Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

PubMed

Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

2016-05-15

A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. Copyright © 2016 Elsevier B.V. All rights reserved.

Headspace sorptive extraction-gas chromatography-mass spectrometry method to measure volatile emissions from human airway cell cultures.

PubMed

Yamaguchi, Mei S; McCartney, Mitchell M; Linderholm, Angela L; Ebeler, Susan E; Schivo, Michael; Davis, Cristina E

2018-05-12

The human respiratory tract releases volatile metabolites into exhaled breath that can be utilized for noninvasive health diagnostics. To understand the origin of this metabolic process, our group has previously analyzed the headspace above human epithelial cell cultures using solid phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS). In the present work, we improve our model by employing sorbent-covered magnetic stir bars for headspace sorptive extraction (HSSE). Sorbent-coated stir bar analyte recovery increased by 52 times and captured 97 more compounds than SPME. Our data show that HSSE is preferred over liquid extraction via stir bar sorptive extraction (SBSE), which failed to distinguish volatiles unique to the cell samples compared against media controls. Two different cellular media were also compared, and we found that Opti-MEM® is preferred for volatile analysis. We optimized HSSE analytical parameters such as extraction time (24 h), desorption temperature (300 °C) and desorption time (7 min). Finally, we developed an internal standard for cell culture VOC studies by introducing 842 ng of deuterated decane per 5 mL of cell medium to account for error from extraction, desorption, chromatography and detection. This improved model will serve as a platform for future metabolic cell culture studies to examine changes in epithelial VOCs caused by perturbations such as viral or bacterial infections, opening opportunities for improved, noninvasive pulmonary diagnostics. Copyright © 2018 Elsevier B.V. All rights reserved.

Fabric phase sorptive extraction: Two practical sample pretreatment techniques for brominated flame retardants in water.

PubMed

Huang, Guiqi; Dong, Sheying; Zhang, Mengfei; Zhang, Haihan; Huang, Tinglin

2016-09-15

Sample pretreatment is the critical section for residue monitoring of hazardous pollutants. In this paper, using the cellulose fabric as host matrix, three extraction sorbents such as poly (tetrahydrofuran) (PTHF), poly (ethylene glycol) (PEG) and poly (dimethyldiphenylsiloxane) (PDMDPS), were prepared on the surface of the cellulose fabric. Two practical extraction techniques including stir bar fabric phase sorptive extraction (stir bar-FPSE) and magnetic stir fabric phase sorptive extraction (magnetic stir-FPSE) have been designed, which allow stirring of fabric phase sorbent during the whole extraction process. In the meantime, three brominated flame retardants (BFRs) [tetrabromobisphenol A (TBBPA), tetrabromobisphenol A bisallylether (TBBPA-BAE), tetrabromobisphenol A bis(2,3-dibromopropyl)ether (TBBPA-BDBPE)] in the water sample were selected as model analytes for the practical evaluation of the proposed two techniques using high-performance liquid chromatography (HPLC). Moreover, various experimental conditions affecting extraction process such as the type of fabric phase, extraction time, the amount of salt and elution conditions were also investigated. Due to the large sorbent loading capacity and unique stirring performance, both techniques possessed high extraction capability and fast extraction equilibrium. Under the optimized conditions, high recoveries (90-99%) and low limits of detection (LODs) (0.01-0.05 μg L(-1)) were achieved. In addition, the reproducibility was obtained by evaluating the intraday and interday precisions with relative standard deviations (RSDs) less than 5.1% and 6.8%, respectively. The results indicated that two pretreatment techniques were promising and practical for monitoring of hazardous pollutants in the water sample. Due to low solvent consumption and high repeated use performance, proposed techniques also could meet green analytical criteria. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of ultraviolet filters in bathing waters by stir bar sorptive-dispersive microextraction coupled to thermal desorption-gas chromatography-mass spectrometry.

PubMed

Benedé, Juan L; Chisvert, Alberto; Giokas, Dimosthenis L; Salvador, Amparo

2016-01-15

In this work, a new approach that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive solid phase extraction (DSPE), i.e. stir bar sorptive-dispersive microextraction (SBSDµE), is employed as enrichment and clean-up technique for the sensitive determination of eight lipophilic UV filters in water samples. The extraction is accomplished using a neodymium stir bar magnetically coated with oleic acid-coated cobalt ferrite magnetic nanoparticles (MNPs) as sorbent material, which are detached and dispersed into the solution at high stirring rate. When stirring is stopped, MNPs are magnetically retrieved onto the stir bar, which is subjected to thermal desorption (TD) to release the analytes into the gas chromatography-mass spectrometry (GC-MS) system. The SBSDµE approach allows for lower extraction time than SBSE and easier post-extraction treatment than DSPE, while TD allows for an effective and solvent-free injection of the entire quantity of desorbed analytes into GC-MS, and thus achieving a high sensitivity. The main parameters involved in TD, as well as the extraction time, were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ngL(-1) range and good intra- and inter-day repeatability (RSD<12%). This accurate and sensitive analytical method was applied to the determination of trace amounts of UV filters in three bathing water samples (river, sea and swimming pool) with satisfactory relative recovery values (80-116%). Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of steroid sex hormones in wastewater by stir bar sorptive extraction based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material and liquid chromatographic analysis.

PubMed

Huang, Xiaojia; Lin, Jianbin; Yuan, Dongxing; Hu, Rongzong

2009-04-17

In this study, a simple and rapid method was developed for the determination of seven steroid hormones in wastewater. Sample preparation and analysis were performed by stir bar sorptive extraction (SBSE) based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material (SBSEM) combined with high-performance liquid chromatography with diode array detection. To achieve the optimum extraction performance, several main parameters, including extraction and desorption time, pH value and contents of inorganic salt in the sample matrix, were investigated. Under the optimized experimental conditions, the method showed good linearity and repeatability, as well as advantages such as sensitivity, simplicity, low cost and high feasibility. The extraction performance of SBSEM to the target compounds also compared with commercial SBSE which used polydimethylsiloxane as coating. Finally, the proposed method was successfully applied to the determination of the target compounds in wastewater samples. The recoveries of spiked target compounds in real samples ranged from 48.2% to 110%.

Determination of phenylurea herbicides in water samples using online sorptive preconcentration and high-performance liquid chromatography with UV or electrospray mass spectrometric detection.

PubMed

Baltussen, E; Snijders, H; Janssen, H G; Sandra, P; Cramers, C A

1998-04-10

A recently developed method for the extraction of organic micropollutants from aqueous samples based on sorptive enrichment in columns packed with 100% polydimethylsiloxane (PDMS) particles was coupled on-line with HPLC analysis. The sorptive enrichment procedure originally developed for relatively nonpolar analytes was used to preconcentrate polar phenylurea herbicides from aqueous samples. PDMS extraction columns of 5, 10 and 25 cm were used to extract the herbicides from distilled, tap and river water samples. A model that allows prediction of retention and breakthrough volumes is presented. Despite the essentially apolar nature of the PDMS material, it is possible to concentrate sample volumes up to 10 ml on PDMS cartridges without losses of the most polar analyte under investigation, fenuron. For less polar analytes significantly larger sample volumes can be applied. Since standard UV detection does not provide adequate selectivity for river water samples, an electrospray (ES)-MS instrument was used to determine phenylurea herbicides in a water sample from the river Dommel. Methoxuron was present at a level of 80 ng/l. The detection limit of the current set-up, using 10 ml water samples and ES-MS detection is 10 ng/l in river water samples. Strategies for further improvement of the detection limits are identified.

Integrated sampling and analysis unit for the determination of sexual pheromones in environmental air using fabric phase sorptive extraction and headspace-gas chromatography-mass spectrometry.

PubMed

Alcudia-León, M Carmen; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

2017-03-10

This article presents a novel unit that integrates for the first time air sampling and preconcentration based on the use of fabric phase sorptive extraction principles. The determination of Tuta absoluta sexual pheromone traces in environmental air has been selected as analytical problem. For this aim, a novel laboratory-built unit made up of commercial brass elements as holder of the sol-gel coated fabric extracting phase has been designed and optimized. The performance of the integrated unit was evaluated analyzing environmental air sampled in tomato crops. The unit can work under sampling and analysis mode which eliminates any need for sorptive phase manipulation prior to instrumental analysis. In the sampling mode, the unit can be connected to a sampling pump to pass the air through the sorptive phase at a controlled flow-rate. In the analysis mode, it is placed in the gas chromatograph autosampler without any instrumental modification. It also diminishes the risk of cross contamination between sampling and analysis. The performance of the new unit has been evaluated using the main components of the sexual pheromone of Tuta absoluta [(3E,8Z,11Z)-tetradecatrien-1-yl acetate and (3E,8Z)-tetradecadien-1-yl acetate] as model analytes. The limits of detection for both compounds resulted to be 1.6μg and 0.8μg, respectively, while the precision (expressed as relative standard deviation) was better than 3.7%. Finally, the unit has been deployed in the field to analyze a number of real life samples, some of them were found positive. Copyright © 2017 Elsevier B.V. All rights reserved.

Do complex matrices modify the sorptive properties of polydimethylsiloxane (PDMS) for non-polar organic chemicals?

PubMed

Jahnke, Annika; Mayer, Philipp

2010-07-16

The partitioning of non-polar analytes into the silicone polydimethylsiloxane (PDMS) is the basis for many analytical approaches such as solid phase microextraction (SPME), stir bar sorptive extraction (SBSE) and environmental passive sampling. Recently, the methods have been applied to increasingly complex sample matrices. The present work investigated the possible effect of complex matrices on the sorptive properties of PDMS. First, SPME fibers with a 30 microm PDMS coating were immersed in 15 different matrices, including sediment, suspensions of soil and humic substances, mayonnaise, meat, fish, olive oil and fish oil. Second, the surface of the fibers was wiped clean, and together with matrix-free control fibers, they were exposed via headspace to 7 non-polar halogenated organic chemicals in spiked olive oil. The fibers were then solvent-extracted, analyzed, and the ratios of the mean concentrations in the matrix-immersed fibers to the control fibers were determined for all matrices. These ratios ranged from 92% to 112% for the four analytes with the highest analytical precision (i.e. polychlorinated biphenyls (PCBs) 3, 28, 52 and brominated diphenyl ether (BDE) 3), and they ranged from 74% to 133% for the other three compounds (i.e. PCBs 101, 105 and gamma-hexachlorocyclohexane (HCH)). We conclude that, for non-polar, hydrophobic chemicals, the sorptive properties of the PDMS were not modified by the diverse investigated media and consequently that PDMS is suited for sampling of these analytes even in highly complex matrices. 2010 Elsevier B.V. All rights reserved.

Preparation of a polar monolithic stir bar based on methacrylic acid and divinylbenzene for the sorptive extraction of polar pharmaceuticals from complex water samples.

PubMed

Bratkowska, D; Fontanals, N; Cormack, P A G; Borrull, F; Marcé, R M

2012-02-17

A monolithic, hydrophilic stir bar coating based upon a copolymer of methacrylic acid and divinylbenzene [poly(MAA-co-DVB)] was synthesised and evaluated as a new polymeric phase for the stir bar sorptive extraction (SBSE) of polar compounds from complex environmental water samples. The experimental conditions for the extraction and liquid desorption in SBSE were optimised. Liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was used for the determination of a group of polar pharmaceuticals in environmental water matrices. The extraction performance of the poly(MAA-co-DVB) stir bar was compared to the extraction performance of a commercially available polydimethylsiloxane stir bar; it was found that the former gave rise to significantly higher extraction efficiency of polar analytes (% recovery values near to 100% for most of the studied analytes) than the commercial product. The developed method was applied to determine the studied analytes at low ng L⁻¹ in different complex environmental water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Use of headspace sorptive extraction coupled to gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in herbal infusions.

PubMed

Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

2014-08-22

A solvent-free method is described for the determination of 10 volatile polycyclic aromatic hydrocarbons (PAHs), considered as priority pollutants by the EU, in different herbal infusions using headspace sorptive extraction (HSSE) and gas chromatography-mass spectrometry (GC-MS). The parameters affecting both the extraction and thermal desorption steps in the HSSE were optimized by means of Plackett-Burman designs. Ten millilitres of the herbal infusion was submitted to the HSSE preconcentration in the presence of salt for 4h at 88 °C. The use of d(10)-phenanthrene as internal standard not only improved the repeatability of the method but allowed quantification of the samples against external aqueous standards. Detection limits ranged between 11 and 26 ng L(-1). Copyright © 2014 Elsevier B.V. All rights reserved.

GC-MS determination of parabens, triclosan and methyl triclosan in water by in situ derivatisation and stir-bar sorptive extraction.

PubMed

Casas Ferreira, Ana María; Möder, Monika; Fernández Laespada, María Esther

2011-01-01

Stir-bar sorptive extraction in combination with an in situ derivatisation reaction and thermal desorption-gas chromatography-mass spectrometry was successfully applied to determine parabens (methylparaben, isopropylparaben, n-propylparaben, butylparaben and benzylparaben), triclosan and methyltriclosan in water samples. This approach improves both the extraction efficiency and the sensitivity in the GC in a simple way since the derivatisation reaction occurs at the same time as the extraction procedure. The in situ derivatisation reaction was carried out with acetic anhydride under alkaline conditions. Thermal desorption parameters (cryofocusing temperature, desorption flow, desorption time, desorption temperature) were optimised using a Box-Behnken experimental design. All the analytes gave recoveries higher than 79%, except methylparaben (22%). The method afforded detection limits between 0.64 and 4.12 ng/L, with good reproducibility and accuracy values. The feasibility of the method for the determination of analytes in water samples was checked in tap water and untreated and treated wastewater.

Determination of Carvedilol Enantiomers in Pharmaceutical Dosages by SBSE-HPLC Based on Diastereomer Formation.

PubMed

Taraji, Maryam; Talebpour, Zahra; Adib, Nuoshin; Karimi, Shima; Haghighi, Farideh; Aboul-Enein, Hassan Y

2015-09-01

A sensitive, selective and simple method for the simultaneous determination of carvedilol enantiomers in aqueous solution has been developed using stir bar sorptive extraction (SBSE) followed by high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection. This method is based on the reaction of carvedilol enantiomers with (-)-menthyl chloroformate (MCF) after extraction by the SBSE method to produce diastereomeric derivatives. The separation was achieved by use of a C18 analytical column and the influence of mobile phase composition on the enantioseparation of carvedilol was studied. The applicability of two sorptive phases, poly(methyl methacrylate/ethyleneglycol dimethacrylate) (PA-EG) and polydimethylsiloxane, were tested for extraction of carvedilol enantiomers from aqueous samples. The obtained results showed excellent linear dynamic ranges and precisions for each of them. The least limit of detection for (S)- and (R)-carvedilol obtained 8 and 11 µg L(-1), respectively, using the PA-EG sorptive phase. Inter- and intra-mean recoveries were also satisfactory, ranging from 98 to 103%, with coefficient of variation in the range of 1-5% at three fortified levels using a PA-EG coated stir bar. The proposed SBSE (PA-EG)-MCF derivatization-HPLC-UV method was successfully applied to enantioselective analysis of carvedilol in water and pharmaceutical dosages, confirming the application of this method. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC-MS/MS method for methoxypyrazine analysis in wine.

PubMed

Hjelmeland, Anna K; Wylie, Philip L; Ebeler, Susan E

2016-02-01

Methoxypyrazines are volatile compounds found in plants, microbes, and insects that have potent vegetal and earthy aromas. With sensory detection thresholds in the low ng L(-1) range, modest concentrations of these compounds can profoundly impact the aroma quality of foods and beverages, and high levels can lead to consumer rejection. The wine industry routinely analyzes the most prevalent methoxypyrazine, 2-isobutyl-3-methoxypyrazine (IBMP), to aid in harvest decisions, since concentrations decrease during berry ripening. In addition to IBMP, three other methoxypyrazines IPMP (2-isopropyl-3-methoxypyrazine), SBMP (2-sec-butyl-3-methoxypyrazine), and EMP (2-ethyl-3-methoxypyrazine) have been identified in grapes and/or wine and can impact aroma quality. Despite their routine analysis in the wine industry (mostly IBMP), accurate methoxypyrazine quantitation is hindered by two major challenges: sensitivity and resolution. With extremely low sensory detection thresholds (~8-15 ng L(-1) in wine for IBMP), highly sensitive analytical methods to quantify methoxypyrazines at trace levels are necessary. Here we were able to achieve resolution of IBMP as well as IPMP, EMP, and SBMP from co-eluting compounds using one-dimensional chromatography coupled to positive chemical ionization tandem mass spectrometry. Three extraction techniques HS-SPME (headspace-solid phase microextraction), SBSE (stirbar sorptive extraction), and HSSE (headspace sorptive extraction) were validated and compared. A 30 min extraction time was used for HS-SPME and SBSE extraction techniques, while 120 min was necessary to achieve sufficient sensitivity for HSSE extractions. All extraction methods have limits of quantitation (LOQ) at or below 1 ng L(-1) for all four methoxypyrazines analyzed, i.e., LOQ's at or below reported sensory detection limits in wine. The method is high throughput, with resolution of all compounds possible with a relatively rapid 27 min GC oven program. Copyright © 2015 Elsevier B.V. All rights reserved.

Fabric phase sorptive extraction of selected penicillin antibiotic residues from intact milk followed by high performance liquid chromatography with diode array detection.

PubMed

Samanidou, Victoria; Michaelidou, Katia; Kabir, Abuzar; Furton, Kenneth G

2017-06-01

Fabric phase sorptive extraction (FPSE), a novel sorbent-based microextraction method, was evaluated as a simple and rapid strategy for the extraction of four penicillin antibiotic residues (benzylpenicillin, cloxacillin, dicloxacillin and oxacillin) from cows' milk, without prior protein precipitation. Time-consuming solvent evaporation and reconstitution steps were eliminated successfully from the sample preparation workflow. FPSE utilizes a flexible fabric substrate, chemically coated with sol-gel derived, highly efficient, organic-inorganic hybrid sorbent as the extraction medium. Herein short-chain poly(ethylene glycol) provided optimum extraction sensitivity for the selected penicillins, which were analysed using an RP-HPLC method, validated according to the European Decision 657/2002/EC. The limit of quantitation was 10μg/kg for benzylpenicillin, 20μg/kg for cloxacillin, 25μg/kg dicloxacillin and 30μg/kg oxacillin. These are a similar order of magnitude with those reported in the literature and (with the exception of benzylpenicillin) are less than the maximum residue limits (MRL) set by European legislation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Development of monolith-based stir bar sorptive extraction and liquid chromatography tandem mass spectrometry method for sensitive determination of ten sulfonamides in pork and chicken samples.

PubMed

Huang, Xiaojia; Chen, Linli; Yuan, Dongxing

2013-08-01

A highly sensitive method was developed for the simultaneous determination of ten sulfonamides in pork and chicken samples by monolith-based stir bar sorptive extraction (SBSE) coupled to high-performance liquid chromatography tandem mass spectrometry. The samples were freeze-dried and extracted by acetonitrile, then enriched and further extracted by SBSE which was based on poly(vinylphthalimide-co-N,N-methylenebisacrylamide) monolith (SBSE-VPMB) as coating. To achieve optimum extraction performance of SBSE for sulfonamides, several parameters, including pH value and ionic strength in the sample matrix and extraction and desorption time, were investigated in detail. Under the optimal conditions, the limits of detection (S/N = 3) for target sulfonamides were 1.2-6.1 ng/kg in pork and 2.0-14.6 ng/kg in chicken, respectively. Real samples spiked at the concentration of 0.5 and 5.0 μg/kg showed recoveries above 55% and relative standard deviations below 12%. At the same time, the extraction performances of target sulfonamides on SBSE-VPMB were compared with other SBSE based on porous monolith and commercial SBSE.

C18-coated stir bar sorptive extraction combined with high performance liquid chromatography-electrospray tandem mass spectrometry for the analysis of sulfonamides in milk and milk powder.

PubMed

Yu, Chunhe; Hu, Bin

2012-02-15

A simple, rapid, sensitive, inexpensive and less sample consuming method of C(18)-stir bar sorptive extraction (SBSE)-high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) was proposed for the determination of six sulfonamides in milk and milk powder samples. C(18) silica particles coated stir bar was prepared by adhesion method, and two kinds of adhesive glue, polydimethylsiloxane (PDMS) sol and epoxy glue were tried. It was found that the C(18)-coated stir bar prepared by PDMS sol as adhesive glue is more robust than that prepared by epoxy glue when liquid desorption was employed, in terms of both lifetime and organic solvent tolerance. The preparation of C(18) stir bar was simple with good mechanic strength and the stir bar could be reused for more than 20 times. Granular coating has relatively high specific surface area and is propitious to sorptive extraction based process. Compared to conventional PDMS SBSE coating, C(18) coating shows good affinity to the target polar/weak polar sulfonamides. To achieve optimum SBSE extraction performance, several parameters including extraction and desorption time, ionic strength, sample pH and stirring speed were investigated. The detection limits of the proposed method for six sulfonamides were in the range of 0.9-10.5 μg/L for milk and 2.7-31.5 μg/kg for milk powder. Good linearities were obtained for sulfonamides with the correlation coefficients (R) above 0.9922. Finally, the proposed method was successfully applied to the determination of sulfonamides in milk and milk powder samples and satisfied recoveries of spiked target compounds in real samples were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

Polytetrafluoroethylene-jacketed stirrer modified with graphene oxide and polydopamine for the efficient extraction of polycyclic aromatic hydrocarbons.

PubMed

Zhang, Zinxin; Mwadini, Mwadini Ahmada; Chen, Zilin

2016-10-01

Steel stirrers jacketed with polytetrafluoroethylene can be regarded as an ideal substrate for stirrer bar sorptive extraction. However, it is still a great challenge to immobilize graphene onto a polytetrafluoroethylene stirrer due to the high chemical resistance of the surface of a polytetrafluoroethylene stirrer. We describe here a method to modify the surface of polytetrafluoroethylene stirrers with graphene. In this work, graphene was used as the sorbent due to its excellent adsorption capability for aromatic compounds, such as polycyclic aromatic compounds. Graphene was successfully immobilized onto polytetrafluoroethylene-stirrer by a bio-inspired polydopamine functionalization method. The graphene-modified polytetrafluoroethylene-stirrer shows good stability and tolerance to stirring, ultrasonication, strong acidic and basic solutions, and to organic solvents. The multilayer coating was characterized by scanning electronic microscopy and Fourier transform infrared spectroscopy. After the optimization of some experimental conditions, the graphene-modified polytetrafluoroethylene stirrer was used for the stirrer bar sorptive extraction of polycyclic aromatic hydrocarbons, in which the binding between the polycyclic aromatic hydrocarbons and the graphene layer was mainly based on π-π stacking and hydrophobic interactions. The graphene-modified polytetrafluoroethylene-stirrer-based stirrer bar sorptive extraction and high-performance liquid chromatography method was developed for the determination of polycyclic aromatic hydrocarbons with great extraction efficiency, with enrichment factors from 18 to 62. The method has low limits of detection of 1-5 pg/mL, wide linear range (5-100 and 10-200 pg/mL), good linearity (R ≥ 0.9957) and good reproducibility (RSD ≤ 6.45%). The proposed method has been applied to determine polycyclic aromatic hydrocarbons in real dust samples. Good recoveries were obtained, ranging from 88.53 to 109.43%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development and application of stir bar sorptive extraction with polyurethane foams for the determination of testosterone and methenolone in urine matrices.

PubMed

Sequeiros, R C P; Neng, N R; Portugal, F C M; Pinto, M L; Pires, J; Nogueira, J M F

2011-04-01

This work describes the development, validation, and application of a novel methodology for the determination of testosterone and methenolone in urine matrices by stir bar sorptive extraction using polyurethane foams [SBSE(PU)] followed by liquid desorption and high-performance liquid chromatography with diode array detection. The methodology was optimized in terms of extraction time, agitation speed, pH, ionic strength and organic modifier, as well as back-extraction solvent and desorption time. Under optimized experimental conditions, convenient accuracy were achieved with average recoveries of 49.7 8.6% for testosterone and 54.2 ± 4.7% for methenolone. Additionally, the methodology showed good precision (<9%), excellent linear dynamic ranges (>0.9963) and convenient detection limits (0.2-0.3 μg/L). When comparing the efficiency obtained by SBSE(PU) and with the conventional polydimethylsiloxane phase [SBSE(PDMS)], yields up to four-fold higher are attained for the former, under the same experimental conditions. The application of the proposed methodology for the analysis of testosterone and methenolone in urine matrices showed negligible matrix effects and good analytical performance.

Chiral imprinted polymers as enantiospecific coatings of stir bar sorptive extraction devices.

PubMed

Gomez-Caballero, Alberto; Guerreiro, Antonio; Karim, Kal; Piletsky, Sergey; Goicolea, M Aranzazu; Barrio, Ramon J

2011-10-15

This paper reports the design of Molecularly Imprinted Polymers (MIP) with affinity towards (S)-citalopram using computational modeling for the selection of functional monomers and monomer:template ratio. Acrylamide was selected as functional monomer and the final complex functional monomer/template resulted in a 3:1 ratio. The polymer was synthesized by radical polymerization initiated by UV onto magnetic stir-bars in order to obtain a stir bar sorptive extraction (SBSE) device capable of selective enantiomeric recognition. After successful template removal, the parameters affecting the SBSE procedure (sample volume, ionic strength, extraction time and pH) were optimized for the effective rebinding of the target analyte. The resultant chirally imprinted polymer based stir-bar was able to selectively extract (S)-citalopram from a racemic mixture in an aqueous media with high specificity (specificity factor 4) between 25 and 500 μgL(-1). The MIP coated stir-bars can have significance for enantiospecific sample pre-concentration and subsequent analysis without the need for any chiral chromatographic separation. Copyright © 2011 Elsevier B.V. All rights reserved.

Graphene oxide-coated stir bar sorptive extraction of trace aflatoxins from soy milk followed by high performance liquid chromatography-laser-induced fluorescence detection.

PubMed

Ma, Haiyan; Ran, Congcong; Li, Mengjiao; Gao, Jinglin; Wang, Xinyu; Zhang, Lina; Bian, Jing; Li, Junmei; Jiang, Ye

2018-04-01

Mycotoxins are potential food pollutants produced by fungi. Among them, aflatoxins (AFs) are the most toxic. Therefore, AFs were selected as models, and a sensitive, simple and green graphene oxide (GO)-based stir bar sorptive extraction (SBSE) method was developed for extraction and determination of AFs with high performance liquid chromatography-laser-induced fluorescence detector (HPLC-LIF). This method improved the sensitivity of AFs detection and solved the deposition difficulty of the direct use of GO as adsorbent. Several parameters including a spiked amount of NaCl, stirring rate, extraction time and desorption time were investigated. Under optimal conditions, the quantitative method had low limits of detection of 2.4-8.0 pg/mL, which were better than some reported AFs analytical methods. The developed method has been applied to soy milk samples with good recoveries ranging from 80.5 to 102.3%. The prepared GO-based SBSE can be used as a sensitive screening technique for detecting AFs in soy milk.

A novel sorptive extraction method based on polydimethylsiloxane frit for determination of lung cancer biomarkers in human serum.

PubMed

Xu, Hui; Wang, Shuyu

2012-04-29

In this study, a porous polypropylene frit was coated with polydimethylsiloxane (PDMS) as extraction medium, based on the home-made PDMS-frit, a rapid, simple and sensitive sorptive extraction method was established for analysis of potential biomarkers of lung cancer (hexanal and heptanal) in human serum samples. In the method, derivatization and extraction occurred simultaneously on the PDMS-frit, then the loaded frit was ultrasonically desorbed in acetonitrile. Polymerization, derivatization-extraction and desorption conditions were optimized. Under the optimal conditions, satisfactory results were gained, a wide linear application range was obtained in the range of 0.002-5.0 μmol L(-1) (R>0.997) for two aldehydes, the detection limits (SN(-1)=3) were 0.5 nmol L(-1) for hexanal and 0.4 nmol L(-1) for heptanal. The relative standard deviations (RSDs, n=5) of the method were below 7.9% and the recoveries were above 72.7% for the spiked serum. All these results hint that the proposed method is potential for disease markers analysis in complex biological samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Quantitative 31P NMR for Simultaneous Trace Analysis of Organophosphorus Pesticides in Aqueous Media Using the Stir Bar Sorptive Extraction Method

NASA Astrophysics Data System (ADS)

Ansari, S.; Talebpour, Z.; Molaabasi, F.; Bijanzadeh, H. R.; Khazaeli, S.

2016-09-01

The analysis of pesticides in water samples is of primary concern for quality control laboratories due to the toxicity of these compounds and their associated public health risk. A novel analytical method based on stir bar sorptive extraction (SBSE), followed by 31P quantitative nuclear magnetic resonance (31P QNMR), has been developed for simultaneously monitoring and determining four organophosphorus pesticides (OPPs) in aqueous media. The effects of factors on the extraction efficiency of OPPs were investigated using a Draper-Lin small composite design. An optimal sample volume of 4.2 mL, extraction time of 96 min, extraction temperature of 42°C, and desorption time of 11 min were obtained. The results showed reasonable linearity ranges for all pesticides with correlation coefficients greater than 0.9920. The limit of quantification (LOQ) ranged from 0.1 to 2.60 mg/L, and the recoveries of spiked river water samples were from 82 to 94% with relative standard deviation (RSD) values less than 4%. The results show that this method is simple, selective, rapid, and can be applied to other sample matrices.

Rapid monitoring of residual UV-stabilizers in seawater samples from beaches using fabric phase sorptive extraction and UHPLC-MS/MS.

PubMed

García-Guerra, Romualdo B; Montesdeoca-Esponda, Sarah; Sosa-Ferrera, Zoraida; Kabir, Abuzar; Furton, Kenneth G; Santana-Rodríguez, José Juan

2016-12-01

Benzotriazole UV stabilizers (BUVSs) are a group of compounds added to personal care products such as sunscreens, hair dyes, make up formulations, soaps or shampoos, among others. Direct input from beaches or another aquatic recreational areas is the main source of BUVSs incorporation to the environment, where they can be mutagenic, toxic, pseudo-persistent and bioaccumulative. Due to the low levels of concentration of these compounds found in environmental samples, an extraction process is required prior to their determination. Fabric phase sorptive extraction integrates the advanced material properties of sol-gel hybrid inorganic-organic sorbents with flexible, permeable and functionally active fabric substrates, being a highly responsive, efficient and cheap device that also can be reused. In this paper, we applied fabric phase sorptive extraction methodology to analyse six BUVSs in twenty-four seawater samples from different coastal areas of Gran Canaria Island (Spain). It was coupled to ultra high performance liquid chromatography with tandem mass spectrometry in order to achieve a fast, reliable and sensitive separation and determination of the analytes from different simple matrices, regardless of its complexity and composition. Under the optimum conditions, the proposed method provided enrichment factors of 25 times with limits of detection from 1.06 to 8.96 ng L -1 and limits of quantification from 3.54 to 29.9 ng L -1 for the analytes under study in spiked samples. Intra and inter-day relative standard deviations were between 3.97 and 20.8% for all compounds. The application of the optimized methodology to non-spiked seawater samples allows detecting and quantifying the UV 360 in the range from 41.12 to 544.9 ng L -1 . Copyright © 2016 Elsevier Ltd. All rights reserved.

Characterisation, quantity and sorptive properties of microplastics extracted from cosmetics.

PubMed

Napper, Imogen E; Bakir, Adil; Rowland, Steven J; Thompson, Richard C

2015-10-15

Cosmetic products, such as facial scrubs, have been identified as potentially important primary sources of microplastics to the marine environment. This study characterises, quantifies and then investigates the sorptive properties of plastic microbeads that are used as exfoliants in cosmetics. Polyethylene microbeads were extracted from several products, and shown to have a wide size range (mean diameters between 164 and 327 μm). We estimated that between 4594 and 94,500 microbeads could be released in a single use. To examine the potential for microbeads to accumulate and transport chemicals they were exposed to a binary mixture of (3)H-phenanthrene and (14)C-DDT in seawater. The potential for transport of sorbed chemicals by microbeads was broadly similar to that of polythene (PE) particles used in previous sorption studies. In conclusion, cosmetic exfoliants are a potentially important, yet preventable source of microplastic contamination in the marine environment. Copyright © 2015 Elsevier Ltd. All rights reserved.

Novel coatings for stir bar sorptive extraction to determine pharmaceuticals and personal care products in environmental waters by liquid chromatography and tandem mass spectrometry.

PubMed

Gilart, Núria; Miralles, Núria; Marcé, Rosa Maria; Borrull, Francesc; Fontanals, Núria

2013-04-24

Two new commercially available polar coatings for stir bar sorptive extraction (SBSE), consisting of polyacrylate (PA) with a proportion of polyethyleneglycol (PEG) (Acrylate Twister(®)) and PEG modified silicone (EG Silicone Twister(®)), were evaluated and compared with the classic coating based on polydimethylsiloxane (PDMS Twister(®)) for the extraction of a group of pharmaceuticals and personal care products (PPCPs) from wastewater samples. The SBSE parameters, such as sample pH, agitation speed, extraction temperature, extraction time, desorption solvent and time, were optimised in order to achieve suitable sorption of the target analytes. The EG Silicone coating enabled more efficient extraction of some polar compounds as well as improving the sorption of apolar compounds, in comparison with the other two coatings. Finally, the method of SBSE followed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) using the EG Silicone coating was validated achieving good linearity (r(2)>0.994, except for CBZ (r(2)>0.989)), precision (%RSD<17%) and low limits of quantification (LOQs) (20-40 ng L(-1)). The SBSE/LC-MS/MS methodology was applied for the determination of PPCPs in wastewater samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation a new sorbent based on polymeric ionic liquid for stir cake sorptive extraction of organic compounds and inorganic anions.

PubMed

Huang, Xiaojia; Wang, Yulei; Hong, Qiuyun; Liu, Yi; Yuan, Dongxing

2013-11-01

A new multi-interaction sorbent (MIS) based on polymeric ionic liquid was prepared and used as extractive medium of stir cake sorptive extraction (SCSE). In the presence of dimethyl sulfoxide, an ionic liquid, 1-vinylbenzyl-3-methylimidazolium chloride was used as monomer to copolymerize in situ with divinylbenzene to form the MIS. The influences of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance were investigated thoroughly. The MIS was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. Parabens and aromatic amines were used to investigate the extraction performance of MIS-SCSE for apolar and strongly polar analytes, respectively. The extraction parameters for parabens and aromatic amines were optimized. At the same time, simple and sensitive analytical methods for parabens and aromatic amines in real samples were developed by the combination of MIS-SCSE and HPLC/DAD. Some inorganic anions, such as F(-), Br(-), NO3(-), PO4(3-) and SO4(2-), were used to test the extraction performance of MIS-SCSE for anions. Results indicated that mechanism involved in the extraction of MIS is the multi-interaction modes including π-π, hydrophobic, hydrogen-bonding, dipole-dipole and anion-exchange interactions. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation of a novel sorptive stir bar based on vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer for the simultaneous extraction of diazepam and nordazepam from human plasma.

PubMed

Torabizadeh, Mahsa; Talebpour, Zahra; Adib, Nuoshin; Aboul-Enein, Hassan Y

2016-04-01

A new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The polymerization step was performed using different contents of monomer, cross-linker and porogenic solvent, and the best formulation was selected. The quality of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate stir bars was satisfactory, demonstrating good repeatability within batch (relative standard deviation < 3.5%) and acceptable reproducibility between batches (relative standard deviation < 6.0%). The prepared stir bar was utilized in combination with ultrasound-assisted liquid desorption, followed by high-performance liquid chromatography with ultraviolet detection for the simultaneous determination of diazepam and nordazepam in human plasma samples. To optimize the extraction step, a three-level, four-factor, three-block Box-Behnken design was applied. Under the optimum conditions, the analytical performance of the proposed method displayed excellent linear dynamic ranges for diazepam (36-1200 ng/mL) and nordazepam (25-1200 ng/mL), with correlation coefficients of 0.9986 and 0.9968 and detection limits of 12 and 10 ng/mL, respectively. The intra- and interday recovery ranged from 93 to 106%, and the relative standard deviations were less than 6%. Finally, the proposed method was successfully applied to the analysis of diazepam and nordazepam at their therapeutic levels in human plasma. The novelty of this study is the improved polarity of the stir bar coating and its application for the simultaneous extraction of diazepam and its active metabolite, nordazepam in human plasma sample. The method was more rapid than previously reported stir bar sorptive extraction techniques based on monolithic coatings, and exhibited lower detection limits in comparison with similar methods for the determination of diazepam and nordazepam in biological fluids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validated determination of losartan and valsartan in human plasma by stir bar sorptive extraction based on acrylate monolithic polymer, liquid chromatographic analysis and experimental design methodology.

PubMed

Babarahimi, Vida; Talebpour, Zahra; Haghighi, Farideh; Adib, Nuoshin; Vahidi, Hamed

2018-05-10

In our previous work, a new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The formulation of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer was optimized and the satisfactory quality of prepared coated stir bar was demonstrated. In this work, the prepared stir bar was utilized in combination with ultrasound-assisted liquid desorption, followed by high-performance liquid chromatography with ultraviolet detection for the simultaneous determination of losartan (LOS) and valsartan (VAS) in human plasma samples. In a comparison study, the extraction efficiency of the prepared stir bar was accompanied much higher extraction efficiency than the two commercial stir bars (polydimethylsiloxand and polyacrylate) for both target compounds. In order to improve the desorption efficiency of LOS and VAS, the best values for effective parameters on desorption step were selected systematically. Also, the effective parameters on extraction step were optimized using a Box-Behnken design. Under the optimum conditions, the analytical performance of the proposed method displayed excellent linear dynamic ranges for LOS (24-1000 ng mL -1 ) and VAS (91-1000 ng mL -1 ), with correlation coefficients of 0.9998 and 0.9971 and detection limits of 7 and 27 ng mL -1 , respectively. The intra- and inter-day recovery ranged from 98 to 117%, and the relative standard deviations were less than 8%. Finally, the proposed technique was successfully applied to the analysis of LOS and VAS at their therapeutic levels in volunteer patient plasma sample. The obtained results were confirmed using liquid chromatography-mass spectrometry. The proposed technique was more rapid than previously reported stir bar sorptive extraction techniques based on monolithic coatings, and exhibited lower detection limits in comparison with similar methods for the determination of LOS and VLS in biological fluids. The obtained results were demonstrated that the lower selectivity of UV in comparison with MS detection was rectified by appropriate sample preparation through proposed extraction method to eliminate as many interfering compounds as possible. Copyright © 2018 Elsevier B.V. All rights reserved.

Application of a Stir Bar Sorptive Extraction sample preparation method with HPLC for soil fungal biomass determination in soils from a detrital manipulation study.

PubMed

Beni, Áron; Lajtha, Kate; Kozma, János; Fekete, István

2017-05-01

Ergosterol is a sterol found ubiquitously in cell membranes of filamentous fungi. Although concentrations in different fungal species span the range of 2.6 to 42μg/mL of dry mass, many studies have shown a strong correlation between soil ergosterol content and fungal biomass. The analysis of ergosterol in soil therefore could be an effective tool for monitoring changes in fungal biomass under different environmental conditions. Stir Bar Sorptive Extraction (SBSE) is a new sample preparation method to extract and concentrate organic analytes from liquid samples. SBSE was here demonstrated to be a simple, fast, and cost effective method for the quantitative analysis of ergosterol from field-collected soils. Using this method we observed that soil ergosterol as a measure of fungal biomass proved to be a sensitive indicator of soil microbial dynamics that were altered by changes in plant detrital inputs to soils in a long-term field experiment. Copyright © 2017 Elsevier B.V. All rights reserved.

Quantitative analysis of perfumes in talcum powder by using headspace sorptive extraction.

PubMed

Ng, Khim Hui; Heng, Audrey; Osborne, Murray

2012-03-01

Quantitative analysis of perfume dosage in talcum powder has been a challenge due to interference of the matrix and has so far not been widely reported. In this study, headspace sorptive extraction (HSSE) was validated as a solventless sample preparation method for the extraction and enrichment of perfume raw materials from talcum powder. Sample enrichment is performed on a thick film of poly(dimethylsiloxane) (PDMS) coated onto a magnetic stir bar incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace vial by using a holder. The stir bar is then thermally desorbed online with capillary gas chromatography-mass spectrometry. The HSSE method is based on the same principles as headspace solid-phase microextraction (HS-SPME). Nevertheless, a relatively larger amount of extracting phase is coated on the stir bar as compared to SPME. Sample amount and extraction time were optimized in this study. The method has shown good repeatability (with relative standard deviation no higher than 12.5%) and excellent linearity with correlation coefficients above 0.99 for all analytes. The method was also successfully applied in the quantitative analysis of talcum powder spiked with perfume at different dosages. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparation, characterization and application of a new stir bar sorptive extraction based on poly(vinylphthalimide-co-N,N'-methylenebisacrylamide) monolith.

PubMed

Huang, Xiaojia; Chen, Linli; Yuan, Dongxing; Luo, Xianbin

2011-12-01

In this study, a new stir bar sorptive extraction (SBSE) coating based on poly(vinylphthalimide-co-N,N'-methylenebisacrylamide) monolith (SBSE-VPMB) was prepared. The influences of the contents of monomer in polymerization mixture and the percentage of porogen solvent on the extraction performance were investigated thoroughly. Several characteristic techniques, such as elemental analysis, scanning electron microscopy, mercury intrusion porosimetry and infrared spectroscopy, were used to characterize the monolithic material. The analysis of oxfendazole (OFZ) and mebendazole (MBZ) in milk and honey samples by the combination of SBSE with HPLC with diode array detection was selected as paradigms for the practical evaluation of the new coating. Under the optimized extraction conditions, the limits of detection (S/N=3) for OFZ and MBZ were 0.23-0.60 μg/L in milk and 0.24-1.08 μg/L in honey, respectively. The method also showed good linearity, repeatability, high feasibility and acceptable recoveries for real samples. At the same time, the extraction performance and the distribution coefficients (K(VPMB/W)) of OFZ and MBZ on SBSE-VPMB were compared with other SBSEs based on porous monoliths and commercial SBSE. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Suitability of polydimethylsiloxane rods for the headspace sorptive extraction of polybrominated diphenyl ethers from water samples.

PubMed

Montes, R; Rodríguez, I; Rubí, E; Cela, R

2007-03-02

The suitability of an inexpensive polydimethysiloxane (PDMS) sorbent, produced on an industrial scale, for the extraction of polybrominated diphenyl ethers (PBDEs), from tetra- to hexabrominated congeners, from water samples was assessed. Experiments were carried out using samples spiked with a pentabromo diphenyl ether (pentaBDE) mixture, PDMS rods with a diameter of 2 mm and gas chromatography with micro-electron-capture detection (GC-micro-ECD). Influence of several variables on the efficiency of the enrichment step and the further desorption of the analytes was investigated in detail. The best performance was achieved in the headspace sorptive extraction (HSSE) mode, at 95 degrees C, using 80 mL water samples containing a 30% of sodium chloride. Extractions were performed overnight using disposable PDMS rods with a length of 10 mm (31 microL volume). Analytes were further recovered from the PDMS sorbent using just 1 mL of diethyl ether. This solvent was evaporated and extracts reconstituted with 25 microL of isooctane. Under final working conditions absolute extraction efficiencies from 69 to 93% and enrichment factors higher than 2200 folds were achieved for all species. The proposed method provided acceptable precisions (relative standard deviations values under 12%), correlation coefficients higher than 0.998 and the yield of the HSSE process remained constant for different water samples.

Static headspace analysis using polyurethane phases--application to roasted coffee volatiles characterization.

PubMed

Rodrigues, C; Portugal, F C M; Nogueira, J M F

2012-01-30

Static headspace sorptive extraction using polyurethane foams (HSSE(PU)) followed by gas chromatography coupled to mass spectrometry is proposed for volatile analysis. The application of this novel analytical approach to characterize the volatiles profile from roasted coffee samples, selected as model system, revealed remarkable advantages under convenient experimental conditions. The comparison of HSSE(PU) with other well-established procedures, such as headspace sorptive extraction using polydimethylsiloxane (HSSE(PDMS)) and headspace solid phase microextraction using carboxen/polydimethylsiloxane fibers (HS-SPME(CAR/PDMS)), showed that the former presented much higher capacity, sensitivity and even selectivity, where larger abundance and number of roasted coffee volatile compounds (e.g. furans, pyrazines, ketones, acids and pyrroles) could be achieved, under similar experimental conditions. The data presented herein proved, for the first time, that PU foams present great performance for static headspace sorption-based procedures, showing to be an alternative polymeric phase for volatile analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

Analysis of hop-derived terpenoids in beer and evaluation of their behavior using the stir bar-sorptive extraction method with GC-MS.

PubMed

Kishimoto, Toru; Wanikawa, Akira; Kagami, Noboru; Kawatsura, Katsuyuki

2005-06-15

Hop aroma components, which mainly comprise terpenoids, contribute to the character of beers. However, pretreatments are necessary before analyzing these components because of their trace levels and complicated matrixes. Here, the stir bar-sorptive extraction (SBSE) method was used to detect and quantify many terpenoids simultaneously from small samples. This simple technique showed low coefficients of variation, high accuracy, and low detection limits. An investigation of the behavior of terpenoids identified two distinct patterns of decreasing concentration during wort boiling. The first, which was seen in myrcene and linalool, involved a rapid decrease that was best fitted by a quadratic curve. The second, which was observed in beta-eudesmol, humulene, humulene epoxide I, beta-farnesene, caryophyllene, and geraniol, involved a gentle linear decrease. Conversely, the concentration of beta-damascenone increased after boiling. As the aroma composition depended on the hop variety, we also examined the relationship between terpenoid content and sensory analysis in beer.

Evaluation of a method for the simultaneous quantification of N-nitrosamines in water samples based on stir bar sorptive extraction combined with high-performance liquid chromatography and diode array detection.

PubMed

Talebpour, Zahra; Rostami, Simindokht; Rezadoost, Hassan

2015-05-01

A simple, sensitive, and reliable procedure based on stir bar sorptive extraction coupled with high-performance liquid chromatography was applied to simultaneously extract and determine three semipolar nitrosamines including N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine. To achieve the optimum conditions, the effective parameters on the extraction efficiency including desorption solvent and time, ionic strength of sample, extraction time, and sample volume were systematically investigated. The optimized extraction procedure was carried out by stir bars coated with polydimethylsiloxane. Under optimum extraction conditions, the performance of the proposed method was studied. The linear dynamic range was obtained in the range of 0.95-1000 ng/mL (r = 0.9995), 0.26-1000 ng/mL (r = 0.9988) and both 0.32-100 ng/mL (r = 0.9999) and 100-1000 ng/mL (r = 0.9998) with limits of detection of 0.28, 0.08, and 0.09 ng/mL for N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine, respectively. The average recoveries were obtained >81%, and the reproducibility of the proposed method presented as intra- and interday precision were also found with a relative standard deviation <6%. Finally, the proposed method was successfully applied to the determination of trace amounts of selected nitrosamines in various water and wastewater samples and the obtained results were confirmed using mass spectrometry. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Capillary electrophoresis for analyzing pesticides in fruits and vegetables using solid-phase extraction and stir-bar sorptive extraction.

PubMed

Juan-García, Ana; Picó, Yolanda; Font, Guillermina

2005-05-06

Two procedures based on solid-phase extraction (SPE) and stir-bar sorptive extraction (SBSE) in combination with micellar electrokinetic chromatography (MEKC)--diode array detection (DAD) were compared for the simultaneous extraction of acrinathrin, bitertanol, cyproconazole, fludioxonil, flutriafol, myclobutanil, pyriproxyfen, and tebuconazole in lettuce, tomato, grape, and strawberry. Selectivity and resolution of the MEKC procedure were studied changing the pH and the molarity of the buffer, the type and the concentration of surfactant, and the methanol content in the mobile phase. A buffer consisting of 6 mM sodium tetraborate decahydrate with 75 mM of cholic acid sodium solution (pH 9.2) gave the best results. Linearity, extraction efficiencies and limits of quantitation (LOQs) of both extraction methods were compared. The recoveries obtained by SPE ranged from 40 to 106% with relative standard deviations (R.S.D.s) from 10 to 19% whereas by the SBSE method, the recoveries were 12-47% and the R.S.D.s 3-17%. The LOQs were much better by SPE (0.2-0.5 mg kg(-1) depending on the processed sample amount) than those obtained by SBSE (1 mg kg(-1) for each compound). Advantages and disadvantages of both procedures are also discussed. As SPE is more robust, rapid, and sensitive than SBSE, its application in combination with MEKC is recommended because provided LOQs below the MRLs established, which is not always attained by SBSE.

One-pot polymerization of monolith coated stir bar for high efficient sorptive extraction of perfluoroalkyl acids from environmental water samples followed by high performance liquid chromatography-electrospray tandem mass spectrometry detection.

PubMed

Yao, Xuezi; Zhou, Zhen; He, Man; Chen, Beibei; Liang, Yong; Hu, Bin

2018-06-08

In this work, poly(1-vinylimidazole-ethyleneglycol dimethacrylate) (poly(VI-EDMA)) monolith coated stir bars were synthesized by one-pot polymerization, and they exhibited higher extraction efficiency and faster extraction dynamics for selected PFAAs than commercial ethylene glycol modified silicone (EG-silicone) and polydimethylsiloxane (PDMS) coated stir bars. Taking eleven PFAAs as target analytes, including C4-C12 perfluoroalkyl carboxylates (PFCAs) and C6, C8 perfluoroalkane sulfonates (PFSAs), a method combining monolith-based stir bar sorptive extraction (SBSE) with high performance liquid chromatography (HPLC) - electrospray tandem mass spectrometry (ESI-MS/MS) was proposed for the determination of multiplex PFAAs in environmental water samples. Under the optimized conditions, low limits of detection (0.06-0.40 ng/L) and wide linear range (0.6-400 ng/L) were obtained for target PFAAs with. The developed method was then applied for the analysis of target PFAAs in environmental water samples, and recoveries of 80.1-117% and 80.3-122% were obtained for target PFAAs in spiked Yangtze River and East Lake water samples respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

Ultra-trace determination of Persistent Organic Pollutants in Arctic ice using stir bar sorptive extraction and gas chromatography coupled to mass spectrometry.

PubMed

Lacorte, S; Quintana, J; Tauler, R; Ventura, F; Tovar-Sánchez, A; Duarte, C M

2009-12-04

This study presents the optimization and application of an analytical method based on the use of stir bar sorptive extraction (SBSE) gas chromatography coupled to mass spectrometry (GC-MS) for the ultra-trace analysis of POPs (Persistent Organic Pollutants) in Arctic ice. In a first step, the mass-spectrometry conditions were optimized to quantify 48 compounds (polycyclic aromatic hydrocarbons, brominated diphenyl ethers, chlorinated biphenyls, and organochlorinated pesticides) at the low pg/L level. In a second step, the performance of this analytical method was evaluated to determine POPs in Arctic cores collected during an oceanographic campaign. Using a calibration range from 1 to 1800 pg/L and by adjusting acquisition parameters, limits of detection at the 0.1-99 and 102-891 pg/L for organohalogenated compounds and polycyclic aromatic hydrocarbons, respectively, were obtained by extracting 200 mL of unfiltered ice water. alpha-hexachlorocyclohexane, DDTs, chlorinated biphenyl congeners 28, 101 and 118 and brominated diphenyl ethers congeners 47 and 99 were detected in ice cores at levels between 0.5 to 258 pg/L. We emphasise the advantages and disadvantages of in situ SBSE in comparison with traditional extraction techniques used to analyze POPs in ice.

Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

PubMed

Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

2016-10-01

A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

Solvent-assisted stir bar sorptive extraction by using swollen polydimethylsiloxane for enhanced recovery of polar solutes in aqueous samples: Application to aroma compounds in beer and pesticides in wine.

PubMed

Ochiai, Nobuo; Sasamoto, Kikuo; David, Frank; Sandra, Pat

2016-07-15

A novel solvent-assisted stir bar sorptive extraction (SA-SBSE) technique was developed for enhanced recovery of polar solutes in aqueous samples. A conventional PDMS stir bar was swollen in several solvents with log Kow ranging from 1.0 to 3.5 while stirring for 30min prior to extraction. After extraction, thermal desorption - gas chromatography - (tandem) mass spectrometry (TD-GC-(MS/)MS) or liquid desorption - large volume injection (LD-LVI)-GC-MS were performed. An initial study involved investigation of potential solvents for SA-SBSE by weighing of the residual solvent in the swollen PDMS stir bar before and after extraction. Compared to conventional SBSE, SA-SBSE using diethyl ether, methyl isobutyl ketone, dichloromethane, diisopropyl ether and toluene provided higher recoveries from water samples for test solutes with log Kow<2.5. For SA-SBSE using dichloromethane, recoveries were improved by factors of 1.4-4.1, while maintaining or even improving the recoveries for test solutes with log Kow>2.5. The performance of the SA-SBSE method using dichloromethane, diisopropyl ether, and cyclohexane is illustrated with analyses of aroma compounds in beer and of pesticides in wine. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Multiresidue screening of endocrine-disrupting chemicals and pharmaceuticals in aqueous samples by multi-stir bar sorptive extraction-single desorption-capillary gas chromatography/mass spectrometry.

PubMed

Van Hoeck, Els; Canale, Francesca; Cordero, Chiara; Compernolle, Sien; Bicchi, Carlo; Sandra, Pat

2009-02-01

A multiresidue method for screening endocrine-disrupting chemicals (EDCs) and pharmaceuticals in aqueous samples is presented. Four 10-mL aliquots of water were taken for stir bar sorptive extraction (SBSE) and they were treated in the following way. In sample one, in situ derivatization was performed with acetic acid anhydride to improve the extraction efficiencies and chromatographic analysis of phenolic compounds. For the same reasons, aliquot two was treated with ethyl chloroformate to improve amine and acid extraction and analysis, and aliquot three with tetraethylborate to enhance organotin compound extraction and analysis. Methanol was added to sample four to stop adsorption of apolar solutes on the wall. After SBSE, the four stir bars, together with a plug of glass wool impregnated with bis(trimethylylsilyl)trifluoroacetamide (BSTFA) to derivatize hydroxyl functionalities, were introduced into the same thermal desorption tube, heat-desorbed, and analyzed simultaneously by capillary GC/MS. The figures of merit of the method were evaluated with an EDC model mixture. In scan-mode MS, the limits of detection (LODs) were in the range 1-500 ng/L, while the LODs dropped by a factor of 50-100 when ion monitoring MS was applied to the targets. The performance of the method was illustrated by analysing some real-world water samples.

One-pot synthesis of zeolitic imidazolate framework-8/poly (methyl methacrylate-ethyleneglycol dimethacrylate) monolith coating for stir bar sorptive extraction of phytohormones from fruit samples followed by high performance liquid chromatography-ultraviolet detection.

PubMed

You, Linna; He, Man; Chen, Beibei; Hu, Bin

2017-11-17

In this work, zeolitic imidazolate framework-8 (ZIF-8)/poly (methyl methacrylate-ethyleneglycol dimethacrylate) (MMA-EGDMA) composite monolith was in situ synthesized on stir bar by one-pot polymerization. Compared with the neat monolith, ZIF-8/poly(MMA-EGDMA) composite monolith has larger surface area and pore volume. It also exhibits higher extraction efficiency for target phytohormones than poly(MMA-EGDMA) monolith and commercial polyethylene glycol (PEG) coated stir bar. Based on it, a method of ZIF-8/poly(MMA-EGDMA) monolith coated stir bar sorptive extraction (SBSE)-high performance liquid chromatography-ultraviolet detection (HPLC-UV) was established for the analysis of five phytohormones in apple and pear samples. The developed method exhibited low limits of detection (0.11-0.51μg/L), wide linear range (0.5-500μg/L) and good recoveries (82.7-111%), which demonstrated good application potential of the ZIF-8/monolith coated stir bar in trace analysis of organic compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

Stir bar sorptive extraction coupled to gas chromatography-mass spectrometry for the determination of bisphenols in canned beverages and filling liquids of canned vegetables.

PubMed

Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

2012-07-20

This paper describes a method for the simultaneous determination of bisphenol A (BPA), bisphenol F (BPF), bisphenol Z (BPZ) and biphenol (BP), using stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Several parameters affecting both extraction and thermal desorption of the SBSE stages were carefully optimized by multivariate designs. SBSE was performed with two derivatization procedures, in situ acetylation and in tube silylation, and the results were compared with those obtained when the analytes were not derivatized. The proposed method, determining the analytes as acyl derivatives, was applied to analyze commercially canned beverages, as well as the filling liquids of canned vegetables, providing detection limits of between 4.7 and 12.5 ng L⁻¹, depending on the compound. The intraday and interday precisions were lower than 6% in terms of relative standard deviation. Recovery studies at two concentration levels, 0.1 and 1 μg L⁻¹, were performed providing recoveries in the 86-122% range. The samples analyzed contained higher concentrations of BPA than of the other analytes. Copyright © 2012 Elsevier B.V. All rights reserved.

Evaluation of three headspace sorptive extraction coatings for the determination of volatile terpenes in honey using gas chromatography-mass spectrometry.

PubMed

Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

2015-06-19

Headspace sorptive extraction (HSSE) was used to preconcentrate seven monoterpenes (eucalyptol, linalool, menthol, geraniol, carvacrol, thymol and eugenol) for separation by gas chromatography and mass spectrometry (GC-MS). Three commercially available coatings for the stir bars, namely Polydimethylsiloxane (PDMS), polyacrilate (PA) and Ethylene glycol-silicone (EG-Silicone), were tested, and the influential parameters both in the adsorption and the thermal desorption steps were optimized. PDMS provided the best sensitivity for linalool, geraniol, menthol and eucalyptol, whereas EG-Silicone was best for extracting the phenolic monoterpenes studied. Considering the average obtained slopes from all compounds, PDMS pointed as the best option, and the analytical characteristics for the HSSE-TD-GC-MS method using this coating were obtained. Quantification of the samples was carried out by matrix-matched calibration using a synthetic honey. Detection limits ranged between 0.007 and 0.032 ng g(-1), depending on the compound. Twelve honey samples of different floral origins were analyzed using the HSSE-GC-MS method, the analytes being detected at concentrations up to 64 ng g(-1). Copyright © 2015 Elsevier B.V. All rights reserved.

Polydimethylsiloxane/covalent triazine frameworks coated stir bar sorptive extraction coupled with high performance liquid chromatography-ultraviolet detection for the determination of phenols in environmental water samples.

PubMed

Zhong, Cheng; He, Man; Liao, Huaping; Chen, Beibei; Wang, Cheng; Hu, Bin

2016-04-08

In this work, covalent triazine frameworks (CTFs) were introduced in stir bar sorptive extraction (SBSE) and a novel polydimethylsiloxane(PDMS)/CTFs stir bar coating was prepared by sol-gel technique for the sorptive extraction of eight phenols (including phenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4-dimethylphenol, p-chloro-m-cresol and 2,4-dichlorophenol, 2,4,6-trichlorophenol) from environmental water samples followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. The prepared PDMS/CTFs coated stir bar showed good preparation reproducibility with the relative standard deviations (RSDs) ranging from 3.5 to 5.7% (n=7) in one batch, and from 3.7 to 9.3% (n=7) among different batches. Several parameters affecting SBSE of eight target phenols including extraction time, stirring rate, sample pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.08-0.30 μg/L. The linear range was 0.25-500 μg/L for 2-nitrophenol, 0.5-500 μg/L for phenol, 2-chlorophenol, 4-nitrophenol as well as 2,4-dimethylphenol, and 1-500 μg/L for p-chloro-m-cresol, 2,4-dichlorophenol as well as 2,4,6-trichlorophenol, respectively. The intra-day relative standard deviations (RSDs) were in the range of 4.3-9.4% (n=7, c=2 μg/L) and the enrichment factors ranged from 64.9 to 145.6 fold (theoretical enrichment factor was 200-fold). Compared with commercial PDMS coated stir bar (Gerstel) and PEG coated stir bar (Gerstel), the prepared PDMS/CTFs stir bar showed better extraction efficiency for target phenol compounds. The proposed method was successfully applied to the analysis of phenols in environmental water samples and good relative recoveries were obtained with the spiking level at 2, 10, 50 μg/L, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Water-compatible graphene oxide/molecularly imprinted polymer coated stir bar sorptive extraction of propranolol from urine samples followed by high performance liquid chromatography-ultraviolet detection.

PubMed

Fan, Wenying; He, Man; You, Linna; Zhu, Xuewei; Chen, Beibei; Hu, Bin

2016-04-22

Due to the high selectivity and stability, molecularly imprinted polymers (MIPs) have been successfully applied in stir bar sorptive extraction (SBSE) as a special coating to improve the selective extraction capability for target analytes. However, traditional MIPs usually suffer from incompatibility in aqueous media and low adsorption capacity, which limit the application of MIP coated stir bar in aqueous samples. To solve these problems, a water-compatible graphene oxides (GO)/MIP composite coated stir bar was prepared in this work by in situ polymerization. The prepared water-compatible GO/MIP coated stir bar presented good mechanical strength and chemical stability, and its recognition ability in aqueous samples was improved due to the polymerization of MIP in water environment, the adsorption capacity for target analytes was also increased by the addition of GO in MIP pre-polymer solution. Based on it, a method of water-compatible GO/MIP coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detector (HPLV-UV) was proposed for the analysis of propranolol (PRO) in aqueous solution. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limit of detection (LOD) of the proposed method for PRO was about 0.37 μg L(-1), and the enrichment factor (EF) was 59.7-fold (theoretical EF was 100-fold). The reproducibility was also investigated at concentrations of 5 μg L(-1) and the relative standard deviation (RSD) was found to be 7.3% (n=7). The proposed method of GO/MIP coating-SBSE-HPLC-UV was successfully applied for the assay of the interested PRO drug in urine samples, and further extended to the investigation of the excretion of the drugs by monitoring the variation of the concentration of PRO in urine within 10h after drug-taking. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of pressurized subcritical water extraction combined with stir bar sorptive extraction for the analysis of organochlorine pesticides and chlorobenzenes in soils.

PubMed

Rodil, Rosario; Popp, Peter

2006-08-18

An analytical method for the determination of several organochlorine pesticides (OCPs) like hexachlorocyclohexanes (HCHs), cyclodiene derivates (dieldrin, aldrin, endrin, heptachlor, heptachlor epoxide, endrin aldehyde, endosulfan and ensodulfan sulphate) and DDX compounds (p,p'-DDE, p,p'-DDD and p,p'-DDT) as well as chlorobenzenes in soils has been developed. The procedure is based on pressurized subcritical water extraction (PSWE) followed by stir bar sorptive extraction (SBSE) and subsequent thermodesorption-gas chromatography/mass spectrometry analysis. Significant PSWE and SBSE parameters were optimized using spiked soil and water samples. For the PSWE of the organochlorine compounds, water modified with acetonitrile as the extraction solvent, at an extraction temperature of 120 degrees C, and three cycles of 10 min extraction proved to be optimal. Under optimized conditions, the figures of merit, such as precision, accuracy and detection limits were evaluated. The detection limits obtained for soil samples were in the range 0.002-4.7 ng/g. Recoveries between 4.1 and 85.2% were achieved from samples spiked at a concentration level of 25-155 ng/g. The main advantages of this method are the avoidance of clean-up and concentration procedures as well as the significant reduction of the required volume of organic solvents. The described method was applied to the determination of the pollutants in soil samples collected from a polluted area, the Bitterfeld region (Germany). The results obtained by PSWE-SBSE were in a good agreement with those obtained by a reference method, a conventional pressurized liquid extraction (PLE).

Coupling of multi-walled carbon nanotubes/polydimethylsiloxane coated stir bar sorptive extraction with pulse glow discharge-ion mobility spectrometry for analysis of triazine herbicides in water and soil samples.

PubMed

Zou, Nan; Yuan, Chunhao; Liu, Shaowen; Han, Yongtao; Li, Yanjie; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

2016-07-29

An analytical method based on stir bar sorptive extraction (SBSE) coupled with pulse glow discharge-ion mobility spectrometry (PGD-IMS) was developed for analysis of three triazine pesticide residues in water and soil samples. An injection port with sealing device and stir bars hold device were designed and constructed to directly position the SBSE fiber including the extracted samples into the heating device, making desorption and detection of analytes proceeded simultaneously. The extraction conditions such as SBSE solid phase material, extraction time, extraction temperature, pH value and salt concentration were optimized. Mixture of MWCNTs-COOH and PDMS were shown to be effective in enriching the triazines. The LODs and LOQs of three triazines were found to be 0.006-0.015μgkg(-1) and 0.02-0.05μgkg(-1), and the linear range was 0.05-10μgL(-1) with determination coefficients from 0.9987 to 0.9993. The SBSE-PGD-IMS method was environmentally friendly without organic solvent consumption in the entire experimental procedures, and it was demonstrated to be a commendable rapid analysis technique for analysis of triazine pesticide residues in environmental samples on site. The proposed method was applied for the analysis of real ground water, surface water and soil samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Novel combined stir bar sorptive extraction coupled with ultrasonic assisted extraction for the determination of brominated flame retardants in environmental samples using high performance liquid chromatography.

PubMed

Yu, Chunhe; Hu, Bin

2007-08-10

A combined stir bar coated with poly (dimethysiloxane)-beta-cyclodextrin (PDMS-beta-CD) on single side has been prepared for the first time by sol-gel method and was coupled with ultrasonic assisted extraction (UAE) for the determination of some brominated flame-retardant compounds (BFRs) in soil and dust samples by high performance liquid chromatography (HPLC). Four different kinds of coatings including PDMS-beta-CD, PDMS, carbowax (CW)-PDMS-poly (vinyl alcohol) (PVA) and PDMS-PVA were evaluated for stir bar sorptive extraction of BFRs by orthogonal experiment design. The experimental results reveal that the PDMS-beta-CD combined stir bar exhibited the best extraction efficiency for the target analytes. The reproducibility for the preparation of PDMS-beta-CD combined stir bar ranged from 1.3% to 15.7% in one batch, and 7.2% to 15.1% among batches. Extraction time, desorption solvent, concentration of methanol and NaCl in the matrix, pH, temperature and stirring speed were optimized. The combined stir bar can avoid direct friction of the coating with the bottom of the vessel, and could be used for more than 100 times. Linearity (>0.993), repeatability (<10.5%), reproducibility (<16.5%), recovery (56-118%) and detection limits (2.9-4.2 microg L(-1)) were proper to determine the seven BFRs. The developed method was applied to the determination of BFRs in soil and dust with satisfactory results.

Stir bar sorptive extraction and liquid chromatography-tandem mass spectrometry determination of polar and non-polar emerging and priority pollutants in environmental waters.

PubMed

Aparicio, Irene; Martín, Julia; Santos, Juan Luis; Malvar, José Luis; Alonso, Esteban

2017-06-02

An analytical method based on stir bar sorptive extraction (SBSE) was developed and validated for the determination of environmental concern pollutants in environmental waters by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Target compounds include six water and oil repellents (perfluorinated compounds), four preservatives (butylated hydroxytoluene and three parabens), two plasticizers (bisphenol A and di(2-ethylhexyl)phthalate), seven surfactants (four linear alkylbenzene sulfonates, nonylphenol and two nonylphenol ethoxylates), a flame retardant (hexabromocyclododecane), four hormones, fourteen pharmaceutical compounds, an UV-filter (2-ethylhexyl 4-methoxycinnamate) and nine pesticides. To achieve the simultaneous extraction of polar and non-polar pollutants two stir bar coatings were tested, the classic polydimethylsiloxane (PDMS) coating and the novel ethylene glycol modified silicone (EG-silicone). The best extraction recoveries were obtained using EG-silicone coating. The effects of sample pH, volume and ionic strength and extraction time on extraction recoveries were evaluated. The analytical method was validated for surface water and tap water samples. The method quantification limits ranged from 7.0ngL -1 to 177ngL -1 . The inter-day precision, expressed as relative standard deviation, was lower than 20%. Accuracy, expressed as relative recovery values, was in the range from 61 to 130%. The method was applied for the determination of the 48 target compounds in surface and tap water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimization of a multiple headspace sorptive extraction method coupled to gas chromatography-mass spectrometry for the determination of volatile compounds in macroalgae.

PubMed

Maruti, Astrid; Durán-Guerrero, Enrique; Barroso, Carmelo G; Castro, Remedios

2018-05-25

A novel extraction technique is proposed in which the Multiple Headspace Extraction (MHE) approach is used in conjunction with Headspace Sorptive Extraction (HSSE) and Gas Chromatography-Mass Spectrometry (GC-MS) detection. The extraction method was developed to determine volatile compounds in macroalgae. Optimization of the extraction parameters was carried out using design of experiments to identify factors that affect the extraction: extraction time, temperature, twister length and amount of sample. The results of the optimization led to an extraction of 2 g of sample using a 20 mm Twister ® at 66 °C for 180 min. The progression constants (β) were calculated for 43 volatile compounds, 29 of which could be quantified using the method. Linearity was attained with a determination coefficient higher than 0.99 for all studied compounds. Inter-day and inter-twister precisions ranged from 0.22% to 19.01% and from 0.69% to 14.76% respectively, and values below 10% were obtained for the majority of compounds. LOD and LOQ values ranged from the values obtained for diethyl succinate (0.012 μg/L and 0.088 μg/L, respectively) and those obtained for dimethyl sulfide (5.544 μg/L and 40.286 μg/L, respectively). However, for the majority of compounds values obtained were below 1 μg/L (LOD) and 5 μg/L (LOQ). Compounds such as ethyl acetate, hexanal, heptadecane, 2-hexenal, 6-methyl-5-hepten-2-one, dimethyl sulfide, benzyl alcohol, beta ionone, or beta cyclocitral, among others were correctly determined in three species of macroalgae: Ulva sp., Gracillaria sp. and Enteromorpha sp. Copyright © 2018 Elsevier B.V. All rights reserved.

Submerged Cultivation of Pleurotus sapidus with Molasses: Aroma Dilution Analyses by Means of Solid Phase Microextraction and Stir Bar Sorptive Extraction.

PubMed

Trapp, Tobias; Zajul, Martina; Ahlborn, Jenny; Stephan, Alexander; Zorn, Holger; Fraatz, Marco Alexander

2018-03-14

The basidiomycete Pleurotus sapidus (PSA) was grown in submerged cultures with molasses as substrate for the production of mycelium as a protein source for food applications. The volatilomes of the substrate, the submerged culture, and the mycelia were analyzed by gas chromatography-tandem mass spectrometry-olfactometry. For compound identification, aroma dilution analyses by means of headspace solid phase microextraction and stir bar sorptive extraction were performed via variation of the split vent flow rate. Among the most potent odorants formed by PSA were arylic compounds (e.g., p-anisaldehyde), unsaturated carbonyls (e.g., 1-octen-3-one, ( E)-2-octenal, ( E, E)-2,4-decadienal), and cyclic monoterpenoids (e.g., 3,9-epoxy- p-menth-1-ene, 3,6-dimethyl-3a,4,5,7a-tetrahydro-1-benzofuran-2(3 H)-one). Several compounds from the latter group were described for the first time in Pleurotus spp. After separation of the mycelia from the medium, the aroma compounds were mainly enriched in the culture supernatant. The sensory analysis of the mycelium correlated well with the instrumental results.

Automated multisyringe stir bar sorptive extraction using robust montmorillonite/epoxy-coated stir bars.

PubMed

Ghani, Milad; Saraji, Mohammad; Maya, Fernando; Cerdà, Víctor

2016-05-06

Herein we present a simple, rapid and low cost strategy for the preparation of robust stir bar coatings based on the combination of montmorillonite with epoxy resin. The composite stir bar was implemented in a novel automated multisyringe stir bar sorptive extraction system (MS-SBSE), and applied to the extraction of four chlorophenols (4-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) as model compounds, followed by high performance liquid chromatography-diode array detection. The different experimental parameters of the MS-SBSE, such as sample volume, selection of the desorption solvent, desorption volume, desorption time, sample solution pH, salt effect and extraction time were studied. Under the optimum conditions, the detection limits were between 0.02 and 0.34μgL(-1). Relative standard deviations (RSD) of the method for the analytes at 10μgL(-1) concentration level ranged from 3.5% to 4.1% (as intra-day RSD) and from 3.9% to 4.3% (as inter-day RSD at 50μgL(-1) concentration level). Batch-to-batch reproducibility for three different stir bars was 4.6-5.1%. The enrichment factors were between 30 and 49. In order to investigate the capability of the developed technique for real sample analysis, well water, wastewater and leachates from a solid waste treatment plant were satisfactorily analyzed. Copyright © 2016 Elsevier B.V. All rights reserved.

[Application of Stir Bar Sorptive Extraction and Gas Chromatograph Mass Spectrometer to the Phthalic Acid Esters Analysis in Seawater].

PubMed

Gao, Chen-chen; Li, Feng-min; Lu, Lun; Sun, Yue

2015-10-01

For the determination of trace amounts of phthalic acid esters (PAEs) in complex seawater matrix, a stir bar sorptive extraction gas chromatography mass spectrometry (SBSE-GC-MS) method was established. Dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), dibutyl phthalate (2-ethylhexyl) phthalate (DEHP) and dioctyl phthalate (DOP) were selected as study objects. The effects of extraction time, amount of methanol, amount of sodium chloride, desorption time and desorption solvent were optimized. The method of SBSE-GC-MS was validated through recoveries and relative standard deviation. The optimal extraction time was 2 h. The optimal methanol content was 10%. The optimal sodium chloride content was 5% . The optimal desorption time was 50 min. The optimal desorption solvent was the mixture of methanol to acetonitrile (4:1, volume: volume). The linear relationship between the peak area and the concentration of PAEs was relevant. The correlation coefficients were greater than 0.997. The detection limits were between 0.25 and 174.42 ng x L(-1). The recoveries of different concentrations were between 56.97% and 124.22% . The relative standard deviations were between 0.41% and 14.39%. On the basis of the method, several estuaries water sample of Jiaozhou Bay were detected. DEP was detected in all samples, and the concentration of BBP, DEHP and DOP were much higher than the rest.

Potentialities of polyurethane foams for trace level analysis of triazinic metabolites in water matrices by stir bar sorptive extraction.

PubMed

Portugal, Fátima C M; Pinto, Moisés L; Pires, João; Nogueira, J M F

2010-06-04

Polyurethane (PU) foams were applied for stir bar sorptive extraction of five triazinic metabolites (desethyl-2-hydroxyatrazine, desisopropylatrazine, desethylatrazine, 2-hydroxyatrazine and desethylterbuthylazine) in water matrices, followed by liquid desorption and high performance liquid chromatography with diode array detection (SBSE(PU)-LD/HPLC-DAD). The optimum conditions for SBSE(PU)-LD were 5h of extraction (1000 rpm) and 5% (v/v) of methanol for the analysis of desethyl-2-hydroxyatrazine and 2-hydroxyatrazine, 15% (w/v) of sodium chloride for the remaining compounds and acetonitrile as back-extraction solvent (5 mL) under ultrasonic treatment (60 min). The methodology provided recoveries up to 26.3%, remarkable precision (RSD<2.4%), excellent linear dynamic ranges between 5.0 and 122.1 microg/L (r(2)>0.9993) and convenient detection limits (0.4-1.3 microg/L). The proposed method was applied in the analysis of triazinic metabolites in tap, river and ground waters, with remarkable performance and negligible matrix effects. The comparison of the recoveries obtained by PU and commercial stir bars was also performed, where the yields achieved with the former were up to ten times higher proving that PU is appropriate for analysis at trace level of this type of polar compounds in water matrices. Copyright 2010 Elsevier B.V. All rights reserved.

