitophenylethylamine (2) to provide (R)-2-hydroxy-N-[2-(4-nitrophenyl)ethyl]-2-phenylacetamide (4) during mirabegron synthesis. Plausible reaction mechanism is proposed by isolating and elucidating the active α-hydroxy ester intermediate 16 from the reaction mass. Trimethyl borate mediated approach proved to be selective in providing 4 without disturbing α-hydroxyl group and stereochemistry of the chiral center, and is also a greener, more economic and production friendly over the reported methods. The developed approach is rapid and efficient for the preparation of 4 with an overall yield of 85-87% and around 99.0% purity by HPLC at scale.

  5. FTIR of binary lead borate glass: Structural investigation

    NASA Astrophysics Data System (ADS)

    Othman, H. A.; Elkholy, H. S.; Hager, I. Z.

    2016-02-01

    The glass samples were prepared according to the following formula: (100-x) B2O3 - x PbO, where x = 20-80 mol% by melt quenching method. The density of the prepared samples was measured and molar volume was calculated. IR spectra were measured for the prepared samples to investigate the glass structure. The IR spectra were deconvoluted using curves of Gaussian shape at approximately the same frequencies. The deconvoluted data were used to study the effect of PbO content on all the structural borate groups. Some structural parameters such as density, packing density, bond length and bond force constant were theoretically calculated and were compared to the obtained experimental results. Deviation between the experimental and theoretically calculated parameters reflects the dual role of PbO content on the network of borate glass.

  6. Visible luminescence of dysprosium ions in oxyhalide lead borate glasses.

    PubMed

    Pisarska, Joanna; Żur, Lidia; Pisarski, Wojciech A

    2011-08-15

    Visible luminescence of Dy(3+) ions in oxyhalide lead borate glasses was examined. Luminescence spectra show two intense bands at 480 nm and 573 nm due to (4)F(9/2)→(6)H(15/2) (blue) and (4)F(9/2)→(6)H(13/2) (yellow) transitions of Dy(3+). Luminescence decays from (4)F(9/2) state and yellow-to-blue luminescence intensity ratios (Y/B) were analysed with PbX(2) (X=F, Cl) content. An introduction of PbX(2) to the borate glass results in the increasing of (4)F(9/2) lifetime and the decreasing of yellow-to-blue luminescence intensity ratio, which is due to reduction of covalency between Dy(3+) and O(2-)/X(-) ions. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. Dual-responsive surfaces modified with phenylboronic acid-containing polymer brush to reversibly capture and release cancer cells.

    PubMed

    Liu, Hongliang; Li, Yingying; Sun, Kang; Fan, Junbing; Zhang, Pengchao; Meng, Jingxin; Wang, Shutao; Jiang, Lei

    2013-05-22

    Artificial stimuli-responsive surfaces that can mimic the dynamic function of living systems have attracted much attention. However, there exist few artificial systems capable of responding to dual- or multistimulation as the natural system does. Herein, we synthesize a pH and glucose dual-responsive surface by grafting poly(acrylamidophenylboronic acid) (polyAAPBA) brush from aligned silicon nanowire (SiNW) array. The as-prepared surface can reversibly capture and release targeted cancer cells by precisely controlling pH and glucose concentration, exhibiting dual-responsive AND logic. In the presence of 70 mM glucose, the surface is pH responsive, which can vary from a cell-adhesive state to a cell-repulsive state by changing the pH from 6.8 to 7.8. While keeping the pH at 7.8, the surface becomes glucose responsive--capturing cells in the absence of glucose and releasing cells by adding 70 mM glucose. Through simultaneously changing the pH and glucose concentration from pH 6.8/0 mM glucose to pH 7.8/70 mM glucose, the surface is dual responsive with the capability to switch between cell capture and release for at least 5 cycles. The cell capture and release process on this dual-responsive surface is noninvasive with cell viability higher than 95%. Moreover, topographical interaction between the aligned SiNW array and cell protrusions greatly amplifies the responsiveness and accelerates the response rate of the dual-responsive surface between cell capture and release. The responsive mechanism of the dual-responsive surface is systematically studied using a quartz crystal microbalance, which shows that the competitive binding between polyAAPBA/sialic acid and polyAAPBA/glucose contributes to the dual response. Such dual-responsive surface can significantly impact biomedical and biological applications including cell-based diagnostics, in vivo drug delivery, etc.

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

    Warner, Thomas; Jalilehvand, Farideh

    Mercury(II) ions precipitate from aqueous cysteine (H 2Cys) solutions containing H 2Cys/Hg(II) mole ratio ≥ 2.0 as Hg( S-HCys) 2. In absence of additional cysteine, the precipitate dissolves at pH ~12 with the [Hg( S, N-Cys) 2] 2- complex dominating. With excess cysteine (H 2Cys/Hg(II) mole ratio ≥ 4.0), higher complexes form and the precipitate dissolves at lower pH values. Previously, we found that tetrathiolate [Hg( S-Cys) 4] 6- complexes form at pH = 11.0; in this work we extend the investigation to pH values of physiological interest. We examined two series of Hg(II)-cysteine solutions in which C Hg(II) variedmore » between 8 – 9 mM and 80 – 100 mM, respectively, with H 2Cys/Hg(II) mole ratios from 4 to ~20. The solutions were prepared in the pH range 7.1 – 8.8, at the pH at which the initial Hg( S-HCys) 2 precipitate dissolved. The variations in the Hg(II) speciation were followed by 199Hg NMR, X-ray absorption and Raman spectroscopic techniques. Our results show that in the dilute solutions (C Hg(II) = 8 – 9 mM), mixtures of di-, tri- (major) and tetrathiolate complexes exist at moderate cysteine excess (C H2Cys ~ 0.16 M) at pH 7.1. In the more concentrated solutions (C Hg(II) = 80 – 100 mM) with high cysteine excess (C H2Cys > 0.9 M), tetrathiolate [Hg( S-cysteinate) 4] m-6 ( m = 0 – 4) complexes dominate in the pH range 7.3 – 7.8, with lower charge than for the [Hg( S-Cys) 4] 6- complex due to protonation of some ( m) of the amino groups of the coordinated cysteine ligands. In conclusion, the results of this investigation could provide a key to the mechanism of biosorption and accumulation of Hg(II) ions in biological / environmental systems.« less

  9. Pulmonary hypertension is associated with worse survival in hypertrophic cardiomyopathy.

    PubMed

    Ong, Kevin C; Geske, Jeffrey B; Hebl, Virginia B; Nishimura, Rick A; Schaff, Hartzell V; Ackerman, Michael J; Klarich, Kyle W; Siontis, Konstantinos C; Coutinho, Thais; Dearani, Joseph A; Ommen, Steve R; Gersh, Bernard J

    2016-06-01

    Pulmonary hypertension (PH) is associated with increased mortality in various forms of left-sided heart disease. However, the implications of PH in hypertrophic cardiomyopathy (HCM) have not been elucidated. The objective of this study was to determine the prevalence and prognostic implications of PH in HCM. The study cohort consisted of 1570 (54 ± 15 years; 53% male) adults with HCM followed for a median of 3.3 years. PH [pulmonary artery systolic pressure (PASP) >36 mmHg] was identified in 38% of patients who were older (57 ± 15 vs. 52 ± 15 years, P < 0.0001), more likely to be female (59 vs. 40%, P < 0.0001), and were characterized by a higher prevalence of New York Heart Association (NYHA) class 3 or 4 symptoms (61 vs. 45%, P < 0.0001) and atrial fibrillation (29 vs. 15%, P < 0.0001) vs. those without PH. Only 12% had moderate or severe PH (PASP >50 mmHg). In multivariate Cox regression analyses adjusted for age, sex, NYHA class 3 or 4 symptoms, and atrial fibrillation, PASP was an independent predictor of all-cause mortality in patients with non-obstructive HCM (HR 1.59 per 10 mmHg PASP increase, 95% CI 1.28-1.96, P < 0.0001) and in those with obstructive physiology who did not undergo septal reduction therapy (SRT) (HR 1.15 per 10 mmHg PASP, 95% CI 1.01-1.31, P = 0.035). However, PH was not predictive of outcomes in patients with obstructive HCM who underwent SRT. Over one-third of adults evaluated in our referral HCM clinic demonstrated concomitant PH, and this was associated with increased mortality except in those with obstructive HCM who underwent SRT. Published on behalf of the European Society of Cardiology. All rights reserved. © The Author 2016. For permissions please email: journals.permissions@oup.com.

  10. Benzoate- and Salicylate-Tolerant Strains of Escherichia coli K-12 Lose Antibiotic Resistance during Laboratory Evolution.

    PubMed

    Creamer, Kaitlin E; Ditmars, Frederick S; Basting, Preston J; Kunka, Karina S; Hamdallah, Issam N; Bush, Sean P; Scott, Zachary; He, Amanda; Penix, Stephanie R; Gonzales, Alexandra S; Eder, Elizabeth K; Camperchioli, Dominic W; Berndt, Adama; Clark, Michelle W; Rouhier, Kerry A; Slonczewski, Joan L

    2017-01-15

    Escherichia coli K-12 W3110 grows in the presence of membrane-permeant organic acids that can depress cytoplasmic pH and accumulate in the cytoplasm. We conducted experimental evolution by daily diluting cultures in increasing concentrations of benzoic acid (up to 20 mM) buffered at external pH 6.5, a pH at which permeant acids concentrate in the cytoplasm. By 2,000 generations, clones isolated from evolving populations showed increasing tolerance to benzoate but were sensitive to chloramphenicol and tetracycline. Sixteen clones grew to stationary phase in 20 mM benzoate, whereas the ancestral strain W3110 peaked and declined. Similar growth occurred in 10 mM salicylate. Benzoate-evolved strains grew like W3110 in the absence of benzoate, in media buffered at pH 4.8, pH 7.0, or pH 9.0, or in 20 mM acetate or sorbate at pH 6.5. Genomes of 16 strains revealed over 100 mutations, including single-nucleotide polymorphisms (SNPs), large deletions, and insertion knockouts. Most strains acquired deletions in the benzoate-induced multiple antibiotic resistance (Mar) regulon or in associated regulators such as rob and cpxA, as well as the multidrug resistance (MDR) efflux pumps emrA, emrY, and mdtA Strains also lost or downregulated the Gad acid fitness regulon. In 5 mM benzoate or in 2 mM salicylate (2-hydroxybenzoate), most strains showed increased sensitivity to the antibiotics chloramphenicol and tetracycline; some strains were more sensitive than a marA knockout strain. Thus, our benzoate-evolved strains may reveal additional unknown drug resistance components. Benzoate or salicylate selection pressure may cause general loss of MDR genes and regulators. Benzoate is a common food preservative, and salicylate is the primary active metabolite of aspirin. In the gut microbiome, genetic adaptation to salicylate may involve loss or downregulation of inducible multidrug resistance systems. This discovery implies that aspirin therapy may modulate the human gut microbiome to favor salicylate tolerance at the expense of drug resistance. Similar aspirin-associated loss of drug resistance might occur in bacterial pathogens found in arterial plaques. Copyright © 2016 American Society for Microbiology.

  11. Estimating right ventricular stroke work and the pulsatile work fraction in pulmonary hypertension.

    PubMed

    Chemla, Denis; Castelain, Vincent; Zhu, Kaixian; Papelier, Yves; Creuzé, Nicolas; Hoette, Susana; Parent, Florence; Simonneau, Gérald; Humbert, Marc; Herve, Philippe

    2013-05-01

    The mean pulmonary artery pressure (mPAP) replaces mean systolic ejection pressure (msePAP) in the classic formula of right ventricular stroke work (RVSW) = (mPAP - RAP) × stroke volume, where RAP is mean right atrial pressure. Only the steady work is thus taken into account, not the pulsatile work, whereas pulmonary circulation is highly pulsatile. Our retrospective, high-fidelity pressure study tested the hypothesis that msePAP was proportional to mPAP, and looked at the implications for RVSW. Eleven patients with severe, precapillary pulmonary hypertension (PH) (six patients with idiopathic pulmonary arterial hypertension and five with chronic thromboembolic PH; mPAP = 57 ± 10 mm Hg) were studied at rest and during mild to moderate exercise. Eight non-PH control subjects were also studied at rest (mPAP = 16 ± 2 mm Hg). The msePAP was averaged from end diastole to dicrotic notch. In the full data set (53 pressure-flow points), mPAP ranged from 14 to 99.5 mm Hg, cardiac output from 2.38 to 11.1 L/min, and heart rate from 53 to 163 beats/min. There was a linear relationship between msePAP and mPAP (r² = 0.99). The msePAP matched 1.25 mPAP (bias, -0.5 ± 2.6 mm Hg). Results were similar in the resting non-PH group and in resting and the exercising PH group. This implies that the classic formula markedly underestimates RVSW and that the pulsatile work may be a variable 20% to 55% fraction of RVSW, depending on RAP and mPAP. At rest, RVSW in patients with PH was twice as high as that of the non-PH group (P < .05), but pulsatile work fraction was similar between the two groups (26 ± 4% vs 24 ± 1%) because of the counterbalancing effects of high RAP (11 ± 5 mm Hg vs 4 ± 2 mm Hg), which increases the fraction, and high mPAP, which decreases the fraction. Our study favored the use of an improved formula that takes into account the variable pulsatile work fraction: RVSW = (1.25 mPAP - RAP) × stroke volume. Increased RAP and increased mPAP have opposite effects on the pulsatile work fraction.

  12. Noninvasive model including right ventricular speckle tracking for the evaluation of pulmonary hypertension.

    PubMed

    Mahran, Yossra; Schueler, Robert; Weber, Marcel; Pizarro, Carmen; Nickenig, Georg; Skowasch, Dirk; Hammerstingl, Christoph

    2016-08-26

    To find parameters from transthorathic echocardiography (TTE) including speckle-tracking (ST) analysis of the right ventricle (RV) to identify precapillary pulmonary hypertension (PH). Forty-four patients with suspected PH undergoing right heart catheterization (RHC) were consecutively included (mean age 63.1 ± 14 years, 61% male gender). All patients underwent standardized TTE including ST analysis of the RV. Based on the subsequent TTE-derived measurements, the presence of PH was assessed: Left ventricular ejection fraction (LVEF) was calculated by Simpsons rule from 4Ch. Systolic pulmonary artery pressure (sPAP) was assessed with continuous wave Doppler of systolic tricuspid regurgitant velocity and regarded raised with values ≥ 30 mmHg as a surrogate parameter for RA pressure. A concomitantly elevated PCWP was considered a means to discriminate between the precapillary and postcapillary form of PH. PCWP was considered elevated when the E/e' ratio was > 12 as a surrogate for LV diastolic pressure. E/e' ratio was measured by gauging systolic and diastolic velocities of the lateral and septal mitral valve annulus using TDI mode. The results were then averaged with conventional measurement of mitral valve inflow. Furthermore, functional testing with six minutes walking distance (6MWD), ECG-RV stress signs, NT pro-BNP and other laboratory values were assessed. PH was confirmed in 34 patients (precapillary PH, n = 15, postcapillary PH, n = 19). TTE showed significant differences in E/e' ratio (precapillary PH: 12.3 ± 4.4, postcapillary PH: 17.3 ± 10.3, no PH: 12.1 ± 4.5, P = 0.02), LV volumes (ESV: 25.0 ± 15.0 mL, 49.9 ± 29.5 mL, 32.2 ± 13.6 mL, P = 0.027; EDV: 73.6 ± 24.0 mL, 110.6 ± 31.8 mL, 87.8 ± 33.0 mL, P = 0.021) and systolic pulmonary arterial pressure (sPAP: 61.2 ± 22.3 mmHg, 53.6 ± 20.1 mmHg, 31.2 ± 24.6 mmHg, P = 0.001). STRV analysis showed significant differences for apical RV longitudinal strain (RVAS: -7.5% ± 5.6%, -13.3% ± 4.3%, -14.3% ± 6.3%, P = 0.03). NT pro-BNP was higher in patients with postcapillary PH (4677.0 ± 7764.1 pg/mL, precapillary PH: 1980.3 ± 3432.1 pg/mL, no PH: 367.5 ± 420.4 pg/mL, P = 0.03). Patients with precapillary PH presented significantly more often with ECG RV-stress signs (P = 0.001). Receiver operating characteristics curve analyses displayed the most significant area under the curve (AUC) for RVAS (cut-off < -6.5%, AUC 0.91, P < 0.001), sPAP (cut-off > 33 mmHg, AUC 0.86, P < 0.001) and ECG RV stress signs (AUC 0.83, P < 0.001). The combination of these parameters had a sensitivity of 82.8% and a specificity of 17.2% to detect precapillary PH. The combination of non-invasive measurements allows feasible assessment of PH and seems beneficial for the differentiation between the pre- and postcapillary form of this disease.