Development of a sensitive determination method for benzotriazole UV stabilizers in enviromental water samples with stir bar sorption extraction and liquid desorption prior to ultra-high performance liquid chromatography with tandem mass spectrometry.

PubMed

Montesdeoca-Esponda, Sarah; del Toro-Moreno, Adrián; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

2013-07-01

Benzotriazole UV stabilizers are emerging compounds used in personal care products and can enter surface water after passing through wastewater treatment plants without being removed. Because these analytes are strongly hydrophobic, there is an environmental risk of accumulation in solid matrices and magnification through the trophic chain. In this work, a method based on stir bar sorption extraction with liquid desorption is presented for the extraction of benzotriazole UV stabilizers from water samples. Stir bar sorptive extraction was combined with ultra-high performance LC with MS/MS detection. All important factors affecting the stir bar sorptive extraction procedure are discussed, and the optimized method was applied to seawater and wastewater samples from Gran Canaria Island, providing good selectivity and sensitivity with LODs and limits of quantification in the range of 18.4-55.1 and 61.5-184 ng/L, respectively. Recoveries between 68.4-92.2% were achieved for the more polar compounds, whereas the recoveries were lower for the two less polar compounds, most likely due to their strong absorption into the polydimethylsiloxane stir bar phase that does not allows the complete desorption. The repeatability studies gave RSDs of between 6.45 and 12.6% for all compounds in the real samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of low-cost disposable polymeric materials for sorptive extraction of organic pollutants in water samples.

PubMed

Prieto, Ailette; Rodil, Rosario; Quintana, José Benito; Rodríguez, Isaac; Cela, Rafael; Möder, Monika

2012-02-24

The capabilities of four commercially available and low cost polymeric materials for the extraction of polar and non-polar contaminants (logK(ow)=-0.07-6.88, from caffeine to octocrylene, respectively) from water samples was compared. Tested sorbents were polyethersulphone, polypropylene and Kevlar, compared to polydimethylsiloxane as reference material. Parameters that affect the extraction process such as pH and ionic strength of the sample, extraction time and desorption conditions were thoroughly investigated. A set of experimental partition coefficients (K(pw)), at two different experimental conditions, was estimated for the best suited materials and compared with the theoretical octanol-water (K(ow)) partition coefficients of the analytes. Polyethersulphone displayed the largest extraction yields for both polar and non-polar analytes, with higher K(pw) and lower matrix effects than polydimethylsiloxane and polypropylene. Thus, a sorptive microextraction method, followed by large volume injection (LVI) gas chromatography-tandem mass spectrometry (GC-MS/MS), was proposed using the former sorbent (2 mg) for the simultaneous determination of model compounds in water samples. Good linearity (>0.99) was obtained for most of the analytes, except in the case of 4-nonylphenol (0.9466). Precision (n=4) at 50 and 500 ng L(-1) levels was in the 2-24% and limits of detection (LODs) were in the 0.6-25 ng L(-1) range for all the analytes studied. Copyright © 2011 Elsevier B.V. All rights reserved.

A fast stir bar sorptive extraction method for the analysis of geosmin and 2-methylisoborneol in source and drinking water.

PubMed

Bauld, T; Teasdale, P; Stratton, H; Uwins, H

2007-01-01

The presence of unpleasant taste and odour in drinking water is an ongoing aesthetic concern for water providers worldwide. The need for a sensitive and robust method capable of analysis in both natural and treated waters is essential for early detection of taste and odour events. The purpose of this study was to develop and optimise a fast stir bar sorptive extraction (SBSE) method for the analysis of geosmin and 2-methylisoborneol (MIB) in both natural water and drinking water. Limits of detection with the optimised fast method (45 min extraction time at 60 degrees C using 24 microL stir bars) were 1.1 ng/L for geosmin and 4.2 ng/L for MIB. Relative standard deviations at the detection limits were under 17% for both compounds. Use of multiple stir bars can be used to decrease the detection limits further. The use of 25% NaCl and 5% methanol sample modifiers decreased the experimental recoveries. Likewise, addition of 1 mg/L and 1.5 mg/L NaOCI decreased the recoveries and this effect was not reversed by addition of 10% thiosulphate. The optimised method was used to measure geosmin concentrations in treated and untreated drinking water. MIB concentrations were below the detection limits in these waters.

Development of Carbon Nanotube-Polyamide Nanocomposite-based Stir Bar Sorptive Extraction Coupled to HPLC-UV Applying Response Surface Methodology for the Analysis of Bisphenol A in Aqueous Samples.

PubMed

Ayazi, Z; Matin, A A

2016-11-01

A novel nanocomposite based on reinforcing of multiwalled carbon nanotubes in polyamide (PA) was prepared by solvent exchange method as stir bar coating. The morphology and surface characteristic of PA and CNT/PA coated stir bars were investigated using scanning electron microscopy. The stir bar coated by CNT/PA nanocomposite was used as an extraction device for stir bar sorptive extraction of bisphenol A from aqueous samples followed by high performance liquid chromatography-UV detection. The effect of CNTs doping level and oxidation of CNTs on the extraction capability of the coating was investigated. Response surface methodology applying central composite design was used for modeling and optimization of important factors influencing the extraction and desorption processes including extraction time, salt and methanol content, desorption solvent, its volume and desorption time. Limit of detection and linear dynamic range of the method were 0.3 ng mL -1 and 1-10 ng mL -1 , respectively. The method precision (RSD%) with four replicate determinations was 4.9% for distilled water at the concentration level of 10 ng mL -1 The obtained RSD% for reproducibility of stir bars was 7.4%. The developed method was successfully applied to the bottled mineral water samples, while the relative recoveries (RR%) were obtained to be in the range of 92.0-101.9%. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Stir bar sorptive extraction of diclofenac from liquid formulations: a proof of concept study.

PubMed

Kole, Prashant Laxman; Millership, Jeff; McElnay, James C

2011-03-25

A new stir bar sorptive extraction (SBSE) technique coupled with HPLC-UV method for quantification of diclofenac in pharmaceutical formulations has been developed and validated as a proof of concept study. Commercially available polydimethylsiloxane stir bars (Twister™) were used for method development and SBSE extraction (pH, phase ratio, stirring speed, temperature, ionic strength and time) and liquid desorption (solvents, desorption method, stirring time etc) procedures were optimised. The method was validated as per ICH guidelines and was successfully applied for the estimation of diclofenac from three liquid formulations viz. Voltarol(®) Optha single dose eye drops, Voltarol(®) Ophtha multidose eye drops and Voltarol(®) ampoules. The developed method was found to be linear (r=0.9999) over 100-2000ng/ml concentration range with acceptable accuracy and precision (tested over three QC concentrations). The SBSE extraction recovery of the diclofenac was found to be 70% and the LOD and LOQ of the validated method were found to be 16.06 and 48.68ng/ml, respectively. Furthermore, a forced degradation study of a diclofenac formulation leading to the formation of structurally similar cyclic impurity (indolinone) was carried out. The developed extraction method showed comparable results to that of the reference method, i.e. method was capable of selectively extracting the indolinone and diclofenac from the liquid matrix. Data on inter and intra stir bar accuracy and precision further confirmed robustness of the method, supporting the multiple re-use of the stir bars. Copyright © 2010 Elsevier B.V. All rights reserved.

On the role of organic adlayers in the anomalous water sorptivity of Lépine limestone.

PubMed

Ioannou, Ioannis; Hoff, William D; Hall, Christopher

2004-11-01

Sorptivity data are reported for the capillary absorption of water, ethanol, propan-2-ol, and n-heptane by the calcitic limestone Lépine (Lavoux à grain). The data confirm that the water sorptivity is anomalously low, an indication of partial wetting by water. Results are expressed in terms of a wetting index. The water sorptivity increases after heat treatment and chemical oxidation by hydrogen peroxide bleaching, while the sorptivity with organic liquids is unchanged. These treatments, therefore, increase the water wetting index. The results provide strong evidence that the presence of a natural organic adlayer is responsible for the anomalously low water sorptivity of this particular limestone. This natural water repellency effect may be exploited in developing chemical treatments to modify the water transport properties of stone.

A comparison of solid-phase microextraction and stir bar sorptive extraction coupled to liquid chromatography for the rapid analysis of resveratrol isomers in wines, musts and fruit juices.

PubMed

Viñas, Pilar; Campillo, Natalia; Hernández-Pérez, Mónica; Hernández-Córdoba, Manuel

2008-03-17

A comparison of direct immersion solid-phase microextraction (DI-SPME) and stir bar sorptive extraction (SBSE) coupled to liquid chromatography (HPLC) with fluorimetric detection for the rapid analysis of resveratrol isomers is described. For DI-SPME, a polar Carbowax-template resin (CW/TPR) 50mum fiber was the most efficient and optimum extraction conditions were 40 degrees C and an extraction time of 30min, stirring in the presence of 5% (m/v) sodium chloride and 0.07M acetate/acetic acid buffer (pH 6). Desorption was carried out using the static mode for 10min. Linearity was obtained in the 5-150 and 2-150ngmL(-1) ranges for trans- and cis-resveratrol, with detection limits of 2 and 0.5ngmL(-1), respectively. When using SBSE, a polydimethylsiloxane (PDMS) twister provided best extraction by means of a derivatization reaction in the presence of acetic anhydride and potassium carbonate. The same time and temperature were used for the extraction step in the presence of 2.5% (m/v) sodium chloride, and liquid desorption was performed with 150microL of a 50/50 (v/v) acetonitrile/1% (v/v) acetic acid solution in a desorption time of 15min. Linearity was now between 0.5 and 50ngmL(-1) for trans-resveratrol with a detection limit of 0.1ngmL(-1), while cis-resveratrol could not be extracted. The proposed methods were successfully applied to determining the resveratrol isomer content of wine, must and fruit juices.

Use of experimental design in the investigation of stir bar sorptive extraction followed by ultra-high-performance liquid chromatography-tandem mass spectrometry for the analysis of explosives in water samples.

PubMed

Schramm, Sébastien; Vailhen, Dominique; Bridoux, Maxime Cyril

2016-02-12

A method for the sensitive quantification of trace amounts of organic explosives in water samples was developed by using stir bar sorptive extraction (SBSE) followed by liquid desorption and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The proposed method was developed and optimized using a statistical design of experiment approach. Use of experimental designs allowed a complete study of 10 factors and 8 analytes including nitro-aromatics, amino-nitro-aromatics and nitric esters. The liquid desorption study was performed using a full factorial experimental design followed by a kinetic study. Four different variables were tested here: the liquid desorption mode (stirring or sonication), the chemical nature of the stir bar (PDMS or PDMS-PEG), the composition of the liquid desorption phase and finally, the volume of solvent used for the liquid desorption. On the other hand, the SBSE extraction study was performed using a Doehlert design. SBSE extraction conditions such as extraction time profiles, sample volume, modifier addition, and acetic acid addition were examined. After optimization of the experimental parameters, sensitivity was improved by a factor 5-30, depending on the compound studied, due to the enrichment factors reached using the SBSE method. Limits of detection were in the ng/L level for all analytes studied. Reproducibility of the extraction with different stir bars was close to the reproducibility of the analytical method (RSD between 4 and 16%). Extractions in various water sample matrices (spring, mineral and underground water) have shown similar enrichment compared to ultrapure water, revealing very low matrix effects. Copyright © 2016 Elsevier B.V. All rights reserved.

Sorptive extraction using polydimethylsiloxane/metal-organic framework coated stir bars coupled with high performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

PubMed

Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

2014-08-22

In this work, metal-organic frameworks (MOFs, Al-MIL-53-NH₂) were synthesized via the hydrothermal method, and novel polydimethylsiloxane/metal-organic framework (PDMS/MOFs, PDMS/Al-MIL-53-NH₂)-coated stir bars were prepared by the sol-gel technique. The preparation reproducibility of the PDMS/MOFs-coated stir bar was good, with relative standard deviations (RSDs) ranging from 4.8% to 14.9% (n=7) within one batch and from 6.2% to 16.9% (n=6) among different batches. Based on this fact, a new method of PDMS/MOFs-coated stir bar sorptive extraction (SBSE) and ultrasonic-assisted liquid desorption (UALD) coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. To obtain the best extraction performance for PAHs, several parameters affecting SBSE, such as extraction time, stirring rate, and extraction temperature, were investigated. Under optimal experimental conditions, wide linear ranges and good RSDs (n=7) were obtained. With enrichment factors (EFs) of 16.1- to 88.9-fold (theoretical EF, 142-fold), the limits of detection (LODs, S/N=3) of the developed method for the target PAHs were found to be in the range of 0.05-2.94 ng/L. The developed method was successfully applied to the analysis of PAHs in Yangtze River and East Lake water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Double-disk solid-phase extraction--Simultaneous cleanup and trace enrichment of herbicides and metabolites from environmental samples

USGS Publications Warehouse

Ferrar, Imma; Barceló, Damià; Thurman, E.M.

1999-01-01

Phenylurea and triazine herbicides, including some metabolites, were isolated from water and soil extracts by solid-phase extraction using a layered system of two extraction disks, a method called double-disk solid-phase extraction. The first disk consisted of strong anion exchange (SAX) of 10-μm styrene divinylbenzene (SDB) particles embedded in Teflon, and the second disk was a C18 disk of 10-μm particles also embedded in Teflon. A volume of 500 mL of water or aqueous soil extract is passed through the layered system with the SAX disk first. The purpose of the SAX disk is to remove the humic and fulvic acids from the water or aqueous soil extract by ion exchange through their carboxyl groups. Even during methanol elution of herbicides, the humic substances remain bound to the SAX disk with >85% retention. Elution with methanol results in more than 90% recovery of the herbicides from the layered extraction disks. Removal of the humic and fulvic acids results in greater sensitivity for diode array detection quantitation (0.05 μg/L for herbicides) by substantially reducing the absorbance of the humic peak on the LC chromatogram. The herbicides adsorb to the SAX disk either through hydrogen bonding to the anion-exchange sites or by hydrophobic interaction with the SDB surface of the anion-exchange disk. The method was tested for the analysis of natural water samples from the Mississippi Embayment, a cotton-growing area of the southeastern United States.

Polydimethylsiloxane/metal-organic frameworks coated stir bar sorptive extraction coupled to high performance liquid chromatography-ultraviolet detector for the determination of estrogens in environmental water samples.

PubMed

Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

2013-10-04

In this work, three kinds of metal-organic frameworks (MOFs), MOF-5, MOF-199 and IRMOF-3, were introduced in stir bar sorptive extraction (SBSE) and novel polydimethylsiloxane (PDMS)/MOFs (including PDMS/MOF-5, PDMS/MOF-199 and PDMS/IRMOF-3) coated stir bars were prepared by sol-gel technique. These PDMS/MOFs coatings were characterized and critically compared for the extraction of seven target estrogens (17-β-estradiol, dienestrol, diethylstilbestrol, estrone, 4-t-octylphenol, bisphenol-A and 17α-ethynylestradiol) by SBSE, and the results showed that PDMS/IRMOF-3 exhibited highest extraction efficiency. Based on the above facts, a novel method of PDMS/IRMOF-3 coating SBSE-high performance liquid chromatography ultraviolet (HPLC-UV) detection was developed for the determination of seven target estrogens in environmental waters. Several parameters affecting extraction of seven target estrogens by SBSE (PDMS/IRMOF-3) including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.15-0.35 μg/L. The linear range was 2-2,500 μg/L for 17α-ethynylestradiol and 1-2,500 μg/L for other estrogens. The relative standard deviations (RSDs) were in the range of 3.7-9.9% (n=8, c=20 μg/L) and the enrichment factors were from 30.3 to 55.6-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of estrogens in environmental water samples, and quantitative recoveries were obtained for the spiking experiments. Copyright © 2013 Elsevier B.V. All rights reserved.

Stir bar sorptive extraction approaches with a home-made portable electric stirrer for the analysis of polycyclic aromatic hydrocarbon compounds in environmental water.

PubMed

Mao, Xiangju; Hu, Bin; He, Man; Fan, Wenying

2012-10-19

In this study, novel off/on-site stir bar sorptive extraction (SBSE) approaches with a home-made portable electric stirrer have been developed for the analysis of polycyclic aromatic hydrocarbon compounds (PAHs). In these approaches, a miniature battery-operated electric stirrer was employed to provide agitation of sample solutions instead of the commonly used large size magnetic stirrer powered by alternating current in conventional SBSE process, which could extend the SBSE technique from the conventional off-site analysis to the on-site sampling. The applicability of the designed off/on-site SBSE sampling approaches was evaluated by polydimethylsiloxane (PDMS) coating SBSE-high performance liquid chromatography-fluorescence detection (HPLC-FLD) analysis of six target PAHs in environmental water. The home-made portable electric stirrer is simple, easy-to-operate, user friendly, low cost, easy-to-be-commercialized, and can be processed in direct immersion SBSE, headspace sorptive extraction (HSSE) and continuous flow (CF)-SBSE modes. Since the stir bar was fixed onto the portable device by magnetic force, it is very convenient to install, remove and replace the stir bar, and the coating friction loss which occurred frequently in conventional SBSE process could be avoided. The parameters affecting the extraction of six target PAHs by the home-made portable SBSE sampling device with different sampling modes were studied. Under the optimum extraction conditions, good linearity was obtained by all of three SBSE extraction modes with correlation coefficient (R) higher than 0.9971. The limits of detection (LODs, S/N=3) were 0.05-3.41 ng L(-1) for direct immersion SBSE, 0.03-2.23 ng L(-1) for HSSE and 0.09-3.75 ng L(-1) for CF-SBSE, respectively. The proposed portable PDMS-SBSE-HPLC-FLD method was applied for the analysis of six target PAHs in East Lake water, and the analytical results obtained by on-site SBSE sampling were in good agreement with that obtained by off-site SBSE sampling. The accuracy of the developed method was evaluated by recovery test and the recoveries for the spiked sample were found to be in the range of 87.1-122.8% for off-site CF-SBSE, 88.8-114.3% for on-site sampling, and 87.7-123.6% for off-site SBSE, respectively. The developed method is one of the most sensitive methods for PAHs determination and the home-designed SBSE system is feasible for the field sampling. Copyright © 2012 Elsevier B.V. All rights reserved.

Stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry: an effective tool for determining persistent organic pollutants and nonylphenol in coastal waters in compliance with existing Directives.

PubMed

Sánchez-Avila, Juan; Quintana, Jordi; Ventura, Francesc; Tauler, Romà; Duarte, Carlos M; Lacorte, Silvia

2010-01-01

A multi-residual method based on stir bar sorptive extraction coupled with thermal desorption-gas chromatography-mass spectrometry (SBSE-TD-GC-MS) has been developed to measure 49 organic pollutants (organochlorine pesticides, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, polybrominated diphenyl ethers and nonylphenol) in seawater. Using 100ml of water, the method exhibited good linearity, with recoveries between 86% and 118% and relative standard deviation between 2% and 24% for almost all compounds. The method was applied to determine target contaminants in Catalonian seawater, including coastal areas, ports and desalination plant feed water. Overall individual compound levels oscillated between 0.16 and 597 ng l(-1); PAHs and nonylpenol were the compounds found at the highest concentrations. The method provided LODs between 0.011 and 2.5 ng l(-1), lower than the Environmental Quality Standards (EQS) fixed by Directive 2008/105/EC. In compliance with the directive, this method can be used as a tool to survey target compounds and is aimed at protecting coastal ecosystems from chemical pollution. Copyright 2009 Elsevier Ltd. All rights reserved.

Influence of polydimethylsiloxane outer coating and packing material on analyte recovery in dual-phase headspace sorptive extraction.

PubMed

Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Sgorbini, Barbara; David, Frank; Sandra, Pat; Rubiolo, Patrizia

2007-09-14

Dual phase twisters (DP twisters), consisting of a polydimethylsiloxane (PDMS) outer coating and a second complementary (ad)sorbent as inner packing, have recently been shown to extend the applicability of headspace sorptive extraction (HSSE). In comparison to HSSE using PDMS only, the recovery of analytes from the headspace of a solid or liquid matrix is increased by combining the concentration capabilities of two sampling materials operating on different mechanisms (sorption and adsorption). This study compares the performance of DP twisters consisting of different PDMS outer coatings and different packing materials, including Tenax GC, a bisphenol-PDMS copolymer, Carbopack coated with 5% of Carbowax and beta-cyclodextrin, for the analysis of the headspace of roasted Arabica coffee, dried sage leaves and an aqueous test mixture containing compounds with different water solubility, acidity, polarity and volatility as test samples. In general, DP twisters showed a higher concentration capability than the corresponding conventional PDMS twisters for the analytes considered. The highest recoveries were obtained with DP twisters consisting of 0.2mm thick PDMS coating combined with Tenax GC, a bisphenol-PDMS copolymer and Carbopack coated with 5% of Carbowax as inner adsorption phase.

Continental bottled water assessment by stir bar sorptive extraction followed by gas chromatography-tandem mass spectrometry (SBSE-GC-MS/MS).

PubMed

Guart, Albert; Calabuig, Ignacio; Lacorte, Silvia; Borrell, Antonio

2014-02-01

This study was aimed to determine the presence of 69 organic contaminants in 77 representative bottled waters collected from 27 countries all over the world. All water samples were contained in polyethylene terephthalate bottles. Target compounds were (1) environmental contaminants (including 13 polycyclic aromatic hydrocarbons (PAHs), 31 pesticides including organochlorine (OCPs), organophosphorus, and pyrethroids; 7 polychlorinated biphenyls (PCBs); and 7 triazines) and (2) plasticizers (including 6 phthalates and 5 other compounds). Samples were analyzed by stir bar sorptive extraction followed by gas chromatography-tandem mass spectrometry. PAHs, OCPs, PCBs, and triazines, which are indicators of groundwater pollution, were not detected in most of the samples, except for naphthalene (0.005-0.202 μg/L, n = 16). On the other hand, plastic components were detected in 77 % of the samples. Most frequently detected compounds were dimethyl phthalate and benzophenone at concentrations of 0.005-0.125 (n = 41) and 0.014-0.921 (n = 32), respectively. Levels detected are discussed in terms of contamination origin and geographical distribution. Target compounds were detected at low concentrations. Results obtained showed the high quality of bottled water in the different countries around the world.

Sorptive tape extraction in the analysis of the volatile fraction emitted from biological solid matrices.

PubMed

Bicchi, C; Cordero, C; Liberto, E; Rubiolo, P; Sgorbini, B; Sandra, P

2007-05-04

Sorptive tape extraction (STE) is a recent sorption-based sampling technique in which a flexible polydimethylsiloxane (PDMS) tape is used to recover analytes at the surface of a solid matrix by direct contact as well as from the headspace in equilibrium with it. Solutes thus enriched on the inert PDMS material can be recovered either by solvent desorption or by thermo-desorption. The concentration capability of both direct contact and headspace STE was evaluated by sampling (a) aromatic plants to study the reaction of a vegetable matrix submitted to stress, and (b) fruits at the surface of the pulp or inside the pulp; the composition of the volatile fraction released from the skin when a perfume is sprayed on the back of the hand was also studied. The concentration capability of direct contact and headspace STE was compared to that of HSSE with a 20 microL PDMS twister and HS-SPME with a PDMS 100 microm fibre, by determining the relative abundances (RA) of the characterizing components of the aromatic plants under investigation. Repeatability and influence of tape surface on STE recovery were also evaluated.

Optimum Installation of Sorptive Building Materials Using Contribution Ratio of Pollution Source for Improvement of Indoor Air Quality.

PubMed

Park, Seonghyun; Seo, Janghoo

2016-04-01

Reinforcing the insulation and airtightness of buildings and the use of building materials containing new chemical substances have caused indoor air quality problems. Use of sorptive building materials along with removal of pollutants, constant ventilation, bake-out, etc. are gaining attention in Korea and Japan as methods for improving such indoor air quality problems. On the other hand, sorptive building materials are considered a passive method of reducing the concentration of pollutants, and their application should be reviewed in the early stages. Thus, in this research, activated carbon was prepared as a sorptive building material. Then, computational fluid dynamics (CFD) was conducted, and a method for optimal installation of sorptive building materials was derived according to the indoor environment using the contribution ratio of pollution source (CRP) index. The results show that a method for optimal installation of sorptive building materials can be derived by predicting the contribution ratio of pollutant sources according to the CRP index.

Analysis of 2-Acetyl-1-Pyrroline in rice by HSSE/GC/MS.

USDA-ARS?s Scientific Manuscript database

An alternative method for the analysis of 2-acetyl-1-pyrroline (2AP) in rice employing stir bar sorptive extraction (Twister™), is described. The Twister stir bar is placed in the headspace of a 20 ml vial containing 1 g rice kernels, 5 ml 0.1 M KOH, 2,2 g NaCl, and a second Teflon™ coated stir bar...

Etched poly(ether ether ketone) jacket stir bar with detachable dumbbell-shaped structure for stir bar sorptive extraction.

PubMed

Zhou, Wei; Wang, Chenlu; Wang, Xuemei; Chen, Zilin

2018-06-08

Development of stir bar sorptive extraction (SBSE) device with high stability and extraction efficiency is critical and challenging by date. In this work, etched poly(ether ether ketone) (PEEK) tube with high mechanical strength and large specific surface area was used as jacket for SBSE device. By etching with concentrated sulfuric acid, the smooth outer surface of PEEK become porous with plenty of micro holes, which was beneficial for coating of sorbents and significantly improved the extraction performance. After functionalized by bio-polydopamine method, strong hydrophobic p-naphtholbenzein molecular was immobilized onto the chemical resistant PEEK surface (PNB@E-PEEK) as stationary phase. We also firstly developed a simple detachable dumbbell-shaped structure for improving the workability of PEEK jacket stir bar. The dumbbell-shaped construction can eliminate the friction between stir bar and container, and the design of detachable structure make elution can be accomplished easier with small amount of organic solvent. It was interesting that the developed detachable dumbbell-shaped PNB@E-PEEK stir bar showed exceptional stability and extraction efficiency for SBSE enrichment of multiple analytes including several Sudan dyes, triazines, polycyclic aromatic hydrocarbons (PAHs), alkaloids and flavonoid. By coupling with high performance liquid chromatography-ultraviolet detection (HPLC-UV), PNB@E-PEEK stir bar based SBSE-HPLC-UV method was applied for the analysis of common Sudan dye pollutants. The method showed low limits of detection (0.02-0.03 ng/mL), good linearity (R 2  ≥ 0.9979) and good reproducibility (relative standard deviation ≤ 7.96%). It has been successfully applied to determine three dye pollutants in tap and lake water. Copyright © 2018 Elsevier B.V. All rights reserved.

Polydimethylsiloxane/MIL-100(Fe) coated stir bar sorptive extraction-high performance liquid chromatography for the determination of triazines in environmental water samples.

PubMed

Lei, Yun; Chen, Beibei; You, Linna; He, Man; Hu, Bin

2017-12-01

Polydimethylsiloxane (PDMS)/MIL-100(Fe) coated stir bar was prepared by sol gel technique, and good preparation reproducibility was achieved with relative standard deviations (RSDs) ranging from 2.6% to 7.5% (n=7) and 3.6% to 10.8% (n=7) for bar-to-bar and batch-to-batch, respectively. Compared with commercial PDMS coated stir bar (Gerstel) and PEG coated stir bar (Gerstel), the prepared PDMS/MIL-100(Fe) stir bar showed better extraction efficiency for target triazines compounds. It also exhibited relatively fast extraction/desorption kinetics and long lifespan. Based on it, a method of PDMS/MIL-100(Fe) coated stir bar sorptive extraction (SBSE)-high performance liquid chromatography-ultraviolet detector (HPLC-UV) was developed for the determination of six triazines (simazine, atrazine, prometon, ametryn, prometryne and prebane) in environmental water samples. Several parameters affecting SBSE of six target triazines including extraction time, stirring rate, sample pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.021-0.079μgL -1 . The repeatability RSDs were in the range of 2.3-6.3% (n=7, c=0.5μgL -1 ) and the enrichment factors (EFs) ranged from 51.1 to 102-fold (theoretical EF was 200-fold). The proposed method was applied to the analysis of target triazines in environmental water samples, with recoveries of 98.0-118% and 94.0-107% for spiked East Lake water and local pond water samples, respectively. Copyright © 2017. Published by Elsevier B.V.

A new solid-phase extraction disk based on a sheet of single-walled carbon nanotubes.

PubMed

Niu, Hong Yun; Cai, Ya Qi; Shi, Ya Li; Wei, Fu Sheng; Liu, Jie Min; Jiang, Gui Bin

2008-11-01

A new kind of solid-phase extraction disk based on a sheet of single-walled carbon nanotubes (SWCNTs) is developed in this study. The properties of such disks are tested, and different disks showed satisfactory reproducibility. One liter of aqueous solution can pass through the disk within 10-100 min while still allowing good recoveries. Two disks (DD-disk) can be stacked to enrich phthalate esters, bisphenol A (BPA), 4-n-nonylphenol (4-NP), 4-tert-octylphenol (4-OP) and chlorophenols from various volumes of solution. The results show that SWCNT disks have high extraction ability for all analytes. The SWCNT disk can extract polar chlorophenols more efficiently than a C(18) disk from water solution. Unlike the activated carbon disk, analytes adsorbed by the new disks can be eluted completely with 8-15 mL of methanol or acetonitrile. Finally, the DD-disk system is used to pretreat 1000-mL real-world water samples spiked with BPA, 4-OP and 4-NP. Detection limits of 7, 25, and 38 ng L(-1) for BPA, 4-OP, and 4-NP, respectively, were achieved under optimized conditions. The advantages of this new disk include its strong adsorption ability, its high flow rate and its easy preparation.

An alternative method for analysis of food taints using stir bar sorptive extraction.

PubMed

Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

2010-09-10

The determination of taints in food products currently can involve the use of several sample extraction techniques, including direct headspace (DHS), steam distillation extraction (SDE) and more recently solid phase microextraction (SPME). Each of these techniques has disadvantages, such as the use of large volumes of solvents (SDE), or limitations in sensitivity (DHS), or have only been applied to date for determination of individual or specific groups of tainting compounds (SPME). The use of stir bar sorptive extraction (SBSE) has been evaluated as a quantitative screening method for unknown tainting compounds in foods. A range of commonly investigated problem compounds, with a range of physical and chemical properties, were examined. The method was optimised to give the best response for the majority of compounds and the performance was evaluated by examining the accuracy, precision, linearity, limits of detection and quantitation and uncertainties for each analyte. For most compounds SBSE gave the lowest limits of detection compared to steam distillation extraction or direct headspace analysis and in general was better than these established techniques. However, for methyl methacrylate and hexanal no response was observed following stir bar extraction under the optimised conditions. The assays were carried out using a single quadrupole GC-MS in scan mode. A comparison of acquisition modes and instrumentation was performed using standards to illustrate the increase in sensitivity possible using more targeted ion monitoring or a more sensitive high resolution mass spectrometer. This comparison illustrated the usefulness of this approach as an alternative to specialised glassware or expensive instrumentation. SBSE in particular offers a 'greener' extraction method by a large reduction in the use of organic solvents and also minimises the potential for contamination from external laboratory sources, which is of particular concern for taint analysis. Copyright © 2010 Elsevier B.V. All rights reserved.

Determination of tributyltin in environmental water matrices using stir bar sorptive extraction with in-situ derivatisation and large volume injection-gas chromatography-mass spectrometry.

PubMed

Neng, N R; Santalla, R P; Nogueira, J M F

2014-08-01

Stir bar sorptive extraction with in-situ derivatization using sodium tetrahydridoborate (NaBH4) followed by liquid desorption and large volume injection-gas chromatography-mass spectrometry detection under the selected ion monitoring mode (SBSE(NaBH4)in-situ-LD/LVI-GC-MS(SIM)) was successfully developed for the determination of tributyltin (TBT) in environmental water matrices. NaBH4 proved to be an effective and easy in-situ speciation agent for TBT in aqueous media, allowing the formation of adducts with enough stability and suitable polarity for SBSE analysis. Assays performed on water samples spiked at the 10.0μg/L, yielded convenient recoveries (68.2±3.0%), showed good accuracy, suitable precision (RSD<9.0%), low detection limits (23ng/L) and excellent linear dynamic range (r(2)=0.9999) from 0.1 to 170.0µg/L, under optimized experimental conditions. By using the standard addition method, the application of the present methodology to real surface water samples allowed very good performance at the trace level. The proposed methodology proved to be a feasible alternative for routine quality control analysis, easy to implement, reliable and sensitive to monitor TBT in environmental water matrices. Copyright © 2014 Elsevier B.V. All rights reserved.

High polar organic-inorganic hybrid coating stir bar sorptive extraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of seleno-amino acids and seleno-oligopeptides in biological samples.

PubMed

Mao, Xiangju; Hu, Bin; He, Man; Chen, Beibei

2012-09-21

In this work, partially sulfonated polystyrene-titania (PSP-TiO(2)) organic-inorganic hybrid stir bar coating was prepared by sol-gel and blending methods, and a new method of PSP-TiO(2) coating stir bar sorptive extraction (SBSE)-high performance liquid chromatography (HPLC)-inductively coupled plasma mass spectrometry (ICP-MS) was established for the analysis of seleno-amino acids (selenocystine (SeCys(2)), methylseleno-cysteine (MeSeCys), selenomethionine (SeMet) and selenoethionine (SeEt)) and seleno-oligopeptides (γ-glutamyl-Se-methyl-selenocysteine (γ-GluMeSeCys) and selenodiglutathione (GS-Se-SG)) in biological samples. The prepared high polar PSP-TiO(2) hybrid coating avoided the swelling of PSP and cracking of TiO(2) coating by combining the good film-forming property of PSP with the high mechanical strength of TiO(2). The scanning electron microscope (SEM) showed that no obvious swelling and damage occurred for the PSP-TiO(2) hybrid stir bar coating after 30 extraction/desorption cycles. The preparation reproducibility of PSP-TiO(2) coated stir bar, evaluated with the relative standard deviations (RSDs), was in the range of 6.7-12.6% (n=5) in one batch, and 9.9-17.6% (n=7) among different batches. The limits of detection (LODs) of the developed method for six target selenium species were in the range of 50.2-185.5 ngL(-1) (as (77)Se) and 45.9-158.8 ngL(-1) (as (82)Se) with the RSDs within 4.9-11.7%. The dynamic linear range was found to cover three orders of magnitude with correlation coefficient of 0.9995-0.9999. The developed method was applied for the analysis of Certified Reference Material SELM-1 selenium enriched yeast and the determined values were in good agreement with the certified values. The method has also been applied for the analysis of seleno-amino acids and seleno-oligopeptides in human urine and garlic samples. Different from the conventional organic polymer SBSE coatings (such as polydimethylsiloxane, PDMS), the extraction mechanism of PSP-TiO(2) organic-inorganic hybrid SBSE coating was based on the cation exchange interaction, which made it feasible to directly extract high polar seleno-amino acids and seleno-oligopeptides in biological samples without derivatization. This coating could also be suitable for stir bar sorptive extraction of other cationic compounds from the environmental and biological samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Optimization and application of fabric phase sorptive extraction coupled to ultra-high performance liquid chromatography tandem mass spectrometry for the determination of cytostatic drug residues in environmental waters.

PubMed

Santana-Viera, Sergio; Guedes-Alonso, Rayco; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan; Kabir, Abuzar; Furton, Kenneth G

2017-12-22

Every year, hundreds of tons of organic pollutants reach the environment through effluents released from wastewater treatment plants worldwide, and many of these compounds have harmful effects on the aquatic ecosystem. A new class of emerging pollutants of high concern is cytostatic drugs, which are designed to treat different types of cancers by attacking cells. Environmental concentrations of cytostatic drugs are known to be in the range of ngL -1 , and for this reason, it is imperative to develop analytical methods of extraction and preconcentration to allow for subsequent instrumental analysis of these drugs. In this work, a rapid, simple and green method for the analysis of seven cytostatic drug compounds that are commonly used in anti-cancer therapies was developed using a novel extraction process based on a powerful miniaturized technique, fabric phase sorptive extraction (FPSE) coupled to ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The major parameters that affect the extraction process were optimized. The new method shows good linearity, with a relative standard deviation (RSD) of less than 12%. Relative recoveries higher than 40% were obtained for the studied compounds, and the detection limit of the method was within the values at which these compounds are usually found in environmental water (0.20ngL -1 to 80ngL -1 ). The Limit of Quantification ranged from 0.68 to 267ngL -1 . Significant suppression of the signal due to the matrix effect, a common shortcoming attributed to interference from the extraction process as well as the use of ionization mode, was not observed. Subsequently, the method was applied to real wastewater samples from an effluent obtained from a hospital area and three wastewater treatment plants located in Gran Canaria Island, Spain. Copyright © 2017 Elsevier B.V. All rights reserved.

In-port derivatization coupled to different extraction techniques for the determination of alkylphenols in environmental water samples.

PubMed

Cavalheiro, J; Monperrus, M; Amouroux, D; Preud'Homme, H; Prieto, A; Zuloaga, O

2014-05-02

Large volume injection (LVI)-in port silylation coupled to gas chromatography-mass spectrometry (GC-MS) for the determination of alkylphenols (APs) in water samples applying four different extraction approaches was evaluated. Among the variables studied for in-port derivatization, vent time, cryo-focusing temperature and the ratio solvent volume/N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) volume were optimized using an experimental design approach. Regarding the extraction techniques, different approaches previously optimized in the research group were tested. On the one hand different polymeric materials were tested: silicon rod (SR), polyethersulfone (PES) and polydimethylsiloxane (PDMS), the latter in the stir-bar sorptive extraction format (SBSE-PDMS). PES was chosen among the polymeric materials due to the higher recoveries (compared with SR) and lower price (compared to PDMS in the stir-bar sorptive extraction, SBSE-PDMS). Both MASE and PES protocols were selected at this point for further method validation and application to real samples. Finally, the developed methods were validated and applied to the determination of target analytes in various aqueous environmental matrices, including estuarine water and wastewater. Acceptable repeatability in the case of MASE (5-17%) and PES (7-21%) procedures and method detection limits (MDLs, 5-123 and 28-328 ng L(-1) for PES and MASE, respectively) were obtained for most analytes. In terms of apparent recoveries in the presence of matrix, estuarine and effluent samples showed no significant matrix effect (apparent recoveries in the 73-121% for PES and 74-128% for MASE), while a stronger matrix effect was observed for influent wastewater samples (98-132% for PES and 65-156% for MASE). Both MASE and PES extractions combined with LVI-in-port derivatization-GC-MS were applied to the determination of APs in the estuary of Bilbao (Gulf of Biscay, Spain). Copyright © 2014 Elsevier B.V. All rights reserved.

Polydimethylsiloxane rod extraction, a novel technique for the determination of organic micropollutants in water samples by thermal desorption-capillary gas chromatography-mass spectrometry.

PubMed

Montero, L; Popp, P; Paschke, A; Pawliszyn, J

2004-01-30

A novel, simple and inexpensive approach to absorptive extraction of organic compounds from environmental samples is presented. It consists of a polydimethylsiloxane rod used as an extraction media, enriched with analytes during shaking, then thermally desorbed and analyzed by GC-MS. Its performance was illustrated and evaluated for the enrichment of sub- to ng/l of selected chlorinated compounds (chlorobenzenes and polychlorinated biphenyls) in water samples. The new approach was compared to the stir bar sorptive extraction performance. A natural ground water sample from Bitterfeld, Germany, was also extracted using both methods, showing good agreement. The proposed approach presented good linearity, high sensitivity, good blank levels and recoveries comparable to stir bars, together with advantages such as simplicity, lower cost and higher feasibility.

New biomimetic approach to determine the bioavailability of triclosan in soils and its validation with the wheat plant uptake bioassay.

PubMed

Jachero, Lourdes; Ahumada, Inés; Fuentes, Edwar; Richter, Pablo

2015-01-01

A new biomimetic approach for triclosan (TCS) was developed based on the leaching of the analyte from different biosolid-amended agricultural soils and the subsequent extraction of the leachates, using a rotating disk sorptive extraction (RDSE) procedure. The leaching equilibrium for TCS was reached at 3h when the ISO method (ISO/TS 21268-1:2007) was followed. The concentrations determined by this biomimetic method were compared with the bioavailability of TCS, determined by its accumulation in the roots of wheat plants grown in the same soil-biosolid systems. It was observed that the amount of organic matter in the soil matrix was a determining factor for mobilization of TCS. An increasing biosolid rate applied to soils resulted in a reduced mobility of TCS because the high amount of organic matter provided by the biosolid increased the hydrophobic interaction between TCS and the matrix. Similarly, increasing biosolid concentrations in the soil significantly decreased the bioavailability of TCS to the wheat plant. Thus, the bioavailability factor in wheat roots decreased from 0.22 to 0.08 for a soil having a pH of 8.2, when the biosolid rate was increased from 30 to 200 Mg ha(-1), respectively. A significant correlation (R=0.98) was obtained between TCS concentration in wheat plants and the proposed biomimetic methodology, indicating that the latter can predict the bioavailability in a time period as short as 180 min. The results of this study confirm our previous findings that amending soils with biosolids is beneficial for immobilizing low polarity contaminants and helps prevent their percolation through the soil profile and into groundwater. Copyright © 2014 Elsevier Ltd. All rights reserved.

Graphene oxide/polyethyleneglycol composite coated stir bar for sorptive extraction of fluoroquinolones from chicken muscle and liver.

PubMed

Fan, Wenying; He, Man; Wu, Xiaoran; Chen, Beibei; Hu, Bin

2015-10-30

Graphene oxide (GO) is an ideal adsorbent for polar and less polar compounds due to its hexagonal carbon network structure with oxygen-containing groups, while its strong hydrophilicity and water solubility limited its application in sample pretreatment techniques. Herein, GO was composited with polyethyleneglycol (PEG) or polyaniline (PAN) through intermolecular interactions to improve its stability, and the GO/PEG and GO/PAN composite coated stir bars were prepared by sol-gel technique. Compared with GO/PAN composite and polydimethylsiloxane (PDMS) coated stir bar, the prepared GO/PEG composite coated stir bar exhibited higher extraction efficiency for five fluoroquinolones (FQs). Based on it, a method of GO/PEG composite coated stir bar sorptive extraction (SBSE) combined with high-performance liquid chromatography-fluorescence detector (HPLC-FLD) was proposed. The factors influencing SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-FLD method was evaluated. The limits of detection (LODs) for five FQs were in the range of 0.0045-0.0079μgL(-1), and the enrichment factors (EFs) were in the range of 41.5-65.5-fold (theoretical enrichment factor was 100-fold). The reproducibility was also investigated at concentrations of 0.05μgL(-1) and the relative standard deviations (RSDs, n=6) were found to be in the range of 4.6-12.1%. The proposed method was successfully applied for the determination of FQs in chicken muscle and chicken liver samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of novel sol-gel coatings by chemically bonded ionic liquids for stir bar sorptive extraction--application for the determination of NSAIDS in real samples.

PubMed

Fan, Wenying; Mao, Xiangju; He, Man; Chen, Beibei; Hu, Bin

2014-11-01

In this work, a novel ionic liquid (IL) chemically bonded sol-gel coating was prepared for stir bar sorptive extraction (SBSE) of nonsteroidal anti-inflammatory drugs (NSAIDs) followed by high-performance liquid chromatography-ultraviolet detection (HPLC-UV). By using γ-(methacryloxypropyl)trimethoxysilane (KH-570) as a bridging agent, 1-allylimidazolium tetrafluoroborate ([AIM][BF4]) was chemically bonded onto the bare stir bar, and the prepared IL-bonded sol-gel stir bar coating showed higher extraction efficiency and better adsorption/desorption kinetics for target NSAIDs over other polydimethylsiloxane (PDMS)-based or monolithic stir bar coatings. The mechanical strength and durability (chemical/thermal stability) of the prepared IL-bonded sol-gel coating were excellent. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent, and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limits of detection (LODs) of the proposed method for three NSAIDs were in the range of 0.23-0.31 μg L(-1), and the enrichment factors (EFs) were in the range of 51.6-56.3 (theoretical enrichment factor was 100). The reproducibility was also investigated at concentrations of 5, 20, and 100 μg L(-1), and the relative standard deviations (RSDs) were found to be less than 9.5, 7.5, and 7.6 %, respectively. The proposed method was successfully applied for the determination of NSAIDs in environmental water, urine, and milk samples.

Multiresidue analysis of acidic and polar organic contaminants in water samples by stir-bar sorptive extraction-liquid desorption-gas chromatography-mass spectrometry.

PubMed

Quintana, José Benito; Rodil, Rosario; Muniategui-Lorenzo, Soledad; López-Mahía, Purificación; Prada-Rodríguez, Darío

2007-12-07

The feasibility of stir-bar sorptive extraction (SBSE) followed by liquid desorption in combination with large volume injection (LVI)-in port silylation and gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of a broad range of 46 acidic and polar organic pollutants in water samples has been evaluated. The target analytes included phenols (nitrophenols, chlorophenols, bromophenols and alkylphenols), acidic herbicides (phenoxy acids and dicamba) and several pharmaceuticals. Experimental variables affecting derivatisation yield and peak shape as a function of different experimental PTV parameters [initial injection time, pressure and temperature and the ratio solvent volume/N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) volume] were first optimised by an experimental design approach. Subsequently, SBSE conditions, such as pH, ionic strength, agitation speed and extraction time were investigated. After optimisation, the method failed only for the extraction of most polar phenols and some pharmaceuticals, being suitable for the determination of 37 (out of 46) pollutants, with detection limits for these analytes ranging between 1 and 800 ng/L and being lower than 25 ng/L in most cases. Finally, the developed method was validated and applied to the determination of target analytes in various aqueous environmental matrices, including ground, river and wastewater. Acceptable accuracy (70-130%) and precision values (<20%) were obtained for most analytes independently of the matrix, with the exception of some alkylphenols, where an isotopically labelled internal standard would be required in order to correct for matrix effects. Among the drawbacks of the method, carryover was identified as the main problem even though the Twisters were cleaned repeatedly.

Validation of a GC-MS/MS method for simultaneous determination of 86 persistent organic pollutants in marine sediments by pressurized liquid extraction followed by stir bar sorptive extraction.

PubMed

Camino-Sánchez, F J; Zafra-Gómez, Alberto; Pérez-Trujillo, J P; Conde-González, J E; Marques, J C; Vílchez, José Luis

2011-08-01

A multiresidue method for the analysis of 86 persistent pollutants in marine sediments at ultra-trace level has been developed and validated using pressurized liquid extraction (PLE) and stir-bar sorptive extraction (SBSE) coupled with thermal desorption and gas chromatography-triple quadrupole mass spectrometry (TD-GC-MS/MS QqQ). The compounds analyzed belong to various families such as polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenylethers, organophosphorus and organochlorine pesticides and other pesticides such as urons, and triazines. The analytes have very different polarities and log K(ow) values, which is an important parameter in the optimization of a SBSE method. Due to PLE high efficiency and throughput rates, along with the proven ability for multiresidue analysis and excellent sensitivity of SBSE, we present an efficient method. The limits of quantification obtained ranged from 0.014 to 1.0 ng g(-1), with detection limits below pg g(-1) levels. In order to validate the proposed methodology, quality parameters such as recovery, linearity and reproducibility were studied. Recoveries ranged from 63% to 119%, reproducibility (in terms of Relative Standard Deviation for ten determinations) was lower than 35% in all cases, and determination coefficients higher than 0.990 for all analytes. The main factors that affect PLE, SBSE and GC-MS/MS procedures were optimized. The method was applied to the analysis of nine marine sediments obtained from the nine main submarine wastewater discharge points (emissaries) presents along the coast of Tenerife Island (Canary Islands, Spain). Copyright © 2011 Elsevier Ltd. All rights reserved.

Polyaniline/cyclodextrin composite coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detection for the analysis of trace polychlorinated biphenyls in environmental waters.

PubMed

Lei, Yun; He, Man; Chen, Beibei; Hu, Bin

2016-04-01

A novel polyaniline/α-cyclodextrin (PANI/α-CD) composite coated stir bar was prepared by sol-gel process for the analysis of polychlorinated biphenyls (PCBs) in this work. The preparation reproducibility of the PANI/α-CD-coated stir bar was good, with relative standard deviations (RSDs) ranging from 2.3% to 3.7% (n=7) and 2.0% to 3.8% (n=7) for bar to bar and batch to batch, respectively. Based on it, a novel method of PANI/α-CD-coated stir bar sorptive extraction (SBSE) followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for the determination of trace PCBs in environmental waters. To obtain the best extraction performance for target PCBs, several parameters affecting SBSE, such as extraction time, stirring rate, and ionic strength were investigated. Under optimal experimental conditions, the limits of detection (LODs) of the proposed method for seven PCBs were in the range of 0.048-0.22 μg/L, and the RSDs were 5.3-9.8% (n=7, c=1 μg/L). Enrichment factors (EFs) ranging from 39.8 to 68.4-fold (theoretical EF, 83.3-fold) for target analytes were achieved. The proposed method was successfully applied for the determination of seven target PCBs in Yangtze River water and East Lake water, and the recoveries were in the range of 73.0-120% for the spiked East Lake water samples and 82.7-121% for the spiked Yangtze River water samples, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of alkylphenols and phthalate esters in vegetables and migration studies from their packages by means of stir bar sorptive extraction coupled to gas chromatography-mass spectrometry.

PubMed

Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

2012-06-08

This paper describes a method for the determination of three alkylphenols (APs), 4-tert-octylphenol (tOP), 4-n-octylphenol (OP) and 4-nonylphenol (NP), and six phthalate esters (PEs), dimethylphthalate (DMP), diethylphthalate (DEP), di-n-butylphthalate (DBP), n-butylbenzylphthalate (BBP), di-2-ethylhexylphthalate (DEHP) and di-n-octylphthalate (DOP), in vegetables using stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Ultrasonic radiation was used to extract the analytes from the solid food matrix, and the extract obtained was preconcentrated by SBSE. The different parameters affecting both stages were carefully optimized. The method was applied to analyze commercial vegetables, in the form of plastic packed salads and canned greens, as well as the corresponding filling liquids of the canned food. Quantification of the samples was carried out against aqueous standards using an internal standard (anthracene). The analysis of a 2 g vegetable sample provided detection limits between 12.7 and 105.8 pg g⁻¹ for OP and DEHP, respectively. Migration studies from the plastic packages of the vegetables samples analyzed were carried out. DEP, DBP and DEHP were found to have migrated from the bags to the simulant and the same compounds were quantified in lettuce, corn salad, arugula, parsley and chard, at concentration levels in the 8-51 ng g⁻¹ range. However, OP and NP were found in only two vegetable samples and one filling liquid, but neither was detected in any package. The proposed method provided recoveries of 83-118%. Copyright © 2012 Elsevier B.V. All rights reserved.

Preparation of stir cake sorptive extraction based on polymeric ionic liquid for the enrichment of benzimidazole anthelmintics in water, honey and milk samples.

PubMed

Wang, Yulei; Zhang, Jie; Huang, Xiaojia; Yuan, Dongxing

2014-08-20

In this work, a new stir cake sorptive extraction (SCSE) using polymeric ionic liquid monolith as sorbent was prepared. The sorbent was obtained by in situ copolymerization of an ionic liquid, 1-allyl-3-methylimidazolium bis[(trifluoro methyl)sulfonyl]imide (AMII) and divinylbenzene (DB) in the presence of N,N-dimethylformamide. The influence of the content of ionic liquid and the porogen in the polymerization mixture on extraction performance was studied thoroughly. The physicochemical properties of the polymeric ionic liquid were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The usefulness of SCSE-AMIIDB was demonstrated by the enrichment of trace benzimidazole anthelmintics. Several parameters affecting the extraction efficiency were investigated, and under the optimized conditions, a simple and effective method for the determination of trace benzimidazoles residues in water, milk and honey samples was established by coupling SCSE-AMIIDB with high performance liquid chromatography/diode array detection (SCSE-AMIIDB-HPLC/DAD). Results indicated that the limits of detection (S/N=3) for target compounds were 0.020-0.072 μg L(-1), 0.035-0.10 μg L(-1) and 0.026-0.076 μg L(-1) in water, milk and honey samples, respectively. In addition, an acceptable reproducibility was achieved by evaluating the repeatability and intermediate precision with relative standard deviations (RSD) of less than 9% and 11%, respectively. Finally, the established AMII-SCSE-HPLC/DAD method was successfully applied for the determination of benzimidazoles residues in milk, honey and environmental water samples. Recoveries obtained for the determination of benzimidazole anthelmintics in spiking samples ranged from 70.2% to 117.6%, with RSD below 12% in all cases. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of Summon Preferred Food Source on feeding, tunneling, and bait station discovery by the formosan subterranean termite (Isoptera: Rhinotermitidae).

PubMed

Cornelius, Mary L; Lax, Alan R

2005-04-01

This study evaluated the effect of Summon Preferred Food Source on feeding, tunneling, and bait station discovery by the Formosan subterranean termite, Coptotermes formosanus Shiraki. Bioassays were conducted to determine whether Summon disks affected the aggregation and feeding behavior of termites and to determine whether the presence of Summon disks caused increased recruitment of termites to wood blocks. When termites encountered the disk, they immediately clustered on top of the disk. Termites were observed aggregating on top of the disk throughout the experiment. Consumption of Summon disks was significantly greater than consumption of cardboard disks in paired choice tests. The presence of a Summon disk on top of a wood block caused a significant increase in consumption of the wood block. Bioassays also were conducted to determine whether water extracts of Summon disks affected termite behavior. Consumption of filter paper disks treated with a water extract of Summon disks was significantly greater than consumption of control filter paper disks. Termites tunneled through sand treated with a water extract of Summon disks faster than they tunneled through untreated sand. In a field test, the rate of infestation of monitoring stations with a Summon disk was 3 times greater than the rate of infestations of stations without a disk.

Characterisation of dissolved organic compounds in hydrothermal fluids by stir bar sorptive extraction - gas chomatography - mass spectrometry. Case study: the Rainbow field (36°N, Mid-Atlantic Ridge)

PubMed Central

2012-01-01

The analysis of the dissolved organic fraction of hydrothermal fluids has been considered a real challenge due to sampling difficulties, complexity of the matrix, numerous interferences and the assumed ppb concentration levels. The present study shows, in a qualitative approach, that Stir Bar Sorptive Extraction (SBSE) followed by Thermal Desorption – Gas Chromatography – Mass Spectrometry (TD-GC-MS) is suitable for extraction of small sample volumes and detection of a wide range of volatile and semivolatile organic compounds dissolved in hydrothermal fluids. In a case study, the technique was successfully applied to fluids from the Rainbow ultramafic-hosted hydrothermal field located at 36°14’N on the Mid-Atlantic Ridge (MAR). We show that n-alkanes, mono- and poly- aromatic hydrocarbons as well as fatty acids can be easily identified and their retention times determined. Our results demonstrate the excellent repeatability of the method as well as the possibility of storing stir bars for at least three years without significant changes in the composition of the recovered organic matter. A preliminary comparative investigation of the organic composition of the Rainbow fluids showed the great potential of the method to be used for assessing intrafield variations and carrying out time series studies. All together our results demonstrate that SBSE-TD-GC-MS analyses of hydrothermal fluids will make important contributions to the understanding of geochemical processes, geomicrobiological interactions and formation of mineral deposits. PMID:23134621

Determination of glyoxal and methylglyoxal in environmental and biological matrices by stir bar sorptive extraction with in-situ derivatization.

PubMed

Neng, N R; Cordeiro, C A A; Freire, A P; Nogueira, J M F

2007-10-26

Stir bar sorptive extraction with in-situ derivatization using 2,3-diaminonaphthalene (DAN) followed by liquid desorption and high performance liquid chromatography with diode array detection (SBSE(DAN)in-situ-LD-HPLC-DAD) was developed for the determination of glyoxal (Gly) and methylglyoxal (MGly) in environmental and biological matrices. DAN proved very good specificity as in-situ derivatising agent for Gly and MGly in aqueous media, allowing the formation of adducts with remarkable sensitivity, selectivity and the absence of photodegradation. Assays performed on spiked (1.0 microg L(-1)) water samples, under convenient experimental conditions, yielded recoveries of 96.2+/-7.9% for Gly and 96.1+/-6.4% for MGly. The analytical performance showed good accuracy, suitable precision (<12.0%), low detection limits (15 ng L(-1) for Gly and 25 ng L(-1) for MGly adducts) and excellent linear dynamic ranges (r2>0.99) from 0.1 to 120.0 microg L(-1). By using the standard addition method, the application of the present method to tap and swimming-pool water, beer, yeast cells suspension and urine samples allowed very good performance at the trace level. The proposed methodology proved to be a feasible alternative for routine quality control analysis, showing to be easy to implement, reliable, sensitive and with a low sample volume requirement to monitor Gly and MGly in environmental and biological matrices.

Determination of 129I in environmental samples by AMS and NAA using an anion exchange resin disk

NASA Astrophysics Data System (ADS)

Suzuki, Takashi; Banba, Shigeru; Kitamura, Toshikatsu; Kabuto, Shoji; Isogai, Keisuke; Amano, Hikaru

2007-06-01

We have developed a new extraction method for the measurement of 129I by accelerator mass spectrometry (AMS) utilizing an anion exchange resin disk. In comparison to traditional methods such as solvent extraction and ion exchange, this method provides for simple and quick sample handling. This extraction method was tested on soil, seaweed and milk samples, but because of disk clogging, the milk samples and some of the seaweed could not be applied successfully. Using this new extraction method to prepare samples for AMS analysis produced isotope ratios of iodine in good agreement with neutron activation analysis (NAA). The disk extraction method which take half an hour is faster than previous techniques, such as solvent extraction or ion exchange which take a few hours. The combination of the disk method and the AMS measurement is a powerful tool for the determination of 129I. Furthermore, these data will be available for the environmental monitoring before and during the operation of a new nuclear fuel reprocessing plant in Japan.

Ultra-high-performance liquid chromatography-Time-of-flight high resolution mass spectrometry to quantify acidic drugs in wastewater.

PubMed

Becerra-Herrera, Mercedes; Honda, Luis; Richter, Pablo

2015-12-04

A novel analytical approach involving an improved rotating-disk sorptive extraction (RDSE) procedure and ultra-high-performance liquid chromatography (UHPLC) coupled to an ultraspray electrospray ionization source (UESI) and time-of-flight mass spectrometry (TOF/MS), in trap mode, was developed to identify and quantify four non-steroidal anti-inflammatory drugs (NSAIDs) (naproxen, ibuprofen, ketoprofen and diclofenac) and two anti-cholesterol drugs (ACDs) (clofibric acid and gemfibrozil) that are widely used and typically found in water samples. The method reduced the amount of both sample and reagents used and also the time required for the whole analysis, resulting in a reliable and green analytical strategy. The analytical eco-scale was calculated, showing that this methodology is an excellent green analysis, increasing its ecological worth. The detection limits (LOD) and precision (%RSD) were lower than 90ng/L and 10%, respectively. Matrix effects and recoveries were studied using samples from the influent of a wastewater treatment plant (WWTP). All the compounds exhibited suppression of their signals due to matrix effects, and the recoveries were approximately 100%. The applicability and reliability of this methodology were confirmed through the analysis of influent and effluent samples from a WWTP in Santiago, Chile, obtaining concentrations ranging from 1.1 to 20.5μg/L and from 0.5 to 8.6μg/L, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Novel strategies for sample preparation in forensic toxicology.

PubMed

Samanidou, Victoria; Kovatsi, Leda; Fragou, Domniki; Rentifis, Konstantinos

2011-09-01

This paper provides a review of novel strategies for sample preparation in forensic toxicology. The review initially outlines the principle of each technique, followed by sections addressing each class of abused drugs separately. The novel strategies currently reviewed focus on the preparation of various biological samples for the subsequent determination of opiates, benzodiazepines, amphetamines, cocaine, hallucinogens, tricyclic antidepressants, antipsychotics and cannabinoids. According to our experience, these analytes are the most frequently responsible for intoxications in Greece. The applications of techniques such as disposable pipette extraction, microextraction by packed sorbent, matrix solid-phase dispersion, solid-phase microextraction, polymer monolith microextraction, stir bar sorptive extraction and others, which are rapidly gaining acceptance in the field of toxicology, are currently reviewed.

Method and apparatus for optimized sampling of volatilizable target substances

DOEpatents

Lindgren, Eric R.; Phelan, James M.

2004-10-12

An apparatus for capturing, from gases such as soil gas, target analytes. Target analytes may include emanations from explosive materials or from residues of explosive materials. The apparatus employs principles of sorption common to solid phase microextraction, and is best used in conjunction with analysis means such as a gas chromatograph. To sorb target analytes, the apparatus functions using various sorptive structures to capture target analyte. Depending upon the embodiment, those structures may include a capillary tube including an interior surface on which sorptive material (similar to that on the surface of a SPME fiber) is supported (along with means for moving gases through the capillary tube so that the gases come into close proximity to the sorptive material). In one disclosed embodiment, at least one such sorptive structure is associated with an enclosure including an opening in communication with the surface of a soil region potentially contaminated with buried explosive material such as unexploded ordnance. Emanations from explosive materials can pass into and accumulate in the enclosure where they are sorbed by the sorptive structures. Also disclosed is the use of heating means such as microwave horns to drive target analytes into the soil gas from solid and liquid phase components of the soil.

Membrane protected C18 coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detection for the determination of non-steroidal anti-inflammatory drugs in water samples.

PubMed

Mao, Xiangju; He, Man; Chen, Beibei; Hu, Bin

2016-11-11

By wrapping a porous membrane around the coated stir bar, a novel membrane protected stir bar sorptive extraction (MPSBSE) was proposed to filter out the high molecular weight interferences (such as humic acid), resulting in the analysis of real environmental water samples without filtration or centrifugation. Hydrophilic and hydrophobic membranes were compared and hydrophobic polytetrafluoroethylene (PTFE) membrane impregnated with methanol was employed to protect the C 18 coated stir bar. The impregnated methanol improves the transfer of target analytes from sample solution to the pores and lumen of the membrane, and then to the coated stir bar inside. By combining C 18 -MPSBSE with HPLC-UV, a method was proposed for the direct determination of two common non-steroidal anti-inflammatory drugs, Ketoprofen (KEP) and Naproxen (NAP) in complex water samples. Under the optimized conditions, the limit of detections of KEP and NAP are 7.89, 9.52μgL -1 in the waste water and 7.69, 6.90μgL -1 in the pure water, respectively, with the enrichment factors of 32.0-49.1-fold. Besides, the lifetime of the prepared C 18 stir bar protected by PTFE membrane (50 times) is longer than that of C 18 stir bar without membrane protection (20 times), indicating that the friction damage of SBSE coating during extraction was effectively avoided. The developed method was successfully applied to the analysis of KEP and NAP in domestic sewage and campus lake water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Atmospheric pressure gas chromatography-time-of-flight-mass spectrometry (APGC-ToF-MS) for the determination of regulated and emerging contaminants in aqueous samples after stir bar sorptive extraction (SBSE).

PubMed

Pintado-Herrera, Marina G; González-Mazo, Eduardo; Lara-Martín, Pablo A

2014-12-03

This work presents the development, optimization and validation of a multi-residue method for the simultaneous determination of 102 contaminants, including fragrances, UV filters, repellents, endocrine disruptors, biocides, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and several types of pesticides in aqueous matrices. Water samples were processed using stir bar sorptive extraction (SBSE) after the optimization of several parameters: agitation time, ionic strength, presence of organic modifiers, pH, and volume of the derivatizing agent. Target compounds were extracted from the bars by liquid desorption (LD). Separation, identification and quantification of analytes were carried out by gas chromatography (GC) coupled to time-of-flight (ToF-MS) mass spectrometry. A new ionization source, atmospheric pressure gas chromatography (APGC), was tested. The optimized protocol showed acceptable recovery percentages (50-100%) and limits of detection below 1ngL(-1) for most of the compounds. Occurrence of 21 out of 102 analytes was confirmed in several environmental aquatic matrices, including seawater, sewage effluent, river water and groundwater. Non-target compounds such as organophosphorus flame retardants were also identified in real samples by accurate mass measurement of their molecular ions using GC-APGC-ToF-MS. To the best of our knowledge, this is the first time that this technique has been applied for the analysis of contaminants in aquatic systems. By employing lower energy than the more widely used electron impact ionization (EI), AGPC provides significant advantages over EI for those substances very susceptible to high fragmentation (e.g., fragrances, pyrethroids). Copyright © 2014 Elsevier B.V. All rights reserved.

Stir bar sorptive extraction and high performance liquid chromatographic determination of carvedilol in human serum using two different polymeric phases and an ionic liquid as desorption solvent.

PubMed

Talebpour, Zahra; Taraji, Maryam; Adib, Nuoshin

2012-05-04

This article presents a method employing stir bar coated with a film of poly (methyl methacrylate/ethyleneglycol dimethacrylate) (PA-EG) and polydimethylsiloxane (PDMS) in combination with liquid desorption (LD) using ionic liquid, followed by high performance liquid chromatography (HPLC) equipped with ultraviolet (UV) detection for the determination of carvedilol in human serum samples. Stir bar sorptive extraction (SBSE) variables, such as desorption and extraction time and temperature, desorption solvent and pH of the matrix were optimized, in order to achieve suitable analytical sensitivity in a short period of time. Also, the concentration effect of 1-methyl-3-octylimidazolium tetrafluoroborate [Omim][BF4] ionic liquid on the efficiency of LD was investigated. A comparison between PA-EG/SBSE and PDMS/SBSE was made by calculating the experimental recovery and partition coefficient (K), where PA-EG phase demonstrated to be an excellent alternative for the enrichment of the carvedilol from serum samples. The effect of [Omim][BF4] on carryover was studied and no carryover was observed. Under optimized experimental conditions, the analytical performance showed excellent linear dynamic range, with correlation coefficients higher than 0.999 and limits of detection and quantification of 0.3 and 1.0 ng mL(-1), respectively. Intra- and inter-day recovery ranged from 94 to 103% and the coefficients of variations were less than 3.2%. The proposed method was shown to be simple, highly sensitive and suitable for the measurement of trace concentration levels of carvedilol in biological fluid media. Copyright © 2012 Elsevier B.V. All rights reserved.

Advances in stir bar sorptive extraction for the determination of acidic pharmaceuticals in environmental water matrices Comparison between polyurethane and polydimethylsiloxane polymeric phases.

PubMed

Silva, Ana Rita M; Portugal, Fátima C M; Nogueira, J M F

2008-10-31

Stir bar sorptive extraction with polyurethane (PU) and polydimethylsiloxane (PDMS) polymeric phases followed by high-performance liquid chromatography with diode array detection [SBSE(PU or PDMS)/HPLC-DAD] was studied for the determination of six acidic pharmaceuticals [o-acetylsalicylic acid (ACA), ibuprofen (IBU), diclofenac sodium (DIC), naproxen (NAP), mefenamic acid (MEF) and gemfibrozil (GEM)], selected as non-steroidal acidic anti-inflammatory drugs and lipid regulators model compounds in environmental water matrices. The main parameters affecting the efficiency of the proposed methodology are fully discussed. Assays performed on 25 mL of water samples spiked at the 10 microg L(-1) level under optimized experimental conditions, yielded recoveries ranging from 45.3+/-9.0% (ACA) to 90.6+/-7.2% (IBU) by SBSE(PU) and 9.8+/-1.6% (NAP) to 73.4+/-5.0% (GEM) by SBSE(PDMS), where the former polymeric phase presented a better affinity to extract these target analytes from water matrices at the trace level. The methodology showed also excellent linear dynamic ranges for the six acidic pharmaceuticals studied, with correlation coefficients higher than 0.9976, limits of detection and quantification between 0.40-1.7 microg L(-1) and 1.5-5.8 microg L(-1), respectively, and suitable precision (RSD <15%). Moreover, the developed methodology was applied for the determination of these target analytes in several environmental matrices, including river, sea and wastewater samples, having achieved good performance and moderate matrix effects. In short, the PU foams demonstrated to be an excellent alternative for the enrichment of the more polar metabolites from water matrices by SBSE, overcoming the limitations of the conventional PDMS phase.

Jacket-free stir bar sorptive extraction with bio-inspired polydopamine-functionalized immobilization of cross-linked polymer on stainless steel wire.

PubMed

Zhang, Zixin; Zhang, Wenpeng; Bao, Tao; Chen, Zilin

2015-08-14

Stainless steel wire (SSW) is a good substrate for stir bar sorptive extraction (SBSE). However, it is still a challenge to immobilize commonly used cross-linked polymers onto SSW. In this work, we present a new approach for immobilization of the cross-linked organic polymer onto SSW for jacket-free SBSE. A dopamine derivative was firstly synthesized; by introducing a mussel-inspired polydopamine process, a stable coating layer was finally generated on the surface of SSW. Secondly, the cross-linked polymer was synthesized on the polydopamine-modified SSW by using acetonitrile as the porogen, acrylamide (AA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker and 2,2'-azobis (2-methylpropionitrile) as the initiator. A diluted pre-polymerization solution was carefully prepared to generate a thin layer of the polymer. The prepared poly(EGDMA-AA)-modified stir bar showed high stability and good tolerance toward stirring, ultrasonication, organic solvents, and strong acidic and basic conditions. Morphology and structure characterization of coatings were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The prepared poly(EGDMA-AA)-modified stir bar showed great extraction efficiency toward protoberberines, with enrichment factors of 19-42. An SBSE-HPLC method was also developed for quantitative analysis of protoberberines. The method showed low limits of detection (0.06-0.15 ng mL(-1)), wide linear range (0.5-400 ng mL(-1)), good linearity (R≥0.9980) and good reproducibility (RSD≤3.60% for intra-day, RSD≤4.73% for inter-day). The developed method has been successfully applied to determine protoberberines in herb and rat plasma samples, with recoveries of 88.53-114.61%. Copyright © 2015 Elsevier B.V. All rights reserved.

Non-planar chemical preconcentrator

DOEpatents

Manginell, Ronald P [Albuquerque, NM; Adkins, Douglas R [Albuquerque, NM; Sokolowski, Sara S [Albuquerque, NM; Lewis, Patrick R [Albuquerque, NM

2006-10-10

A non-planar chemical preconcentrator comprises a high-surface area, low mass, three-dimensional, flow-through sorption support structure that can be coated or packed with a sorptive material. The sorptive material can collect and concentrate a chemical analyte from a fluid stream and rapidly release it as a very narrow temporal plug for improved separations in a microanalytical system. The non-planar chemical preconcentrator retains most of the thermal and fabrication benefits of a planar preconcentrator, but has improved ruggedness and uptake, while reducing sorptive coating concerns and extending the range of collectible analytes.

A sublimate sorbent for stir-bar sorptive extraction of aqueous endocrine disruptor pesticides for gas chromatography-electron capture detection.

PubMed

Huang, Yu-Wen; Lee, Hua Kwang; Shih, Hou-Kuang; Jen, Jen-Fon

2018-06-06

A dumbbell-shaped magnetic stir-bar with sublimate sorbent was prepared for the stir bar sorptive extraction (SBSE) of pesticides in an aqueous sample prior to gas chromatography-micro-electron capture detection (GC-μECD). Cyclododecane (CDD) was coated onto a magnetic stir-bar surface as a sublimate sorbent, and steel balls were placed on both ends to form a dumbbell-shaped magnetic stir-bar for SBSE. Four EDC pesticides including chlorpyrifos, ethion, bromopropylate, and λ-cyhalothrin in aqueous samples were selected as model species to examine the proposed SBSE and the following desorption. The parameters studied were those affecting the extraction efficiencies including the coating (solvent for CDD and thickness), extraction (sample pH, stirring rate, time, and salting out effect), dissolution solvent volume, and the loss of CDD sublimated in air. The maximum extraction efficiency was obtained under the following conditions. The stir bar (with CDD thickness of 5.2 μm) was added into a 10 mL sample solution (at pH 7) for a 20-min extraction at 600 rpm. Then, the stir bar was gently removed from the sample solution, disassembled, and immersed into a 0.2 mL insert tube consisting of 3 μL hexane to dissolve; 1 μL was used for GC-ECD analysis. The linear ranges were 0.005-5 μg L -1 with coefficients of determination ranging from 0.9950 - 0.9994. Detection limits (based on S/N = 3) of the four EDCs were 0.4-4.5 ngL -1 with a relative standard deviation (RSD) of 2.4-6.3%, and quantitation limits (based on S/N = 5) were 1-15 ngL -1 . The relative recoveries of the spiked samples were in the range of 83.2-98.7% with RSDs of 2.1-8.4% in farm field waters. The proposed sublimation sorbent obtained excellent enrichment factors (101-834) and provided a simple, rapid, sensitive, and eco-friendly sample preparation method. Copyright © 2018 Elsevier B.V. All rights reserved.

A new strategy for accelerated extraction of target compounds using molecularly imprinted polymer particles embedded in a paper-based disk.

PubMed

Zarejousheghani, Mashaalah; Schrader, Steffi; Möder, Monika; Schmidt, Matthias; Borsdorf, Helko

2018-03-01

In this study, a general simple and inexpensive method is introduced for the preparation of a paper-based selective disk-type solid phase extraction (SPE) technique, appropriate for fast and high throughput monitoring of target compounds. An ion exchange molecularly imprinted polymer (MIP) was synthesized for the extraction and analysis of acesulfame, an anthropogenic water quality marker. Acesulfame imprinting was used as an example for demonstrating the benefits of a nanosized, swellable MIP extraction sorbents integrated in an on-site compatible concept for water quality monitoring. Compared with an 8 mL standard SPE cartridge, the paper-based MIP disk (47 mm ø) format allowed (1) high sample flow rates up to 30 mL•min -1 without losing extraction efficiency (2) extracting sample volumes up to 500 mL in much shorter times than with standard SPE, (3) the reuse of the disks (up to 3 times more than SPE cartridge) due to high robustness and an efficient post-cleaning, and (4) reducing the sampling time from 100 minutes (using the standard SPE format) to about 2 minutes with the MIP paper disk for 50 mL water sample. Different parameters like cellulose fiber/polymer ratios, sample volume, sample flow-rate, washing, and elution conditions were evaluated and optimized. Using developed extraction technique with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) analysis, a new protocol was established that provides detection and quantification limits of 0.015 μg•L -1 and 0.05 μg•L -1 , respectively. The developed paper disks were used in-field for the selective extraction of target compounds and transferred to the laboratory for further analysis. Copyright © 2017 John Wiley & Sons, Ltd.

HEURISTIC OPTIMIZATION AND ALGORITHM TUNING APPLIED TO SORPTIVE BARRIER DESIGN

EPA Science Inventory

While heuristic optimization is applied in environmental applications, ad-hoc algorithm configuration is typical. We use a multi-layer sorptive barrier design problem as a benchmark for an algorithm-tuning procedure, as applied to three heuristics (genetic algorithms, simulated ...