  13. Shiga-Like Toxin 2 of Enterohemorrhagic Escherichia Coli (EHEC): Genetic Organization and Effects of Toxin in a Murine Model of EHEC Infection

    DTIC Science & Technology

    1990-04-27

    centrifugation. Cells were resuspended in 3.5 ml of 4 M guanidinium isothiocyanate, 20 mM sodium acetate pH 5.2, 0.1 mM DTT, and 0.5% N- lauryl sarcosine. The... sulfate , and 0.4 M sodium chloride. The mixture was heated to 80°C for 5 minutes and then at 37°C for 2 hours to permit the annealing of the...complex was then mixed with 200 /tl of 0.25 M sodium chloride, 30 mM sodium acetate pH 4.5, and 1 mM zinc sulfate , followed by 10 units of SI

  14. Gold Nanocluster-DNase 1 Hybrid Materials for DNA Contamination Sensing

    DTIC Science & Technology

    2014-01-01

    or 1 mM) was added to 2 mL of protein solution under vigorous stirring at 37 ̊ C. After 5 minutes 200 µL of NaOH (1 M) was added to raise the pH to...12 for the 1, 5, and 10 mM HAuCl4 samples whereas 400 µL of NaOH (1M) was required. The various protein/gold mixtures were then left to react for...1: AuNCs were carried out in a final volume of 20 µL buffer (100 mM sodium acetate, 6.25 mM magnesium sulfate pH 5.0), containing 2 µg of dsDNA

  15. Effectiveness of partially hydrolyzed rice glutelin as a food emulsifier: Comparison to whey protein.

    PubMed

    Xu, Xingfeng; Zhong, Junzhen; Chen, Jun; Liu, Chengmei; Luo, Liping; Luo, Shunjing; Wu, Lixin; McClements, David Julian

    2016-12-15

    The emulsifying properties of partially hydrolyzed rice glutelin (H-RG, 2% degree of hydrolysis) were compared to those of whey isolate protein (WPI), a commonly used protein-based emulsifier. The surface load of WPI (1% emulsifier, d32=167.5nm) was 2.8 times lower than that of H-RG (3% emulsifier, d32=159.0nm). Emulsions containing WPI-coated lipid droplets had better stability to pH changes (2-8), NaCl addition (0-500mM) and thermal processing (30-90°C, 0 or 200mM NaCl). Nevertheless, H-RG emulsions were stable over a range of conditions: pH 6-8; NaCl≤200 (pH 7); temperatures≤90°C in the absence of salt (pH 7); and temperatures≤50°C in the presence of 200mM NaCl (pH 7). This study indicates that H-RG may be utilized as a natural emulsifier in the development of label-friendly emulsion-based food products, but that further work is needed to increase the range of applications. Copyright © 2016. Published by Elsevier Ltd.

  16. Actinomyces naeslundii GroEL-dependent initial attachment and biofilm formation in a flow cell system.

    PubMed

    Arai, Toshiaki; Ochiai, Kuniyasu; Senpuku, Hidenobu

    2015-02-01

    Actinomyces naeslundii is an early colonizer with important roles in the development of the oral biofilm. The effects of butyric acid, one of short chain fatty acids in A. naeslundii biofilm formation was observed using a flow cell system with Tryptic soy broth without dextrose and with 0.25% sucrose (TSB sucrose). Significant biofilms were established involving live and dead cells in TSB sucrose with 60mM butyric acid but not in concentrations of 6, 30, 40, and 50mM. Biofilm formation failed in 60mM sodium butyrate but biofilm level in 60mM sodium butyrate (pH4.7) adjusted with hydrochloric acid as 60mM butyric media (pH4.7) was similar to biofilm levels in 60mM butyric acid. Therefore, butyric acid and low pH are required for significant biofilm formation in the flow cell. To determine the mechanism of biofilm formation, we investigated initial A. naeslundii colonization in various conditions and effects of anti-GroEL antibody. The initial colonization was observed in the 60mM butyric acid condition and anti-GroEL antibody inhibited the initial colonization. In conclusion, we established a new biofilm formation model in which butyric acid induces GroEL-dependent initial colonization of A. naeslundii resulting in significant biofilm formation in a flow system. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Open-framework gallium borate with boric and metaboric acid molecules inside structural channels showing photocatalysis to water splitting.

    PubMed

    Gao, Wenliang; Jing, Yan; Yang, Jia; Zhou, Zhengyang; Yang, Dingfeng; Sun, Junliang; Lin, Jianhua; Cong, Rihong; Yang, Tao

    2014-03-03

    An open-framework gallium borate with intrinsic photocatalytic activities to water splitting has been discovered. Small inorganic molecules, H3BO3 and H3B3O6, are confined inside structural channels by multiple hydrogen bonds. It is the first example to experimentally show the structural template effect of boric acid in flux synthesis.

  18. Growth and Evaluation of Nonlinear Optical Crystals for Laser Applications: Lithium Borate, Barium Borate and Silver Gallium Selenide.

    DTIC Science & Technology

    1994-12-08

    communication 2. S. A. Kutovi, V. V. Laptev and S. Yu. Matsnev, " Lanthanum scandoborate as a new highly efficient active medium of solid state lasers," Sov. J...34Noncritical detection of tunable C02 laser radiation into green by upconversion in silver thio- gallate ," Applied Physics B53, 19 (1991). 3. N.-H

  19. Tetrakis(1-imidazolyl) borate (BIM4) based zwitterionic and related molecules used as electron injection layers

    DOEpatents

    Li, Huaping; Xu, Yunhua; Bazan, Guillermo C

    2013-02-05

    Tetrakis(1-imidazolyl)borate (BIm4) based zwitterionic and/or related molecules for the fabrication of PLEDs is provided. Device performances with these materials approaches that of devices with Ba/Al cathodes for which the cathode contact is ohmic. Methods of producing such materials, and electron injection layers and devices containing these materials are also provided.

  20. Spectroscopic and ultrasonic investigations on structural characterization of borate glass specimen doped with transition metal ions.

    PubMed

    Sathish, K; Thirumaran, S

    2015-08-05

    The present work describes the glass samples of composition (x% V₂O₅-(80-x)% B₂O₃-20% Na₂CO₃) VBS glass system and (x%MnO₂-(80-x)% B₂O₃-20% Na₂CO₃) in MBS glass system with mol% ranging from x=3, 6, 9, 12, 15 and 18 in steps of 3 mol% are prepared by melt quenching technique. For these prepared glass systems, sound velocity (longitudinal and shear velocities) and density have been measured. The sound velocity (longitudinal and shear) was measured by using pulse-echo technique at 5 MHz. The XRD study was carried to out to ascertain the amorphous nature of the glass specimen. Using these measured values, the elastic moduli, Poisson's ratio, Debye temperature, acoustic impedance and thermal expansion coefficient of the two glass systems were evaluated. The elastic and mechanical properties of the prepared glass systems are analyzed from ultrasonic study and the structural characterization from spectroscopic study. The effects due to the doping of transition metal ions with borate have been discussed. In the V₂O₅ doped glass system,(VBS glass system) the sound velocity, density and elastic moduli, steeply increases after 12 mol% comparatively with MnO₂ doped glass system (VBS glass system). The present study critically observes the doping of V₂O₅ with borate enhances the strengthening of network linkage and hardening of the glassy network structure than MnO₂. The IR spectral analysis reveals depolymerization of the borate network and conversion of BO₃ or BO4 units with the formation of non-bridging oxygen. The FTIR spectral studies confirm the presence of various functional groups of the sample. FTIR spectrum of sample exhibits broad absorption bands indicating the wide distribution of borate structural units. The effect of Na₂CO₃, V₂O₅ and MnO₂ contents on the structures of borate glass is evaluated from the FTIR spectra. The topological aspects of the prepared glass samples are exhaustively reported from SEM micrographs. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Spectroscopic and ultrasonic investigations on structural characterization of borate glass specimen doped with transition metal ions

    NASA Astrophysics Data System (ADS)

    Sathish, K.; Thirumaran, S.

    2015-08-01

    The present work describes the glass samples of composition (x% V2O5-(80-x)% B2O3-20% Na2CO3) VBS glass system and (x% MnO2-(80-x)% B2O3-20% Na2CO3) in MBS glass system with mol% ranging from x = 3, 6, 9, 12, 15 and 18 in steps of 3 mol% are prepared by melt quenching technique. For these prepared glass systems, sound velocity (longitudinal and shear velocities) and density have been measured. The sound velocity (longitudinal and shear) was measured by using pulse-echo technique at 5 MHz. The XRD study was carried to out to ascertain the amorphous nature of the glass specimen. Using these measured values, the elastic moduli, Poisson's ratio, Debye temperature, acoustic impedance and thermal expansion coefficient of the two glass systems were evaluated. The elastic and mechanical properties of the prepared glass systems are analyzed from ultrasonic study and the structural characterization from spectroscopic study. The effects due to the doping of transition metal ions with borate have been discussed. In the V2O5 doped glass system, (VBS glass system) the sound velocity, density and elastic moduli, steeply increases after 12 mol% comparatively with MnO2 doped glass system (VBS glass system). The present study critically observes the doping of V2O5 with borate enhances the strengthening of network linkage and hardening of the glassy network structure than MnO2. The IR spectral analysis reveals depolymerization of the borate network and conversion of BO3 or BO4 units with the formation of non-bridging oxygen. The FTIR spectral studies confirm the presence of various functional groups of the sample. FTIR spectrum of sample exhibits broad absorption bands indicating the wide distribution of borate structural units. The effect of Na2CO3, V2O5 and MnO2 contents on the structures of borate glass is evaluated from the FTIR spectra. The topological aspects of the prepared glass samples are exhaustively reported from SEM micrographs.

  2. Calibration of the borated ion chamber at NIST reactor thermal column.

    PubMed

    Wang, Z; Hertel, N E; Lennox, A

    2007-01-01

    In boron neutron capture therapy and boron neutron capture enhanced fast neutron therapy, the absorbed dose of tissue due to the boron neutron capture reaction is difficult to measure directly. This dose can be computed from the measured thermal neutron fluence rate and the (10)B concentration at the site of interest. A borated tissue-equivalent (TE) ion chamber can be used to directly measure the boron dose in a phantom under irradiation by a neutron beam. Fermilab has two Exradin 0.5 cm(3) Spokas thimble TE ion chambers, one loaded with boron, available for such measurements. At the Fermilab Neutron Therapy Facility, these ion chambers are generally used with air as the filling gas. Since alpha particles and lithium ions from the (10)B(n,alpha)(7)Li reactions have very short ranges in air, the Bragg-Gray principle may not be satisfied for the borated TE ion chamber. A calibration method is described in this paper for the determination of boron capture dose using paired ion chambers. The two TE ion chambers were calibrated in the thermal column of the National Institute of Standards and Technology (NIST) research reactor. The borated TE ion chamber is loaded with 1,000 ppm of natural boron (184 ppm of (10)B). The NIST thermal column has a cadmium ratio of greater than 400 as determined by gold activation. The thermal neutron fluence rate during the calibration was determined using a NIST fission chamber to an accuracy of 5.1%. The chambers were calibrated at two different thermal neutron fluence rates: 5.11 x 10(6) and 4.46 x 10(7)n cm(-2) s(-1). The non-borated ion chamber reading was used to subtract collected charge not due to boron neutron capture reactions. An optically thick lithium slab was used to attenuate the thermal neutrons from the neutron beam port so the responses of the chambers could be corrected for fast neutrons and gamma rays in the beam. The calibration factor of the borated ion chamber was determined to be 1.83 x 10(9) +/- 5.5% (+/- 1sigma) n cm(-2) per nC at standard temperature and pressure condition.

  3. Nucleation, growth, and repair of a cobalt-based oxygen evolving catalyst.

    PubMed

    Surendranath, Yogesh; Lutterman, Daniel A; Liu, Yi; Nocera, Daniel G

    2012-04-11

    The mechanism of nucleation, steady-state growth, and repair is investigated for an oxygen evolving catalyst prepared by electrodeposition from Co(2+) solutions in weakly basic electrolytes (Co-OEC). Potential step chronoamperometry and atomic force microscopy reveal that nucleation of Co-OEC is progressive and reaches a saturation surface coverage of ca. 70% on highly oriented pyrolytic graphite substrates. Steady-state electrodeposition of Co-OEC exhibits a Tafel slope approximately equal to 2.3 × RT/F. The electrochemical rate law exhibits a first order dependence on Co(2+) and inverse orders on proton (third order) and proton acceptor, methylphosphonate (first order for 1.8 mM ≤ [MeP(i)] ≤ 18 mM and second order dependence for 32 mM ≤ [MeP(i)] ≤ 180 mM). These electrokinetic studies, combined with recent XAS studies of catalyst structure, suggest a mechanism for steady state growth at intermediate MeP(i) concentration (1.8-18 mM) involving a rapid solution equilibrium between aquo Co(II) and Co(III) hydroxo species accompanied with a rapid surface equilibrium involving electrolyte dissociation and deprotonation of surface bound water. These equilibria are followed by a chemical rate-limiting step for incorporation of Co(III) into the growing cobaltate clusters comprising Co-OEC. At higher concentrations of MeP(i) ([MeP(i)] ≥ 32 mM), MePO(3)(2-) equilibrium binding to Co(II) in solution is suggested by the kinetic data. Consistent with the disparate pH profiles for oxygen evolution electrocatalysis and catalyst formation, NMR-based quantification of catalyst dissolution as a function of pH demonstrates functional stability and repair at pH values >6 whereas catalyst corrosion prevails at lower pH values. These kinetic insights provide a basis for developing and operating functional water oxidation (photo)anodes under benign pH conditions. © 2012 American Chemical Society

  4. Residual stress measurements via neutron diffraction of additive manufactured stainless steel 17-4 PH.

    PubMed

    Masoomi, Mohammad; Shamsaei, Nima; Winholtz, Robert A; Milner, Justin L; Gnäupel-Herold, Thomas; Elwany, Alaa; Mahmoudi, Mohamad; Thompson, Scott M

    2017-08-01

    Neutron diffraction was employed to measure internal residual stresses at various locations along stainless steel (SS) 17-4 PH specimens additively manufactured via laser-powder bed fusion (L-PBF). Of these specimens, two were rods (diameter=8 mm, length=80 mm) built vertically upward and one a parallelepiped (8×80×9 mm 3 ) built with its longest edge parallel to ground. One rod and the parallelepiped were left in their as-built condition, while the other rod was heat treated. Data presented provide insight into the microstructural characteristics of typical L-PBF SS 17-4 PH specimens and their dependence on build orientation and post-processing procedures such as heat treatment. Data have been deposited in the Data in Brief Dataverse repository (doi:10.7910/DVN/T41S3V).

  5. Single-channel measurements of an N-acetylneuraminic acid-inducible outer membrane channel in Escherichia coli

    PubMed Central

    Giri, Janhavi; Tang, John M.; Wirth, Christophe; Peneff, Caroline M.

    2012-01-01

    NanC is an Escherichia coli outer membrane protein involved in sialic acid (Neu5Ac, i.e., N-acetylneuraminic acid) uptake. Expression of the NanC gene is induced and controlled by Neu5Ac. The transport mechanism of Neu5Ac is not known. The structure of NanC was recently solved (PDB code: 2WJQ) and includes a unique arrangement of positively charged (basic) side chains consistent with a role in acidic sugar transport. However, initial functional measurements of NanC failed to find its role in the transport of sialic acids, perhaps because of the ionic conditions used in the experiments. We show here that the ionic conditions generally preferred for measuring the function of outer-membrane porins are not appropriate for NanC. Single channels of NanC at pH 7.0 have: (1) conductance 100 pS to 800 pS in 100 mM KCl to 3 M KCl), (2) anion over cation selectivity (Vreversal = +16 mV in 250 mM KCl || 1 M KCl), and (3) two forms of voltage-dependent gating (channel closures above ±200 mV). Single-channel conductance decreases by 50% when HEPES concentration is increased from 100 μM to 100 mM in 250 mM KCl at pH 7.4, consistent with the two HEPES binding sites observed in the crystal structure. Studying alternative buffers, we find that phosphate interferes with the channel conductance. Single-channel conductance decreases by 19% when phosphate concentration is increased from 0 mM to 5 mM in 250 mM KCl at pH 8.0. Surprisingly, TRIS in the baths reacts with Ag|AgCl electrodes, producing artifacts even when the electrodes are on the far side of agar–KCl bridges. A suitable baseline solution for NanC is 250 mM KCl adjusted to pH 7.0 without buffer. PMID:22246445

  6. Buoyancy Driven Coolant Mixing Studies of Natural Circulation Flows at the ROCOM Test Facility Using ANSYS CFX

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

    Hohne, Thomas; Kliem, Soren; Rohde, Ulrich

    2006-07-01

    Coolant mixing in the cold leg, downcomer and the lower plenum of pressurized water reactors is an important phenomenon mitigating the reactivity insertion into the core. Therefore, mixing of the de-borated slugs with the ambient coolant in the reactor pressure vessel was investigated at the four loop 1:5 scaled ROCOM mixing test facility. Thermal hydraulics analyses showed, that weakly borated condensate can accumulate in particular in the pump loop seal of those loops, which do not receive safety injection. After refilling of the primary circuit, natural circulation in the stagnant loops can re-establish simultaneously and the de-borated slugs are shiftedmore » towards the reactor pressure vessel (RPV). In the ROCOM experiments, the length of the flow ramp and the initial density difference between the slugs and the ambient coolant was varied. From the test matrix experiments with 0 resp. 2% density difference between the de-borated slugs and the ambient coolant were used to validate the CFD software ANSYS CFX. To model the effects of turbulence on the mean flow a higher order Reynolds stress turbulence model was employed and a mesh consisting of 6.4 million hybrid elements was utilized. Only the experiments and CFD calculations with modeled density differences show a stratification in the downcomer. Depending on the degree of density differences the less dense slugs flow around the core barrel at the top of the downcomer. At the opposite side the lower borated coolant is entrained by the colder safety injection water and transported to the core. The validation proves that ANSYS CFX is able to simulate appropriately the flow field and mixing effects of coolant with different densities. (authors)« less

  7. The new silver borate Ag{sub 3}B{sub 5}O{sub 9}

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

    Sohr, Gerhard; Falkowski, Viktoria; Huppertz, Hubert, E-mail: hubert.huppertz@uibk.ac.at

    2015-05-15

    Single crystals of Ag{sub 3}B{sub 5}O{sub 9} were obtained via high-pressure synthesis at 3 GPa and 600 °C, using a Walker-type multianvil high-pressure device. Ag{sub 3}B{sub 5}O{sub 9} crystalizes with a=674.7(2), b=943.5(2), c=1103.5(2) pm, V=0.7025(2) nm{sup 3}, and Z=4 in the noncentrosymmetric space group P2{sub 1}2{sub 1}2{sub 1} (no. 19). The orthorhombic structure was refined from 3740 independent reflections with R1=0.0496 and wR2=0.587 (all data). It is built up from infinite corner-sharing chains of BO{sub 4} tetrahedra along the a axis, which are interconnected by BO{sub 3} groups to form a network. In the structure, three crystallographically independent sites aremore » occupied with Ag{sup +} cations exhibiting argentophillic interactions. The synthetic conditions as well as the results of the single crystal structure analysis are presented. - Graphical abstract: Noncentrosymmetric silver borate: During investigations in the system Ag–B–O, a new noncentrosymmetric silver borate Ag{sub 3}B{sub 5}O{sub 9} was discovered. The new structure type is built up from corner-sharing BO{sub 3} and BO{sub 4} groups, forming a network. Argentophillic interactions are clearly indicated by the Ag{sup +}⋯Ag{sup +} distances present in the structure. - Highlights: • A noncentrosymmetric borate Ag{sub 3}B{sub 5}O{sub 9} is accessible via high-pressure synthesis. • Ag{sub 3}B{sub 5}O{sub 9} is the second high-pressure silver borate. • Ag{sup +}⋯Ag{sup +} distances in Ag3B5O9 clearly indicate the presence of argentophillic interactions.« less

  8. Nonclinical safety evaluation of boric acid and a novel borate-buffered contact lens multi-purpose solution, Biotrue™ multi-purpose solution.