LAUNCHING AND QUENCHING OF BLACK HOLE RELATIVISTIC JETS AT LOW ACCRETION RATE

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

Pu, Hung-Yi; Chang, Hsiang-Kuang; Hirotani, Kouichi

2012-10-20

Relativistic jets are launched from black hole (BH) X-ray binaries and active galactic nuclei when the disk accretion rate is below a certain limit (i.e., when the ratio of the accretion rate to the Eddingtion accretion rate, m-dot , is below about 0.01) but quenched when above. We propose a new paradigm to explain this observed coupling between the jet and the accretion disk by investigating the extraction of the rotational energy of a BH when it is surrounded by different types of accretion disk. At low accretion rates (e.g., when m-dot {approx}<0.1), the accretion near the event horizon ismore » quasi-spherical. The accreting plasmas fall onto the event horizon in a wide range of latitudes, breaking down the force-free approximation near the horizon. To incorporate the plasma inertia effect, we consider the magnetohydrodynamical (MHD) extraction of the rotational energy from BHs by the accreting MHD fluid, as described by the MHD Penrose process. It is found that the energy extraction operates, and hence a relativistic jet is launched, preferentially when the accretion disk consists of an outer Shakura-Sunyaev disk (SSD) and an inner advection-dominated accretion flow. When the entire accretion disk type changes into an SSD, the jet is quenched because the plasmas bring more rest-mass energy than what is extracted from the hole electromagnetically to stop the extraction. Several other issues related to observed BH disk-jet couplings, such as why the radio luminosity increases with increasing X-ray luminosity until the radio emission drops, are also explained.« less

Tunable Polarity Carbon Fibers, a Holistic Approach to Environmental Protection.

PubMed

García-Valverde, M Teresa; Ledesma-Escobar, Carlos A; Lucena, Rafael; Cárdenas, Soledad

2018-04-27

The pollution of environmental resources is an issue of social concern worldwide. Chemistry is essential for the design of decontamination strategies and analytical approaches to detect and monitor the contamination. Sorptive materials are usually required in both approaches and green synthesis should be used to minimize their own environmental impact. Carbon fibers (CFs) obtained by the pyrolysis of natural cellulose-rich materials fulfill these requirements. In this article, thirty CFs obtained under different conditions are chemically characterized and their sorption ability towards selected pollutants, covering a wide range of polarity, is evaluated. This study provides more profound knowledge related to the polarity of these materials, their interactions with chemical substances and allows the prediction of more appropriate materials (pyrolysis temperature and time) in order to remove the given pollutant. Furthermore, the use of CFs as sorptive materials for the extraction of contaminants from water samples to assist with their instrumental detection is outlined. In this sense, the use of CFs and gas chromatography with mass spectrometric detection allows the detection of selected pollutants in the low ng/mL range. Thus, this article provides an integrated approach to the potential of CFs for environmental protection.

Chemical preconcentrator

DOEpatents

Manginell, Ronald P.; Frye-Mason, Gregory C.

2001-01-01

A chemical preconcentrator is disclosed with applications to chemical sensing and analysis. The preconcentrator can be formed by depositing a resistive heating element (e.g. platinum) over a membrane (e.g. silicon nitride) suspended above a substrate. A coating of a sorptive material (e.g. a microporous hydrophobic sol-gel coating or a polymer coating) is formed on the suspended membrane proximate to the heating element to selective sorb one or more chemical species of interest over a time period, thereby concentrating the chemical species in the sorptive material. Upon heating the sorptive material with the resistive heating element, the sorbed chemical species are released for detection and analysis in a relatively high concentration and over a relatively short time period. The sorptive material can be made to selectively sorb particular chemical species of interest while not substantially sorbing other chemical species not of interest. The present invention has applications for use in forming high-sensitivity, rapid-response miniaturized chemical analysis systems (e.g. a "chem lab on a chip").

Released fraction of polychlorinated biphenyls from soil-biosolid system using a leaching procedure and its comparison with bioavailable fraction determined by wheat plant uptake.

PubMed

Jachero, Lourdes; Leiva, Claudio; Ahumada, Inés; Richter, Pablo

2017-11-01

The bioavailability of polychlorinated biphenyls (PCBs) in soils amended with biosolids was estimated using an aqueous leaching process of the compounds combined with rotating disk sorptive extraction (RDSE), and compared with bioavailability determined through of PCB absorption in wheat plants growing in the same soil-biosolid matrix. The matrices consisted of soil amended with biosolids at doses of 30, 90, and 200 Mg/ha, which increase concomitantly the organic matter content of the matrix. Considering that PCBs were natively absent in both the biosolids and soil used, the compounds were spiked in the biosolids and aged for 10 days. For each biosolid dose, the aqueous leaching profile was studied and equilibrium time was calculated to be 33 h. The leaching fractions determined by RDSE, considering total PCBs studied, were 12, 7, and 6% and the bioavailable fractions absorbed by the wheat root were found to be 0.5, 0.3, and 0.2% for 30, 90, and 200 Mg/ha doses, respectively. Both fractions leachable and bioavailable decrease with both increasing hydrophobicity of the compound (Kow) and increasing in the biosolid dose. It was found that both fractions (leaching and bioavailable) correlated according to the bivariate least squares regression, represented by a coefficient of correlation of 0.86. Therefore, the application of the chemical method involving a leaching procedure is an alternative to estimate the bioavailable fraction of PCBs in wheat plants in a simpler and in a shorter time.

Characterization of volatiles and identification of odor-active compounds of rocket leaves.

PubMed

Raffo, Antonio; Masci, Maurizio; Moneta, Elisabetta; Nicoli, Stefano; Sánchez Del Pulgar, José; Paoletti, Flavio

2018-02-01

The volatile profile of crushed rocket leaves (Eruca sativa and Diplotaxis tenuifolia) was investigated by applying Headspace Solid-Phase MicroExtraction (HS-SPME), combined with GC-MS, to an aqueous extract obtained by homogenization of rocket leaves, and stabilized by addition of CaCl 2 . A detailed picture of volatile products of the lipoxygenase pathway (mainly C6-aldehydes) and of glucosinolate hydrolysis (mainly isothiocyanates), and their dynamics of formation after tissue disruption was given. Odor-active compounds of leaves were characterized by GC-Olfactometry (GC-O) and Aroma Extract Dilution Analysis (AEDA): volatile isolates obtained by HS-SPME from an aqueous extract and by Stir-Bar Sorptive Extraction (SBSE) from an ethanolic extract were analyzed. The most potent odor-active compounds fully or tentatively identified were (Z)- and (E)-3-hexenal, (Z)-1,5-octadien-3-one, responsible for green olfactory notes, along with 4-mercaptobutyl and 4-(methylthio)butyl isothiocyanate, associated with typical rocket and radish aroma. Relatively high odor potency was observed for 1-octen-3-one, (E)-2-octenal and 1-penten-3-one. Copyright © 2017 Elsevier Ltd. All rights reserved.

A High Throughput Method for Measuring Polycyclic Aromatic Hydrocarbons in Seafood Using QuEChERS Extraction and SBSE.

PubMed

Pfannkoch, Edward A; Stuff, John R; Whitecavage, Jacqueline A; Blevins, John M; Seely, Kathryn A; Moran, Jeffery H

2015-01-01

National Oceanic and Atmospheric Administration (NOAA) Method NMFS-NWFSC-59 2004 is currently used to quantitatively analyze seafood for polycyclic aromatic hydrocarbon (PAH) contamination, especially following events such as the Deepwater Horizon oil rig explosion that released millions of barrels of crude oil into the Gulf of Mexico. This method has limited throughput capacity; hence, alternative methods are necessary to meet analytical demands after such events. Stir bar sorptive extraction (SBSE) is an effective technique to extract trace PAHs in water and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction strategy effectively extracts PAHs from complex food matrices. This study uses SBSE to concentrate PAHs and eliminate matrix interference from QuEChERS extracts of seafood, specifically oysters, fish, and shrimp. This method provides acceptable recovery (65-138%) linear calibrations and is sensitive (LOD = 0.02 ppb, LOQ = 0.06 ppb) while providing higher throughput and maintaining equivalency between NOAA 2004 as determined by analysis of NIST SRM 1974b mussel tissue.

Gas chromatography and ultra high performance liquid chromatography tandem mass spectrometry methods for the determination of selected endocrine disrupting chemicals in human breast milk after stir-bar sorptive extraction.

PubMed

Rodríguez-Gómez, R; Zafra-Gómez, A; Camino-Sánchez, F J; Ballesteros, O; Navalón, A

2014-07-04

In the present work, two specific, accurate and sensitive methods for the determination of endocrine disrupting chemicals (EDCs) in human breast milk are developed and validated. Bisphenol A and its main chlorinated derivatives, five benzophenone-UV filters and four parabens were selected as target analytes. The method involves a stir-bar sorptive extraction (SBSE) procedure followed by a solvent desorption prior to GC-MS/MS or UHPLC-MS/MS analysis. A derivatization step is also necessary when GC analysis is performed. The GC column used was a capillary HP-5MS with a run time of 26min. For UHPLC analysis, the stationary phase was a non-polar Acquity UPLC(®) BEH C18 column and the run time was 10min. In both cases, the analytes were detected and quantified using a triple quadrupole mass spectrometer (QqQ). Quality parameters such as linearity, accuracy (trueness and precision), sensitivity and selectivity were examined and yielded good results. The limits of quantification (LOQs) ranged from 0.3 to 5.0ngmL(-1) for GC and from 0.2 to 1.0ngmL(-1) for LC. The relative standard deviation (RSD) was lower than 15% and the recoveries ranged from 92 to 114% in all cases, being slightly unfavorable the results obtained with LC. The methods were satisfactorily applied for the determination of target compounds in human milk samples from 10 randomly selected women. Copyright © 2014 Elsevier B.V. All rights reserved.

Impact of phase ratio, polydimethylsiloxane volume and size, and sampling temperature and time on headspace sorptive extraction recovery of some volatile compounds in the essential oil field.

PubMed

Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara; Sandra, Pat

2005-04-15

This study evaluates concentration capability of headspace sorptive extraction (HSSE) and the influence of sampling conditions on HSSE recovery of an analyte. A standard mixture in water of six high-to-medium volatility analytes (isobutyl methyl ketone, 3-hexanol, isoamyl acetate, 1,8-cineole, linalool and carvone) was used to sample the headspace by HSSE with stir bars coated with different polydimethylsiloxane (PDMS) volumes (20, 40, 55 and 110 microL, respectively), headspace vial volumes (8, 21.2, 40, 250 and 1000 mL), sampling temperatures (25, 50 and 75 degrees C) and sampling times (30, 60 and 120 min, and 4, 8 and 16 h). The concentration factors (CFs) of HSSE versus static headspace (S-HS) were also determined. Analytes sampled by the PDMS stir bars were recovered by thermal desorption (TDS) and analysed by capillary GC-MS. This study demonstrates how analyte recovery depends on its physico-chemical characteristics and affinity for PDMS (octanol-water partition coefficients), sampling temperatures (50 degrees C) and times (60 min), the volumes of headspace (40 mL) and of PDMS (in particular, for high volatility analytes). HSSE is also shown to be very effective for trace analysis. The HSSE CFs calculated versus S-HS with a 1000 mL headspace volumes at 25 degrees C during 4 h sampling ranged between 10(3) and 10(4) times for all analytes investigated while the limits of quantitation determined under the same conditions were in the nmol/L range.

Development, optimisation and application of polyurethane foams as new polymeric phases for stir bar sorptive extraction.

PubMed

Neng, N R; Pinto, M L; Pires, J; Marcos, P M; Nogueira, J M F

2007-11-09

In this contribution, polyurethane foams are proposed as new polymeric phases for stir bar sorptive extraction (SBSE). Assays performed for polyurethane synthesis demonstrated that four series of formulations (P(1), P(2), P(3) and P(4)) present remarkable stability and excellent mechanical resistance to organic solvents. For polymer clean-up treatment, acetonitrile proved to be the best solvent under sonification, ensuring the reduction of the contamination and interferences. SBSE assays performed on these polyurethane polymers followed by liquid desorption and high-performance liquid chromatography-diode array detection (LD-HPLC-DAD) or large volume injection-capillary gas chromatography-mass spectrometry (LD-LVI-GC-MS), showed that P(2) presents the best recovery yields for atrazine, 2,3,4,5-tetrachlorophenol and fluorene, used as model compounds in water samples at a trace level. SBSE(P(2)) assays performed on this polymer mixed up with several adsorbent materials, i.e. activated carbon, a mesoporous material and a calixarene, did not bring any advantages in relation with the polymeric matrix alone. The comparison between assays performed by SBSE(P(2)) and by the conventional SBSE(PDMS) showed much better performance for the former phase on aqueous samples spiked with atrazine, 2,3,4,5-tetrachlorophenol and fluorene, in which the foremost two analytes present recovery values 3- and 10-fold higher, respectively. The polyurethanes proposed as new polymeric phases for SBSE provided powerful capabilities for the enrichment of organic compounds from aqueous matrices, showing to be indicated mainly in the case of the more polar analytes.

Enantioselective extraction of (+)-(S)-citalopram and its main metabolites using a tailor-made stir bar chiral imprinted polymer for their LC-ESI-MS/MS quantitation in urine samples.

PubMed

Unceta, Nora; Gómez-Caballero, Alberto; García, Deiene; Díaz, Goretti; Guerreiro, Antonio; Piletsky, Sergey; Goicolea, M Aránzazu; Barrio, Ramón J

2013-11-15

This paper reports the application of a chiral imprinted polymer (CIP)-coated stir bar for the selective extraction of (+)-(S)-citalopram (SCIT) and its main metabolites, (+)-(S)-desmethylcitalopram (SDCIT) and (+)-(S)-didesmethylcitalopram (SDDCIT), from urine samples. The developed device has been demonstrated to be capable of selectively extracting the three target analytes from urine samples without saturating the imprinted sites. A CIP-coated stir bar sorptive extraction procedure (CIP-SBSE) is proposed for the isolation of SCIT, SDCIT and SDDCIT followed by their subsequent analysis using liquid chromatography ion trap mass spectrometry (LC-ITMS). Deuterated SCIT-d6 was used as an internal standard. The method was validated using a standard procedure, which revealed that a quantification of 5 ng mL(-1) was obtained in urine samples and that the accuracy and precision were within the established values while no matrix effect was observed. Copyright © 2013 Elsevier B.V. All rights reserved.

Automated solid-phase extraction of phenolic acids using layered double hydroxide-alumina-polymer disks.

PubMed

Ghani, Milad; Palomino Cabello, Carlos; Saraji, Mohammad; Manuel Estela, Jose; Cerdà, Víctor; Turnes Palomino, Gemma; Maya, Fernando

2018-01-26

The application of layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks for solid-phase extraction is reported for the first time. Al 2 O 3 is embedded in a polymer matrix followed by an in situ metal-exchange process to obtain a layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disk with excellent flow-through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using sequential injection analysis of organic acids (p-hydroxybenzoic acid, 3,4-dihydroxybenzoic acid, gallic acid) following an anion-exchange mechanism. After the solid-phase extraction, phenolic acids were quantified by reversed-phase high-performance liquid chromatography with diode-array detection using a core-shell silica-C18 stationary phase and isocratic elution (acetonitrile/0.5% acetic acid in pure water, 5:95, v/v). High sensitivity and reproducibility were obtained with limits of detection in the range of 0.12-0.25 μg/L (sample volume, 4 mL), and relative standard deviations between 2.9 and 3.4% (10 μg/L, n = 6). Enrichment factors of 34-39 were obtained. Layered double hydroxide-Al 2 O 3 -polymer mixed-matrix disks had an average lifetime of 50 extractions. Analyte recoveries ranged from 93 to 96% for grape juice and nonalcoholic beer samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel method for the rapid and specific extraction of multiple β2 -agonist residues in food by tailor-made Monolith-MIPs extraction disks and detection by gas chromatography with mass spectrometry.

PubMed

Liu, Haibo; Gan, Ning; Chen, Yinji; Ding, Qingqing; Huang, Jie; Lin, Saichai; Cao, Yuting; Li, Tianhua

2016-09-01

A quick and specific pretreatment method based on a series of extraction clean-up disks, consisting of molecularly imprinted polymer monoliths and C18 adsorbent, was developed for the specific enrichment of salbutamol and clenbuterol residues in food. The molecularly imprinted monolithic polymer disk was synthesized using salbutamol as a template through a one-step synthesis process. It can simultaneously and specifically recognize salbutamol and clenbuterol. The monolithic polymer disk and series of C18 disks were assembled with a syringe to form a set of tailor-made devices for the extraction of target molecules. In a single run, salbutamol and clenbuterol can be specifically extracted, cleaned, and eluted by methanol/acetic acid/H2 O. The target molecules, after a silylation derivatization reaction were detected by gas chromatography-mass spectrometry. The parameters including solvent desorption, sample pH, and the cycles of reloading were investigated and discussed. Under the optimized extraction and clean-up conditions, the limits of detection and quantitation were determined as 0.018-0.022 and 0.042-0.049 ng/g for salbutamol and clenbuterol, respectively. The assay described was convenient, rapid, and specific; thereby potentially efficient in the high-throughput analysis of β2 -agonists residues in real food samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Method and apparatus for optimized sampling of volatilizable target substances

DOEpatents

Lindgren, Eric R.; Phelan, James M.

2002-01-01

An apparatus for capturing, from gases such as soil gas, target analytes. Target analytes may include emanations from explosive materials or from residues of explosive materials. The apparatus employs principles of sorption common to solid phase microextraction, and is best used in conjunction with analysis means such as a gas chromatograph. To sorb target analytes, the apparatus functions using various sorptive structures to capture target analyte. Depending upon the embodiment, those structures may include 1) a conventional solid-phase microextraction (SPME) fiber, 2) a SPME fiber suspended in a capillary tube (with means provided for moving gases through the capillary tube so that the gases come into close proximity to the suspended fiber), and 3) a capillary tube including an interior surface on which sorptive material (similar to that on the surface of a SPME fiber) is supported (along with means for moving gases through the capillary tube so that the gases come into close proximity to the sorptive material). In one disclosed embodiment, at least one such sorptive structure is associated with an enclosure including an opening in communication with the surface of a soil region potentially contaminated with buried explosive material such as unexploded ordnance. Emanations from explosive materials can pass into and accumulate in the enclosure where they are sorbed by the sorptive structures. Also disclosed is the use of heating means such as microwave horns to drive target analytes into the soil gas from solid and liquid phase components of the soil.

Quantitative analysis of phosphoric acid esters in aqueous samples by isotope dilution stir-bar sorptive extraction combined with direct analysis in real time (DART)-Orbitrap mass spectrometry.

PubMed

Bridoux, Maxime C; Malandain, Hélène; Leprince, Françoise; Progent, Frédéric; Machuron-Mandard, Xavier

2015-04-15

A novel hyphenated technique, namely the combination of stir bar sorptive extraction (SBSE) with isotope dilution direct analysis in real time (DART) Orbitrap™ mass spectrometry (OT-MS) is presented for the extraction of phosphoric acid alkyl esters (tri- (TnBP), di- (HDBP), and mono-butyl phosphate (H2MBP)) from aqueous samples. First, SBSE of phosphate esters was performed using a Twister™ coated with 24 μL of polydimethylsiloxane (PDMS) as the extracting phase. SBSE was optimized for extraction pH, phase ratio (PDMS volume/aqueous phase volume), stirring speed, extraction time and temperature. Then, coupling of SBSE to DART/Orbitrap-MS was achieved by placing the Twister™ in the middle of an open-ended glass tube between the DART and the Orbitrap™. The DART mass spectrometric response of phosphate esters was probed using commercially available and synthesized alkyl phosphate ester standards. The positive ion full scan spectra of alkyl phosphate triesters (TnBP) was characterized by the product of self-protonation [M+H](+) and, during collision-induced dissociation (CID), the major fragmentation ions corresponded to consecutive loss of alkyl chains. Negative ionization gave abundant [M-H](-) ions for both HDnBP and H2MnBP. Twisters™ coated with PDMS successfully extracted phosphate acid esters (tri-, di- and mono-esters) granted that the analytes are present in the aqueous solution in the neutral form. SBSE/DART/Orbitrap-MS results show a good linearity between the concentrations and relative peak areas for the analytes in the concentration range studied (0.1-750 ng mL(-1)). Reproducibility of this SBSE/DART/Orbitrap-MS method was evaluated in terms of %RSD by extracting a sample of water fortified with the analytes. The %RSDs for TnBP, HDnBP and H2MnBP were 4, 3 and 3% (n=5) using the respective perdeuterated internal standards. Matrix effects were investigated by matrix matched calibration standards using underground water samples (UWS) and river water samples (RWS). Matrix effects were effectively compensated by the addition of the perdeuterated internal standards. The application of this new SBSE/DART/Orbitrap-MS method should be very valuable for on-site sampling/monitoring, limiting the transport of large volumes of water samples from the sampling site to the laboratory. Copyright © 2015 Elsevier B.V. All rights reserved.

Sample preparation techniques for the determination of trace residues and contaminants in foods.

PubMed

Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

2007-06-15

The determination of trace residues and contaminants in complex matrices, such as food, often requires extensive sample extraction and preparation prior to instrumental analysis. Sample preparation is often the bottleneck in analysis and there is a need to minimise the number of steps to reduce both time and sources of error. There is also a move towards more environmentally friendly techniques, which use less solvent and smaller sample sizes. Smaller sample size becomes important when dealing with real life problems, such as consumer complaints and alleged chemical contamination. Optimal sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification, confirmation and quantification. This review considers all aspects of sample preparation, covering general extraction techniques, such as Soxhlet and pressurised liquid extraction, microextraction techniques such as liquid phase microextraction (LPME) and more selective techniques, such as solid phase extraction (SPE), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The applicability of each technique in food analysis, particularly for the determination of trace organic contaminants in foods is discussed.

Determination of steroid sex hormones in water and urine matrices by stir bar sorptive extraction and liquid chromatography with diode array detection.

PubMed

Almeida, C; Nogueira, J M F

2006-06-16

In this study, stir bar sorptive extraction and liquid desorption followed by high performance liquid chromatography with diode array detection (SBSE-LD-HPLC/DAD) were combined for the simultaneous determination of nine steroid sex hormones (estrone, 17alpha-estradiol, 17beta-estradiol, 17alpha-ethynylestradiol, diethylstilbestrol, mestranol, progesterone, 19-norethisterone and norgestrel) in water and urine matrices. During the method development, it has been demonstrated that equilibrium time, ionic strength and back extraction solvents are the most important parameters to control, for determining the nine-hormones in water matrices, in which stir bars coated with 126 microl of polydimethylsiloxane were used. Assays performed on 30 ml water samples spiked at 10 microg/l levels under optimised experimental conditions, yielded recoveries ranging from 11.1+/-4.9% (17beta-estradiol) to 100.2+/-10.4% (mestranol), showed that the methodology is well described by the octanol-water partition coefficients (K(PDMS/W) approximately K(O/W)) for the latter, while pronounced deviations to the theoretical efficiency (K(PDMS/W) not equal K(O/W)) were observed for the remaining hormones. From calibration studies, a good analytical performance for all hormones was attained, including a suitable precision (2.1-17.1%), low limits of detection (0.3-1.0 microg/l) and an excellent linear dynamic range (1.25-50.0 microg/l). Assays on environmental water and urine matrices showed recovery yields in worthy good agreement with the spiking level (10 microg/l), and suitability for profiling low microg/l levels of natural hormones in urine samples taken from pregnant women. The present methodology is easy, reliable and sensitive at the trace level, only requiring a low sample volume, showing to be a good analytical alternative to routine quality control for environmental and biomedical laboratories.

Fabric phase sorptive extraction-high performance liquid chromatography-photo diode array detection method for simultaneous monitoring of three inflammatory bowel disease treatment drugs in whole blood, plasma and urine.

PubMed

Kabir, Abuzar; Furton, Kenneth G; Tinari, Nicola; Grossi, Laurino; Innosa, Denise; Macerola, Daniela; Tartaglia, Angela; Di Donato, Valentina; D'Ovidio, Cristian; Locatelli, Marcello

2018-05-01

This paper reports a novel fabric phase sorptive extraction-high performance liquid chromatography-photodiode array detection (FPSE-HPLC-PDA) method for the simultaneous extraction and analysis of three drug residues (ciprofloxacin, sulfasalazine, and cortisone) in human whole blood, plasma, and urine samples, generally administered in human patients to treat inflammatory bowel disease (IBD). The drugs of interest were well resolved using a Luna C 18 column (250 mm × 4.6 mm; 5 μm particle size) in gradient elution mode within 20 min. The analytical method was optimized and validated in the range 0.05-10 μg/mL for whole blood, 0.25-10 μg/mL for human plasma, and 0.10-10 μg/mL for human urine. Blank human whole blood, plasma, and urine were used as the sample matrix for the method development and validation; while methyl-p-hydroxybenzoate was used as the internal standard (IS). Weighted-matrix matched standard calibration curves showed a good linearity up to a concentration of 10 μg/mL. The intra- and inter-day accuracy values (precision and trueness) were found in the range from -10.9% to 12.3%, and the performances of the validated FPSE-HPLC-PDA were further tested on real IBD patient samples. This is the first FPSE procedure applied simultaneously to whole blood, plasma, and urine samples for the determination of residual IBD drugs, which possess a wide range of polarity (logP values ranging from 2.30 for Ciprofloxacin, to 1.66 for Cortisone, and 2.92 for Sulfasalazine). The new approach exhibits high potential for immediate adoptation as a rapid, robust and green analytical tool for future clinical and pharmaceutical applications. Copyright © 2018 Elsevier B.V. All rights reserved.

Sorptive capacity of membrane lipids, storage lipids, and proteins: a preliminary study of partitioning of organochlorines in lean fish from a PCB-contaminated freshwater lake.

PubMed

Mäenpää, Kimmo; Leppänen, Matti T; Figueiredo, Kaisa; Tigistu-Sahle, Feven; Käkelä, Reijo

2015-01-01

Knowledge on the internal distribution of halogenated organic chemicals (HOCs) would improve our understanding of dose-effect relationships and subsequently improve risk assessment of contaminated sites. Herein, we determine the concentrations of HOCs based on equilibrium partitioning in storage lipids, membrane lipids, and proteins in field-contaminated fish using equilibrium sampling devices. The study shows the importance of protein as a sorptive phase in lean fish. Our results provide a basis for using species-specific equilibrium partitioning coefficients between sorptive tissues and fish internal water as a substitute for K(ow) in, for example, upgrading models that simulate food-chain accumulation of the chemical.

Amino modified multi-walled carbon nanotubes/polydimethylsiloxane coated stir bar sorptive extraction coupled to high performance liquid chromatography-ultraviolet detection for the determination of phenols in environmental samples.

PubMed

Hu, Cong; Chen, Beibei; He, Man; Hu, Bin

2013-07-26

In this work, amino modified multi-walled carbon nanotubes/polydimethylsiloxane (multi-walled carbon nanotubes-4,4'-diaminodiphenylmethane/polydimethylsiloxane, MWCNTs-DDM/PDMS) was synthesized, and utilized as a novel coating for stir bar sorptive extraction (SBSE) of seven phenols (phenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4-dimethylphenol, p-choro-m-cresol and 2,4,6-trichlorphenol) in environmental water and soil samples, followed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The prepared MWCNTs-DDM/PDMS coated stir bar was characterized and good preparation reproducibility was obtained with the relative standard deviations (RSDs) ranging from 4.7% to 11.3% (n=9) in one batch, and from 4.8% to 13.9% (n=8) among different batches. Several parameters affecting the extraction of seven target phenols by MWCNTs-DDM/PDMS-SBSE including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.14μg/L (2-nitrophenol) to 1.76μg/L (phenol) and the limits of quantification (LOQs, S/N=10) were found to be in the range of 0.46μg/L (2-nitrophenol) to 5.8μg/L (phenol). The linear range was 5-1000μg/L for phenol and 4-nitrophenol, 1-1000μg/L for 2-nitrophenol and 2-1000μg/L for other phenols, respectively. The RSDs of the developed method were in the range of 6.2-11.6% (n=8, c=10μg/L) and the enrichment factors were from 6.5 to 62.8-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of phenols in environmental water and soil samples, and good recoveries were obtained for the spiked samples. The proposed method is simple, highly sensitive and suitable for the analysis of trace phenols in environmental samples with complex matrix. Copyright © 2013 Elsevier B.V. All rights reserved.

A fabric phase sorptive extraction-High performance liquid chromatography-Photo diode array detection method for the determination of twelve azole antimicrobial drug residues in human plasma and urine.

PubMed

Locatelli, Marcello; Kabir, Abuzar; Innosa, Denise; Lopatriello, Teresa; Furton, Kenneth G

2017-01-01

This paper reports a novel fabric phase sorptive extraction-high performance liquid chromatography-photodiode array detection (FPSE-HPLC-PDA) method for the simultaneous extraction and analysis of twelve azole antimicrobial drug residues that include ketoconazole, terconazole, voriconazole, bifonazole, clotrimazole, tioconazole, econazole, butoconazole, miconazole, posaconazole, ravuconazole, and itraconazole in human plasma and urine samples. The selected azole antimicrobial drugs were well resolved by using a Luna C 18 column (250mm×4.6mm; 5μm particle size) in gradient elution mode within 36min. The analytical method was calibrated and validated in the range from 0.1 to 8μg/mL for all the drug compounds. Blank human plasma and urine were used as the sample matrix for the analysis; while benzyl-4-hydroxybenzoate was used as the internal standard (IS). The limit of quantification of the FPSE-HPLC-PDA method was found as 0.1μg/mL and the weighted-matrix matched standard calibration curves of the drugs showed a good linearity upto a concentration of 8μg/mL. The parallelism tests were also performed to evaluate whether overrange sample can be analyzed after dilution, without compromising the analytical performances of the validated method. The intra- and inter-day precision (RSD%) values were found ≤13.1% and ≤13.9%, respectively. The intra- and inter-day trueness (bias%) values were found in the range from -12.1% to 10.5%. The performances of the validated FPSE-HPLC-PDA were further tested on real samples collected from healthy volunteers after a single dose administration of itraconazole and miconazole. To the best of our knowledge, this is the first FPSE extraction procedure applied on plasma and urine samples for the simultaneous determination of twelve azole drugs possessing a wide range of logK ow values (extending from 0.4 for fluconazole to 6.70 of butoconazole) and could be adopted as a rapid and robust green analytical tool for clinical and pharmaceutical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Method for analysis of psychopharmaceuticals in real industrial wastewater and groundwater with suspended organic particulate matter using solid phase extraction disks extraction and ultra-high performance liquid chromatography/time-of-flight mass spectrometry.

PubMed

Křesinová, Zdena; Linhartová, Lucie; Petrů, Klára; Krejčová, Lucie; Šrédlová, Kamila; Lhotský, Ondřej; Kameník, Zdeněk; Cajthaml, Tomáš

2016-04-01

A rapid and reliable analytical method was developed for the quantitative determination of psychopharmaceuticals, their precursors and by-products in real contaminated samples from a pharmaceutical company in Olomouc (Czech Republic), based on SPE disk extraction and detection by ultra performance liquid chromatography, combined with time-of-flight mass spectrometry. The target compounds were quantified in the real whole-water samples (water including suspended particles), both in the presence of suspended particulate matter (SPM) and high concentrations of other organic pollutants. A total of nine compounds were analyzed which consisted of three commonly used antidepressants (tricyclic antidepressants and antipsychotics), one antitussive agent and five by-products or precursors. At first, the SPE disk method was developed for the extraction of water samples (dissolved analytes, recovery 84-104%) and pressurised liquid extraction technique was verified for solid matrices (sludge samples, recovery 81-95%). In order to evaluate the SPE disk technique for whole water samples containing SPM, non contaminated groundwater samples were also loaded with different amounts (100 and 300mgL(-1)) of real contaminated sludge originating from the same locality. The recoveries from the whole-water samples obtained by SPE disk method ranged between 67 and 119% after the addition of the most contaminated sludge. The final method was applied to several real groundwater (whole-water) samples from the industrial area and high concentrations (up to 10(3)μgL(-1)) of the target compounds were detected. The results of this study document and indicate the feasibility of the SPE disk method for analysis of groundwater. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantitative analysis of fragrance in selectable one dimensional or two dimensional gas chromatography-mass spectrometry with simultaneous detection of multiple detectors in single injection.

PubMed

Tan, Hui Peng; Wan, Tow Shi; Min, Christina Liew Shu; Osborne, Murray; Ng, Khim Hui

2014-03-14

A selectable one-dimensional ((1)D) or two-dimensional ((2)D) gas chromatography-mass spectrometry (GC-MS) system coupled with flame ionization detector (FID) and olfactory detection port (ODP) was employed in this study to analyze perfume oil and fragrance in shower gel. A split/splitless (SSL) injector and a programmable temperature vaporization (PTV) injector are connected via a 2-way splitter of capillary flow technology (CFT) in this selectable (1)D/(2)D GC-MS/FID/ODP system to facilitate liquid sample injections and thermal desorption (TD) for stir bar sorptive extraction (SBSE) technique, respectively. The dual-linked injectors set-up enable the use of two different injector ports (one at a time) in single sequence run without having to relocate the (1)D capillary column from one inlet to another. Target analytes were separated in (1)D GC-MS/FID/ODP and followed by further separation of co-elution mixture from (1)D in (2)D GC-MS/FID/ODP in single injection without any instrumental reconfiguration. A (1)D/(2)D quantitative analysis method was developed and validated for its repeatability - tR; calculated linear retention indices (LRI); response ratio in both MS and FID signal, limit of detection (LOD), limit of quantitation (LOQ), as well as linearity over a concentration range. The method was successfully applied in quantitative analysis of perfume solution at different concentration level (RSD≤0.01%, n=5) and shower gel spiked with perfume at different dosages (RSD≤0.04%, n=5) with good recovery (96-103% for SSL injection; 94-107% for stir bar sorptive extraction-thermal desorption (SBSE-TD). Copyright © 2014 Elsevier B.V. All rights reserved.

Polydimethylsiloxane/metal-organic frameworks coated stir bar sorptive extraction coupled to gas chromatography-flame photometric detection for the determination of organophosphorus pesticides in environmental water samples.

PubMed

Xiao, Zuowei; He, Man; Chen, Beibei; Hu, Bin

2016-08-15

In this work, the metal-organic frameworks (MOFs), MIL-101-Cr-NH2 was synthesized via a direct hydrothermal method, and a polydimethylsiloxane (PDMS)/MIL-101-Cr-NH2 coated stir bar was prepared by sol-gel technique. Good reproducibility was obtained for the preparation of PDMS/MIL-101-Cr-NH2 coated stir bar with the relative standard deviations (RSDs) ranging from 3.7 to 5.2% (n=7) in one batch, and from 5.4 to 9.2% (n=7) among different batches. With the high surface area and rich benzene ring structure of MIL-101-Cr-NH2, the prepared PDMS/MIL-101-Cr-NH2 coated stir bar presented higher extraction efficiency for target organophosphorus pesticides (OPPs, including phorate, diazinon, malathion, fenthion, quinalphos and ethion) over PDMS coated stir bar. Based on it, a new method of PDMS/MIL-101-Cr-NH2 coated stir bar sorptive extraction (SBSE) coupled to gas chromatography-flame photometric detection (GC-FPD) was proposed for the determination of six OPPs in environmental water samples. The operation parameters affecting the extraction efficiency of SBSE, including extraction time, stirring rate, desorption time and ionic strength, were investigated. Under the optimal conditions, the limits of detection (S/N=3) were found to be in the range of 0.043-0.085μgL(-1) for the six target OPPs, and the linear range was 0.5-100μgL(-1) for malathion and 0.2-100μgL(-1) for other five OPPs. The RSDs of the proposed method evaluated at 1µgL(-1) for each OPP were in the range of 5.9-8.7% (intra-day, n=7) and 6.1-10.7% (inter-day, n=5), respectively. The enrichment factors were varied from 110 to 151-fold (theoretical enrichment factor was 200-fold). The proposed method was applied to the analysis of OPPs in East Lake and pond water samples with recoveries in the range of 89.3-115% and 80.0-113% for the spiked East Lake and pond water samples, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Silicone rod extraction followed by liquid desorption-large volume injection-programmable temperature vaporiser-gas chromatography-mass spectrometry for trace analysis of priority organic pollutants in environmental water samples.

PubMed

Delgado, Alejandra; Posada-Ureta, Oscar; Olivares, Maitane; Vallejo, Asier; Etxebarria, Nestor

2013-12-15

In this study a priority organic pollutants usually found in environmental water samples were considered to accomplish two extraction and analysis approaches. Among those compounds organochlorine compounds, pesticides, phthalates, phenols and residues of pharmaceutical and personal care products were included. The extraction and analysis steps were based on silicone rod extraction (SR) followed by liquid desorption in combination with large volume injection-programmable temperature vaporiser (LVI-PTV) and gas chromatography-mass spectrometry (GC-MS). Variables affecting the analytical response as a function of the programmable temperature vaporiser (PTV) parameters were firstly optimised following an experimental design approach. The SR extraction and desorption conditions were assessed afterwards, including matrix modification, time extraction, and stripping solvent composition. Subsequently, the possibility of performing membrane enclosed sorptive coating extraction (MESCO) as a modified extraction approach was also evaluated. The optimised method showed low method detection limits (3-35 ng L(-1)), acceptable accuracy (78-114%) and precision values (<13%) for most of the studied analytes regardless of the aqueous matrix. Finally, the developed approach was successfully applied to the determination of target analytes in aqueous environmental matrices including estuarine and wastewater samples. © 2013 Elsevier B.V. All rights reserved.

Sampling methods for the study of volatile profile of PDO wine vinegars. A comparison using multivariate data analysis.

PubMed

Ríos-Reina, Rocío; Morales, M Lourdes; García-González, Diego L; Amigo, José M; Callejón, Raquel M

2018-03-01

High-quality wine vinegars have been registered in Spain under protected designation of origin (PDO): "Vinagre de Jerez", "Vinagre de Condado de Huelva" and "Vinagre de Montilla-Moriles". The raw material, production and aging processes determine their quality and their aromatic composition. Vinegar volatile profile is usually analyzed by gas chromatography-mass spectrometry (GC-MS), being necessary a previous extraction step. Thus, three different sampling methods (Headspace solid phase microextraction "HS-SPME", Headspace stir bar sorptive extraction "HSSE" and Dynamic headspace extraction "DHS") were studied for the analysis of the volatile composition of Spanish PDO wine vinegars. Multivariate curve resolution (MCR) was used to solve chromatographic problems, improving the results obtained. Principal component analysis (PCA) showed that not all the sampling methods were equally suitable for the characterization and differentiation between PDOs and categories, being HSSE the technique that made able the best vinegar characterization. Copyright © 2017 Elsevier Ltd. All rights reserved.

A novel HS-SBSE system coupled with gas chromatography and mass spectrometry for the analysis of organochlorine pesticides in water samples.

PubMed

Grossi, Paula; Olivares, Igor R B; de Freitas, Diego R; Lancas, Fernando M

2008-10-01

A methodology to analyze organochlorine pesticides (OCPs) in water samples has been accomplished by using headspace stir bar sorptive extraction (HS-SBSE). The bars were in house coated with a thick film of PDMS in order to properly work in the headspace mode. Sampling was done by a novel HS-SBSE system whereas the analysis was performed by capillary GC coupled mass spectrometric detection (HS-SBSE-GC-MS). The extraction optimization, using different experimental parameters has been established by a standard equilibrium time of 120 min at 85 degrees C. A mixture of ACN/toluene as back extraction solvent promoted a good performance to remove the OCPs sorbed in the bar. Reproducibility between 2.1 and 14.8% and linearity between 0.96 and 1.0 were obtained for pesticides spiked in a linear range between 5 and 17 ng/g in water samples during the bar evaluation.

Early age compressive strength, porosity, and sorptivity of concrete using peat water to produce and cure concrete

NASA Astrophysics Data System (ADS)

Olivia, Monita; Ismeddiyanto, Wibisono, Gunawan; Sitompul, Iskandar R.

2017-09-01

Construction in peatland has faced scarce water sources for mixing and curing concrete. It is known that peat water has high organic content and low pH that can be harmful to concrete in the environment. In some remote areas in Riau Province, contractors used peat water directly without sufficient treatments to comply with SKSNI requirements of concrete mixing water. This paper presents a study of compressive strength, porosity and sorptivity of Ordinary Portland Cement (OPC) and blended OPC-Palm Oil Fuel Ash (OPC-POFA) concrete. The specimens were mixed using natural water and peat water, then some of them were cured in fresh water and peat water. Six mixtures were investigated using a variation of cement, mixing water and curing water. Tap water is used as control mixing and curing water for all specimens. The compressive strength, porosity and sorptivity were calculated at seven and 28 days. Results indicate that the use of peat water will cause low compressive strength, high porosity and sorptivity for both OPC and OPC-POFA concrete. Using peat water and curing the specimens in tap water could improve the early strength, porosity and sorptivity of OPC concrete; however, it has an adverse effect on OPC-POFA specimens. The properties of early age concrete of both types (OPC and OPC-POFA) using peat water were as good as those with tap water. Therefore, it is suggested that peat water should be considered as mixing and curing water for concrete where tap water resources are scarce. Investigation of its long-term properties, as well as extending the observed age of concrete is recommended before any use of peat water.

Analysis of preservatives with different polarities in beverage samples by dual-phase dual stir bar sorptive extraction combined with high-performance liquid chromatography.

PubMed

Xu, Jin; Chen, Beibei; He, Man; Hu, Bin

2013-02-22

A new concept of "dual-phase dual stir bar sorptive extraction (SBSE)" was proposed to simultaneously extract six preservatives with different polarities (logKo/w values of 1.27-3.41), namely, benzoic acid (BA), sorbic acid (SA), methyl p-hydroxybenzoate (MP), ethyl p-hydroxybenzoate (EP), propyl p-hydroxybenzoate (PP), and butyl p-hydroxybenzoate (BP). The dual-phase dual SBSE apparatus was consisted of two differently coated stir bars, a 3-aminopropyltriethoxysilane (APTES)-hydroxy-terminated silicone oil (OH-TSO)-coated stir bar that was prepared by sol-gel technique and a C(18) silica (C(18))-polydimethylsiloxane (PDMS)-coated stir bar that was prepared by adhesion. In dual-phase dual SBSE, the two stir bars with different coatings were placed in the same sample solution for the simultaneous extraction of the target analytes with different polarities, and then the bars were desorbed in the same desorption solvent. The extraction performance of the dual-phase dual SBSE for the six preservatives was evaluated by comparing with the conventional SBSE (individual stir bar) with different coatings, including commercial PDMS, homemade PDMS, C(18)-APTES-OH-TSO, APTES-OH-TSO, and C(18)-PDMS. The experimental results showed that the dual-phase dual SBSE had the highest extraction efficiency for the six target preservatives. Based on this fact, a novel method by combining the dual-phase dual SBSE which was consisted of the APTES-OH-TSO-coated and C(18)-PDMS-coated stir bars with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was developed for the simultaneous analysis of six target beverage preservatives in beverages. Under optimal conditions, the limits of detection (LODs) for six target preservatives ranged from 0.6 to 2.7 μgL(-1) with the relative standard deviations (RSDs) of 4.6-9.2% (C(BA,SA)=5 μgL(-1),C(MP)=20 μgL(-1),C(EP,PP,BP)=10 μgL(-1), n=7). The enrichment factors (EFs) were approximately 16-42-fold (theoretical EF was 50-fold). The proposed method was validated by the analysis of six target preservatives in three kinds of beverage samples, and the recoveries for the spiked samples were in the range of 76.6-118.6% for cola, 74.6-17.5% for orange juice, and 83.0-119.1% for herbal tea, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

Solid-phase extraction element based on epoxy polymer monolith for determination of polar organic compounds in aqueous media.

PubMed

Takahashi, Tadashi; Odagiri, Kayo; Watanabe, Atsushi; Watanabe, Chuichi; Kubo, Takuya; Hosoya, Ken

2011-10-01

A solid-phase extraction element based on epoxy polymer monolith was fabricated for sorptive enrichment of polar compounds from liquid and gaseous samples. After ultrasonication of the element in an aqueous solution for a given period of time, the thermal desorption (TD) using a pyrolyzer with gas chromatography/mass spectrometry (GC/MS), in which TD temperature was programmed from 50 to 250 °C for the analytes absorbed in the element, was used to evaluate the element for basic extraction performance using the aqueous standard mixtures consisting of compounds having varied polarities such as hexanol, isoamyl acetate, linalool, furfural and decanoic acid, in concentrations ranging from 10 μg/L to 1 mg/L. Excellent linear relationships were observed for all compounds in the standard mixture, except decanoic acid. In the extraction of beverages such as red wine, the extraction element showed stronger adsorption characteristics for polar compounds such as alcohols and acids than a non-polar polydimethylsiloxane-based element. This feature is derived from the main polymer structure along with hydroxyl and amino groups present in the epoxy-based monolith polymer matrix. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tortuous path chemical preconcentrator

DOEpatents

Manginell, Ronald P.; Lewis, Patrick R.; Adkins, Douglas R.; Wheeler, David R.; Simonson, Robert J.

2010-09-21

A non-planar, tortuous path chemical preconcentrator has a high internal surface area having a heatable sorptive coating that can be used to selectively collect and concentrate one or more chemical species of interest from a fluid stream that can be rapidly released as a concentrated plug into an analytical or microanalytical chain for separation and detection. The non-planar chemical preconcentrator comprises a sorptive support structure having a tortuous flow path. The tortuosity provides repeated twists, turns, and bends to the flow, thereby increasing the interfacial contact between sample fluid stream and the sorptive material. The tortuous path also provides more opportunities for desorption and readsorption of volatile species. Further, the thermal efficiency of the tortuous path chemical preconcentrator is comparable or superior to the prior non-planar chemical preconcentrator. Finally, the tortuosity can be varied in different directions to optimize flow rates during the adsorption and desorption phases of operation of the preconcentrator.

Determination of wear metals in engine oil by mild acid digestion and energy dispersive X-ray fluorescence spectrometry using solid phase extraction disks.

PubMed

Yang, Zheng; Hou, Xiandeng; Jones, Bradley T

2003-03-10

A simple, particle size-independent spectrometric method has been developed for the multi-element determination of wear metals in used engine oil. A small aliquot (0.5 ml) of an acid-digested oil sample is spotted onto a C-18 solid phase extraction disk to form a uniform thin film. The dried disk is then analyzed directly by energy dispersive X-ray fluorescence spectrometry. This technique provides a homogeneous and reproducible sample surface to the instrument, thus overcoming the typical problems associated with uneven particle size distribution and sedimentation. As a result, the method provides higher precision and accuracy than conventional methods. Furthermore, the disk sample may be stored and re-analyzed or extracted at a later date. The signals arising from the spotted disks, and the calibration curves constructed from them, are stable for at least 2 months. The limits of detection for Fe, Cu, Zn, Pb, and Cr are 5, 1, 4, 2, and 4 microg g(-1), respectively. Recoveries of these elements from spiked oil samples range from 92 to 110%. The analysis of two standard reference materials and a used oil sample produced results comparable to those found by inductively coupled plasma atomic emission spectrometry.

[Determination of 44 organophosphorus pesticides in food by SPE disk extraction-capillary gas chromatography with pulsed flame photometric detection].

PubMed

Luo, Xiao-Fei; Yang, Yuan; Sun, Cheng-Jun

2012-01-01

To develop a method for the simultaneous determination of 44 organophosphorus pesticides in food by SPE disk extraction-capillary gas chromatography with pulsed flame photometric detection. Organophosphorus pesticides in food were extracted ultrasonically with water. Then the extract was cleaned-up with SPE disk and eluted with ethyl acetate. Finally the eluent was condensed to 1mL under N2 at 55 degrees C. Gas chromatography was applied for quantitative detection of the organophosphorus pesticides in the sample. The linear range of the method for all the pesticides were in the range of 0.01-0.5 mg/kg with correlation coefficients of 0.992-1.000. The detection limits of the method were in the range of 0.0005-0.01 mg/kg. The recoveries for most pesticides were 60%-120% with relative standard deviations of less than 15%. The method is simple, sensitive, environmentally friendly and suitable for the determination of organophosphorous pesticides in food.

Zirconia coated stir bar sorptive extraction combined with large volume sample stacking capillary electrophoresis-indirect ultraviolet detection for the determination of chemical warfare agent degradation products in water samples.

PubMed

Li, Pingjing; Hu, Bin; Li, Xiaoyong

2012-07-20

In this study, a sensitive, selective and reliable analytical method by combining zirconia (ZrO₂) coated stir bar sorptive extraction (SBSE) with large volume sample stacking capillary electrophoresis-indirect ultraviolet (LVSS-CE/indirect UV) was developed for the direct analysis of chemical warfare agent degradation products of alkyl alkylphosphonic acids (AAPAs) (including ethyl methylphosphonic acid (EMPA) and pinacolyl methylphosphonate (PMPA)) and methylphosphonic acid (MPA) in environmental waters. ZrO₂ coated stir bar was prepared by adhering nanometer-sized ZrO₂ particles onto the surface of stir bar with commercial PDMS sol as adhesion agent. Due to the high affinity of ZrO₂ to the electronegative phosphonate group, ZrO₂ coated stir bars could selectively extract the strongly polar AAPAs and MPA. After systematically optimizing the extraction conditions of ZrO₂-SBSE, the analytical performance of ZrO₂-SBSE-CE/indirect UV and ZrO₂-SBSE-LVSS-CE/indirect UV was assessed. The limits of detection (LODs, at a signal-to-noise ratio of 3) obtained by ZrO₂-SBSE-CE/indirect UV were 13.4-15.9 μg/L for PMPA, EMPA and MPA. The relative standard deviations (RSDs, n=7, c=200 μg/L) of the corrected peak area for the target analytes were in the range of 6.4-8.8%. Enhancement factors (EFs) in terms of LODs were found to be from 112- to 145-fold. By combining ZrO₂ coating SBSE with LVSS as a dual preconcentration strategy, the EFs were magnified up to 1583-fold, and the LODs of ZrO₂-SBSE-LVSS-CE/indirect UV were 1.4, 1.2 and 3.1 μg/L for PMPA, EMPA, and MPA, respectively. The RSDs (n=7, c=20 μg/L) were found to be in the range of 9.0-11.8%. The developed ZrO₂-SBSE-LVSS-CE/indirect UV method has been successfully applied to the analysis of PMPA, EMPA, and MPA in different environmental water samples, and the recoveries for the spiked water samples were found to be in the range of 93.8-105.3%. Copyright © 2012 Elsevier B.V. All rights reserved.

Ultrastructural and biochemical localization of N-RAP at the interface between myofibrils and intercalated disks in the mouse heart.

PubMed

Zhang, J Q; Elzey, B; Williams, G; Lu, S; Law, D J; Horowits, R

2001-12-11

N-RAP is a recently discovered muscle-specific protein found at cardiac intercalated disks. Double immunogold labeling of mouse cardiac muscle reveals that vinculin is located immediately adjacent to the fascia adherens region of the intercalated disk membrane, while N-RAP extends approximately 100 nm further toward the interior of the cell. We partially purified cardiac intercalated disks using low- and high-salt extractions followed by density gradient centrifugation. Immunoblots show that this preparation is highly enriched in desmin and junctional proteins, including N-RAP, talin, vinculin, beta1-integrin, N-cadherin, and connexin 43. Electron microscopy and immunolabeling demonstrate that N-RAP and vinculin are associated with the large fragments of intercalated disks that are present in this preparation, which also contains numerous membrane vesicles. Detergent treatment of the partially purified intercalated disks removed the membrane vesicles and extracted vinculin and beta1-integrin. Further separation on a sucrose gradient removed residual actin and myosin and yielded a fraction morphologically similar to fasciae adherentes that was highly enriched in N-RAP, N-cadherin, connexin 43, talin, desmin, and alpha-actinin. The finding that N-RAP copurifies with detergent-extracted intercalated disk fragments even though beta-integrin and vinculin have been completely removed suggests that N-RAP association with the adherens junction region is mediated by the cadherin system. Consistent with this hypothesis, we found that recombinant N-RAP fragments bind alpha-actinin in a gel overlay assay. In addition, immunofluorescence shows that N-RAP remains bound at the ends of isolated, detergent-treated cardiac myofibrils. These results demonstrate that N-RAP remains tightly bound to myofibrils and fasciae adherentes during biochemical purification and may be a key constituent in the mechanical link between these two structures.

Linking hydraulic properties of fire-affected soils to infiltration and water repellency

USGS Publications Warehouse

Moody, John A.; David Kinner,; Xavier Úbeda,

2009-01-01

Heat from wildfires can produce a two-layer system composed of extremely dry soil covered by a layer of ash, which when subjected to rainfall, may produce extreme floods. To understand the soil physics controlling runoff for these initial conditions, we used a small, portable disk infiltrometer to measure two hydraulic properties: (1) near-saturated hydraulic conductivity, Kf and (2) sorptivity, S(θi), as a function of initial soil moisture content, θi, ranging from extremely dry conditions (θi < 0.02 cm3 cm−3) to near saturation. In the field and in the laboratory replicate measurements were made of ash, reference soils, soils unaffected by fire, and fire-affected soils. Each has a different degrees of water repellency that influences Kf and S(θi).Values of Kf ranged from 4.5 × 10−3 to 53 × 10−3 cm s−1 for ash; from 0.93 × 10−3 to 130 × 10−3 cm s−1 for reference soils; and from 0.86 × 10−3 to 3.0 × 10−3 cm s−1, for soil unaffected by fire, which had the lowest values of Kf. Measurements indicated that S(θi) could be represented by an empirical non-linear function of θi with a sorptivity maximum of 0.18–0.20 cm s−0.5, between 0.03 and 0.08 cm3 cm−3. This functional form differs from the monotonically decreasing non-linear functions often used to represent S(θi) for rainfall–runoff modeling. The sorptivity maximum may represent the combined effects of gravity, capillarity, and adsorption in a transitional domain corresponding to extremely dry soil, and moreover, it may explain the observed non-linear behavior, and the critical soil-moisture threshold of water repellent soils. Laboratory measurements of Kf and S(θi) are the first for ash and fire-affected soil, but additional measurements are needed of these hydraulic properties for in situ fire-affected soils. They provide insight into water repellency behavior and infiltration under extremely dry conditions. Most importantly, they indicate how existing rainfall–runoff models can be modified to accommodate a possible two-layer system in extremely dry conditions. These modified models can be used to predict floods from burned watersheds under these initial conditions.

Automated Solar Flare Detection and Feature Extraction in High-Resolution and Full-Disk Hα Images

NASA Astrophysics Data System (ADS)

Yang, Meng; Tian, Yu; Liu, Yangyi; Rao, Changhui

2018-05-01

In this article, an automated solar flare detection method applied to both full-disk and local high-resolution Hα images is proposed. An adaptive gray threshold and an area threshold are used to segment the flare region. Features of each detected flare event are extracted, e.g. the start, peak, and end time, the importance class, and the brightness class. Experimental results have verified that the proposed method can obtain more stable and accurate segmentation results than previous works on full-disk images from Big Bear Solar Observatory (BBSO) and Kanzelhöhe Observatory for Solar and Environmental Research (KSO), and satisfying segmentation results on high-resolution images from the Goode Solar Telescope (GST). Moreover, the extracted flare features correlate well with the data given by KSO. The method may be able to implement a more complicated statistical analysis of Hα solar flares.

Sorptive Activity and Hydrophobic Behavior of Aerogels Based on Reduced Graphene Oxide and Carbon Nanotubes

NASA Astrophysics Data System (ADS)

Sultanov, F.; Bakbolat, B.; Daulbaev, Ch.; Urazgalieva, A.; Azizov, Z.; Mansurov, Z.; Tulepov, M.; Pei, S. S.

2017-07-01

A study has been made of the possibility of obtaining three-dimensional porous aerogel structures based on reduced graphene oxide and carbon nanotubes. Carbon nanotubes in the structure of the finished aerogel based on reduced graphene oxide were grown by thermal decomposition of ferrocene into cyclopentadienyl and iron ions which served as the source of carbon and a catalyst respectively. The obtained composite aerogels exhibit high sorptive activity for organic liquids of different densities.

Microextraction techniques for the determination of volatile and semivolatile organic compounds from plants: a review.

PubMed

Yang, Cui; Wang, Juan; Li, Donghao

2013-10-17

Vegetables and fruits are necessary for human health, and traditional Chinese medicine that uses plant materials can cure diseases. Thus, understanding the composition of plant matrix has gained increased attention in recent years. Since plant matrix is very complex, the extraction, separation and quantitation of these chemicals are challenging. In this review we focus on the microextraction techniques used in the determination of volatile and semivolatile organic compounds (such as esters, alcohols, aldehydes, hydrocarbons, ketones, terpenes, sesquiterpene, phenols, acids, plant secondary metabolites and pesticides) from plants (e.g., fruits, vegetables, medicinal plants, tree leaves, etc.). These microextraction techniques include: solid phase microextraction (SPME), stir-bar sorptive extraction (SBSE), single drop microextraction (SDME), hollow fiber liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME), and gas purge microsyringe extraction (GP-MSE). We have taken into consideration papers published from 2008 to the end of January 2013, and provided critical and interpretative review on these techniques, and formulated future trends in microextraction for the determination of volatile and semivolatile compounds from plants. Copyright © 2013 Elsevier B.V. All rights reserved.

Automated feature extraction in color retinal images by a model based approach.

PubMed

Li, Huiqi; Chutatape, Opas

2004-02-01

Color retinal photography is an important tool to detect the evidence of various eye diseases. Novel methods to extract the main features in color retinal images have been developed in this paper. Principal component analysis is employed to locate optic disk; A modified active shape model is proposed in the shape detection of optic disk; A fundus coordinate system is established to provide a better description of the features in the retinal images; An approach to detect exudates by the combined region growing and edge detection is proposed. The success rates of disk localization, disk boundary detection, and fovea localization are 99%, 94%, and 100%, respectively. The sensitivity and specificity of exudate detection are 100% and 71%, correspondingly. The success of the proposed algorithms can be attributed to the utilization of the model-based methods. The detection and analysis could be applied to automatic mass screening and diagnosis of the retinal diseases.

A new approach for the extraction of pollutants from wastewaters handled by the graphic industry.

PubMed

Monteiro, C; Ventura, C; Martins, F

2013-06-15

It is widely recognized that the Graphic Industry handles toxic products and produces, in its various operations, toxic wastes. These wastes can cause serious environmental damages and can lead to severe health problems. In this work we report an efficient, simple and cheap to run method for the removal of some of the most common pollutants involved in the various stages of the Graphic Industry production, using a Solid-Phase Extraction (SPE) methodology. We have determined equilibrium constants, K(eq), and adsorption (k(up)) and desorption (k(off)) rate constants for the extraction of benzene, xylene, toluene and ethylbenzene (BXTE) from water, using C18 disks. The removal of these compounds was monitored by UV-vis spectroscopy, at room temperature. Average extraction efficiencies were of 60% in a mixture of BXTEs and close to 80% when pollutants were assessed separately. Since the retention mechanism in the C18 disk is essentially governed by hydrophobic interactions between the compounds and the alkyl chains of the disk, we have also shown that these pollutants' lipophilicity plays an important role in the rationalization of their behavior during the extraction process. Copyright © 2013 Elsevier Ltd. All rights reserved.

Pressure-driven mesofluidic platform integrating automated on-chip renewable micro-solid-phase extraction for ultrasensitive determination of waterborne inorganic mercury.

PubMed

Portugal, Lindomar A; Laglera, Luis M; Anthemidis, Aristidis N; Ferreira, Sérgio L C; Miró, Manuel

2013-06-15

A dedicated pressure-driven mesofluidic platform incorporating on-chip sample clean-up and analyte preconcentration is herein reported for expedient determination of trace level concentrations of waterborne inorganic mercury. Capitalizing upon the Lab-on-a-Valve (LOV) concept, the mesofluidic device integrates on-chip micro-solid phase extraction (μSPE) in automatic disposable mode followed by chemical vapor generation and gas-liquid separation prior to in-line atomic fluorescence spectrometric detection. In contrast to prevailing chelating sorbents for Hg(II), bare poly(divinylbenzene-N-vinylpyrrolidone) copolymer sorptive beads were resorted to efficient uptake of Hg(II) in hydrochloric acid milieu (pH=2.3) without the need for metal derivatization nor pH adjustment of prior acidified water samples for preservation to near-neutral conditions. Experimental variables influencing the sorptive uptake and retrieval of target species and the evolvement of elemental mercury within the miniaturized integrated reaction chamber/gas-liquid separator were investigated in detail. Using merely <10 mg of sorbent, the limits of detection and quantification at the 3s(blank) and 10s(blank) levels, respectively, for a sample volume of 3 mL were 12 and 42 ng L(-1) Hg(II) with a dynamic range extending up to 5.0 μg L(-1). The proposed mesofluidic platform copes with the requirements of regulatory bodies (US-EPA, WHO, EU-Commission) for drinking water quality and surface waters that endorse maximum allowed concentrations of mercury spanning from 0.07 to 6.0 μg L(-1). Demonstrated with the analysis of aqueous samples of varying matrix complexity, the LOV approach afforded reliable results with relative recoveries of 86-107% and intermediate precision down to 9% in the renewable μSPE format. Copyright © 2013 Elsevier B.V. All rights reserved.

Scalable isosurface visualization of massive datasets on commodity off-the-shelf clusters

PubMed Central

Bajaj, Chandrajit

2009-01-01

Tomographic imaging and computer simulations are increasingly yielding massive datasets. Interactive and exploratory visualizations have rapidly become indispensable tools to study large volumetric imaging and simulation data. Our scalable isosurface visualization framework on commodity off-the-shelf clusters is an end-to-end parallel and progressive platform, from initial data access to the final display. Interactive browsing of extracted isosurfaces is made possible by using parallel isosurface extraction, and rendering in conjunction with a new specialized piece of image compositing hardware called Metabuffer. In this paper, we focus on the back end scalability by introducing a fully parallel and out-of-core isosurface extraction algorithm. It achieves scalability by using both parallel and out-of-core processing and parallel disks. It statically partitions the volume data to parallel disks with a balanced workload spectrum, and builds I/O-optimal external interval trees to minimize the number of I/O operations of loading large data from disk. We also describe an isosurface compression scheme that is efficient for progress extraction, transmission and storage of isosurfaces. PMID:19756231

Disk-Anchored Magnetic Propellers - A Cure for the SW Sex Syndrome

NASA Astrophysics Data System (ADS)

Horne, Keith

In AE Aqr, magnetic fields transfer energy and angular momentum from a rapidly-spinning white dwarf to material in the gas stream from the companion star, with the effect of spinning down the white dwarf while flinging the gas stream material out of the binary system. This magnetic propeller produces a host of observable signatures, chief among which are broad, single-peaked, flaring emission lines with phase-shifted orbital kinematics. SW Sex stars have accretion disks, but also broad, single-peaked, phase-shifted emission lines similar to those seen in AE Aqr. We propose that a magnetic propeller similar to that which operates in AE Aqr is also at work in SW Sex stars - and to some extent in all nova-like systems. The propeller is anchored in the inner accretion disk, rather than, or in addition to, the white dwarf. Energy and angular momentum are thereby extracted from the inner disk and transferred to gas-stream material flowing above the disk, which is consequently pitched out of the system. This provides a non-local, dissipationless angular-momentum-extraction mechanism, which should result in cool inner disks with temperature profiles flatter than T propto R^{-3/4}, as observed in eclipse mapping studies of nova-like variables. The disk-anchored magnetic propeller model appears to explain qualitatively most if not all of the peculiar features of the SW Sex syndrome.

Separation and purification of thymopentin with molecular imprinting membrane by solid phase extraction disks.

PubMed

Wang, Chaoli; Hu, Xiaoling; Guan, Ping; Wu, Danfeng; Qian, Liwei; Li, Ji; Song, Renyuan

2015-01-01

The synthesis and performance of molecularly imprinted membranes (MIMs) as a solid phase extraction packing materials for the separation and purification of thymopentin from crude samples was described. In order to increase structural selectivity and imprinting efficiency, surface-initiated ATRP and ionic liquid (1-vinyl-3-ethyl acetate imidazolium chloride) were used to prepare molecularly imprinting membranes. The results demonstrated that solid phase extraction disks stuffed by MIMs with ionic liquids as functional monomer demonstrated high isolation and purification of performance to the thymopentin. The molecular recognition of thymopentin was analyzed by using molecular modeling software. Copyright © 2014 Elsevier B.V. All rights reserved.

Characterization of mesoporous silica used for drug delivery by sorptive interaction - multiple headspace extraction-gas chromatography.

PubMed

Aspromonte, Juan; Wolfs, Kris; Kahsay, Getu; Van Schepdael, Ann; Adams, Erwin

2018-09-01

A multiple headspace extraction experiment coupled to gas chromatography (MHE-GC) is used for the classification and qualification of different mesoporous silica (MPSi) materials used for drug delivery. In this MHE experiment, a pure liquid solvent probe is fully evaporated in a sealed headspace vial in the presence of the MPSi sample, leading to a gas-solid partitioning that is theoretically described. The obtained results matched with the known characteristics of the studied samples, such as adsorption capacity due to differences in porosity and passivation treatments. Moreover, it proves the effectiveness of a poly dimethyl siloxane (PDMS) coating treatment over a thermal one in reducing the specific interactions of the MPSi. In addition, it evidences the important role of confinement effects when the pore diameter is close to the microporosity range. Finally, a simple experiment for fast screening is proposed by comparison of the results obtained for four different probes used as a mixture. Copyright © 2018 Elsevier B.V. All rights reserved.

Laboratory Comparison of the Anti-Bacterial Effects of Spearmint Extract and Hypochlorite Sodium on Enterococcus Faecalis Bacteria.

PubMed

S, Hajimaghsoodi; H, Zandi; M, Bahrami; R, Hakimian

2016-12-01

It is necessary to use irrigation solutions during cleaning and shaping of root canals to efficiently reduce the number of micro organisms. Sodium hypochlorite is used as an effective antibacterial endodontic irrigants. However, the extract of pennyroyal plant has also shown anti-bacterial characteristics comparable with antibacterial drugs. To compare the anti-bacterial effect of spearmint extract on Enterococcus faecalis bacteria with that of sodium hypochlorite 5.25%. In this experimental study, Muller Hinton medium, including 5% sheep blood was prepared. The two solutions used including sodium hypochlorite 5.25% and spearmint extracts were put adjacent to Enterococcus faecalis bacteria after preparing. Two groups, each containing 10 samples, with the total of 20 samples were used. The disks, including each solution were placed 2 cm apart on a plate containing Muller Hinton medium and the bacteria. The plate was subsequently incubated at 37°C for 48 hours. After incubation, the mean diameter of the halo around each disk, which represents the lack of bacterial growth, was measured and compared using a ruler. Penicillin disk was used for positive control and a sterile blank disk containing physiologic serum was utilized as the negative control. This process was repeated 10 times for each solution. Data were analyzed in SPSS 17 statistical software using t -test. The results showed that the mean diameter of halo in the spearmint extract group was zero and in the sodium hypochlorite group it was 23.7 ± 1.49 mm. There was a significant difference between the mean diameter of the lack of growth halo of the spearmint extract and that of hypochlorite sodium 5.25% on Enterococcus faecalis bacteria ( p ≤ 0.001). Considering the limitations of an experimental study, it seems that spearmint extract does not have any anti-bacterial effect against Enterococcus faecalis bacteria, in contrast to hypochlorite sodium 5.25%.

Disk diffusion antimicrobial susceptibility testing of members of the family Legionellaceae including erythromycin-resistant variants of Legionella micdadei.

PubMed Central

Dowling, J N; McDevitt, D A; Pasculle, A W

1984-01-01

Disk diffusion antimicrobial susceptibility testing of members of the family Legionellaceae was accomplished on buffered charcoal yeast extract agar by allowing the bacteria to grow for 6 h before placement of the disks, followed by an additional 42-h incubation period before the inhibitory zones were measured. This system was standardized by comparing the zone sizes with the MICs for 20 antimicrobial agents of nine bacterial strains in five Legionella species and of 19 laboratory-derived, erythromycin-resistant variants of Legionella micdadei. A high, linear correlation between zone size and MIC was found for erythromycin, trimethoprim, penicillin, ampicillin, carbenicillin, cephalothin, cefamandole, cefoxitin, moxalactam, chloramphenicol, vancomycin, and clindamycin. Disk susceptibility testing could be employed to screen Legionella isolates for resistance to any of these antimicrobial agents, of which only erythromycin is known to be efficacious in the treatment of legionellosis. With selected antibiotics, disk susceptibility patterns also appeared to accurately identify to the species level the legionellae. The range of the MICs of the legionellae for rifampin and the aminoglycosides was too small to determine whether the correlation of zone size with MIC was linear. However, laboratory-derived, high-level rifampin-resistant variants of L. micdadei demonstrated no inhibition zone around the rifampin disk, indicating that disk susceptibility testing would likely identify a rifampin-resistant clinical isolate. Of the antimicrobial agents tested, the only agents for which disk susceptibility testing was definitely not possible on buffered charcoal yeast extract agar were oxacillin, the tetracyclines, and the sulfonamides. PMID:6565706

Determination of trace metals in drinking water using solid-phase extraction disks and X-ray fluorescence spectrometry.

PubMed

Hou, Xiandeng; Peters, Heather L; Yang, Zheng; Wagner, Karl A; Batchelor, James D; Daniel, Meredith M; Jones, Bradley T

2003-03-01

A convenient method is described for monitoring Cd, Ni, Cu, and Pb at trace levels in drinking water samples. These metals are preconcentrated on a chelating solid-phase extraction disk and then determined by X-ray fluorescence spectrometry. The method tolerates a wide pH range (pH 6-14) and a large amount of alkaline and alkaline earth elements. The preconcentration factor is well over 1600, assuming a 1 L water sample volume. The limits of detection for Cd, Ni, Cu, and Pb are 3.8, 0.6, 0.4, and 0.3 ng/mL, respectively. These are well below the federal maximum contaminant level values, which are 5, 100, 1300, and 15 ng/mL, respectively. The proposed method has many advantages including ease of operation, multielement capability, nondestructiveness, high sensitivity, and relative cost efficiency. The solid-phase extraction step can be conducted in the field and then the disks can be mailed to a laboratory for the analysis, eliminating the cost of transporting large volumes of water samples. Furthermore, the color of the used extraction disk provides an initial estimate of the degree of contamination for some transition metals (for example, Ni and Cu). Thus, the overall cost for analysis of metals in drinking water can be minimized by implementing the method, and small water supply companies with limited budgets will be better able to comply with the Safe Drinking Water Act.

Trace determination of volatile polycyclic aromatic hydrocarbons in natural waters by magnetic ionic liquid-based stir bar dispersive liquid microextraction.

PubMed

Benedé, Juan L; Anderson, Jared L; Chisvert, Alberto

2018-01-01

In this work, a novel hybrid approach called stir bar dispersive liquid microextraction (SBDLME) that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) has been employed for the accurate and sensitive determination of ten polycyclic aromatic hydrocarbons (PAHs) in natural water samples. The extraction is carried out using a neodymium stir bar magnetically coated with a magnetic ionic liquid (MIL) as extraction device, in such a way that the MIL is dispersed into the solution at high stirring rates. Once the stirring is ceased, the MIL is magnetically retrieved onto the stir bar, and subsequently subjected to thermal desorption (TD) coupled to a gas chromatography-mass spectrometry (GC-MS) system. The main parameters involved in TD, as well as in the extraction step affecting the extraction efficiency (i.e., MIL amount, extraction time and ionic strength) were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ng L -1 level, good intra- and inter-day repeatability (RSD < 13%) and good enrichment factors (18 - 717). This sensitive analytical method was applied to the determination of trace amounts of PAHs in three natural water samples (river, tap and rainwater) with satisfactory relative recovery values (84-115%), highlighting that the matrices under consideration do not affect the extraction process. Copyright © 2017 Elsevier B.V. All rights reserved.

Gamma-BHC/Cereclor—a new, long-acting lindane formulation for malaria control

PubMed Central

Hocking, K. S.; Armstrong, J. A.; Downing, F. S.

1960-01-01

Sorption of insecticides by muds and other materials used in the construction of native huts prolongs their duration of action or persistence. The use of gamma-BHC as a residual insecticide has been limited by the fact that its sorption by most materials is of a low order, so that it is comparatively short acting. If gamma-BHC is melted with a resin, the solid solution can be converted into a water-dispersible powder which is much more persistent on sorptive and semi-sorptive surfaces. Laboratory experiments had shown that the best results were obtained with a proprietary resin known as Cereclor. Field trials conducted by the authors have now demonstrated that this formulation retained its efficacy for at least six months, even on surfaces of low sorptive power, such as thatch and sisal. Gamma-BHC alone was much less persistent, except on mud walls, but even here bioassay showed the formulation with Cereclor to be more active. The authors consider that gamma-BHC/Cereclor approximates to the ideal insecticide for the spraying of native huts in malaria control. PMID:14402213

Interlaboratory comparison of extraction efficiency of pesticides from surface and laboratory water using solid-phase extraction disks.

PubMed

Senseman, Scott A; Mueller, Thomas C; Riley, Melissa B; Wauchope, R Don; Clegg, Chris; Young, Roddy W; Southwick, Lloyd M; Moye, H Anson; Dumas, Jose A; Mersie, Wondi; Mattice, John D; Leidy, Ross B

2003-06-18

A continuation of an earlier interlaboratory comparison was conducted (1) to assess solid-phase extraction (SPE) using Empore disks to extract atrazine, bromacil, metolachlor, and chlorpyrifos from various water sources accompanied by different sample shipping and quantitative techniques and (2) to compare quantitative results of individual laboratories with results of one common laboratory. Three replicates of a composite surface water (SW) sample were fortified with the analytes along with three replicates of deionized water (DW). A nonfortified DW sample and a nonfortified SW sample were also extracted. All samples were extracted using Empore C(18) disks. After extraction, part of the samples were eluted and analyzed in-house. Duplicate samples were evaporated in a 2-mL vial, shipped dry to a central laboratory (SDC), redissolved, and analyzed. Overall, samples analyzed in-house had higher recoveries than SDC samples. Laboratory x analysis type and laboratory x water source interactions were significant for all four compounds. Seven laboratories participated in this interlaboratory comparison program. No differences in atrazine recoveries were observed from in-house samples analyzed by laboratories A, B, D, and G compared with the recovery of SDC samples. In-house atrazine recoveries from laboratories C and F were higher when compared with recovery from SDC samples. However, laboratory E had lower recoveries from in-house samples compared with SDC samples. For each laboratory, lower recoveries were observed for chlorpyrifos from the SDC samples compared with samples analyzed in-house. Bromacil recovery was <65% at two of the seven laboratories in the study. Bromacil recoveries for the remaining laboratories were >75%. Three laboratories showed no differences in metolachlor recovery; two laboratories had higher recoveries for samples analyzed in-house, and two other laboratories showed higher metolachlor recovery for SDC samples. Laboratory G had a higher recovery in SW for all four compounds compared with DW. Other laboratories that had significant differences in pesticide recovery between the two water sources showed higher recovery in DW than in the SW regardless of the compound. In comparison to earlier work, recovery of these compounds using SPE disks as a temporary storage matrix may be more effective than shipping dried samples in a vial. Problems with analytes such as chlorpyrifos are unavoidable, and it should not be assumed that an extraction procedure using SPE disks will be adequate for all compounds and transferrable across all chromatographic conditions.

Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

PubMed

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2013-12-20

Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

Rapid, specific determination of iodine and iodide by combined solid-phase extraction/diffuse reflectance spectroscopy

NASA Technical Reports Server (NTRS)

Arena, Matteo P.; Porter, Marc D.; Fritz, James S.