    PubMed

    Lehmann, David M; Cavet, Megan E; Richardson, Mary E

    2010-12-01

    Multipurpose solutions (MPS) often contain low concentrations of boric acid as a buffering agent. Limited published literature has suggested that boric acid and borate-buffered MPS may alter the corneal epithelium; an effect attributed to cytotoxicity induced by boric acid. However, this claim has not been substantiated. We investigated the effect of treating cells with relevant concentrations of boric acid using two cytotoxicity assays, and also assessed the impact of boric acid on corneal epithelial barrier function by measuring TEER and immunostaining for tight junction protein ZO-1 in human corneal epithelial cells. Boric acid was also assessed in an in vivo ocular model when administered for 28 days. Additionally, we evaluated Biotrue multi-purpose solution, a novel borate-buffered MPS, alone and with contact lenses for ocular compatibility in vitro and in vivo. Boric acid passed both cytotoxicity assays and did not alter ZO-1 distribution or corneal TEER. Furthermore, boric acid was well-tolerated on-eye following repeated administration in a rabbit model. Finally, Biotrue multi-purpose solution demonstrated good ocular biocompatibility both in vitro and in vivo. This MPS was not cytotoxic and was compatible with the eye when administered alone and when evaluated with contact lenses. We demonstrate that boric acid and a borate-buffered MPS is compatible with the ocular environment. Our findings provide evidence that ocular effects reported for some borate-buffered MPS may be incorrectly attributed to boric acid and are more likely a function of the unique combination of ingredients in the MPS formulation tested. Copyright © 2010 British Contact Lens Association. Published by Elsevier Ltd. All rights reserved.

  9. Earth Observation taken during the Expedition 37 mission

    NASA Image and Video Library

    2013-10-30

    ISS037-E-022990 (30 Oct. 2013) --- This detailed image, photographed by an Expedition 37 crew member on the International Space Station, features the former US Borax mine located to the northwest of Boron, California. The mine, currently owned by the Rio Tinto Group, is the largest open-pit mine in California (covering approximately 54 square kilometers) and is among the largest borate mines in the world. Borates, chemical compounds that include the element boron (B), are important both as providers of an essential plant micronutrient, for metallurgical applications, and as components of specialized types of glass, anticorrosive coatings, fire retardants, and detergents (among other uses). Borate minerals such as borax, kernite, and ulexite are found in deposits at the Rio Tinto borax mine. The geologic setting is a structural, nonmarine basin ? a permanent shallow lake ? fed by thermal springs rich in sodium and boron that existed approximately 16 million years ago, according to scientists. The first mining claim in the area was filed in 1913, following discovery of boron-bearing nodules during well drilling. Much of the mine workings were underground until 1957, when US Borax changed to open-pit mining. The open pit is clearly visible at center; concentric benches along the pit wall are accentuated by shadows and mark successive levels of material extraction. Mine tailings are visible as stacked terraces along the northern boundary of the mine. Ore processing facilities occupy a relatively small percentage of the mine area, and are located directly to the west of the open pit. The Rio Tinto mine is one of the Earth?s richest borate deposits; together with mines in Argentina, they produce almost 40 percent of the world?s supply of industrial borate minerals.

  10. Order–Disorder Transitions and Superionic Conductivity in the Sodium nido -Undeca(carba)borates

    DOE PAGES

    Tang, Wan Si; Dimitrievska, Mirjana; Stavila, Vitalie; ...

    2017-11-20

    The salt compounds NaB 11H 14, Na-7-CB10H13, Li-7-CB 10H 13, Na-7,8-C 2B 9H 12, and Na-7,9-C 2B 9H 12 all contain geometrically similar, monocharged, nido-undeca(carba)borate anions (i.e., truncated icosohedral-shaped clusters constructed of only 11 instead of 12 {B-H} + {C-H} vertices and an additional number of compensating bridging and/or terminal H atoms). We used first-principles calculations, X-ray powder diffraction, differential scanning calorimetry, neutron vibrational spectroscopy, neutron elastic-scattering fixed-window scans, quasielastic neutron scattering, and electrochemical impedance measurements to investigate their structures, bonding potentials, phase-transition behaviors, anion orientational mobilities, and ionic conductivities compared to those of their closo-poly(carba)borate cousins. All exhibited order-disordermore » phase transitions somewhere between room temperature and 375 K. All disordered phases appear to possess highly reorientationally mobile anions (> ~10 10 jumps s -1 above 300 K) and cation-vacancy-rich, close-packed or body-center-cubic-packed structures [like previously investigated closo-poly(carba)borates]. Moreover, all disordered phases display superionic conductivities but with generally somewhat lower values compared to those for the related sodium and lithium salts with similar monocharged 1-CB 9H 10- and CB 11H 12- closo-carbaborate anions. This study significantly expands the known toolkit of solid-state, poly(carba)borate-based salts capable of superionic conductivities and provides valuable insights into the effect of crystal lattice, unit cell volume, number of carbon atoms incorporated into the anion, and charge polarization on ionic conductivity.« less

  11. Pb4(BO3)2(SO4) and Pb2[(BO2)(OH)](SO4): New lead(II) borate-sulfate mixed-anion compounds with two types of 3D network structures

    NASA Astrophysics Data System (ADS)

    Ruan, Ting-Ting; Wang, Wen-Wen; Hu, Chun-Li; Xu, Xiang; Mao, Jiang-Gao

    2018-04-01

    Two new lead(II) borate-sulfate mixed-anion compounds, namely, Pb4(BO3)2(SO4) and Pb2[(BO2)(OH)](SO4), have been prepared by using high-temperature melt method or hydrothermal reaction. These compounds exhibit two different types of 3D structures composed of the same anionic units of BO3 triangles and SO4 tetrahedra which are interconnected by lead(II) cations. In Pb4(BO3)2(SO4), the lead(II) ions are bridged by borate anions into 3D [Pb4(BO3)2]2+ architectures with 1D tunnels of 8-member rings along the a-axis, which are filled by the sulfate anions. In Pb2[(BO2)(OH)](SO4), the lead(II) ions are interconnected by borate and sulfate anions into 2D Pb-B-O and Pb-S-O layers parallel to the ab plane, respectively, and these layers are further condensed into the 3D lead(II) borate-sulfate framework. TGA and DSC studies indicate that Pb4(BO3)2(SO4) is congruently melting with a melting point of 689 °C whereas Pb2[(BO2)(OH)](SO4) decomposes at approximately 335 °C. UV/Vis/NIR optical diffuse reflectance spectrum measurements reveal the optical band gaps of 4.03 and 4.08 eV for Pb4(BO3)2(SO4) and Pb2[(BO2)(OH)](SO4), respectively. Furthermore, the electronic structures of Pb4(BO3)2(SO4) have also been calculated.

  12. Synthesis, Tribological and Hydrolysis Stability Study of Novel Benzotriazole Borate Derivative

    PubMed Central

    Liping, Xiong; Zhongyi, He; Liang, Qian; Lin, Mu; Aixi, Chen; Sheng, Han; Jianwei, Qiu; Xisheng, Fu

    2014-01-01

    Benzotriazole and borate derivatives have long been used as multifunctional additives to lubricants. A novel, environmentally friendly additive borate ester (NHB), which contains boron, ethanolamine, and benzotriazole groups in one molecule, was synthesized by a multi-step reaction, and its tribological properties in rapeseed oil (RSO) were investigated by a four-ball tribometer. The hydrolysis stability of the additive was investigated by half-time and open observation methods, and the mechanism of hydrolysis stability was discussed through Gaussian calculation. The novel compound NHB showed excellent performance under extreme pressure, against wearing, and in reducing friction, and its hydrolysis time is more than 1,220 times, which is better than that of triethyl borate. The mass ratio of NHB is bigger than that of the mixed liquid of triethyl borate and ethanolamine. The lone electron of amino N atoms forms a coordination effect with the B atom to compensate for the shortage of electrons in the B atom and to improve the hydrolysis stability of NHB. The surface morphology and the traces of different elements in the tribofilms formed with 1.0 wt.% NHB in were detected with scanning electron microscopy(SEM), energy dispersive X-ray spectroscopy (EDX)and X-ray photoelectron spectroscopy(XPS). The results shown that the additive caused a tribochemical reaction with the steel ball surface during the lubricating process. A mixed boundary lubrication film that contains organic nitrogen and inorganic salts, such as BN, B2O3, FeOx, Fe–O–B, and FeB, was also formed, and the formation of the lubricating film improved the tribological properties of the base oil. PMID:24465382

  13. Hydrothermal synthesis and characterization of the first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3}

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

    Ortner, Teresa S.; Wurst, Klaus; Perfler, Lukas

    2015-01-15

    The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} was synthesized under hydrothermal conditions from Na{sub 2}B{sub 4}O{sub 7}·10H{sub 2}O and K{sub 2}B{sub 4}O{sub 7}·4H{sub 2}O using KNO{sub 3} as a nitrate source. The compound crystallizes in the space group Pnnm (no. 58) with the lattice parameters a=1320.8(3), b=910.7(2), and c=1232.5(3) pm (Z=4). Isolated Sechserrings formed by BO{sub 4} and BO{sub 3} groups are linked through hydrogen bridges to form a three-dimensional network. - Graphical abstract: The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} was synthesized under hydrothermal conditions from Na{sub 2}B{sub 4}O{sub 7}·10H{sub 2}Omore » and K{sub 2}B{sub 4}O{sub 7}·4H{sub 2}O using KNO{sub 3} as a nitrate source. - Highlights: • The first mixed alkali borate-nitrate K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3} is reported. • Hydrothermal conditions (240 °C, 3d) were used for the synthesis of K{sub 3}Na[B{sub 6}O{sub 9}(OH){sub 3}]NO{sub 3}. • Borate Sechserrings are interconnected through hydrogen-bonding.« less

  14. Formulation and comparative in vitro evaluation of various dexamethasone-loaded pH-sensitive polymeric nanoparticles intended for dermal applications.

    PubMed

    Sahle, Fitsum Feleke; Gerecke, Christian; Kleuser, Burkhard; Bodmeier, Roland

    2017-01-10

    pH-sensitive nanoparticles have a great potential for dermal and transfollicular drug delivery. In this study, pH-sensitive, dexamethasone-loaded Eudragit ® L 100, Eudragit ® L 100-55, Eudragit ® S 100, HPMCP-50, HPMCP-55 and cellulose acetate phthalate nanoparticles were prepared by nanoprecipitation and characterized. The pH-dependent swelling, erosion, dissolution and drug release kinetics were investigated in vitro using dynamic light scattering and Franz diffusion cells, respectively. Their toxicity potential was assessed by the ROS and MTT assays. 100-700nm nanoparticles with high drug loading and entrapment efficiency were obtained. The nanoparticles bear no toxicity potential. Cellulose phthalates nanoparticles were more sensitive to pH than acrylates nanoparticles. They dissolved in 10mM pH 7.5 buffer and released>80% of the drug within 7h. The acrylate nanoparticles dissolved in 40mM pH 7.5 buffer and released 65-70% of the drug within 7h. The nanoparticles remained intact in 10 and 40mM pH 6.0 buffers (HPMCP nanoparticles dissolved in 40mM pH 6.0 buffer) and released slowly. The nanoparticles properties could be modulated by blending the different polymers. In conclusion, various pH-sensitive nanoparticles that could release differently on the skin surface and dissolve and release in the hair follicles were obtained. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Formation of Hg(II) tetrathiolate complexes with cysteine at neutral pH

    DOE PAGES

    Warner, Thomas; Jalilehvand, Farideh

    2016-01-04

    Mercury(II) ions precipitate from aqueous cysteine (H 2Cys) solutions containing H 2Cys/Hg(II) mole ratio ≥ 2.0 as Hg( S-HCys) 2. In absence of additional cysteine, the precipitate dissolves at pH ~12 with the [Hg( S, N-Cys) 2] 2- complex dominating. With excess cysteine (H 2Cys/Hg(II) mole ratio ≥ 4.0), higher complexes form and the precipitate dissolves at lower pH values. Previously, we found that tetrathiolate [Hg( S-Cys) 4] 6- complexes form at pH = 11.0; in this work we extend the investigation to pH values of physiological interest. We examined two series of Hg(II)-cysteine solutions in which C Hg(II) variedmore » between 8 – 9 mM and 80 – 100 mM, respectively, with H 2Cys/Hg(II) mole ratios from 4 to ~20. The solutions were prepared in the pH range 7.1 – 8.8, at the pH at which the initial Hg( S-HCys) 2 precipitate dissolved. The variations in the Hg(II) speciation were followed by 199Hg NMR, X-ray absorption and Raman spectroscopic techniques. Our results show that in the dilute solutions (C Hg(II) = 8 – 9 mM), mixtures of di-, tri- (major) and tetrathiolate complexes exist at moderate cysteine excess (C H2Cys ~ 0.16 M) at pH 7.1. In the more concentrated solutions (C Hg(II) = 80 – 100 mM) with high cysteine excess (C H2Cys > 0.9 M), tetrathiolate [Hg( S-cysteinate) 4] m-6 ( m = 0 – 4) complexes dominate in the pH range 7.3 – 7.8, with lower charge than for the [Hg( S-Cys) 4] 6- complex due to protonation of some ( m) of the amino groups of the coordinated cysteine ligands. In conclusion, the results of this investigation could provide a key to the mechanism of biosorption and accumulation of Hg(II) ions in biological / environmental systems.« less

  16. Distinct structural changes detected by X-ray fiber diffraction in stabilization of F-actin by lowering pH and increasing ionic strength.

    PubMed

    Oda, T; Makino, K; Yamashita, I; Namba, K; Maéda, Y

    2001-02-01

    Lowering pH or raising salt concentration stabilizes the F-actin structure by increasing the free energy change associated with its polymerization. To understand the F-actin stabilization mechanism, we studied the effect of pH, salt concentration, and cation species on the F-actin structure. X-ray fiber diffraction patterns recorded from highly ordered F-actin sols at high density enabled us to detect minute changes of diffraction intensities and to precisely determine the helical parameters. F-actin in a solution containing 30 mM NaCl at pH 8 was taken as the control. F-actin at pH 8, 30 to 90 mM NaCl or 30 mM KCl showed a helical symmetry of 2.161 subunits per turn of the 1-start helix (12.968 subunits/6 turns). Lowering pH from 8 to 6 or replacing NaCl by LiCl altered the helical symmetry to 2.159 subunits per turn (12.952/6). The diffraction intensity associated with the 27-A meridional layer-line increased as the pH decreased but decreased as the NaCl concentration increased. None of the solvent conditions tested gave rise to significant changes in the pitch of the left-handed 1-start helix (approximately 59.8 A). The present results indicate that the two factors that stabilize F-actin, relatively low pH and high salt concentration, have distinct effects on the F-actin structure. Possible mechanisms will be discussed to understand how F-actin is stabilized under these conditions.

  17. Deposition mechanisms of TiO2 nanoparticles in a parallel plate system.

    PubMed

    Chowdhury, Indranil; Walker, Sharon L

    2012-03-01

    In this study, a microscope-based technique was utilized to understand the fundamental mechanisms involved in deposition of TiO(2) nanoparticles (TNPs). Transport and deposition studies were conducted in a parallel plate (PP) flow chamber with TNP labeled with fluorescein isothiocyanate (FITC) for visualization. Attachment of FITC-labeled TNPs on surfaces is a function of a combination of parameters, including ionic strength (IS), pH and flowrate. Significantly higher deposition rates were observed at pH 5 versus pH 7. This is attributed to the conditions being chemically favorable for deposition at pH 5 as compared to pH 7, as predicted by DLVO theory. Additionally, deposition rates at pH 5 were reduced with IS below 10 mM due to the decrease in range of electrostatic attractive forces. Above 10 mM, aggregate size increased, resulting in higher deposition rates. At pH 7, no deposition was observed below 10 mM and above this concentration, deposition increased with IS. The impact of flowrate was also observed, with decreasing flowrate leading to greater deposition due to the reduction in drag force acting on the aggregate (regardless of pH). Comparisons between experimental and theoretical approximations indicate that non-DLVO type forces also play a significant role. This combination of observations suggest that the deposition of these model nanoparticles on glass surfaces was controlled by a combination of DLVO and non-DLVO-type forces, shear rate, aggregation state, and gravitational force acting on TNPs. Copyright © 2011 Elsevier Inc. All rights reserved.

  18. Comment on “A critical evaluation of the boron isotope-pH proxy: The accuracy of ancient ocean pH estimates” by M. Pagani, D. Lemarchand, A. Spivack and J. Gaillardet

    NASA Astrophysics Data System (ADS)

    Hönisch, Bärbel; Hemming, N. Gary; Loose, Brice

    2007-03-01

    Pagani et al. [Pagani M., Lemarchand D., Spivack A., and Gaillardet J. (2005). A critical evaluation of the boron isotope-pH proxy: the accuracy of ancient ocean pH estimates. Geochim. Cosmochim. Acta69(4), 953-961] use data from previous boron isotope studies to suggest that the fractionation between boric acid and borate in seawater as well as the history of δ 11B in seawater are poorly understood, thus limiting our ability to capture realistic ocean pH with this proxy. Although we agree with the authors that the long recognized uncertainty in the secular variation of δ 11B seawater imposes a temporal limit on paleo-pH reconstructions, their evaluation of the δ 11B/pH relationship in carbonates is flawed. Potential complications from vital, temperature and dissolution effects reported in that paper are based on studies that are experimentally and/or analytically poorly constrained. Using published validation studies we will demonstrate that many of the problems outlined by Pagani et al. have already been addressed, or are based on misinterpretations of previous work. Most importantly, statistical evaluation suggests empirical data are best described by a fractionation of ˜20‰. Recent paleoreconstructions confirm that the boron isotope proxy can be used with confidence, if sample selection and analyses are done carefully.

  19. Biochemical characterization of soluble proteins in pecan [Carya illinoinensis (Wangenh.) K. Koch].

    PubMed

    Venkatachalam, Mahesh; Roux, Kenneth H; Sathe, Shridhar K

    2008-09-10

    Pecans (cv. Desirable) contained approximately 10% protein on a dry weight basis. The minimum nitrogen solubility (5.9-7.5%) at 0.25-0.75 M trichloroacetic acid represented the nonprotein nitrogen. Among the solvents assessed for protein solubilization, 0.1 M NaOH was the most effective, while borate saline buffer (pH 8.45) was judged to be optimal for protein solubilization. The protein solubility was minimal in the pH range of 3-7 and significantly increased on either side of this pH range. Increasing the NaCl concentration from 0 to 4 M significantly improved ( approximately 8-fold increase) protein solubilization. Following Osborne protein fractionation, the alkali-soluble glutelin fraction (60.1%) accounted for a major portion of pecan proteins followed by globulin (31.5%), prolamin (3.4%), and albumin (1.5%), respectively. The majority of pecan polypeptides were in the molecular mass range of 12-66 kDa and in the pI range of 4.0-8.3. The pecan globulin fraction was characterized by the presence of several glycoprotein polypeptides. Lysine was the first limiting essential amino acid in the defatted flour, globulin, prolamin, and alkaline glutelin fractions. Leucine and tryptophan were the first limiting essential amino acids in albumin and acid glutelin fractions, respectively. Rabbit polyclonal antibodies detected a range of pecan polypeptides in the 12-60 kDa range, of which the globulin fraction contained the most reactive polypeptides.

  20. Weakly nucleophilic potassium aryltrifluoroborates in palladium-catalyzed Suzuki-Miyaura reactions: relative reactivity of K[4-RC6F4BF3] and the role of silver-assistance in acceleration of transmetallation.

    PubMed

    Bardin, Vadim V; Shabalin, Anton Yu; Adonin, Nicolay Yu

    2015-01-01

    Small differences in the reactivity of weakly nucleophilic potassium aryltrifluoroborates are revealed in the silver-assisted Pd-catalyzed cross-coupling of K[4-RC6F4BF3] (R = H, Bu, MeO, EtO, PrO, iPrO, BuO, t-BuO, CH2=CHCH2O, PhCH2O, PhCH2CH2O, PhO, F, pyrazol-1-yl, pyrrol-1-yl, and indol-1-yl) with ArX (4-BrC6H4CH3, 4-IC6H4F and 3-IC6H4F). An assumed role of silver(I) compounds Ag m Y (Y = O, NO3, SO4, BF4, F) consists in polarization of the Pd-X bond in neutral complex ArPdL n X with the generation of the related transition state or formation of [ArPdL n ][XAg m Y] with a highly electrophilic cation and subsequent transmetallation with the weakly nucleophilic borate. Efficiency of Ag m Y as a polarizing agent decreases in order Ag2O > AgNO3 ≈ Ag2SO4 > Ag[BF4] > AgF. No clear correlation between the reactivity of K[4-RC6F4BF3] and substituent electron parameters, σI and σR°, of the aryl group 4-RC6F4 was found.

  1. Weakly nucleophilic potassium aryltrifluoroborates in palladium-catalyzed Suzuki–Miyaura reactions: relative reactivity of K[4-RC6F4BF3] and the role of silver-assistance in acceleration of transmetallation

    PubMed Central

    Bardin, Vadim V; Shabalin, Anton Yu

    2015-01-01

    Summary Small differences in the reactivity of weakly nucleophilic potassium aryltrifluoroborates are revealed in the silver-assisted Pd-catalyzed cross-coupling of K[4-RC6F4BF3] (R = H, Bu, MeO, EtO, PrO, iPrO, BuO, t-BuO, CH2=CHCH2O, PhCH2O, PhCH2CH2O, PhO, F, pyrazol-1-yl, pyrrol-1-yl, and indol-1-yl) with ArX (4-BrC6H4CH3, 4-IC6H4F and 3-IC6H4F). An assumed role of silver(I) compounds AgmY (Y = O, NO3, SO4, BF4, F) consists in polarization of the Pd–X bond in neutral complex ArPdLnX with the generation of the related transition state or formation of [ArPdLn][XAgmY] with a highly electrophilic cation and subsequent transmetallation with the weakly nucleophilic borate. Efficiency of AgmY as a polarizing agent decreases in order Ag2O > AgNO3 ≈ Ag2SO4 > Ag[BF4] > AgF. No clear correlation between the reactivity of K[4-RC6F4BF3] and substituent electron parameters, σI and σR°, of the aryl group 4-RC6F4 was found. PMID:26124862

  2. Determination of hydrolyzable tannins in the fruit of Terminalia chebula Retz. by high-performance liquid chromatography and capillary electrophoresis.

    PubMed

    Juang, Lih-Jeng; Sheu, Shuenn-Jyi; Lin, Ta-Chen

    2004-06-01

    A RP-HPLC method for determining fourteen components (gallic acid, chebulic acid, 1,6-di-O-galloyl-D-glucose, punicalagin, 3,4,6-tri-O-galloyl-D-glucose, casuarinin, chebulanin, corilagin, neochebulinic acid, terchebulin, ellagic acid, chebulagic acid, chebulinic acid, and 1,2,3,4,6-penta-O-galloyl-D-glucose) in the fruit of Terminalia chebula Retz. is described. The separation was achieved within 80 min using a binary gradient with mobile phases consisting of a pH 2.7 phosphoric acid solution and an 80% CH3CN solution. Capillary electrophoretic analyses were also attempted, and it was found that CZE (25 mM Na2B4O7, 5 mM NaH2PO4, pH 7.0) was an efficient method for the separation of gallotannins, while an MEKC method (25 mM Na2B4O7, 5 mM NaH2PO4, 20 mM SDS, pH 7.0, and 10% acetonitrile) provided a better separation for most of the tannins examined. The HPLC and CE methods developed were both successfully applied to the assay of tannins in commercial samples of Chebulae Fructus.

  3. Pulmonary hypertension registry of Kerala, India (PRO-KERALA) - Clinical characteristics and practice patterns.

    PubMed

    Harikrishnan, S; Sanjay, G; Ashishkumar, M; Menon, Jaideep; Rajesh, Gopalan Nair; Kumar, Raman Krishna; George Koshy, A; Attacheril, Thankachan V; George, Raju; Punnoose, Eapen; Ashraf, S M; Arun, S R; Cholakkal, Mohammed; Jeemon, Panniyammakal

    2018-08-15

    Epidemiological data on pulmonary hypertension (PH) are scarce from developing countries including India. We established a multi-center registry of PH, the PRO-KERALA registry, in Kerala, India. Fifty hospitals enrolled consecutive adult (>18 years) patients for one year. Echocardiographic criteria (right ventricular systolic pressure - RVSP > 50 mmHg) or invasively obtained mean pulmonary artery pressure > 25 mmHg was the criteria for entry. There were 2003 patients (52% Women, mean age 56 ± 16.1 years) enrolled. The mean RVSP was 68.2 (SD = 17.9) mmHg. Majority of the study participants (59%) belonged to group 2 of the WHO Nice Classification 2013 (PH secondary to left heart disease). One-fifth (21.2%) belonged to group 1, while 13.3%, 3.8% and 2.4% of the study population belonged to groups 3, 4 and 5 respectively. More than a quarter (27%) reported PH due to left heart disease with valvular disease etiology; while 20.7% had coronary artery disease. The other common etiological factors were chronic obstructive pulmonary disease (10.6%), congenital heart disease (14.6%), idiopathic pulmonary hypertension (5.8%), and chronic thromboembolic pulmonary hypertension (3.8%). Only one of two patients with pulmonary artery hypertension was receiving PH specific therapies. The use of combination therapy was negligible and PH-specific therapies were prescribed off-label to a small proportion of patients too. PRO-KERALA is the first PH registry from South Asia and the second largest globally. Left heart diseases attribute to three fifths of patients with PH. Utilization rates of PH specific drug therapies are remarkably lower than the Western population. Copyright © 2018 Elsevier B.V. All rights reserved.

  4. Rapid analysis of clenbuterol, salbutamol, procaterol, and fenoterol in pharmaceuticals and human urine by capillary electrophoresis.

    PubMed

    Sirichai, Somsak; Khanatharana, Proespichaya

    2008-09-15

    Capillary electrophoresis (CE) with UV detection for the simultaneous and short-time analysis of clenbuterol, salbutamol, procaterol, fenoterol is described and validated. Optimized conditions were found to be a 10 mmoll(-1) borate buffer (pH 10.0), an separation voltage of 19 kV, and a separation temperature of 32 degrees C. Detection was set at 205 nm. Under the optimized conditions, analyses of the four analytes in pharmaceutical and human urine samples were carried out in approximately 1 min. The interference of the sample matrix was not observed. The LOD (limits of detection) defined at S/N of 3:1 was found between 0.5 and 2.0 mgl(-1) for the analytes. The linearity of the detector response was within the range from 2.0 to 30 mgl(-1) with correlation coefficient >0.996.

  5. Kinetics and mechanism of degradation of some 2-sulfanilamidopyrimidine derivatives. Part VI. The use of Hammett equation for kinetic investigation of 2-sulfanilamidopyrimidine derivatives hydrolysis.

    PubMed

    Zajac, M

    1977-01-01

    General, k, and specific, k1 and k2, first-order rate constants for the parallel reaction of hydrolysis catalized by H+ ions were estimated for sulfadiazine (I), sulfamerazine (II), sulfadimidine (III), sulfaperine (IV) and sulfamethoxydiazine (V), hydrolyzed in 1 mole/dm3 HCl at 333, 343, 355 and 363 K. General first-order rate constants for the spontaneous hydrolysis of I--V in borate buffer pH 9.20 at 403, 411 and 418 K were also determined. Thermodynamic parameters of the reaction (delta Ha, deltaH not equal to, deltaS not equal to, deltaG not equal to and log A) were calculated. The effect of substituents in positions 4, 5 and 6 of the pyrimidine ring on the rate of hydrolysis was interpreted in terms of Hammett equation.

  6. Fast separation of enantiomers by capillary electrophoresis using a combination of two capillaries with different internal diameters.

    PubMed

    Šebestová, Andrea; Petr, Jan

    2017-12-01

    The combination of capillaries with different internal diameters was used to accelerate the separation of enantiomers in capillary electrophoresis. Separation of R,S-1,1'-binaphthalene-2,2'-diyl hydrogen phosphate using isopropyl derivative of cyclofructan 6 was studied as a model system. The best separation conditions included 500 mM sodium borate pH 9.5 with 60 mM concentration of the chiral selector. Separation lasted approx. 1.5 min using the combination of 50 and 100 μm id capillaries of 9.7 cm and 22.9 cm, respectively. It allowed approx. 12-fold acceleration in comparison to the traditional long-end separation mainly due to the higher electroosmotic flow generated in the connected capillaries. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. pH-Dependent Antimicrobial Properties of Copper Oxide Nanoparticles in Staphylococcus aureus

    PubMed Central

    Hsueh, Yi-Huang; Tsai, Ping-Han; Lin, Kuen-Song

    2017-01-01

    The antimicrobial properties of CuO nanoparticles have been investigated, but the underlying mechanisms of toxicity remain the subject of debate. Here, we show that CuO nanoparticles exhibit significant toxicity at pH 5 against four different Staphylococcus aureus (S. aureus) strains, including Newman, SA113, USA300, and ATCC6538. At this pH, but not at pH 6 and 7, 5 mM CuO nanoparticles effectively caused reduction of SA113 and Newman cells and caused at least 2 log reduction, whereas 20 mM killed most strains but not USA300. At 5 mM, the nanoparticles were also found to dramatically decrease reductase activity in SA113, Newman, and ATCC6538 cells, but not USA300 cells. In addition, analysis of X-ray absorption near-edge structure and extended X-ray absorption fine structure confirmed that S. aureus cells exposed to CuO nanoparticles contain CuO, indicating that Cu2+ ions released from nanoparticles penetrate bacterial cells and are subsequently oxidized intracellularly to CuO at mildly acidic pH. The CuO nanoparticles were more soluble at pH 5 than at pH 6 and 7. Taken together, the data conclusively show that the toxicity of CuO nanoparticles in mildly acidic pH is caused by Cu2+ release, and that USA300 is more resistant to CuO nanoparticles (NPs) than the other three strains. PMID:28397766

  8. A study of physical and optical absorption spectra of VO2+ ions in potassium and sodium oxide borate glasses

    NASA Astrophysics Data System (ADS)

    Srinivas, G.; Ramesh, B.; Kumar, J. Siva; Shareefuddin, Md.; Chary, M. N.; Sayanna, R.

    2016-05-01

    Spectroscopic and physical properties of V2O5 doped mixed alkali borate glasses are investigated. Borate glasses containing fixed concentrations of alkaline earth oxides (MgO and BaO) and alkali oxides (K2O and Na2O) were changes and are prepared by melt quenching technique. The values of ri, rp, Rm, αm molar volume and Λth increase and oxygen packing density, density and dopant ion concentration decrease with increasing of K2O content. As a result there shall be an increase in the disorder of the glass network. The optical band gap energies, Urbach energy, boron-boron separation,refractive index, dielectric constant, electronic polarizability and reflection loss values are varies nonlinearly with the K2O content which manifests the mixed alkali effect.

  9. Lipophilic polyelectrolyte gel derived from phosphonium borate can absorb a wide range of organic solvents.

    PubMed

    Sunaga, Sokuro; Kokado, Kenta; Sada, Kazuki

    2018-01-24

    Herein, we demonstrate a polyelectrolyte gel which can absorb a wide range of organic solvents from dimethylsulfoxide (DMSO, permittivity: ε = 47.0) to tetrahydrofuran (ε = 5.6). The gel consists of polystyrene chains with small amounts (∼5 mol%) of lipophilic electrolytes derived from triphenylphosphonium tetraaryl borate. The swelling ability of the polyelectrolyte gel was higher than that of the alkyl ammonium tetraaryl borate previously reported by us, and this is attributed to the higher compatibility with organic solvents, as well as the higher dissociating ability, of the triphenyl phosphonium salt. The role of the ionic moieties was additionally confirmed by post modification of the polyelectrolyte gel via a conventional Wittig reaction, resulting in a nonionic gel. Our findings introduced here will lead to a clear-cut molecular design for polyelectrolyte gels which absorb all solvents.

  10. Method of repressing the precipitation of calcium fluozirconate

    DOEpatents

    Newby, B.J.; Rhodes, D.W.