2002-01-01

A new, rapid methodology for trace analysis using solid-phase extraction is described. The two-step methodology is based on the concentration of an analyte onto a membrane disk and on the determination by diffuse reflectance spectroscopy of the amount of analyte extracted on the disk surface. This method, which is adaptable to a wide range of analytes, has been used for monitoring ppm levels of iodine and iodide in spacecraft water. Iodine is used as a biocide in spacecraft water. For these determinations, a water sample is passed through a membrane disk by means of a 10-mL syringe that is attached to a disk holder assembly. The disk, which is a polystyrene-divinylbenzene composite, is impregnated with poly(vinylpyrrolidone) (PVP), which exhaustively concentrates iodine as a yellow iodine-PVP complex. The amount of concentrated iodine is then determined in only 2 s by using a hand-held diffuse reflectance spectrometer by comparing the result with a calibration curve based on the Kubelka-Munk function. The same general procedure can be used to determine iodide levels after its facile and exhaustive oxidation to iodine by peroxymonosulfate (i.e., Oxone reagent). For samples containing both analytes, a two-step procedure can be used in which the iodide concentration is calculated from the difference in iodine levels before and after treatment of the sample with peroxymonosulfate. With this methodology, iodine and iodide levels in the 0.1-5.0 ppm range can be determined with a total workup time of approximately 60 s with a RSD of approximately 6%.

On the Star Formation Rate, Initial Mass Function, and Hubble Type of Disk Galaxies and the Age of the Universe

NASA Astrophysics Data System (ADS)

Sommer-Larsen, Jesper

1996-01-01

Evolutionary models for the disks of large disk galaxies, including effects of star formation, non-instantaneous gas recycling from stars, and infall of low-metallicity gas from the halo, have been calculated and compared with data for nearby, generally large disk galaxies on present disk star-formation rates (based on integrated Hα luminosities) as a function of disk gas fractions. The data were extracted from the work by Kennicutt, Tamblyn, & Congdon. The result of the comparison suggests that for disk galaxies the Hubble sequence is a disk age sequence, with early-type disks being the oldest and late types the youngest. Under the assumption of a minimum age of the Galactic disk of 10 Gyr, the mean age of Sa/Sab galaxies, and hence the age of the universe, is found to be at least 17±2 Gyr. It is furthermore found that the disk star-formation timescale is approximately independent of disk-galaxy type. Finally, it is found that the global initial mass function (IMF) in galactic disks is 2-3 times more weighted toward high-mass stars than the Scalo "best-fitting" model for the solar-neighborhood IMF. The more top-heavy model of Kennicutt provides a good fit to observation.

Method for optical pumping of thin laser media at high average power

DOEpatents

Zapata, Luis E [Livermore, CA; Beach, Raymond J [Livermore, CA; Honea, Eric C [Sunol, CA; Payne, Stephen A [Castro Valley, CA

2004-07-13

A thin, planar laser material is bonded to a light guide of an index-matched material forming a composite disk. Diode array or other pump light is introduced into the composite disk through the edges of the disk. Pump light trapped within the composite disk depletes as it multi-passes the laser medium before reaching an opposing edge of the disk. The resulting compound optical structure efficiently delivers concentrated pump light and to a laser medium of minimum thickness. The external face of the laser medium is used for cooling. A high performance cooler attached to the external face of the laser medium rejects heat. Laser beam extraction is parallel to the heat flux to minimize optical distortions.

The influence of microtopography on soil nutrients in created mitigation wetlands

USGS Publications Warehouse

Moser, K.F.; Ahn, C.; Noe, G.B.

2009-01-01

This study explores the relationship between microtopography and soil nutrients (and trace elements), comparing results for created and reference wetlands in Virginia, and examining the effects of disking during wetland creation. Replicate multiscale tangentially conjoined circular transects were used to quantify microtopography both in terms of elevation and by two microtopographic indices. Corresponding soil samples were analyzed for moisture content, total C and N, KCl-extractable NH4-N and NO3-N, and Mehlich-3 extractable P, Ca, Mg, K, Al, Fe, and Mn. Means and variances of soil nutrient/element concentrations were compared between created and natural wetlands and between disked and nondisked created wetlands. Natural sites had higher and more variable soil moisture, higher extractable P and Fe, lower Mn than created wetlands, and comparatively high variability in nutrient concentrations. Disked sites had higher soil moisture, NH4-N, Fe, and Mn than did nondisked sites. Consistently low variances (Levene test for inequality) suggested that nondisked sites had minimal nutrient heterogeneity. Across sites, low P availability was inferred by the molar ratio (Mehlich-3 [P/(Al + Fe)] < 0.06); strong intercorrelations among total C, total N, and extractable Fe, Al, and P suggested that humic-metal-P complexes may be important for P retention and availability. Correlations between nutrient/element concentrations and microtopographic indices suggested increased Mn and decreased K and Al availability with increased surface roughness. Disking appears to enhance water and nutrient retention, as well as nutrient heterogeneity otherwise absent from created wetlands, thus potentially promoting ecosystem development. ?? 2008 Society for Ecological Restoration International.

Analytical methods for the assessment of endocrine disrupting chemical exposure during human fetal and lactation stages: a review.

PubMed

Jiménez-Díaz, I; Vela-Soria, F; Rodríguez-Gómez, R; Zafra-Gómez, A; Ballesteros, O; Navalón, A

2015-09-10

In the present work, a review of the analytical methods developed in the last 15 years for the determination of endocrine disrupting chemicals (EDCs) in human samples related with children, including placenta, cord blood, amniotic fluid, maternal blood, maternal urine and breast milk, is proposed. Children are highly vulnerable to toxic chemicals in the environment. Among these environmental contaminants to which children are at risk of exposure are EDCs -substances able to alter the normal hormone function of wildlife and humans-. The work focuses mainly on sample preparation and instrumental techniques used for the detection and quantification of the analytes. The sample preparation techniques include, not only liquid-liquid extraction (LLE) and solid-phase extraction (SPE), but also modern microextraction techniques such as extraction with molecular imprinted polymers (MIPs), stir-bar sorptive extraction (SBSE), hollow-fiber liquid-phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME), matrix solid phase dispersion (MSPD) or ultrasound-assisted extraction (UAE), which are becoming alternatives in the analysis of human samples. Most studies focus on minimizing the number of steps and using the lowest solvent amounts in the sample treatment. The usual instrumental techniques employed include liquid chromatography (LC), gas chromatography (GC) mainly coupled to tandem mass spectrometry. Multiresidue methods are being developed for the determination of several families of EDCs with one extraction step and limited sample preparation. Copyright © 2015 Elsevier B.V. All rights reserved.

Misaligned Accretion and Jet Production

NASA Astrophysics Data System (ADS)

King, Andrew; Nixon, Chris

2018-04-01

Disk accretion onto a black hole is often misaligned from its spin axis. If the disk maintains a significant magnetic field normal to its local plane, we show that dipole radiation from Lense–Thirring precessing disk annuli can extract a significant fraction of the accretion energy, sharply peaked toward small disk radii R (as R ‑17/2 for fields with constant equipartition ratio). This low-frequency emission is immediately absorbed by surrounding matter or refracted toward the regions of lowest density. The resultant mechanical pressure, dipole angular pattern, and much lower matter density toward the rotational poles create a strong tendency to drive jets along the black hole spin axis, similar to the spin-axis jets of radio pulsars, also strong dipole emitters. The coherent primary emission may explain the high brightness temperatures seen in jets. The intrinsic disk emission is modulated at Lense–Thirring frequencies near the inner edge, providing a physical mechanism for low-frequency quasi-periodic oscillations (QPOs). Dipole emission requires nonzero hole spin, but uses only disk accretion energy. No spin energy is extracted, unlike the Blandford–Znajek process. Magnetohydrodynamic/general-relativistic magnetohydrodynamic (MHD/GRMHD) formulations do not directly give radiation fields, but can be checked post-process for dipole emission and therefore self-consistency, given sufficient resolution. Jets driven by dipole radiation should be more common in active galactic nuclei (AGN) than in X-ray binaries, and in low accretion-rate states than high, agreeing with observation. In non-black hole accretion, misaligned disk annuli precess because of the accretor’s mass quadrupole moment, similarly producing jets and QPOs.

Determination of diphenylarsinic acid, phenylarsonic acid and inorganic arsenic in drinking water by graphite-furnace atomic-absorption spectrometry after simultaneous separation and preconcentration with solid-phase extraction disks.

PubMed

Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Nakamura, Toshihiro

2013-01-01

A simple method of graphite-furnace atomic-absorption spectrometry (GFAAS) after solid-phase extraction (SPE) was developed for the determination of diphenylarsinic acid (DPAA), phenylarsonic acid (PAA), and inorganic arsenic (iAs) in drinking water. This method involves the simultaneous collection of DPAA, PAA, and iAs using three stacked SPE disks, i.e., an Empore SDB-XD disk (the upper layer), an activated carbon disk (the middle layer), and a Cation-SR disk loaded with Zr and Ca (ZrCa-CED; the lower layer). A 200-mL aqueous sample was adjusted to pH 3 with nitric acid and passed through the SPE disks at a flow rate of 15 mL min(-1), to concentrate DPAA on the SDB-XD disk, PAA on the activated carbon disk, and iAs on the ZrCa-CED. The As compounds were eluted from the disks with 10 mL of ethanol containing 0.5 mol L(-1) ammonia solution for DPAA, 20 mL of 1 mol L(-1) ammonia solution for PAA, and 20 mL of 6 mol L(-1) hydrochloric acid for iAs. The eluates of DPAA, PAA, and iAs were diluted to 20, 25, and 25 mL, respectively, with deionized water, and then analyzed by GFAAS. The detection limits of As (three-times the standard deviation (n = 3) of the blank values) were 0.13 and 0.16 μg L(-1) at enrichment factors of 10 and 8, respectively, using a 200-mL water sample. Spike tests with 2 μg (10 μg L(-1)) of DPAA, PAA, and iAs in 200 mL of tap water and bottled drinking water showed good recoveries (96.1-103.8%).

Limited Area Coverage/High Resolution Picture Transmission (LAC/HRPT) tape IJ grid pixel extraction processor user's manual

NASA Technical Reports Server (NTRS)

Obrien, S. O. (Principal Investigator)

1980-01-01

The program, LACREG, extracted all pixels that are contained in a specific IJ grid section. The pixels, along with a header record are stored in a disk file defined by the user. The program will extract up to 99 IJ grid sections.

Metal-organic framework mixed-matrix disks: Versatile supports for automated solid-phase extraction prior to chromatographic separation.

PubMed

Ghani, Milad; Font Picó, Maria Francesca; Salehinia, Shima; Palomino Cabello, Carlos; Maya, Fernando; Berlier, Gloria; Saraji, Mohammad; Cerdà, Víctor; Turnes Palomino, Gemma

2017-03-10

We present for the first time the application of metal-organic framework (MOF) mixed-matrix disks (MMD) for the automated flow-through solid-phase extraction (SPE) of environmental pollutants. Zirconium terephthalate UiO-66 and UiO-66-NH 2 MOFs with different size (90, 200 and 300nm) have been incorporated into mechanically stable polyvinylidene difluoride (PVDF) disks. The performance of the MOF-MMDs for automated SPE of seven substituted phenols prior to HPLC analysis has been evaluated using the sequential injection analysis technique. MOF-MMDs enabled the simultaneous extraction of phenols with the concomitant size exclusion of molecules of larger size. The best extraction performance was obtained using a MOF-MMD containing 90nm UiO-66-NH 2 crystals. Using the selected MOF-MMD, detection limits ranging from 0.1 to 0.2μgL -1 were obtained. Relative standard deviations ranged from 3.9 to 5.3% intra-day, and 4.7-5.7% inter-day. Membrane batch-to-batch reproducibility was from 5.2 to 6.4%. Three different groundwater samples were analyzed with the proposed method using MOF-MMDs, obtaining recoveries ranging from 90 to 98% for all tested analytes. Copyright © 2017 Elsevier B.V. All rights reserved.

Acoustics of multiscale sorptive porous materials

NASA Astrophysics Data System (ADS)

Venegas, R.; Boutin, C.; Umnova, O.

2017-08-01

This paper investigates sound propagation in multiscale rigid-frame porous materials that support mass transfer processes, such as sorption and different types of diffusion, in addition to the usual visco-thermo-inertial interactions. The two-scale asymptotic method of homogenization for periodic media is successively used to derive the macroscopic equations describing sound propagation through the material. This allowed us to conclude that the macroscopic mass balance is significantly modified by sorption, inter-scale (micro- to/from nanopore scales) mass diffusion, and inter-scale (pore to/from micro- and nanopore scales) pressure diffusion. This modification is accounted for by the dynamic compressibility of the effective saturating fluid that presents atypical properties that lead to slower speed of sound and higher sound attenuation, particularly at low frequencies. In contrast, it is shown that the physical processes occurring at the micro-nano-scale do not affect the macroscopic fluid flow through the material. The developed theory is exemplified by introducing an analytical model for multiscale sorptive granular materials, which is experimentally validated by comparing its predictions with acoustic measurements on granular activated carbons. Furthermore, we provide empirical evidence supporting an alternative method for measuring sorption and mass diffusion properties of multiscale sorptive materials using sound waves.

Dual Microstructure Heat Treatment of a Nickel-Base Disk Alloy

NASA Technical Reports Server (NTRS)

Gayda, John

2001-01-01

Existing Dual Microstructure Heat Treat (DMHT) technology was successfully applied to Alloy 10, a high strength, nickel-base disk alloy, to produce a disk with a fine grain bore and coarse grain rim. Specimens were extracted from the DMHT disk and tested in tension, creep, fatigue, and crack growth using conditions pertinent to disk applications. These data were then compared with data from "traditional" subsolvus and supersolvus heat treatments for Alloy 10. The results showed the DMHT disk to have a high strength, fatigue resistant bore comparable to that of subsolvus Alloy 10. Further, creep resistance of the DMHT rim was comparable to that of supersolvus Alloy 10. Crack growth resistance in the DMHT rim, while better than that for subsolvus, was inferior to that of supersolvus Alloy 10. The slow cool at the end of the DMHT conversion and/or the subsolvus resolution step are thought to be responsible for degrading rim DMHT crack growth resistance.

Rapid determination of ions by combined solid-phase extraction--diffuse reflectance spectroscopy

NASA Technical Reports Server (NTRS)

Fritz, James S.; Arena, Matteo P.; Steiner, Steven A.; Porter, Marc D.

2003-01-01

We introduce colorimetric solid-phase extraction (C-SPE) for the rapid determination of selected ions. This new technique links the exhaustive concentration of an analyte by SPE onto a membrane disk surface for quantitative measurement with a hand-held diffuse reflectance spectrometer. The concentration/measurement procedure is complete in approximately 1 min and can be performed almost anywhere. This method has been used to monitor iodine and iodide in spacecraft water in the 0.1-5.0 ppm range and silver(I) in the range of 5.0-1000 microg/l. Applications to the trace analysis of copper(II), nickel(II), iron(III) and chromium(VI) are described. Studies on the mechanism of extraction showed that impregnation of the disk with a surfactant as well as a complexing reagent results in uptake of additional water, which markedly improves the extraction efficiency.

Isolation and recovery of selected polybrominated diphenyl ethers from human serum and sheep serum: coupling reversed-phase solid-phase disk extraction and liquid-liquid extraction techniques with a capillary gas chromatographic electron capture negative ion mass spectrometric determinative technique.

PubMed

Loconto, Paul R; Isenga, David; O'Keefe, Michael; Knottnerus, Mark

2008-01-01

Polybrominated diphenyl ethers (PBDEs) are isolated and recovered with acceptable percent recoveries from human serum via liquid-liquid extraction and column chromatographic cleanup and fractionation with quantitation using capillary gas chromatography-mass spectrometry with electron capture negative ion and selected ion monitoring. PBDEs are found in unspiked serum. An alternative sample preparation approach is developed using sheep serum that utilizes a formic acid pre-treatment followed by reversed-phase solid-phase disk extraction and normal-phase solid-phase cleanup using acidified silica gel that yields>50% recoveries. When these percent recoveries are combined with a minimized phase ratio for human serum and very low instrument detection limits, method detection limits below 500 parts-per-trillion are realized.

Colorimetric Solid Phase Extraction for the Measurement of Total I (Iodine, Iodide, and Triiodide) in Spacecraft Drinking Water

NASA Technical Reports Server (NTRS)

Lipert, Robert J.; Porter, Marc D.; Siperko, Lorraine M.; Gazda, Daniel B.; Rutz, Jeff A.; Schultz, John R.; Carrizales, Stephanie M.; McCoy, J. Torin

2009-01-01

An experimental drinking water monitoring kit for the measurement of iodine and silver(I) was recently delivered to the International Space Station (ISS). The kit is based on Colorimetric Solid Phase Extraction (CSPE) technology, which measures the change in diffuse reflectance of indicator disks following exposure to a water sample. To satisfy additional spacecraft water monitoring requirements, CSPE has now been extended to encompass the measurement of total I (iodine, iodide, and triiodide) through the introduction of an oxidizing agent, which converts iodide and triiodide to iodine, for measurement using the same indicator disks currently being tested on ISS. These disks detect iodine, but are insensitive to iodide and triiodide. We report here the operational considerations, design, and ground-based performance of the CSPE method for total I. The results demonstrate that CSPE technology is poised to meet NASA's total I monitoring requirements.

Soil-borne polycyclic aromatic hydrocarbons in El Paso, Texas: Analysis of a potential problem in the United States/Mexico border region

PubMed Central

De La Torre-Roche, Roberto J.; Lee, Wen-Yee; Campos-Díaz, Sandra I.

2009-01-01

Ultrasonic extraction followed by Stir Bar Sorptive Extraction (SBSE) and thermal desorption inline coupled with Gas Chromatography and Mass Spectrometry (TD/GC/MS)was used to perform a comprehensive determination of soil-borne polycyclic aromatic hydrocarbons (PAHs) in El Paso, Texas. The method provided good sensitivity and faster processing time for the analysis. The total PAHs in El Paso soil ranged from 0.1 to 2225.5 µg kg−1. Although the majority of PAH concentrations did not exceed the soil screening levels regulated by the United States Environmental Protection Agency, the existence of PAHs in this ecosystem is ubiquitous. Naphthalene were found in 100% of the soil samples; while the heavy PAHs (five- and six-ring) were not often detected and mostly remained in closer proximity to industrial areas and major traffic points. The results ruled out the possibility of petroleum refining as the significant source of local soil-borne PAH contamination, but they suggested that the PAHs found in El Paso soil were closely linked to human activities and possible other industrial processes. PMID:18768257

Angular Momentum in Disk Wind Revealed in the Young Star MWC 349A

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

Zhang, Qizhou; Claus, Brian; Watson, Linda

Disk winds are thought to play a critical role in star birth. As winds extract excess angular momentum from accretion disks, matter in the disk can be transported inward to the star to fuel mass growth. However, observational evidence of wind carrying angular momentum has been very limited. We present Submillimeter Array (SMA) observations of the young star MWC 349A in the H26 α and H30 α recombination lines. The high signal-to-noise ratios made possible by the maser emission process allow us to constrain the relative astrometry of the maser spots to milli-arcsecond precision. Previous observations of the H30 αmore » line with the SMA and the Plateau de Bure interferometer (PdBI) showed that masers are distributed in the disk and wind. Our new high-resolution observations of the H26 α line reveal differences in spatial distribution from that of the H30 α line. H26 α line masers in the disk are excited in a thin annulus with a radius of about 25 au, while the H30 α line masers are formed in a slightly larger annulus with a radius of 30 au. This is consistent with expectations for maser excitation in the presence of an electron density variation of approximately R {sup −4}. In addition, the H30 α and H26 α line masers arise from different parts in the wind. This difference is also expected from maser theory. The wind component of both masers exhibits line-of-sight velocities that closely follow a Keplerian law. This result provides strong evidence that the disk wind extracts significant angular momentum, thereby facilitating mass accretion in the young star.« less

Elastic and hydrodynamic torques on a colloidal disk within a nematic liquid crystal.

PubMed

Rovner, Joel B; Borgnia, Dan S; Reich, Daniel H; Leheny, Robert L

2012-10-01

The orientationally dependent elastic energy and hydrodynamic behavior of colloidal disks with homeotropic surface anchoring suspended in the nematic liquid crystal 4-cyano-4'-pentylbiphenyl (5CB) have been investigated. In the absence of external torques, the disks align with the normal of the disk face â parallel to the nematic director n[over ^]. When a magnetic field is applied, the disks rotate â by an angle θ so that the magnetic torque and the elastic torque caused by distortion of the nematic director field are balanced. Over a broad range of angles, the elastic torque increases linearly with θ in quantitative agreement with a theoretical prediction based on an electrostatic analogy. When the disks are rotated to angles θ>π/2, the resulting large elastic distortion makes the disk orientation unstable, and the director undergoes a topological transition in which θ→π-θ. In the transition, a defect loop is shed from the disk surface, and the disks spin so that â sweeps through π radians as the loop collapses back onto the disk. Additional measurements of the angular relaxation of disks to θ=0 following removal of the external torque show a quasi-exponential time dependence from which an effective drag viscosity for the nematic can be extracted. The scaling of the angular time dependence with disk radius and observations of disks rotating about â indicate that the disk motion affects the director field at surprisingly modest Ericksen numbers.

Silicone rubber selection for passive sampling of pesticides in water.

PubMed

Martin, A; Margoum, C; Randon, J; Coquery, M

2016-11-01

Silicone rubber can extract organic compounds with a broad range of polarities (logKow>2-3) from aqueous samples. Such compounds include substances of major concern in the protection of aquatic ecosystems and human health, e.g. pesticides. Silicone rubbers (SRs) with various characteristics have been successfully used in sorptive methods for water sample extraction in the laboratory (SPME, SBSE), and for passive sampling in aquatic environments. However, only few studies have evaluated variability in organic compound sorption due to the origin of SRs, particularly for pesticides. The aim of this study was to select an SR for the extraction of pesticides from water samples by passive sampling. To this end we measured the impact of seven SR formulations on sorption capacity, defined by the partition coefficient (Ksw). Kinetic experiments and sorption isotherms were performed to determine extraction recovery as a selection criterion for SRs, and pesticide partition coefficients. Very large differences in affinity for pesticides were found between two kinds of SRs: "Polymerized SR kits" and "Manufactured SRs". One SR was chosen among the "Manufactured SRs", and the Ksw values of 21 pesticides were determined, filling a gap in the literature (1.50

Potential transfer of organic pollutants from littoral plastics debris to the marine environment.

PubMed

León, Víctor M; García, Inés; González, Emilia; Samper, Raquel; Fernández-González, Verónica; Muniategui-Lorenzo, Soledad

2018-05-01

Plastic polymers act as passive samplers in air system and concentrate hydrophobic organic contaminants by sorption or specific interactions, which can be transported to other systems such as the marine environment. In this study plastic debris was sampled in the surrounding area of a Mediterranean lagoon in order to determine the concentration of persistent and emerging organic contaminants. More specifically, desorption of 91 regulated and emerging organic contaminants (polycyclic aromatic hydrocarbons, polychlorinated biphenyls, organochlorinated pesticides, current-use pesticides, personal care products, other pesticides and plastic additives) was characterized for the first 24 h from different polymers to seawater and the remaining content of these contaminants was also extracted by ultrasonic extraction with methanol. All samples were analyzed by Stir Bar Sorptive Extraction coupled to GC/MS. A significant fraction of sorbed contaminants in polymers was desorbed in the first 24 h, particularly for triazines and organophosphorus pesticides due to their lower hydrophobicity than other considered analytes. The remaining contaminants contained in plastics can be also transferred to seawater, sediments or biota. Considering 24 h desorbed fraction plus the remaining methanol extracted fraction, the highest transfer levels corresponded to personal care products, plastic additives, current-use pesticides and PAHs. This is the first study to show the relevance of the transport of organic contaminants on plastic debris from littoral areas to the marine environment. Copyright © 2018 Elsevier Ltd. All rights reserved.

Does Tribolium brevicornis Cuticular Chemistry Deter Cannibalism and Predation of Pupae?

PubMed Central

Alabi, T; Dean, J; Michaud, JP; Verheggen, F; Lognay, G; Haubruge, E

2011-01-01

The cuticular hydrocarbons of insects are species-specific and often function as semiochemicals. The activity of Tribolium brevicornis cuticular hydrocarbons as feeding deterrents that ostensibly function to prevent pupal cannibalism and predation was evaluated. The cuticular hydrocarbons of T. brevicornis pupae were characterized and flour disk bioassays conducted with individual and combined extract components incorporated into artificial diets on which Tribolium adults fed for six days. Feeding by T. brevicornis and T. castaneum on flour disks containing cuticular extracts of T. brevicornis pupae resulted in reduced consumption and weight loss relative to feeding on control flour disks. In both cases, feeding deterrence indices exceeded 80% suggesting that T. brevicornis cuticular hydrocarbons could function to deter cannibalism and predation of pupae by larvae and adult beetles. Sixteen different cuticular hydrocarbons were identified in T. brevicornis pupal extracts. Eight of the commercially available linear alkanes were tested individually in feeding trials with eight Tribolium species. One compound (C28) significantly reduced the amount of food consumed by three species compared to control disks, whereas the compounds C25, C26, and C27 elicited increased feeding in some species. Four other compounds had no effect on consumption for any species. When four hydrocarbon mixtures were tested for synergistic deterrence on T. brevicornis and T. castaneum, none significantly influenced consumption. Our results indicate that the cuticular chemistry of T. brevicornis pupae could serve to deter predation by conspecific and congeneric beetles. PMID:22224957

Towards an automatic lab-on-valve-ion mobility spectrometric system for detection of cocaine abuse.

PubMed

Cocovi-Solberg, David J; Esteve-Turrillas, Francesc A; Armenta, Sergio; de la Guardia, Miguel; Miró, Manuel

2017-08-25

A lab-on-valve miniaturized system integrating on-line disposable micro-solid phase extraction has been interfaced with ion mobility spectrometry for the accurate and sensitive determination of cocaine and ecgonine methyl ester in oral fluids. The method is based on the automatic loading of 500μL of oral fluid along with the retention of target analytes and matrix clean-up by mixed-mode cationic/reversed-phase solid phase beads, followed by elution with 100μL of 2-propanol containing (3% v/v) ammonia, which are online injected into the IMS. The sorptive particles are automatically discarded after every individual assay inasmuch as the sorptive capacity of the sorbent material is proven to be dramatically deteriorated with reuse. The method provided a limit of detection of 0.3 and 0.14μgL -1 for cocaine and ecgonine methyl ester, respectively, with relative standard deviation values from 8 till 14% with a total analysis time per sample of 7.5min. Method trueness was evaluated by analyzing oral fluid samples spiked with cocaine at different concentration levels (1, 5 and 25μgL -1 ) affording relative recoveries within the range of 85±24%. Fifteen saliva samples were collected from volunteers and analysed following the proposed automatic procedure, showing a 40% cocaine occurrence with concentrations ranging from 1.3 to 97μgL -1 . Field saliva samples were also analysed by reference methods based on lateral flow immunoassay and gas chromatography-mass spectrometry. The application of this procedure to the control of oral fluids of cocaine consumers represents a step forward towards the development of a point-of-care cocaine abuse sensing system. Copyright © 2017 Elsevier B.V. All rights reserved.

Investigation of metal ions sorption of brown peat moss powder

NASA Astrophysics Data System (ADS)

Kelus, Nadezhda; Blokhina, Elena; Novikov, Dmitry; Novikova, Yaroslavna; Chuchalin, Vladimir

2017-11-01

For regularities research of sorptive extraction of heavy metal ions by cellulose and its derivates from aquatic solution of electrolytes it is necessary to find possible mechanism of sorption process and to choice a model describing this process. The present article investigates the regularities of aliovalent metals sorption on brown peat moss powder. The results show that sorption isotherm of Al3+ ions is described by Freundlich isotherm and sorption isotherms of Na+ i Ni2+ are described by Langmuir isotherm. To identify the mechanisms of brown peat moss powder sorption the IR-spectra of the initial brown peat moss powder samples and brown peat moss powder samples after Ni (II) sorption were studied. Metal ion binding mechanisms by brown peat moss powder points to ion exchange, physical adsorption, and complex formation with hydroxyl and carboxyl groups.

Effect of aqueous and ethanolic extracts of Lippia citriodora on candida albicans

PubMed Central

Ghasempour, Maryam; Omran, Saeid Mahdavi; Moghadamnia, Ali Akbar; Shafiee, Faranak

2016-01-01

Introduction Because of resistance and side effects to common antifungal drugs activity, the research on herbal substances with antifungal activity is frequent. Lemon verbena (Lippia citriodora) is a member of Verbenaceae family. The aim of this study was to determine the anti-candida activities of the ethanolic and aqueous extracts of the lemon verbena leaves and compare them with nystatin and fluconazole. Methods In this 2015 study, 15 clinical isolates and standard strain of candida albicans PTCC 5027 were used, and the inhibitory effects of the ethanolic and aqueous extracts, Nystatin and Fluconazole, were evaluated using disk and well diffusion methods. Also, the minimal inhibitory concentration (MIC) was determined. Five concentrations of aqueous and ethanolic extracts (156–2500 μg/ml), Nystatin (8–128 μg/ml) and Fluconazole (4–64 μg/ml) were used in disk and well diffusion methods, and nine concentrations of aqueous and ethanolic extracts (19–5000 μg/ml), Nystatin (0.5–128 μg/ml), and Fluconazole (0.25–64 μg/ml) were applied for MIC. Data were analyzed using Tukey’s post-hoc and one-way ANOVA tests. The significant level was considered p < 0.05 in the current study. Results In the well and disk diffusion techniques, limited growth inhibition halos were produced around some clinical isolates at different concentrations of ethanolic extract; however, no growth inhibitory halo was observed with any concentrations of the aqueous extract. The MIC values of ethanolic extract, aqueous extract, Nystatin and Fluconazole for clinical isolated and standard strain were 833 ± 78.5and 625μg/ml; 4156 ± 67.4 and 2500 μg/ml; 10.13 ± 1.91 and 4 μg/ml; and 1.97 ± 0.25 and 1 μg/ml, respectively. Conclusion The results showed that the ethanolic extract was stronger than the aqueous extract of this plant, which can be used as an alternative for drugs. It is recommended that the ethanolic extract of this plant be investigated in vivo for better evaluation of its efficacy and properties. PMID:27757185

Anti-pseudomonas activity of essential oil, total extract, and proanthocyanidins of Pinus eldarica Medw. bark.

PubMed

Sadeghi, Masoud; Zolfaghari, Behzad; Jahanian-Najafabadi, Ali; Abtahi, Seyed Reza

2016-01-01

Pinus eldarica Medw. (Iranian pine) is native to Transcaucasian region and has been vastly planted in Iran, Afghanistan, and Pakistan. Various parts of this plant have been widely used in traditional medicine for the treatment of various diseases including infectious conditions (e.g. infectious wounds). In this study we aimed to investigate the antibacterial activity of P. eldarica bark extract, essential oil and proanthocyanidins on three important bacteria, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa. Antibacterial analysis was performed using standard disk diffusion method with different concentrations of essential oil, bark total hydroalcoholic extract, and bark proanthocyanidins (0.5, 1, 2 and 3 mg/ml). After incubation at 37°C for 24 h, the antibacterial activity was assessed by measuring the zone of growth inhibition surrounding the disks. The results indicated that the essential oil, total hydroalcoholic extract, and proanthocyanidins of the bark of the P. eldarica were effective against the gram negative bacteria, P. aeruginosa, and significantly inhibited its growth in disk diffusion method (P<0.001) of which the essential oil had the most potent inhibitory effect. However, none of the bark preparations could significantly inhibit the growth of S. aureus or E. coli. Our findings showed that P. eldarica bark components have significant anti-pseudomonas activity having potentials for new sources of antibacterial agents or antibacterial herbal preparations.

Polyvinylidene Fluoride Micropore Membranes as Solid-Phase Extraction Disk for Preconcentration of Nanoparticulate Silver in Environmental Waters.

PubMed

Zhou, Xiao-Xia; Lai, Yu-Jian; Liu, Rui; Li, Sha-Sha; Xu, Jing-Wen; Liu, Jing-Fu

2017-12-05

Efficient separation and preconcentration of trace nanoparticulate silver (NAg) from large-volume environmental waters is a prerequisite for reliable analysis and therefore understanding the environmental processes of silver nanoparticles (AgNPs). Herein, we report the novel use of polyvinylidene fluoride (PVDF) filter membrane for disk-based solid phase extraction (SPE) of NAg in 1 L of water samples with the disk-based SPE system, which consists of a syringe pump and a syringe filter holder to embed the filter membrane. While the PVDF membrane can selectively adsorb NAg in the presence of Ag + , aqueous solution of 2% (m/v) FL-70 is found to efficiently elute NAg. Analysis of NAg is performed following optimization of filter membrane and elution conditions with an enrichment factor of 1000. Additionally, transmission electron microscopy (TEM), UV-vis spectroscopy, and size-exclusion chromatography coupled with ICP-MS (SEC-ICP-MS) analysis showed that the extraction gives rise to no change in NAg size or shape, making this method attractive for practical applications. Furthermore, feasibility of the protocol is verified by applying it to extract NAg in four real waters with recoveries of 62.2-80.2% at 0.056-0.58 μg/L spiked levels. This work will facilitate robust studies of trace NAg transformation and their hazard assessments in the environment.

Comprehensive analytical methodology to determine hydrocarbons in marine waters using extraction disks coupled to glass fiber filters and compound-specific isotope analyses.

PubMed

Ternon, Eva; Tolosa, Imma

2015-07-24

Solid-phase extraction of both aliphatic (AHs) and aromatic polycyclic hydrocarbons (PAHs) from seawater samples was evaluated using a GFF filter stacked upon an octadecyl bonded silica (C18) disk. Stable-isotope measurements were developed on hydrocarbons extracted from both GFF and C18-disks in order to characterize the source of hydrocarbons. A clear partition of hydrocarbon compounds between the dissolved and the particulate phase was highlighted. PAHs showed a higher affinity with the dissolved phase (recoveries efficiency of 48-71%) whereas AHs presented strong affinity with the particulate phase (up to 76% of extraction efficiency). Medium volumes of seawater samples were tested and no breakthrough was observed for a 5L sample. Isotopic fractionation was investigated within all analytical steps but none was evidenced. This method has been applied to harbor seawater samples and very low AH and PAH concentrations were achieved. Due to the low concentration levels of hydrocarbons in the samples, the source of hydrocarbons was determined by molecular indices rather than isotopic measurements and a pyrolytic origin was evidenced. The aliphatic profile also revealed the presence of long-chain linear alkylbenzenes (LABs). The methodology presented here would better fit to polluted coastal environments affected by recent oil spills. Copyright © 2015 Elsevier B.V. All rights reserved.

Anti-pseudomonas activity of essential oil, total extract, and proanthocyanidins of Pinus eldarica Medw. bark

PubMed Central

Sadeghi, Masoud; Zolfaghari, Behzad; Jahanian-Najafabadi, Ali; Abtahi, Seyed Reza

2016-01-01

Pinus eldarica Medw. (Iranian pine) is native to Transcaucasian region and has been vastly planted in Iran, Afghanistan, and Pakistan. Various parts of this plant have been widely used in traditional medicine for the treatment of various diseases including infectious conditions (e.g. infectious wounds). In this study we aimed to investigate the antibacterial activity of P. eldarica bark extract, essential oil and proanthocyanidins on three important bacteria, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa. Antibacterial analysis was performed using standard disk diffusion method with different concentrations of essential oil, bark total hydroalcoholic extract, and bark proanthocyanidins (0.5, 1, 2 and 3 mg/ml). After incubation at 37°C for 24 h, the antibacterial activity was assessed by measuring the zone of growth inhibition surrounding the disks. The results indicated that the essential oil, total hydroalcoholic extract, and proanthocyanidins of the bark of the P. eldarica were effective against the gram negative bacteria, P. aeruginosa, and significantly inhibited its growth in disk diffusion method (P<0.001) of which the essential oil had the most potent inhibitory effect. However, none of the bark preparations could significantly inhibit the growth of S. aureus or E. coli. Our findings showed that P. eldarica bark components have significant anti-pseudomonas activity having potentials for new sources of antibacterial agents or antibacterial herbal preparations. PMID:27051433

Stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet/inductively coupled plasma mass spectrometry for analysis of thyroxine in urine samples.

PubMed

Fan, Wenying; Mao, Xiangju; He, Man; Chen, Beibei; Hu, Bin

2013-11-29

tIn this work, polyethyleneglycol (PEG)/hydroxyl polydimethylsiloxane (OH-PDMS)/γ -mercaptopropyltrimethoxysilane (γ -MPTS) coated stir bar was prepared by sol–gel process and its extraction performance for the extraction of amphoteric thyroxines (3,3',5,5'-tetraiodothyronin, T(4); 3,3',5-triiodothyronine, T(3); reversed-3,3',5-triiodothyronine, rT(3)) and their metabolite (3,5-diiodothyronine,T2) was studied. The preparation reproducibility of PEG/OH-PDMS/γ -MPTS coated stir bar was investigated, and the relative standard deviations (RSDs) in the same batch and among different batches were 3.3–14.3% (n = 5) and 7.7–16.6% (n = 3), respectively. The prepared PEG/OH-PDMS/γ -MPTS coated stir bar could be reused for more than 20 times. Based on this fact, a novel method of stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV)and HPLC-inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of target thyroxinesin human urine samples was developed. The influencing factors of SBSE, such as sample pH, extraction time, stirring rate, salt effect, desorption solution and desorption time, were studied in detail, and the analytical performance of the proposed method was evaluated under the optimized conditions. The enrichment factors (EFs) of the developed method for four target thyroxines were in the range of 14.9–70.4(theoretical enrichment factor was 100). The RSDs were ranging from 4.0% to 13.8% for SBSE-HPLC-UV (c = 25 μg/L, n = 6) and from 3.7% to 6.1% for SBSE-HPLC-ICP-MS (c = 0.5 μg/L, n = 5). The linear range obtained by SBSE-HPLC-UV was 2–500 μg/L for T(2)and 5–500 μg/L for rT3, T(3)and T(4), with correlation coefficients (r) ranging from 0.9957 to 0.9998, respectively, while the linear range obtained by SBSE-HPLC-ICP-MS was 0.05–500 μg/L for T(2) and rT(3), 0.10–200 μg/L for T(3) and 0.05–200 μg/L for T(4)with r ranging from 0.9979 to 0.9998, respectively. The limits of detection (LODs) for the target thyroxines were 0.60–2.20 μg/L for SBSE-HPLC-UV and 0.0071–0.0355 μg/L SBSE-HPLC-ICP-MS, respectively. The developed method was applied for the determination of target thyroxines in urine samples, and the recovery for the spiking samples obtained by SBSE-HPLC-UV was in the range of 81.6–137.6% for human urine,while the recovery for the spiking urine samples obtained by SBSE-HPLC-ICP-MS were in the range of 72.0–121.5%.

The sorptive and reductive capacities of biochar supported nanoscaled zero-valent iron (nZVI) in relation to its crystallite size.

PubMed

Wang, Shengsen; Zhou, Yanxia; Gao, Bin; Wang, Xiaozhi; Yin, Xianqiang; Feng, Ke; Wang, Jun

2017-11-01

In this work, nZVI was immobilized by bamboo derived biochars (nZVI/BB), hydrogen peroxide (H 2 O 2 ) (nZVI/PBB) and nitric acid (HNO 3 ) (nZVI/HBB) modified BB. H 2 O 2 and HNO 3 deceased surface area and pore volume of pristine biochars. Total iron (Fe) contents were 16.50, 24.40, and 13.08% for nZVI/BB, nZVI/PBB and nZVI/HBB, respectively. The X-ray diffraction revealed that nZVI in biochar matrix was dominantly metallic Fe coated with Fe oxides. The transmission electron microscopy indicated nZVI particle sizes were 41.5, 30.5 and 6.1 nm for nZVI/BB, nZVI/HBB and nZVI/PBB, respectively. The removal capacities of arsenate (AsV) and silver ions (Ag + ) by nZVI nanocomposites were compared in a batch experiment. Greater reductive removal of Ag + (1217 g kg -1 nZVI) and sorptive removal of AsV (109.1 g kg -1 nZVI) were achieved in nZVI/PBB, indicating smaller-sized nZVI was more reactive. Thus, particle size of nZVI affected the sorptive and reductive capacities for AsV and Ag + . Copyright © 2017 Elsevier Ltd. All rights reserved.

Field Performance of Dieldrin/Resin Wettable Powders on Sorptive Mud Surface

PubMed Central

Van Tiel, N.

1961-01-01

Recent field experiments on the relative performance of dieldrin and dieldrin/resin wettable powders on sorptive mud surface have not confirmed the promising results obtained with the latter products in earlier laboratory tests. In view of this a renewed investigation into the possible factors governing the performance of such products was considered desirable, and further laboratory and field experiments were carried out in co-operation with the Colonial Pesticides Research Unit at Arusha, Tanganyika. The results of these experiments have given a better understanding of the factors involved, and a coherent interpretation of the differences in performance shown by various products under different conditions. The main factors to be taken into account appear to be: mobility of the insects during exposure, as influenced by insect species and exposure conditions; inherent toxicity of the dieldrin/resin particles; and the average relative humidity inside the experimental huts. The sorption phenomenon can be demonstrated in the field, but in view of the humidity conditions it does not seem likely that it will interfere seriously with practical mosquito control. A potential critical condition might be prevalent only in areas where the presence of sorptive mud is coupled with long periods of low humidity inside the huts, but further experimental data are necessary to confirm this. PMID:13780061

Sorptive Uptake Studies of an Aryl-Arsenical with Iron Oxide Composites on an Activated Carbon Support

PubMed Central

Kwon, Jae H.; Wilson, Lee D.; Sammynaiken, Ramaswami

2014-01-01

Sorption uptake kinetics and equilibrium studies for 4-hydroxy-3-nitrobenzene arsonic acid (roxarsone) was evaluated with synthetic magnetite (Mag-P), commercial magnetite (Mag-C), magnetite 10%, 19%, and 32% composite material (CM-10, -19, -32) that contains granular activated carbon (GAC), and synthetic goethite at pH 7.00 in water at 21 °C for 24 h. GAC showed the highest sorptive removal of roxarsone and the relative uptake for each sorbent material with roxarsone are listed in descending order as follows: GAC (471 mg/g) > goethite (418 mg/g) > CM-10 (377 mg/g) CM-19 (254 mg/g) > CM-32 (227 mg/g) > Mag-P (132 mg/g) > Mag-C (29.5 mg/g). The As (V) moiety of roxarsone is adsorbed onto the surface of the iron oxide/oxyhydrate and is inferred as inner-sphere surface complexes; monodentate-mononuclear, bidentate-mononuclear, and bidentate-binuclear depending on the protolytic speciation of roxarsone. The phenyl ring of roxarsone provides the primary driving force for the sorptive interaction with the graphene surface of GAC and its composites. Thus, magnetite composites are proposed as multi-purpose adsorbents for the co-removal of inorganic and organic arsenicals due to the presence of graphenic and iron oxide active adsorption sites. PMID:28788545

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

Rajauria, Sukumar, E-mail: sukumar.rajauria@hgst.com; Canchi, Sripathi V., E-mail: sripathi.canchi@hgst.com; Schreck, Erhard

The kinetic friction and wear at high sliding speeds is investigated using the head-disk interface of hard disk drives, wherein the head and the disk are less than 10 nm apart and move at sliding speeds of 5–10 m/s relative to each other. While the spacing between the sliding surfaces is of the same order of magnitude as various AFM based fundamental studies on friction, the sliding speed is nearly six orders of magnitude larger, allowing a unique set-up for a systematic study of nanoscale wear at high sliding speeds. In a hard disk drive, the physical contact between the head andmore » the disk leads to friction, wear, and degradation of the head overcoat material (typically diamond like carbon). In this work, strain gauge based friction measurements are performed; the friction coefficient as well as the adhering shear strength at the head-disk interface is extracted; and an experimental set-up for studying friction between high speed sliding surfaces is exemplified.« less

Nanoscale wear and kinetic friction between atomically smooth surfaces sliding at high speeds

NASA Astrophysics Data System (ADS)

Rajauria, Sukumar; Canchi, Sripathi V.; Schreck, Erhard; Marchon, Bruno

2015-02-01

The kinetic friction and wear at high sliding speeds is investigated using the head-disk interface of hard disk drives, wherein the head and the disk are less than 10 nm apart and move at sliding speeds of 5-10 m/s relative to each other. While the spacing between the sliding surfaces is of the same order of magnitude as various AFM based fundamental studies on friction, the sliding speed is nearly six orders of magnitude larger, allowing a unique set-up for a systematic study of nanoscale wear at high sliding speeds. In a hard disk drive, the physical contact between the head and the disk leads to friction, wear, and degradation of the head overcoat material (typically diamond like carbon). In this work, strain gauge based friction measurements are performed; the friction coefficient as well as the adhering shear strength at the head-disk interface is extracted; and an experimental set-up for studying friction between high speed sliding surfaces is exemplified.

Graphene-based solid-phase extraction disk for fast separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Wang, Zonghua; Han, Qiang; Xia, Jianfei; Xia, Linhua; Ding, Mingyu; Tang, Jie

2013-06-01

Graphene has great potentials for the use in sample preparation due to its ultra high specific surface area, superior chemical stability, and excellent thermal stability. In our work, a novel graphene-based SPE disk was developed for separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples. Based on the strong π-π stacking interaction between the analytes and graphene, the analytes extracted by graphene were eluted by cyclohexane and then determined by GC-MS. Under the optimized conditions, high flow rate (30 mL/min) and sensitivity (0.84-13 ng/L) were achieved. The proposed method was successfully applied to the analysis of real environmental water samples with recoveries ranging from 72.8 to 106.2%. Furthermore, the property of anticlogging and reusability was also improved. This work reveals great potentials of graphene-based SPE disk in environmental analytical. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Speciation of inorganic arsenic in drinking water by wavelength-dispersive X-ray fluorescence spectrometry after in situ preconcentration with miniature solid-phase extraction disks.

PubMed

Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Aizawa, Mamoru; Nakamura, Toshihiro

2015-03-01

A rapid and simple method using wavelength-dispersive X-ray fluorescence (WDXRF) spectrometry after in situ solid-phase extraction (SPE) was developed for the speciation and evaluation of the concentration of inorganic arsenic (As) in drinking water. The method involves the simultaneous collection of As(III) and As(V) using 13 mm ϕ SPE miniature disks. The removal of Pb(2+) from the sample water was first conducted to avoid the overlapping PbLα and AsKα spectra on the XRF spectrum. To this end, a 50 mL aqueous sample (pH 5-9) was passed through an iminodiacetate chelating disk. The filtrate was adjusted to pH 2-3 with HCl, and then ammonium pyrrolidine dithiocarbamate solution was added. The solution was passed through a hydrophilic polytetrafluoroethylene filter placed on a Zr and Ca loaded cation-exchange disk at a flow rate of 12.5 mL min(-1) to separate As(III)-pyrrolidine dithiocarbamate complex and As(V). Each SPE disk was affixed to an acrylic plate using adhesive cellophane tape, and then examined by WDXRF spectrometry. The detection limits of As(III) and As(V) were 0.8 and 0.6 μg L(-1), respectively. The proposed method was successfully applied to screening for As speciation and concentration evaluation in spring water and well water. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Espaillat, C.; D'Alessio, P.; Hernandez, J.

In the past few years, several disks with inner holes that are relatively empty of small dust grains have been detected and are known as transitional disks. Recently, Spitzer has identified a new class of 'pre-transitional disks' with gaps based on near-infrared photometry and mid-infrared spectra; these objects have an optically thick inner disk separated from an optically thick outer disk by an optically thin disk gap. A near-infrared spectrum provided the first confirmation of a gap in the pre-transitional disk of LkCa 15 by verifying that the near-infrared excess emission in this object was due to an optically thickmore » inner disk. Here, we investigate the difference between the nature of the inner regions of transitional and pre-transitional disks using the same veiling-based technique to extract the near-infrared excess emission above the stellar photosphere. However, in this work we use detailed disk models to fit the excess continua as opposed to the simple blackbody fits previously used. We show that the near-infrared excess emission of the previously identified pre-transitional disks of LkCa 15 and UX Tau A in the Taurus cloud as well as the newly identified pre-transitional disk of ROX 44 in Ophiuchus can be fit with an inner disk wall located at the dust destruction radius. We also present detailed modeling of the broadband spectral energy distributions of these objects, taking into account the effect of shadowing by the inner disk on the outer disk, but considering the finite size of the star, unlike other recent treatments. The near-infrared excess continua of these three pre-transitional disks, which can be explained by optically thick inner disks, are significantly different from that of the transitional disks of GM Aur, whose near-infrared excess continuum can be reproduced by emission from sub-micron-sized optically thin dust, and DM Tau, whose near-infrared spectrum is consistent with a disk hole that is relatively free of small dust. The structure of pre-transitional disks may be a sign of young planets forming in these disks and future studies of pre-transitional disks will provide constraints to aid in theoretical modeling of planet formation.« less

Polar stir bars for isolation and preconcentration of perfluoroalkyl substances from human milk samples prior to UHPLC-MS/MS analysis.

PubMed

Martín, Julia; Rodríguez-Gómez, Rocío; Zafra-Gómez, Alberto; Alonso, Esteban; Vílchez, José L; Navalón, Alberto

2016-04-01

A new method for the determination of four perfluoroalkyl carboxylic acids (from C5 to C8) and perfluorooctane sulfonate in human milk samples using stir-bar sorptive extraction-ultra-HPLC-MS/MS has been accurately optimized and validated. Polydimethylsiloxane and polyethyleneglycol modified silicone materials were evaluated. Overall, polyethyleneglycol led to a better sensitivity. After optimizing experimental variables, the method was validated reaching detection limits in the range of 0.05-0.20 ng ml(-1); recovery rates from 81 to 105% and relative standard deviations fewer than 13% in all cases. The method was applied to milk samples from five randomly selected women. All samples were positive for at least one of the target compounds with concentrations ranging between 0.8 and 6.6 ng ml(-1), being the most abundant perfluorooctane sulfonate.

A Comparative biochemical study on two marine endophytes, Bacterium SRCnm and Bacillus sp. JS, Isolated from red sea algae.

PubMed

Ahmed, Eman Fadl; Hassan, Hossam Mokhtar; Rateb, Mostafa Ezzat; Abdel-Wahab, Noha; Sameer, Somayah; Aly Taie, Hanan Anwar; Abdel-Hameed, Mohammed Sayed; Hammouda, Ola

2016-01-01

Two marine endophytic bacteria were isolated from the Red Sea algae; a red alga; Acanthophora dendroides and the brown alga Sargassum sabrepandum. The isolates were identified based on their 16SrRNA sequences as Bacterium SRCnm and Bacillus sp. JS. The objective of this study was to investigate the potential anti-microbial and antioxidant activities of the extracts of the isolated bacteria grown in different nutrient conditions. Compared to amoxicillin (25μg/disk) and erythromycin (15μg/disk), the extracts of Bacterium SRCn min media II, III, IV and V were potent inhibitors of the gram-positive bacterium Sarcina maxima even at low concentrations. Also, the multidrug resistant Staphylococcus aureus(MRSA) was more sensitive to the metabolites produced in medium (II) of the same endophyte than erythromycin (15μg/disk). A moderate activity of the Bacillus sp. JS extracts of media I and II was obtained against the same pathogen. The total compounds (500ug/ml) of both isolated endophytes showed moderate antioxidant activities (48.9% and 46.1%, respectively). LC/MS analysis of the bacterial extracts was carried out to investigate the likely natural products produced. Cyclo(D-cis-Hyp-L-Leu), dihydrosphingosine and 2-Amino-1,3-hexadecanediol were identified in the fermentation medium of Bacterium SRCnm, whereas cyclo (D-Pro-L-Tyr) and cyclo (L-Leu-L-Pro) were the suggested compounds of Bacillus sp. JS.

Retention and chemical speciation of uranium in an oxidized wetland sediment from the Savannah River Site.

PubMed

Li, Dien; Seaman, John C; Chang, Hyun-Shik; Jaffe, Peter R; Koster van Groos, Paul; Jiang, De-Tong; Chen, Ning; Lin, Jinru; Arthur, Zachary; Pan, Yuanming; Scheckel, Kirk G; Newville, Matthew; Lanzirotti, Antonio; Kaplan, Daniel I

2014-05-01

Uranium speciation and retention mechanisms onto Savannah River Site (SRS) wetland sediments was studied using batch (ad)sorption experiments, sequential extraction, U L3-edge X-ray absorption near-edge structure (XANES) spectroscopy, fluorescence mapping and μ-XANES. Under oxidized conditions, U was highly retained by the SRS wetland sediments. In contrast to other similar but much lower natural organic matter (NOM) sediments, significant sorption of U onto the SRS sediments was observed at pH < 4 and pH > 8. Sequential extraction indicated that the U species were primarily associated with the acid soluble fraction (weak acetic acid extractable) and organic fraction (Na-pyrophosphate extractable). Uranium L3-edge XANES spectra of the U-bound sediments were nearly identical to that of uranyl acetate. Based on fluorescence mapping, U and Fe distributions in the sediment were poorly correlated, U was distributed throughout the sample and did not appear as isolated U mineral phases. The primary oxidation state of U in these oxidized sediments was U(VI), and there was little evidence that the high sorptive capacity of the sediments could be ascribed to abiotic or biotic reduction to the less soluble U(IV) species or to secondary mineral formation. Collectively, this study suggests that U may be strongly bound to wetland sediments, not only under reducing conditions by reductive precipitation, but also under oxidizing conditions through NOM-uranium bonding. Published by Elsevier Ltd.

Evaluation of polyethersulfone performance for the microextraction of polar chlorinated herbicides from environmental water samples.

PubMed

Prieto, Ailette; Rodil, Rosario; Quintana, José Benito; Cela, Rafael; Möder, Monika; Rodríguez, Isaac

2014-05-01

In this work, the suitability of bulk polyethersulfone (PES) for sorptive microextraction of eight polar, chlorinated phenoxy acids and dicamba from environmental water samples is assessed and the analytical features of the optimized method are compared to those reported for other microextraction techniques. Under optimized conditions, extractions were performed with samples (18 mL) adjusted at pH 2 and containing a 30% (w/v) of sodium chloride, using a tubular PES sorbent (1 cm length × 0.7 mm o.d., sorbent volume 8 µL). Equilibrium conditions were achieved after 3h of direct sampling, with absolute extraction efficiencies ranging from 39 to 66%, depending on the compound. Analytes were recovered soaking the polymer with 0.1 mL of ethyl acetate, derivatized and determined by gas chromatography-mass spectrometry (GC-MS). Achieved quantification limits (LOQs) varied between 0.005 and 0.073 ng mL(-1). After normalization with the internal surrogate (IS), the efficiency of the extraction was only moderately affected by the particular characteristics of different water samples (surface and sewage water); thus, pseudo-external calibration, using spiked ultrapure water solutions, can be used as quantification technique. The reduced cost of the PES polymer allowed considering it as a disposable sorbent, avoiding variations in the performance of the extraction due to cross-contamination problems and/or surface modification with usage. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of a metal-dielectric structure introduced in the plasma chamber of the Frankfurt 14 GHz electron cyclotron resonance ion source

NASA Astrophysics Data System (ADS)

Schächter, L.; Stiebing, K. E.; Dobrescu, S.; Badescu-Singureanu, Al. I.; Schmidt, L.; Hohn, O.; Runkel, S.

1999-02-01

A new approach of the possibility to significantly increase the high charge state ion beams delivered by electron cyclotron resonance (ECR) ion sources by using metal-dielectric (MD) structures characterized by high secondary electron emission properties is presented. The intensities of argon ion beams extracted from the 14 GHz electron cyclotron resonance ion source of the Institut für Kernphysik (IKF) der Johann Wolfgang Goethe-Universität in Frankfurt/Main were measured when a 26 mm diam disk of a specially treated MD structure (Al-Al2O3) was introduced axially close to the ECR plasma. The Ar beam intensities and charge-state distributions obtained with this disk are compared to measurements with disks of iron and pure aluminum at the same position relative to the plasma. All measurements were performed with the disk at the plasma chamber potential. The results with the MD structure show a net shift of the beam intensity towards higher charge states as compared with the other disk materials. Enhancement factors of the beam current of up to 10 (for Ar12+) when using a MD disk compared to the output when using an aluminum disk and up to 40 (for Ar11+) when using an iron disk were measured.

A New Paradigm for Gamma Ray Bursts: Long Term Accretion Rate Modulation by an External Accretion Disk

NASA Technical Reports Server (NTRS)

Cannizzo, John; Gehrels, Neil

2009-01-01

We present a new way of looking at the very long term evolution of GRBs in which the disk of material surrounding the putative black hole powering the GRB jet modulates the mass flow, and hence the efficacy of the process that extracts rotational energy from the black hole and inner accretion disk. The pre-Swift paradigm of achromatic, shallow-to-steep "breaks" in the long term GRB light curves has not been borne out by detailed Swift data amassed in the past several years. We argue that, given the initial existence of a fall-back disk near the progenitor, an unavoidable consequence will be the formation of an "external disk" whose outer edge continually moves to larger radii due to angular momentum transport and lack of a confining torque. The mass reservoir at large radii moves outward with time and gives a natural power law decay to the GRB light curves. In this model, the different canonical power law decay segments in the GRB identified by Zhang et al. and Nousek et al. represent different physical states of the accretion disk. We identify a physical disk state with each power law segment.

Molecularly imprinted polymers based stir bar sorptive extraction for determination of cefaclor and cefalexin in environmental water.

PubMed

Peng, Jun; Liu, Donghao; Shi, Tian; Tian, Huairu; Hui, Xuanhong; He, Hua

2017-07-01

Although stir bar sportive extraction was thought to be a highly efficiency and simple pretreatment approach, its wide application was limited by low selectivity, short service life, and relatively high cost. In order to improve the performance of the stir bar, molecular imprinted polymers and magnetic carbon nanotubes were combined in the present study. In addition, two monomers were utilized to intensify the selectivity of molecularly imprinted polymers. Fourier transform infrared spectroscopy, scanning electron microscopy, and selectivity experiments showed that the molecularly imprinted polymeric stir bar was successfully prepared. Then micro-extraction based on the obtained stir bar was coupled with HPLC for determination of trace cefaclor and cefalexin in environmental water. This approach had the advantages of stir bar sportive extraction, high selectivity of molecular imprinted polymers, and high sorption efficiency of carbon nanotubes. To utilize this pretreatment approach, pH, extraction time, stirring speed, elution solvent, and elution time were optimized. The LOD and LOQ of cefaclor were found to be 3.5 ng · mL -1 and 12.0 ng · mL -1 , respectively; the LOD and LOQ of cefalexin were found to be 3.0 ng · mL -1 and 10.0 ng · mL -1 , respectively. The recoveries of cefaclor and cefalexin were 86.5 ~ 98.6%. The within-run precision and between-run precision were acceptable (relative standard deviation <7%). Even when utilized in more than 14 cycles, the performance of the stir bar did not decrease dramatically. This demonstrated that the molecularly imprinted polymeric stir bar based micro-extraction was a convenient, efficient, low-cost, and a specific method for enrichment of cefaclor and cefalexin in environmental samples.

Genetic analysis of geraniol metabolism during fermentation.

PubMed

Steyer, Damien; Erny, Claude; Claudel, Patricia; Riveill, Geneviève; Karst, Francis; Legras, Jean-Luc

2013-04-01

Geraniol produced by grape is the main precursor of terpenols which play a key role in the floral aroma of white wines. We investigated the fate of geraniol during wine fermentation by Saccharomyces cerevisiae. The volatile compounds produced during fermentation of a medium enriched with geraniol were extracted by Stir-bar sorptive extraction and analysed by GC-MS. We were able to detect and quantify geranyl acetate but also citronellyl- and neryl-acetate. The presence of these compounds partly explains the disparition of geraniol. The amounts of terpenyl esters are strain dependant. We demonstrated both by gene overexpression and gene-deletion the involvement of ATF1 enzyme but not ATF2 in the acetylation of terpenols. The affinity of ATF1 enzyme for several terpenols and for isoamyl alcohol was compared. We also demonstrated that OYE2 is the enzyme involved in geraniol to citronellol reduction. Fermenting strain deleted from OYE2 gene produces far less citronellol than wild type strain. Moreover lab strain over-expressing OYE2 allows 87% geraniol to citronellol reduction in bioconversion experiment compared to about 50% conversion with control strain. Copyright © 2012 Elsevier Ltd. All rights reserved.

Application of minidisk infiltrometer to estimate soil water repellency

NASA Astrophysics Data System (ADS)

Alagna, Vincenzo; Iovino, Massimo; Bagarello, Vincenzo; Mataix-Solera, Jorge; Lichner, Ľubomír

2016-04-01

Soil water repellency (SWR) reduces affinity of soils to water resulting in detrimental implication for plants growth as well as for hydrological processes. During the last decades, it has become clear that SWR is much more widespread than formerly thought, having been reported for a wide variety of soils, land uses and climatic conditions. The repellency index (RI), based on soil-water to soil-ethanol sorptivity ratio, was proposed to characterize subcritical SWR that is the situation where a low degree of repellency impedes infiltration but does not prevent it. The minidisk infiltrometer allows adequate field assessment of RI inherently scaled to account for soil physical properties other than hydrophobicity (e.g., the volume, connectivity and the geometry of pores) that directly influence the hydrological processes. There are however some issues that still need consideration. For example, use of a fixed time for both water and ethanol sorptivity estimation may lead to inaccurate RI values given that water infiltration could be negligible whereas ethanol sorptivity could be overestimated due to influence of gravity and lateral diffusion that rapidly come into play when the infiltration process is very fast. Moreover, water and ethanol sorptivity values need to be determined at different infiltration sites thus implying that a large number of replicated runs should be carried out to obtain a reliable estimate of RI for a given area. Minidisk infiltrometer tests, conducted under different initial soil moisture and management conditions in the experimental sites of Ciavolo, Trapani (Italy) and Javea, Alicante (East Spain), were used to investigate the best applicative procedure to estimate RI. In particular, different techniques to estimate the water, Sw, and ethanol, Se, sorptivities were compared including i) a fixed 1-min time interval, ii) the slope of early-time 1D infiltration equation and iii) the two-term transient 3D infiltration equation that explicitly accounts for the effects of gravity and lateral expansion. According to Pekárová et al. (2015), the combination of all the ethanol and water sorptivities was used to calculate an aggregated repellency index, RIa, that accounts for the influence of spatial variability. Alternatively, the plot of the water cumulative infiltration vs. square root of time, exhibiting a clear "hockey-stick-like" shape, was used to estimate a single-test repellency index, RI∗, that overcomes the limitations of the traditional approach given that information on both the hydrophobic and the wettable states of soil are gathered from a unique infiltration test. The mean RI values were affected by the technique used to estimate Sw and Se. In particular, the choice of a fixed time interval lead to overestimation of RI up to a factor of 3.2 as compared with the other techniques. The RIa yielded unbiased estimations of the mean RI values and also allowed to quantify the variability of SWR within a given area. A statistically significant relationship was found between RI∗ and RI but also between RI∗ and the water retention cessation time, that is the time hydrophobic turns into wettable soil, thus indicating that RI∗ is potentially able detect both the degree and the persistence of SWR. Pekárová P., Pekár J., Lichner Ľ. 2015. A new method for estimating soil water repellency index. Biologia, 70(11):1450-1455.

Diagnosis of Enterocytozoon bieneusi by PCR in Stool Samples Eluted from Filter Paper Disks

PubMed Central

Carnevale, Silvana; Velásquez, Jorge N.; Labbé, Jorge H.; Chertcoff, Agustín; Cabrera, Marta G.; Rodríguez, Mónica I.

2000-01-01

We report a PCR-based assay for the detection of Enterocytozoon bieneusi. We extracted DNA from feces which had been applied to filter paper disks and evaluated four preserving solutions. Infected specimens were identified by electrophoresis of amplicons from concentrated formalin-fixed samples and unconcentrated fresh feces. Our findings demonstrate that this methodology is effective for sample collection, mailing, and diagnosis of this pathogen. PMID:10799469

Image processing techniques applied to the detection of optic disk: a comparison

NASA Astrophysics Data System (ADS)

Kumari, Vijaya V.; Narayanan, Suriya N.

2010-02-01

In retinal image analysis, the detection of optic disk is of paramount importance. It facilitates the tracking of various anatomical features and also in the extraction of exudates, drusens etc., present in the retina of human eye. The health of retina crumbles with age in some people during the presence of exudates causing Diabetic Retinopathy. The existence of exudates increases the risk for age related macular Degeneration (AMRD) and it is the leading cause for blindness in people above the age of 50.A prompt diagnosis when the disease is at the early stage can help to prevent irreversible damages to the diabetic eye. Screening to detect diabetic retinopathy helps to prevent the visual loss. The optic disk detection is the rudimentary requirement for the screening. In this paper few methods for optic disk detection were compared which uses both the properties of optic disk and model based approaches. They are uniquely used to give accurate results in the retinal images.

Fatigue Failure Modes of the Grain Size Transition Zone in a Dual Microstructure Disk

NASA Technical Reports Server (NTRS)

Gabb, Timothy P.; Kantzos, Pete T.; Palsa, Bonnie; Telesman, Jack; Gayda, John; Sudbrack, Chantal K.

2012-01-01

Mechanical property requirements vary with location in nickel-based superalloy disks. In order to maximize the associated mechanical properties, heat treatment methods have been developed for producing tailored grain microstructures. In this study, fatigue failure modes of a grain size transition zone in a dual microstructure disk were evaluated. A specialized heat treatment method was applied to produce varying grain microstructure in the bore to rim portions of a powder metallurgy processed nickel-based superalloy disk. The transition in grain size was concentrated in a zone of the disk web, between the bore and rim. Specimens were extracted parallel and transversely across this transition zone, and multiple fatigue tests were performed at 427 C and 704 C. Grain size distributions were characterized in the specimens, and related to operative failure initiation modes. Mean fatigue life decreased with increasing maximum grain size, going out through the transition zone. The scatter in limited tests of replicates was comparable for failures of uniform gage specimens in all transition zone locations examined.

Evaluation of stir-bar sorptive extraction coupled with thermal desorption GC-MS for the detection of leachables from polymer single use systems to drugs.

PubMed

Scherer, Nicole; Marcseková, Klaudia; Posset, Tobias; Winter, Gerhard

2018-04-15

Stir-bar Sorptive Extraction (SBSE) in combination with thermal desorption and gas chromatography-mass spectrometry (TD-GC-MS) is widely accepted as the gold-standard analysis method for trace amounts of organic substances, including leachables in aqueous matrices. Meanwhile, as far as pharmaceutical quality control in protein-based parenteral drugs is concerned, the use of SBSE analysis remains unexplored. Previous studies reported a strong influence of the matrix on the method's recovery. The scope of the present work was to fill in the unexplored territory in a threefold manner 1) by quantifying the effects that various matrices commonly found in pharmaceutical processing have on the recovery, 2) by comparing between different coating materials for stir bar (namely between polydimethylsiloxane (PDMS) material and ethylene-glycol (EG)-PDMS), and 3) by proposing a preparation step for stir-bar to mitigate inhibitory effects. The current study shows no inhibition of SBSE by protein matrices (p > 0.15). Further the influence of various drug matrices on the recovery of leachables with a log K o/w  ≥ 3.6 is negligible (-3.9 to 3.8%). In contrast, the inhibition effect caused by an alkaline media led to a recovery decrease of -42.9%. For leachables with a log K o/w  < 3.6, the relative recovery in the presence of various proteins ranged from -72.8% to 15.6%, depending on the excipients of the drug product and not on the protein itself. The highest loss in sensitivity was observed when the excipient benzyl alcohol was present in the drug. Nonetheless, the limit of detection for the tested leachables in the inhibitory matrices was still below 3 μg/L (ppb). Additionally, SBSE was observed to be quantitatively reliable in all tested drug matrices for concentrations from 0.005 to 0.1 mg/mL (r 2  > 0.992). On average, the conventional PDMS coating resulted in a 28-fold higher signal-to-noise ratio compared to EG-PDMS. Furthermore, a broader range of leachables was detectable with the PDSM coating. Preceding stir-bar preparation consisting of a simple soaking step improved the enrichment by 14%, effectively lowering the limit of detection. Copyright © 2018 Elsevier B.V. All rights reserved.

Near-Infrared Polarimetric Imaging of Disks around Young Intermediate-mass Stars in SEEDS

NASA Astrophysics Data System (ADS)

Fukagawa, Misato; Hashimoto, Jun; Grady, C. A.; Momose, Munetake; Wisniewski, J. P.; Okamoto, Yoshiko; Muto, Takayuki; Kusakabe, Nobuhiko; Bonnefoy, Mickael; Kotani, Takayuki; Maruta, Yayoi; Tamura, Motohide; Seeds/Hiciao/Ao188 Collaboration,

2013-07-01

We present our recent results to directly image circumstellar disks around Herbig Fe/Ae/Be stars in scattered light with Subaru. Observations of such young disks are critically important to understand how disks evolve possibly under the mutual interaction with new-born planets. One of the observational approaches is direct imaging in scattered light, and the progress in this field since PPV can be found in the ability to prove inner regions of disks. This improvement largely owes to the technique of polarization differential imaging (PDI) which provides higher contrast by extracting scattered light from the disk while suppressing unpolarized stellar light. Strategic Exploration of Exoplanets and Disks with Subaru (SEEDS) is the project dedicated to exoplanet hunting and study of circumstellar disks by direct imaging. Since its beginning in 2009, thirteen Herbig Fe/Ae/Be stars have been observed primarily in H band (1.6 micron). The PDI method has been employed with adaptive optics, enabling us to look into the inner region as close as 0.2 arcsec (˜30 AU) in radius with the typical angular resolution of 0.06 arcsec (˜8 AU). As a result, the SEEDS imagery has newly uncovered rich structures such as spiral arms, inner holes, and gaps for (pre-)transitional disks while suggested the variably illuminated disks for primordial systems. The highlight is the discovery of two spiral arms each for SAO 206462 and MWC 758. The spiral feature has been uniquely found toward Herbig Fe/Aes so far, which might be due to their warmer disks producing arms loosely wound and more easily detected. The observed morphology can be interpreted by the density-wave model, and those disks are implied to harbor Jupiter-mass companions as the exciting sources of the spiral structures according to these models.

Modeling Self-subtraction in Angular Differential Imaging: Application to the HD 32297 Debris Disk

NASA Astrophysics Data System (ADS)

Esposito, Thomas M.; Fitzgerald, Michael P.; Graham, James R.; Kalas, Paul

2014-01-01

We present a new technique for forward-modeling self-subtraction of spatially extended emission in observations processed with angular differential imaging (ADI) algorithms. High-contrast direct imaging of circumstellar disks is limited by quasi-static speckle noise, and ADI is commonly used to suppress those speckles. However, the application of ADI can result in self-subtraction of the disk signal due to the disk's finite spatial extent. This signal attenuation varies with radial separation and biases measurements of the disk's surface brightness, thereby compromising inferences regarding the physical processes responsible for the dust distribution. To compensate for this attenuation, we forward model the disk structure and compute the form of the self-subtraction function at each separation. As a proof of concept, we apply our method to 1.6 and 2.2 μm Keck adaptive optics NIRC2 scattered-light observations of the HD 32297 debris disk reduced using a variant of the "locally optimized combination of images" algorithm. We are able to recover disk surface brightness that was otherwise lost to self-subtraction and produce simplified models of the brightness distribution as it appears with and without self-subtraction. From the latter models, we extract radial profiles for the disk's brightness, width, midplane position, and color that are unbiased by self-subtraction. Our analysis of these measurements indicates a break in the brightness profile power law at r ≈ 110 AU and a disk width that increases with separation from the star. We also verify disk curvature that displaces the midplane by up to 30 AU toward the northwest relative to a straight fiducial midplane.

Fast, safe, and reliable methods for extraction of major inorganic cations from small quantities of woody plant tissues

Treesearch

Rakesh Minocha; Walter C. Shortle

1993-01-01

Two simple and fast methods for the extraction of major inorganic cations (Ca, Mg, Mn, K) from small quantities of stemwood and needles of woody plants were developed. A 3.2- or 6.4-mm cobalt drill bit was used to shave samples from disks and increment cores of stemwood. For ion extraction, wood (ground or shavings) or needles were either homogenzied using a Tekmar...

Magnetically driven jets and winds: Exact solutions

NASA Technical Reports Server (NTRS)

Contopoulos, J.; Lovelace, R. V. E.

1994-01-01

We present a general class of self-similar solutions of the full set of MHD equations that include matter flow, electromagnetic fields, pressure, and gravity. The solutions represent axisymmetric, time-independent, nonrelativistic, ideal, magnetohydrodynamic, collimated outflows (jet and winds) from magnetized accretion disks around compact objects. The magnetic field extracts angular momentum from the disk, accelerates the outflows perpedicular to the disk, and provides collimation at large distances. The terminal outflow velocities are of the order of or greater than the rotational velocity of the disk at the base of the flow. When a nonzero electric current flows along the jet, the outflow radius oscillates with axial distance, whereas when the total electric current is zero (with the return current flowing across the jet's cross section), the outflow radius increase to a maximum and then decreases. The method can also be applied to relativistic outflows.

Flotation of metal-loaded clay anion exchangers. Part II: the case of arsenates.

PubMed

Lazaridis, N K; Hourzemanoglou, A; Matis, K A

2002-04-01

Hydrotalcite-like materials, or otherwise termed layered double hydroxides, are clays with an ability to remove anions. As they usually are in powder form, these sorbents often present appreciable problems in the solid/liquid separation process following the sorption stage. Sorptive flotation of metal-loaded particles was investigated in this paper, as an alternative two-stage process. In the sorption process, satisfactory removals of arsenic(V) were obtained onto synthetic hydrotalcite particles from water. The effect of some parameters, like the solution ionic strength, concentrations, temperature, etc. was examined. During the second stage of the process, hydrotalcite fine particles were removed from the liquid phase by dispersed-air flotation; various surfactants were tested in relation to the ionic strength of the solution. The combined process of sorptive flotation provides promising results for arsenic removal.

Mineralization of surfactants by the microbiota of submerged plant detritus.

PubMed

Federle, T W; Ventullo, R M

1990-02-01

In wetlands and canopied bodies of water, plant detritus is an important source of carbon and energy. Detrital materials possess a large surface area for sorption of dissolved organics and are colonized by a large and diverse microbiota. To examine the biodegradation of surfactants by these microorganisms, submerged oak leaves were obtained from a laundromat wastewater pond, its overflow, and a pristine control pond. Leaves were cut into disks and incubated in sterile water amended with 50 mug of C-labeled linear alkylbenzene sulfonate (LAS), linear alcohol ethoxylate, stearyltrimethyl ammonium chloride, distearyldimethyl ammonium chloride, benzoic acid, or mixed amino acids per liter. Sorption of the test compounds to the detritus and evolution of CO(2) were followed with time. All of the compounds sorbed to the detritus to various degrees, with LAS and stearyltrimethyl ammonium chloride the most sorptive and benzoic acid the least. All compounds were mineralized without a lag. With leaves from the laundromat wastewater pond, half-lives were 12.6 days for LAS, 8.4 days for linear alcohol ethoxylate, 14.2 days for stearyltrimethyl ammonium chloride, 1.0 days for benzoic acid, and 2.7 days for mixed amino acids. Mineralization of LAS and linear alcohol ethoxylate by control pond leaves was slower and exhibited an S-shaped rather than a typical first-order pattern. This study shows that detritus represents a significant site of surfactant removal in detritus-rich systems.

One-Dimensional Signal Extraction Of Paper-Written ECG Image And Its Archiving

NASA Astrophysics Data System (ADS)

Zhang, Zhi-ni; Zhang, Hong; Zhuang, Tian-ge

1987-10-01

A method for converting paper-written electrocardiograms to one dimensional (1-D) signals for archival storage on floppy disk is presented here. Appropriate image processing techniques were employed to remove the back-ground noise inherent to ECG recorder charts and to reconstruct the ECG waveform. The entire process consists of (1) digitization of paper-written ECGs with an image processing system via a TV camera; (2) image preprocessing, including histogram filtering and binary image generation; (3) ECG feature extraction and ECG wave tracing, and (4) transmission of the processed ECG data to IBM-PC compatible floppy disks for storage and retrieval. The algorithms employed here may also be used in the recognition of paper-written EEG or EMG and may be useful in robotic vision.

The Influence of Erosional Hotspots on Watershed-scale Phosphorus Dynamics in Intensively Managed Agricultural Landscapes

NASA Astrophysics Data System (ADS)

Baker, A.; Finlay, J. C.; Gran, K. B.; Karwan, D. L.; Engstrom, D. R.; Atkins, W.; Muramoto-Mathieu, M.

2017-12-01

The Minnesota River Basin is an intensively-managed agricultural watershed which contributes disproportionately to downstream sediment and nutrient loading. The Le Sueur River, an actively eroding tributary to the Minnesota River, has been identified as a disproportionate contributor of sediment and nutrients to this system. In an effort to identify best practices for reduction of phosphorus (P) in the context of intensifying agriculture and climate change pressure, we coupled investigation of source sediment P chemistry with an existing fine sediment budget to create a watershed mass balance for sediment-associated P. Sediments collected from primary source areas including agricultural fields, glacial till bluffs, alluvial streambanks, ravines, and agricultural ditches were analyzed for total- and extractable-P, and sorptive properties. Preliminary integration of these data into a mass-balance suggests that less than a quarter of the total-P exported from this watershed can be attributed directly to sediment inputs, likely due to the low P concentration of most sediment sources. While sediment may supply less than 25% of the total-P exiting the Le Sueur, a high proportion of total-P load ( 66% on average) is in particulate form. This finding indicates that sorption of dissolved-P from upstream sources onto fine sediment plays a major role in determining the form and reactivity of P in the watershed. Sorption processes convert dissolved-P into particulate-P, and may substantially alter the fate and reactivity of P in downstream channels and lakes. In highly erosive rivers, as the Le Sueur, where inputs of sediment from deep soil horizons are dominant, the dynamic relationship between sediment and dissolved-P must be evaluated and incorporated into models to forecast potential for P retention and export from the landscape. By incorporating results of this mass balance and analysis of sediment sorptive properties into existing models, we can develop strategies that most effectively address both of these interwoven pollutants to aquatic ecosystems.

Determination of endocrine disrupting chemicals and antiretroviral compounds in surface water: A disposable sorptive sampler with comprehensive gas chromatography - Time-of-flight mass spectrometry and large volume injection with ultra-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Wooding, Madelien; Rohwer, Egmont R; Naudé, Yvette

2017-05-05

Many rural dwellers and inhabitants of informal settlements in South Africa are without access to treated water and collect untreated water from rivers and dams for personal use. Endocrine disrupting chemicals (EDCs) have been detected in surface water and wildlife of South Africa. EDCs are often present in complex environmental matrices at ultra-trace levels complicating detection thereof. We report a simplified multi-residue approach for the detection and quantification of EDCs, emerging EDCs, and antiretroviral drugs in surface water. A low cost (less than one US dollar), disposable, sorptive extraction sampler was prepared in-house. The disposable samplers consisted of polydimethylsiloxane (PDMS) tubing fashioned into a loop which was then placed in water samples to concentrate EDCs and emerging pollutants. The PDMS samplers were thermally desorbed directly in the inlet of a GC, thereby eliminating the need for expensive consumable cryogenics. Comprehensive gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOFMS) was used for compound separation and identification. Linear retention indices of EDCs and emerging pollutants were determined on a proprietary Crossbond ® phase Rtx ® -CLPesticides II GC capillary column. In addition, large volume injection of surface water into an ultra-performance liquid chromatograph tandem mass spectrometer (UPLC-MS/MS) was used as complementary methodology for the detection of less volatile compounds. Large volume injection reduced tedious and costly sample preparation steps. Limits of detection for the GC method ranged from 1 to 98pg/l and for the LC method from 2 to 135ng/l. Known and emerging EDCs such as pharmaceuticals, personal care products and pesticides, as well as the antiretroviral compounds, efavirenz and nevirapine, were detected in surface water from South Africa at concentration levels ranging from 0.16ng/l to 227ng/l. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of ionic liquids supported on silica as a sorbent for fully automated online solid-phase extraction with LC-MS determination of sulfonamides in bovine milk samples.

PubMed

da Silva, Meire Ribeiro; Mauro Lanças, Fernando

2018-03-10

Sulfonamides are antibiotics widely used in the treatment of diseases in dairy cattle. However, their indiscriminate use for disease control may lead to their presence in tissues and milk and their determination requires a sample preparation step as part of an analytical approach. Among the several sample preparation techniques available, those based upon the use of sorptive materials have been widely employed. Recently, the application of ionic liquids immobilized on silica surfaces or polymeric materials has been evaluated for such an application. This manuscript addresses the evaluation of silica-based ionic liquid obtained by a sol-gel synthesis process by basic catalysis as sorbent for online solid-phase extraction with liquid chromatography and electrospray ionization time-of-flight mass spectrometry for sulfonamides determination. Infrared vibrational spectroscopy confirmed the presence of the ionic liquid on the silica surface, suggesting that the ionic liquid was anchored on to the silica surface. Other sorbents varying the ionic liquid alkyl chain were also synthesized and evaluated by off-line solid-phase extraction in the sulfonamide extraction. As the length of the alkyl chain increased, the amount of extracted sulfonamides decreased, possibly due to a decrease in the electrostatic interaction caused by the reduction in the polarity, as well as the presence of a hexafluorophosphate anion that increases the hydrophobic character of the material. The use of 1-butyl-3-methylimidazolium hexafluorophosphate as a selective ionic liquid sorbent enabled the isolation and sulfonamide preconcentration in bovine milk by online solid-phase extraction with liquid chromatography and electrospray ionization time-of-flight mass spectrometry. The limit of quantification for the method developed was 5-7, 5 μg/mL, with extraction recoveries ranging between 74 and 93% and intra- and interassay between 1.5-12.5 and 2.3-13.1, respectively. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Temperature characteristics of epitaxially grown InAs quantum dot micro-disk lasers on silicon for on-chip light sources

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

Wan, Yating; Li, Qiang; Lau, Kei May, E-mail: eekmlau@ust.hk

2016-07-04

Temperature characteristics of optically pumped micro-disk lasers (MDLs) incorporating InAs quantum dot active regions are investigated for on-chip light sources. The InAs quantum dot MDLs were grown on V-groove patterned (001) silicon, fully compatible with the prevailing complementary metal oxide-semiconductor technology. By combining the high-quality whispering gallery modes and 3D confinement of injected carriers in quantum dot micro-disk structures, we achieved lasing operation from 10 K up to room temperature under continuous optical pumping. Temperature dependences of the threshold, lasing wavelength, slope efficiency, and mode linewidth are examined. An excellent characteristic temperature T{sub o} of 105 K has been extracted.

LIQUID-SOLID DISK EXTRACTION FOLLOWED BY SFE AND GC-ION-TRAP MS FOR THE DETERMINATION OF TRACE ORGANIC POLLUTANTS IN WATER

EPA Science Inventory

The U.S. Environmental Protection Agency's (EPA) Industrial Toxic 33-50 Program, which is part of the Pollution Prevention Act of 1990, outlines a plan to reduce the use of some commonly used liquid solvents. One of the most widely used solvents for extraction of organic contamin...

Epsilon Aurigae's dark side: A thermal phase curve investigation of the near-eclipse phases

NASA Astrophysics Data System (ADS)

Pearson, Richard L.; Stencel, Robert E.; Howell, Steve B.; Hoard, D. W.; Kim, Daryl L.; Russell, Ray W.; Sitko, Michael L.

2017-06-01

The epsilon Aurigae disk-eclipsing binary system moves through a primary eclipse that lasts just over two years and occurs every 27.1-years. It comprises of a warm F0Ia-star (around 7750 K) and an opaque, circumstellar disk hiding an internal B-star (with a temperature greater than 15,000 K). We present new infrared observations from Spitzer's Infrared Array Camera (IRAC, at 3.6 and 4.5 microns) and The Aerospace Corporation’s Broadband Array Spectrograph System (BASS, a 116-element prism system spectrograph spanning 3 - 14 microns) in order to extract the thermal signature of the disk. Previous findings indicate a variable temperature of the disk, depending on its location within the system’s orbit: a 550 +\\- 50 K temperature was identified during eclipse phases, while a 1150 +\\- 50 K temperature was found near secondary—or anti-eclipse—phases by Hoard et al. (2010) and Hoard et al. (2012). We use the latest observations in combination with previously published IRAC and BASS data to compile a more complete thermal phase curve (TPC) of the disk across nearly one-third of the system’s orbit. The TPC indicates heating and cooling effects of the disk, pointing to specific ranges of material properties and disk structure. The observations, process, results, and implications will be presented.

COSOLVENT EFFECTS ON SORPTION ISOTHERM LINEARITY

EPA Science Inventory

Sorption-desorption hysteresis, slow desorption kinetics, and other nonideal phenomena have been attributed to the differing sorptive characteristics of the natural organic polymers associated with soils and sediments. In this study, aqueous and mixed solvent systems were used t...

Removal of copper(II) from some environmental samples by sorptive-flotation using powdered marble wastes as sorbents and oleic acid as surfactant.

PubMed

Ghazy, S E; Samra, S E; Mahdy, A F M; El-Morsy, S M

2004-11-01

A simple and economic experimental sorptive -flotation procedure is presented for the removal of copper(II) species from aqueous solutions. It is based on using powdered marble wastes (PMW), which are widespread and inexpensive and may represent an environmental problem, as the effective inorganic sorbent and oleic (HOL) as the surfactant. The main parameters (i.e. initial solution pH, sorbent, surfactant and copper concentrations, stirring times, ionic strength, temperature and the presence of foreign ions) influencing the flotation of PMW and /or Cu(II) were examined. Nearly, 100% of PMW and Cu(II) were removed from aqueous solutions at pH7 after stirring for 10 min and at room temperature, (approximately 25 degrees C). The procedure was successfully applied to recover Cu(II) spiked to some natural water samples. A mechanism for sorption and flotation is suggested.

Sol-gel coated polydimethylsiloxane/beta-cyclodextrin as novel stationary phase for stir bar sorptive extraction and its application to analysis of estrogens and bisphenol A.

PubMed

Hu, Yuling; Zheng, Yanjie; Zhu, Fei; Li, Gongke

2007-04-27

A sol-gel technique was used for the preparation of a stir bar coated with a composite composed of polydimethysiloxane and beta-cyclodextrin (PDMS/beta-CD). The sol-gel mechanism during coating procedure was discussed and successful binding of beta-CD to the sol-gel network was confirmed by the IR spectra. Scanning electron micrographs of the stir bars revealed a homogeneous surface with a film thickness of 30-150 microm attributing to different coating times. Good thermal stability and solvent-resistance of the stir bar were found thanks to chemical binding formed between the stationary phase and the glass substrate. The PDMS/beta-CD coated stir bar was proved to have better selectivity to polar compounds compared to the PDMS coated stir bar, and higher extraction capacity compared to the corresponding PDMS/beta-CD coated fiber. Methods for the determinations of estrogens in environmental water, bisphenol A in drinking water and in leachate of one-off dishware by the PDMS/beta-CD coated stir bar coupled with high-performance liquid chromatography (HPLC) were developed. The limits of detection were within the range of 0.04-0.11 microg l(-1) for estrogens using UV detection and 8 ngl(-1) for bisphenol A using fluorescence detection. Reproducibility with RSD less than 9.7% for extractions of real water samples at microg l(-1) or ngl(-1) level was obtained.

Automated headspace solid-phase dynamic extraction to analyse the volatile fraction of food matrices.

PubMed

Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara

2004-01-23

High concentration capacity headspace techniques (headspace solid-phase microextraction (HS-SPME) and headspace sorptive extraction (HSSE)) are a bridge between static and dynamic headspace, since they give high concentration factors as does dynamic headspace (D-HS), and are as easy to apply and as reproducible as static headspace (S-HS). In 2000, Chromtech (Idstein, Germany) introduced an inside-needle technique for vapour and liquid sampling, solid-phase dynamic extraction (SPDE), also known as "the magic needle". In SPDE, analytes are concentrated on a 50 microm film of polydimethylsiloxane (PDMS) and activated carbon (10%) coated onto the inside wall of the stainless steel needle (5 cm) of a 2.5 ml gas tight syringe. When SPDE is used for headspace sampling (HS-SPDE), a fixed volume of the headspace of the sample under investigation is sucked up an appropriate number of times with the gas tight syringe and an analyte amount suitable for a reliable GC or GC-MS analysis accumulates in the polymer coating the needle wall. This article describes the preliminary results of both a study on the optimisation of sampling parameters conditioning HS-SPDE recovery, through the analysis of a standard mixture of highly volatile compounds (beta-pinene, isoamyl acetate and linalool) and of the HS-SPDE-GC-MS analyses of aromatic plants and food matrices. This study shows that HS-SPDE is a successful technique for HS-sampling with high concentration capability, good repeatability and intermediate precision, also when it is compared to HS-SPME.

A Comparison between Antibacterial Activity of Propolis and Aloe vera on Enterococcus faecalis (an In Vitro Study).

PubMed

Ehsani, Maryam; Amin Marashi, Mahmood; Zabihi, Ebrahim; Issazadeh, Maryam; Khafri, Soraya

2013-01-01

Removing the bacteria, including Enterococcus faecalis, from the root canal is one of the important aims in endodontic treatment.We aimed to compare the antibacterial activity of Chlorhexidine with two natural drugs. The antibacterial activities of three different propolis extracts (alcohol concentrations: 0, 15, 40%) and Aloe vera gel on E. faecalis were compared using three methods: disk diffusion, microdilution and direct contact test. In addition to the above bacterium, the Aloe vera gel effect on Staphylococcus aureus and Streptococcus mutans was evaluated. Disk diffusion test revealed that propolis ethanolic extracts (the alcohol concentration of 15 and 40%) and Aloe vera gel have antibacterial activities but aqueous extract of propolis did not show any effect in this test. The MICs for propolis ethanolic extracts, Aloe vera gel and aqueous extract of propolis (0% alcohol) were 313 µg/ml, 750 µg/ml, 2250 µg/ml, and ≥ 500 µg/ml respectively, much higher than the Chlorhexidine one. In direct contact test, contrary to Aloe vera, all three propolis extracts showed antibacterial effects on E. faecalis. The Aloe vera gel also showed significant antibacterial effect on S.aureus and S.mutans. The hydroalcoholic extracts of propolis and Aloe vera gel had antibacterial effects on E. faecalis, however, propolis is more potent than Aloe vera. The antibacterial effect of Aloe vera on S. aureus and S. mutans is low (MIC ≥ 2250 µg/ml). Appropriate concentrations of alcoholic extracts of propolis and some fractions of Aloe vera gel might be good choices for disinfecting the root canal in endodontic treatments.

An in vitro evaluation of the antibacterial efficacy of chlorine dioxide on E. faecalis in bovine incisors.

PubMed

Eddy, Russell S; Joyce, Anthony P; Roberts, Steven; Buxton, Thomas B; Liewehr, Frederick

2005-09-01

This study investigated the ability of chlorine dioxide to eliminate Enterococcus faecalis from dentinal tubules of bovine incisors. Thirty-seven extracted bovine incisor roots were sectioned into seventy-four 5 mm disks. Standardized lumens were filled with either sterile Brain Heart Infusion Broth (contamination controls, n = 10) or BHI containing E. faecalis (1.0 x 10 cfu/ml). Disks were incubated in 5% CO2 at 37 degrees C for 72 h. To simulate endodontic instrumentation the lumens were again enlarged. Sixty disks were randomly divided into four experimental groups and filled with one of the following irrigants: 10% Clidox-S (chlorine dioxide), 13.8% BioClenz (chlorine dioxide), 5.25% Clorox, or saline. The disks were incubated for 30 min and were then frozen, pulverized, serially diluted in phosphate buffered saline, and plated on BHI plates in triplicate. Total colony forming units were counted macroscopically. Statistical analysis of the data was performed with a Kruskal-Wallis one-way ANOVA on ranks (p < 0.05, n = 60). Bacterial counts, expressed in log10 cfu/disk were as follows (">" denotes significant differences): Saline > Clidox-S = BioClenz > Clorox. All negative controls were sterile. Chlorine dioxide and NaOCL were both effective in eliminating E. faecalis from the dentinal disks within 30 min.

Pinot noir wine volatile and anthocyanin composition under different levels of vine fruit zone leaf removal.

PubMed

Feng, Hui; Skinkis, Patricia A; Qian, Michael C

2017-01-01

The impacts of fruit zone leaf removal on volatile and anthocyanin compositions of Pinot noir wine were investigated over two growing seasons. Wine volatiles were analyzed by multiple techniques, including headspace solid phase microextraction-GC-MS (HS-SPME-GC-MS), headspace-GC-FID (HS-GC-FID) and stir bar sorptive extraction-GC-MS (SBSE-GC-MS). Fruit zone leaf removal affected the concentration of many grape-derived volatile compounds such as terpene alcohols and C13-norisoprenoids in wine, although the degree of impact depended on the vintage year and severity of leaf removal. Fruit zone leaf removal resulted in greater concentrations of linalool, α-terpineol and β-damascenone but had no impact on other terpene alcohols or β-ionone. Fruit zone leaf removal had no consistent impact on C6 alcohols, volatile phenols, lactones, fermentation-derived alcohols, acids, or most esters. Fruit zone leaf removal increased anthocyanins in final wine. Copyright © 2016 Elsevier Ltd. All rights reserved.

Metals removal from aqueous solution by iron-based bonding agents.

PubMed

Deliyanni, Eleni A; Lazaridis, Nikolaos K; Peleka, Efrosini N; Matis, Konstantinos A

2004-01-01

GOAL AND SCOPE AND BACKGROUND: The application of a promising method, termed sorptive flotation, for the removal of chromium(VI) and zinc ions was the aim of the present paper. A special case of sorptive flotation is adsorbing colloid flotation. Suitable sorbent preparation techniques have been developed in the laboratory. Sorptive flotation, consisting of the sorption and flotation processes combined in series, has proved to give fast and satisfactory treatment of the industrial streams and effluents bearing dilute aqueous solutions of zinc and chromium(VI). Goethite has proved to be effective for the removal of chromium(VI) and zinc ions. Also, adsorbing colloid flotation with ferric hydroxide (as the co-precipitant) could be an alternative method to the above-mentioned separation of metal ions. In both cases, chromium(VI) (pH=4) and zinc (pH=7) removal was about 100%. The reasons for selecting the iron-based bonding materials, like goethite and/or in-situ produced ferric hydroxide, are that they are cheap, easily synthesized, suitable both for cation and anion sorption, and, furthermore, that they present low risks for adding a further pollutant to the system. Promising results were obtained. The application of goethite and in-situ produced ferric hydroxide has demonstrated their effectiveness in the removal of heavy metal ions, such as chromium anions and zinc cations. A proposed continuation of current work is the utilization of similar iron oxides, for instance synthesized akaganeite. The comparison between the results reported in this paper with the results reported in the literature, also deserves attention.

COSOLVENT EFFECTS ON ORGANIC CHEMICAL PARTITIONING TO SEDIMENT ORGANIC CARBON

EPA Science Inventory

Sorption-desorption hysteresis, slow desorption kinetics and resultant bioavailability, and other nonideal phenomena have been attributed to the differing sorptive characteristics of the natural organic polymers associated with soils and sediments. The objectives of this study we...

USING METHANOL-WATER SYSTEMS TO INVESTIGATE PHENANTHRENE SORPTION-DESORPTION ON SEDIMENT

EPA Science Inventory

Sorption isotherm nonlinearity, sorption-desorption hysteresis, slow desorption kinetics, and other nonideal phenomena have been attributed to the differing sorptive characteristics of the natural organic matter (NOM) polymers associated with soils and sediments. A conceptualizat...

ALMA REVEALS THE ANATOMY OF THE mm-SIZED DUST AND MOLECULAR GAS IN THE HD 97048 DISK

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

Walsh, Catherine; Maud, Luke T.; Juhász, Attila

Transitional disks show a lack of excess emission at infrared wavelengths due to a large dust cavity, that is often corroborated by spatially resolved observations at ∼ mm wavelengths. We present the first spatially resolved ∼ mm-wavelength images of the disk around the Herbig Ae/Be star, HD 97048. Scattered light images show that the disk extends to ≈640 au. ALMA data reveal a circular-symmetric dusty disk extending to ≈350 au, and a molecular disk traced in CO J = 3-2 emission, extending to ≈750 au. The CO emission arises from a flared layer with an opening angle ≈30°–40°. HD 97048more » is another source for which the large (∼ mm-sized) dust grains are more centrally concentrated than the small (∼ μ m-sized) grains and molecular gas, likely due to radial drift. The images and visibility data modeling suggest a decrement in continuum emission within ≈50 au, consistent with the cavity size determined from mid-infrared imaging (34 ± 4 au). The extracted continuum intensity profiles show ring-like structures with peaks at ≈50, 150, and 300 au, with associated gaps at ≈100 and 250 au. This structure should be confirmed in higher-resolution images (FWHM ≈ 10–20 au). These data confirm the classification of HD 97048 as a transitional disk that also possesses multiple ring-like structures in the dust continuum emission. Additional data are required at multiple and well-separated frequencies to fully characterize the disk structure, and thereby constrain the mechanism(s) responsible for sculpting the HD 97048 disk.« less

ALMA Reveals the Anatomy of the mm-sized Dust and Molecular Gas in the HD 97048 Disk

NASA Astrophysics Data System (ADS)

Walsh, Catherine; Juhász, Attila; Meeus, Gwendolyn; Dent, William R. F.; Maud, Luke T.; Aikawa, Yuri; Millar, Tom J.; Nomura, Hideko

2016-11-01

Transitional disks show a lack of excess emission at infrared wavelengths due to a large dust cavity, that is often corroborated by spatially resolved observations at ˜ mm wavelengths. We present the first spatially resolved ˜ mm-wavelength images of the disk around the Herbig Ae/Be star, HD 97048. Scattered light images show that the disk extends to ≈640 au. ALMA data reveal a circular-symmetric dusty disk extending to ≈350 au, and a molecular disk traced in CO J = 3-2 emission, extending to ≈750 au. The CO emission arises from a flared layer with an opening angle ≈30°-40°. HD 97048 is another source for which the large (˜ mm-sized) dust grains are more centrally concentrated than the small (˜μm-sized) grains and molecular gas, likely due to radial drift. The images and visibility data modeling suggest a decrement in continuum emission within ≈50 au, consistent with the cavity size determined from mid-infrared imaging (34 ± 4 au). The extracted continuum intensity profiles show ring-like structures with peaks at ≈50, 150, and 300 au, with associated gaps at ≈100 and 250 au. This structure should be confirmed in higher-resolution images (FWHM ≈ 10-20 au). These data confirm the classification of HD 97048 as a transitional disk that also possesses multiple ring-like structures in the dust continuum emission. Additional data are required at multiple and well-separated frequencies to fully characterize the disk structure, and thereby constrain the mechanism(s) responsible for sculpting the HD 97048 disk.

A Study of Inner Disk Gas around Young Stars in the Lupus Complex

NASA Astrophysics Data System (ADS)

Arulanantham, Nicole Annemarie; France, Kevin; Hoadley, Keri

2018-06-01

We present a study of molecular hydrogen at the surfaces of the disks around five young stars in the Lupus complex: RY Lupi, RU Lupi, MY Lupi, Sz 68, and TYC 7851. Each system was observed with the Cosmic Origins Spectrograph (COS) onboard the Hubble Space Telescope (HST), and we detect a population of fluorescent H2 in all five sources. The temperatures required for LyA fluorescence to proceed (T ~ 1500-2500 K) place the gas within ~15 AU of the central stars. We have used these features to extract the radial distribution of H2 in the inner disk, where planet formation may already be taking place. The objects presented here have very different outer disk morphologies, as seen by ALMA via 890 micron dust continuum emission, ranging from full disks with no signs of cavities to systems with large regions that are clearly depleted (e.g. TYC 7851, with a cavity extending to 75 and 60 AU in dust and gas, respectively). Our results are interpreted in conjunction with sub-mm data from the five systems in an effort to piece together a more complete picture of the overall disk structure. We have previously applied this multi-wavelength approach to RY Lupi, including 4.7 micron IR-CO emission in our analysis. These IR-CO and UV-H2 observations were combined with 10 micron silicate emission, the 890 micron dust continuum, and 1.3 mm CO observations from the literature to infer a gapped structure in the inner disk. This single system has served as a testing ground for the larger Lupus complex sample, which we compare here to examine any trends between the outer disk morphology and inner disk gas distributions.

Consequences of Relativistic Neutron Outflow beyond the Accretion Disks of Active Galaxies

NASA Astrophysics Data System (ADS)

Ekejiuba, I. E.; Okeke, P. N.

1993-05-01

Three channels of relativistic electron injection in the jets of extragalactic radio sources (EGRSs) are discussed. With the assumption that an active galactic nucleus (AGN) is powered by a spinning supermassive black hole of mass ~ 10(8) M_⊙ which sits at the center of the nucleus and ingests matter and energy through an accretion disk, a model for extracting relativistic neutrons from the AGN is forged. In this model, the inelastic proton--proton and proton--photon interactions within the accretion disk, of relativistic protons with background thermal protons and photons, respectively, produce copious amounts of relativistic neutrons. These neutrons travel ballistically for ~ 10(3gamma_n ) seconds and escape from the disk before they decay. The secondary particles produced from the neutron decays then interact with the ambient magnetic field and/or other particles to produce the radio emissions observed in the jets of EGRSs. IEE acknowledges the support of the World Bank and the Federal University of Technology, Yola, Nigeria as well as the hospitality of Georgia State University.

Assessing levels and seasonal variations of current-use pesticides (CUPs) in the Tuscan atmosphere, Italy, using polyurethane foam disks (PUF) passive air samplers.

PubMed

Estellano, Victor H; Pozo, Karla; Efstathiou, Christos; Pozo, Katerine; Corsolini, Simonetta; Focardi, Silvano

2015-10-01

Polyurethane foam disks (PUF) passive air samplers (PAS) were deployed over 4 sampling periods of 3-5-months (≥ 1 year) at ten urban and rural locations throughout the Tuscany Region. The purpose was to assess the occurrence and seasonal variations of ten current-use pesticides (CUPs). PUF disk extracts were analyzed using GC-MS. The organophosphates insecticides; chlorpyrifos (3-580 pg m(-3)) and chlorpyrifos-methyl (below detection limit - to 570 pg m(-3)) presented the highest levels in air, and showed seasonal fluctuation coinciding with the growing seasons. The relative proportion urban/(urban + rural) ranged from 0.4 to 0.7 showing no differences between urban and rural concentrations. Air back trajectories analysis showed air masses passing over agricultural fields and potentially enhancing the drift of pesticides into the urban sites. This study represents the first information regarding CUPs in the atmosphere of Tuscany region using PAS-PUF disk. Copyright © 2015 Elsevier Ltd. All rights reserved.

Damage detection of engine bladed-disks using multivariate statistical analysis

NASA Astrophysics Data System (ADS)

Fang, X.; Tang, J.

2006-03-01

The timely detection of damage in aero-engine bladed-disks is an extremely important and challenging research topic. Bladed-disks have high modal density and, particularly, their vibration responses are subject to significant uncertainties due to manufacturing tolerance (blade-to-blade difference or mistuning), operating condition change and sensor noise. In this study, we present a new methodology for the on-line damage detection of engine bladed-disks using their vibratory responses during spin-up or spin-down operations which can be measured by blade-tip-timing sensing technique. We apply a principle component analysis (PCA)-based approach for data compression, feature extraction, and denoising. The non-model based damage detection is achieved by analyzing the change between response features of the healthy structure and of the damaged one. We facilitate such comparison by incorporating the Hotelling's statistic T2 analysis, which yields damage declaration with a given confidence level. The effectiveness of the method is demonstrated by case studies.

Characterizing the thermal distributions of warm molecular hydrogen in protoplanetary disks

NASA Astrophysics Data System (ADS)

Hoadley, Keri; France, Kevin

2016-01-01

Probing the surviving molecular gas within the inner regions of protoplanetary disks (PPDs) around T Tauri stars (1 - 10 Myr) provides insight into the conditions in which planet formation and migration occurs while the gas disk is still present. Recent studies done by Hoadley et al. 2015 and Banzatti & Pontipoddan 2015 suggest that gas in the inner disks of PPDs appear to "respond" to the loss of small dust grains with evolving PPD stage, and IR-CO emission may either be thermally or photo-excited by stellar UV radiation, depending on PPD evolutionary stage. Because far-UV H2 emission lines are dominantly photo-excited by stellar HI-Lyman alpha photons, we observe H2 absorption features against the stellar Lyman alpha wings in a large sample of PPDs at various evolutionary stages. We aim to characterize whether the inner disk H2 environment is in thermal equilibrium at various stages of PPD evolution. We use a sophisticated first-principles approach to fitting multiple absorption features along the red- and blue-wings of the observed stellar Lyman alpha profiles to extract column density estimates of H2 along the line of sight to the target. We find that the high kinetic energy H2 observed in absorption against the LyA wing may be described as a part of the thermal distribution with high kinetic temperature - a potential indication of an inner disk molecular hazy "envelope" around the cooler bulk disk. Ongoing research may help determine the state of the gas and whether it evolves with disk evolutionary stage.

DETERMINATION OF SORPTION PARAMETERS FOR 36 VOC/MATERIAL COMBINATIONS

EPA Science Inventory

EPA's Air Pollution Prevention and Control Division is currently investigating sorptive interactions (sink effects) of volatile organic compounds and semi-volatile organic compounds when exposed to common indoor surface materials. The objective is to recommend the best sink mode...

Rapid method for determination of 90Sr in seawater by liquid scintillation counting with an extractive scintillator.

PubMed

Uesugi, Masaki; Watanabe, Ryosuke; Sakai, Hiroaki; Yokoyama, Akihiko

2018-02-01

A rapid determination method of 90 Sr is developed for the monitoring of seawater around the Fukushima Daiichi Nuclear Power Plant (FDNPP). Three ideas of chemical separation and measurements to accelerate 90 Sr analysis are investigated. Strontium is co-precipitated in a two-step procedure with hydroxyapatite after the removal of magnesium phosphate in the presence of citric acid. The purification process of strontium is in combination with solid phase extraction disks. One or two sheets of Sr Rad disk and cyclic operations are examined to eliminate interfering substances and secure the exchange capacity. The suitable conditions of adsorption and stripping are determined with a 85 Sr tracer. Seawater samples up to 1L can be analyzed within 4h. Additionally, the appropriate pH conditions to extract strontium to the scintillator are studied, and the 90 Sr activity is assessed via liquid scintillation counting using an extractive scintillator based on the di-(2-etyl hexyl)-phosphoric acid (HDEHP) extraction method. The new scintillation counting method involves a small quenching effect and a low background compared to the conventional emulsion scintillator method. The minimum detectable activity (MDA) is 35mBq/L of 90 Sr in 180min of counting. The proposed method provides analytical results within a day after receipt of the samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Bioanalytical effect-balance model to determine the bioavailability of organic contaminants in sediments affected by black and natural carbon.

PubMed

Bräunig, Jennifer; Tang, Janet Y M; Warne, Michael St J; Escher, Beate I

2016-08-01

In sediments several binding phases dictate the fate and bioavailability of organic contaminants. Black carbon (BC) has a high sorptive capacity for organic contaminants and can limit their bioavailability, while the fraction bound to organic carbon (OC) is considered to be readily desorbable and bioavailable. We investigated the bioavailability and mixture toxicity of sediment-associated contaminants by combining different extraction techniques with in vitro bioanalytical tools. Sediments from a harbour with high fraction of BC, and sediments from remote, agricultural and urban areas with lower BC were treated with exhaustive solvent extraction, Tenax extraction and passive sampling to estimate total, bioaccessible and bioavailable fractions, respectively. The extracts were characterized with cell-based bioassays that measure dioxin-like activity (AhR-CAFLUX) and the adaptive stress response to oxidative stress (AREc32). Resulting bioanalytical equivalents, which are effect-scaled concentrations, were applied in an effect-balance model, consistent with a mass balance-partitioning model for single chemicals. Sediments containing BC had most of the bioactivity associated to the BC fraction, while the OC fraction played a role for sediments with lower BC. As effect-based sediment-water distribution ratios demonstrated, most of the bioactivity in the AhR-CAFLUX was attributable to hydrophobic chemicals while more hydrophilic chemicals activated AREc32, even though bioanalytical equivalents in the aqueous phase remained negligible. This approach can be used to understand the fate and effects of mixtures of diverse organic contaminants in sediments that would not be possible if single chemicals were targeted by chemical analysis; and make informed risk-based decisions concerning the management of contaminated sediments. Copyright © 2016 Elsevier Ltd. All rights reserved.

Development of a microwave assisted extraction method for the analysis of 2,4,6-trichloroanisole in cork stoppers by SIDA-SBSE-GC-MS.

PubMed

Vestner, Jochen; Fritsch, Stefanie; Rauhut, Doris

2010-02-15

The aim of this research work was focused on the replacement of the time-consuming soaking of cork stoppers which is mainly used as screening method for cork lots in connection with sensory analysis and/or analytical methods to detect releasable 2,4,6-trichloroanisole (TCA) of natural cork stoppers. Releasable TCA from whole cork stoppers was analysed with the application of a microwave assisted extraction method (MAE) in combination with stir bar sorptive extraction (SBSE). The soaking of corks (SOAK) was used as a reference method to optimise MAE parameters. Cork lots of different quality and TCA contamination levels were used to adapt MAE. Pre-tests indicated that an MAE at 40 degrees C for 120 min with 90 min of cooling time are suitable conditions to avoid an over-extraction of TCA of low and medium tainted cork stoppers in comparison to SOAK. These MAE parameters allow the measuring of almost the same amounts of releasable TCA as with the application of the soaking procedure in the relevant range (<25 ng L(-1) releasable TCA from one cork) to evaluate the TCA level of cork stoppers. Stable isotope dilution assay (SIDA) was applied to optimise quantification of the released TCA with deuterium-labelled TCA (TCA-d(5)) using a time-saving GC-MS technique in single ion monitoring (SIM) mode. The developed MAE method allows the measuring of releasable TCA from the whole cork stopper under improved conditions and in connection with a low use of solvent and a higher sample throughput. Copyright 2009 Elsevier B.V. All rights reserved.

Application of modified stir bar with nickel:zinc sulphide nanoparticles loaded on activated carbon as a sorbent for preconcentration of losartan and valsartan and their determination by high performance liquid chromatography.

PubMed

Pebdani, Arezou Amiri; Dadfarnia, Shayesteh; Shabani, Ali Mohammad Haji; Khodadoust, Saeid; Haghgoo, Soheila

2016-03-11

In this study, the stir bar was coated for the first time with the ​nicel:zins sulphide nanoparticles (Ni:ZnS NPs) loaded on activated carbon (AC) (Ni:ZnS-AC) as well as 1-ethyl-3-methylimidazolium hexafluorophosphate ionic liquid (IL) using sol gel technique and was used for stir bar sorptive extraction (SBSE) of losartan (LOS) and valsartan (VAL) as the model compounds. The extracted analytes were then quantified by high performance liquid chromatography (HPLC) equipped with an ultra violet detector. The best extraction performance for LOS and VAL was obtained through the optimization of the parameters affecting SBSE including pH of sample solution, ionic strength, extraction time, volume of desorption solvent, desorption time, and stirring speed. The fractional factorial design (FFD) was used to find the most important parameters, which were then optimized by the central composite design (CCD) and the desirability function (DF). Under the optimal experimental conditions, wide linear ranges of 0.4-50μgL(-1) and 0.5-50μgL(-1) and good RSDs (at level of 5μgL(-1) and n=6) of 4.4 and 4.9% were obtained for LOS and VAL, respectively. With the enrichment factors (EFs) of 188.6 and 184.8-fold, the limits of detection (LODs, S/N=3) of the developed method were found to be 0.12 and 0.15μgL(-1) for LOS and VAL, respectively. The developed method was successfully applied to the determination of LOS and VAL in urine and plasma matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

Disentangling The Evolution Of S0 Galaxies Using Spectral Data Cubes

NASA Astrophysics Data System (ADS)

Johnston, Evelyn; Tabor, Martha; Merrifield, Michael; Aragón-Salamanca, Alfonso; Häussler, Boris; Bamford, Steven; Cappellari, Michele

2016-09-01

While it is fairly well accepted that S0 galaxies evolve from spiral disk systems, the mechanism by which they do so is not well determined. A number of processes, ranging from simply running out of gas to environmentally-driven gas removal, interactions and mergers, have been proposed, and the reality is probably that there are multiple routes between these two states.One key way to explore how the disk and bulge components in S0 galaxies reached their current states is provided by studies of their spectra: stellar population analysis provides information on the sequence in which these components formed, while the kinematic information in these data holds clues to the degree of violence in the transformation process.With the availability of large integral-field unit (IFU) spectral surveys of nearby galaxies, there is now the potential to extract this information in a systematic way, to address the questions of which evolutionary channels S0 have galaxies evolved down, and whether these channels depend on other properties of the galaxy such as its mass or environment. Accordingly, we have been developing new tools to extract optimally the information contained within such data, to isolate the spectral properties of these galaxies' disks and bulges.Results to date are already proving interesting, with bulges of S0s in clusters systematically younger than the disks that surround them, implying a last chaotic burst of star formation near their centres in a reasonably violent transition, while those in less dense environments seem to show older bulges, consistent with star formation in a spiral galaxy simply ceasing.

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

EPA Science Inventory

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

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

EPA Science Inventory

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

Mineralization of Surfactants by the Microbiota of Submerged Plant Detritus

PubMed Central

Federle, Thomas W.; Ventullo, Roy M.

1990-01-01

In wetlands and canopied bodies of water, plant detritus is an important source of carbon and energy. Detrital materials possess a large surface area for sorption of dissolved organics and are colonized by a large and diverse microbiota. To examine the biodegradation of surfactants by these microorganisms, submerged oak leaves were obtained from a laundromat wastewater pond, its overflow, and a pristine control pond. Leaves were cut into disks and incubated in sterile water amended with 50 μg of 14C-labeled linear alkylbenzene sulfonate (LAS), linear alcohol ethoxylate, stearyltrimethyl ammonium chloride, distearyldimethyl ammonium chloride, benzoic acid, or mixed amino acids per liter. Sorption of the test compounds to the detritus and evolution of 14CO2 were followed with time. All of the compounds sorbed to the detritus to various degrees, with LAS and stearyltrimethyl ammonium chloride the most sorptive and benzoic acid the least. All compounds were mineralized without a lag. With leaves from the laundromat wastewater pond, half-lives were 12.6 days for LAS, 8.4 days for linear alcohol ethoxylate, 14.2 days for stearyltrimethyl ammonium chloride, 1.0 days for benzoic acid, and 2.7 days for mixed amino acids. Mineralization of LAS and linear alcohol ethoxylate by control pond leaves was slower and exhibited an S-shaped rather than a typical first-order pattern. This study shows that detritus represents a significant site of surfactant removal in detritus-rich systems. Images PMID:16348111

Biochemistry of Suberization

PubMed Central

Agrawal, Vishwanath P.; Kolattukudy, P. E.

1977-01-01

A cell-free extract obtained from suberizing potato (Solanum tuberosum L.) tuber disks catalyzed the conversion of 16-hydroxy[G-3H]hexadecanoic acid to the corresponding dicarboxylic acid with NADP or NAD as the cofactor, with a slight preference for the former. This ω-hydroxyacid dehydrogenase activity, located largely in the 100,000g supernatant fraction, has a pH optimum of 9.5. It showed an apparent Km of 50 μM for 16-hydroxyhexadecanoic acid. The dehydrogenase activity was inhibited by thiol reagents, such as p-chloromercuribenzoate, N-ethylmaleimide, and iodoacetamide, and this dehydrogenase is shown to be different from alcohol dehydrogenase. That 16-oxohexadecanoic acid was an intermediate in the conversion of 16-hydroxyhexadecanoic acid to the corresponding dicarboxylic acid was suggested by the observation that the cell-free extract also catalyzed the conversion of 16-oxohexadecanoic acid to the dicarboxylic acid, with NADP as the preferred cofactor. The time course of development of the ω-hydroxyacid dehydrogenase activity in the suberizing potato disks correlated with the rate of deposition of suberin. Experiments with actinomycin D and cycloheximide suggested that the transcriptional processes, which are directly related to suberin biosynthesis and ω-hydroxyacid dehydrogenase biosynthesis, occurred between 72 and 96 hours after wounding. These results strongly suggest that a wound-induced ω-hydroxyacid dehydrogenase is involved in suberin biosynthesis in potato disks. PMID:16659915

Modelling of Tc migration in an un-oxidized fractured drill core from Äspö, Sweden

NASA Astrophysics Data System (ADS)

Huber, F. M.; Totskiy, Y.; Montoya Garcia, V.; Enzmann, F.; Trumm, M.; Wenka, A.; Geckeis, H.; Schaefer, T.

2015-12-01

The radionuclide retention of redox sensitive radionuclides (e.g. Pu, Np, U, Tc) in crystalline host rock greatly depends on the rock matrix and the rock redox capacity. Preservation of drill cores concerning oxidation is therefore of paramount importance to reliably predict the near-natural radionuclide retention properties. Here, experimental results of HTO and Tc laboratory migration experiments in a naturally single fractured Äspö un-oxidized drill core are modelled using two different 2D models. Both models employ geometrical information obtained by μ-computed tomography (μCT) scanning of the drill core. The models differ in geometrical complexity meaning the first model (PPM-MD) consists of a simple parallel plate with a porous matrix adjacent to the fracture whereas the second model (MPM) uses the mid-plane of the 3D fracture only (no porous matrix). Simulation results show that for higher flow rates (Peclet number > 1), the MPM satisfactorily describes the HTO breakthrough curves (BTC) whereas the PPM-MD model nicely reproduces the HTO BTC for small Pe numbers (<1). These findings clearly highlight the influence of fracture geometry/flow field complexity on solute transport for Pe numbers > 1 and the dominating effect of matrix diffusion for Peclet numbers < 1. Retention of Tc is modelled using a simple Kd-approach in case of the PPM-MD and including 1st order sorptive reduction/desorption kinetics in case of the MPM. Batch determined sorptive reduction/desorption kinetic rates and Kd values for Tc on non-oxidized Äspö diorite are used in the model and compared to best fit values. By this approach, the transferability of kinetic data concerning sorptive reduction determined in static batch experiments to dynamic transport experiments is examined.

Alteration of soil hydraulic properties and soil water repellency by fire and vegetation succession in a sagebrush steppe ecosystem

NASA Astrophysics Data System (ADS)

Chandler, D. G.; Seyfried, M. S.

2016-12-01

This study explores the impacts of fire and plant community succession on soil water repellency (SWR) and infiltration properties to improve understanding the long term impacts of prescribed fire on SWR and infiltration properties in sagebrush-steppe ecosystem. The objectives of this study were: 1) To explore the temporal effects of prescribed burning in sagebrush dominated landscape; 2) To investigate spatial variability of soil hydrologic properties; 3) To determine the relationship among soil organic fraction, soil hydrophobicity and infiltration properties. Fieldwork was conducted in paired catchments with three dominant vegetation cover communities: Low sage, big mountain sage and aspen. Detailed, heavily replicated analyses were conducted for unsaturated hydraulic conductivity, sorptivity water drop penetration time and static soil-water-air contact angle. The results show that the severity and presence of surface soil water repellency were considerably reduced six years after fire and that hydraulic conductivity increased significantly in each vegetation cover compared to pre-burn condition. Comparisons among soil hydrological properties shows that hydraulic conductivity is not strongly related to SWR, and that sorptivity is negatively correlated with SWR. The spatial variance of hydraulic properties within the burned high sage and low sage, in particularly, spatial variability of hydraulic conductivity is basically controlled by soil texture and sorptivity is affected by soil wettability. The average water repellency in Low Sage area was significantly different with Big Sage and Aspen as the gap of organic content between Low Sage and other vegetation area. The result of contact angle measurement and organic content analysis shows a strong positive correlation between SWR and organic matter.

Sorptive and desorptive fractionation of dissolved organic matter by mineral soil matrices.

PubMed

Oren, Adi; Chefetz, Benny

2012-01-01

Interactions of dissolved organic matter (DOM) with soil minerals, such as metal oxides and clays, involve various sorption mechanisms and may lead to sorptive fractionation of certain organic moieties. While sorption of DOM to soil minerals typically involves a degree of irreversibility, it is unclear which structural components of DOM correspond to the irreversibly bound fraction and which factors may be considered determinants. To assist in elucidating that, the current study aimed at investigating fractionation of DOM during sorption and desorption processes in soil. Batch DOM sorption and desorption experiments were conducted with organic matter poor, alkaline soils. Fourier-transform infrared (FTIR) and UV-Vis spectroscopy were used to analyze bulk DOM, sorbed DOM, and desorbed DOM fractions. Sorptive fractionation resulted mainly from the preferential uptake of aromatic, carboxylic, and phenolic moieties of DOM. Soil metal-oxide content positively affected DOM sorption and binding of some specific carboxylate and phenolate functional groups. Desorptive fractionation of DOM was expressed by the irreversible-binding nature of some carboxylic moieties, whereas other bound carboxylic moieties were readily desorbed. Inner-sphere, as opposed to outer-sphere, ligand-exchange complexation mechanisms may be responsible for these irreversible, as opposed to reversible, interactions, respectively. The interaction of aliphatic DOM constituents with soil, presumably through weak van der Waals forces, was minor and increased with increasing proportion of clay minerals in the soil. Revealing the nature of DOM-fractionation processes is of great importance to understanding carbon stabilization mechanisms in soils, as well as the overall fate of contaminants that might be associated with DOM. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

Evaluation of Antioxidant Activity and Growth Control Properties of Nonoscale Structure Produced from Aloe vera var. littoralis Extract on Clinical Isolates of Salmonella.

PubMed

Ranjbar, Reza; Arjomandzadegan, Mohammad; Hosseiny, Hossein

2017-07-31

The aim of the study was to examine antibacterial properties of microemulsion structure produced from Aloe vera var. littoralis extract as a new tool of nanoscale drug-like materials. Aloe vera var. littoralis ( A. littoralis ) extract was prepared by distillation method. A nonocarrier structure in the microemulsion system was prepared from the extract. Serial concentrations were prepared from 8 mg/mL extract and the nonocarrier containing 0.1 mg/mL pure extract and were evaluated by a disk diffusion method for 35 Salmonella clinical isolates. Minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) were determined by microbroth dilution assay using MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) method by an enzyme-linked immunosorbent assay(ELISA) Microplate Reader apparatus. Antioxidant activity of the extract was determined by measuring the ferric reducing ability of plasma (FRAP) assay. From 35 clinical isolates of Salmonella , 17 isolates-including resistant isolates of S.E.1103 and S.E.49-had a zone of inhibition (ZI) of 7 to 32 mm in 0.007 mg/mL of the extract. S.E.76 isolate exposed to 30 µg/mL ceftazidime disk had a ZI of 12 mm but had 10 mm in 7µg/mL of A. littoralis extract. The inhibitory effect of a nanocarrier at a concentration of 25 µg/mL by 20 mm ZI was comparable by the ceftazidime (30 µg/mL) effect. MIC 50 was 0.25 mg/mL and MBC 50 was 0.5 mg/mL by MTT method for the extract. It was shown that A.littoralis extract had antioxidant activity of 31.67 µM/mg that could be increased based on concentration. It was concluded that the nanocarrier had a significant effect on the studied isolates in comparison with ordinary antibiotics and had potential for use as a natural antioxidant and antimicrobial material in complementary medicine.

Imaging of the CO snow line in a solar nebula analog.

PubMed

Qi, Chunhua; Öberg, Karin I; Wilner, David J; D'Alessio, Paola; Bergin, Edwin; Andrews, Sean M; Blake, Geoffrey A; Hogerheijde, Michiel R; van Dishoeck, Ewine F

2013-08-09

Planets form in the disks around young stars. Their formation efficiency and composition are intimately linked to the protoplanetary disk locations of "snow lines" of abundant volatiles. We present chemical imaging of the carbon monoxide (CO) snow line in the disk around TW Hya, an analog of the solar nebula, using high spatial and spectral resolution Atacama Large Millimeter/Submillimeter Array observations of diazenylium (N2H(+)), a reactive ion present in large abundance only where CO is frozen out. The N2H(+) emission is distributed in a large ring, with an inner radius that matches CO snow line model predictions. The extracted CO snow line radius of ~30 astronomical units helps to assess models of the formation dynamics of the solar system, when combined with measurements of the bulk composition of planets and comets.

Sorption characteristics of organic compounds on hexadecyltrimethylammonium-smectite

USGS Publications Warehouse

Boyd, Stephen A.; Mortland, Max M.; Chiou, Cary T.

1988-01-01

When hexadedyltrimethylammonium (HDTMA) ion is exchanged for metal cations like calcium in smectite, the sorptive properties of the clay are greatly modified. The resultant HDTMA-smectite complex behaves as a dual sorbent, in the sorption of organic compounds, in which the mineral fraction functions as a solid adsorbent and the organic (HDTMA) phase as a partition medium. Capacities of mineral adsorption and partition uptake by HDTMA in the HDTMA-smectites are illustrated by sorption of benzene, trichloroethene (TCE), and water as vapors on the dry sample and by sorption of benzene and TCE from water. The exchanged HDTMA in clay is found to be a much more powerful partition medium than ordinary soil organic matter in the uptake of benzene and TCE. Based on this finding, HDTMA-smectite appears to be an effective sorbent for removing organic contaminants from water. It is suggested that such sorptive organo-clay complexes could be used to enhance the containment capabilities of clay landfill liners and bentonite slurry walls.

Removal of natural hormones in dairy farm wastewater using reactive and sorptive materials.

PubMed

Cai, Kai; Phillips, Debra H; Elliott, Christopher T; Muller, Marc; Scippo, Marie-Louise; Connolly, Lisa

2013-09-01

The objective of this study was to examine the oestrogen and androgen hormone removal efficiency of reactive (Connelly zero-valent iron (ZVI), Gotthart Maier ZVI) and sorptive (AquaSorb 101 granular activated carbon (GAC) and OrganoLoc PM-100 organoclay (OC)) materials from HPLC grade water and constructed wetland system (CWS) treated dairy farm wastewater. Batch test studies were performed and hormone concentration analysis carried out using highly sensitive reporter gene assays (RGAs). The results showed that hormonal interaction with these materials is selective for individual classes of hormones. Connelly ZVI and AquaSorb 101 GAC were more efficient in removing testosterone (Te) than 17β-estradiol (E2) and showed faster removal rates of oestrogen and androgen than the other materials. Gotthart Maier ZVI was more efficient in removing E2 than Te. OrganoLoc PM-100 OC achieved the lowest final concentration of E2 equivalent (EEQ) and provided maximum removal of both oestrogens and androgens. Copyright © 2013 Elsevier B.V. All rights reserved.

Combined Mini-Cylex & Disk Acceleration Tests in Type K Copper.

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

Maines, Warren Russell; Kittell, David E.; Hobbs, Michael L.

We combined the miniature cylinder expansion test (Mini-Cylex), with the Disk Acceleration Test (DAX) using Type K copper, Picatinny Liquid Explosive, and photonic Doppler velocimetry. We estimated the CJ state using plate reverberation methods at the test cap. We extracted velocities at 2, 7, and 10 volume expansions to fit Jones-Wilkins-Lee Equation of State at the tube wall. And we estimated Gurney velocity both at the test cap and tube wall. Our experiments and simulations are within expected uncertainty. The test and the analysis effectively reduce costs while keeping similar fidelity compared with more expensive tests.

Powdered activated carbons as effective phases for bar adsorptive micro-extraction (BAμE) to monitor levels of triazinic herbicides in environmental water matrices.

PubMed

Neng, N R; Mestre, A S; Carvalho, A P; Nogueira, J M F

2011-02-15

Bar adsorptive micro-extraction using three powdered activated carbons (ACs) as adsorbent phases followed by liquid desorption and high performance liquid chromatography with diode array detection (BAμE(ACs)-LD/HPLC-DAD), was developed to monitor triazinic herbicides (atrazine, simazine and terbutylazine) in environmental water matrices. ACs used present apparent surface areas around 1000 m(2) g(-1) with an important mesoporous volume and distinct surface chemistry characteristics (pH(PZC) ranging from 6.5 to 10.4). The textural and surface chemistry properties of the ACs adsorbent phases were correlated with the analytical data for a better understanding of the overall enrichment process. Assays performed on 10 mL water samples spiked at the 10.0 μg L(-1) levels under optimized experimental conditions yielded recoveries around 100% for the three herbicides under study. The analytical performance showed good precision (RSD<15.0%), convenient detection limits (≈0.1 μg L(-1)) and suitable linearity (1.0-12.0 μg L(-1)) with good correlation coefficients (r(2)>0.9914). By using the standard addition method, the application of the present method on real water matrices, such as surface water and wastewater, allowed very good performances at the trace level. The proposed methodology proved to be a suitable sorptive extraction alternative for the analysis of priority pollutants with polar characteristics, showing to be easy to implement, reliable, sensitive and requiring a low sample volume to monitor triazinic compounds in water matrices. Copyright © 2010 Elsevier B.V. All rights reserved.

Multicriteria decision analysis in ranking of analytical procedures for aldrin determination in water.

PubMed

Tobiszewski, Marek; Orłowski, Aleksander

2015-03-27

The study presents the possibility of multi-criteria decision analysis (MCDA) application when choosing analytical procedures with low environmental impact. A type of MCDA, Preference Ranking Organization Method for Enrichment Evaluations (PROMETHEE), was chosen as versatile tool that meets all the analytical chemists--decision makers requirements. Twenty five analytical procedures for aldrin determination in water samples (as an example) were selected as input alternatives to MCDA analysis. Nine different criteria describing the alternatives were chosen from different groups--metrological, economical and the most importantly--environmental impact. The weights for each criterion were obtained from questionnaires that were sent to experts, giving three different scenarios for MCDA results. The results of analysis show that PROMETHEE is very promising tool to choose the analytical procedure with respect to its greenness. The rankings for all three scenarios placed solid phase microextraction and liquid phase microextraction--based procedures high, while liquid-liquid extraction, solid phase extraction and stir bar sorptive extraction--based procedures were placed low in the ranking. The results show that although some of the experts do not intentionally choose green analytical chemistry procedures, their MCDA choice is in accordance with green chemistry principles. The PROMETHEE ranking results were compared with more widely accepted green analytical chemistry tools--NEMI and Eco-Scale. As PROMETHEE involved more different factors than NEMI, the assessment results were only weakly correlated. Oppositely, the results of Eco-Scale assessment were well-correlated as both methodologies involved similar criteria of assessment. Copyright © 2015 Elsevier B.V. All rights reserved.

Pharmacological evaluation of Musa seminifera Lour. fruit.

PubMed

Saha, Sanjib; Hossain, Faroque; Anisuzzman, Md; Islam, Md Khirul

2013-07-01

To study potential antioxidant, analgesic, antidiarrheal, and antibacterial activities of the ethanol extract of Musa seminifera Lour. fruit in different established in vivo and in vitro experimental models. In vitro antioxidant activity was studied in 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging assay. Phenolic content was determined using Folin-Ciocalteu's reagent. Reducing ability was evaluated by ferric reducing power assay. Peripherally and centrally acting analgesic activity was studied in three different in vivo models, namely, acetic acid-induced writhing, hot-plate test, and tail-flick test in Swiss albino mice. In vivo antidiarrheal activity was evaluated in castor oil- and magnesium sulfate-induced diarrhea in mice. Gastrointestinal motility test was also carried out in mice. All studies in mice were undertaken at the doses of 250 and 500 mg/kg body weight. Antibacterial activity was assessed by disk diffusion assay against some Gram-positive and Gram-negative bacterial strains. Acute toxicity test was conducted to assess the safe doses of the extract. The extract showed 50% inhibitory concentration value of 12.65 μg/mL in DPPH radical-scavenging assay. Phenolic content was found to be 589.83 mg gallic acid equivalent per 100 g of dried fruits extract. Reducing power was in a concentration-dependent manner, and strongly comparable with the standard ascorbic acid. The extract demonstrated significant inhibition of writhing in acetic acid-induced writhing test at both dose levels (P<0.01). The extract also raised pain threshold in both hot-plate and tail-flick test in a dose-dependent manner, and the results were statistically significant (P<0.01). The extract significantly (P<0.01) increased latent period, and decreased defecation in both castor oil- and magnesium sulfate-induced diarrhea. The extract also decreased gastrointestinal motility in mice. In disk diffusion assay, the extract showed potential antibacterial activity against all the tested bacterial strains. The results suggest that the ethanol extract of M. seminifera fruit has potential antioxidant, analgesic, antidiarrheal, and antibacterial activities.

Disk Rock Cutting Tool for the Implementation of Resource-Saving Technologies of Mining of Solid Minerals

NASA Astrophysics Data System (ADS)

Manietyev, Leonid; Khoreshok, Aleksey; Tsekhin, Alexander; Borisov, Andrey

2017-11-01

The directions of a resource and energy saving when creating a boom-type effectors of roadheaders of selective action with disc rock cutting tools on a multi-faceted prisms for the destruction of formation of minerals and rocks pricemax are presented. Justified reversing the modes of the crowns and booms to improve the efficiency of mining works. Parameters of destruction of coal and rock faces by the disk tool of a biconical design with the unified fastening knots to many-sided prisms on effectors of extraction mining machines are determined. Parameters of tension of the interfaced elements of knots of fastening of the disk tool at static interaction with the destroyed face of rocks are set. The technical solutions containing the constructive and kinematic communications realizing counter and reverse mode of rotation of two radial crowns with the disk tool on trihedral prisms and cases of booms with the disk tool on tetrahedral prisms in internal space between two axial crowns with the cutter are proposed. Reserves of expansion of the front of loading outside a table of a feeder of the roadheader of selective action, including side zones in which loading corridors by blades of trihedral prisms in internal space between two radial crowns are created are revealed.

A male-predominant cuticular hydrocarbon, 7-methyltricosane, is used as a contact pheromone in the western flower thrips Frankliniella occidentalis.

PubMed

Olaniran, Oladele A; Sudhakar, Akella V S; Drijfhout, Falko P; Dublon, Ian A N; Hall, David R; Hamilton, James G C; Kirk, William D J

2013-04-01

In a laboratory bioassay, adult female Frankliniella occidentalis (Pergande) (Thysanoptera: Thripidae) spent more time near filter paper disks that had been exposed to adult males than near unexposed disks; this effect was not observed on disks exposed to adult females. The response could only partly be explained by the known male-produced aggregation pheromone, neryl (S)-2-methylbutanoate, suggesting the presence of an unknown male-produced compound. In gas chromatography/mass spectrometry analyses, 7-methyltricosane was detected on disks exposed to males, but not on disks exposed to females. Extracts of cuticular lipids also showed relatively large amounts of 7-methyltricosane on males, whereas only trace amounts were found on females and none on larvae. Bioassays of synthetic 7-methyltricosane showed that adults responded only after contact. The response to this compound was clearly different from that to n-tricosane or hexane-only controls. Females that contacted 7-methyltricosane on glass beads stayed in the vicinity and frequently raised the abdomen, a behavior that rejects mating attempts by males. Males stayed in the vicinity and wagged the abdomen sideways, a behavior used in fighting between males. This is the first identification of a contact pheromone in the order Thysanoptera.

Bioactivity of Y2O3 and CeO2 doped SiO2-SrO-Na2O glass-ceramics.

PubMed

Placek, L M; Keenan, T J; Wren, A W

2016-08-01

The bioactivity of yttrium and cerium are investigated when substituted for Sodium (Na) in a 0.52SiO2-0.24SrO-0.24-xNa2O-xMO glass-ceramics (where x = 0.08 and MO = Y2O3 or CeO2). Bioactivity is monitored through pH and inductively coupled plasma-optical emission spectrometry where pH of simulated body fluid ranged from 7.5 to 7.6 and increased between 8.2 and 10.0 after 14-day incubation with the glass-ceramic disks. Calcium (Ca) and phosphorus (P) levels in simulated body fluid after incubation with yttrium and cerium containing disks show a continual decline over the 14-day period. In contrast, Con disks (not containing yttrium or cerium) caused the elimination of Ca in solution after 1 day and throughout the incubation period, and initially showed a decline in P levels followed by an increase at 14 days. Scanning electron microscopy and energy dispersive spectroscopy confirmed the presence of Ca and P on the surface of the simulated body fluid-incubated disks and showed precipitates on Con and HCe (8 mol% cerium) samples. Cell viability of MC3T3 osteoblasts was not significantly affected at a 9% extract concentration. Optical microscopy after 24 h cell incubation with disks showed that Con samples do not support osteoblast or Schwann cell growth, while all yttrium and cerium containing disks have direct contact with osteoblasts spread across the wells. Schwann cells attached in all wells, but only showed spreading with the HY-S (8 mol% yttrium, heated to sintering temperature) and YCe (4 mol% yttrium and cerium) disks. Scanning electron microscopy of the compatible disks shows osteoblast and sNF96.2 Schwann cells attachment and spreading directly on the disk surfaces. © The Author(s) 2016.

A KINETIC MODEL FOR CELL DENSITY DEPENDENT BACTERIAL TRANSPORT IN POROUS MEDIA

EPA Science Inventory

A kinetic transport model with the ability to account for variations in cell density of the aqueous and solid phases was developed for bacteria in porous media. Sorption kinetics in the advective-dispersive-sorptive equation was described by assuming that adsorption was proportio...

Isosurface Extraction in Time-Varying Fields Using a Temporal Hierarchical Index Tree

NASA Technical Reports Server (NTRS)

Shen, Han-Wei; Gerald-Yamasaki, Michael (Technical Monitor)

1998-01-01

Many high-performance isosurface extraction algorithms have been proposed in the past several years as a result of intensive research efforts. When applying these algorithms to large-scale time-varying fields, the storage overhead incurred from storing the search index often becomes overwhelming. this paper proposes an algorithm for locating isosurface cells in time-varying fields. We devise a new data structure, called Temporal Hierarchical Index Tree, which utilizes the temporal coherence that exists in a time-varying field and adoptively coalesces the cells' extreme values over time; the resulting extreme values are then used to create the isosurface cell search index. For a typical time-varying scalar data set, not only does this temporal hierarchical index tree require much less storage space, but also the amount of I/O required to access the indices from the disk at different time steps is substantially reduced. We illustrate the utility and speed of our algorithm with data from several large-scale time-varying CID simulations. Our algorithm can achieve more than 80% of disk-space savings when compared with the existing techniques, while the isosurface extraction time is nearly optimal.

A review of surface-water sediment fractions and their interactions with persistent manmade organic compounds

USGS Publications Warehouse

Witkowski, P.J.; Smith, J.A.; Fusillo, T.V.; Chiou, C.T.

1987-01-01

This paper reviews the suspended and surficial sediment fractions and their interactions with manmade organic compounds. The objective of this review is to isolate and describe those contaminant and sediment properties that contribute to the persistence of organic compounds in surface-water systems. Most persistent, nonionic organic contaminants, such as the chlorinated insecticides and polychlorinated biphenyls (PCBs), are characterized by low water solubilities and high octanol-water partition coefficients. Consequently, sorptive interactions are the primary transformation processes that control their environmental behavior. For nonionic organic compounds, sorption is primarily attributed to the partitioning of an organic contaminant between a water phase and an organic phase. Partitioning processes play a central role in the uptake and release of contaminants by sediment organic matter and in the bioconcentration of contaminants by aquatic organisms. Chemically isolated sediment fractions show that organic matter is the primary determinant of the sorptive capacity exhibited by sediment. Humic substances, as dissolved organic matter, contribute a number of functions to the processes cycling organic contaminants. They alter the rate of transformation of contaminants, enhance apparent water solubility, and increase the carrying capacity of the water column beyond the solubility limits of the contaminant. As a component of sediment particles, humic substances, through sorptive interactions, serve as vectors for the hydrodynamic transport of organic contaminants. The capabilities of the humic substances stem in part from their polyfunctional chemical composition and also from their ability to exist in solution as dissolved species, flocculated aggregates, surface coatings, and colloidal organomineral and organometal complexes. The transport properties of manmade organic compounds have been investigated by field studies and laboratory experiments that examine the sorption of contaminants by different sediment size fractions. Field studies indicate that organic contaminants tend to sorb more to fine-grained sediment, and this correlates significantly with sediment organic matter content. Laboratory experiments have extended the field studies to a wider spectrum of natural particulates and anthropogenic compounds. Quantitation of isotherm results allows the comparison of different sediment sorbents as well as the estimation of field partition coefficients from laboratory-measured sediment and contaminant properties. Detailed analyses made on the basis of particle-size classes show that all sediment fractions need to be considered in evaluating the fate and distribution of manmade organic compounds. This conclusion is based on observations from field studies and on the variety of natural organic sorbents that demonstrate sorptive capabilities in laboratory isotherm experiments.

Solventless and solvent-minimized sample preparation techniques for determining currently used pesticides in water samples: a review.

PubMed

Tankiewicz, Maciej; Fenik, Jolanta; Biziuk, Marek

2011-10-30

The intensification of agriculture means that increasing amounts of toxic organic and inorganic compounds are entering the environment. The pesticides generally applied nowadays are regarded as some of the most dangerous contaminants of the environment. Their presence in the environment, especially in water, is hazardous because they cause human beings to become more susceptible to disease. For these reasons, it is essential to monitor pesticide residues in the environment with the aid of all accessible analytical methods. The analysis of samples for the presence of pesticides is problematic, because of the laborious and time-consuming operations involved in preparing samples for analysis, which themselves may be a source of additional contaminations and errors. To date, it has been standard practice to use large quantities of organic solvents in the sample preparation process; but as these solvents are themselves hazardous, solventless and solvent-minimized techniques are coming into use. This paper discusses the most commonly used over the last 15 years sample preparation techniques for monitoring organophosphorus and organonitrogen pesticides residue in water samples. Furthermore, a significant trend in sample preparation, in accordance with the principles of 'Green Chemistry' is the simplification, miniaturization and automation of analytical techniques. In view of this aspect, several novel techniques are being developed in order to reduce the analysis step, increase the sample throughput and to improve the quality and the sensitivity of analytical methods. The paper describes extraction techniques requiring the use of solvents - liquid-liquid extraction (LLE) and its modifications, membrane extraction techniques, hollow fibre-protected two-phase solvent microextraction, liquid phase microextraction based on the solidification of a floating organic drop (LPME-SFO), solid-phase extraction (SPE) and single-drop microextraction (SDME) - as well as solvent-free techniques - solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The advantages and drawbacks of these techniques are also discussed, and some solutions to their limitations are proposed. Copyright © 2011 Elsevier B.V. All rights reserved.

Homarine as a feeding deterrent in common shallow-water antarctic lamellarian gastropodMarseniopsis mollis: A rare example of chemical defense in a marine prosobranch.

PubMed

McClintock, J B; Baker, B J; Hamann, M T; Yoshida, W; Slattery, M; Heine, J N; Bryan, P J; Jayatilake, G S; Moon, B H

1994-10-01

The common bright yellow antarctic lamellarian gastropodMarseniopsis mollis was examined for the presence of defensive chemistry. Proton nuclear magnetic resonance (NMR) spectroscopy indicated that a major component of ethanolic extracts purified by reversed-phase column chromatography was homarine. Further high-performance liquid chromatography (HPLC) analysis of the mantle, foot, and viscera verified the presence of homarine in all body tissues at concentrations ranging from 6 to 24 mg/g dry tissue. A conspicuous macroinvertebrate predator of the shallow antarctic benthos, the sea starOdontaster validus, always rejected live individuals ofM. mollis, while readily feeding on pieces of fish tail muscle. Filter paper disks treated with shrimp elicited a broad range of feeding behaviors in the sea starO. validus (movement of disc to mouth, extrusion of cardiac stomach, humped feeding posture). Shrimp disks treated with homarine (0.4 and 4 mg/disk) were rejected byO. validus significantly more frequently than control disks treated with solvent carrier and shrimp or shrimp alone. The highest concentration of homarine tested not only caused feeding deterrence, but in several sea stars a flight response was noted. Homarine was not detected in the tunic of the antarctic ascidianCnemidocarpa verrucosa, a presumed primary prey ofM. mollis. Nonetheless, crude extracts of the epizooites that foul the tunic (primarily the bryozoans and hydroids) contain homarine, suggestingM. mollis may ingest and derive its chemistry from these organisms. This appears to be only the third example of chemical defense in a member of the Order Mesogastropoda. As the vestigial internalized shell ofM. mollis is considered a primitive condition, the findings of this study lend support to the hypothesis that chemical defense evolved prior to shell loss in shell-less gastropods.

Antibacterial efficacy of the seed extracts of Melia azedarach against some hospital isolated human pathogenic bacterial strains

PubMed Central

Khan, Abdul Viqar; Ahmed, Qamar Uddin; Mir, M Ramzan; Shukla, Indu; Khan, Athar Ali

2011-01-01

Objective To investigate the antibacterial potential of the polar and non-polar extracts of the seeds of Melia azedarach (M. azedarach) L. (Meliaceae) against eighteen hospital isolated human pathogenic bacterial strains. Methods Petrol, benzene, ethyl acetate, methanol, and aqueous extracts at five different concentrations (1, 2, 5, 10 and 15 mg/mL) were evaluated. Disk diffusion method was followed to evaluate the antibacterial efficacy. Results All extracts of the seeds demonstrated significant antibacterial activity against tested pathogens. Among all extracts, ethyl acetate extract revealed the highest inhibition comparatively. The present study also favored the traditional uses reported earlier. Conclusions Results of this study strongly confirm that the seed extracts of M. azedarach could be effective antibiotics, both in controlling gram-positive and gram-negative human pathogenic infections. PMID:23569812

Phytosynthesis of Silver Nanoparticles Using Myrtus communis L. Leaf Extract and Investigation of Bactericidal Activity

NASA Astrophysics Data System (ADS)

Ajdari, M. R.; Tondro, G. H.; Sattarahmady, N.; Parsa, A.; Heli, H.

2017-12-01

Silver nanoparticles have been synthesized using only Myrtus communis L. leaf extract by a facile procedure without other reagents. The extract played the roles of both reducing and capping agent. The nanoparticles were characterized using field-emission scanning microscopy, and remained stable for at least 3 weeks. Antibacterial activity of the nanoparticles was evaluated toward Escherichia coli, Bacillus subtilis, Pseudomonas aeruginosa, Staphylococcus aureus, methicillin-resistant Staphylococcus aureus, and Enterococcus faecalis based on inhibition zone disk diffusion assays. The minimum inhibitory and bactericidal concentrations of the nanoparticles were obtained. Mechanisms for the antibacterial activity were proposed.

COMPARISON OF SORPTION ENERGTICS FOR HYDROPHOBIC ORGANIC CHEMICALS BY SYNTHETIC AND NATURAL SORBENTS FROM METHANOL/WATER SOLVENT MIXTURES

EPA Science Inventory

Reversed-phase liquid chromatography (RPLC) was used to investigate the thermodynamics and mechanisms of hydrophobic organic chemical (HOC) retention from methanol/water solvent mixtures. The enthalpy-entropy compensation model was used to infer that the hydro- phobic sorptive me...

Trace contaminant adsorption and sorbent regeneration in closed ecological systems

NASA Technical Reports Server (NTRS)

Arnold, C. R.; Kersels, G. J.; Merrill, R. P.; Robell, A. J.; Wheeler, A.

1972-01-01

Correlation was obtained for determining sorptive capacity of carbon for pure and mixed contaminants under dry and humid conditions at various temperatures. Vacuum desorption rates were investigated for single particles and for sorbent beds. For sorbent beds, rate-determining step is Knudsen diffusion through interparticle voids.

Sampling for silver nanoparticles in aqueous media using a rotating disk electrode: evidence for selective sampling of silver nanoparticles in the presence of ionic silver.

PubMed

Steinberg, Spencer; Hodge, Vernon; Schumacher, Brian; Sovocool, Wayne

2017-03-01

Amendment of a carbon paste electrode consisting of graphite and Nujol®, with a variety of organic and inorganic materials, allows direct adsorption of silver nanoparticles (AgNPs) from aqueous solution in either open or close circuit modes. The adsorbed AgNPs are detected by stripping voltammetry. Detection limits of less than 1 ppb Ag are achievable with a rotating disk system. More than one silver peak was apparent in many of the stripping voltammograms. The appearance of multiple peaks could be due to different species of silver formed upon stripping or variation in the state of aggregation or size of nanoparticles. With most of these packing materials, dissolved Ag + was also extracted from aqueous solution, but, with a packing material made with Fe(II,III) oxide nanoparticles, only AgNPs were extracted. Therefore, it is the best candidate for determination of metallic AgNPs in aqueous environmental samples without interference from Ag + .

Evidence of Spin and Energy Extraction in a Galactic Black Hole Candidate: The XMM-NEWTON/EPIC SPECTRUM of XTE 11650-500

NASA Technical Reports Server (NTRS)

Miller, J. M.; Fabian, A. C.; Wunands, R.; Reynolds, C. S.; Ehle, M.; Freyberg, M. J.; VanDerKlis, M.; Lewin, W. H. G.; Sanchez-Fernandez, C.; Castro-Tirado, A. J.

2002-01-01

We observed the Galactic black hole candidate XTE J1650-500 early in its fall of 2001 outburst with the XMM-Newton European Photon Imaging pn Camera (EPIC-pn). The observed spectrum is consistent with the source having been in the very high state. We h d a broad, skewed Fe Kar emission line that suggests the primary in this system may be a Kerr black hole and that indicates a steep disk emissivity profile that is hard to explain in terms of a standard accretion disk model. These results are quantitatively and qualitatively similar to those from an XMM-Newton observation of the Seyfert galaxy MCG -6-30-15. The steep emissivity in MCG -6-30-15 may be explained by the extraction and dissipation of rotational energy from a black hole with nearly maximal angular momentum or from material in the plunging region via magnetic connections to the inner accretion disk. If this process is at work in both sources, an exotic but fundamental general relativistic prediction may be confirmed across a factor of l0(exp 6) in black hole mass. We discuss these results in terms of the accretion flow geometry in stellar-mass black holes and the variety of enigmatic phenomena often observed in the very high state.