    1973-12-25

    Boric acid or a borate salt is added to aqueous solutions of fluoride containing radioactive wastes generated during the reprocessing of zirconium alloy nuclear fuels which are to be converted to solid form by calcining in a fluidized bed. The addition of calcium nitrate to the aqueous waste solutions to prevent fluoride volatility during calcination, causes the precipitation of calcium fluozirconate, which tends to form a gel at fluoride concentrations of 3.0 M or greater. The boron containing species introduced into the solution by the addition of the boric acid or borate salt retard the formation of the calcium fluozirconate precipitate and prevent formation of the gel. These boron containing species can be introduced into the solution by the addition of a borate salt but preferably are introduced by the addition of an aqueous solution of boric acid. (Official Gazette)

  11. Cyclisation versus 1,1-Carboboration: Reactions of B(C6F5)3 with Propargyl Amides.

    PubMed

    Melen, Rebecca L; Hansmann, Max M; Lough, Alan J; Hashmi, A Stephen K; Stephan, Douglas W

    2013-09-02

    A series of propargyl amides were prepared and their reactions with the Lewis acidic compound B(C6F5)3 were investigated. These reactions were shown to afford novel heterocycles under mild conditions. The reaction of a variety of N-substituted propargyl amides with B(C6F5)3 led to an intramolecular oxo-boration cyclisation reaction, which afforded the 5-alkylidene-4,5-dihydrooxazolium borate species. Secondary propargyl amides gave oxazoles in B(C6F5)3 mediated (catalytic) cyclisation reactions. In the special case of disubstitution adjacent to the nitrogen atom, 1,1-carboboration is favoured as a result of the increased steric hindrance (1,3-allylic strain) in the 5-alkylidene-4,5-dihydrooxazolium borate species. Copyright © 2013 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Thermoluminescence (TL) dosimeter of dysprosium doped strontium borate glass for different glass modifiers (Na, Li, Ca) subjected from 1 to 9 Gy doses

    NASA Astrophysics Data System (ADS)

    Hamzah, S. A.; Saeed, M. A.; Wagiran, H.; Hashim, I. H.

    2017-10-01

    This article reports TL response for different glass modifier and doping concentration. Alkali oxides (Na2O and Li2O) and alkali earth oxide (CaO) will be used as a glass modifier for strontium borate based glass. The samples were prepared by melt quenching technique. Dy2O3 concentrations ranging from 0.00 to 0.70 mol% and exposure doses of 1 to 9 Gy will be varied. All glass samples exhibit the prominent peak temperature positioned at 186 oC to 232 oC. From all the samples, one of the samples shows an excellent linearity dose response, higher TL and show good reproducibility after 5 cycles exposure which is sodium strontium borate doped with 0.1 mol% Dy2O3 (optimum concentration).

  13. Development of cement solidification process for sodium borate waste generated from PWR plants

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

    Hirofumi Okabe; Tatsuaki Sato; Yuichi Shoji

    2013-07-01

    A cement solidification process for treating sodium borate waste produced in pressurized water reactor (PWR) plants was studied. To obtain high volume reduction and high mechanical strength of the waste, simulated concentrated borate liquid waste with a sodium / boron (Na/B) mole ratio of 0.27 was dehydrated and powdered by using a wiped film evaporator. To investigate the effect of the Na/B mole ratio on the solidification process, a sodium tetraborate decahydrate reagent with a Na/B mole ratio of 0.5 was also used. Ordinary portland cement (OPC) and some additives were used for the solidification. Solidified cement prepared from powderedmore » waste with a Na/B mole ratio 0.24 and having a high silica sand content (silica sand/cement>2) showed to improved uniaxial compressive strength. (authors)« less

  14. Characterization, stabilization and activity of uricase loaded in lipid vesicles.

    PubMed

    Tan, Q Y; Wang, N; Yang, H; Zhang, L K; Liu, S; Chen, L; Liu, J; Zhang, L; Hu, N N; Zhao, C J; Zhang, J Q

    2010-01-15

    Uricase-containing lipid vesicles (UOXLVs) were prepared by reverse-phase evaporation method with high efficiency and the characteristics of UOXLVs were described. The average size and zeta potential of UOXLVs obtained by the optimized formulation were 205.47 nm and -37.33 mV, respectively. Uricase was encapsulated in the alkaline aqueous phase of the lipid vesicle and the stability of its tetrameric structure was thus improved and its activity preserved. The storage stability of uricase in lipid vesicles was significantly increased compared to that of free uricase at 4 degrees C in borate buffer of pH 8.5. At 55 degrees C, free uricase was deactivated much more quickly especially at lower concentration predominantly due to enhanced dissociation of uricase into subunits. An intrinsic tryptophan of uricase recovered from the lipid vesicle thermally treated at 55 degrees C revealed that a partially denatured uricase molecule was stabilized through its hydrophobic interaction with lipid vesicle membrane. This interaction was depressed mainly by dissociation of uricase into subunits. At the physiological pH, significant increase of enzyme activity was found for the uricase entrapped in the lipid vesicles (1.8 times that of free uricase) at their respective optimum pH. The shift of optimum pH and increased uricolytic activity suggested the conformation change of the uricase during the entrapment process. The stability to proteolytic digestion was increased obviously by entrapping the uricase in the lipid vesicles. UOXLVs also showed relatively slower loss in activity compared with free uricase when treated with some chemical reagents. Lastly, in vitro study explicitly indicated that the uricase entrapped by UOXLVs possessed higher uricolytic activity than that of native uricase solution.

  15. Detection of the 267 GHz J = 1-0 rotational transition of PH3 in Saturn with a new Fourier transform spectrometer

    NASA Technical Reports Server (NTRS)

    Weisstein, Eric W.; Serabyn, E.

    1994-01-01

    In recent observations at the Caltech Submillimeter Observatory, the highly pressure-broadened (FWHM = 11.2 GHz) J = 1-0 rotational transition of PH3 (phosphine) was detected on Saturn. By modeling the Saturnian atmosphere with a radiative transfer code, the observed line profile was consistent with a constant PH3 mole fraction of 3.0 plus or minus 1.0 ppm in the upper troposphere. A best-fit to the depth of the line implies a cutoff at high altitudes, with no PH3 present at pressures approximately less than 100 mbar. The observed line depth, combined with the lack of a detectable emission core, implies that a cutoff in the PH3 abundance occurs at a pressure between 13 and 140 mbar. PH3 in Jupiter was not detected, nor any other molecular lines between 195 and 295 GHz (1.54 mm and 1.02 mm, respectively) in either Jupiter or Saturn.

  16. Evaluation of gamma-ray attenuation properties of bismuth borate glass systems using Monte Carlo method

    NASA Astrophysics Data System (ADS)

    Tarim, Urkiye Akar; Ozmutlu, Emin N.; Yalcin, Sezai; Gundogdu, Ozcan; Bradley, D. A.; Gurler, Orhan

    2017-11-01

    A Monte Carlo method was developed to investigate radiation shielding properties of bismuth borate glass. The mass attenuation coefficients and half-value layer parameters were determined for different fractional amounts of Bi2O3 in the glass samples for the 356, 662, 1173 and 1332 keV photon energies. A comparison of the theoretical and experimental attenuation coefficients is presented.

  17. Synthesis, structural characterization and scalable preparation of new amino-zinc borates

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

    Imer, M. R.; González, M.; Veiga, N.

    2017-01-01

    Zinc borates are important materials. We report the preparation of three novel ones: [Zn(NH 3) 3B 4O 5(OH) 4]·H 2O (ZB1), Zn 3(H 2B 3O 7) 2·2NH 3·4H 2O (ZB2), and [Zn(NH 3) 4][B 4O 5(OH) 4]·4H 2O (ZB3).

  18. Scale-up synthesis of zinc borate from the reaction of zinc oxide and boric acid in aqueous medium

    NASA Astrophysics Data System (ADS)

    Kılınç, Mert; Çakal, Gaye Ö.; Yeşil, Sertan; Bayram, Göknur; Eroğlu, İnci; Özkar, Saim

    2010-11-01

    Synthesis of zinc borate was conducted in a laboratory and a pilot scale batch reactor to see the influence of process variables on the reaction parameters and the final product, 2ZnO·3B 2O 3·3.5H 2O. Effects of stirring speed, presence of baffles, amount of seed, particle size and purity of zinc oxide, and mole ratio of H 3BO 3:ZnO on the zinc borate formation reaction were examined at a constant temperature of 85 °C in a laboratory (4 L) and a pilot scale (85 L) reactor. Products obtained from the reaction in both reactors were characterized by chemical analysis, X-ray diffraction, particle size distribution analysis, thermal gravimetric analysis and scanning electron microscopy. The kinetic data for the zinc borate production reaction was fit by using the logistic model. The results revealed that the specific reaction rate, a model parameter, decreases with increase in particle size of zinc oxide and the presence of baffles, but increases with increase in stirring speed and purity of zinc oxide; however, it is unaffected with the changes in the amount of seed and reactants ratio. The reaction completion time is unaffected by scaling-up.

  19. In vitro evaluation of cytotoxicity of silver-containing borate bioactive glass.

    PubMed

    Luo, Shi-Hua; Xiao, Wei; Wei, Xiao-Juan; Jia, Wei-Tao; Zhang, Chang-Qing; Huang, Wen-Hai; Jin, Dong-Xu; Rahaman, Mohamed N; Day, Delbert E

    2010-11-01

    The cytotoxicity of silver-containing borate bioactive glass was evaluated in vitro from the response of osteoblastic and fibroblastic cells in media containing the dissolution products of the glass. Glass frits containing 0-2 weight percent (wt %) Ag were prepared by a conventional melting and quenching process. The amount of Ag dissolved from the glass into a simulated body fluid (SBF), measured using atomic emission spectroscopy, increased rapidly within the first 48 h, but slowed considerably at longer times. Structural and microchemical analysis showed that the formation of a hydroxyapatite-like layer on the glass surface within 14 days of immersion in the SBF. The response of MC3T3-E1 and L929 cells to the dissolution products of the glass was evaluated using SEM observation of cell morphology, and assays of MTT hydrolysis, lactate dehydrogenase release, and alkaline phosphatase activity after incubation for up to 48 h. Cytotoxic effects were found for the borate glass containing 2 wt % Ag, but not for 0.75 and 1 wt % Ag. This borate glass containing up to ∼1 wt % Ag could provide a coating material for bacterial inhibition and enhanced bioactivity of orthopaedic implant materials such as titanium. © 2010 Wiley Periodicals, Inc.

  20. Silicate, borosilicate, and borate bioactive glass scaffolds with controllable degradation rate for bone tissue engineering applications. I. Preparation and in vitro degradation.

    PubMed

    Fu, Qiang; Rahaman, Mohamed N; Fu, Hailuo; Liu, Xin

    2010-10-01

    Bioactive glass scaffolds with a microstructure similar to that of dry human trabecular bone but with three different compositions were evaluated for potential applications in bone repair. The preparation of the scaffolds and the effect of the glass composition on the degradation and conversion of the scaffolds to a hydroxyapatite (HA)-type material in a simulated body fluid (SBF) are reported here (Part I). The in vitro response of osteogenic cells to the scaffolds and the in vivo evaluation of the scaffolds in a rat subcutaneous implantation model are described in Part II. Scaffolds (porosity = 78-82%; pore size = 100-500 microm) were prepared using a polymer foam replication technique. The glasses consisted of a silicate (13-93) composition, a borosilicate composition (designated 13-93B1), and a borate composition (13-93B3), in which one-third or all of the SiO2 content of 13-93 was replaced by B2O3, respectively. The conversion rate of the scaffolds to HA in the SBF increased markedly with the B2O3 content of the glass. Concurrently, the pH of the SBF also increased with the B2O3 content of the scaffolds. The compressive strengths of the as-prepared scaffolds (5-11 MPa) were in the upper range of values reported for trabecular bone, but they decreased markedly with immersion time in the SBF and with increasing B2O3 content of the glass. The results show that scaffolds with a wide range of bioactivity and degradation rate can be achieved by replacing varying amounts of SiO(2) in silicate bioactive glass with B2O3. Copyright 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part A, 2010.

  1. High temperature set retarded well cement compositions and methods

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

    Vinson, E.F.; Brothers, L.E.; Bour, D.L.

    1991-03-05

    This patent describes a set retarded cement composition which is substantially non-thinning at high temperatures. It comprises: hydraulic cement; sufficient water to form a pumpable slurry; a set retarder comprising at least one member selected from the group consisting of a copolymer of 2-acrylamido, 2-methylpropane sulfonic acid (AMPS) and acrylic acid having an average molecular weight below about 5000 and comprising from about 40 to about 60 mole percent AMPS, the copolymer being present in an amount in the range of from about 0.1 to about 5% by weight of cement, lignosulfonates present in an amount in the range ofmore » from about 0.1 to about 5% by weight of cement, borates present in an amount in the range of from about 0.2 to about 5% by weight of cement and organic acids present in an amount of from about 0.2 to about 5% by weight of cement; and a galactomannan gum which has been treated with a hydrophobing agent selected from the group consisting of potassium pyroantimonate present on the gum in an amount of from about 0.001 to about 0.3 percent by weight of the gum and compounds capable of liberating borate ions when added to water present on the gum in an amount of from about 0.5 to about 1.0 percent by weight of the gum, whereby the hydration rate of the gum is retarded at temperatures below about 120 degrees F. and at pH levels above about 10, but the hydration rate increases at temperatures above about 120 degrees F., the treated gum being present in the composition in an amount of at least about 0.5% by weight of cement.« less

  2. A simple method for the determination of glyphosate and aminomethylphosphonic acid in seawater matrix with high performance liquid chromatography and fluorescence detection.

    PubMed

    Wang, Shu; Liu, Baomin; Yuan, Dongxing; Ma, Jian

    2016-12-01

    Glyphosate (GLYP) is an important herbicide which is also used as the phosphorus source for marine organisms. The wide applications of GLYP can lead to its accumulation in oceans and coastal waters, thus creating environmental issues. However, there is limited methods for detection of GLYP and its degradation product, aminomethylphosphonic acid (AMPA) in saline samples. Therefore, a simple and fast method for the quantification of GLYP and AMPA in seawater matrix has been developed based on the derivatization with 9-fluorenylmethylchloroformate (FMOC-Cl), separation with high performance liquid chromatography (HPLC) and detection with fluorescence detector (FLD). In order to maximize sensitivity, the derivatization procedure was carefully optimized regarding concentration of FMOC-Cl, volume of borate buffer, pH of borate buffer, mixing and derivatization time. The derivatization reaction could be completed within 30min in seawater samples without any additional clean-up or desalting steps. Under the optimized conditions, the developed HPLC method showed a wide linear response (up to several mg/L, R 2 >0.99). The limits of detection were 0.60μg/L and 0.30μg/L for GLYP and AMPA in seawater matrix, respectively. The relative standard deviation was 14.0% for GLYP (1.00mg/L) and 3.1% for AMPA (100μg/L) in saline samples with three different operators (n=24). This method was applied to determine the concentration of GLYP and AMPA in seawater culture media and the recovery data indicated minimal matrix interference. Due to its simplicity, high reproducibility and successful application in seawater culture media analysis, this method is a potentially useful analytical technique for both marine research and environmental science. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Noninvasive model including right ventricular speckle tracking for the evaluation of pulmonary hypertension

    PubMed Central

    Mahran, Yossra; Schueler, Robert; Weber, Marcel; Pizarro, Carmen; Nickenig, Georg; Skowasch, Dirk; Hammerstingl, Christoph

    2016-01-01

    AIM To find parameters from transthorathic echocardiography (TTE) including speckle-tracking (ST) analysis of the right ventricle (RV) to identify precapillary pulmonary hypertension (PH). METHODS Forty-four patients with suspected PH undergoing right heart catheterization (RHC) were consecutively included (mean age 63.1 ± 14 years, 61% male gender). All patients underwent standardized TTE including ST analysis of the RV. Based on the subsequent TTE-derived measurements, the presence of PH was assessed: Left ventricular ejection fraction (LVEF) was calculated by Simpsons rule from 4Ch. Systolic pulmonary artery pressure (sPAP) was assessed with continuous wave Doppler of systolic tricuspid regurgitant velocity and regarded raised with values ≥ 30 mmHg as a surrogate parameter for RA pressure. A concomitantly elevated PCWP was considered a means to discriminate between the precapillary and postcapillary form of PH. PCWP was considered elevated when the E/e’ ratio was > 12 as a surrogate for LV diastolic pressure. E/e’ ratio was measured by gauging systolic and diastolic velocities of the lateral and septal mitral valve annulus using TDI mode. The results were then averaged with conventional measurement of mitral valve inflow. Furthermore, functional testing with six minutes walking distance (6MWD), ECG-RV stress signs, NT pro-BNP and other laboratory values were assessed. RESULTS PH was confirmed in 34 patients (precapillary PH, n = 15, postcapillary PH, n = 19). TTE showed significant differences in E/e’ ratio (precapillary PH: 12.3 ± 4.4, postcapillary PH: 17.3 ± 10.3, no PH: 12.1 ± 4.5, P = 0.02), LV volumes (ESV: 25.0 ± 15.0 mL, 49.9 ± 29.5 mL, 32.2 ± 13.6 mL, P = 0.027; EDV: 73.6 ± 24.0 mL, 110.6 ± 31.8 mL, 87.8 ± 33.0 mL, P = 0.021) and systolic pulmonary arterial pressure (sPAP: 61.2 ± 22.3 mmHg, 53.6 ± 20.1 mmHg, 31.2 ± 24.6 mmHg, P = 0.001). STRV analysis showed significant differences for apical RV longitudinal strain (RVAS: -7.5% ± 5.6%, -13.3% ± 4.3%, -14.3% ± 6.3%, P = 0.03). NT pro-BNP was higher in patients with postcapillary PH (4677.0 ± 7764.1 pg/mL, precapillary PH: 1980.3 ± 3432.1 pg/mL, no PH: 367.5 ± 420.4 pg/mL, P = 0.03). Patients with precapillary PH presented significantly more often with ECG RV-stress signs (P = 0.001). Receiver operating characteristics curve analyses displayed the most significant area under the curve (AUC) for RVAS (cut-off < -6.5%, AUC 0.91, P < 0.001), sPAP (cut-off > 33 mmHg, AUC 0.86, P < 0.001) and ECG RV stress signs (AUC 0.83, P < 0.001). The combination of these parameters had a sensitivity of 82.8% and a specificity of 17.2% to detect precapillary PH. CONCLUSION The combination of non-invasive measurements allows feasible assessment of PH and seems beneficial for the differentiation between the pre- and postcapillary form of this disease. PMID:27621775

  4. Pulmonary hypertension in chronic obstructive pulmonary disease and interstitial lung diseases.

    PubMed

    Weitzenblum, Emmanuel; Chaouat, Ari; Canuet, Matthieu; Kessler, Romain

    2009-08-01

    Pulmonary hypertension (PH) is a common complication of chronic respiratory diseases and particularly of chronic obstructive pulmonary disease (COPD) and interstitial lung diseases (ILD). Owing to its frequency COPD is by far the most common cause of PH. It is generally a mild to moderate PH, pulmonary artery mean pressure (PAP) usually ranging between 20 and 25 mm Hg, but PH may worsen during exercise, sleep, and particularly during exacerbations of the disease. These acute increases in PAP may lead to the development of right heart failure. A small proportion of COPD patients may present "disproportionate" PH defined by a resting PAP >35 to 40 mm Hg. The prognosis is particularly poor in these patients. PH is relatively frequent in advanced ILD and particularly in idiopathic pulmonary fibrosis. As in COPD the diagnosis is suggested by Doppler echocardiography, but the confirmation still requires right heart catheterization. As in COPD, functional (alveolar hypoxia) and morphological factors (vascular remodeling, destruction of the pulmonary parenchyma) explain the elevation of pulmonary vascular resistance that leads to PH. Also as in COPD PH is most often mild to moderate. In ILD the presence of PH predicts a poor prognosis. The treatment of PH relies on long-term oxygen therapy. "New" vasodilator drugs have rarely been used in COPD and ILD patients exhibiting severe PH. In advanced ILD the presence of PH is a supplemental argument for considering lung transplantation.

  5. Microbial production of hydrogen and ethanol from glycerol-containing wastes discharged from a biodiesel fuel production plant in a bioelectrochemical reactor with thionine.

    PubMed

    Sakai, Shinsuke; Yagishita, Tatsuo

    2007-10-01

    H(2) and ethanol production from glycerol-containing wastes discharged from a biodiesel fuel production plant by Enterobacter aerogenes NBRC 12010 was demonstrated in bioelectrochemical cells. Thionine as an exogenous electron transfer mediator was reduced by E. aerogenes, and was re-oxidized by a working electrode applied at +0.2 V against a Ag/AgCl reference electrode by a potentiostat (electrode system). At the initial glycerol concentration of 110 mM, 92.9 mM glycerol was consumed in the electrode system with 2 mM thionine after 48 h. On the other hand, the concentration of glycerol consumed was only 50.3 mM under the control conditions without thionine and the electrodes (normal fermentation). There are no differences in the yields of H(2) and ethanol against glycerol consumed between the control conditions and the conditions with the electrode system. A pH of 6.0 was suitable for the H(2) production in the range between pH 6 and pH 7.5 in the electrode system. At pH values of 7.0 and 7.5, H(2) production decreased and formate was remarkably produced in the reaction solution. The rates of both glycerol consumption and the H(2) and ethanol production increased as the thionine concentration and the surface area of the working electrode increased. After 60 h, 154 mM of the initial 161 mM glycerol concentration in the wastes was consumed in the electrode system, which is a 2.6-fold increase compared to the control experiment. Biotechnol. Bioeng. 2007;98: 340-348. (c) 2007 Wiley Periodicals, Inc.

  6. Astringent compounds suppress taste responses in gerbil.

    PubMed

    Schiffman, S S; Suggs, M S; Simon, S A

    1992-11-06

    Astringent tastes are generally considered those that induce long-lasting puckering and drying sensations on the tongue and membranes of the oral cavity. Electrophysiological recordings were made here from the whole chorda tympani nerve in gerbil to understand the interactive effect of astringent-tasting molecules with a broad spectrum of tastants including mono- and divalent salts, bitter compounds, acids, and sweeteners. The astringent tasting compounds were tannic acid (24 mM at pH's 2.9 and 5.5), aluminum ammonium sulfate (30 mM), aluminum potassium sulfate (10 mM) and gallic acid (30 mM). Hydrochloric acid (1 mM, pH 2.9) was also tested to control for acidity, since aqueous solutions of astringent-tasting compounds are acidic. Adaptation of the tongue to tannic acid (24 mM) at both pH 2.9 and 5.5 markedly inhibited responses elicited by salts, acids, sweeteners, and bitter-tasting compounds. The degree of the inhibition at these two pH values is about the same which suggests that tannic acid itself (as opposed to acidity) may produce this inhibition. Chorda tympani responses to sweeteners were completely suppressed by tannic acid; responses to KCl, NH4Cl, and urea were the least suppressed. The aluminum salts also inhibited the chorda tympani responses to all stimuli tested. Gallic acid, which is weakly astringent, had minimal effects on the chorda tympani responses to the test compounds. These data suggest that both tannic acid and the aluminum salts inhibit a variety of transport pathways and receptors in taste cells for a broad spectrum of tastants. The inhibition of some of these pathways may contribute to the astringent taste sensation.

  7. Development of in situ CO2 and pH sensor for AUVs and ROVs

    NASA Astrophysics Data System (ADS)

    Nakano, Yoshiyuki; Kimoto, Hideshi; Miwa, Tetsuya; Yoshida, Hiroshi

    2013-04-01

    Japan Agency for Marine-Earth Science and Technology (JAMSTEC) has been developing two-type autonomous underwater vehicles (AUVs): a cruising AUV and a working AUV, since October 2010. These vehicles will perform carbon dioxide (CO2) and pH observations to explore hydrothermal plume on seabed mineral resources and to monitor a leak of CO2 in carbon capture and storage (CCS) up to depth of 3,000 meters. We here have been developing the compact in situ CO2 and pH sensor (Hybrid CO2-pH sensor: HCS) for the AUVs to obtain vertical and horizontal distributions of CO2 and pH. The HCS consists of an aluminum pressure housing (diameter 84 mm, length 570 mm, weight 4 kg) and an acrylic silicon-oil filled, pressure-compensated vessel (diameter 90 mm, length 355 mm, weight 2 kg) containing valves and pump unit. The HCS is also useful for the observation by remotely operated vehicles (ROVs). The measured data were transmitted to the AUVs or ROVs by serial communications. We can monitor the data of in situ pCO2, pH and so on in real time on board. The measurement principle for the CO2 sensor is based on spectrophotometry. The pCO2 is calculated from the optical absorbance of the pH indicator solution equilibrated with CO2 in seawater through a gas permeable membrane. On the other hand, we adopt potentiometric analysis using original glass and reference electrodes as a pH sensor because of the most commonly used technique for sea water pH measurements and high-speed response (within 20 seconds). From simultaneously measured data of in situ pCO2 and pH, we can also calculate dissolved inorganic carbon (DIC) and total alkalinity (TA) as other carbonate species in the ocean. The resolutions of HCS are 1 μatm for pCO2 and 0.001 pH. In the laboratory experiment, the HCS obtained precisions within 3 μatm and within 0.01 pH, respectively. Our first in situ observational test of the HSC with cruising AUV was made in the coast of the Japan Sea last August. And also first in situ test of the HCS with ROV was performed at Okinawa Trough last September. The data obtained from each tests are consistent with predictions based on past studies.

  8. Prebiotic formation of 'energy-rich' thioesters from glyceraldehyde and N-acetylcysteine

    NASA Technical Reports Server (NTRS)

    Weber, A. L.

    1984-01-01

    The 'energy-rich' thioester, N-acetyl-S-lactoylcysteine, is formed from low concentrations of glyceraldehyde and N-acetylcysteine under anaerobic conditions at ambient temperature in aqueous solutions of sodium phosphate (pH 7.0). Reactions with 2mM glyceraldehyde, 2mM N-acetylcysteine, and 500 mM sodium phosphate (pH 7.0) convert about 0.3 percent/day of the glyceraldehyde to lactoyl thioester. The formation of lactoyl thioester in similar reactions with 500 mM imidazole hydrochloride (pH 7.0) is supported by the thiol-dependence of lactate formation, which is 3-fold greater in the presence of thiol (0.11 percent/day) than in the absence of thiol (0.04 percent/day). The formation of lactoly thioester is thought to proceed by the phosphate (or imidazole)-catalyzed dehydration of glyceraldehyde, which adds to the thiol to form a hemithioacetal that rearranges to the thioester. A limited amount of a second thioester, N-acetyl-S-glyceroyl-cysteine, is also formed at the beginning of these reactions. The significance of these reactions to the origin of life is discussed.

  9. Prebiotic formation of `energy-rich' thioesters from glyceraldehyde and N-acetylcysteine

    NASA Astrophysics Data System (ADS)

    Weber, Arthur L.

    1984-03-01

    The ‘energy-rich’ thioester, N-acetyl-S-lactoylcysteine, is formed from low concentrations of glyceraldehyde and N-acetylcysteine under anaerobic conditions at ambient temperature in aqueous solutions of sodium phosphate (pH 7.0). Reactions with 2 mM glyceraldehyde, 2 mM N-acetylcysteine, and 500 mM sodium phosphate (pH 7.0) convert about 0.3%/day of the glyceraldehyde to lactoyl thioester. The formation of lactoyl thioester in similar reactions with 500 mM imidazole hydrochloride (pH 7.0) is supported by the thiol-dependence of lactate formation, which is 3-fold greater in the presence of thiol (0.11%/day) than in the absence of thiol (0.04%/day). The formation of lactoyl thioester is thought to proceed by the phosphate (or imidazole)-catalyzed dehydration of glyceraldehyde to give pyruvaldehyde, which adds to the thiol to form a hemithioacetal that rearranges to the thioester. A limited amount of a second thioester, N-acetyl-S-glyceroyl-cysteine, is also formed at the beginning of these reactions. The significance of these reactions to the origin of life is discussed.

  10. Borate-polyol complexes in aqueous solution: determination of enthalpies by thermometric titrimetry.

    PubMed

    Aruga, R

    1985-06-01

    Enthalpies for the reaction of borate with 1,2-ethanediol, 1,2-propanediol, 1,2,3-propanetriol and d-mannitol have been determined by thermometric titrimetry. From these enthalpies and equilibrium constants taken from the literature, corresponding entropies have been calculated. The data refer to aqueous solutions at 25 degrees and I = 1.0M (NaNO(3)). The results indicate reasons for the differences in the stabilities of the complexes.

  11. Vibrational spectroscopy of the borate mineral tunellite SrB6O9(OH)2·3(H2O) - Implications for the molecular structure

    NASA Astrophysics Data System (ADS)

    Frost, Ray L.; López, Andrés; Scholz, Ricardo; Xi, Yunfei

    2014-02-01

    Tunellite is a strontium borate mineral with formula: SrB6O9(OH)2·3(H2O) and occurs as colorless crystals in the monoclinic pyramidal crystal system. An intense Raman band at 994 cm-1 was assigned to the BO stretching vibration of the B2O3 units. Raman bands at 1043, 1063, 1082 and 1113 cm-1 are attributed to the in-plane bending vibrations of trigonal boron. Sharp Raman bands observed at 464, 480, 523, 568 and 639 cm-1 are simply defined as trigonal and tetrahedral borate bending modes. The Raman spectrum clearly shows intense Raman bands at 3567 and 3614 cm-1, attributed to OH units. The molecular structure of a natural tunellite has been assessed by using vibrational spectroscopy.

  12. Extraction of heavy metal ions from waste colored glass through phase separation.

    PubMed

    Chen, Danping; Masui, Hirotsugu; Miyoshi, Hiroshi; Akai, Tomoko; Yazawa, Tetsuo

    2006-01-01

    A new method utilizing phase separation phenomena for the extraction of heavy metal ions used as colorants in colored glass is proposed. Colored soda-lime-silica glass containing Co or Cr as a colorant was remelted with B2O3 to yield soda-lime-borosilicate glass. The soda-lime-borosilicate glass thus obtained was leached in 1M nitric acid at 90 degrees C to dissolve the borate phase. All cations (Na, Ca, Cr and Co) concentrated in the borate phase are successfully leached out with the dissolution of the borate phase, when the amount of the B2O3 added to the glass and heat treatment conditions are properly chosen. Porous silicate glass powders with high SiO2 purity are obtained as the result of the leaching. Porous glass can also be formed as bulk material by controlling the composition of additives during the remelting.

  13. Growth and characterization of a novel nonlinear optical borate crystal - Yttrium calcium borate (YCB)

    NASA Astrophysics Data System (ADS)

    Arun Kumar, R.; Arivanandhan, M.; Dhanasekaran, R.; Hayakawa, Y.

    2013-06-01

    A new nonlinear optical single crystal yttrium calcium borate Y2CaB10O19 (YCB) was grown for the first time from its melt. The starting materials were prepared by the solid-state reaction method. The melting point of the synthesized material was identified to be 967 °C. YCB crystal exhibits monoclinic crystal structure with the space group C2. The crystalline perfection of the grown YCB crystal was found to be good. From the UV-VIS-NIR studies, the lower cutoff wavelength of the crystal occurs below 200 nm. The functional groups of the grown crystal were assigned using the FTIR data. The second harmonic generation (SHG) of the YCB crystal was observed using a Nd:YAG laser with a fundamental wavelength of 1064 nm. The laser damage threshold value of the YCB crystal was found to be very high - 10.5 GW/cm2.

  14. In Situ Detection of Boron by ChemCam on Mars

    DOE PAGES

    Gasda, Patrick J.; Haldeman, Ethan Brian; Wiens, Roger Craig; ...

    2017-09-05

    Here, we report the first in situ detection of boron on Mars. Boron has been detected in Gale crater at levels <0.05 wt % B by the NASA Curiosity rover ChemCam instrument in calcium-sulfate-filled fractures, which formed in a late-stage groundwater circulating mainly in phyllosilicate-rich bedrock interpreted as lacustrine in origin. We also consider two main groundwater-driven hypotheses to explain the presence of boron in the veins: leaching of borates out of bedrock or the redistribution of borate by dissolution of borate-bearing evaporite deposits. Our results suggest that an evaporation mechanism is most likely, implying that Gale groundwaters were mildlymore » alkaline. On Earth, boron may be a necessary component for the origin of life; on Mars, its presence suggests that subsurface groundwater conditions could have supported prebiotic chemical reactions if organics were also present and provides additional support for the past habitability of Gale crater.« less

  15. In Situ Detection of Boron by ChemCam on Mars

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

    Gasda, Patrick J.; Haldeman, Ethan Brian; Wiens, Roger Craig

    Here, we report the first in situ detection of boron on Mars. Boron has been detected in Gale crater at levels <0.05 wt % B by the NASA Curiosity rover ChemCam instrument in calcium-sulfate-filled fractures, which formed in a late-stage groundwater circulating mainly in phyllosilicate-rich bedrock interpreted as lacustrine in origin. We also consider two main groundwater-driven hypotheses to explain the presence of boron in the veins: leaching of borates out of bedrock or the redistribution of borate by dissolution of borate-bearing evaporite deposits. Our results suggest that an evaporation mechanism is most likely, implying that Gale groundwaters were mildlymore » alkaline. On Earth, boron may be a necessary component for the origin of life; on Mars, its presence suggests that subsurface groundwater conditions could have supported prebiotic chemical reactions if organics were also present and provides additional support for the past habitability of Gale crater.« less

  16. In Situ Detection of Boron by ChemCam on Mars

    NASA Technical Reports Server (NTRS)

    Gasda, Patrick J.; Haldeman, Ethan B.; Wiens, Roger C.; Rapin, William; Bristow, Thomas F.; Bridges, John C.; Schwenzer, Susanne P.; Clark, Benton; Herkenhoff, Kenneth; Frydenvang, Jens; hide

    2017-01-01

    We report the first in situ detection of boron on Mars. Boron has been detected in Gale crater at levels less than 0.05 wt Percent B by the NASA Curiosity rover ChemCam instrument in calcium-sulfate-filled fractures, which formed in a late-stage groundwater circulating mainly in phyllosilicate-rich bedrock interpreted as lacustrine in origin. We consider two main groundwater-driven hypotheses to explain the presence of boron in the veins: leaching of borates out of bedrock or the redistribution of borate by dissolution of borate-bearing evaporite deposits. Our results suggest that an evaporation mechanism is most likely, implying that Gale groundwaters were mildly alkaline. On Earth, boron may be a necessary component for the origin of life; on Mars, its presence suggests that subsurface groundwater conditions could have supported prebiotic chemical reactions if organics were also present and provides additional support for the past habitability of Gale crater.