Barbell-shaped stir bar sorptive extraction using dummy template molecularly imprinted polymer coatings for analysis of bisphenol A in water.

PubMed

Liu, Ruimei; Feng, Feng; Chen, Guolin; Liu, Zhimin; Xu, Zhigang

2016-07-01

This study reports the development of a novel dummy template molecularly imprinted polymer (MIP)-coated barbell-shaped stir bar. The MIP stir bar coatings were prepared by using 2,2-bis(4-hydroxyphenyl)butane (BPB), 4,4'-dihydroxydiphenylmethane (BPF), 4-tert-butylphenol (PTBP), and tetrabromobisphenol A (TBBA) as dummy templates using a capillary in situ polymerization method. Uniform coatings can be prepared controllably. The method is simple, easy, and reproducible. The barbell-shaped stir bar was developed by using medical silicone tubes as wheels. The wheels could be removed and reinstalled when necessary; therefore, the barbell-shaped stir bar was easy to disassemble and reassemble. The novel MIP-coated stir bar showed good selectivity for the target analyte, bisphenol A (BPA). The established method is selective and sensitive with a lower detection limit for BPA of 0.003 μg/L. The dummy template MIP-coated stir bar is suitable for trace BPA analysis in real environmental water samples without template leakage. The novel stir bar can be used at least 100 times.

Comprehensive authentication of (E)-alpha(beta)-ionone from raspberries, using constant flow MDGC-C/P-IRMS and enantio-MDGC-MS.

PubMed

Sewenig, Sabine; Bullinger, Dino; Hener, Uwe; Mosandl, Armin

2005-02-23

A new coupling system of GC-GC, connected via a Multi Column Switching Device MCS2 for measuring isotope ratios, is introduced. By means of several standard substances the precise and accurate measurement of isotopic values is proved. First applications concerning the authentication of raspberry aroma compounds are established. Consequently, the combination of constant flow multidimensional gas chromatography-combustion/pyrolysis-isotope ratio mass spectrometry (MDGC-C/P-IRMS) is applied to the authenticity assessment of (E)-alpha(beta)-ionone from six different raspberry cultivars. Furthermore, 12 commercially available raspberry products and samples of (E)-alpha(beta)-ionone, some declared to be natural, are investigated. delta(2)Eta(V)(-)(SMOW) and delta(13)C(V)(-)(PDB) values of (E)-alpha(beta)-ionone are determined, and characteristic authenticity ranges were concluded from raspberries by correlation of both delta(2)Eta(V)(-)(SMOW) and delta(13)C( V)(-)(PDB) values. The results are correlated with the determination of enantiomeric purities of (E)-alpha-ionone, using stir bar sorptive extraction enantio-multidimensional gas chromatography mass spectrometry (SBSE-enantio-MDGC-MS).

A new validated analytical method for the determination of tributyltin in water samples at the quantification level set by the European Union.

PubMed

Devos, Christophe; David, Frank; Sandra, Pat

2012-10-26

According to recent directives of the European Union (EU), limits of quantification (LOQ) for the determination of tributyltin (TBT) in surface waters should be ca. 60 pg/L (ppq). This put very stringent requirements on analytical methodologies; definitely when they have to be applied in a routine environment. Stir bar sorptive extraction (SBSE), followed by thermal desorption (TD) and capillary gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) can provide accurate and precise data at the 2 ng/L level (ppt). For lower concentrations, matrix and reagent interferences together with contamination may provide too high TBT values. A two-dimensional heart-cut GC method was developed to fractionate TBT from interferences. The GC-GC-MS/MS method shows excellent linearity in the range 50 pg/L-4 ng/L, good repeatability (RSD<20% at 200 pg/L), and a limit of detection of 11 pg/L. The method performance is demonstrated with representative samples i.e. harbor water and waste water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of inductively coupled plasma surface treatment on silica gel and mesoporous MCM-41 particles

NASA Astrophysics Data System (ADS)

J, A. JUAREZ-MORENO; U, CHACON-ARGAEZ; J, BARRON-ZAMBRANO; C, CARRERA-FIGUEIRAS; P, QUINTANA-OWEN; W, TALAVERA-PECH; Y, PEREZ-PADILLA; A, AVILA-ORTEGA

2018-06-01

Silica gel and MCM-41 synthesized mesoporous materials were treated with either oxygen (O2), hexamethyldisiloxane (HMDSO) and organic vapors like ethanol (EtOH), and acrylonitrile (AN) inductive plasma. The radiofrequency power for the modification was fixed to 120 W and 30 min, assuring a high degree of organic ionization energy in the plasma. The surface properties were studied by infrared spectroscopy (FTIR), scanning electron microscopy, x-ray photoelectron spectroscopy and dynamic light scattering technique was used for characterizing size distributions. When the silica and MCM-41 particles were modified by AN and HMDSO plasma gases, the surface morphology of the particles was changed, presenting another color, size or shape. In contrast, the treatments of oxygen and EtOH did not affect the surface morphology of both particles, but increased the oxygen content at the surface bigger than the AN and HMDSO plasma treatments. In this study, we investigated the influence of different plasma treatments on changes in morphology and the chemical composition of the modified particles which render them a possible new adsorbent for utilization in sorptive extraction techniques for polar compounds.

Haloanisole and halophenol contamination in Spanish aged red wines.

PubMed

Copete, M L; Zalacain, A; Lorenzo, C; Carot, J M; Esteve, M D; Climent, M; Salinas, M R

2009-01-01

This is the first study to be carried out on the incidence of halophenols and haloanisoles, including trichloroanisole, in aged red wines. A total of 966 red wines, aged for 6, 12 and 24 months in oak barrels and from different Spanish production areas, were analysed by stir bar sorptive extraction followed by gas chromatography/mass spectrometry (GC/MS). From the wines sampled, 155 (16.1%) were contaminated with one or several compounds, with 7.6, 6.9 and 1.5% corresponding to the 12- (aged-12), 6- (aged-6) and 24-month-aged (aged-24) wines, respectively. The most abundant compounds causing taint were 2,3,4,6-tetrachloroanisole and 2,4,6-trichloroanisol (6.8 and 5.3%, respectively). No 2,4,6-tribromophenol was found in any of the samples. Contamination with halo compounds was highest in samples from South-West Spain, followed by those from Northern Spain. The mean concentration for all compounds were always higher than their respective olfactory threshold, but none of these halo compounds represent a health hazard to humans through the consumption of commercial red aged wines.

Characterization of the Key Aroma Compounds in Chinese Syrah Wine by Gas Chromatography-Olfactometry-Mass Spectrometry and Aroma Reconstitution Studies.

PubMed

Zhao, Pengtao; Gao, Jinxin; Qian, Michael; Li, Hua

2017-06-24

The key aroma compounds and the organoleptic quality of two Chinese Syrah wines from the Yunnan Shangri-La region and Ningxia Helan mountain region were characterized. The most important eighty aroma-active compounds were identified by Gas Chromatography-Olfactometry. In both Syrah samples, ethyl 2-methylpropanoate, ethyl 3-methylbutanoate, 3-methylbutyl acetate, 2- and 3-methyl-1-butanol, ethyl hexanoate, ethyl octanoate, 2-phenethyl acetate, methional, 3-methylbutanoic acid, hexanoic acid, octanoic acid, β -damascenone, guaiacol, 2-phenylethanol, trans -whiskylactone, 4-ethylguaiacol, eugenol, 4-ethylphenol, and sotolon were detected to have the highest odor intensities. In the chemical analysis, 72 compounds were quantitated by Stir Bar Sorptive Extraction combined with Gas Chromatography Mass Spectrometry. Based on the Odor Activity Value (OAV), the aromas were reconstituted by combining aroma compounds in the synthetic wine, and sensory descriptive analysis was used to verify the chemical data. Fatty acid ethyl esters, acetate esters, and β -damascenone were found with higher OAVs in the more fruity-smelling sample of Helan Mountain rather than Shangri-La.

A disk asymmetry in motion around the B[e] star MWC158

NASA Astrophysics Data System (ADS)

Kluska, J.; Benisty, M.; Soulez, F.; Berger, J.-P.; Le Bouquin, J.-B.; Malbet, F.; Lazareff, B.; Thiébaut, E.

2016-06-01

Context. MWC158 is a star with the B[e] phenomenon that shows strong spectrophotometric variability (in lines and in UV and visible continuum) attributed to phases of shell ejection. The evolutionary stage of this star was never clearly determined. Previous interferometric, spectropolarimetric and spectro-interferometric studies suggest a disk morphology for its environment. Aims: We investigate the origin of the variability within the inner astronomical unit of the central star using near-infrared interferometric observations with PIONIER at the VLTI over a two-year period. Methods: We performed an image reconstruction of the circumstellar environment using the SPARCO method. We discovered that the morphology of the circumstellar environment could vary on timescales of weeks or days. We carried out a parametric fit of the data with a model consisting of a star, a disk and a bright spot that represents a brighter emission in the disk. Results: We detect strong morphological changes in the first astronomical unit around the star, that happen on a timescale of few months. We cannot account for such variability well with a binary model. Our parametric model fits the data well and allows us to extract the location of the asymmetry for different epochs. Conclusions: For the first time, we detect a morphological variability in the environment of MWC158. This variability is reproduced by a model of a disk and a bright spot. The locations of the bright spot suggest that it is located in the disk, but its precise motion is not determined. The origin of the asymmetry in the disk is complex and may be related to asymmetric shell ejections. Based on observations performed with PIONIER mounted on the ESO Very Large Telescope interferometer (programmes: 089.C-0211, 190.C-0963).

CHEMISTRY IN A FORMING PROTOPLANETARY DISK: MAIN ACCRETION PHASE

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

Yoneda, Haruaki; Tsukamoto, Yusuke; Furuya, Kenji

We investigate the chemistry in a radiation-hydrodynamics model of a star-forming core that evolves from a cold (∼10 K) prestellar core to the main accretion phase in ∼10{sup 5} years. A rotationally supported gravitationally unstable disk is formed around a protostar. We extract the temporal variation of physical parameters in ∼1.5 × 10{sup 3} SPH particles that end up in the disk, and perform post-processing calculations of the gas-grain chemistry adopting a three-phase model. Inside the disk, the SPH particles migrate both inward and outward. Since a significant fraction of volatiles such as CO can be trapped in the water-dominant ice inmore » the three-phase model, the ice mantle composition depends not only on the current position in the disk, but also on whether the dust grain has ever experienced higher temperatures than the water sublimation temperature. Stable molecules such as H{sub 2}O, CH{sub 4}, NH{sub 3}, and CH{sub 3}OH are already abundant at the onset of gravitational collapse and are simply sublimated as the fluid parcels migrate inside the water snow line. On the other hand, various molecules such as carbon chains and complex organic molecules (COMs) are formed in the disk. The COMs abundance sensitively depends on the outcomes of photodissociation and diffusion rates of photofragments in bulk ice mantle. As for S-bearing species, H{sub 2}S ice is abundant in the collapse phase. In the warm regions in the disk, H{sub 2}S is sublimated to be destroyed, while SO, H{sub 2}CS, OCS, and SO{sub 2} become abundant.« less

Limited Area Coverage/High Resolution Picture Transmission (LAC/HRPT) data vegetative index calculation processor user's manual

NASA Technical Reports Server (NTRS)

Obrien, S. O. (Principal Investigator)

1980-01-01

The program, LACVIN, calculates vegetative indexes numbers on limited area coverage/high resolution picture transmission data for selected IJ grid sections. The IJ grid sections were previously extracted from the full resolution data tapes and stored on disk files.

Antimycobacterial activity assessment of three ethnobotanical plants against Mycobacterium Tuberculosis: An In Vitro study.

PubMed

Arjomandzadegan, Mohammad; Emami, Navid; Habibi, Ghasem; Farazi, Ali Asghar; Kahbazi, Manijeh; Sarmadian, Hossein; Jabbari, Mansooreh; Hosseini, Hossein; Ramezani, Mona

2016-12-01

Resistances to herbal medicines are still not defined and finding natural remedies against drug resistant Mycobacterium tuberculosis (MTB) has research priority. The antimycobacterial susceptibility method for herbal extracts is unclearly defined and there is no standard method for assessment of the materials against bacteria. In the present study, time kill of three medicinal plants was determined against MTB. The clinical isolate of MTB from a patient who harbored confirmed tuberculosis was used in the study. Aqueous extracts of Aloe vera leaves, mint, and Hypericum perforatum were prepared using reflux distillation. Disk diffusion methods were conducted in Petri dishes and McCartney bottles containing Löwenstein-Jensen medium to measure the sensitivity of plant extracts in serial concentrations of 0.25-8mg/mL. A pour plate method was performed by mixing 0.7mL of each concentration of extract in 5mL Löwenstein-Jensen medium followed by surface culturing of MTB fresh cells. The time kill method was conducted by bacterial suspension in equal amounts of the extract and viable evaluation in fresh culture at the beginning, and at 24-h, 48-h, 72-h, and 1-week intervals. All cultures were incubated at 37°C for 4weeks. Inoculum concentrations were considered as a variable. The zones of inhibition of A. vera, H. perforatum, and mint extracts in the disk diffusion method in McCartney bottles were 60mm, 41mm, and zero, respectively, but Petri dishes did not have repeatable results. In the pour plate method, an extract concentration up to 1mg/mL could inhibit cell growth. In mint extract, colony forming was four times more than the others at 0.5mg/mL. Time kill of 95% of cells occurred when exposed to extracts of A. vera and H. perforatum separately, but was 50% in 24 h and 20% in 10 min. The time kill for mint was 95% in 1week. The results give some scientific basis to the use of plant extracts for growth control of MTB cells. Clinical trials are recommended for assessment of the extract as complementary medicine, as well as for antisepsis. Copyright © 2016.

Evaluation of Antioxidant Activity and Growth Control Properties of Nonoscale Structure Produced from Aloe vera var. littoralis Extract on Clinical Isolates of Salmonella

PubMed Central

Hosseiny, Hossein

2017-01-01

The aim of the study was to examine antibacterial properties of microemulsion structure produced from Aloe vera var. littoralis extract as a new tool of nanoscale drug-like materials. Aloe vera var. littoralis (A. littoralis) extract was prepared by distillation method. A nonocarrier structure in the microemulsion system was prepared from the extract. Serial concentrations were prepared from 8 mg/mL extract and the nonocarrier containing 0.1 mg/mL pure extract and were evaluated by a disk diffusion method for 35 Salmonella clinical isolates. Minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) were determined by microbroth dilution assay using MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) method by an enzyme-linked immunosorbent assay(ELISA) Microplate Reader apparatus. Antioxidant activity of the extract was determined by measuring the ferric reducing ability of plasma (FRAP) assay. From 35 clinical isolates of Salmonella, 17 isolates—including resistant isolates of S.E.1103 and S.E.49—had a zone of inhibition (ZI) of 7 to 32 mm in 0.007 mg/mL of the extract. S.E.76 isolate exposed to 30 µg/mL ceftazidime disk had a ZI of 12 mm but had 10 mm in 7µg/mL of A. littoralis extract. The inhibitory effect of a nanocarrier at a concentration of 25 µg/mL by 20 mm ZI was comparable by the ceftazidime (30 µg/mL) effect. MIC50 was 0.25 mg/mL and MBC50 was 0.5 mg/mL by MTT method for the extract. It was shown that A.littoralis extract had antioxidant activity of 31.67 µM/mg that could be increased based on concentration. It was concluded that the nanocarrier had a significant effect on the studied isolates in comparison with ordinary antibiotics and had potential for use as a natural antioxidant and antimicrobial material in complementary medicine. PMID:28758958

Simultaneous determination of four trace estrogens in feces, leachate, tap and groundwater using solid-liquid extraction/auto solid-phase extraction and high-performance liquid chromatography with fluorescence detection.

PubMed

Liu, Na; Shi, Yue-e; Li, Mengyan; Zhang, Ting-di; Gao, Song

2015-10-01

A simple and selective high-performance liquid chromatography method coupled with fluorescence detection was developed for the simultaneous measurement of trace levels of four estrogens (estrone, estradiol, estriol and 17α-ethynyl estradiol) in environmental matrices. For feces samples, solid-liquid extraction was applied with a 1:1 v/v mixture of acetonitrile and ethyl acetate as the extraction solvent. For liquid samples (e.g., leachate and groundwater), hydrophobic/lipophilic balanced automated solid-phase extraction disks were selected due to their high recoveries compared to conventional C18 disks. Chromatographic separations were performed on a reversed-phase C18 column gradient-eluted with a 45:55 v/v mixture of acetonitrile and water. The detection limits were down to 1.1 × 10(-2) (estrone), 4.11 × 10(-4) (estradiol), 5.2 × 10(-3) (estriol) and 7.18 × 10(-3) μg/L (17α-ethynyl estradiol) at excitation/emission wavelengths of 288/310 nm, with recoveries in the range of 96.9 ± 3.2-105.4 ± 3.2% (n = 3). The method was successfully applied to determine estrogens in feces and water samples collected at livestock farms and a major river in Northeast China. We observed relatively high abundance and widespread distribution of all four estrogens in our sample collections, implying the urgency for a comprehensive and intricate investigation of estrogenic fate and contamination in our researched area. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Morphogenetic variability of faradiol monoesters in marigold Calendula officinalis L.

PubMed

Zitterl-Eglseer, K; Reznicek, G; Jurenitsch, J; Novak, J; Zitterl, W; Franz, C

2001-01-01

The main compounds of lipophilic extracts of flower heads of marigold (Calendula officinalis L.) are triterpendiol esters, mainly faradiol laurate, faradiol myristate and faradiol palmitate. These faradiol-3-O-monoesters have been quantified for the first time by means of reversed phase HPLC with internal standardisation in different parts of C. officinalis plants, namely ray florets, disk florests, involucral bracts, receptacles, levaes and seeds. The amounts of the esters were highest in ray florets, approximately 10 times lower in disk florets than in the ray florets, and approximately 10 times lower in involucral bracts than in the disk florets. In the leaves only traces of the esters could be detected, and in the receptacles no esters could be detected at all. Quantification in the seed was not possible using this method because of interfering fatty compounds. Concerning the faradiol esters, the dried ray and disk florets only should be preferred as primary products for remedies as demanded in the recently published supplement of the Pharmacopoiea Europaea (1999). Breeding work should focus on varieties with a greater number of ray florets in order to improve the quality of herbal medicinal products derived from marigoid.

Exploring Properties of HI Clouds in Dwarf Irregular Galaxies

NASA Astrophysics Data System (ADS)

Berger, Clara; Hunter, Deidre Ann

2018-01-01

Dwarf Irregular galaxies form stars and maintain exponential stellar disks at extremely low gas densities. One proposed method of maintaining such regular outer disks is scattering stars off of HI clouds. In order to understand the processes present in dwarf irregular stellar disks, we present a survey of atomic hydrogen clouds in and around a subset of representative galaxies from the LITTLE THINGS survey. We apply a cloud identification program to the 21 cm HI line emission cubes and extract masses, radii, surface densities, and distances from the center of the galaxy in the plane of the galaxy of each cloud. Our data show a wide range of clouds characterized by low surface densities but varied in mass and size. The number of clouds found and the mass of the most massive cloud show no correlation to integrated star forming rates or luminosity in these galaxies. However, they will be used as input for models of stars scattering off of HI clouds to better understand the regular stellar disks in dwarf Irregular galaxies.We acknowledge support from the National Science Foundation grant AST-1461200 to Northern Arizona University for Research Experiences for Undergraduates summer internships.

Retention of heavy metals by carboxyl functional groups of biochars in small arms range soil

USDA-ARS?s Scientific Manuscript database

Long-term effectiveness of biochar for heavy metal stabilization depends upon biochar’s sorptive property and recalcitrance in soil. To understand the role of carboxyl functional groups on heavy metal stabilization, cottonseed hull biochar and flax shive steam activated biochar having low O/C ratio...

In-situ Subaqueous Capping of Mercury-Contaminated Sediments in a Fresh-Water Aquatic System, Part II-Evaluation of Sorption Materials

EPA Science Inventory

The function and longevity of traditional, passive, isolation caps can be augmented through the use of more chemically active capping materials which have higher sorptive capacities, ideally rendering metals non-bioavailable. In the case of Hg, active caps also mitigate the rate...

Cleaning oil refining drainage waters out of emulsified oil products with thermic treated cedar nut shell

NASA Astrophysics Data System (ADS)

Pyatanova, P. A.; Adeeva, L. N.

2017-08-01

It was elaborated the ability of the sorbent produced by thermic treatment of cedar nut shell to destruct model and real first kind (direct) emulsions in static and dynamic conditions. In static conditions optimal ratio sorbent-emulsion with the original concentration of oil products 800 mg/l was in the range of 2.0 g per 100 ml of emulsion which corresponds to the level of treatment 94.9%. The time of emulsion destruction was 40 minutes. This sorbent is highly active in dynamic processes of oil-contaminated water treatment, the level of treatment 96.0% is being achieved. Full dynamic sorptive capacity of the sorbent is 0.85 g/g. Sorbent based on the thermic treated cedar nut shell can be elaborated as sorptive filter element of local treatment facilities of oil refining and petrochemical processes. After the treatment with this sorbent of drainage waters of oil refinery in dynamic conditions the concentration of oil products became less than mpc on oil products for waste waters coming to biological treatment.

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

Hedman, Matthew M.; Stark, Christopher C., E-mail: mhedman@uidaho.edu, E-mail: cstark@stsci.edu

The appearance of debris disks around distant stars depends upon the scattering/phase function (SPF) of the material in the disk. However, characterizing the SPFs of these extrasolar debris disks is challenging because only a limited range of scattering angles are visible to Earth-based observers. By contrast, Saturn’s tenuous rings can be observed over a much broader range of geometries, so their SPFs can be much better constrained. Since these rings are composed of small particles released from the surfaces of larger bodies, they are reasonable analogs to debris disks and so their SPFs can provide insights into the plausible scatteringmore » properties of debris disks. This work examines two of Saturn’s dusty rings: the G ring (at 167,500 km from Saturn’s center) and the D68 ringlet (at 67,600 km). Using data from the cameras on board the Cassini spacecraft, we are able to estimate the rings’ brightnesses at scattering angles ranging from 170° to 0.°5. We find that both of the rings exhibit extremely strong forward-scattering peaks, but for scattering angles above 60° their brightnesses are nearly constant. These SPFs can be well approximated by a linear combination of three Henyey–Greenstein functions, and are roughly consistent with the SPFs of irregular particles from laboratory measurements. Comparing these data to Fraunhofer and Mie models highlights several challenges involved in extracting information about particle compositions and size distributions from SPFs alone. The SPFs of these rings also indicate that the degree of forward scattering in debris disks may be greatly underestimated.« less

Fatigue Resistance of the Grain Size Transition Zone in a Dual Microstructure Superalloy Disk

NASA Technical Reports Server (NTRS)

Gabb, T. P.; Kantzos, P. T.; Telesman, J.; Gayda, J.; Sudbrack, C. K.; Palsa, B. S.

2010-01-01

Mechanical property requirements vary with location in nickel-based superalloy disks. To maximize the associated mechanical properties, heat treatment methods have been developed for producing tailored microstructures. In this study, a specialized heat treatment method was applied to produce varying grain microstructures from the bore to the rim portions of a powder metallurgy processed nickel-based superalloy disk. The bore of the contoured disk consisted of fine grains to maximize strength and fatigue resistance at lower temperatures. The rim microstructure of the disk consisted of coarse grains for maximum resistance to creep and dwell crack growth at high temperatures up to 704 C. However, the fatigue resistance of the grain size transition zone was unclear, and needed to be evaluated. This zone was located as a band in the disk web between the bore and rim. Specimens were extracted parallel and transverse to the transition zone, and multiple fatigue tests were performed at 427 and 704 C. Mean fatigue lives were lower at 427 C than for 704 C. Specimen failures often initiated at relatively large grains, which failed on crystallographic facets. Grain size distributions were characterized in the specimens, and related to the grains initiating failures as well as location within the transition zone. Fatigue life decreased with increasing maximum grain size. Correspondingly, mean fatigue resistance of the transition zone was slightly higher than that of the rim, but lower than that of the bore. The scatter in limited tests of replicates was comparable for all transition zone locations examined.

RESONANT CLUMPING AND SUBSTRUCTURE IN GALACTIC DISKS

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

Molloy, Matthew; Smith, Martin C.; Shen, Juntai

2015-05-10

We describe a method to extract resonant orbits from N-body simulations, exploiting the fact that they close in frames rotating with a constant pattern speed. Our method is applied to the N-body simulation of the Milky Way by Shen et al. This simulation hosts a massive bar, which drives strong resonances and persistent angular momentum exchange. Resonant orbits are found throughout the disk, both close to the bar and out to the very edges of the disk. Using Fourier spectrograms, we demonstrate that the bar is driving kinematic substructure even in the very outer parts of the disk. We identifymore » two major orbit families in the outskirts of the disk, one of which makes significant contributions to the kinematic landscape, namely, the m:l = 3:−2 family, resonating with the bar. A mechanism is described that produces bimodal distributions of Galactocentric radial velocities at selected azimuths in the outer disk. It occurs as a result of the temporal coherence of particles on the 3:−2 resonant orbits, which causes them to arrive simultaneously at pericenter or apocenter. This resonant clumping, due to the in-phase motion of the particles through their epicycle, leads to both inward and outward moving groups that belong to the same orbital family and consequently produce bimodal radial velocity distributions. This is a possible explanation of the bimodal velocity distributions observed toward the Galactic anticenter by Liu et al. Another consequence is that transient overdensities appear and dissipate (in a symmetric fashion), resulting in a periodic pulsing of the disk’s surface density.« less

Preparation of polydimethylsiloxane/beta-cyclodextrin/divinylbenzene coated "dumbbell-shaped" stir bar and its application to the analysis of polycyclic aromatic hydrocarbons and polycyclic aromatic sulfur heterocycles compounds in lake water and soil by high performance liquid chromatography.

PubMed

Yu, Chunhe; Yao, Zhimin; Hu, Bin

2009-05-08

A "dumbbell-shaped" stir bar was proposed to prevent the friction loss of coating during the stirring process, and thus prolonged the lifetime of stir bars. The effects of the coating components, including polydimethylsiloxane (PDMS), beta-cyclodextrin (beta-CD) and divinylbenzene (DVB) were investigated according to an orthogonal experimental design, using three polycyclic aromatic hydrocarbons (PAHs) and four polycyclic aromatic sulfur heterocycles (PASHs) as model analytes. Four kinds of stir bars coated with PDMS, PDMS/beta-CD, PDMS/DVB and PDMS/beta-CD/DVB were prepared and their extraction efficiencies for the target compounds were compared. It was demonstrated that PDMS/beta-CD/DVB-coated stir bar showed the best affinity to the studied compounds. The preparation reproducibility of PDMS/beta-CD/DVB-coated stir bar ranged from 3.2% to 15.2% (n = 6) in one batch, and 5.2% to 13.4% (n = 6) among batches. The "dumbbell-shaped" stir bar could be used for about 40 times, which were 10 extractions more than a normal stir bar. The prepared PDMS/beta-CD/DVB-coated "dumbbell-shaped" stir bar was used for stir bar sorptive extraction (SBSE) of PAHs and PASHs and the desorbed solution was introduced into HPLC-UV for subsequent analysis. The limits of detection of the proposed method for seven target analytes ranged from 0.007 to 0.103 microg L(-1), the relative standard deviations were in the range of 6.3-12.9% (n = 6, c = 40 microg L(-1)), and the enrichment factors were 19-86. The proposed method was successfully applied to the analysis of seven target analytes in lake water and soil samples.

Soil water repellency of the artificial soil and natural soil in rocky slopes as affected by the drought stress and polyacrylamide.

PubMed

Chen, Zhang; Wang, Ruixin; Han, Pengyuan; Sun, Hailong; Sun, Haifeng; Li, Chengjun; Yang, Lixia

2018-04-01

Soil water repellency (SWR) causes reduced soil water storage, enhanced runoff and reduced ecosystem productivity. Therefore, characterization of SWR is a prerequisite for effective environmental management. SWR has been reported under different soils, land uses and regions of the world, particularly in forest land and after wildfires; however, the understanding of this variable in the artificial soil of rocky slope eco-engineering is still rather limited. This study presented the characterization of SWR in the artificial soil affected by the polyacrylamide (PAM) and drought stress. There were two molecular weights of PAM, and the CK was without PAM application. Three types of soil were studied: natural soil and two types of artificial soil which have been sprayed for 1y and 5y, respectively. The drought stress experiments had three drought gradients, lasted for three weeks. Water repellency index (WRI) and soil-water contact angle (β) were determined using intrinsic sorptivity method by measuring the water sorptivity (S W ) and ethanol sorptivity (S E ) in all soil samples. The results showed that (1) Polyacrylamide treatments significantly increased S W by 3% to 38%, and reduced S E by 1% to 15%, WRI by 6% to 38%, β by 3% to 23% compared to the control group. Polyacrylamide treatments also increased water-stable aggregates content and total porosity by 22% to 33%, 11% to 20% relative to the control, while PAM with a higher molecular weight performed best. (2) The interaction between PAM and drought stress had a significant effect on WRI and β for all soil types (P<0.01) while it only had a significant effect on S W and S E for the artificial soil (P<0.01). (3) The artificial soil had a greater WRI and β than the natural soil. Copyright © 2017 Elsevier B.V. All rights reserved.

Role of biofilms in sorptive removal of steroidal hormones and 4-nonylphenol compounds from streams

USGS Publications Warehouse

Writer, Jeffrey H.; Ryan, Joseph N.; Barber, Larry B.

2011-01-01

Stream biofilms play an important role in geochemical processing of organic matter and nutrients, however, the significance of this matrix in sorbing trace organic contaminants is less understood. This study focused on the role of stream biofilms in sorbing steroidal hormones and 4-nonylphenol compounds from surface waters using biofilms colonized in situ on artificial substrata and subsequently transferred to the laboratory for controlled batch sorption experiments. Steroidal hormones and 4-nonylphenol compounds readily sorb to stream biofilms as indicated by organic matter partition coefficients (Kom, L kg–1) for 17β-estradiol (102.5–2.8 L kg–1), 17α-ethynylestradiol (102.5–2.9 L kg–1), 4-nonylphenol (103.4–4.6 L kg–1), 4-nonylphenolmonoethoxylate (103.5–4.0 L kg–1), and 4-nonylphenoldiethoxylate (103.9–4.3 L kg–1). Experiments using water quality differences to induce changes in the relative composition of periphyton and heterotrophic bacteria in the stream biofilm did not significantly affect the sorptive properties of the stream biofilm, providing additional evidence that stream biofilms will sorb trace organic compounds under of variety of environmental conditions. Because sorption of the target compounds to stream biofilms was linearly correlated with organic matter content, hydrophobic partition into organic matter appears to be the dominant mechanism. An analysis of 17β-estradiol and 4-nonylphenol hydrophobic partition into water, biofilm, sediment, and dissolved organic matter matrices at mass/volume ratios typical of smaller rivers showed that the relative importance of the stream biofilm as a sorptive matrix was comparable to bed sediments. Therefore, stream biofilms play a primary role in attenuating these compounds in surface waters. Because the stream biofilm represents the base of the stream ecosystem, accumulation of steroidal hormones and 4-nonylphenol compounds in the stream biofilm may be an exposure pathway for organisms in higher trophic levels.

Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water.

PubMed

Ahrens, Lutz; Daneshvar, Atlasi; Lau, Anna E; Kreuger, Jenny

2016-08-03

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study provides a protocol for the passive sampler preparation, calibration, extraction method and instrumental analysis. Sampling rates (RS) and passive sampler-water partition coefficients (KPW) were calculated for silicone rubber, polar organic chemical integrative sampler POCIS-A, POCIS-B, SDB-RPS and C18 disk. The uptake of the selected compounds depended on their physicochemical properties, i.e., silicone rubber showed a better uptake for more hydrophobic compounds (log octanol-water partition coefficient (KOW) > 5.3), whereas POCIS-A, POCIS-B and SDB-RPS disk were more suitable for hydrophilic compounds (log KOW < 0.70).

Combined Mini-Cylex & Disk Acceleration Tests in Type K Copper

DOE PAGES

Maines, Warren Russell; Kittell, David E.; Hobbs, Michael L.

2018-04-16

In this work, we combined the miniature cylinder expansion test (Mini-Cylex), with the Disk Acceleration Test (DAX) using Type K copper, Picatinny Liquid Explosive, and photonic Doppler velocimetry. We estimated the CJ state using plate reverberation methods at the test cap. We extracted velocities at 2, 7, and 10 volume expansions to fit Jones-Wilkins-Lee Equation of State and estimated Gurney velocity at the tube wall. The test also provides an additional method to estimate reaction products Hugoniot through knowledge of the copper test cap. Our experiments and simulations are within expected uncertainty. Lastly, the test and the analysis effectively reducemore » costs while keeping or increasing fidelity.« less

Determining mechanical behavior of solid materials using miniature specimens

DOEpatents

Manahan, Michael P.; Argon, Ali S.; Harling, Otto K.

1986-01-01

A Miniaturized Bend Test (MBT) capable of extracting and determining mechanical behavior information from specimens only so large as to have at least a volume or smallest dimension sufficient to satisfy continuum behavior in all directions. The mechanical behavior of the material is determined from the measurements taken during the bending of the specimen and is processed according to the principles of linear or nonlinear material mechanics or both. In a preferred embodiment the determination is carried out by a code which is constructed according to the finite element method, and the specimen used for the determinations is a miniature disk simply supported for central loading at the axis on the center of the disk.

Combined Mini-Cylex & Disk Acceleration Tests in Type K Copper

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

Maines, Warren Russell; Kittell, David E.; Hobbs, Michael L.

In this work, we combined the miniature cylinder expansion test (Mini-Cylex), with the Disk Acceleration Test (DAX) using Type K copper, Picatinny Liquid Explosive, and photonic Doppler velocimetry. We estimated the CJ state using plate reverberation methods at the test cap. We extracted velocities at 2, 7, and 10 volume expansions to fit Jones-Wilkins-Lee Equation of State and estimated Gurney velocity at the tube wall. The test also provides an additional method to estimate reaction products Hugoniot through knowledge of the copper test cap. Our experiments and simulations are within expected uncertainty. Lastly, the test and the analysis effectively reducemore » costs while keeping or increasing fidelity.« less

[The use of semi-synthetic polymers in the formulation of sucking and chewable tablets containing sage extract and zinc gluconate].

PubMed

Linka, Wojciech Andrzej; Golenia, Ewa; Zgoda, Marian Mikołaj; Kołodziejczyk, Michał Krzysztof

2014-01-01

Halitosis and gingivitis are most common pathologies (15-60% of population) which, if left untreated, lead to periodontal diseases and tooth loss. The aim of this study was to develop, based on polymers of dry sage extract and zinc gluconate, tablets intended for sucking and chewing that can be applied in the treatment of halitosis and gingivitis. Dried aqueous sage extract, zinc gluconate, Pharmagum M, Prosolv SMCC90 and SMCCHD90, Vivapur 102, sorbitol, mannitol, ludipress. Direct tableting. Testing pharmacopeial parameters and pharmaceutical availability (using basket and rotating disk methods) of tablets intended for sucking and chewing. Approximation of the obtained results. Grey and green color tablets were obtained with smooth and uniform surface, without stains, spalls or mechanical damage. The determined average mass (weight) of a tablet complied with the standard. The friability and crushing strength test revealed that tablets containing Prosolv SMCCHD90, Vivapur 102 and mannitol demonstrated the highest mechanical strength. Tablets containing these substances and intended for sucking had prolonged disintegration and release time. Tablets intended for chewing had a hardness at the level of 124 N.They demonstrated compressibility, low friability and prolonged release. The release profiles of tablets intended for sucking (v2) and those for chewing, obtained by basket and rotating disk methods, were similar. The addition of Prosolv SMCCHD90, Vivapur 102 and mannitol increased significantly the mechanical strength (higher hardness, lower friability), prolonged the disintegration time and slowed the release from the obtained tablets intended for sucking and chewing. The application of Prosolv SMCCHD90 in the formulation of tablets for chewing carries the risk for sorption of active components to the polymer structure. This process takes place in the early stage of the release. Rotating disk method used in pharmaceutical availability testing gives better results while analyzing the phenomenon than the standard basket method. The suggested and tested formulations of tablets intended for sucking and chewing may be used as an alternative to formulations containing dried titrated extracts from plants of antimicrobial activity (sage - Salvia officinalis) in combination with substances binding volatile sulfur compounds (zinc gluconate).

Efficiency of extracting stereo-driven object motions

PubMed Central

Jain, Anshul; Zaidi, Qasim

2013-01-01

Most living things and many nonliving things deform as they move, requiring observers to separate object motions from object deformations. When the object is partially occluded, the task becomes more difficult because it is not possible to use two-dimensional (2-D) contour correlations (Cohen, Jain, & Zaidi, 2010). That leaves dynamic depth matching across the unoccluded views as the main possibility. We examined the role of stereo cues in extracting motion of partially occluded and deforming three-dimensional (3-D) objects, simulated by disk-shaped random-dot stereograms set at randomly assigned depths and placed uniformly around a circle. The stereo-disparities of the disks were temporally oscillated to simulate clockwise or counterclockwise rotation of the global shape. To dynamically deform the global shape, random disparity perturbation was added to each disk's depth on each stimulus frame. At low perturbation, observers reported rotation directions consistent with the global shape, even against local motion cues, but performance deteriorated at high perturbation. Using 3-D global shape correlations, we formulated an optimal Bayesian discriminator for rotation direction. Based on rotation discrimination thresholds, human observers were 75% as efficient as the optimal model, demonstrating that global shapes derived from stereo cues facilitate inferences of object motions. To complement reports of stereo and motion integration in extrastriate cortex, our results suggest the possibilities that disparity selectivity and feature tracking are linked, or that global motion selective neurons can be driven purely from disparity cues. PMID:23325345

Phytochemical properties and cytotoxicity evaluation of the aqueous extracts from Rafflesia cantleyi

NASA Astrophysics Data System (ADS)

Bakoush, Sumaia Mohamed Mohamed; Yaacob, Wan Ahmad; Adam, Jumaat; Ibrahim, Nazlina

2015-09-01

In the present study, phytochemical properties and cytotoxic evaluation of aqueous extract of Rafflesia cantleyi bud parts were done. Three bud parts including disk, bract and perigone tube were extracted in water to produce crude aqueous extract. Cytotoxic activity of R. cantleyi bud parts was assessed by conducting 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay against normal cells Vero, 3T3 cell lines and mice peripheral blood mononuclear cells PBMC. Phytochemical analyses revealed the presence of tannins, flavonoids, steroids and alkaloids. The CC50 value against Vero, 3T3 and PBMC cells were equal or more than 125 µg/ml indicating the non-cytotoxic effect of the bud parts extracts. The finding revealed that crude extracts of all the tested bud parts contained potential bioactive compounds which can be used for various biological activities and have no cytotoxicity to selected normal cells.

Planetary influence in the gap of a protoplanetary disk: structure formation and an application to V1247 Ori

NASA Astrophysics Data System (ADS)

Alvarez-Meraz, R.; Nagel, E.; Rendon, F.; Barragan, O.

2017-10-01

We present a set of hydrodynamical models of a planetary system embedded in a protoplanetary disk in order to extract the number of dust structures formed in the disk, their masses and sizes, within optical depth ranges τ≤0.5, 0.5<τ<2 and τ≥2. The study of the structures shows: (1) an increase in the number of planets implies an increase in the creation rate of massive structures; (2) a lower planetary mass accretion corresponds to slower time effects for optically thin structures; (3) an increase in the number of planets allows a faster evolution of the structures in the Hill radius for the different optical depth ranges of the inner planets. An ad-hoc simulation was run using the available information of the stellar system V1247 Ori, leading to a model of a planetary system which explains the SED and is consistent with interferometric observations of structures.

Organics in hydrothermal fluids from ultramafics on the Mid-Atlantic Ridge (MAR) - Abiogenic and/or biogenic origin?

NASA Astrophysics Data System (ADS)

Charlou, J.; Donval, J.; Fouquet, Y.; Jean-Baptiste, P.; Dehairs, F.; Holm, N.; Godfroy, A.

2005-12-01

Between 12°N and the Azores Triple Junction along the MAR, CH4 anomalies over axial ultramafic sites are common and point to the association of high or low temperature hydrothermal activity and mantle degassing indicative of ongoing serpentinization process. The general occurrence of isotopically-heavy methane shows the possible abiogenic synthesis of hydrocarbons in hydrothermal systems. The abiogenic formation of CH4 and more complex organic compounds is related to the process of serpentinization of mantellic rocks. Three sites (Logachev, 14°45'N; Rainbow, 36°14'N; Lost City Field, 30°N) are known on the MAR. New fresh fluids were recently sampled at Rainbow and Lost City by the French ROV-Victor during EXOMAR cruise (July 24 to August 28, 2005). The Rainbow and Lost City fluids issued from contrasted ultramafic environments are both enriched in H2, CH4 and hydrocarbons. Hydrogen gas represents more than 40 per cent total gas volume extracted from fluids. SPME (Solid Phase Micro-Extraction) and SBSE (Stir-Bar Sorptive Extraction) extraction techniques were used on board for organic recovery and the analysis was performed on shore by direct GC/MS or by Thermo-Desorption/GC/MS. The hydration of olivine and pyroxen minerals with conversion of Fe(II) to Fe(III) in magnetite during serpentinization leads to production of H2 and conversion of dissolved CO2 to reduced-C species including methane, ethane, propane. In addition heavier straight chain hydrocarbons as alcohols, aldehydes, ketones, aromatics, and cyclic compounds are identified at Rainbow. These compounds may be generated in ultramafic rocks through catalytic reactions (Fischer-Tropsch type reactions), but a biogenic contribution cannot be excluded. Abiogenic organic compounds may be produced from crystalline basement, from volcanic structures, from riftogenic zones and probably from sedimented margins.

Medicinal activities of the leaves of Musa sapientum var. sylvesteris in vitro

PubMed Central

Sahaa, Repon Kumer; Acharyaa, Srijan; Shovon, Syed Sohidul Haque; Royb, Priyanka

2013-01-01

Objective This study is to investigate the medicinal value of methanolic extract of the leaves of Musa sapientum var. sylvesteris in Bangladesh. Methods Several biochemical assays, thin layer chormatogarphy and ultra-violet spectroscopy were used to detect the presence of various types of compounds in this extract. Antioxidant effects were measured by DPPH scavenging assay, total reducing assay and hydrogen peroxide scavenging assay. Receptor binding activities and hydrogen peroxide induced hemolysis assay were performed by hemagglutination assay and hemolysis assay using erythrocytes. Disk diffusion assay was performed to show the antibacterial effect of the extract. Results Methanolic extract of the leaves showed antioxidant and antibacterial activity in vitro. The extract showed hemaglutination inhibition activities and hydrogen peroxide induced hemolysis inhibition activity of human red blood cells. Conclusion Musa sapientum var. sylvesteris can be an useful medicinal plant. PMID:23730561

Method to Recover Media Ligand Losses During Sorption of Rare Earth Elements from Simulated Geothermal Brines

DOE Data Explorer

Dean Stull

2016-05-24

This document describes the method and results of an in-situ experiment used to confirm that ligand bleed from a sorptive media can be contained. The experiment focused on maintaining the media's sorption of rare earth elements (REE) obtained from a simulated geothermal brine doped with known mineral concentrations.

Methods for improved preconcentrators

DOEpatents

Manginell, Ronald P [Albuquerque, NM; Lewis, Patrick R [Albuquerque, NM; Okandan, Murat [Edgewood, NM

2010-06-01

The present invention relates generally to chemical analysis (e.g. by gas chromatography), and in particular to a compact chemical preconcentrator formed on a substrate with a heatable sorptive membrane that can be used to accumulate and concentrate one or more chemical species of interest over time and then rapidly release the concentrated chemical species upon demand for chemical analysis.

Simplifying pyrolysis; using gasification to produce corn stover and wheat straw biochar for sorptive and horitcultural media

USDA-ARS?s Scientific Manuscript database

Biochar is a renewable, useful material that can be utilized in many different applications. Biochar is commonly produced via pyrolysis methods using a retort-style oven with inert gas. Gasification is another method that can utilize pyrolysis to produce biochar, but with the advantage of not requir...

Colorimetric-Solid Phase Extraction Technology for Water Quality Monitoring: Evaluation of C-SPE and Debubbling Methods in Microgravity

NASA Technical Reports Server (NTRS)

Hazen-Bosveld, April; Lipert, Robert J.; Nordling, John; Shih, Chien-Ju; Siperko, Lorraine; Porter, Marc D.; Gazda, Daniel B.; Rutz, Jeff A.; Straub, John E.; Schultz, John R.;

Automatic detection of magnetic flux emergings in the solar atmosphere from full-disk magnetogram sequences.

PubMed

Fu, Gang; Shih, Frank Y; Wang, Haimin

2008-11-01

In this paper, we present a novel method to detect Emerging Flux Regions (EFRs) in the solar atmosphere from consecutive full-disk Michelson Doppler Imager (MDI) magnetogram sequences. To our knowledge, this is the first developed technique for automatically detecting EFRs. The method includes several steps. First, the projection distortion on the MDI magnetograms is corrected. Second, the bipolar regions are extracted by applying multiscale circular harmonic filters. Third, the extracted bipolar regions are traced in consecutive MDI frames by Kalman filter as candidate EFRs. Fourth, the properties, such as positive and negative magnetic fluxes and distance between two polarities, are measured in each frame. Finally, a feature vector is constructed for each bipolar region using the measured properties, and the Support Vector Machine (SVM) classifier is applied to distinguish EFRs from other regions. Experimental results show that the detection rate of EFRs is 96.4% and of non-EFRs is 98.0%, and the false alarm rate is 25.7%, based on all the available MDI magnetograms in 2001 and 2002.

AMBER-NACO aperture-synthesis imaging of the half-obscured central star and the edge-on disk of the red giant L2 Puppis

NASA Astrophysics Data System (ADS)

Ohnaka, K.; Schertl, D.; Hofmann, K.-H.; Weigelt, G.

2015-09-01

Aims: The red giant L2 Pup started a dimming event in 1994, which is considered to be caused by the ejection of dust clouds. We present near-IR aperture-synthesis imaging of L2 Pup achieved by combining data from VLT/NACO and the AMBER instrument of the Very Large Telescope Interferometer (VLTI). Our aim is to spatially resolve the innermost region of the circumstellar environment. Methods: We carried out speckle interferometric observations at 2.27 μm with VLT/NACO and long-baseline interferometric observations with VLTI/AMBER at 2.2-2.35 μm with baselines of 15-81 m. We also extracted an 8.7 μm image from the mid-IR VLTI instrument MIDI. Results: The diffraction-limited image obtained by bispectrum speckle interferometry with NACO with a spatial resolution of 57 mas shows an elongated component. The aperture-synthesis imaging combining the NACO speckle data and AMBER data with a spatial resolution of 5.6 × 7.3 mas further resolves not only this elongated component, but also the central star. The reconstructed image reveals that the elongated component is a nearly edge-on disk with a size of ~180 × 50 mas lying in the E-W direction, and furthermore, that the southern hemisphere of the central star is severely obscured by the equatorial dust lane of the disk. The angular size of the disk is consistent with the distance that the dust clouds that were ejected at the onset of the dimming event should have traveled by the time of our observations, if we assume that the dust clouds moved radially. This implies that the formation of the disk may be responsible for the dimming event. The 8.7 μm image with a spatial resolution of 220 mas extracted from the MIDI data taken in 2004 (seven years before the AMBER and NACO observations) shows an approximately spherical envelope without a signature of the disk. This suggests that the mass loss before the dimming event may have been spherical. Based on AMBER, NACO, and MIDI observations made with the Very Large Telescope and Very Large Telescope Interferometer of the European Southern Observatory. Program ID: 074.D-0075(A), 074.D-0101(A), 074.D-0198(B), 088.D-0150(A/B), and 288.D-5041(A). Appendices are available in electronic form at http://www.aanda.org

YAdumper: extracting and translating large information volumes from relational databases to structured flat files.

PubMed

Fernández, José M; Valencia, Alfonso

2004-10-12

Downloading the information stored in relational databases into XML and other flat formats is a common task in bioinformatics. This periodical dumping of information requires considerable CPU time, disk and memory resources. YAdumper has been developed as a purpose-specific tool to deal with the integral structured information download of relational databases. YAdumper is a Java application that organizes database extraction following an XML template based on an external Document Type Declaration. Compared with other non-native alternatives, YAdumper substantially reduces memory requirements and considerably improves writing performance.

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

Dullo, Bililign T.; Graham, Alister W., E-mail: Bdullo@astro.swin.edu.au

We have used the full radial extent of images from the Hubble Space Telescope's Advanced Camera for Surveys and Wide Field Planetary Camera 2 to extract surface brightness profiles from a sample of six, local lenticular galaxy candidates. We have modeled these profiles using a core-Sersic bulge plus an exponential disk model. Our fast rotating lenticular disk galaxies with bulge magnitudes M{sub V} {approx}< -21.30 mag have central stellar deficits, suggesting that these bulges may have formed from ''dry'' merger events involving supermassive black holes (BHs) while their surrounding disk was subsequently built up, perhaps via cold gas accretion scenarios.more » The central stellar mass deficits M{sub def} are roughly 0.5-2 M{sub BH} (BH mass), rather than {approx}10-20 M{sub BH} as claimed from some past studies, which is in accord with core-Sersic model mass deficit measurements in elliptical galaxies. Furthermore, these bulges have Sersic indices n {approx}3, half-light radii R{sub e} < 2 kpc and masses >10{sup 11} M{sub Sun }, and therefore appear to be descendants of the compact galaxies reported at z {approx} 1.5-2. Past studies which have searched for these local counterparts by using single-component galaxy models to provide the z {approx} 0 size comparisons have overlooked these dense, compact, and massive bulges in today's early-type disk galaxies. This evolutionary scenario not only accounts for what are today generally old bulges-which must be present in z {approx} 1.5 images-residing in what are generally young disks, but it eliminates the uncomfortable suggestion of a factor of three to five growth in size for the compact, z {approx} 1.5 galaxies that are known to possess infant disks.« less

Central Stellar Mass Deficits in the Bulges of Local Lenticular Galaxies, and the Connection with Compact z ~ 1.5 Galaxies

NASA Astrophysics Data System (ADS)

Dullo, Bililign T.; Graham, Alister W.

2013-05-01

We have used the full radial extent of images from the Hubble Space Telescope's Advanced Camera for Surveys and Wide Field Planetary Camera 2 to extract surface brightness profiles from a sample of six, local lenticular galaxy candidates. We have modeled these profiles using a core-Sérsic bulge plus an exponential disk model. Our fast rotating lenticular disk galaxies with bulge magnitudes MV <~ -21.30 mag have central stellar deficits, suggesting that these bulges may have formed from "dry" merger events involving supermassive black holes (BHs) while their surrounding disk was subsequently built up, perhaps via cold gas accretion scenarios. The central stellar mass deficits M def are roughly 0.5-2 M BH (BH mass), rather than ~10-20 M BH as claimed from some past studies, which is in accord with core-Sérsic model mass deficit measurements in elliptical galaxies. Furthermore, these bulges have Sérsic indices n ~3, half-light radii Re < 2 kpc and masses >1011 M ⊙, and therefore appear to be descendants of the compact galaxies reported at z ~ 1.5-2. Past studies which have searched for these local counterparts by using single-component galaxy models to provide the z ~ 0 size comparisons have overlooked these dense, compact, and massive bulges in today's early-type disk galaxies. This evolutionary scenario not only accounts for what are today generally old bulges—which must be present in z ~ 1.5 images—residing in what are generally young disks, but it eliminates the uncomfortable suggestion of a factor of three to five growth in size for the compact, z ~ 1.5 galaxies that are known to possess infant disks.

Determination of Chromium(III), Chromium(VI), and Chromium(III) acetylacetonate in water by ion-exchange disk extraction/metal furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Kamakura, Nao; Inui, Tetsuo; Kitano, Masaru; Nakamura, Toshihiro

A new method for the separate determination of Chromium(III) (Cr(III)), Chromium(VI) (Cr(VI)), and Cr(III) acetylacetonate (Cr(acac)3) in water was developed using a cation-exchange extraction disk (CED) and an anion-exchange extraction disk (AED) combined with metal furnace atomic absorption spectrometry (MFAAS). A 100-mL water sample was adjusted to pH 5.6 and passed through the CED placed on the AED. Cr(acac)3 and Cr(III) were adsorbed on the CED, and Cr(VI) was adsorbed on the AED. The adsorbed Cr(acac)3 was eluted with 50 mL of carbon tetrachloride, followed by the elution of Cr(III) with 50 mL of 3 mol L- 1 nitric acid. Cr(VI) was eluted with 50 mL of 3 mol L- 1 nitric acid. The chemical species of Cr eluted from the CED with carbon tetrachloride was identified as Cr(acac)3 using infrared spectroscopy. The eluate of Cr(acac)3 was diluted to 100 mL with carbon tetrachloride, and those of Cr(III) and Cr(VI) were diluted to 100 mL with deionized water. All of the solutions were subsequently analyzed by MFAAS. The calibration curve for the Cr(acac)3 aqueous solutions exhibited good linearity in the range of 0.1 to 1 ng. The detection limit of Cr, which corresponded to three times the standard deviation (n = 10) of the blank values, was 20 pg. The recovery test for Cr(III), Cr(VI), and Cr(acac)3 exhibited desirable results (96.0%-107%) when 5 μg of each species (50 μg L- 1) was added to 100 mL water samples (i.e., tap water, rainwater, and bottled drinking water). In a humic acid solution, Cr(acac)3 was quantitatively recovered (103%), but Cr(III) and Cr(VI) exhibited poor recoveries (i.e., 84.8% and 78.4%, respectively).

Biologically active traditional medicinal herbs from Balochistan, Pakistan.

PubMed

Zaidi, Mudassir A; Crow, Sidney A

2005-01-04

The biological activities of the following four important medicinal plants of Balochistan, Pakistan were checked; Grewia erythraea Schwein f. (Tiliaceae), Hymenocrater sessilifolius Fisch. and C.A. Mey (Lamiaceae), Vincetoxicum stocksii Ali and Khatoon (Asclepiadaceae) and Zygophyllum fabago L. (Zygophyllaceae). The methanolic extracts were fractionated into hexane, ethyl acetate, chloroform, butanol and water. The antifungal and antibacterial activities of these plants were determined against 12 fungal and 12 bacterial strains by agar well diffusion and disk diffusion assays. The extract of Zygophyllum fabago was found to be highly effective against Candida albicans and Escherichia coli. The extract of Vincetoxicum stocksii was also found to be significantly active against Candida albicans, Bacillus subtilis and Bacillus cereus. Extracts of Hymenocrater sessilifolius and Grewia erythraea showed good activity only against Pseudomonas aeruginosa.

Major Effects of Nonmetallic Inclusions on the Fatigue Life of Disk Superalloy Demonstrated

NASA Technical Reports Server (NTRS)

Gabb, Timothy P.; Telesman, Jack; Kantzos, Peter T.; Bonacuse, Peter J.; Barrie, Robert L.

2002-01-01

The fatigue properties of modern powder metallurgy disk alloys can vary because of the different steps of materials and component processing and machining. Among these variables, the effects of nonmetallic inclusions introduced during the powder atomization and handling processes have been shown to significantly degrade low-cycle fatigue life. The levels of inclusion contamination have, therefore, been reduced to less than 1 part per million in state-of-the-art nickel disk powder-processing facilities. Yet the large quantities of compressor and turbine disks weighing from 100 to over 1000 lb have enough total volume and surface area for these rare inclusions to still be present and limit fatigue life. The objective of this study was to investigate the effects on fatigue life of these inclusions, as part of the Crack Resistant Disk Materials task within the Ultra Safe Propulsion Project. Inclusions were carefully introduced at elevated levels in a nickel-base disk superalloy, U720, produced using powder metallurgy processing. Multiple strain-controlled fatigue tests were then performed on extracted test specimens at 650 C. Analyses were performed to compare the low-cycle fatigue lives and failure initiation sites as functions of inclusion content and fatigue conditions. Powder of the nickel-base superalloy U720 was atomized in argon at Special Metals Corporation, Inc., using production-scale high-cleanliness powder-processing facilities and handling practices. The powder was then passed through a 270-mesh screen. One portion of this powder was set aside for subsequent consolidation without introduced inclusions. Two other portions of this powder were seeded with alumina inclusions. Small, polycrystalline soft (Type 2) inclusions of about 50 mm diameter were carefully prepared and blended into one powder lot, and larger hard (Type 1) inclusions of about 150 mm mean diameter were introduced into the other seeded portion of powder. All three portions of powder were then sealed in separate containers, hot isostatically pressurized, extruded, forged into subscale disks, and heat treated. Low-cycle-fatigue specimens were then extracted, machined, and tested. Fatigue tests were performed at 650 C in closed-loop servohydraulic testing machines using induction heating and axial extensometers. All tests were continued to failure, and fractographic evaluations were performed on all specimens to determine the crack initiation sites. A large majority of the failures in specimens with introduced inclusions occurred at cracks initiating from inclusions at the specimen surface, as shown for each type of inclusion in the following bar chart. The inclusions significantly reduced fatigue life from unseeded material levels, as shown in the bar chart. These effects were found to depend on the strain range, strain ratio, and inclusion size. Tests at lower strain ranges and higher strain ratios resulted in larger effects of inclusions on life. Inclusion effects on life were thereby maximized in tests at the lowest strain range of 0.6 percent and the most positive strain ratio of 0.5. Under these conditions, small Type 2 inclusions reduced life substantially-- about 20 times, whereas large Type 1 inclusions dramatically reduced life 100 times. These results clearly demonstrate that it is essential to include the effects of inclusions for realistic predictions of disk fatigue life. Important issues, including temperature dependence, crack initiation versus propagation, surface treatments, realistic disk features and machining, and realistic disk spin testing will be addressed to accurately model inclusion effects on disk fatigue life. Fatigue life varied from well over 105 cycles for no inclusions to a little over 103 cycles for 100-micrometer inclusions. A single crack initiating at a surface-connected seeded inclusion caused failure in each case.

Evolution in the Dust Lane Fraction of Edge-on L* V Spiral Galaxies Since z = 0.8

NASA Astrophysics Data System (ADS)

Holwerda, B. W.; Dalcanton, J. J.; Radburn-Smith, D.; de Jong, R. S.; Guhathakurta, P.; Koekemoer, A.; Allen, R. J.; Böker, T.

2012-07-01

The presence of a well-defined and narrow dust lane in an edge-on spiral galaxy is the observational signature of a thin and dense molecular disk, in which gravitational collapse has overcome turbulence. Using a sample of galaxies out to z ~ 1 extracted from the COSMOS survey, we identify the fraction of massive (L* V ) disks that display a dust lane. Our goal is to explore the evolution in the stability of the molecular interstellar medium (ISM) disks in spiral galaxies over a cosmic timescale. We check the reliability of our morphological classifications against changes in rest-frame wavelength, resolution, and cosmic dimming with (artificially redshifted) images of local galaxies from the Sloan Digital Sky Survey. We find that the fraction of L* V disks with dust lanes in COSMOS is consistent with the local fraction (≈80%) out to z ~ 0.7. At z = 0.8, the dust lane fraction is only slightly lower. A somewhat lower dust lane fraction in starbursting galaxies tentatively supports the notion that a high specific star formation rate can efficiently destroy or inhibit a dense molecular disk. A small subsample of higher redshift COSMOS galaxies display low internal reddening (E[B - V]), as well as a low incidence of dust lanes. These may be disks in which the growth of the dusty ISM disk lags behind that of the stellar disk. We note that at z = 0.8, the most massive galaxies display a lower dust lane fraction than lower mass galaxies. A small contribution of recent mergers or starbursts to this most massive population may be responsible. The fact that the fraction of galaxies with dust lanes in COSMOS is consistent with little or no evolution implies that models to explain the spectral energy distribution or the host galaxy dust extinction of supernovae based on local galaxies are still applicable to higher redshift spirals. It also suggests that dust lanes are long-lived phenomena or can be reformed over very short timescales.

EVOLUTION IN THE DUST LANE FRACTION OF EDGE-ON L*{sub V} SPIRAL GALAXIES SINCE z = 0.8

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

Holwerda, B. W.; Boeker, T.; Dalcanton, J. J.

2012-07-01

The presence of a well-defined and narrow dust lane in an edge-on spiral galaxy is the observational signature of a thin and dense molecular disk, in which gravitational collapse has overcome turbulence. Using a sample of galaxies out to z {approx} 1 extracted from the COSMOS survey, we identify the fraction of massive (L*{sub V}) disks that display a dust lane. Our goal is to explore the evolution in the stability of the molecular interstellar medium (ISM) disks in spiral galaxies over a cosmic timescale. We check the reliability of our morphological classifications against changes in rest-frame wavelength, resolution, andmore » cosmic dimming with (artificially redshifted) images of local galaxies from the Sloan Digital Sky Survey. We find that the fraction of L*{sub V} disks with dust lanes in COSMOS is consistent with the local fraction ( Almost-Equal-To 80%) out to z {approx} 0.7. At z = 0.8, the dust lane fraction is only slightly lower. A somewhat lower dust lane fraction in starbursting galaxies tentatively supports the notion that a high specific star formation rate can efficiently destroy or inhibit a dense molecular disk. A small subsample of higher redshift COSMOS galaxies display low internal reddening (E[B - V]), as well as a low incidence of dust lanes. These may be disks in which the growth of the dusty ISM disk lags behind that of the stellar disk. We note that at z = 0.8, the most massive galaxies display a lower dust lane fraction than lower mass galaxies. A small contribution of recent mergers or starbursts to this most massive population may be responsible. The fact that the fraction of galaxies with dust lanes in COSMOS is consistent with little or no evolution implies that models to explain the spectral energy distribution or the host galaxy dust extinction of supernovae based on local galaxies are still applicable to higher redshift spirals. It also suggests that dust lanes are long-lived phenomena or can be reformed over very short timescales.« less

Determining mechanical behavior of solid materials using miniature specimens

DOEpatents

Manahan, M.P.; Argon, A.S.; Harling, O.K.

1986-02-04

A Miniaturized Bend Test (MBT) capable of extracting and determining mechanical behavior information from specimens only so large as to have at least a volume or smallest dimension sufficient to satisfy continuum behavior in all directions is disclosed. The mechanical behavior of the material is determined from the measurements taken during the bending of the specimen and is processed according to the principles of linear or nonlinear material mechanics or both. In a preferred embodiment the determination is carried out by a code which is constructed according to the finite element method, and the specimen used for the determinations is a miniature disk simply supported for central loading at the axis on the center of the disk. 51 figs.

Untangling Galaxy Components - The Angular Momentum Parameter

NASA Astrophysics Data System (ADS)

Tabor, Martha; Merrifield, Michael; Aragon-Salamanca, Alfonso

2017-06-01

We have developed a new technique to decompose Integral Field spectral data cubes into separate bulge and disk components, allowing us to study the kinematic and stellar population properties of the individual components and how they vary with position. We present here the application of this method to a sample of fast rotator early type galaxies from the MaNGA integral field survey, and demonstrate how it can be used to explore key properties of the individual components. By extracting ages, metallicities and the angular momentum parameter lambda of the bulges and disks, we show how this method can give us new insights into the underlying structure of the galaxies and discuss what this can tell us about their evolution history.

IN VITRO ANTIMICROBIAL SCREENING OF AQUILARIA AGALLOCHA ROOTS.

PubMed

Canlı, Kerem; Yetgin, Ali; Akata, Ilgaz; Altuner, Ergin Murat

2016-01-01

It was previously shown that some parts of Aquilaria agallocha , which is commonly known as oud or oodh, such as roots have been used as a traditional medical herbal in different countries. In Turkey A. agallocha is one of the ingredients while preparing famous Mesir paste, which was invented as a medicinal paste and used from the Ottoman period to now at least for 500 years. The identification the in vitro antimicrobial activity of ethanol extract of A. agallocha roots is main purpose of this analysis. By using 17 bacteria and 1 fungi, which include Bacillus, Candida, Enterobacter, Enterococcus, Escherichia, Klebsiella, Listeria, Pseudomonas, Salmonella and Staphylococcus genera, the activity of A. agallocha root extracts were analysed by the help of the disk diffusion method, that is one of the methods commonly used to determine antimicrobial activities. As a result of the study it was observed that ethanol extracts of A. agallocha roots have a clear antimicrobial activity against nearly all microorganism used in the study, but only two bacteria namely E. coli ATCC 25922 and S. typhimurium SL 1344. According to the disk diffusion test results it may be possible to propose that A. agallocha roots should have a medicinal uses especially against E. faecium , L. monocytogenes ATCC 7644, B. subtilis DSMZ 1971, C. albicans DSMZ 1386, S. epidermidis DSMZ 20044 and S. aureus ATCC 25923.

Investigation of relationships between parameters of solar nano-flares and solar activity

NASA Astrophysics Data System (ADS)

Safari, Hossein; Javaherian, Mohsen; Kaki, Bardia

2016-07-01

Solar flares are one of the important coronal events which are originated in solar magnetic activity. They release lots of energy during the interstellar medium, right after the trigger. Flare prediction can play main role in avoiding eventual damages on the Earth. Here, to interpret solar large-scale events (e.g., flares), we investigate relationships between small-scale events (nano-flares) and large-scale events (e.g., flares). In our method, by using simulations of nano-flares based on Monte Carlo method, the intensity time series of nano-flares are simulated. Then, the solar full disk images taken at 171 angstrom recorded by SDO/AIA are employed. Some parts of the solar disk (quiet Sun (QS), coronal holes (CHs), and active regions (ARs)) are cropped and the time series of these regions are extracted. To compare the simulated intensity time series of nano-flares with the intensity time series of real data extracted from different parts of the Sun, the artificial neural networks is employed. Therefore, we are able to extract physical parameters of nano-flares like both kick and decay rate lifetime, and the power of their power-law distributions. The procedure of variations in the power value of power-law distributions within QS, CH is similar to AR. Thus, by observing the small part of the Sun, we can follow the procedure of solar activity.

Antibacterial Constituents of Hainan Morinda citrifolia (Noni) Leaves.

PubMed

Zhang, Wei-Min; Wang, Wei; Zhang, Jing-Jing; Wang, Zhi-Rong; Wang, Yu; Hao, Wang-Jun; Huang, Wu-Yang

2016-05-01

Noni (Morinda citrifolia L.) is an edible and medicinal plant distributed in Hainan, China. The antibacterial activities of the extracts of water (WE), petroleum ether (PEE), ethyl acetate (EAE), chloroform (CE), and n-butanol (BE) were assayed by the disk diffusion method. The results showed that the extracts from Noni leaves possessed antibacterial effects against Bacillus subtilis, Escherichia coli, Proteus vulgaris, and Staphylococcus aureus. Among 5 different extracts, the BE produced the best antibacterial activity. The samples were first extracted by ethanol, and the primary compounds in the BE fraction of ethanol extract was further isolated and identified. Six phenolic compounds, including 5, 15-dimethylmorindol, ferulic acid, p-hydroxycinamic acid, methyl 4-hydroxybenzoate, methyl ferulate, and methyl 4-hydroxycinnamate, were identifiedby NMR. The results indicated that the phenolic compounds might significantly contribute to antibacterial activities of Noni leaves. © 2016 Institute of Food Technologists®

Physically (CO2) activated hydrochars from hickory and peanut hull: preparation, characterization, and sorption of methylene blue, lead, copper, and cadmium

USDA-ARS?s Scientific Manuscript database

The effects of carbon dioxide activation temperature (600-900 degree Celsius °C) and time (1 and 2 h) on the physicochemical and sorptive characteristics of hickory and peanut hull hydrochars were investigated. The extent of burn-off increased with increasing activation times and temperatures, and r...

2011 Chemical, Biological, Radiological, and Nuclear Survivability Conference

DTIC Science & Technology

2011-05-18

Protection (barrier, sorptive and reactive material technologies) o Top surface antimicrobial treatments (kills spores, bacteria, fungi, viruses ) o...Warning System (TWS) CDD - Countermeasure Anti-Torpedo ( CAT ) CDD UNCLASSIFIED Joint Program Executive Office for Chemical and Biological Defense May...Creating viruses de novo Biological Threats UNCLASSIFIED JPEO-CBD Radiological/Nuclear (RN) Status and Path Forward • Issue: No identified DoD

Sorptivity of rocks and soils of the van Genuchten-Mualem type

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

Zimmerman, R.W.; Bodvarsson, G.S.

1991-06-01

One hydrological process that will have great relevance to the performance of the proposed underground radioactive waste repository at Yucca Mountain, Nevada, is that of the absorption of water from a water-filled fracture into the adjacent unsaturated rock formation. The rate at which water is imbibed by a rock depends on the hydrological properties of the rock and on the initial saturation (or initial capillary suction) of the formation. The hydrological properties that affect imbibition are the relative permeability function and the capillary pressure function. These functions are often collectively referred to as the `characteristic functions` of the porous medium.more » For one-dimensional absorption, it can be shown that, regardless of the details of the characteristic functions, the total amount of water imbibed by the formation, per unit surface area, will be proportional to the square root of the elapsed time. Hence the ability of a rock or soil to imbibe water can be quantified by a parameter known as the sorptivity S, which is defined such that the cumulative volumetric liquid influx per unit area is given by Q = S{radical}t. The paper discusses the simplification of these characteristic functions of porous medium.« less

Weaker soil carbon-climate feedbacks resulting from microbial and abiotic interactions

NASA Astrophysics Data System (ADS)

Tang, Jinyun; Riley, William J.

2015-01-01

The large uncertainty in soil carbon-climate feedback predictions has been attributed to the incorrect parameterization of decomposition temperature sensitivity (Q10; ref. ) and microbial carbon use efficiency. Empirical experiments have found that these parameters vary spatiotemporally, but such variability is not included in current ecosystem models. Here we use a thermodynamically based decomposition model to test the hypothesis that this observed variability arises from interactions between temperature, microbial biogeochemistry, and mineral surface sorptive reactions. We show that because mineral surfaces interact with substrates, enzymes and microbes, both Q10 and microbial carbon use efficiency are hysteretic (so that neither can be represented by a single static function) and the conventional labile and recalcitrant substrate characterization with static temperature sensitivity is flawed. In a 4-K temperature perturbation experiment, our fully dynamic model predicted more variable but weaker soil carbon-climate feedbacks than did the static Q10 and static carbon use efficiency model when forced with yearly, daily and hourly variable temperatures. These results imply that current Earth system models probably overestimate the response of soil carbon stocks to global warming. Future ecosystem models should therefore consider the dynamic interactions between sorptive mineral surfaces, substrates and microbial processes.

Nondestructive reactivation of chemical protective garments. Final report, June 1985-July 1989

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

Chang, K.W.; Chang, S.Y.; Klemperer, E.

In the near future, chemical protective combat uniforms may be worn by Army personnel on a continuous basis. Activated carbon, the operative component, has diminished capacity for sorbing chemical agents after it has been exposed to dirt, sweat, cigarette smoke, engine exhaust, petroleum products and numerous other elements routinely present in the battlefield environment. This report summarizes the development of two nondestructive methods for cleaning and reactivating soiled chemical protective garments. Complete reactivation was achieved when the aqueous i-propanol iodine displacement method of Manes, which removed all but pure hydrocarbon oil soils from the current overgarment Type III foam ormore » Kynol activated carbon fiber material, was applied in nonaqueous solvent. Subsequently, a nonaqueous solvent method that requires less handling was chosen in designing a truck-mounted system. It features non-agitative flow of methylene chloride and methanol around the chemical-protective garments suspended between ultrasonic transducers. Both methods restore full sorptivity to the Type III foam liner. There is a one-time 10% loss of activated carbon without any loss of sorptivity. The volatile solvents are more easily removed, and can be economically recovered. Overall features of a mobile unit have been sketched.« less

Influence of ammonia and carbon dioxide on the sorption of a basic organic pollutant to carpet and latex-painted gypsum board.

PubMed

Ongwandee, Maneerat; Morrison, Glenn C

2008-08-01

Sorptive interactions with indoor surfaces strongly influence indoor exposure to organic pollutants. Adsorption itself may be influenced by indoor levels of common indoor gases such as CO2, NH3, and H2O. We quantified sorption characteristics of trimethylamine (TMA) on carpet and painted wallboard, while challenging the surface with gas-phase CO2, NH3 and H2O. We show that the capacity of the carpet to sorb TMA, doubles when the CO2 mixing ratio is increased from 0 to 1000 ppm CO2 at 90% relative humidity. In contrast, NH3 decreases the surface capacity of both carpet and latex paint. Sorption of TMA to these indoor materials is primarily caused by interactions at one or more interfaces. Dissolution of TMA and aqueous acid-base chemistry appear to also contribute to the overall sorptive capacity of carpet at high relative humidity. The reduction in the distribution coefficient, k(e), in the presence of NH3 is explained by competition between TMA and NH3 molecules for sites on the substrates at low-to-medium relative humidity conditions.

Effects of hydroethanolic extracts of Balanites aegyptiaca (L.) Delile (Balanitaceae) on some resistant pathogens bacteria isolated from wounds.

PubMed

Anani, Kokou; Adjrah, Yao; Ameyapoh, Yaovi; Karou, Simplice Damintoti; Agbonon, Amegnona; de Souza, Comlan; Gbeassor, Messanvi

2015-04-22

The bark of Balanites aegyptiaca (L.) Delile (Balanitaceae) is widely used in the Togolese folk medicine for the treatment of wounds, malaria and skin diseases. This study aimed to evaluate the antioxidant properties and the activity of the bark extract of this plant against some resistant bacteria isolated from wounds. The antimicrobial activity was assayed using the NCCLS microdilution while the DPPH free radical scavenging and ferric reducing antioxidant power (FRAP) were used for the antioxidant activity. The susceptibility to conventional antibiotics of bacteria was assessed by an agar disk diffusion method using commercial disk. Phenolics were quantified using spectrophotometric methods. The hydroethanolic extracts of the bark inhibited in vitro the growth of Pseudomonas aeruginosa and Staphylococcus aureus in a dose-dependent manner. Bacteriostatic effects were observed on 15 (33%) and 21 (47%) strains of Staphylococcus aureus and Pseudomonas aeruginosa respectively. The MICs and MBCs against Staphylococcus aureus strains ranged respectively from 2.5 to 12.5 µg/mL and 2.5 to 50 µg/mL. Concerning Pseudomonas aeruginosa, these values were equal (12.5 µg/mL). Multidrug resistance was 95% against six antibiotics for Pseudomonas aeruginosa and 91% against five antibiotics for Staphylococcus aureus. The DPPH radical scavenging and the FRAP assays yielded weak antioxidant activity, closely linked with the total phenolic contents. This study indicated that the bark extract of Balanites aegyptiaca possess bioactive compounds implicated in the free radical scavenging and antibacterial activities, justifying the use of the plant in the traditional medicines. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Properties of dermonecrotic toxin prepared from sonic extracts Bordetella bronchiseptica.