  17. In situ detection of boron by ChemCam on Mars

    NASA Astrophysics Data System (ADS)

    Gasda, Patrick J.; Haldeman, Ethan B.; Wiens, Roger C.; Rapin, William; Bristow, Thomas F.; Bridges, John C.; Schwenzer, Susanne P.; Clark, Benton; Herkenhoff, Kenneth; Frydenvang, Jens; Lanza, Nina L.; Maurice, Sylvestre; Clegg, Samuel; Delapp, Dorothea M.; Sanford, Veronica L.; Bodine, Madeleine R.; McInroy, Rhonda

    2017-09-01

    We report the first in situ detection of boron on Mars. Boron has been detected in Gale crater at levels <0.05 wt % B by the NASA Curiosity rover ChemCam instrument in calcium-sulfate-filled fractures, which formed in a late-stage groundwater circulating mainly in phyllosilicate-rich bedrock interpreted as lacustrine in origin. We consider two main groundwater-driven hypotheses to explain the presence of boron in the veins: leaching of borates out of bedrock or the redistribution of borate by dissolution of borate-bearing evaporite deposits. Our results suggest that an evaporation mechanism is most likely, implying that Gale groundwaters were mildly alkaline. On Earth, boron may be a necessary component for the origin of life; on Mars, its presence suggests that subsurface groundwater conditions could have supported prebiotic chemical reactions if organics were also present and provides additional support for the past habitability of Gale crater.

  18. Rare earth-doped lead borate glasses and transparent glass-ceramics: structure-property relationship.

    PubMed

    Pisarski, W A; Pisarska, J; Mączka, M; Lisiecki, R; Grobelny, Ł; Goryczka, T; Dominiak-Dzik, G; Ryba-Romanowski, W

    2011-08-15

    Correlation between structure and optical properties of rare earth ions in lead borate glasses and glass-ceramics was evidenced by X-ray-diffraction, Raman, FT-IR and luminescence spectroscopy. The rare earths were limited to Eu(3+) and Er(3+) ions. The observed BO(3)↔BO(4) conversion strongly depends on the relative PbO/B(2)O(3) ratios in glass composition, giving important contribution to the luminescence intensities associated to (5)D(0)-(7)F(2) and (5)D(0)-(7)F(1) transitions of Eu(3+). The near-infrared luminescence and up-conversion spectra for Er(3+) ions in lead borate glasses before and after heat treatment were measured. The more intense and narrowing luminescence lines suggest partial incorporation of Er(3+) ions into the orthorhombic PbF(2) crystalline phase, which was identified using X-ray diffraction analysis. Copyright © 2010 Elsevier B.V. All rights reserved.

  19. Exchange-mediated spin-lattice relaxation of Fe3+ ions in borate glasses.

    PubMed

    Misra, Sushil K; Pilbrow, John R

    2007-03-01

    Spin-lattice relaxation times (T1) of two borate glasses doped with different concentrations of Fe2O3 were measured using the Electron Spin-Echo (ESE) technique at X-band (9.630 GHz) in the temperature range 2-6K. In comparison with a previous investigation of Fe3+-doped silicate glasses, the relaxation rates were comparable and differed by no more than a factor of two. The data presented here extend those previously reported for borate glasses in the 10-250K range but measured using the amplitude-modulation technique. The T1 values were found to depend on temperature (T) as T(n) with n approximately 1 for the 1% and 0.1% Fe2O3-doped glass samples. These results are consistent with spin-lattice relaxation as effected by exchange interaction of a Fe3+ spin exchange-coupled to another Fe3+ spin in an amorphous material.

  20. Spectroscopy and energy transfer in lead borate glasses doubly doped with Dy(3)(+)-Tb(3+) and Tb(3)(+)-Eu(3+) ions.

    PubMed

    Pisarska, Joanna; Kos, Agnieszka; Pisarski, Wojciech A

    2014-08-14

    Lead borate glasses doubly doped with Dy(3)(+)-Tb(3+) and Tb(3+)-Eu(3+) were investigated using optical spectroscopy. Luminescence spectra of rare earths were detected under various excitation wavelengths. The main green emission band due to (5)D4→(7)F5 transition of Tb(3+) is observed under excitation of Dy(3+), whereas the main red emission band related to (5)D0→(7)F2 transition of Eu(3+) is successfully observed under direct excitation of Tb(3+). In both cases, the energy transfer processes from Dy(3+) to Tb(3+) and from Tb(3+) to Eu(3+) in lead borate glasses occur through a nonradiative processes with efficiencies up to 16% and 18%, respectively. The presence of energy transfer process was also confirmed by excitation spectra measurements. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Characterization of the third-order optical nonlinearity spectrum of barium borate glasses

    NASA Astrophysics Data System (ADS)

    Santos, S. N. C.; Almeida, J. M. P.; Paula, K. T.; Tomazio, N. B.; Mastelaro, V. R.; Mendonça, C. R.

    2017-11-01

    Borate glasses have proven to be an important material for applications ranging from radiation dosimetry to nonlinear optics. In particular, B2O3-BaO based glasses are attractive to frequency generation since their barium metaborate phase (β-BaB2O4 or β-BBO) may be crystallized under proper heat treatment. Despite the vast literature covering their linear and second-order optical nonlinear properties, their third-order nonlinearities remain overlooked. This paper thus reports a study on the nonlinear refraction (n2) of BBO and BBS-DyEu glasses through femtosecond Z-scan technique. The results were modeled using the BGO approach, which showed that oxygen ions are playing a role in the nonlinear optical properties of the glasses studied here. In addition, the barium borate glasses containing rare-earths ions were found to exhibit larger nonlinearities, which is in agreement with previous studies.

  2. Implications for Ophthalmic Formulations: Ocular Buffers Show Varied Cytotoxic Impact on Human Corneal-Limbal and Human Conjunctival Epithelial Cells.

    PubMed

    Schuerer, Nadine; Stein, Elisabeth; Inic-Kanada, Aleksandra; Pucher, Marion; Hohenadl, Christine; Bintner, Nora; Ghasemian, Ehsan; Montanaro, Jacqueline; Barisani-Asenbauer, Talin

    2017-06-01

    To investigate toxicity associated with buffers commonly used in topical ocular drug formulations using a human corneal-limbal epithelial (HCLE) and a human conjunctival epithelial (HCjE) cell model. HCLE and HCjE cells were incubated for 10, 30, or 60 minutes with 4 different buffers based on borate, citrate, phosphate, and Tris-HCl at 10, 50, and 100 mM concentrations. To detect possible delayed effects on cell viability, after 60 minutes of buffer incubation, cells were further incubated for 24 hours with a cell medium. Cell viability was determined using a colorimetric XTT-based assay. The morphology of cells was also investigated. HCjE cells showed more sensitivity to buffer incubation than HCLE cells. The 100 mM phosphate buffer displayed significant delayed effects on cell viability of HCLE 16.8 ± 4.8% and HCjE 39.2 ± 6.1% cells after 60 minutes of exposure (P < 0.05). HCjE cell viability was reduced after 60 minutes incubations with 50 and 100 mM citrate buffer to 42.8 ± 6.5% and 39.3 ± 7.9%, respectively, and even lower percentages at the delayed time point (both P < 0.05). HCLE cell morphology was distinctly altered by 100 mM phosphate and Tris buffers after 30 minutes, whereas HCjE cells already showed marked changes after 10 minutes of exposure to 100 mM citrate and phosphate buffers. We observed a time-dependent decrease of viability in both HCLE and HCjE cells exposed to higher buffer concentrations. Therefore, we propose further in vivo studies to translate these finding to humans to discern the real effects of the buffer concentration in eye drops on the ocular surface.

  3. Implications for Ophthalmic Formulations: Ocular Buffers Show Varied Cytotoxic Impact on Human Corneal–Limbal and Human Conjunctival Epithelial Cells

    PubMed Central

    Schuerer, Nadine; Stein, Elisabeth; Inic-Kanada, Aleksandra; Pucher, Marion; Hohenadl, Christine; Bintner, Nora; Ghasemian, Ehsan; Montanaro, Jacqueline

    2017-01-01

    Purpose: To investigate toxicity associated with buffers commonly used in topical ocular drug formulations using a human corneal–limbal epithelial (HCLE) and a human conjunctival epithelial (HCjE) cell model. Methods: HCLE and HCjE cells were incubated for 10, 30, or 60 minutes with 4 different buffers based on borate, citrate, phosphate, and Tris-HCl at 10, 50, and 100 mM concentrations. To detect possible delayed effects on cell viability, after 60 minutes of buffer incubation, cells were further incubated for 24 hours with a cell medium. Cell viability was determined using a colorimetric XTT–based assay. The morphology of cells was also investigated. Results: HCjE cells showed more sensitivity to buffer incubation than HCLE cells. The 100 mM phosphate buffer displayed significant delayed effects on cell viability of HCLE 16.8 ± 4.8% and HCjE 39.2 ± 6.1% cells after 60 minutes of exposure (P < 0.05). HCjE cell viability was reduced after 60 minutes incubations with 50 and 100 mM citrate buffer to 42.8 ± 6.5% and 39.3 ± 7.9%, respectively, and even lower percentages at the delayed time point (both P < 0.05). HCLE cell morphology was distinctly altered by 100 mM phosphate and Tris buffers after 30 minutes, whereas HCjE cells already showed marked changes after 10 minutes of exposure to 100 mM citrate and phosphate buffers. Conclusions: We observed a time-dependent decrease of viability in both HCLE and HCjE cells exposed to higher buffer concentrations. Therefore, we propose further in vivo studies to translate these finding to humans to discern the real effects of the buffer concentration in eye drops on the ocular surface. PMID:28399036

  4. Exercise-Induced Pulmonary Hypertension: Translating Pathophysiological Concepts Into Clinical Practice.

    PubMed

    Naeije, Robert; Saggar, Rajeev; Badesch, David; Rajagopalan, Sanjay; Gargani, Luna; Rischard, Franz; Ferrara, Francesco; Marra, Alberto M; D' Alto, Michele; Bull, Todd M; Saggar, Rajan; Grünig, Ekkehard; Bossone, Eduardo

    2018-01-31

    Exercise stress testing of the pulmonary circulation for the diagnosis of latent or early-stage pulmonary hypertension (PH) is gaining acceptance. There is emerging consensus to define exercise-induced PH by a mean pulmonary artery pressure > 30 mm Hg at a cardiac output < 10 L/min and a total pulmonary vascular resistance> 3 Wood units at maximum exercise, in the absence of PH at rest. Exercise-induced PH has been reported in association with a bone morphogenetic receptor-2 gene mutation, in systemic sclerosis, in left heart conditions, in chronic lung diseases, and in chronic pulmonary thromboembolism. Exercise-induced PH is a cause of decreased exercise capacity, may precede the development of manifest PH in a proportion of patients, and is associated with a decreased life expectancy. Exercise stress testing of the pulmonary circulation has to be dynamic and rely on measurements of the components of the pulmonary vascular equation during, not after exercise. Noninvasive imaging measurements may be sufficiently accurate in experienced hands, but suffer from lack of precision, so that invasive measurements are required for individual decision-making. Exercise-induced PH is caused either by pulmonary vasoconstriction, pulmonary vascular remodeling, or by increased upstream transmission of pulmonary venous pressure. This differential diagnosis is clinical. Left heart disease as a cause of exercise-induced PH can be further ascertained by a pulmonary artery wedge pressure above or below 20 mm Hg at a cardiac output < 10 L/min or a pulmonary artery wedge pressure-flow relationship above or below 2 mm Hg/L/min during exercise. Copyright © 2018 American College of Chest Physicians. Published by Elsevier Inc. All rights reserved.

  5. Phospholipase B activity of a purified phospholipase A from Vipera palestinae venom.

    PubMed

    Shiloah, J; Klibansky, C; de Vries, A; Berger, A

    1973-05-01

    Phospholipase was isolated (in two fractions) from Vipera palestinae venom and it was shown to possess phospholipase A activity (hydrolyzing diacyl-sn-glycerophosphorylcholines, e.g., lecithin, in the 2-position) as well as lysophospholipase (phospholipase B) activity (hydrolyzing 1-monoacyl-sn-glycerophosphorylcholines, e.g., lysolecithin, yielding free fatty acid and glycerophosphorylcholine). Each of the two purified enzyme fractions was homogeneous as judged by electrophoresis on acrylamide gel and by immunodiffusion and immunoelectrophoresis, and both had essentially equal activities. The ratio of the specific activity, at various purification stages, to the specific activity of the whole venom was the same for A activity (substrate lecithin) as for B activity (substrate lysolecithin). The enzyme has a molecular weight of 16,000, six S-S bridges, and no free thiol groups. At pH 7, dimerization was observed in the ultracentrifuge. A dissociation constant of about 10(-5) m was estimated. The amino acid composition for both fractions (140 amino acid residues) was found to be essentially the same. The A activity had a pH optimum at 9; B activity was low at this pH but increased steadily beyond pH 10.5. For the hydrolysis of lysolecithin the Lineweaver-Burk plot was found to be linear, giving K(m) = 1.1 mm and k(cat) = 0.55 sec(-1) at 37 degrees C and pH 10. 2-Deoxylysolecithin was also hydrolyzed by the enzyme at pH 10, with k(cat) = 0.01 sec(-1) (zero-order kinetics in the range 0.5-2.5 mm). For lecithin these constants could not be determined, but at 0.25 mm substrate the hydrolysis rate (at pH 9) of lecithin was about 1000 times the hydrolysis rate of lysolecithin (at pH 10).

  6. Purification and Characterization of a Fibrinolytic Enzyme from Bacillus pumilus 2.g Isolated from Gembus, an Indonesian Fermented Food

    PubMed Central

    Afifah, Diana Nur; Sulchan, Muhammad; Syah, Dahrul; Yanti; Suhartono, Maggy Thenawidjaja; Kim, Jeong Hwan

    2014-01-01

    Bacillus pumilus 2.g isolated from gembus, an Indonesian fermented soybean cake, secretes several proteases that have strong fibrinolytic activities. A fibrinolytic enzyme with an apparent molecular weight of 20 kDa was purified from the culture supernatant of B. pumilus 2.g by sequential application of ammonium sulfate precipitation, ion-exchange chromatography, and hydrophobic chromatography. The partially purified enzyme was stable between pH 5 and pH 9 and temperature of less than 60°C. Fibrinolytic activity was increased by 5 mM MgCl2 and 5 mM CaCl2 but inhibited by 1 mM phenylmethylsulfonyl fluoride (PMSF), 1 mM sodium dodecyl sulfate (SDS), and 1 mM ethylenediaminetetraacetic acid (EDTA). The partially purified enzyme quickly degraded the α and β chains of fibrinogen but was unable to degrade the γ chain. PMID:25320719

  7. Pulmonary hypertension and ventilation during exercise: Role of the pre-capillary component.

    PubMed

    Caravita, Sergio; Faini, Andrea; Deboeck, Gael; Bondue, Antoine; Naeije, Robert; Parati, Gianfranco; Vachiéry, Jean-Luc

    2017-07-01

    Excessive exercise-induced hyperventilation and high prevalence of exercise oscillatory breathing (EOB) are present in patients with post-capillary pulmonary hypertension (PH) complicating left heart disease (LHD). Patients with pre-capillary PH have even higher hyperventilation but no EOB. We sought to determine the impact of a pre-capillary component of PH on ventilatory response to exercise in patients with PH and left heart disease. We retrospectively compared patients with idiopathic or heritable pulmonary arterial hypertension (PAH, n = 29), isolated post-capillary PH (IpcPH, n = 29), and combined post- and pre-capillary PH (CpcPH, n = 12). Diastolic pressure gradient (DPG = diastolic pulmonary artery pressure - pulmonary wedge pressure) was used to distinguish IpcPH (DPG <7 mm Hg) from CpcPH (DPG ≥7 mm Hg). Pulmonary vascular resistance (PVR) was higher in PAH, intermediate in CpcPH, and low in IpcPH. All patients with CpcPH but 1 had PVR >3 Wood unit. Exercise-induced hyperventilation (high minute ventilation over carbon dioxide production, low end-tidal carbon dioxide) was marked in PAH, intermediate in CpcPH, and low in IpcPH (p < 0.001) and correlated with DPG and PVR. Prevalence of EOB decreased from IpcPH to CpcPH to PAH (p < 0.001). Patients with CpcPH may have worse hemodynamics than patients with IpcPH and distinct alterations of ventilatory control, consistent with more exercise-induced hyperventilation and less EOB. This might be explained at least in part by the presence and extent of pulmonary vascular disease. Copyright © 2017 International Society for Heart and Lung Transplantation. Published by Elsevier Inc. All rights reserved.

  8. Formation of N-nitrosodimethylamine (NDMA) by ozonation of dyes and related compounds.

    PubMed

    Oya, Masami; Kosaka, Koji; Asami, Mari; Kunikane, Shoichi

    2008-12-01

    Formation of N-nitrosodimethylamine (NDMA) by ozonation of commercially available dyes and related compounds was investigated. Ozonation was conducted using a semi-batch type reactor, and ozone concentration in gas phase and the ozone gas flow were 10 mg L(-1) and 1.0 L min(-1), respectively. NDMA was formed by 15 min of ozonation of seven out of eight selected target compounds (0.05 mM) at pH 7. All the target compounds with N,N-dimethylamino functions were NDMA precursors in ozonation. The lowest and highest NDMA concentrations after ozonation of the target compounds were 13 ng L(-1) for N,N-dimethylformamide (DMF) and 1600 ng L(-1) for N,N-dimethyl-p-phenylenediamine (DMPD), respectively. NDMA concentrations after 15 min of ozonation of 0.05 mM methylene blue (MB) and DMPD increased with an increase in pH in its range of 6-8. The effects of coexisting compounds on NDMA concentrations after 15 min of ozonation of 0.05 mM MB and DMPD were examined at pH 7. NDMA concentrations after ozonation of MB and DMPD increased by the presence of 0.05 mM (0.7 mg L(-1) as N) nitrite (NO(2)(-)); 5000 ng L(-1) for MB and 4000 ng L(-1) for DMPD. NDMA concentration after MB ozonation decreased by the presence of 5mM tertiary butyl alcohol (TBA), a hydroxyl radical (HO.) scavenger, but that after DMPD ozonation was increased by the presence of TBA. NDMA concentrations after ozonation of MB and DMPD were not affected by the presence of 0.16 mM (5.3 mg L(-1)) hydrogen peroxide (H(2)O(2)). When 0.05 mM MB and DMPD were added to the Yodo and Tone river water samples, NDMA concentrations after 15 min of their ozonation at pH 7 increased compared with those in the case of addition to ultrapure water samples.

  9. Influence of collector surface composition and water chemistry on the deposition of cerium dioxide nanoparticles: QCM-D and column experiment approaches.

    PubMed

    Liu, Xuyang; Chen, Gexin; Su, Chunming

    2012-06-19

    The deposition behavior of cerium dioxide (CeO(2)) nanoparticles (NPs) in dilute NaCl solutions was investigated as a function of collector surface composition, pH, ionic strength, and organic matter (OM). Sensors coated separately with silica, iron oxide, and alumina were applied in quartz crystal microbalance with dissipation (QCM-D) to examine the effect of these mineral phases on CeO(2) deposition in NaCl solution (1-200 mM). Frequency and dissipation shift followed the order: silica > iron oxide > alumina in 10 mM NaCl at pH 4.0. No significant deposition was observed at pH 6.0 and 8.5 on any of the tested sensors. However, ≥ 94.3% of CeO(2) NPs deposited onto Ottawa sand in columns in 10 mM NaCl at pH 6.0 and 8.5. The inconsistency in the different experimental approaches can be mainly attributed to NP aggregation, surface heterogeneity of Ottawa sand, and flow geometry. In QCM-D experiments, the deposition kinetics was found to be qualitatively consistent with the predictions based on the classical colloidal stability theory. The presence of low levels (1-6 mg/L) of Suwannee River humic acid, fulvic acid, alginate, citric acid, and carboxymethyl cellulose greatly enhanced the stability and mobility of CeO(2) NPs in 1 mM NaCl at pH 6.5. The poor correlation between the transport behavior and electrophoretic mobility of CeO(2) NPs implies that the electrosteric effect of OM was involved.

  10. Effects of pH and phosphate on glyphosate adsorption to Argentina soils.

    NASA Astrophysics Data System (ADS)

    De Geronimo, Eduardo; Aparicio, Virginia; Costa, José Luis

    2017-04-01

    Glyphosate is a non-selective, post-emergence herbicide that is widely used in Argentina. Due to the similar molecular structures, glyphosate and phosphate compete for the same adsorption sites in soil. Soil pH has a strong influence in glyphosate and phosphate adsorption since it modifies the net charge of the molecules and, consequently, the force of the electrostatic interaction between these molecules and soil components. Glyphosate adsorption generally decreases as the soil pH was increased, although there were exceptions. In this work, we study the effects of pH and the presence of phosphate on the adsorption of glyphosate on six different types of Argentina soils. Batch equilibrium technique was employed to study the adsorption of glyphosate onto soils at different pH values (from 3 to 9) and phosphate content (0.5 and 1 mM). Stepwise multiple linear regression analysis was applied to obtain a relationship between the sorption parameters and soil properties. The results indicated that Freundlich equations used to simulate glyphosate adsorption isotherms gave high correlation coefficients with Kf values range from 24.9 to 397.4. Clay contents and soil pH were found to be the most significant soil factors affecting the glyphosate adsorption process. The presence of phosphate significantly decreased the adsorption of glyphosate to soils. The Kf values obtained for all six soils decreased a 40% at 0.5 mM of phosphate and a 55% at 1 mM of phosphate. On the other hand, the affinity parameters of glyphosate to soils varied with changes in pH. A general trend of decrease in glyphosate adsorption with increase in pH was observed for all six studied soils. In turn, there appears to be a maximum glyphosate adsorption at pH close to 6 for most soils when the net charge of the molecule at this pH was approximately -1.7.

  11. Extraction and characterization of oil bodies from soy beans: a natural source of pre-emulsified soybean oil.

    PubMed

    Iwanaga, Daigo; Gray, David A; Fisk, Ian D; Decker, Eric Andrew; Weiss, Jochen; McClements, David Julian

    2007-10-17

    Soybeans contain oil bodies that are coated by a layer of oleosin proteins. In nature, this protein coating protects the oil bodies from environmental stresses and may be utilized by food manufacturers for the same purpose. In this study, oil bodies were extracted from soybean using an aqueous extraction method that involved blending, dispersion (pH 8.6), filtration, and centrifugation steps. The influence of NaCl (0-250 mM), thermal processing (30-90 degrees C, 20 min) and pH (2-8) on the properties and stability of the oil bodies was analyzed using zeta-potential, particle size, and creaming stability measurements. The extracted oil bodies were relatively small ( d 32 approximately 250 nm), and their zeta-potential went from around +12 mV to -20 mV as the pH was increased from 2 to 8, with an isoelectric point around pH 4. The oil bodies were stable to aggregation and creaming at low (pH = 2) and high (pH >/= 6) pH values but were unstable at intermediate values (3

  12. An efficient process for obtaining prebiotic oligosaccharides derived from lactulose using isomerized and purified whey permeate.

    PubMed

    Sabater, Carlos; Olano, Agustín; Prodanov, Marin; Montilla, Antonia; Corzo, Nieves

    2017-12-01

    One of the most promising uses of whey permeate (WP) is the synthesis of prebiotic oligosaccharides. Herein, commercial WP was submitted to chemical isomerization catalysed by sodium borate at an alkaline pH and subsequent purification using anion-exchange resins to remove boron. Subsequently, purified mixtures were used to synthesize prebiotic oligosaccharides using β-galactosidase from Bacillus circulans. Isomerization of concentrated WP (200 g L -1 lactose) gave rise to levels of lactulose up to 155.5 g L -1 after 30 min of reaction (molar ratio of boron/lactose, 1/1; pH 12; 70 °C). Boron was removed from the isomerized WP (IWP) using the combination of a strong acid (IR-120, H + ) and a weak base (IRA-743) anion-exchange resins, reducing its level to <1 ppm, without loss of lactulose. During the transglycosylation reaction of purified IWP (lactose/lactulose ratio, 1/2.4) maximum content of prebiotic compounds was achieved, i.e. 690 g kg -1 WP after 3 h of reaction. This study shows that combined chemical-enzymatic reactions together with the purification of IWP results in an efficient synthesis of prebiotic oligosaccharides. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  13. Development of a CZE method for the quantification of pseudoephedrine and cetirizine.

    PubMed

    Alnajjar, Ahmed O; Idris, Abubakr M

    2014-10-01

    Pseudoephedrine and cetirizine have been combined in dosage forms with more therapeutic benefits when compared with single-drug treatment. The current manuscript reports the development of the first capillary zone electrophoresis (CZE) assay method for that combination. The effects of pH and buffer concentration on resolution, noise, migration time and peak area were examined employing experimental design approach. The analytes were electropherographed into a 50.2 cm-long and 50 µm i.d. fused-silica capillary column using 10 mmol/L borate at pH 8.3 with a potential of 25 kV at 25°C and UV detection at 214 nm. The method was successfully validated in order to verify its suitability for pharmaceutical analysis for the purposes of quality control. Over previous high-performance liquid chromatographic methods, the current CZE method features the benefits of the use of cost-effective electrolyte, besides high sample throughput (11 samples/h). Furthermore, other analytical results including linear dynamic ranges, recovery (96.9-98.1%), intra- and interday precision (relative standard deviation ≤ 1.70%) as well as the limits of detection and quantification (≤2.65 µg/mL) were all satisfactory for the intended purpose. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  14. Performance and Safety Testing of Varta Li-Ion Polymer Cells

    NASA Technical Reports Server (NTRS)

    Patel, Pranav; Jeevarajan, Judith

    2009-01-01

    Varta Cell Characteristics: Voltage : 3.7 V Capacity : 1.21 Ah Dimensions : 5mm X 37mm X 38.5 mm MOSFET switches for Overvoltage and Undervoltage. Initial Screening Results 29 Cells delivered: Statistics on Ph ysical Screening: Thickness (mm): Average- 5.08; Weight(g)- 22.8938; OCV (V)- 3.787; CCV (V)- 3.491.

  15. Determination of parabens in human milk and other food samples by capillary electrophoresis after dispersive liquid-liquid microextraction with back-extraction.

    PubMed

    Alshana, Usama; Ertaş, Nusret; Göğer, Nilgün G

    2015-08-15

    Dispersive liquid-liquid microextraction (DLLME) with back-extraction was used prior to capillary electrophoresis (CE) for the extraction of four parabens. Optimum extraction conditions were: 200 μL chloroform (extraction solvent), 1.0 mL acetonitrile (disperser solvent) and 1 min extraction time. Back-extraction of parabens from chloroform into a 50mM sodium hydroxide solution within 10s facilitated their direct injection into CE. The analytes were separated at 12°C and 25 kV with a background electrolyte of 25 mM borate buffer containing 5.0% (v/v) acetonitrile. Enrichment factors were in the range of 4.3-10.7 and limits of detection ranged from 0.1 to 0.2 μg mL(-1). Calibration graphs showed good linearity with coefficients of determination (R(2)) higher than 0.9957 and relative standard deviations (%RSDs) lower than 3.5%. DLLME-CE was demonstrated to be a simple and rapid method for the determination of parabens in human milk and food with relative recoveries in the range of 86.7-103.3%. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. The 2-Aminoethylphosphonate-Specific Transaminase of the 2-Aminoethylphosphonate Degradation Pathway

    PubMed Central

    Kim, Alexander D.; Baker, Angela S.; Dunaway-Mariano, Debra; Metcalf, W. W.; Wanner, B. L.; Martin, Brian M.

    2002-01-01

    The 2-aminoethylphosphonate transaminase (AEPT; the phnW gene product) of the Salmonella enterica serovar Typhimurium 2-aminoethylphosphonate (AEP) degradation pathway catalyzes the reversible reaction of AEP and pyruvate to form phosphonoacetaldehyde (P-Ald) and l-alanine (l-Ala). Here, we describe the purification and characterization of recombinant AEPT. pH rate profiles (log Vm and log Vm/Km versus pH) revealed a pH optimum of 8.5. At pH 8.5, Keq is equal to 0.5 and the kcat values of the forward and reverse reactions are 7 and 9 s−1, respectively. The Km for AEP is 1.11 ± 0.03 mM; for pyruvate it is 0.15 ± 0.02 mM, for P-Ald it is 0.09 ± 0.01 mM, and for l-Ala it is 1.4 ± 0.03 mM. Substrate specificity tests revealed a high degree of discrimination, indicating a singular physiological role for the transaminase in AEP degradation. The 40-kDa subunit of the homodimeric enzyme is homologous to other members of the pyridoxalphosphate-dependent amino acid transaminase superfamily. Catalytic residues conserved within well-characterized members are also conserved within the seven known AEPT sequences. Site-directed mutagenesis demonstrated the importance of three selected residues (Asp168, Lys194, and Arg340) in AEPT catalysis. PMID:12107130

  17. Elucidation of the mechanism of enzymatic browning inhibition by sodium chlorite.

    PubMed

    He, Qiang; Luo, Yaguang; Chen, Pei

    2008-10-15

    Sodium chlorite (SC) is a well known anti-microbial agent and its strong inhibitory effect on enzymatic browning of fresh-cut produce has recently been identified. We investigated the effect of SC on polyphenol oxidase (PPO) and its substrate, chlorogenic acid (CA), as it relates to the mechanisms of browning inhibition by SC. Results indicate that the browning reaction of CA (1.0mM) catalyzed by PPO (33U/mL) was significantly inhibited by 1.0mM SC at pH 4.6. Two PPO isoforms were identified by native polyacrylamide gel electrophoresis, and both were inactivated by SC (3.0mM). This suggests that SC serves as a PPO inhibitor to prevent enzymatic browning. Furthermore, the effect of SC on the stability of CA in both acidic (pH 4.5) and basic conditions (pH 8.3) was studied by UV-Vis scan and LC-MS analysis. The results showed that at the presence of SC (3.0mM), CA (0.1mM) degraded to quinic acid and caffeic acid as well as other intermediates. Hence, the anti-browning property of SC can be attributed to the two modes of action: the inactivation of polyphenol oxidase directly and the oxidative degradation of phenolic substrates. Published by Elsevier Ltd.

  18. Can Adverse Effects of Acidity and Aluminum Toxicity Be Alleviated by Appropriate Rootstock Selection in Cucumber?

    PubMed Central

    Rouphael, Youssef; Rea, Elvira; Cardarelli, Mariateresa; Bitterlich, Michael; Schwarz, Dietmar; Colla, Giuseppe

    2016-01-01

    Low-pH and aluminum (Al) stresses are the major constraints that limit crop yield in acidic soils. Grafting vegetable elite cultivars onto appropriate rootstocks may represent an effective tool to improve crop tolerance to acidity and Al toxicity. Two greenhouse hydroponic experiments were performed to evaluate growth, yield, biomass production, chlorophyll index, electrolyte leakage, mineral composition, and assimilate partitioning in plant tissues of cucumber plants (Cucumis sativus L. “Ekron”) either non-grafted or grafted onto “P360” (Cucurbita maxima Duchesne × Cucurbita moschata Duchesne; E/C) or figleaf gourd (Cucurbita ficifolia Bouché; E/F). Cucumber plants were cultured in pots and supplied with nutrient solutions having different pH and Al concentrations: pH 6, pH 3.5, pH 3.5 + 1.5 mM Al, and pH 3.5 + 3 mM Al (Experiment 1, 14 days) and pH 6, pH 3.5, and pH 3.5 + 0.75 mM Al (Experiment 2, 67 days). Significant depression in shoot and root biomass was observed in response to acidity and Al concentrations, with Al-stress being more phytotoxic than low pH treatment. Significant decrease in yield, shoot, and root biomass, leaf area, SPAD index, N, K, Ca, Mg, Mn, and B concentration in aerial parts (leaves and stems) in response to low pH with more detrimental effects at pH 3.5 + Al. Grafted E/C plants grown under low pH and Al had higher yield, shoot, and root biomass compared to E/F and non-grafted plants. This better crop performance of E/C plants in response to Al stress was related to (i) a reduced translocation of Al from roots to the shoot, (ii) a better shoot and root nutritional status in K, Ca, Mg, Mn, and Zn concentration, (iii) a higher chlorophyll synthesis, as well as (iv) the ability to maintain cell membrane stability and integrity (lower electrolyte leakage). Data provide insight into the role of grafting on Al stress tolerance in cucumber. PMID:27621740

  19. Casein maps: Effect of ethanol, pH, temperature, and CaCl2 on the particle size of reconstituted casein micelles

    PubMed Central

    Ye, Ran; Harte, Federico

    2015-01-01

    Although conditions favoring casein micelle aggregation are well known, factors promoting the dissociation of the casein micelle are not fully understood. It was our objective to investigate the ethanol-induced dissociation of micellar casein as affected by temperature and a wide range of pH, along with the concentrations of calcium and casein. Two different concentrations of casein micelles were dispersed in imidazole buffer with 0 to 80% ethanol (vol/vol) and 2 and 10 mM calcium. Apparent micelle size was determined by dynamic light scattering at 5, 30, and 60°C. In the absence of ethanol, casein precipitation occurred at pH 4.6 in imidazole buffer. Ten to forty percent ethanol promoted casein aggregation (>1,000 nm) and higher temperature (30 and 60°C) enhanced this effect. Higher ethanol concentrations at 50 to 80% induced the dissociation (<40 nm) of the casein micelle upon acidification (pH <5) and alkalization (pH >8) in imidazole buffer. In addition, higher concentrations of casein (0.25 mg/mL) and calcium (20 mM) caused the formation of larger aggregates (>1,000 nm) in the presence of ethanol when comparing with the initial lower concentrations of casein (0.1 mg/mL) and calcium (2 mM). Casein micelle dissociation can be achieved near the isoelectric pH by modifying the solvent composition and temperature. PMID:23200467

  20. Casein maps: effect of ethanol, pH, temperature, and CaCl2 on the particle size of reconstituted casein micelles.

    PubMed

    Ye, Ran; Harte, Federico

    2013-02-01

    Although conditions favoring casein micelle aggregation are well known, factors promoting the dissociation of the casein micelle are not fully understood. It was our objective to investigate the ethanol-induced dissociation of micellar casein as affected by temperature and a wide range of pH, along with the concentrations of calcium and casein. Two different concentrations of casein micelles were dispersed in imidazole buffer with 0 to 80% ethanol (vol/vol) and 2 and 10mM calcium. Apparent micelle size was determined by dynamic light scattering at 5, 30, and 60°C. In the absence of ethanol, casein precipitation occurred at pH 4.6 in imidazole buffer. Ten to forty percent ethanol promoted casein aggregation (>1,000 nm) and higher temperature (30 and 60°C) enhanced this effect. Higher ethanol concentrations at 50 to 80% induced the dissociation (<40 nm) of the casein micelle upon acidification (pH <5) and alkalization (pH>8) in imidazole buffer. In addition, higher concentrations of casein (0.25mg/mL) and calcium (20mM) caused the formation of larger aggregates (>1,000 nm) in the presence of ethanol when comparing with the initial lower concentrations of casein (0.1mg/mL) and calcium (2mM). Casein micelle dissociation can be achieved near the isoelectric pH by modifying the solvent composition and temperature. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

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