PubMed

Kume, K; Nakai, T; Samejima, Y; Sugimoto, C

1986-05-01

A toxin with dermonecrotic activity (DNT) was purified from sonic extracts of Bordetella bronchiseptica L3 of pig origin at phase I by chromatographic and electrophoretic methods. The purification procedure was one developed for obtaining the Pasteurella multocida DNT from sonic extracts with some modifications. Dermonecrotizing activity of B. bronchiseptica-purified DNT was increased by 600-fold compared with that of the crude extract, and the average yield was about 3%. The toxin was homogeneous, as determined by Ouchterlony double immunodiffusion, crossed immunoelectrophoresis, and disk isoelectric focusing in polyacrylamide gels. The toxin gave a single band on polyacrylamide disk gel electrophoresis (PAGE) and sodium dodecyl sulfate-SDS PAGE. The molecular weight of the toxin was ca. 190,000 +/- 5,000, as determined by SDS-PAGE. The isoelectric point of the toxin was ca. 6.5 to 6.6. The minimal necrotizing dose of the toxin for guinea pigs was about 2 ng of protein per 0.1 ml, the 50% lethal dose per mouse was about 0.3 micrograms, and the minimal cytotoxic dose for embryonic bovine lung cells was about 2 ng/ml. The toxin was heat labile and sensitive to inactivation by trypsin, Formalin, and glutaraldehyde. The mildly trypsinized B. bronchiseptica DNT preparation dissociated into two polypeptide chains, with molecular weights of ca. 75,000 +/- 4,000 (fragment 1) and ca. 118,000 +/- 5,000 (fragment 2), after treatment with dithiothreitol-SDS or urea. Upon removal of dithiothreitol and urea from the dissociated DNT preparation, the fragments reassociated, and the DNT that was formed was indistinguishable from the native toxin.

Chemosignaling diversity in songbirds: chromatographic profiling of preen oil volatiles in different species.

PubMed

Soini, Helena A; Whittaker, Danielle J; Wiesler, Donald; Ketterson, Ellen D; Novotny, Milos V

2013-11-22

Large foraging seabirds are known to navigate to food sources using their excellent sense of smell, but much less is known about the use of olfaction by the songbirds (passerine birds). Some evidence of individual recognition based on the bird preen oil volatile organic compound (VOC) compositions, which is the main odor source in birds, have been reported for dark-eyed junco and house finch. In this study we have investigated preen oil VOCs in 16 different songbird species and two other small bird species in order to determine whether the VOC compositions follow phylogenetic and evolutionary relatedness. We have used the stir bar sorptive extraction (SBSE) methodology followed by gas chromatography-mass spectrometry (GC-MS) to determine preen oil VOCs during the long light summer conditions for mostly wild caught birds. Large diversity among the VOC compositions was observed, while some compound classes were found in almost all species. The divergent VOC profiles did not follow the phylogenetic family lines among the bird species. This suggests that songbirds may use VOC odors as a mate recognition cue. Copyright © 2013 Elsevier B.V. All rights reserved.

Individual and gender fingerprints in human body odour.

PubMed

Penn, Dustin J; Oberzaucher, Elisabeth; Grammer, Karl; Fischer, Gottfried; Soini, Helena A; Wiesler, Donald; Novotny, Milos V; Dixon, Sarah J; Xu, Yun; Brereton, Richard G

2007-04-22

Individuals are thought to have their own distinctive scent, analogous to a signature or fingerprint. To test this idea, we collected axillary sweat, urine and saliva from 197 adults from a village in the Austrian Alps, taking five sweat samples per subject over 10 weeks using a novel skin sampling device. We analysed samples using stir bar sorptive extraction in connection with thermal desorption gas chromatograph-mass spectrometry (GC-MS), and then we statistically analysed the chromatographic profiles using pattern recognition techniques. We found more volatile compounds in axillary sweat than in urine or saliva, and among these we found 373 peaks that were consistent over time (detected in four out of five samples per individual). Among these candidate compounds, we found individually distinct and reproducible GC-MS fingerprints, a reproducible difference between the sexes, and we identified the chemical structures of 44 individual and 12 gender-specific volatile compounds. These individual compounds provide candidates for major histocompatibility complex and other genetically determined odours. This is the first study on human axillary odour to sample a large number of subjects, and our findings are relevant to understanding the chemical nature of human odour, and efforts to design electronic sensors (e-nose) for biometric fingerprinting and disease diagnoses.

Herbicide sorption to fine particulate matter suspended downwind of agricultural operations: field and laboratory investigations.

PubMed

Clymo, Amelia S; Shin, Jin Young; Holmen, Britt A

2005-01-15

Tillage-induced erosion of herbicides bound to airborne soil particles has not been quantified as a mechanism for offsite herbicide transport. This study quantifies the release of two preemergent herbicides, metolachlor and pendimethalin, to the atmosphere as gas- and particle-phase species during soil incorporation operations. Fine particulate matter (PM2.5) and gas-phase samples were collected at three sampling heights during herbicide disking into the soil in Davis, CA, in May 2000 and May 2001 using filter/PUF sampling. Quartz fiber filters (QFFs) were used in May 2000, and Teflon membrane filters (TMFs) were used in May 2001. The field data were combined with laboratory filter/PUF partitioning experiments to account for adsorption to the filter surfaces and quantify the mass of PM2.5-bound herbicides in the field samples. Laboratory results indicate a significant adsorption of metolachlor, but not pendimethalin, to the quartz filter surfaces. Metolachlor partitioning to PM2.5 collected on TMF filters resulted in corrected PM2.5 field partition coefficient values, Kp,corr = Cp/Cg, of approximately 10(-3.5) m3/microg, indicating its preference for the gas phase. Pendimethalin exhibited more semivolatile behavior,with Kp,corr values that ranged from 10(-3) to 10(-1) m3/ microg and increased with sampling height and distance downwind of the operation. An increase in pendimethalin enrichment at a height of 5 m suggests winnowing of finer, more sorptive soil components with corresponding higher transport potential. Pendimethalin was enriched in the PM2.5 samples by up to a factor of 250 compared to the field soil, indicating thatfurther research on the processes controlling the generation of PM-bound herbicides during agricultural operations is warranted to enable prediction of off-site mass fluxes by this mechanism.

Desorption of polycyclic aromatic hydrocarbons from field-contaminated soil to a two-dimensional hydrophobic surface before and after bioremediation.

PubMed

Hu, Jing; Aitken, Michael D

2012-10-01

Dermal exposure can represent a significant health risk in settings involving potential contact with soil contaminated with polycyclic aromatic hydrocarbons (PAHs). However, there is limited work on the ability of PAHs in contaminated soil to reach the skin surface via desorption from the soil. We evaluated PAH desorption from a field-contaminated soil to a two-dimensional hydrophobic surface (C18 extraction disk) as a measure of potential dermal exposure as a function of soil loading (5-100 mg dry soil cm(-2)), temperature (20-40°C), and soil moisture content (2-40%) over periods up to 16d. The efficacy of bioremediation in removing the most readily desorbable PAH fractions was also evaluated. Desorption kinetics were described well by an empirical two-compartment kinetic model. PAH mass desorbed to the C18 disk kept increasing at soil loadings well above the estimated monolayer coverage, suggesting mechanisms for PAH transport to the surface other than by direct contact. Such mechanisms were reinforced by observations that desorption occurred even with dry or moist glass microfiber filters placed between the C18 disk and the soil. Desorption of all PAHs was substantially reduced at a soil moisture content corresponding to field capacity, suggesting that transport through pore air contributed to PAH transport to the C18 disk. The lower molecular weight PAHs had greater potential to desorb from soil than higher molecular weight PAHs. Biological treatment of the soil in a slurry-phase bioreactor completely eliminated PAH desorption to the C18 disks. Copyright © 2012 Elsevier Ltd. All rights reserved.

Rings of Molecular Line Emission in the Disk Orbiting the Young, Close Binary V4046 Sgr

NASA Astrophysics Data System (ADS)

Dickson-Vandervelde, Dorothy; Kastner, Joel H.; Qi, C.; Forveille, Thierry; Hily-Blant, Pierre; Oberg, Karin; Wilner, David; Andrews, Sean; Gorti, Uma; Rapson, Valerie; Sacco, Germano; Principe, David

2018-01-01

We present analysis of a suite of subarcsecond ALMA Band 6 (1.1 - 1.4 mm) molecular line images of the circumbinary, protoplanetary disk orbiting V4046 Sgr. The ~20 Myr-old V4046 Sgr system, which lies a mere ~73 pc from Earth, consists of a close (separation ~10 Rsun) pair of roughly solar-mass stars that are orbited by a gas-rich crcumbinary disk extending to ~350 AU in radius. The ALMA images reveal that the molecules CO and HCN and their isotopologues display centrally peaked surface brightness morphologies, whereas the cyanide group molecules (HC3N, CH3CN), deuterated molecules (DCN, DCO+), hydrocarbons (as traced by C2H), and potential CO ice line tracers (N2H+, and H2CO) appear as a sequence of sharp and diffuse rings of increasing radii. The characteristic sizes of these molecular emission rings, which range from ~25 to >100 AU in radius, are evident in radial emission-line surface brightness profiles extracted from the deprojected disk images. We find that emission from 13CO emission transitions from optically thin to thick within ~50 AU, whereas C18O emission remains optically thin within this radius. We summarize the insight into the physical and chemical processes within this evolved protoplanetary disk that can be obtained from comparisons of the various emission-line morphologies with each other and with that of the continuum (large-grain) emission on size scales of tens of AU.This research is supported by NASA Exoplanets program grant NNX16AB43G to RIT

Desorption of polycyclic aromatic hydrocarbons from field-contaminated soil to a two-dimensional hydrophobic surface before and after bioremediation

PubMed Central

Hu, Jing; Aitken, Michael D.

2012-01-01

Dermal exposure can represent a significant health risk in settings involving potential contact with soil contaminated with polycyclic aromatic hydrocarbons (PAHs). However, there is limited work on the ability of PAHs in contaminated soil to reach the skin surface via desorption from the soil. We evaluated PAH desorption from a field-contaminated soil to a two-dimensional hydrophobic surface (C18 extraction disk) as a measure of potential dermal exposure as a function of soil loading (5 to 100 mg dry soil/cm2), temperature (20 °C to 40 °C), and soil moisture content (2% to 40%) over periods up to 16 d. The efficacy of bioremediation in removing the most readily desorbable PAH fractions was also evaluated. Desorption kinetics were described well by an empirical two-compartment kinetic model. PAH mass desorbed to the C18 disk kept increasing at soil loadings well above the estimated monolayer coverage, suggesting mechanisms for PAH transport to the surface other than by direct contact. Such mechanisms were reinforced by observations that desorption occurred even with dry or moist glass microfiber filters placed between the C18 disk and the soil. Desorption of all PAHs was substantially reduced at a soil moisture content corresponding to field capacity, suggesting that transport through pore air contributed to PAH transport to the C18 disk. The lower molecular weight PAHs had greater potential to desorb from soil than higher molecular weight PAHs. Biological treatment of the soil in a slurry-phase bioreactor completely eliminated PAH desorption to the C18 disks. PMID:22704210

Torque Enhancement, Spin Equilibrium, and Jet Power from Disk-Induced Opening of Pulsar Magnetic Fields

NASA Astrophysics Data System (ADS)

Parfrey, Kyle; Spitkovsky, Anatoly; Beloborodov, Andrei M.

2016-05-01

The interaction of a rotating star’s magnetic field with a surrounding plasma disk lies at the heart of many questions posed by neutron stars in X-ray binaries. We consider the opening of stellar magnetic flux due to differential rotation along field lines coupling the star and disk, using a simple model for the disk-opened flux, the torques exerted on the star by the magnetosphere, and the power extracted by the electromagnetic wind. We examine the conditions under which the system enters an equilibrium spin state, in which the accretion torque is instantaneously balanced by the pulsar wind torque alone. For magnetic moments, spin frequencies, and accretion rates relevant to accreting millisecond pulsars, the spin-down torque from this enhanced pulsar wind can be substantially larger than that predicted by existing models of the disk-magnetosphere interaction, and is in principle capable of maintaining spin equilibrium at frequencies less than 1 kHz. We speculate that this mechanism may account for the non-detection of frequency increases during outbursts of SAX J1808.4-3658 and XTE J1814-338, and may be generally responsible for preventing spin-up to sub-millisecond periods. If the pulsar wind is collimated by the surrounding environment, the resulting jet can satisfy the power requirements of the highly relativistic outflows from Cir X-1 and Sco X-1. In this framework, the jet power scales relatively weakly with accretion rate, {L}{{j}}\\propto {\\dot{M}}4/7, and would be suppressed at high accretion rates only if the stellar magnetic moment is sufficiently low.

Bioactivity of Malva Sylvestris L., a Medicinal Plant from Iran

PubMed Central

Razavi, Seyed Mehdi; Zarrini, Gholamreza; Molavi, Ghader; Ghasemi, Ghader

2011-01-01

Objective(s) Malva sylvestris L. (Malvaceae), an annual plant, has been already commonly used as a medicinal plant in Iran. In the present work, we evaluate some bioactivities of the plant extracts. Materials and Methods The aired-dried plant flowers and leaves were extracted by soxhlet apparatus with n-hexane, dichloromethane and methanol. The antimicrobial, cytotoxic, and phytotoxic of the plant extracts were evaluated using disk diffusion method, MTT, and Lettuce assays, respectively. Results Both flowers and leaves of M. sylvestris methanol extracts exhibited strong antibacterial effects against Erwinia carotovora, a plant pathogen, with MIC value of 128 and 256 µg/ml, respectively. The flowers extract also showed high antibacterial effects against some human pathogen bacteria strains such as Staphylococcus aureus, Streptococcus agalactiae, Entrococcus faecalis, with MIC value of 192, 200 and 256 µg/ml, respectively. The plant methanol extracts had relatively high cytotoxic activity against MacCoy cell line. Conclusion We concluded that Malva sylvestris can be candidated as an antiseptic, a chemopreventive or a chemotherapeutic agent. PMID:23493458

Rotor Wake Vortex Definition: Initial Evaluation of 3-C PIV Results of the Hart-II Study

NASA Technical Reports Server (NTRS)

Burley, Casey L.; Brooks, Thomas F.; vanderWall, Berend; Richard, Hughes; Raffel, Markus; Beaumier, Philippe; Delrieux, Yves; Lim, Joon W.; Yu, Yung H.; Tung, Chee

2002-01-01

An initial evaluation is made of extensive three-component (3C) particle image velocimetry (PIV) measurements within the wake across a rotor disk plane. The model is a 40 percent scale BO-105 helicopter main rotor in forward flight simulation. This study is part of the HART II test program conducted in the German-Dutch Wind Tunnel (DNW). Included are wake vortex field measurements over the advancing and retreating sides of the rotor operating at a typical descent landing condition important for impulsive blade-vortex interaction (BVI) noise. Also included are advancing side results for rotor angle variations from climb to steep descent. Using detailed PIV vector maps of the vortex fields, methods of extracting key vortex parameters are examined and a new method was developed and evaluated. An objective processing method, involving a center-of-vorticity criterion and a vorticity 'disk' integration, was used to determine vortex core size, strength, core velocity distribution characteristics, and unsteadiness. These parameters are mapped over the rotor disk and offer unique physical insight for these parameters of importance for rotor noise and vibration prediction.

Velocity Data in a Fully Developed Wind Turbine Array Boundary Layer

NASA Astrophysics Data System (ADS)

Turner, John; Wosnik, Martin

2016-11-01

Results are reported from an experimental study of an array of porous disks simulating offshore wind turbines. The disks mimic power extraction of similarly scaled wind turbines via drag matching, and the array consists of 19x5 disks of 0.25 m diameter. The study was conducted in the UNH Flow Physics Facility (FPF), which has test section dimensions of 6.0 m wide, 2.7 m high and 72.0 m long. The FPF can achieve a boundary layer height on the order of 1 m at the entrance of the wind turbine array which puts the model turbines in the bottom third of the boundary layer, which is typical of field application. Careful consideration was given to an expanded uncertainty analysis, to determine possible measurements in this type of flow. For a given configuration (spacing, initial conditions, etc.), the velocity levels out and the wind farm approaches fully developed behavior, even within the maintained growth of the simulated atmospheric boundary layer. Benchmark pitot tube data was acquired in vertical profiles progressing streamwise behind the centered column at every row in the array.

ALMA Shows that Gas Reservoirs of Star-forming Disks over the Past 3 Billion Years Are Not Predominantly Molecular

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

Cortese, Luca; Catinella, Barbara; Janowiecki, Steven, E-mail: luca.cortese@uwa.edu.au

Cold hydrogen gas is the raw fuel for star formation in galaxies, and its partition into atomic and molecular phases is a key quantity for galaxy evolution. In this Letter, we combine Atacama Large Millimeter/submillimeter Array and Arecibo single-dish observations to estimate the molecular-to-atomic hydrogen mass ratio for massive star-forming galaxies at z ∼ 0.2 extracted from the HIGHz survey, i.e., some of the most massive gas-rich systems currently known. We show that the balance between atomic and molecular hydrogen in these galaxies is similar to that of local main-sequence disks, implying that atomic hydrogen has been dominating the coldmore » gas mass budget of star-forming galaxies for at least the past three billion years. In addition, despite harboring gas reservoirs that are more typical of objects at the cosmic noon, HIGHz galaxies host regular rotating disks with low gas velocity dispersions suggesting that high total gas fractions do not necessarily drive high turbulence in the interstellar medium.« less

Vibrissal touch sensing in the harbor seal (Phoca vitulina): how do seals judge size?

PubMed

Grant, Robyn; Wieskotten, Sven; Wengst, Nina; Prescott, Tony; Dehnhardt, Guido

2013-06-01

"Whisker specialists" such as rats, shrews, and seals actively employ their whiskers to explore their environments and extract object properties such as size, shape, and texture. It has been suggested that whiskers could be used to discriminate between different sized objects in one of two ways: (i) to use whisker positions, such as angular position, spread or amplitude to approximate size; or (ii) to calculate the number of whiskers that contact an object. This study describes in detail how two adult harbor seals use their whiskers to differentiate between three sizes of disk. The seals judged size very fast, taking <400 ms. In addition, they oriented their smaller, most rostral, ventral whiskers to the disks, so that more whiskers contacted the surface, complying to a maximal contact sensing strategy. Data from this study supports the suggestion that it is the number of whisker contacts that predict disk size, rather than how the whiskers are positioned (angular position), the degree to which they are moved (amplitude) or how spread out they are (angular spread).

Inhibition of Listeria monocytogenes in Fish and Meat Systems by Use of Oregano and Cranberry Phytochemical Synergies

PubMed Central

Lin, Y. T.; Labbe, R. G.; Shetty, Kalidas

2004-01-01

Optimized phenolics from oregano and cranberry extracts were evaluated for antimicrobial activity against Listeria monocytogenes in laboratory media and in beef and fish. The antimicrobial activity increased when oregano and cranberry extracts were mixed at a ratio of 75% oregano and 25% cranberry (wt/wt) with 0.1 mg of phenolic per disk or ml, and the efficacy was further enhanced by lactic acid. The inhibition by phytochemical and lactic acid synergies was most effective when beef and fish slices were stored at 4°C. PMID:15345457

Prediction of the Critical Curvature for LX-17 with the Time of Arrival Data from DNS

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

Yao, Jin; Fried, Laurence E.; Moss, William C.

2017-01-10

We extract the detonation shock front velocity, curvature and acceleration from time of arrival data measured at grid points from direct numerical simulations of a 50mm rate-stick lit by a disk-source, with the ignition and growth reaction model and a JWL equation of state calibrated for LX-17. We compute the quasi-steady (D, κ) relation based on the extracted properties and predicted the critical curvatures of LX-17. We also proposed an explicit formula that contains the failure turning point, obtained from optimization for the (D, κ) relation of LX-17.

Feasibility of Isotope Harvesting at a Projectile Fragmentation Facility: 67Cu

PubMed Central

Mastren, Tara; Pen, Aranh; Peaslee, Graham F.; Wozniak, Nick; Loveless, Shaun; Essenmacher, Scott; Sobotka, Lee G.; Morrissey, David J.; Lapi, Suzanne E.

2014-01-01

The work presented here describes a proof-of-principle experiment for the chemical extraction of 67Cu from an aqueous beam stop at the National Superconducting Cyclotron Laboratory (NSCL). A 76 MeV/A 67Cu beam was stopped in water, successfully isolated from the aqueous solution through a series of chemical separations involving a chelating disk and anion exchange chromatography, then bound to NOTA-conjugated Herceptin antibodies, and the bound activity was validated using instant thin-layer chromatography (ITLC). The chemical extraction efficiency was found to be 88 ± 3% and the radiochemical yield was ≥95%. These results show that extraction of radioisotopes from an aqueous projectile-fragment beam dump is a feasible method for obtaining radiochemically pure isotopes. PMID:25330839

Sorptive fractionation of organic matter and formation of organo-hydroxy-aluminum complexes during litter biodegradation in the presence of gibbsite

Treesearch

K. Heckman; A.S. Grandy; X. Gao; M. Keiluweit; K. Wickings; K. Carpenter; J. Chorover; C. Rasmussen

2013-01-01

Solid and aqueous phase Al species are recognized to affect organic matter (OM) stabilization in forest soils. However, little is known about the dynamics of formation, composition and dissolution of organo-Al hydroxide complexes in microbially-active soil systems, where plant litter is subject to microbial decomposition in close proximity to mineral weathering...

Wood chemical composition as related to properties of handsheets made from loblolly pine refiner groundwood

Treesearch

Charles W. McMillin

1969-01-01

Burst and tear strengths of handsheets made from 48 pulps disk-refined from chips of varying chemical composition decreased with incressing extractive content after the independent effects of fiber morphology were specified. This result was attributed to lessened bond strength caused by reduced surface tension forces and blocking of reactive sites on the fiber surfaces...

Scent trailing by virgin females ofPseudococcm calceolariae.

PubMed

Rotundo, G; Tremblay, E

1981-01-01

Virgin females of the citrophilous mealybugPseudococcus calceolariae (Mask.) deposit scent marks as trails on the substrate on which they rest or move. These substances elicit attraction and sexual behavior by conspecific males. The same responses were obtained when males were bioassayed on extracts from filter paper disks on which females had rested. The significance of scent trailing in mealybugs is discussed.

Application of Artificial Intelligence to the Prediction of the Antimicrobial Activity of Essential Oils.

PubMed

Daynac, Mathieu; Cortes-Cabrera, Alvaro; Prieto, Jose M

2015-01-01

Essential oils (EOs) are vastly used as natural antibiotics in Complementary and Alternative Medicine (CAM). Their intrinsic chemical variability and synergisms/antagonisms between its components make difficult to ensure consistent effects through different batches. Our aim is to evaluate the use of artificial neural networks (ANNs) for the prediction of their antimicrobial activity. Methods. The chemical composition and antimicrobial activity of 49 EOs, extracts, and/or fractions was extracted from NCCLS compliant works. The fast artificial neural networks (FANN) software was used and the output data reflected the antimicrobial activity of these EOs against four common pathogens: Staphylococcus aureus, Escherichia coli, Candida albicans, and Clostridium perfringens as measured by standardised disk diffusion assays. Results. ANNs were able to predict >70% of the antimicrobial activities within a 10 mm maximum error range. Similarly, ANNs were able to predict 2 or 3 different bioactivities at the same time. The accuracy of the prediction was only limited by the inherent errors of the popular antimicrobial disk susceptibility test and the nature of the pathogens. Conclusions. ANNs can be reliable, fast, and cheap tools for the prediction of the antimicrobial activity of EOs thus improving their use in CAM.

In vitro antibacterial effects of glass-ionomer cement containing ethanolic extract of propolis on Streptococcus mutans

PubMed Central

Topcuoglu, Nursen; Ozan, Fatih; Ozyurt, Mustafa; Kulekci, Guven

2012-01-01

Objective: The aim of this study was to evaluate the antibacterial property of glass-ionomer cement (GIC) containing propolis against Streptococcus mutans and its effect on the in vitro S. mutans biofilm formation. Methods: Ethanolic extract of propolis (EEP) was prepared at two concentrations as 25 and 50%. Three different experimental GIC disks were prepared using pure liquid and liquid solutions diluted with 25 and 50 percent of EEP concentrations. Minimum inhibitory concentration (MIC) of EEP on the growth of S. mutans ATCC 25175 was determined by using agar dilution method. Agar diffusion test and an in vitro S. mutans biofilm assay for GIC disks with and without EEP were performed. Results: MIC values of Turkish propolis for S. mutans ATCC 25175 was found as 25 μg/mL. Experimental GICs containing propolis exhibited inhibition zones and their dry biofilm weights were less than the pure GIC. The bacterial density was lower in the GIC containing 50% EEP. Conclusions: A distinct antibacterial and antibiofilm efficacy of propolis containing GIC on S. mutans has been observed. Although further research is needed to show clinical results, antibacterial GIC containing propolis would be a promising material for restoration. PMID:23077424

Application of Artificial Intelligence to the Prediction of the Antimicrobial Activity of Essential Oils

PubMed Central

Daynac, Mathieu; Cortes-Cabrera, Alvaro; Prieto, Jose M.

2015-01-01

Essential oils (EOs) are vastly used as natural antibiotics in Complementary and Alternative Medicine (CAM). Their intrinsic chemical variability and synergisms/antagonisms between its components make difficult to ensure consistent effects through different batches. Our aim is to evaluate the use of artificial neural networks (ANNs) for the prediction of their antimicrobial activity. Methods. The chemical composition and antimicrobial activity of 49 EOs, extracts, and/or fractions was extracted from NCCLS compliant works. The fast artificial neural networks (FANN) software was used and the output data reflected the antimicrobial activity of these EOs against four common pathogens: Staphylococcus aureus, Escherichia coli, Candida albicans, and Clostridium perfringens as measured by standardised disk diffusion assays. Results. ANNs were able to predict >70% of the antimicrobial activities within a 10 mm maximum error range. Similarly, ANNs were able to predict 2 or 3 different bioactivities at the same time. The accuracy of the prediction was only limited by the inherent errors of the popular antimicrobial disk susceptibility test and the nature of the pathogens. Conclusions. ANNs can be reliable, fast, and cheap tools for the prediction of the antimicrobial activity of EOs thus improving their use in CAM. PMID:26457111

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

PubMed

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

2018-07-15

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

Fine structure of modal focusing effect in a three dimensional plasma-sheath-lens formed by disk electrodes

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

Stamate, Eugen, E-mail: eust@dtu.dk; Venture Business Laboratory, Nagoya University, C3-1, Chikusa-ku, Nagoya 464-8603; Yamaguchi, Masahito

2015-08-31

Modal and discrete focusing effects associated with three-dimensional plasma-sheath-lenses show promising potential for applications in ion beam extraction, mass spectrometry, plasma diagnostics and for basic studies of plasma sheath. The ion focusing properties can be adjusted by controlling the geometrical structure of the plasma-sheath-lens and plasma parameters. The positive and negative ion kinetics within the plasma-sheath-lens are investigated both experimentally and theoretically and a modal focusing ring is identified on the surface of disk electrodes. The focusing ring is very sensitive to the sheath thickness and can be used to monitor very small changes in plasma parameters. Three dimensional simulationsmore » are found to be in very good agreement with experiments.« less

Solid-phase extraction of some heavy metal ions on a double-walled carbon nanotube disk and determination by flame atomic absorption spectrometry.

PubMed

Karatepe, Aslihan; Soylak, Mustafa; Elçi, Latif

2011-01-01

A new preconcentration method was developed for the determination of trace amounts of Cu(II), Fe(III), Pb(II), Ni(II), and Cd(II) on a double-walled carbon nanotube disk. 4-(2-Thiazolylazo) resorcinol was used as a complexing reagent. The effects of parameters, including pH of the solutions, amounts of complexing reagent, eluent type, sample volume, flow rates of solutions, and matrix ions were examined for quantitative recoveries of the studied analyte ions. The retained metal ions were eluted by 2 M HNO3. The LOD values for the analytes were in the range of 0.7-4.4 microg/mL. Natural water samples and standard reference materials were analyzed by the presented method.

Evaluation of Amount of Blood in Dry Blood Spots: Ring-Disk Electrode Conductometry.

PubMed

Kadjo, Akinde F; Stamos, Brian N; Shelor, C Phillip; Berg, Jordan M; Blount, Benjamin C; Dasgupta, Purnendu K

2016-06-21

A fixed area punch in dried blood spot (DBS) analysis is assumed to contain a fixed amount of blood, but the amount actually depends on a number of factors. The presently preferred approach is to normalize the measurement with respect to the sodium level, measured by atomic spectrometry. Instead of sodium levels, we propose electrical conductivity of the extract as an equivalent nondestructive measure. A dip-type small diameter ring-disk electrode (RDE) is ideal for very small volumes. However, the conductance (G) measured by an RDE depends on the depth (D) of the liquid below the probe. There is no established way of computing the specific conductance (σ) of the solution from G. Using a COMSOL Multiphysics model, we were able to obtain excellent agreement between the measured and the model predicted conductance as a function of D. Using simulations over a large range of dimensions, we provide a spreadsheet-based calculator where the RDE dimensions are the input parameters and the procedure determines the 99% of the infinite depth conductance (G99) and the depth D99 at which this is reached. For typical small diameter probes (outer electrode diameter ∼ <2 mm), D99 is small enough for dip-type measurements in extract volumes of ∼100 μL. We demonstrate the use of such probes with DBS extracts. In a small group of 12 volunteers (age 20-66), the specific conductance of 100 μL aqueous extracts of 2 μL of spotted blood showed a variance of 17.9%. For a given subject, methanol extracts of DBS spots nominally containing 8 and 4 μL of blood differed by a factor of 1.8-1.9 in the chromatographically determined values of sulfate and chloride (a minor and major constituent, respectively). The values normalized with respect to the conductance of the extracts differed by ∼1%. For serum associated analytes, normalization of the analyte value by the extract conductance can thus greatly reduce errors from variations in the spotted blood volume/unit area.

Comperative studies with Culex pipiens egg rafts. Immunogenetic, electrophoretic and enzymatic analysis of unfertilized, compatible and incompatible fertilized eggs.

PubMed

Schumann, W

1974-01-01

By applying immunologic, electrophoretic and enzymatic methods, extracts of different raft types of Culex pipiens were analysed. Rafts of the crosses Pa x Pa and Ha x Ha contained four common antigens, while unfertilized rafts of Pa and Ha (no antisera were prepared against them) and rafts of the crosses Og x Og, Og x Pa, and Pa x Og shared three common antigens with the remaining raft extracts. Disk-electrophoresis of raft extracts in acrylamide gel resulted in different electropherograms. Ten protein bands were common to all these raft types. The unfertilized rafts of Pa and Ha yielded three more protein bands, the crosses Pa x Ha and Ha x Pa one more, the crosses Og x Og and Pa x Og three more, and Og x Pa two more. Many enzymes were demonstrated in the raft extracts after they were separated in acrylamide gel and incubated with the corresponding substrate solutions. All the raft types possessed one enzyme type for glutaminate-, lactate-, glucose-6-phosphate-dehydrogenase and catalase. Malate-dehydrogenase and leucine aminopeptidase occurred in each raft type as two isoenzymes. Alkaline phosphatase was observed as a single enzyme, but was lacking in rafts of the crosses Pa X Pa and Ha X Ha. While rafts of the crosses Og x Og and Og x Pa possessed two acid phosphatases, three could be demonstrated for the remaining raft types. Up to eight esterases appeared; rafts of the crosses Og x Og and Og x Pa possessed seven such activities. The results obtained by the Ouchterlony test, disk-electrophoresis and the histochemical enzyme tests are discussed in context and checked according to the phenomenon of incompatibility.

K-65-12.8 condensing steam turbine

NASA Astrophysics Data System (ADS)

Valamin, A. E.; Kultyshev, A. Yu.; Gol'dberg, A. A.; Sakhnin, Yu. A.; Bilan, V. N.; Stepanov, M. Yu.; Polyaeva, E. N.; Shekhter, M. V.; Shibaev, T. L.

2016-11-01

A new condensing steam turbine K-65-12.8 is considered, which is the continuation of the development of the steam turbine family of 50-70 MW and the fresh steam pressure of 12.8 MPa, such as twocylinder T-50-12.8 and T-60/65-12.8 turbines. The turbine was developed using the modular design. The design and the main distinctive features of the turbine are described, such as a single two-housing cylinder with the steam flow loop; the extraction from the blading section for the regeneration, the inner needs, and heating; and the unification of some assemblies of serial turbines with shorter time of manufacture. The turbine uses the throttling steam distribution; steam from a boiler is supplied to a turbine through a separate valve block consisting of a central shut-off valve and two side control valves. The blading section of a turbine consists of 23 stages: the left flow contains ten stages installed in the inner housing and the right flow contains 13 stages with diaphragm placed in holders installed in the outer housing. The disks of the first 16 stages are forged together with a rotor, and the disks of the rest stages are mounted. Before the two last stages, the uncontrolled steam extraction is performed for the heating of a plant with the heat output of 38-75 GJ/h. Also, a turbine has five regenerative extraction points for feed water heating and the additional steam extraction to a collector for the inner needs with the consumption of up to 10 t/h. The feasibility parameters of a turbine plant are given. The main solutions for the heat flow diagram and the layout of a turbine plant are presented. The main principles and features of the microprocessor electro hydraulic control and protection system are formulated.

Determination of perfluorinated chemicals in food and drinking water using high-flow solid-phase extraction and ultra-high performance liquid chromatography/tandem mass spectrometry.

PubMed

Chang, Ying-Chia; Chen, Wen-Ling; Bai, Fang-Yu; Chen, Pau-Chung; Wang, Gen-Shuh; Chen, Chia-Yang

2012-01-01

For this study, we developed methods of determining ten perfluorinated chemicals in drinking water, milk, fish, beef, and pig liver using high-flow automated solid-phase extraction (SPE) and ultra-high performance liquid chromatography/tandem mass spectrometry. The analytes were separated on a core-shell Kinetex C18 column. The mobile phase was composed of methanol and 10-mM N-methylmorpholine. Milk was digested with 0.5 N potassium hydroxide in Milli-Q water, and was extracted with an Atlantic HLB disk to perform automated SPE at a flow rate ranged from 70 to 86 mL/min. Drinking water was directly extracted by the SPE. Solid food samples were digested in alkaline methanol and their supernatants were diluted and also processed by SPE. The disks were washed with 40% methanol/60% water and then eluted with 0.1% ammonium hydroxide in methanol. Suppression of signal intensity of most analytes by matrixes was lower than 50%; it was generally lower in fish and drinking water but higher in liver. Most quantitative biases and relative standard deviations were lower than 15%. The limits of detection for most analytes were sub-nanograms per liter for drinking water and sub-nanograms per gram for solid food samples. This method greatly shortened the time and labor needed for digestion, SPE, and liquid chromatography. This method has been applied to analyze 14 types of food samples. Perfluorooctanoic acid was found to be the highest among the analytes (median at 3.2-64 ng/g wet weight), followed by perfluorodecanoic acid (0.7-25 ng/g) and perfluorododecanoic acid (0.6-15 ng/g).

An Optical/Near-infrared Investigation of HD 100546 b with the Gemini Planet Imager and MagAO

NASA Astrophysics Data System (ADS)

Rameau, Julien; Follette, Katherine B.; Pueyo, Laurent; Marois, Christian; Macintosh, Bruce; Millar-Blanchaer, Maxwell; Wang, Jason J.; Vega, David; Doyon, René; Lafrenière, David; Nielsen, Eric L.; Bailey, Vanessa; Chilcote, Jeffrey K.; Close, Laird M.; Esposito, Thomas M.; Males, Jared R.; Metchev, Stanimir; Morzinski, Katie M.; Ruffio, Jean-Baptiste; Wolff, Schuyler G.; Ammons, S. M.; Barman, Travis S.; Bulger, Joanna; Cotten, Tara; De Rosa, Robert J.; Duchene, Gaspard; Fitzgerald, Michael P.; Goodsell, Stephen; Graham, James R.; Greenbaum, Alexandra Z.; Hibon, Pascale; Hung, Li-Wei; Ingraham, Patrick; Kalas, Paul; Konopacky, Quinn; Larkin, James E.; Maire, Jérôme; Marchis, Franck; Oppenheimer, Rebecca; Palmer, David; Patience, Jennifer; Perrin, Marshall D.; Poyneer, Lisa; Rajan, Abhijith; Rantakyrö, Fredrik T.; Marley, Mark S.; Savransky, Dmitry; Schneider, Adam C.; Sivaramakrishnan, Anand; Song, Inseok; Soummer, Remi; Thomas, Sandrine; Wallace, J. Kent; Ward-Duong, Kimberly; Wiktorowicz, Sloane

2017-06-01

We present H band spectroscopic and Hα photometric observations of HD 100546 obtained with the Gemini Planet Imager and the Magellan Visible AO camera. We detect H band emission at the location of the protoplanet HD 100546 b, but show that the choice of data processing parameters strongly affects the morphology of this source. It appears point-like in some aggressive reductions, but rejoins an extended disk structure in the majority of the others. Furthermore, we demonstrate that this emission appears stationary on a timescale of 4.6 years, inconsistent at the 2σ level with a Keplerian clockwise orbit at 59 au in the disk plane. The H band spectrum of the emission is inconsistent with any type of low effective temperature object or accreting protoplanetary disk. It strongly suggests a scattered-light origin, as this is consistent with the spectrum of the star and the spectra extracted at other locations in the disk. A non-detection at the 5σ level of HD 100546 b in differential Hα imaging places an upper limit, assuming the protoplanet lies in a gap free of extinction, on the accretion luminosity of 1.7 × 10-4 L ⊙ and M\\dot{M}< 6.3× {10}-7 {M}{Jup}2 {{yr}}-1 for 1 R Jup. These limits are comparable to the accretion luminosity and accretion rate of T-Tauri stars or LkCa 15 b. Taken together, these lines of evidence suggest that the H band source at the location of HD 100546 b is not emitted by a planetary photosphere or an accreting circumplanetary disk but is a disk feature enhanced by the point-spread function subtraction process. This non-detection is consistent with the non-detection in the K band reported in an earlier study but does not exclude the possibility that HD 100546 b is deeply embedded.

Influence of different luting protocols on shear bond strength of computer aided design/computer aided manufacturing resin nanoceramic material to dentin

PubMed Central

Poggio, Claudio; Pigozzo, Marco; Ceci, Matteo; Scribante, Andrea; Beltrami, Riccardo; Chiesa, Marco

2016-01-01

Background: The purpose of this study was to evaluate the influence of three different luting protocols on shear bond strength of computer aided design/computer aided manufacturing (CAD/CAM) resin nanoceramic (RNC) material to dentin. Materials and Methods: In this in vitro study, 30 disks were milled from RNC blocks (Lava Ultimate/3M ESPE) with CAD/CAM technology. The disks were subsequently cemented to the exposed dentin of 30 recently extracted bovine permanent mandibular incisors. The specimens were randomly assigned into 3 groups of 10 teeth each. In Group 1, disks were cemented using a total-etch protocol (Scotchbond™ Universal Etchant phosphoric acid + Scotchbond Universal Adhesive + RelyX™ Ultimate conventional resin cement); in Group 2, disks were cemented using a self-etch protocol (Scotchbond Universal Adhesive + RelyX™ Ultimate conventional resin cement); in Group 3, disks were cemented using a self-adhesive protocol (RelyX™ Unicem 2 Automix self-adhesive resin cement). All cemented specimens were placed in a universal testing machine (Instron Universal Testing Machine 3343) and submitted to a shear bond strength test to check the strength of adhesion between the two substrates, dentin, and RNC disks. Specimens were stressed at a crosshead speed of 1 mm/min. Data were analyzed with analysis of variance and post-hoc Tukey's test at a level of significance of 0.05. Results: Post-hoc Tukey testing showed that the highest shear strength values (P < 0.001) were reported in Group 2. The lowest data (P < 0.001) were recorded in Group 3. Conclusion: Within the limitations of this in vitro study, conventional resin cements (coupled with etch and rinse or self-etch adhesives) showed better shear strength values compared to self-adhesive resin cements. Furthermore, conventional resin cements used together with a self-etch adhesive reported the highest values of adhesion. PMID:27076822

Influence of different luting protocols on shear bond strength of computer aided design/computer aided manufacturing resin nanoceramic material to dentin.

PubMed

Poggio, Claudio; Pigozzo, Marco; Ceci, Matteo; Scribante, Andrea; Beltrami, Riccardo; Chiesa, Marco

2016-01-01

The purpose of this study was to evaluate the influence of three different luting protocols on shear bond strength of computer aided design/computer aided manufacturing (CAD/CAM) resin nanoceramic (RNC) material to dentin. In this in vitro study, 30 disks were milled from RNC blocks (Lava Ultimate/3M ESPE) with CAD/CAM technology. The disks were subsequently cemented to the exposed dentin of 30 recently extracted bovine permanent mandibular incisors. The specimens were randomly assigned into 3 groups of 10 teeth each. In Group 1, disks were cemented using a total-etch protocol (Scotchbond™ Universal Etchant phosphoric acid + Scotchbond Universal Adhesive + RelyX™ Ultimate conventional resin cement); in Group 2, disks were cemented using a self-etch protocol (Scotchbond Universal Adhesive + RelyX™ Ultimate conventional resin cement); in Group 3, disks were cemented using a self-adhesive protocol (RelyX™ Unicem 2 Automix self-adhesive resin cement). All cemented specimens were placed in a universal testing machine (Instron Universal Testing Machine 3343) and submitted to a shear bond strength test to check the strength of adhesion between the two substrates, dentin, and RNC disks. Specimens were stressed at a crosshead speed of 1 mm/min. Data were analyzed with analysis of variance and post-hoc Tukey's test at a level of significance of 0.05. Post-hoc Tukey testing showed that the highest shear strength values (P < 0.001) were reported in Group 2. The lowest data (P < 0.001) were recorded in Group 3. Within the limitations of this in vitro study, conventional resin cements (coupled with etch and rinse or self-etch adhesives) showed better shear strength values compared to self-adhesive resin cements. Furthermore, conventional resin cements used together with a self-etch adhesive reported the highest values of adhesion.

Synergy between antibiotics and natural agents results in increased antimicrobial activity against Staphylococcus epidermidis.

PubMed

Abidi, Syed Hani; Ahmed, Khalid; Sherwani, Sikander Khan; Kazmi, Shahana Urooj

2015-09-27

Staphylococcus epidermidis is one of the most frequent causes of biofilm-associated infections on indwelling medical devices. With the emergence of methicillin-resistant S. epidermidis (MRSE), there is an urgent need to discover novel active agents against a range of Gram-positive pathogens. We screened the clinical isolates of S. epidermidis for susceptibility/resistance against commonly prescribed antibiotics. Furthermore, we tested some natural agents alone and in combination with antibiotics to find possible synergistic antimicrobial effects. S. epidermidis clinical isolates were screened for susceptibility/resistance against vancomycin, erythromycin, tetracycline, chloramphenicol, ampicillin, ofloxacin, cephalexin, and gentamicin using the Kirby-Bauer disk diffusion method. The antimicrobial potential of Camellia sinensis, Juglans regia, and Hippophae rhamnoides alone and in combination with antibiotics were examined using the disk diffusion method, where the antimicrobial potential activity was measured in terms of formation of zones of inhibition. Most S. epidermidis isolates were found to be resistant to one or more antibiotics. Gentamycin and ofloxacin were found to be the most effective antibiotics against S. epidermidis isolates. Extracts of Hippophae rhamnoides, Juglans regia, and Camellia sinensis were found to be equally effective against S. epidermidis isolates. In combination with antibiotics, these extracts exhibited appreciable synergistic activity; the highest synergistic activity was observed with erythromycin and cephalexin. In the case of cephalexin, a reversion in resistance was observed. The plant extracts used in the study exhibited additive and synergistic antibacterial activity against S. epidermidis, hence providing an effective alternative to deal with the problem of multidrug resistance.

Optimal control of energy extraction in LES of large wind farms

NASA Astrophysics Data System (ADS)

Meyers, Johan; Goit, Jay; Munters, Wim

2014-11-01

We investigate the use of optimal control combined with Large-Eddy Simulations (LES) of wind-farm boundary layer interaction for the increase of total energy extraction in very large ``infinite'' wind farms and in finite farms. We consider the individual wind turbines as flow actuators, whose energy extraction can be dynamically regulated in time so as to optimally influence the turbulent flow field, maximizing the wind farm power. For the simulation of wind-farm boundary layers we use large-eddy simulations in combination with an actuator-disk representation of wind turbines. Simulations are performed in our in-house pseudo-spectral code SP-Wind. For the optimal control study, we consider the dynamic control of turbine-thrust coefficients in the actuator-disk model. They represent the effect of turbine blades that can actively pitch in time, changing the lift- and drag coefficients of the turbine blades. In a first infinite wind-farm case, we find that farm power is increases by approximately 16% over one hour of operation. This comes at the cost of a deceleration of the outer layer of the boundary layer. A detailed analysis of energy balances is presented, and a comparison is made between infinite and finite farm cases, for which boundary layer entrainment plays an import role. The authors acknowledge support from the European Research Council (FP7-Ideas, Grant No. 306471). Simulations were performed on the computing infrastructure of the VSC Flemish Supercomputer Center, funded by the Hercules Foundation and the Flemish Govern.

Colorimetric Solid Phase Extraction (CSPE): Using Color to Monitor Spacecraft Water Quality

NASA Technical Reports Server (NTRS)

Gazda, Daniel B.; Nolan, Daniel J.; Rutz, Jeffrey A.; Schultz, John R.; Siperko, Lorraine M.; Porter, Marc D.; Lipert, Robert J.; Flint, Stephanie M.; McCoy, J. Torin

2010-01-01

In August 2009, an experimental water quality monitoring kit based on Colorimetric Solid Phase Extraction (CSPE) technology was delivered to the International Space Station (ISS). The kit, called the Colorimetric Water Quality Monitoring Kit (CWQMK), was launched as a Station Development Test Objective (SDTO) experiment to evaluate the suitability of CSPE technology for routine use monitoring water quality on the ISS. CSPE is a sorption-spectrophotometric technique that combines colorimetric reagents, solid-phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water samples. In CSPE, a known volume of sample is metered through a membrane disk that has been impregnated with an analyte-specific colorimetric reagent and any additives required to optimize the formation of the analyte-reagent complex. As the sample flows through the membrane disk, the target analyte is selectively extracted, concentrated, and complexed. Formation of the analyte-reagent complex causes a detectable change in the color of the membrane disk that is proportional to the amount of analyte present in the sample. The analyte is then quantified by measuring the color of the membrane disk surface using a hand-held diffuse reflectance spectrophotometer (DRS). The CWQMK provides the capability to measure the ionic silver (Ag +) and molecular iodine (I2) in water samples on-orbit. These analytes were selected for the evaluation of CSPE technology because they are the biocides used in the potable water storage and distribution systems on the ISS. Biocides are added to the potable water systems on spacecraft to inhibit microbial growth. On the United States (US) segment of the ISS molecular iodine serves as the biocide, while the Russian space agency utilizes silver as a biocide in their systems. In both cases, the biocides must be maintained at a level sufficient to control bacterial growth, but low enough to avoid any negative effects on crew health. For example, the presence of high levels of iodine in water can cause taste and odor issues that result in decreased water consumption by the crew. There are also concerns about potential impacts on thyroid function following exposure to high levels of iodine. With silver, there is a risk of developing argyria, an irreversible blue-gray discoloration of the skin, associated with long term consumption of water containing high concentrations of silver. The need to ensure that safe, effective levels of biocide are maintained in the potable water systems on the ISS provides a perfect platform for evaluating the suitability of CSPE technology for in-flight water quality monitoring. This paper provides an overview of CSPE technology and details on the silver and iodine methods used in the CWQMK. It also reports results obtained during in-flight analyses performed with the CWQMK and briefly discusses other potential applications for CSPE technology in both the spacecraft and terrestrial environments.

Antifungal effect of some plant extracts against factors wheat root rot

NASA Astrophysics Data System (ADS)

Atmaca, Sevim; Şimşek, Şeyda; Denek, Yunus Emre

2017-04-01

Methanol leaf extracts of Humulus lupulus L. and Achillea millefolium L. were evaluated for antifungal activity against economically important phytopathogenic fungi including Fusarium culmorum (W. G. Smith) Sacc. The final concentrations of the methanol extracts obtained from the plants were added to the Potato Dextrose Agar (PDA) at 1%, 2%, 4% and 8% doses. Mycelial disks of pathogens (6 mm in diameter) removed from the margins of a 7 days old culture were transferred to PDA media containing the plant extracts at tested concentrations. Four replicates were used per treatment. For each plant extract and concentration, inhibition of radial growth compared with the untreated control was calculated after 7 days of incubation at 24±1°C, in the dark. Extracts H. lupulus and A. millefolium inhibited the mycelial growth of F. culmorum of mycelial growth of 8% dose of the pathogens by 92.77% and 69.83%, respectively. It has been observed that the antifungal effect of the extracts increases with dose increase. As a result, at least micelle growth and the highest percent inhibition rate were obtained at 8% dose of the extract H. lupulus. H. lupulus extract can be used as a biological preparation.

Diabetic Rethinopathy Screening by Bright Lesions Extraction from Fundus Images

NASA Astrophysics Data System (ADS)

Hanđsková, Veronika; Pavlovičova, Jarmila; Oravec, Miloš; Blaško, Radoslav

2013-09-01

Retinal images are nowadays widely used to diagnose many diseases, for example diabetic retinopathy. In our work, we propose the algorithm for the screening application, which identifies the patients with such severe diabetic complication as diabetic retinopathy is, in early phase. In the application we use the patient's fundus photography without any additional examination by an ophtalmologist. After this screening identification, other examination methods should be considered and the patient's follow-up by a doctor is necessary. Our application is composed of three principal modules including fundus image preprocessing, feature extraction and feature classification. Image preprocessing module has the role of luminance normalization, contrast enhancement and optical disk masking. Feature extraction module includes two stages: bright lesions candidates localization and candidates feature extraction. We selected 16 statistical and structural features. For feature classification, we use multilayer perceptron (MLP) with one hidden layer. We classify images into two classes. Feature classification efficiency is about 93 percent.

Determination of the Three-Dimensional Morphology of ALH84001 and Biogenic MV-1 Magnetite: Comparison of Results from Electron Tomography and Classical Transmission Electron Microscopy

NASA Technical Reports Server (NTRS)

Thomas-Keprta, Kathie L.; Clemett, Simon J.; Schwartz, Cindy; Morphew, Mary; McIntosh, J. Richard; Bazylinski, Dennis A.; Kirschvink, Joseph L.; Wentworth, Susan J.; McKay, David S.; Vali, Hojatollah

2004-01-01

Dated at approximately 3.9 billion years of age, carbonate disks, found within fractures of the host rock of Martian meteorite ALH84001, have been interpreted as secondary minerals that formed at low temperature in an aqueous medium. Heterogeneously distributed within these disks are magnetite nanocrystals that are of Martian origin. Approximately one quarter of these magnetites have morphological and chemical similarities to magnetite particles produced by magnetotactic bacteria strain MV-1, which are ubiquitous in aquatic habitats on Earth. Moreover, these types of magnetite particles are not known or expected to be produced by abiotic means either through geological processes or synthetically in the laboratory. The remaining three quarters of the ALH84001 magnetites are likely products of multiple processes including, but not limited to, precipitation from a hydrothermal fluid, thermal decomposition of the carbonate matrix in which they are embedded, and extracellular formation by dissimilatory Fe-reducing bacteria. We have proposed that the origins of magnetites in ALH84001 can be best explained as the products of multiple processes, one of which is biological. Recently the three-dimensional (3-D) external morphology of the purported biogenic fraction of the ALH84001 magnetites has been the subject of considerable debate. We report here the 3-D geometry of biogenic magnetite crystals extracted from MV-1 and of those extracted from ALH84001 carbonate disks using a combination of high resolution classical and tomographic transmission electron microscopy (TEM). We focus on answering the following questions: (1) which technique provides adequate information to deduce the 3-D external crystal morphology?; and, (2) what is the precise 3-D geometry of the ALH84001 and MV-1 magnetites?

Mechanistic understanding and performance of biosorption of metal ions by grapefruit peel using FTIR spectroscopy, kinetics and adsorption isotherms modeling, alkali and alkaline metal displacement and EDX analysis

USDA-ARS?s Scientific Manuscript database

The performance and mechanism of the sorptive removal of Ni2+ and Zn2+ from aqueous solution using grapefruit peel (GFP) as a new sorbent was investigated. The sorption process was fast, equilibrium was established in 60 min. The equilibrium process was described well by the Langmuir isotherm model,...

Sampling trace-level organic solutes with polymeric tubing. Part 2: Dynamic studies

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

Parker, L.V.; Ranney, T.A.

1998-12-31

This is the second part of a study conducted to determine whether polymeric sampling tubing can affect organic analyte concentrations during a sampling event. In this part of the study, the authors looked for sorption and desorption of trichloroethylene (TCE) and leaching of organic constituents in water pumped through five types of polymeric tubing. The materials tested were a rigid fluoropolymer, a flexible fluoropolymer, low-density polyethylene (LDPE), and two plasticized polypropylene tubings. The effects of tubing length and flow rate were examined. The least sorptive tubings, both initially and at equilibrium, were the fluoropolymers. However, in some instances the LDPEmore » tubing had little effect on TCE concentrations. This was when a slow flow rate was used to sample relatively shallow wells (50 feet [15 m] or less) or when a faster flow rate (1 L/min) was used to sample wells that are less than 500 feet (152 m). Further testing is recommended using more sorptive analytes. Using high performance liquid chromatography (HPLC), the authors were unable to detect any constituents leaching from any of the tubings used in these studies, even when a slow flow rate was used. However, desorption of sorbed analytes is a concern for all the tubings tested, including the rigid fluoropolymer.« less

Spiral Arms, Infall, and Misalignment of the Circumbinary Disk from the Circumstellar Disks in the Protostellar Binary System L1551 NE

NASA Astrophysics Data System (ADS)

Takakuwa, Shigehisa; Saigo, Kazuya; Matsumoto, Tomoaki; Saito, Masao; Lim, Jeremy; Hanawa, Tomoyuki; Yen, Hsi-Wei; Ho, Paul T. P.

2017-03-01

We report the ALMA Cycle 2 observations of the Class I binary protostellar system L1551 NE in the 0.9 mm continuum, C18O (3-2), 13CO (3-2), SO (78-67), and CS (7-6) emission. At 0.″18 (=25 au) resolution, ˜4 times higher than that of our Cycle 0 observations, the circumbinary disk (CBD) as seen in the 0.9 mm emission is shown to be composed of a northern and a southern spiral arm, with the southern arm connecting to the circumstellar disk (CSD) around Source B. The western parts of the spiral arms are brighter than the eastern parts, suggesting the presence of an m = 1 spiral mode. In the C18O emission, the infall gas motions in the interarm regions and the outward gas motions in the arms are identified. These observed features are well reproduced with our numerical simulations, where gravitational torques from the binary system impart angular momenta to the spiral-arm regions and extract angular momenta from the interarm regions. Chemical differentiation of the CBD is seen in the four molecular species. Our Cycle 2 observations have also resolved the CSDs around the individual protostars, and the beam-deconvolved sizes are 0.″29 × 0.″19 (=40 × 26 au) (P.A. = 144°) and 0.″26 × 0.″20 (=36 × 27 au) (P.A. = 147°) for Sources A and B, respectively. The position and inclination angles of these CSDs are misaligned with those of the CBD. The C18O emission traces the Keplerian rotation of the misaligned disk around Source A.

Compact Packaging of Photonic Millimeter-Wave Receiver

NASA Technical Reports Server (NTRS)

Nguyen, Hung; Pouch, John; Miranda, Felix; Levi, Anthony F.

2007-01-01

A carrier structure made from a single silicon substrate is the basis of a compact, lightweight, relatively inexpensive package that holds the main optical/electronic coupling components of a photonic millimeter-wave receiver based on a lithium niobate resonator disk. The design of the package is simple and provides for precise relative placement of optical components, eliminating the need for complex, bulky positioning mechanisms like those commonly used to align optical components to optimize focus and coupling. Although a prototype of the package was fabricated as a discrete unit, the design is amenable to integration of the package into a larger photonic and/or electronic receiver system. The components (see figure) include a lithium niobate optical resonator disk of 5-mm diameter and .200- m thickness, positioned adjacent to a millimeter- wave resonator electrode. Other components include input and output coupling prisms and input and output optical fibers tipped with ball lenses for focusing and collimation, respectively. Laser light is introduced via the input optical fiber and focused into the input coupling prism. The input coupling prism is positioned near (but not in contact with) the resonator disk so that by means of evanescent-wave coupling, the input laser light in the prism gives rise to laser light propagating circumferentially in guided modes in the resonator disk. Similarly, a portion of the circumferentially propagating optical power is extracted from the disk by evanescent-wave coupling from the disk to the output coupling prism, from whence the light passes through the collimating ball lens into the output optical fiber. The lens-tipped optical fibers must be positioned at a specified focal distance from the prisms. The optical fibers and the prisms must be correctly positioned relative to the resonator disk and must be oriented to obtain the angle of incidence (55 in the prototype) required for evanescent-wave coupling of light into and out of the desired guided modes in the resonator disk. To satisfy all these requirements, precise alignment features are formed in the silicon substrate by use of a conventional wet-etching process. These features include a 5-mm-diameter, 50- m-deep cavity that holds the disk; two trapezoidal-cross-section recesses for the prisms; and two grooves that hold the optical fibers at the correct positions and angles relative to the prisms and disk. The fiber grooves contain abrupt tapers, near the prisms, that serve as hard stops for positioning the lenses at the focal distance from the prisms. There are also two grooves for prismadjusting rods. The design provides a little slack in the prism recesses for adjusting the positions of the prisms by means of these rods to optimize the optical coupling.

Feasibility of Isotope Harvesting at a Projectile Fragmentation Facility: 67Cu

DOE PAGES

Mastren, Tara; Pen, Aranh; Peaslee, Graham F.; ...

2014-10-21

The work presented here describes a proof-of-principle experiment for the chemical extraction of 67Cu from an aqueous beam stop at the National Superconducting Cyclotron Laboratory (NSCL). A 76 MeV/A 67Cu beam was stopped in water, successfully isolated from the aqueous solution through a series of chemical separations involving a chelating disk and anion exchange chromatography, then bound to NOTA-conjugated Herceptin antibodies, and the bound activity was validated using instant thin-layer chromatography (ITLC). The chemical extraction efficiency was found to be 88 ± 3% and the radiochemical yield was ≥95%. These results show that extraction of radioisotopes from an aqueous projectile-fragmentmore » beam dump is a feasible method for obtaining radiochemically pure isotopes.« less

[Experimental study of bacteriostatic activity of Chinese herbal medicines on primary cariogenic bacteria in vitro].

PubMed

Wang, S; Fan, M; Bian, Z

2001-09-01

To screen some Chinese herbal medicines for their inhibitory activity on cariogenic bacteria, and investigate their active ingredients, and measure their minimum inhibitory concentration (MIC), minimum bactericidal concentration (MBC). Active components were isolated from every tested Chinese herbal medicine by means of aqueous extraction and ethanolic extraction. Berberine was purified from Coptis chinensis Fra. Disk agar diffusion method was employed in screening herbs with inhibiting effect on cariogenic bacteria. MIC and MBC were determined by broth dilution method. Against Streptococcus mutans Ingbritt, MBCs of Magnolia officinalis ethanolic extract, Berberine, Coptis chinensis Fra aqueous extract and Coptis chinensis Fra ethanolic extract were 0.488, 0.625, 7.800 and 1.950 g/L respectively. Against Streptococcus sobrinus 6715, MBCs of Magnolia extract, Coptis chinensis Fra ethanolic extract, Rhus chinensis Mill ethanolic extract and Phellodendron chinen ethanolic extract were 0.488, 0.625, 1.950, 3.900, 3.900 and 3.900 g/L respectively. Against Actinomyces viscosus ATCC 19246, MBCs of Berberine, Coptis chinensis Fra aqueous extract, Coptis chinensis Fra ethanolic extract, Rheum palmatum L aqueous extract and Rheum palmatum L ethanolic extract were 1.250, 3.900, 3.900, 15.600 and 31.250 g/L respectively. Magnolia officinalis, Coptis chinensis Fran, Rheum palmatum L aqueous extracts exhibit strong inhibition on cariogenic bacteria. Magnolia officinalis ethanolic extract has the strongest bactericidal effects on Streptococcus mutans and Streptococcus sobrinus.

Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction.

PubMed

Chisvert, Alberto; Benedé, Juan L; Anderson, Jared L; Pierson, Stephen A; Salvador, Amparo

2017-08-29

With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67-791), limits of detection (low ng L -1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87-113%, 91-117% and 89-115% for river, sea and swimming pool water samples, respectively). Copyright © 2017 Elsevier B.V. All rights reserved.

In situ solvothermal growth of metal-organic framework-5 supported on porous copper foam for noninvasive sampling of plant volatile sulfides.

PubMed

Hu, Yuling; Lian, Haixian; Zhou, Langjun; Li, Gongke

2015-01-06

The present study reported on an in situ solvothermal growth method for immobilization of metal-organic framework MOF-5 on porous copper foam support for enrichment of plant volatile sulfides. The porous copper support impregnated with mother liquor of MOF-5 anchors the nucleation and growth of MOF crystallites at its surface, and its architecture of the three-dimensional channel enables accommodation of the MOF-5 crystallite seed. A continuous and well-intergrown MOF-5 layer, evidenced from scanning electron microscope imaging and X-ray diffraction, was successfully immobilized on the porous metal bar with good adhesion and high stability. Results show that the resultant MOF-5 coating was thermally stable up to 420 °C and robust enough for replicate extraction for at least 200 times. The MOF-5 bar was then applied to the headspace sorptive extraction of the volatile organic sulfur compounds in Chinese chive and garlic sprout in combination with thermal desorption-gas chromatography/mass spectrometry. It showed high extraction sensitivity and good selectivity to these plant volatile sulfides owing to the extraordinary porosity of the metal-organic framework as well as the interaction between the S-donor sites and the surface cations at the crystal edges. Several primary sulfur volatiles containing allyl methyl sulfide, dimethyl disulfide, diallyl sulfide, methyl allyl disulfide, and diallyl disulfide were quantified. Their limits of detection were found to be in the range of 0.2-1.7 μg/L. The organic sulfides were detected in the range of 6.0-23.8 μg/g with recoveries of 76.6-100.2% in Chinese chive and 11.4-54.6 μg/g with recoveries of 77.1-99.8% in garlic sprout. The results indicate the immobilization of MOF-5 on copper foam provides an efficient enrichment formats for noninvasive sampling of plant volatiles.

Design of a steganographic virtual operating system

NASA Astrophysics Data System (ADS)

Ashendorf, Elan; Craver, Scott

2015-03-01

A steganographic file system is a secure file system whose very existence on a disk is concealed. Customarily, these systems hide an encrypted volume within unused disk blocks, slack space, or atop conventional encrypted volumes. These file systems are far from undetectable, however: aside from their ciphertext footprint, they require a software or driver installation whose presence can attract attention and then targeted surveillance. We describe a new steganographic operating environment that requires no visible software installation, launching instead from a concealed bootstrap program that can be extracted and invoked with a chain of common Unix commands. Our system conceals its payload within innocuous files that typically contain high-entropy data, producing a footprint that is far less conspicuous than existing methods. The system uses a local web server to provide a file system, user interface and applications through a web architecture.

Antimicrobial activity of isothiocyanates (ITCs) extracted from horseradish (Armoracia rusticana) root against oral microorganisms.

PubMed

Park, Ho-Won; Choi, Kyu-Duck; Shin, Il-Shik

2013-01-01

The antimicrobial activity of isothiocyanates (ITCs) extracted from horseradish root was investigated against oral microorganisms: 6 strains of facultative anaerobic bacteria, Streptococcus mutans, Streptococcus sobrinus, Lactobacillus casei, Staphylococcus aureus, Enterococcus faecalis and Aggregatibacter actinomycetemcomitans; one strain of yeast, Candida albicans, and 3 strains of anaerobic bacteria, Fusobacterium nucleatum, Prevotella nigrescens, and Clostridium perfringens. The ITCs extracted from horseradish root showed antimicrobial activity against all oral microorganisms by the paper disk method. The minimum bactericidal concentration (MBC) of the ITCs extracted from horseradish root ranged from 1.25 to 5.00 mg/ml against 6 strains of facultative anaerobic bacteria and one strain of yeast, and 4.17 to 16.67 mg/ml against 3 strains of anaerobic bacteria. The ITCs extracted from horseradish root showed the strongest antimicrobial activity, with a MBC of 1.25 mg/ml, against C. albicans among facultative microorganisms, and 4.17 mg/ml against F. nucleatum among anaerobic bacteria. These results suggest that the ITCs extracted from horseradish root may be a candidate for use as an antimicrobial agent against oral microorganisms.

Green synthesis of silver nanoparticles using flower extract of Malva sylvestris and investigation of their antibacterial activity.

PubMed

Mahmoodi Esfanddarani, Hassan; Abbasi Kajani, Abolghasem; Bordbar, Abdol-Khalegh

2018-06-01

High-quality colloidal silver nanoparticles (AgNP) were synthesised via a green approach by using hydroalcoholic extracts of Malva sylvestris . Silver nitrate was used as a substrate ion while the plant extract successfully played the role of reducing and stabilising agents. The synthesised nanoparticles were carefully characterised by using transmission electron microscopy, atomic-force microscopy, energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy and UV-vis spectroscopy. The maximum absorption wavelengths of the colloidal solutions synthesised using 70 and 96% ethanol and 100% methanol, as extraction solvents, were 430, 485 and 504 nm, respectively. Interestingly, the size distribution of nanoparticles depended on the used solvent. The best particle size distribution belonged to the nanoparticles synthesised by 70% ethanol extract, which was 20-40 nm. The antibacterial activity of the synthesised nanoparticles was studied on Escherichia coli , Staphylococcus aureus and Streptococcus pyogenes using disk diffusion, minimum inhibitory concentrations and minimum bactericidal concentrations assays. The best antibacterial activity obtained for the AgNPs produced by using 96% ethanolic extract.

Analysis of Polyphenolic Compounds in Extracts from Leaves of Some Malus domestica Cultivars: Antiradical and Antimicrobial Analysis of These Extracts

PubMed Central

Sowa, Alina; Zgórka, Grażyna; Szykuła, Aleksandra; Franiczek, Roman; Żbikowska, Beata; Gamian, Andrzej

2016-01-01

In this study, methanol, ethyl acetate, water extracts, and precipitate were obtained from leaves of Malus domestica cultivars: Golden delicious, Jonagold, Elstar, Ligol, and Mutsu. Antiradical activity of these extracts was measured using the ABTS+∙ radical, and antimicrobial activity was measured with the disk-diffusion method. Phenolic compounds were measured with the colorimetric method and identified with high performance liquid chromatography (HPLC). The highest antiradical activity was observed for the Jonagold variety, and in particular strong activity was noted for ethyl acetate extracts. Antimicrobial activity was observed against strains of Staphylococcus aureus, Enterococcus faecalis, and the fungus Candida glabrata. Particularly susceptible to the extracts activity appeared to be Staphylococcus aureus, but the growth of Candida glabrata was inhibited in the presence of ethyl acetate extracts. With the HPLC method we identified a high amount of phloridzin (above 500 mg per g of ethyl acetate extracts), lower amounts of hyperoside, isoquercitrin, and quercitrin, and traces of p-hydroxybenzoic and chlorogenic acids. The contribution of phloridzin to antiradical activity of methanol and ethyl acetate extracts was very high (above 90%). In water extract the contribution of phloridzin was between 38.9 and 55.2%, chlorogenic acid 22.7 and 36.1%, and hyperoside 12.2 and 13.3%. PMID:28097143

Analysis of Polyphenolic Compounds in Extracts from Leaves of Some Malus domestica Cultivars: Antiradical and Antimicrobial Analysis of These Extracts.

PubMed

Sowa, Alina; Zgórka, Grażyna; Szykuła, Aleksandra; Franiczek, Roman; Żbikowska, Beata; Gamian, Andrzej; Sroka, Zbigniew

2016-01-01

In this study, methanol, ethyl acetate, water extracts, and precipitate were obtained from leaves of Malus domestica cultivars: Golden delicious, Jonagold, Elstar, Ligol, and Mutsu. Antiradical activity of these extracts was measured using the ABTS +∙ radical, and antimicrobial activity was measured with the disk-diffusion method. Phenolic compounds were measured with the colorimetric method and identified with high performance liquid chromatography (HPLC). The highest antiradical activity was observed for the Jonagold variety, and in particular strong activity was noted for ethyl acetate extracts. Antimicrobial activity was observed against strains of Staphylococcus aureus , Enterococcus faecalis , and the fungus Candida glabrata . Particularly susceptible to the extracts activity appeared to be Staphylococcus aureus , but the growth of Candida glabrata was inhibited in the presence of ethyl acetate extracts. With the HPLC method we identified a high amount of phloridzin (above 500 mg per g of ethyl acetate extracts), lower amounts of hyperoside, isoquercitrin, and quercitrin, and traces of p -hydroxybenzoic and chlorogenic acids. The contribution of phloridzin to antiradical activity of methanol and ethyl acetate extracts was very high (above 90%). In water extract the contribution of phloridzin was between 38.9 and 55.2%, chlorogenic acid 22.7 and 36.1%, and hyperoside 12.2 and 13.3%.

Ysovar: The First Sensitive, Wide-area, Mid-infrared Photometric Monitoring of the Orion Nebula Cluster

NASA Astrophysics Data System (ADS)

Morales-Calderón, M.; Stauffer, J. R.; Hillenbrand, L. A.; Gutermuth, R.; Song, I.; Rebull, L. M.; Plavchan, P.; Carpenter, J. M.; Whitney, B. A.; Covey, K.; Alves de Oliveira, C.; Winston, E.; McCaughrean, M. J.; Bouvier, J.; Guieu, S.; Vrba, F. J.; Holtzman, J.; Marchis, F.; Hora, J. L.; Wasserman, L. H.; Terebey, S.; Megeath, T.; Guinan, E.; Forbrich, J.; Huélamo, N.; Riviere-Marichalar, P.; Barrado, D.; Stapelfeldt, K.; Hernández, J.; Allen, L. E.; Ardila, D. R.; Bayo, A.; Favata, F.; James, D.; Werner, M.; Wood, K.

2011-05-01

We present initial results from time-series imaging at infrared wavelengths of 0.9 deg2 in the Orion Nebula Cluster (ONC). During Fall 2009 we obtained 81 epochs of Spitzer 3.6 and 4.5 μm data over 40 consecutive days. We extracted light curves with ~3% photometric accuracy for ~2000 ONC members ranging from several solar masses down to well below the hydrogen-burning mass limit. For many of the stars, we also have time-series photometry obtained at optical (Ic ) and/or near-infrared (JK s ) wavelengths. Our data set can be mined to determine stellar rotation periods, identify new pre-main-sequence eclipsing binaries, search for new substellar Orion members, and help better determine the frequency of circumstellar disks as a function of stellar mass in the ONC. Our primary focus is the unique ability of 3.6 and 4.5 μm variability information to improve our understanding of inner disk processes and structure in the Class I and II young stellar objects (YSOs). In this paper, we provide a brief overview of the YSOVAR Orion data obtained in Fall 2009 and highlight our light curves for AA-Tau analogs—YSOs with narrow dips in flux, most probably due to disk density structures passing through our line of sight. Detailed follow-up observations are needed in order to better quantify the nature of the obscuring bodies and what this implies for the structure of the inner disks of YSOs.

Near-infrared Variability in the Orion Nebula Cluster

NASA Astrophysics Data System (ADS)

Rice, Thomas S.; Reipurth, Bo; Wolk, Scott J.; Vaz, Luiz Paulo; Cross, N. J. G.

2015-10-01

Using UKIRT on Mauna Kea, we have carried out a new near-infrared J, H, K monitoring survey of almost a square degree of the star-forming Orion Nebula Cluster with observations on 120 nights over three observing seasons, spanning a total of 894 days. We monitored ˜15,000 stars down to J≈ 20 using the WFCAM instrument, and have extracted 1203 significantly variable stars from our data. By studying variability in young stellar objects (YSOs) in the H - K, K color-magnitude diagram, we are able to distinguish between physical mechanisms of variability. Many variables show color behavior indicating either dust-extinction or disk/accretion activity, but we find that when monitored for longer periods of time, a number of stars shift between these two variability mechanisms. Further, we show that the intrinsic timescale of disk/accretion variability in young stars is longer than that of dust-extinction variability. We confirm that variability amplitude is statistically correlated with evolutionary class in all bands and colors. Our investigations of these 1203 variables have revealed 73 periodic AA Tau type variables, many large-amplitude and long-period (P\\gt 15 days) YSOs, including three stars showing widely spaced periodic brightening events consistent with circumbinary disk activity, and four new eclipsing binaries. These phenomena and others indicate the activity of long-term disk/accretion variability processes taking place in young stars. We have made the light curves and associated data for these 1203 variables available online.

Electrospun polyacrylonitrile nanofibers functionalized with EDTA for adsorption of ionic dyes

NASA Astrophysics Data System (ADS)

Chaúque, Eutilério F. C.; Dlamini, Langelihle N.; Adelodun, Adedeji A.; Greyling, Corinne J.; Ngila, J. Catherine

2017-08-01

The manipulation of nanofibers' surface chemistry could enhance their potential application toward the removal of ionic dyes in wastewater. For this purpose, surface modification of electrospun polyacrylonitrile (PAN) nanofibers with ethylenediaminetetraacetic acid (EDTA) and ethylenediamine (EDA) crosslinker was experimented. The functionalized EDTA-EDA-PAN nanofibers were characterized using Fourier transform infrared (FT-IR) spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) technique. The impregnation of EDA and EDTA chelating agents on the surface of PAN changed the distribution of nanofibers as proximity is increased (accompanied by reduced softness), but the nanofibrous structure of the pristine PAN nanofibers was not substantially altered. Adsorption equilibrium studies were performed with Freundlich, Langmuir and Temkin isotherm models with the former providing better correlation to the experimental data. The modified PAN nanofibers showed efficient sorption of methyl orange (MO) and reactive red (RR) from aqueous synthetic samples, evinced by the maximum adsorption capacities (at 25 °C) of 99.15 and 110.0 mg g-1, respectively. The fabricated nanofibers showed appreciable removal efficiency of the target dye sorptives from wastewater. However, the presence of high metal ions content affected the overall extraction of dyes from wastewater due to the depletion of the adsorbent's active adsorptive sites.

Determination of phenol compounds in surface water matrices by bar adsorptive microextraction-high performance liquid chromatography-diode array detection.

PubMed

Neng, Nuno R; Nogueira, José M F

2014-07-03

Bar adsorptive microextraction combined with liquid desorption followed by high performance liquid chromatography with diode array detection (BAµE-LD/HPLC-DAD) is proposed for the determination of trace levels of five phenol compounds (3-nitrophenol, 4-nitrophenol, bisphenol-A, 4-n-octylphenol and 4-n-nonylphenol) in surface water matrices. By using a polystyrene-divinylbenzene copolymer (PS-DVB) sorbent phase, high selectivity and efficiency is achieved even against polydimethylsiloxane through stir bar sorptive extraction. Assays performed by BAµE(PS-DVB)-LD/HPLC-DAD on 25 mL water samples spiked at the 10.0 µg/L levels yielded recoveries over 88.0%±5.7% for all five analytes, under optimized experimental conditions. The analytical performance showed good precision (RSD<15%), detection limits of 0.25 µg/L and linear dynamic ranges (1.0-25.0 μg/L) with determination coefficient higher than 0.9904. By using the standard addition method, the application of the present method to surface water matrices allowed very good performances at the trace level. The proposed methodology proved to be a suitable alternative to monitor phenol compounds in surface water matrices, showing to be easy to implement, reliable, sensitive and requiring a low sample volume.

Post-acquisition data processing for the screening of transformation products of different organic contaminants. Two-year monitoring of river water using LC-ESI-QTOF-MS and GCxGC-EI-TOF-MS.

PubMed

López, S Herrera; Ulaszewska, M M; Hernando, M D; Martínez Bueno, M J; Gómez, M J; Fernández-Alba, A R

2014-11-01

This study describes a comprehensive strategy for detecting and elucidating the chemical structures of expected and unexpected transformation products (TPs) from chemicals found in river water and effluent wastewater samples, using liquid chromatography coupled to electrospray ionization quadrupole-time-of-flight mass spectrometer (LC-ESI-QTOF-MS), with post-acquisition data processing and an automated search using an in-house database. The efficacy of the mass defect filtering (MDF) approach to screen metabolites from common biotransformation pathways was tested, and it was shown to be sufficiently sensitive and applicable for detecting metabolites in environmental samples. Four omeprazole metabolites and two venlafaxine metabolites were identified in river water samples. This paper reports the analytical results obtained during 2 years of monitoring, carried out at eight sampling points along the Henares River (Spain). Multiresidue monitoring, for targeted analysis, includes a group of 122 chemicals, amongst which are pharmaceuticals, personal care products, pesticides and PAHs. For this purpose, two analytical methods were used based on direct injection with a LC-ESI-QTOF-MS system and stir bar sorptive extraction (SBSE) with bi-dimensional gas chromatography coupled with a time-of-flight spectrometer (GCxGC-EI-TOF-MS).

Field application of passive SBSE for the monitoring of pesticides in surface waters.

PubMed

Assoumani, A; Coquery, M; Liger, L; Mazzella, N; Margoum, C

2015-03-01

Spot sampling lacks representativeness for monitoring organic contaminants in most surface waters. Passive sampling has emerged as a cost-effective complementary sampling technique. We recently developed passive stir bar sorptive extraction (passive SBSE), with Twister from Gerstel, for monitoring moderately hydrophilic to hydrophobic pesticides (2.18 < log K ow < 5.11) in surface water. The aims of the present study were to assess this new passive sampler for the determination of representative average concentrations and to evaluate the contamination levels of two French rivers. Passive SBSE was evaluated for the monitoring of 16 pesticides in two rivers located in a small vineyard watershed during two 1-month field campaigns in spring 2010 and spring 2011. Passive SBSE was applied for periods of 1 or 2 weeks during the field campaigns and compared with spot sampling and weekly average automated sampling. The results showed that passive SBSE could achieve better time-representativeness than spot sampling and lower limits of quantification than automated sampling coupled with analytical SBSE for the pesticides studied. Finally, passive SBSE proved useful for revealing spatial and temporal variations in pesticide contamination of both rivers and the impact of rainfall and runoff on the river water quality.

Experimental Solubility Approach to Determine PDMS-Water Partition Constants and PDMS Activity Coefficients.

PubMed

Grant, Sharon; Schacht, Veronika J; Escher, Beate I; Hawker, Darryl W; Gaus, Caroline

2016-03-15

Freely dissolved aqueous concentration and chemical activity are important determinants of contaminant transport, fate, and toxic potential. Both parameters are commonly quantified using Solid Phase Micro-Extraction (SPME) based on a sorptive polymer such as polydimethylsiloxane (PDMS). This method requires the PDMS-water partition constants, KPDMSw, or activity coefficient to be known. For superhydrophobic contaminants (log KOW >6), application of existing methods to measure these parameters is challenging, and independent measures to validate KPDMSw values would be beneficial. We developed a simple, rapid method to directly measure PDMS solubilities of solid contaminants, SPDMS(S), which together with literature thermodynamic properties was then used to estimate KPDMSw and activity coefficients in PDMS. PDMS solubility for the test compounds (log KOW 7.2-8.3) ranged over 3 orders of magnitude (4.1-5700 μM), and was dependent on compound class. For polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins (PCDDs), solubility-derived KPDMSw increased linearly with hydrophobicity, consistent with trends previously reported for less chlorinated congeners. In contrast, subcooled liquid PDMS solubilities, SPDMS(L), were approximately constant within a compound class. SPDMS(S) and KPDMSw can therefore be predicted for a compound class with reasonable robustness based solely on the class-specific SPDMS(L) and a particular congener's entropy of fusion, melting point, and aqueous solubility.

Sesquiterpene emissions from Alternaria alternata and Fusarium oxysporum: Effects of age, nutrient availability, and co-cultivation

PubMed Central

Weikl, Fabian; Ghirardo, Andrea; Schnitzler, Jörg-Peter; Pritsch, Karin

2016-01-01

Alternaria alternata is one of the most studied fungi to date because of its impact on human life – from plant pathogenicity to allergenicity. However, its sesquiterpene emissions have not been systematically explored. Alternaria regularly co-occurs with Fusarium fungi, which are common plant pathogens, on withering plants. We analyzed the diversity and determined the absolute quantities of volatile organic compounds (VOCs) in the headspace above mycelial cultures of A. alternata and Fusarium oxysporum under different conditions (nutrient rich and poor, single cultures and co-cultivation) and at different mycelial ages. Using stir bar sorptive extraction and gas chromatography–mass spectrometry, we observed A. alternata to strongly emit sesquiterpenes, particularly during the early growth stages, while emissions from F. oxysporum consistently remained comparatively low. The emission profile characterizing A. alternata comprised over 20 sesquiterpenes with few effects from nutrient quality and age on the overall emission profile. Co-cultivation with F. oxysporum resulted in reduced amounts of VOCs emitted from A. alternata although its profile remained similar. Both fungi showed distinct emission profiles, rendering them suitable biomarkers for growth-detection of their phylotype in ambient air. The study highlights the importance of thorough and quantitative evaluations of fungal emissions of volatile infochemicals such as sesquiterpenes. PMID:26915756

Olfactory basis of floral preference of the malaria vector Anopheles gambiae (Diptera: Culicidae) among common African plants.

PubMed

Nikbakhtzadeh, Mahmood R; Terbot, John W; Otienoburu, Philip E; Foster, Woodbridge A

2014-12-01

Mosquitoes of both sexes feed on plants to obtain sugar. Nocturnal species probably locate the plants primarily by their volatile semiochemicals that also form the basis for the mosquitoes' innate plant-species preferences. To evaluate these olfactory preferences quantitatively, we used a two-choice wind-tunnel olfactometer to measure the upwind orientation of Anopheles gambiae Giles, an important vector of malaria in equatorial Africa, toward odor plumes produced by nine plant species common where this mosquito occurs. These plants are reported to induce feeding behaviors in An. gambiae and to produce floral or extrafloral nectar. Results presented here demonstrated that the volatiles of S. didymobotrya, P. hysterophorus, S. occidentalis, and L. camara, in descending order of numbers of mosquitoes responding, were all attractive, compared to a control plant species, whereas D. stramonium, R. communis, S. bicapsularis, T. stans, and T. diversifolia were not. As expected, chromatographic analysis of the headspace of attractive plants whose volatiles were captured by stir-bar sorptive extraction revealed a wide range of compounds, primarily terpenoids. Once their bioactivity and attractiveness for An. gambiae, alone and in blends, has been firmly established, some of these semiochemicals may have applications in population sampling and control. © 2014 The Society for Vector Ecology.

Experimental Parameters Affecting Stripping of Rare Earth Elements from Loaded Sorptive Media in Simulated Geothermal Brines

DOE Data Explorer

Dean Stull

2016-05-24

Experimental results from several studies exploring the impact of pH and acid volume on the stripping of rare earth elements (REEs) loaded onto ligand-based media via an active column. The REEs in this experiment were loaded onto the media through exposure to a simulated geothermal brine with known mineral concentrations. The data include the experiment results, rare earth element concentrations, and the experimental parameters varied.

Lab-on-a-Valve Mesofluidic Platform for On-Chip Handling of Carbon-Coated Titanium Dioxide Nanotubes in a Disposable Microsolid Phase-Extraction Mode.

PubMed

García-Valverde, María Teresa; Rosende, María; Lucena, Rafael; Cárdenas, Soledad; Miró, Manuel

2018-04-03

Mesofluidic lab-on-a-valve (LOV) platforms have been proven suitable to accommodate automatic micro-solid-phase extraction (μSPE) approaches with on-chip handling of micrometer-bead materials in a fully disposable mode to prevent sample cross-contamination and pressure-drop effects. The efficiency of the extraction process notably depends upon the sorptive capacity of the material because the sorbent mass is usually down to 10 mg in LOV devices. Nanomaterials, capitalizing upon their enhanced surface-to-volume ratio and diversity of potential chemical moieties, are appealing alternatives to microbead sorbents. However, the handling and confinement of nanomaterials in fluidic chip structures have been challenging to date. This is most likely a consequence of the aggregation tendency of a number of nanomaterials, including carbon-based sorbents, that leads to excessive back-pressure in flowing systems along with irreproducible bead loading. This paper addresses these challenges by ad hoc synthesis of hybrid nanomaterials, such as porous carbon-coated titanium dioxide nanotubes (TiO 2 -NT@pC). Tailoring of the surface polarity of the carbon coating is proven to foster the dispersion of TiO 2 -NT@pC in LOV settings while affording superior extraction capability of moderately nonpolar species from aqueous matrices. The determination of trace-level concentrations of butylparaben (BPB) and triclosan (TCS) in seawater samples is herein selected as a proof-of-concept of the exploitation of disposable nanomaterials in LOV. The mesofluidic platform accommodating μSPE features online hyphenation to liquid chromatography/tandem mass spectrometry (LC/MS/MS) for reliable determination of the target analytes with excellent limits of detection (0.5 and 0.6 ng/L for BPB and TCS, respectively) and intermediate precision (relative standard deviation <5.8%). For 5.0 mL of sample and 200 μL of eluent, enrichment factors of 23 and 14 with absolute extraction efficiencies of 90% ± 14% and 58 ± 8% for BPB and TCS, respectively, were obtained. The relative recovery values of 107% (BPB) and 97% (TCS) in seawater demonstrate the applicability of online LOV-LC/MS/MS using TiO 2 -NT@pC for handling troublesome environmental samples.

Multi-stir bar sorptive extraction for analysis of odor compounds in aqueous samples.

PubMed

Ochiai, Nobuo; Sasamoto, Kikuo; Ieda, Teruyo; David, Frank; Sandra, Pat

2013-11-08

As reproducible coating of stir bars with more polar phases was found to be very difficult, a supporting grid was used in the development of an ethyleneglycol-modified Silicone (EG Silicone) coated stir bar. This new polar coating showed good performance for the extraction of polar solutes, but long term use also showed degradation of the coating due to friction while stirring. In order to address the lower robustness of the EG Silicone stir bar which has a much softer coating compared to a conventional polydimethylsiloxane (PDMS) stir bar, a novel SBSE procedure termed multi-SBSE ((m)SBSE) was developed. (m)SBSE consists of the robust PDMS stir bar stirring at the bottom of the vial and the EG Silicone stir bar attached on the inner side wall of the vial (a magnetic clip is used for the set-up). After extraction, the two stir bars are placed in a single glass desorption liner and are simultaneously thermally desorbed. The desorbed compounds were analyzed by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Compared to conventional SBSE, (m)SBSE provides more uniform enrichment of a wide range of odor compounds in aqueous sample since both stir bars can complement each other, while eliminating the damage of the EG Silicone phase during the extraction. The robustness of the EG Silicone stir bar was dramatically increased and more than 30 extraction and desorption cycles were possible without loss in performance. The recoveries for polar solutes such as 2-acetyl pyrrole (logKow: 0.55), benzyl alcohol (logKow: 1.08), guaiacol (logKow: 1.34), and indole (logKow: 2.05) were increased by a factor of about 2-7. The (m)SBSE-TD-GC-MS method showed good linearity (r(2)>0.9913) and high sensitivity (limit of detection: 0.011-0.071 ng mL(-1)) for the test compounds spiked in water. The feasibility and benefit of the method was demonstrated with analysis of odor compounds in roasted green tea. The normalized areas obtained from (m)SBSE showed the best enrichment for most of the selected compounds compared to conventional SBSE using the PDMS stir bar or the EG Silicone stir bar. Fifteen compounds were determined in the range of 0.15-210 ng mL(-1) (RSD<14%, n=6). Copyright © 2013 Elsevier B.V. All rights reserved.

Damage-Free Relief-Valve Disassembly

NASA Technical Reports Server (NTRS)

Haselmaier, H.

1986-01-01

Tool safely disassembles relief valves without damage to sensitive parts. Relief-valve disassembly tool used to extract valve nozzle from its housing. Holding device on tool grops nozzle. When user strikes hammer against impact disk, holding device pulls nozzle from press fit. Previously, nozzle dislodged by striking spindle above it, but practice often damaged retaining screw. New tool removes nozzle directly. With minor modifications, tool adapted to valves from different manufacturers.

Antibacterial effect of citrus press-cakes dried by high speed and far-infrared radiation drying methods

PubMed Central

Samarakoon, Kalpa; Senevirathne, Mahinda; Lee, Won-Woo; Kim, Young-Tae; Kim, Jae-Il; Oh, Myung-Cheol

2012-01-01

In this study, the antibacterial effect was evaluated to determine the benefits of high speed drying (HSD) and far-infrared radiation drying (FIR) compared to the freeze drying (FD) method. Citrus press-cakes (CPCs) are released as a by-product in the citrus processing industry. Previous studies have shown that the HSD and FIR drying methods are much more economical for drying time and mass drying than those of FD, even though FD is the most qualified drying method. The disk diffusion assay was conducted, and the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) were determined with methanol extracts of the dried CPCs against 11 fish and five food-related pathogenic bacteria. The disk diffusion results indicated that the CPCs dried by HSD, FIR, and FD prevented growth of all tested bacteria almost identically. The MIC and MBC results showed a range from 0.5-8.0 mg/mL and 1.0-16.0 mg/mL respectively. Scanning electron microscopy indicated that the extracts changed the morphology of the bacteria cell wall, leading to destruction. These results suggest that CPCs dried by HSD and FIR showed strong antibacterial activity against pathogenic bacteria and are more useful drying methods than that of the classic FD method in CPCs utilization. PMID:22808341

Quantitative determination of 1,4-dioxane and tetrahydrofuran in groundwater by solid phase extraction GC/MS/MS.

PubMed

Isaacson, Carl; Mohr, Thomas K G; Field, Jennifer A

2006-12-01

Groundwater contamination by cyclic ethers, 1,4-dioxane (dioxane), a probable human carcinogen, and tetrahydrofuran (THF), a co-contaminant at many chlorinated solvent release sites, are a growing concern. Cyclic ethers are readily transported in groundwater, yet little is known about their fate in environmental systems. High water solubility coupled with low Henry's law constants and octanol-water partition coefficients make their removal from groundwater problematic for both remedial and analytical purposes. A solid-phase extraction (SPE) method based on activated carbon disks was developed for the quantitative determination of dioxane and THF. The method requires 80 mL samples and a total of 1.2 mL of solvent (acetone). The number of steps is minimized due to the "in-vial" elution of the disks. Average recoveries for dioxane and THF were 98% and 95%, respectively, with precision, as indicated by the relative standard deviation of <2% to 6%. The method quantitation limits are 0.31 microg/L for dioxane and 3.1 microg/L for THF. The method was demonstrated by analyzing groundwater samples for dioxane and THF collected during a single sampling campaign at a TCA-impacted site. Dioxane concentrations and areal extent of dioxane in groundwater were greater than those of either TCA or THF.

Repellency of Plant Extracts against the Legume Flower Thrips Megalurothrips sjostedti (Thysanoptera: Thripidae)

PubMed Central

Abtew, Andnet; Subramanian, Sevgan; Cheseto, Xavier; Kreiter, Serge; Tropea Garzia, Giovanna; Martin, Thibaud

2015-01-01

Megalurothrips sjostedti Trybom is an important pest of cowpea (Vigna unguiculata L.) in Africa. To propose an alternative to chemical control, the repellency of 24 plant extracts was evaluated against adult female thrips of M. sjostedti in the laboratory. Plant extracts in ethanol were separately applied on a filter paper disk in a still air visual cue olfactometer. The results showed highly significant differences in repellency among extract type, concentration and their interactions. We classified the level of repellency into four categories as strong, good, moderate and weak or non- repellent based on hierarchical ascendant classification. We identified Piper nigrum, Cinnamomum zeylanicum, Cinnamomum cassia as strong repellents. Five extracts were classified as good, eight as moderate and the remaining eight extracts were weak or non-repellent. Repellency of the extracts increased with the concentration suggesting that the behavioral response of M. sjostedti was dose-dependent. Mono- and sesquiterpene hydrocarbon compounds from seven highly repellent extracts were identified by gas chromatography-mass spectrometry (GC/MS). The use of repellent extracts could be useful in developing integrated pest management strategies for thrips on legume crops. In this regard, the specific modes of action of the identified compounds need to be investigated to incorporate them into the existing crop protection strategies. PMID:26463406

On-tap passive enrichment, a new way to investigate off-flavor episodes in drinking water.

PubMed

Tondelier, Christophe; Thouvenot, Thomas; Genin, Arnaud; Benanou, David

2009-04-03

Because taste and odor events in drinking water are often fleeting and unpredictable phenomena, an innovative enrichment sampler has been developed to trap off-flavor compounds directly at the consumer's tap. The ARISTOT (Advanced Relevant Investigation Sampler for Taste & Odor at Tap) consists of a tap adapter in which seven polydimethylsiloxane (PDMS) coated stir bars are placed, allowing the stir bar sorptive extraction (SBSE) of organic compounds during each tap opening. In order to study the efficiency of ARISTOT, a private network pilot unit has been constructed in our laboratory, equipped with four faucets in parallel, solenoid valves for an automation of the system and a mixing chamber to spike drinking water with odorous compounds in order to have homogenously smelling water at each tap. After enrichment, the stir bars are taken out, in-line thermo-desorbed and analyzed by gas chromatography coupled with a mass spectrometer. The results showed the high sensitivity of ARISTOT, which was able to quickly monitor odorous compounds at the sub ng/L level. A "multishot" method was developed to analyze chemicals concentrated on the seven stir bars in only one chromatographic run, thereby increasing the sensitivity of the system. Higher enrichment factors were obtained under low water flow rates or by using longer stir bars and/or stir bars with a higher PDMS film thickness. No significant loss of extracted compounds was reported for flow rates between 2 and 4L/min. This allowed us to spike the stir bars with an internal standard prior to sampling in order to monitor the analytical variations. It was also observed that hot water increases the loss of enriched solutes but the quantification can be corrected by internal standard addition.

New approach on trace analysis of triclosan in personal care products, biological and environmental matrices.

PubMed

Silva, Ana Rita M; Nogueira, J M F

2008-02-15

Stir bar sorptive extraction and liquid desorption followed by high performance liquid chromatography with diode array detection (SBSE-LD-LC-DAD) is proposed for the determination of triclosan in personal care products, biological and environmental matrices, which is included in the priority lists, set by several international regulatory organizations. Instrumental conditions and experimental parameters that affecting SBSE-LD efficiency are fully discussed. Throughout systematic assays on 25 mL water samples spiked at the 10.0 microg L(-1) level, it had been established that stir bars coated with 126 microL of polydimethylsiloxane, an equilibrium time of 1h (1000 rpm) and acetonitrile under sonification (60 min) as back-extraction solvent, allowed the best analytical performance to determine triclosan in water matrices. From the data obtained, good recovery and remarkable repeatability were attained, providing experimental average yields (78.5+/-2.2%), although slightly lower than the theoretical equilibrium (99.7%) described by the octanol-water partition coefficients (K(PDMS/W)0.9992) from 0.4 to 108.0 microg L(-1). The application of the present method to determine triclosan in real matrices such as commercial toothpaste, saliva and urban wastewater samples, allowed appropriate selectivity, high sensitivity and accuracy using the standard addition methodology. The proposed method showed to be feasible and sensitive with a low-sample volume requirement to monitor triclosan in personal care products, biological and environmental matrices at the trace level, in compliance with international regulatory directives.

Advanced method optimization for volatile aroma profiling of beer using two-dimensional gas chromatography time-of-flight mass spectrometry.

PubMed

Stefanuto, Pierre-Hugues; Perrault, Katelynn A; Dubois, Lena M; L'Homme, Benjamin; Allen, Catherine; Loughnane, Caitriona; Ochiai, Nobuo; Focant, Jean-François

2017-07-21

The complex mixture of volatile organic compounds (VOCs) present in the headspace of Trappist and craft beers was studied to illustrate the efficiency of thermal desorption (TD) comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) for highlighting subtle differences between highly complex mixtures of VOCs. Headspace solid-phase microextraction (HS-SPME), multiple (and classical) stir bar sorptive extraction (mSBSE), static headspace (SHS), and dynamic headspace (DHS) were compared for the extraction of a set of 21 representative flavor compounds of beer aroma. A Box-Behnken surface response methodology experimental design optimization (DOE) was used for convex hull calculation (Delaunay's triangulation algorithms) of peak dispersion in the chromatographic space. The predicted value of 0.5 for the ratio between the convex hull and the available space was 10% higher than the experimental value, demonstrating the usefulness of the approach to improve optimization of the GC×GC separation. Chemical variations amongst aligned chromatograms were studied by means of Fisher Ratio (FR) determination and F-distribution threshold filtration at different significance levels (α=0.05 and 0.01) and based on z-score normalized area for data reduction. Statistically significant compounds were highlighted following principal component analysis (PCA) and hierarchical cluster analysis (HCA). The dendrogram structure not only provided clear visual information about similarities between products but also permitted direct identification of the chemicals and their relative weight in clustering. The effective coupling of DHS-TD-GC×GC-TOFMS with PCA and HCA was able to highlight the differences and common typical VOC patterns among 24 samples of different Trappist and selected Canadian craft beers. Copyright © 2017 Elsevier B.V. All rights reserved.

Structure of Herbig AeBe disks at the milliarcsecond scale . A statistical survey in the H band using PIONIER-VLTI

NASA Astrophysics Data System (ADS)

Lazareff, B.; Berger, J.-P.; Kluska, J.; Le Bouquin, J.-B.; Benisty, M.; Malbet, F.; Koen, C.; Pinte, C.; Thi, W.-F.; Absil, O.; Baron, F.; Delboulbé, A.; Duvert, G.; Isella, A.; Jocou, L.; Juhasz, A.; Kraus, S.; Lachaume, R.; Ménard, F.; Millan-Gabet, R.; Monnier, J. D.; Moulin, T.; Perraut, K.; Rochat, S.; Soulez, F.; Tallon, M.; Thiébaut, E.; Traub, W.; Zins, G.

2017-03-01

Context. It is now generally accepted that the near-infrared excess of Herbig AeBe stars originates in the dust of a circumstellar disk. Aims: The aims of this article are to infer the radial and vertical structure of these disks at scales of order 1 au, and the properties of the dust grains. Methods: The program objects (51 in total) were observed with the H-band (1.6 μm) PIONIER/VLTI interferometer. The largest baselines allowed us to resolve (at least partially) structures of a few tenths of an au at typical distances of a few hundred parsecs. Dedicated UBVRIJHK photometric measurements were also obtained. Spectral and 2D geometrical parameters are extracted via fits of a few simple models: ellipsoids and broadened rings with azimuthal modulation. Model bias is mitigated by parallel fits of physical disk models. Sample statistics were evaluated against similar statistics for the physical disk models to infer properties of the sample objects as a group. Results: We find that dust at the inner rim of the disk has a sublimation temperature Tsub ≈ 1800 K. A ring morphology is confirmed for approximately half the resolved objects; these rings are wide δr/r ≥ 0.5. A wide ring favors a rim that, on the star-facing side, looks more like a knife edge than a doughnut. The data are also compatible with the combination of a narrow ring and an inner disk of unspecified nature inside the dust sublimation radius. The disk inner part has a thickness z/r ≈ 0.2, flaring to z/r ≈ 0.5 in the outer part. We confirm the known luminosity-radius relation; a simple physical model is consistent with both the mean luminosity-radius relation and the ring relative width; however, a significant spread around the mean relation is present. In some of the objects we find a halo component, fully resolved at the shortest interferometer spacing, that is related to the HAeBe class. Full Tables B1-B3, as well as results of other parametric fits, are only available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/599/A85 The calibrated interferometric data can be found as FITS format files at http://oidb.jmmc.fr/collection.html?id=HAeBeLP

Electromagnetic jets from stars and black holes

NASA Astrophysics Data System (ADS)

Gralla, Samuel E.; Lupsasca, Alexandru; Rodriguez, Maria J.

2016-02-01

We present analytic force-free solutions modeling rotating stars and black holes immersed in the magnetic field of a thin disk that terminates at an inner radius. The solutions are exact in flat spacetime and approximate in Kerr spacetime. The compact object produces a conical jet whose properties carry information about its nature. For example, the jet from a star is surrounded by a current sheet, while that of a black hole is smooth. We compute an effective resistance in each case and compare to the canonical values used in circuit models of energy extraction. These solutions illustrate all of the basic features of the Blandford-Znajek process for energy extraction and jet formation in a clean setting.

Dynamics of ultraharmonic resonances in spiral galaxies

NASA Technical Reports Server (NTRS)

Artymowicz, Pawel; Lubow, Stephen H.

1992-01-01

The mildly nonlinear response of a fluid disk with pressure, viscosity, and self-gravity to spiral stellar forcing is considered as a model of the interstellar medium in spiral galaxies. Nonlinear effects are analyzed through a quasi-linear flow analysis ordered by successive powers of a dimensionless spiral perturbing force, which is the ratio of imposed nonaxisymmetric gravitational to axisymmetric gravitational forces. Waves with mn arms are launched from a position where the wavenumber of a free wave matches n times the wavenumber of the spiral forcing. The launched short wave in the gas is an interarm feature that is more tightly wrapped than the stellar wave. The gas wave extracts energy and angular momentum from the stellar wave, causing it to damp. The application of the results to the stellar disk alone reveals even stronger damping, as stars undergo Landau damping of the short wave. For parameters in M81, damping times are less than 10 exp 9 yr.

MIDAS - ESO's new image processing system

NASA Astrophysics Data System (ADS)

Banse, K.; Crane, P.; Grosbol, P.; Middleburg, F.; Ounnas, C.; Ponz, D.; Waldthausen, H.

1983-03-01

The Munich Image Data Analysis System (MIDAS) is an image processing system whose heart is a pair of VAX 11/780 computers linked together via DECnet. One of these computers, VAX-A, is equipped with 3.5 Mbytes of memory, 1.2 Gbytes of disk storage, and two tape drives with 800/1600 bpi density. The other computer, VAX-B, has 4.0 Mbytes of memory, 688 Mbytes of disk storage, and one tape drive with 1600/6250 bpi density. MIDAS is a command-driven system geared toward the interactive user. The type and number of parameters in a command depends on the unique parameter invoked. MIDAS is a highly modular system that provides building blocks for the undertaking of more sophisticated applications. Presently, 175 commands are available. These include the modification of the color-lookup table interactively, to enhance various image features, and the interactive extraction of subimages.

Impact of radius and skew angle on areal density in heat assisted magnetic recording hard disk drives

NASA Astrophysics Data System (ADS)

Cordle, Michael; Rea, Chris; Jury, Jason; Rausch, Tim; Hardie, Cal; Gage, Edward; Victora, R. H.

2018-05-01

This study aims to investigate the impact that factors such as skew, radius, and transition curvature have on areal density capability in heat-assisted magnetic recording hard disk drives. We explore a "ballistic seek" approach for capturing in-situ scan line images of the magnetization footprint on the recording media, and extract parametric results of recording characteristics such as transition curvature. We take full advantage of the significantly improved cycle time to apply a statistical treatment to relatively large samples of experimental curvature data to evaluate measurement capability. Quantitative analysis of factors that impact transition curvature reveals an asymmetry in the curvature profile that is strongly correlated to skew angle. Another less obvious skew-related effect is an overall decrease in curvature as skew angle increases. Using conventional perpendicular magnetic recording as the reference case, we characterize areal density capability as a function of recording position.

A new sum parameter to estimate the bioconcentration and baseline-toxicity of hydrophobic compounds in river water

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

Loon, W.M.G.M. van; Hermens, J.L.M.

1994-12-31

A large part of all aquatic pollutants can be classified as narcosis-type (baseline toxicity) chemicals. Many chemicals contribute to a joint baseline aquatic toxicity even at trace concentrations. A novel surrogate parameter, which simulated bioconcentration of hydrophobic substances from water and estimates internal molar concentrations, has been explored by Verhaar et al.. These estimated biological concentrations can be used to predict narcosis-type toxic effects, using the Lethal Body Burden (LBB) concept. The authors applied this toxicological-analytical concept to river water, and some recent technological developments and field results are pointed out. The simulation of bioconcentration is performed by extracting watermore » samples with empore{trademark} disks. The authors developed two extraction procedures; i.e., laboratory extraction and field extraction. Molar concentrations measurements are performed using vapor pressure osmometry, GC-FID and GC-MS. Results on the molar concentrations of hydrophobic compounds which can be bioaccumulated from several Dutch river systems will be presented.« less

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

PubMed

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

2012-01-15

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

Activity of Aristolochia bracteolata against Moraxella catarrhalis

PubMed Central

Khedr, Amgad I. M.; Abd AlGadir, Haidar; Takeshita, Satoshi; Shah, Mohammad Monir; Ichinose, Yoshio; Maki, Toshihide

2014-01-01

A bioassay-guided fractionation of methanol extract of Aristolochia bracteolata whole plant was carried out in order to evaluate its antimicrobial activity and to identify the active compounds in this extract. Antibacterial and antifungal activities of methanol extract against gram-positive, gram-negative, and fungal strains were investigated by the agar disk diffusion method. Among the strains tested, Moraxella catarrhalis and sea urchin-derived Bacillus sp. showed the highest sensitivity towards the methanol extract and hence they are used as test organisms for the bioassay-guided fractionation. From this extract, aristolochic acid 1 (AA-1) has been isolated and has showed the greatest antibacterial activity against both standard strain and clinical isolates of Moraxella catarrhalis with equal minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) values of 25 and 50 μg/mL. Modification of the AA-1 to AA-1 methyl ester completely abolished the antibacterial activity of the compound and the piperonylic acid moiety of AA-1 which suggested that the coexistence of phenanthrene ring and free carboxylic acid is essential for AA-1 antibacterial activity. PMID:26904734

Development of extract library from indonesian biodiversity: exploration of antibacterial activity of mangrove bruguiera cylindrica leaf extracts

NASA Astrophysics Data System (ADS)

Audah, K. A.; Amsyir, J.; Almasyhur, F.; Hapsari, A. M.; Sutanto, H.

2018-03-01

Antibacterial drugs derived from natural sources play significant roles in the prevention and treatment of bacterial infections since antibiotics have become less effective against many infectious diseases. Mangroves are very potential natural antibacterial sources among great numbers of wild medicinal plants. Bruguiera cylindrica is one of the many mangroves species which spread along Indonesian coastline. The aim of this study was to explore the antibacterial activity of B. cylindrica wet and dried leaf extracts. The wet extracts study was conducted with three different solvents system (water, ethanol, and n-Hexane) against Escherichia coli and Staphylococcus aureus. While, the dried extracts study was conducted with four different solvents system (water, ethanol, chloroform and n-Hexane) against three types of bacteria, Escherichia coli, Staphylococcus epidermidis and Staphylococcus aureus. The study showed that ethanol was the best solvent for extraction of phenolic and flavonoid. Antibacterial actitivity was measured by zone of inhibition which obtained from agar-disk diffusion method. The widest area of zone of inhibition was showed by wet extracts with ethanol against S. aureus and E. coli are 14.30 and 13.30 mm, respectively. While, the zone of inhibition dried extracts with ethanol against S. aureus, S. epidermidis and E. coli are 9.32, 6.59 and 6.20 mm, respectively. In conclusion, both type of extracts showed significant antibacterial activity against gram-positive bacteria as crude extracts.

Spinning-disk generation and drying of monodisperse solid aerosols with output concentrations sufficient for single-breath inhalation studies.

PubMed

Byron, P R; Hickey, A J

1987-01-01

The air-driven spinning-disk aerosol generator was modified to allow the production of monodisperse dry spherical aerosols of disodium fluorescein (as model solute) in high output concentrations. Output concentrations were determined by filtration. Optical and aerodynamic size distributions were determined microscopically (after electrostatic precipitation) and by cascade impaction. The generator housing allowed the entrainment of 25-microns primary aqueous solution droplets in a 10-L X min-1 downward flow of dry, filtered air. Internal equipment surfaces were machined flush and polished to minimize aerosol losses. Primary droplets were dried within a stainless steel pipe encased in a tube furnace. Water vapor was removed by diffusion drying. Disk-driven air, satellite droplets, and additional dilution air were vented to waste without using a vacuum. Generator yields were increased by reducing the size of the satellite droplet extraction gap. Aerosols were generated reproducibly by delivering aqueous solutions at a rate of 0.2 mL X min-1 to the center of the disk and spinning at 1000 rps. Dry aerosols, with mass median aerodynamic diameters of 2, 4.9, and 9 microns, were produced in concentrations of 0.89, 5.48, and 54.6 micrograms X L-1 from aqueous solutions containing 0.0374, 0.584, and 3.4% solute by weight. Geometric standard deviations were less than 1.2 in all cases. Concentrations are several times higher than others in the literature and are suitable for single-breath inhalation studies of therapeutic aerosol deposition and effect.

ACCRETION FLOW DYNAMICS OF MAXI J1659-152 FROM THE SPECTRAL EVOLUTION STUDY OF ITS 2010 OUTBURST USING THE TCAF SOLUTION

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

Debnath, Dipak; Molla, Aslam Ali; Chakrabarti, Sandip K.

2015-04-20

Transient black hole candidates are interesting objects to study in X-rays as these sources show rapid evolutions in their spectral and temporal properties. In this paper, we study the spectral properties of the Galactic transient X-ray binary MAXI J1659-152 during its very first outburst after discovery with the archival data of RXTE Proportional Counter Array instruments. We make a detailed study of the evolution of accretion flow dynamics during its 2010 outburst through spectral analysis using the Chakrabarti–Titarchuk two-component advective flow (TCAF) model as an additive table model in XSPEC. Accretion flow parameters (Keplerian disk and sub-Keplerian halo rates, shockmore » location, and shock strength) are extracted from our spectral fits with TCAF. We studied variations of these fit parameters during the entire outburst as it passed through three spectral classes: hard, hard-intermediate, and soft-intermediate. We compared our TCAF fitted results with standard combined disk blackbody (DBB) and power-law (PL) model fitted results and found that variations of disk rate with DBB flux and halo rate with PL flux are generally similar in nature. There appears to be an absence of the soft state, unlike what is seen in other similar sources.« less

Use of an ultrasonic device for the determination of elastic modulus of dentin.

PubMed

Miyazaki, Masashi; Inage, Hirohiko; Onose, Hideo

2002-03-01

The mechanical properties of dentin substrate are one of the important factors in determining bond strength of dentin bonding systems. The purpose of this study was to determine the elastic modulus of dentin substrate with the use of an ultrasonic device. The dentin disks of about 1 mm thickness were obtaining from freshly extracted human third molars, and the dentin disk was shaped in a rectangular form with a line diamond point. The size and weight of each specimen was measured to calculate the density of the specimen. The ultrasonic equipment employed in this study was composed of a Pulser-Receiver (Model 5900PR, Panametrics), transducers (V155, V156, Panametrics) and an oscilloscope. The measured two-way transit time through the dentin disk was divided by two to account for the down-and-back travel path, and then multiplied by the velocity of sound in the test material. Measuring the longitudinal and share wave sound velocity determine elastic modulus. The mean elastic modulus of horizontally sectioned specimens was 21.8 GPa and 18.5 GPa for the vertically sectioned specimens, and a significant difference was found between the two groups. The ultrasonic method used in this study shows considerable promise for determination of the elastic modulus of the tooth substrate.

Saturation of the Magnetorotational Instability at Large Elssaser Number

NASA Astrophysics Data System (ADS)

Julien, Keith; Jamroz, Benjamin; Knobloch, Edgar

2009-11-01

The MRI is believed to play an important role in accretion disk physics in extracting angular momentum from the disk and allowing accretion to take place. The instability is investigated within the shearing box approximation under conditions of fundamental importance to astrophysical accretion disk theory. The shear is taken to be the dominant source of energy, but the instability itself requires the presence of a weaker vertical magnetic field. Dissipative effects are suffiently weak that the Elsasser number is large. Thus dissipative forces do not play a role in the leading order linear instability mechanism. However, they are sufficiently large to permit a nonlinear feedback mechanism whereby the turbulent stresses generated by the MRI act on and modify the local background shear in the angular velocity profile. To date this response has been omitted in shearing box simulations and is captured by a reduced pde model derived from the global MHD fluid equations using multiscale asymptotic perturbation theory. Results from simulations of the model indicate a linear phase of exponential growth followed by a nonlinear adjustment to algebraic growth and decay in the fluctuating quantities. Remarkably, the velocity and magnetic field correlations associated with these growth and decay laws conspire to achieve saturation of angular momentum transport.

Antibacterial Potential of Northeastern Portugal Wild Plant Extracts and Respective Phenolic Compounds

PubMed Central

Ferreira, Isabel C. F. R.; Barros, Lillian; Carvalho, Ana Maria; Soares, Graça; Henriques, Mariana

2014-01-01

The present work aims to assess the antibacterial potential of phenolic extracts, recovered from plants obtained on the North East of Portugal, and of their phenolic compounds (ellagic, caffeic, and gallic acids, quercetin, kaempferol, and rutin), against bacteria commonly found on skin infections. The disk diffusion and the susceptibility assays were used to identify the most active extracts and phenolic compounds. The effect of selected phenolic compounds on animal cells was assessed by determination of cellular metabolic activity. Gallic acid had a higher activity, against gram-positive (S. epidermidis and S. aureus) and gram-negative bacteria (K. pneumoniae) at lower concentrations, than the other compounds. The caffeic acid, also, showed good antibacterial activity against the 3 bacteria used. The gallic acid was effective against the 3 bacteria without causing harm to the animal cells. Gallic and caffeic acid showed a promising applicability as antibacterial agents for the treatment of infected wounds. PMID:24804249

NICER Eyes on Bursting Stars

NASA Astrophysics Data System (ADS)

Kohler, Susanna

2018-03-01

What happens to a neutron stars accretion disk when its surface briefly explodes? A new instrument recently deployed at the International Space Station (ISS) is now watching bursts from neutron stars and reporting back.Deploying a New X-Ray MissionLaunch of NICER aboard a Falcon 9 rocket in June 2017. [NASA/Tony Gray]In early June of 2017, a SpaceX Dragon capsule on a Falcon 9 rocket launched on a resupply mission to the ISS. The pressurized interior of the Dragon contained the usual manifest of crew supplies, spacewalk equipment, and vehicle hardware. But the unpressurized trunk of the capsule held something a little different: the Neutron star Interior Composition Explorer (NICER).In the two weeks following launch, NICER was extracted from the SpaceX Dragon capsule and installed on the ISS. And by the end of the month, the instrument was already collecting its first data set: observations of a bright X-ray burst from Aql X-1, a neutron star accreting matter from a low-mass binary companion.Impact of BurstsNICERs goal is to provide a new view of neutron-star physics at X-ray energies of 0.212 keV a window that allows us to explore bursts of energy that neutron stars sometimes emit from their surfaces.Artists impression of an X-ray binary, in which a compact object accretes material from a companion star. [ESA/NASA/Felix Mirabel]In X-ray burster systems, hydrogen- and helium-rich material from a low-mass companion star piles up in an accretion disk around the neutron star. This material slowly funnels onto the neutron stars surface, forming a layer that gravitationally compresses and eventually becomes so dense and hot that runaway nuclear fusion ignites.Within seconds, the layer of material is burned up, producing a burst of emission from the neutron star that outshines even the inner regions of the hot accretion disk. Then more material funnels onto the neutron star and the process begins again.Though we have a good picture of the physics that causes these bursts, we dont yet understand the impact that these X-ray flashes have on the accretion disk and the environment surrounding the neutron star. In a new study led by Laurens Keek (University of Maryland), a team of scientists now details what NICER has learned on this subject.Extra X-RaysLight curve (top) and hardness ratio (bottom) for the X-ray burst from Aql X-1 captured by NICER on 3 July 2017. [Keek et al. 2018]In addition to thermal emission from the neutron star, NICER revealed an excess of soft X-ray photons below 1 keV during Aql X-1s burst. The authors propose two possible models for this emission:The burst radiation from the neutron stars surface was reprocessed i.e., either scattered or absorbed and re-emitted by the accretion disk.The persistent, usual accretion flow was enhanced as a result of the bursts radiation drag on the disk, briefly bumping up the disks X-ray flux.While we cant yet conclusively statewhich mechanismdominates, NICERs observations do show that bursts have a substantial impact on their accretion environment. And, as there are over 100 such X-ray burster systems in our galaxy, we can expect that NICER will allow us to better explore the effect of X-ray bursts on neutron-star disks and their surroundings inmany different systems in the future.BonusCheck out the awesome gif below, provided by NASA, which shows NICER being extracted fromthe Dragon capsules trunk by a robotic arm.CitationL. Keek et al 2018 ApJL 855 L4. doi:10.3847/2041-8213/aab104

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

Cohen, J; Dossa, D; Gokhale, M

Critical data science applications requiring frequent access to storage perform poorly on today's computing architectures. This project addresses efficient computation of data-intensive problems in national security and basic science by exploring, advancing, and applying a new form of computing called storage-intensive supercomputing (SISC). Our goal is to enable applications that simply cannot run on current systems, and, for a broad range of data-intensive problems, to deliver an order of magnitude improvement in price/performance over today's data-intensive architectures. This technical report documents much of the work done under LDRD 07-ERD-063 Storage Intensive Supercomputing during the period 05/07-09/07. The following chapters describe:more » (1) a new file I/O monitoring tool iotrace developed to capture the dynamic I/O profiles of Linux processes; (2) an out-of-core graph benchmark for level-set expansion of scale-free graphs; (3) an entity extraction benchmark consisting of a pipeline of eight components; and (4) an image resampling benchmark drawn from the SWarp program in the LSST data processing pipeline. The performance of the graph and entity extraction benchmarks was measured in three different scenarios: data sets residing on the NFS file server and accessed over the network; data sets stored on local disk; and data sets stored on the Fusion I/O parallel NAND Flash array. The image resampling benchmark compared performance of software-only to GPU-accelerated. In addition to the work reported here, an additional text processing application was developed that used an FPGA to accelerate n-gram profiling for language classification. The n-gram application will be presented at SC07 at the High Performance Reconfigurable Computing Technologies and Applications Workshop. The graph and entity extraction benchmarks were run on a Supermicro server housing the NAND Flash 40GB parallel disk array, the Fusion-io. The Fusion system specs are as follows: SuperMicro X7DBE Xeon Dual Socket Blackford Server Motherboard; 2 Intel Xeon Dual-Core 2.66 GHz processors; 1 GB DDR2 PC2-5300 RAM (2 x 512); 80GB Hard Drive (Seagate SATA II Barracuda). The Fusion board is presently capable of 4X in a PCIe slot. The image resampling benchmark was run on a dual Xeon workstation with NVIDIA graphics card (see Chapter 5 for full specification). An XtremeData Opteron+FPGA was used for the language classification application. We observed that these benchmarks are not uniformly I/O intensive. The only benchmark that showed greater that 50% of the time in I/O was the graph algorithm when it accessed data files over NFS. When local disk was used, the graph benchmark spent at most 40% of its time in I/O. The other benchmarks were CPU dominated. The image resampling benchmark and language classification showed order of magnitude speedup over software by using co-processor technology to offload the CPU-intensive kernels. Our experiments to date suggest that emerging hardware technologies offer significant benefit to boosting the performance of data-intensive algorithms. Using GPU and FPGA co-processors, we were able to improve performance by more than an order of magnitude on the benchmark algorithms, eliminating the processor bottleneck of CPU-bound tasks. Experiments with a prototype solid state nonvolative memory available today show 10X better throughput on random reads than disk, with a 2X speedup on a graph processing benchmark when compared to the use of local SATA disk.« less

Molecular identification of marine symbiont bacteria of gastropods from the waters of the Krakal coast Yogyakarta and its potential as a Multi-Drug Resistant (MDR) antibacterial agent

NASA Astrophysics Data System (ADS)

Bahry, Muhammad Syaifudien; Pringgenies, Delianis; Trianto, Agus

2017-01-01

The resistance of pathogenic bacteria may occur to many types of antibiotics, especially in cases of non-compliance use of antibiotics, which likely to allow the evolution of Multi-Drug Resistant (MDR) bacteria. Gastropods seas are marine invertebrates informed capable of production of secondary metabolites as antibacterial MDR. The purpose of the study was the isolation and identification of gastropod symbiont bacteria found in the waters of Krakal, Gunung Kidul, Yogyakarta, which has the ability to produce antibacterial compounds against MDR(Escherichia coli, Enterobacter cloacae, Klebsiella pneumoniae, MRSA (methicillin-Resistant Staphylococcus aureus), Staphylococcus aureus, and Staphylococcus homunis) molecular. Stages of this research began with the isolation of bacteria, bacteria screening for anti-MDR compound, mass culture, and extraction, antibacterial activity test, DNA extraction, amplification by PCR 16S rDNA and sequencing. The results of the study showed that 19 isolates of bacteria were isolated from three species of gastropods namely Littorina scabra, Cypraea moneta and Conus ebraeus. Among them, 4 isolates showed activity against MDR test bacteria (E. coli, E. cloacae, K. pneumoniae, S. aureus and S. homunis). The highest activity was displayed by code LS.G1.8 isolate with the largest inhibition zone 15.47±0.45mm on S. humonis at 250 µg/disk concentration. Isolate CM.G2.1 showed largest inhibition zone, with 21.5±0.07mm on MRSA at 1000 µg/disk concentration and isolate the largest inhibition zone CM.G2.5 14.37±0.81mm on MRSA 14.37±0.81mm at concentrations 1000 µg/disk. The molecular identification of isolates LS.G1.8 has 99% homology with Bacillus subtilis and isolates CM.G2.1 has 99% homology with Bacillus pumillus.

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

Hopwood, J.E.; Affeldt, B.

An IBM personal computer (PC), a Gerber coordinate digitizer, and a collection of other instruments make up a system known as the Coordinate Digitizer Interactive Processor (CDIP). The PC extracts coordinate data from the digitizer through a special interface, and then, after reformatting, transmits the data to a remote VAX computer, a floppy disk, and a display terminal. This system has improved the efficiency of producing printed circuit-board artwork and extended the useful life of the Gerber GCD-1 Digitizer. 1 ref., 12 figs.

Detection of Δ9-tetrahydrocannabinol in exhaled breath collected from cannabis users.

PubMed

Beck, Olof; Sandqvist, Sören; Dubbelboer, Ilse; Franck, Johan

2011-10-01

Exhaled breath has recently been proposed as a new possible matrix for drugs of abuse testing. A key drug is cannabis, and the present study was aimed at investigating the possibility of detecting tetrahydrocannabinol and tetrahydrocannabinol carboxylic acid in exhaled breath after cannabis smoking. Exhaled breath was sampled from 10 regular cannabis users and 8 controls by directing the exhaled breath by suction through an Empore C(18) disk. The disk was extracted with hexane/ethyl acetate, and the resulting extract was evaporated to dryness and redissolved in 100 μL hexane/ethyl acetate. A 3-μL aliquot was injected onto the LC-MS-MS system and analyzed using positive electrospray ionization and selected reaction monitoring. In samples collected 1-12 h after cannabis smoking, tetrahydrocannabinol was detected in all 10 subjects. The rate of excretion was between 9.0 and 77.3 pg/min. Identification of tetrahydrocannabinol was based on correct retention time relative to tetrahydrocannabinol-d(3) and correct product ion ratio. In three samples, peaks were observed for tetrahydrocannabinol carboxylic acid, but these did not fulfill identification criteria. Neither tetrahydrocannabinol or tetrahydrocannabinol carboxylic acid was detected in the controls. These results confirm older reports that tetrahydrocannabinol is present in exhaled breath following cannabis smoking and extend the detection time from minutes to hours. The results further support the idea that exhaled breath is a promising matrix for drugs-of-abuse testing.

Amino acid precursors in lunar fines - Limits to the contribution of jet exhaust

NASA Technical Reports Server (NTRS)

Fox, S. W.; Harada, K.; Hare, P. E.

1976-01-01

A sample of lunar fines collected at a maximum distance, 6.5 km, from the descent engine on Apollo 17 has been analyzed for total amino acids obtainable by hydrolysis of aqueous extracts. The minimum amounts of amino acids, calculated for a disk of 6 km radius are 10,000 to 100,000 times those which could be contributed by the lunar module jet exhaust, on the basis of conservatively limiting assumptions. The amino acids thus obtained are not explainable as due to chemical or biological contamination; their source is accordingly inferred as lunar. Under the conditions of hydrolysis of lunar extracts, cyanide is found to be converted, almost exclusively to glycine, to an extent of 0.0001.

Independent component analysis for automatic note extraction from musical trills

NASA Astrophysics Data System (ADS)

Brown, Judith C.; Smaragdis, Paris

2004-05-01

The method of principal component analysis, which is based on second-order statistics (or linear independence), has long been used for redundancy reduction of audio data. The more recent technique of independent component analysis, enforcing much stricter statistical criteria based on higher-order statistical independence, is introduced and shown to be far superior in separating independent musical sources. This theory has been applied to piano trills and a database of trill rates was assembled from experiments with a computer-driven piano, recordings of a professional pianist, and commercially available compact disks. The method of independent component analysis has thus been shown to be an outstanding, effective means of automatically extracting interesting musical information from a sea of redundant data.

Antibacterial activity study of Attacus atlas cocoon against Staphylococcus aureus and Escherichia coli with diffusion and dilution method

NASA Astrophysics Data System (ADS)

Aminah; Nugraheni, E. R.; Yugatama, A.

2018-03-01

The aim of this study was to evaluate the antibacterial activity from Attacus atlas cocoon extract against Gram-negative bacteria (Escherichia coli) and Gram-positive bacteria (Staphylococcus aureus) with 3 diffferent solvents polar, semi-polar and non polar which was ethanol, ethyl acetate and chloroform, also to determine the Minimum Inhibitory Concentration (MIC) and Minimum Bactericidal Concentration (MBC) of the extract. Cocoon was extracted with maceration method using 3 solvents with ratio of sample and solvent 1:10. Antibacterial activity of the Extracts obtained was evaluated with Agar disk diffusion method. The best result was then continued to determine the MIC and MBC of the extract using broth macro-dilution method. The results show that each of the extracts have antibacterial activity with broad spectrum against two different type of bacteria at concentration of 1 g/mL with different clear zone between these extracts. Clear zone from the biggest to the smallest against Escherichia coli was ethyl acetate (10.5 mm), chloroform (9 mm) and ethanol (8 mm). While against Staphylococcus aureus, was obtained by chloroform (12.5 mm), ethyl acetate (10.5 mm) and ethanol (7 mm). The MIC value of extracts can not be determine. The smallest MBC value against both bacteria was obtained by ethyl acetate with concentration of 3.125% b/v as a bactericidal.

Identification and evaluation of semiochemicals for the biological control of the beetle Omorgus suberosus (F.) (Coleoptera: Trogidae), a facultative predator of eggs of the sea turtle Lepidochelys olivacea (Eschscholtz).

PubMed

Cortez, Vieyle; Verdú, José R; Ortiz, Antonio J; Halffter, Gonzalo

2017-01-01

The beetle Omorgus suberosus (F.) is a facultative predator of eggs of the olive ridley turtle Lepidochelys olivacea (Eschscholtz). Laboratory and field investigations were conducted in order to characterize volatile attractants of O. suberosus and to explore the potential for application of these volatiles in a selective mass trapping method. Headspace sorptive extraction (HSSE) coupled to thermo-desorption gas chromatography-mass spectrometry (TD-GC-MS) analysis of the volatile constituents from beetles or turtle nests revealed 24 potential compounds. However, electroantennographic (EAG) measurements revealed antennal sensitivity only to indole, linoleic acid, trimethylamine, dimethyl sulphide, dimethyl disulphide and ammonia. Behavioural tests showed that these compounds are highly attractive to O. suberosus. Field trapping experiments revealed that indole and ammonia were more attractive than the other volatile compounds and showed similar attractiveness to that produced by conventional baits (chicken feathers). The use of a combined bait of indole and NH3 would therefore be the most effective trap design. The data presented are the first to demonstrate effective massive capture of O. suberosus using an attractant-based trapping method. These findings have potential for the development of an efficient mass trapping method for control of this beetle as part of efforts towards conservation of L. olivacea at La Escobilla in Oaxaca, Mexico.

Silicone passive equilibrium samplers as 'chemometers' in eels and sediments of a Swedish lake.

PubMed

Jahnke, Annika; Mayer, Philipp; McLachlan, Michael S; Wickström, Håkan; Gilbert, Dorothea; MacLeod, Matthew

2014-03-01

Passive equilibrium samplers deployed in two or more media of a system and allowed to come to equilibrium can be viewed as 'chemometers' that reflect the difference in chemical activities of contaminants between the media. We applied silicone-based equilibrium samplers to measure relative chemical activities of seven 'indicator' polychlorinated biphenyls (PCBs) and hexachlorobenzene in eels and sediments from a Swedish lake. Chemical concentrations in eels and sediments were also measured using exhaustive extraction methods. Lipid-normalized concentrations in eels were higher than organic carbon-normalized concentrations in sediments, with biota-sediment accumulation factors (BSAFs) of five PCBs ranging from 2.7 to 12.7. In contrast, chemical activities of the same pollutants inferred by passive sampling were 3.5 to 31.3 times lower in eels than in sediments. The apparent contradiction between BSAFs and activity ratios is consistent with the sorptive capacity of lipids exceeding that of sediment organic carbon from this ecosystem by up to 50-fold. Factors that may contribute to the elevated activity in sediments are discussed, including slower response of sediments than water to reduced emissions, sediment diagenesis and sorption to phytoplankton. The 'chemometer' approach has the potential to become a powerful tool to study the thermodynamic controls on persistent organic chemicals in the environment and should be extended to other environmental compartments.

Identification and evaluation of semiochemicals for the biological control of the beetle Omorgus suberosus (F.) (Coleoptera: Trogidae), a facultative predator of eggs of the sea turtle Lepidochelys olivacea (Eschscholtz)

PubMed Central

Cortez, Vieyle; Ortiz, Antonio J.; Halffter, Gonzalo

2017-01-01

The beetle Omorgus suberosus (F.) is a facultative predator of eggs of the olive ridley turtle Lepidochelys olivacea (Eschscholtz). Laboratory and field investigations were conducted in order to characterize volatile attractants of O. suberosus and to explore the potential for application of these volatiles in a selective mass trapping method. Headspace sorptive extraction (HSSE) coupled to thermo-desorption gas chromatography–mass spectrometry (TD-GC-MS) analysis of the volatile constituents from beetles or turtle nests revealed 24 potential compounds. However, electroantennographic (EAG) measurements revealed antennal sensitivity only to indole, linoleic acid, trimethylamine, dimethyl sulphide, dimethyl disulphide and ammonia. Behavioural tests showed that these compounds are highly attractive to O. suberosus. Field trapping experiments revealed that indole and ammonia were more attractive than the other volatile compounds and showed similar attractiveness to that produced by conventional baits (chicken feathers). The use of a combined bait of indole and NH3 would therefore be the most effective trap design. The data presented are the first to demonstrate effective massive capture of O. suberosus using an attractant-based trapping method. These findings have potential for the development of an efficient mass trapping method for control of this beetle as part of efforts towards conservation of L. olivacea at La Escobilla in Oaxaca, Mexico. PMID:28192472

Changes in total phenol, flavonoid contents and anti-Lactobacillus activity of Callisia fragrans due to extraction solvent

NASA Astrophysics Data System (ADS)

Le, Thom; Cao, Diem Kieu; Pham, Thanh Vy; Huynh, Tan Dat; Ta, Nhat Thuy Anh; Nguyen, Ngoc Thao Linh; Nguyen, Huu Thanh; Le, Hue Huong; Bui, Anh Vo; Truong, Dieu-Hien

2018-04-01

Callisia fragrans is a wonder herb with many medicinal properties such as burn, dental diseases, cancer diseases and arthritis in folk medicine. It is noted that the phytochemical constituents and antimicrobial activity of traditional plants depend on not only the extracting method but also the solvent used for extraction. In this study, the effect of five extraction solvents (i.e., distilled water, 80% methanol, 80% ethanol, 80% ethyl acetate, and 80% chloroform) on yield, total phenolic content (TPC) and total flavonoid content (TFC) of Callisia leaves was determined. Besides, changes in anti-Lactobacillus fermentum activity of C. fragrans freeze-dried extract was also evaluated using disk-diffusion method. The recovery percentage of extractable yield of fresh leaves are ranged from 11.93% w/w for distilled water extract to 16.60% w/w for aqueous ethanol extracts. The yield of 80% aqueous methanol extract (16.27% w/w) is only slightly less than that of the ethanol extract. Significant differences were observed among TPC and TFC obtaining by 80% methanol (0.0522% and 0.0335% w/w, respectively) compared to other solvents (p < 0.05). TPC and TFC of C. fragrans extracts increase in the following order: distilled water < 80% chloroform < 80% ethyl acetate < 80% ethanol < 80% methanol. The results revealed that 80% aqueous methanol Calissia extracts has moderate inhibition (9.0 mm of inhibition zone for 1.5 mg/mL of extracts) of L. fermentum compared to standard antibacterial agent. Based on the study results, it can be concluded that the yield, TPC and TFC of C. frgrans extract varied with the extracting solvent. It also showed that Callisia extracts can prevent dental caries by inhibiting the growth of L. fermentum, towards new insights for treatment of dental caries.

Diffusion of water-soluble sorptive drugs in HEMA/MAA hydrogels.

PubMed

Liu, D E; Dursch, T J; Taylor, N O; Chan, S Y; Bregante, D T; Radke, C J

2016-10-10

We measure and, for the first time, theoretically predict four prototypical aqueous-drug diffusion coefficients in five soft-contact-lens material hydrogels where solute-specific adsorption is pronounced. Two-photon fluorescence confocal microscopy and UV/Vis-absorption spectrophotometry assess transient solute concentration profiles and concentration histories, respectively. Diffusion coefficients are obtained for acetazolamide, riboflavin, sodium fluorescein, and theophylline in 2-hydroxyethyl methacrylate/methacrylic acid (HEMA/MAA) copolymer hydrogels as functions of composition, equilibrium water content (30-90%), and aqueous pH (2 and 7.4). At pH2, MAA chains are nonionic, whereas at pH7.4, MAA chains are anionic (pKa≈5.2). All studied prototypical drugs specifically interact with HEMA and nonionic MAA (at pH2) moieties. Conversely, none of the prototypical drugs adsorb specifically to anionic MAA (at pH7.4) chains. As expected, diffusivities of adsorbing solutes are significantly diminished by specific interactions with hydrogel strands. Despite similar solute size, relative diffusion coefficients in the hydrogels span several orders of magnitude because of varying degrees of solute interactions with hydrogel-polymer chains. To provide a theoretical framework for the new diffusion data, we apply an effective-medium model extended for solute-specific interactions with hydrogel copolymer strands. Sorptive-diffusion kinetics is successfully described by local equilibrium and Henry's law. All necessary parameters are determined independently. Predicted diffusivities are in good agreement with experiment. Copyright © 2016 Elsevier B.V. All rights reserved.

Laboratory longitudinal diffusion tests: 1. Dimensionless formulations and validity of simplified solutions

NASA Astrophysics Data System (ADS)

Takeda, M.; Nakajima, H.; Zhang, M.; Hiratsuka, T.

2008-04-01

To obtain reliable diffusion parameters for diffusion testing, multiple experiments should not only be cross-checked but the internal consistency of each experiment should also be verified. In the through- and in-diffusion tests with solution reservoirs, test interpretation of different phases often makes use of simplified analytical solutions. This study explores the feasibility of steady, quasi-steady, equilibrium and transient-state analyses using simplified analytical solutions with respect to (i) valid conditions for each analytical solution, (ii) potential error, and (iii) experimental time. For increased generality, a series of numerical analyses are performed using unified dimensionless parameters and the results are all related to dimensionless reservoir volume (DRV) which includes only the sorptive parameter as an unknown. This means the above factors can be investigated on the basis of the sorption properties of the testing material and/or tracer. The main findings are that steady, quasi-steady and equilibrium-state analyses are applicable when the tracer is not highly sorptive. However, quasi-steady and equilibrium-state analyses become inefficient or impractical compared to steady state analysis when the tracer is non-sorbing and material porosity is significantly low. Systematic and comprehensive reformulation of analytical models enables the comparison of experimental times between different test methods. The applicability and potential error of each test interpretation can also be studied. These can be applied in designing, performing, and interpreting diffusion experiments by deducing DRV from the available information for the target material and tracer, combined with the results of this study.

Estimation of the water retention curve from the soil hydraulic conductivity and sorptivity in an upward infiltration process

NASA Astrophysics Data System (ADS)

Moret-Fernández, David; Angulo, Marta; Latorre, Borja; González-Cebollada, César; López, María Victoria

2017-04-01

Determination of the saturated hydraulic conductivity, Ks, and the α and n parameters of the van Genuchten (1980) water retention curve, θ(h), are fundamental to fully understand and predict soil water distribution. This work presents a new procedure to estimate the soil hydraulic properties from the inverse analysis of a single cumulative upward infiltration curve followed by an overpressure step at the end of the wetting process. Firstly, Ks is calculated by the Darcy's law from the overpressure step. The soil sorptivity (S) is then estimated using the Haverkamp et al., (1994) equation. Next, a relationship between α and n, f(α,n), is calculated from the estimated Sand Ks. The α and n values are finally obtained by the inverse analysis of the experimental data after applying the f(α,n) relationship to the HYDRUS-1D model. The method was validated on theoretical synthetic curves for three different soils (sand, loam and clay), and subsequently tested on experimental sieved soils (sand, loam, clay loam and clay) of known hydraulic properties. A robust relationship was observed between the theoretical α and nvalues (R2 > 0.99) of the different synthetic soils and those estimated from inverse analysis of the upward infiltration curve. Consistent results were also obtained for the experimental soils (R2 > 0.85). These results demonstrated that this technique allowed accurate estimates of the soil hydraulic properties for a wide range of textures, including clay soils.

Biosorption of uranium by Pseudomonas aeruginosa strain CSU: Characterization and comparison studies

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

Hu, M.Z.C.; Norman, J.M.; Faison, B.D.

1996-07-20

Pseudomonas aeruginosa strain CSU, a nongenetically engineered bacterial strain known to bind dissolved hexavalent uranium (as UO{sub 2}{sup 2+} and/or its cationic hydroxo complexes) was characterized with respect to its sorptive activity. The uranium biosorption equilibrium could be described by the Langmuir isotherm. The rate of uranium adsorption increased following permeabilization of the outer and/or cytoplasmic membrane by organic solvents such as acetone. P. aeruginosa CSU biomass was significantly more sorptive toward uranium than certain novel, patented biosorbents derived from algal or fungal biomass sources. P. aeruginosa CSU biomass was also competitive with commercial cation-exchange resins, particularly in the presencemore » of dissolved transition metals. Uranium binding by P. aeruginosa CSU was clearly pH dependent. Uranium loading capacity increased with increasing pH under acidic conditions, presumably as a function of uranium speciation and due to the H{sup +} competition at some binding sites. Nevertheless, preliminary evidence suggests that this microorganism is also capable of binding anionic hexavalent uranium complexes. Ferric iron was a strong inhibitor of uranium binding to P. aeruginosa CSU biomass, and the presence of uranium also decreased the Fe{sup 3+} loading when the biomass was not saturated with Fe{sup 3+}. Thus, a two-state process in which iron and uranium are removed in consecutive steps was proposed for efficient use of the biomass as a biosorbent in uranium removal from mine wastewater, especially acidic leachates.« less

A novel approach for the analysis of dimethylarsinic acid in various liquid samples by WDXRF combined to pre-concentration with solid phase extraction disk

NASA Astrophysics Data System (ADS)

An, J.; Kim, J.; Kong, M.; Kim, K.; Yoon, H.

2012-12-01

Once dimethylarsinic acid (DMA) was considered to a product of detoxification (biomethylation) of inorganic arsenicals in organisms, it is now thought to have severe health risk. Since DMA had been widely employed in industrial and agricultural fields (e.g., pesticides and herbicides), it was one of the most often determined species in the published literatures for last decades. In the present study, DMA was pre-concentrated from various liquid samples with strong cation exchange (SCX) disk functionalized with sulfonic groups, and then analyzed by wavelength dispersive X-ray fluorescence spectrometry (WDXRF). While arsenate (iAsV), arsenite (iAsIII), and monomethylarsonic acid (MMA) were not retained on the SCX disk at all, DMA was perfectly adsorbed onto the surface of SCX disk. We optimized analytical conditions of SCX-WDXRF system and its calibration curve exhibited a strong linearity (R2 = 0.9996). Limit of detection (LOD) was achieved to 0.254 μg/L if a 1 L of liquid sample was used. We aimed to achieve improved instrumental sensitivity and the LOD for the analysis of DMA in liquid samples compared to high performance liquid chromatography linked to inductively coupled plasma mass spectrometry (HPLC-ICPMS) conventionally used in arsenic speciation researches. Spike tests for iAsV, iAsIII, MMA, and DMA in three types of liquid samples (i.e., deionized water, synthetic seawater and landfill leachate) showed quantitative recoveries (i.e., 95-105%) when the line overlap between As-Kα and Pb-Lα was corrected. This system highlights a very good option in arsenic speciation fields due to its extreme simplicity of operation and low cost.

Comparison of the tensile bond strength of high-noble, noble, and base metal alloys bonded to enamel.

PubMed

Sen, D; Nayir, E; Pamuk, S

2000-11-01

Although the bond strengths of various resin composite luting materials have been reported in the literature, the evaluation of these systems with various cast alloys of different compositions has not been completely clarified. To evaluate the tensile bond strength of sandblasted high-noble, noble, and base metal alloys bonded to etched enamel by 2 different bonding agents of different chemical composition: Panavia-Ex (BIS-GMA) and Super-Bond (4-META acrylic). Flat enamel surfaces were prepared on buccal surfaces of 60 extracted noncarious human incisors. Teeth were divided into 3 groups of 20 each. Twenty circular disks of 5 mm diameter were prepared for casting for each group. Group I was cast with a high-noble, group II with a noble, and group III with a base metal alloy. The surfaces of the disks were sandblasted with 250 microm Al(2)O(3). Ten disks of each group were bonded to exposed enamel surfaces with Super-Bond and 10 disks with Panavia-Ex as recommended by the manufacturer. The tensile bond strength was measured with an Instron universal testing machine with a crosshead speed of 0.5 mm/min until failure occurred. Two-way ANOVA was used to evaluate the results. The differences in bond strengths of Super-Bond and Panavia-Ex with different alloys were not significant. The highest bond strengths were obtained in base metal alloys, followed by noble and high-noble alloys. These results were significant. Panavia-Ex and Super-Bond exhibited comparable tensile bond strengths. For both luting agents, the highest bond strengths were achieved with base metal alloys and the lowest with high-noble alloys.

Chemical Composition and Antibacterial and Cytotoxic Activities of Allium hirtifolium Boiss

PubMed Central

Ismail, Salmiah; Jalilian, Farid Azizi; Talebpour, Amir Hossein; Zargar, Mohsen; Shameli, Kamyar; Sekawi, Zamberi; Jahanshiri, Fatemeh

2013-01-01

Allium hirtifolium Boiss. known as Persian shallot, is a spice used as a traditional medicine in Iran and, Mediterranean region. In this study, the chemical composition of the hydromethanolic extract of this plant was analyzed using GC/MS. The result showed that 9-hexadecenoic acid, 11,14-eicosadienoic acid, and n-hexadecanoic acid are the main constituents. The antibacterial activity of the shallot extract was also examined by disk diffusion and microdilution broth assays. It was demonstrated that Persian shallot hydromethanolic extract was effective against 10 different species of pathogenic bacteria including methicillin resistant Staphylococcus aureus (MRSA), methicillin sensitive Staphylococcus aureus (MSSA), Staphylococcus aureus, Staphylococcus epidermidis, Streptococcus pneumoniae, Escherichia coli, Escherichia coli O157:H7, Salmonella typhimurium, Proteus mirabilis, and Klebsiella pneumoniae. Specifically, the minimum concentration of the extract which inhibited bacterial growth (MIC values) was 1.88 mg/mL for most of the gram-positive bacteria. This concentration was not much different from the concentration that was safe for mammalian cells (1.50 mg/mL) suggesting that the hydromethanolic extract of Persian shallot may be a safe and strong antibacterial agent. PMID:23484141

Antimicrobial activity of essential oil and aqueous and ethanol extracts of Teucrium polium L. subsp. gabesianum (L.H.) from Tunisia.

PubMed

Ben Othman, Mahmoud; Bel Hadj Salah-Fatnassi, Karima; Ncibi, Saida; Elaissi, Amer; Zourgui, Lazhar

2017-07-01

The antimicrobial effects of essential oil, ethanol and aqueous extracts of Teucrium polium L. were investigated against 13 microorganisms. Extracts and essential oil were obtained from maceration, decoction and hydrodistillation respectively. Samples were tested for their antimicrobial activity using the disk diffusion, the agar dilution and the agar incorporation method. Essential oil was analysed using GC/MS, results showed that β-pinene (35.97%) and α-pinene (13.32%) were the main components. Furthermore, essential oil exhibited the highest antimicrobial activity, it was most effective against Proteus mirabilis, Staphylococcus aureus and Citrobacter freundei where inhibition zone ranged between 15 and 25 mm, and with the microbial inhibitory concentration (MIC) values of 0.078-0.156 mg/ml. The oil and ethanol extract showed the best antifungal activity against Microsporum canis , Scopulariopsis brevicaulis , and Trichophyton rubrum with the inhibition percentage (I%) ranging from 18.94 to 100%. However, none of the samples exhibited antifungal activity against Aspergillus fumigatus . In this study, the obtained results showed significant effects of essential oils and ethanol extracts of T. polium which may used as a substitute to the synthetic drugs against certain microbial diseases.

Microextraction with polyethersulfone for bisphenol-A, alkylphenols and hormones determination in water samples by means of gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry analysis.

PubMed

Ros, O; Vallejo, A; Blanco-Zubiaguirre, L; Olivares, M; Delgado, A; Etxebarria, N; Prieto, A

2015-03-01

In the present work, the suitability of polyethersulfone (PES) tube was assessed for the simultaneous sorptive microextraction of commonly found endocrine disrupting compounds in natural waters such as bisphenol-A (BPA), nonylphenol technical mixture (NP mix), 4-tert-octylphenol (4tOP), 4-n-octylphenol (4-nOP), 17β-estradiol (E2) and 17α-ethynilestradiol (EE2). After the concentration of target compounds in the PES polymer, the analytes were recovered soaking the polymer with a suitable solvent (ethyl acetate or methanol), derivatized using N,O-bis(trimethylsilyl)trifluoroacetamide with 1% of trimethylchlorosilane (BSTFA+1% TMCS) and determined by gas chromatography-mass spectrometry (GC-MS). The analysis was also performed without derivatization step by means of liquid chromatography-tandem mass spectrometry (LC-MS/MS). Extraction parameters (addition of MeOH, ionic strength, extraction speed and time and desorption time) were evaluated and the optimum conditions were fixed as follows: 150 mL water samples containing a 10% (w/v) of sodium chloride and using 5 tubular PES sorbent fibers (1.5 cm length×0.7 mm o.d.). Equilibrium conditions were achieved after 9 h, with absolute extraction efficiencies ranging from 27 to 56%. On the whole, good apparent recoveries were achieved (68-103% and 81-122% for GC-MS and LC-MS/MS, respectively) using deuterated analogues as surrogates. Achieved quantification limits (LOQs) varied between 2-154 ng/L and 2-63 ng/L for all the compounds using GC-MS and LC-MS/MS, respectively. The effect of organic matter was evaluated previous to apply the final method to the analysis of estuarine and wastewater real samples. The comparison of both methods showed that overall, PES-LC-MS/MS provided shorter sample preparation time and better LODs, but PES-silylation-GC-MS allowed the simultaneous determination of all the studied compounds with adequate repeatability and accuracy. Copyright © 2014 Elsevier B.V. All rights reserved.

Numerical investigation of interactions between marine atmospheric boundary layer and offshore wind farm

NASA Astrophysics Data System (ADS)

Lyu, Pin; Chen, Wenli; Li, Hui; Shen, Lian

2017-11-01

In recent studies, Yang, Meneveau & Shen (Physics of Fluids, 2014; Renewable Energy, 2014) developed a hybrid numerical framework for simulation of offshore wind farm. The framework consists of simulation of nonlinear surface waves using a high-order spectral method, large-eddy simulation of wind turbulence on a wave-surface-fitted curvilinear grid, and an actuator disk model for wind turbines. In the present study, several more precise wind turbine models, including the actuator line model, actuator disk model with rotation, and nacelle model, are introduced into the computation. Besides offshore wind turbines on fixed piles, the new computational framework has the capability to investigate the interaction among wind, waves, and floating wind turbines. In this study, onshore, offshore fixed pile, and offshore floating wind farms are compared in terms of flow field statistics and wind turbine power extraction rate. The authors gratefully acknowledge financial support from China Scholarship Council (No. 201606120186) and the Institute on the Environment of University of Minnesota.

Liquid-Crystalline Collapse of Pulmonary Surfactant Monolayers

PubMed Central

Schief, William R.; Antia, Meher; Discher, Bohdana M.; Hall, Stephen B.; Vogel, Viola

2003-01-01

During exhalation, the surfactant film of lipids and proteins that coats the alveoli in the lung is compressed to high surface pressures, and can remain metastable for prolonged periods at pressures approaching 70 mN/m. Monolayers of calf lung surfactant extract (CLSE), however, collapse in vitro, during an initial compression at ∼45 mN/m. To gain information on the source of this discrepancy, we investigated how monolayers of CLSE collapse from the interface. Observations with fluorescence, Brewster angle, and light scattering microscopies show that monolayers containing CLSE, CLSE-cholesterol (20%), or binary mixtures of dipalmitoyl phosphatidylcholine(DPPC)-dihydrocholesterol all form bilayer disks that reside above the monolayer. Upon compression and expansion, lipids flow continuously from the monolayer into the disks, and vice versa. In several respects, the mode of collapse resembles the behavior of other amphiphiles that form smectic liquid-crystal phases. These findings suggest that components of surfactent films must collapse collectively rather than being squeezed out individually. PMID:12770885

Multiplex DNA detection of food allergens on a digital versatile disk.

PubMed

Tortajada-Genaro, Luis A; Santiago-Felipe, Sara; Morais, Sergi; Gabaldón, José Antonio; Puchades, Rosa; Maquieira, Ángel

2012-01-11

The development of a DNA microarray method on a digital versatile disk (DVD) is described for the simultaneous detection of traces of hazelnut ( Corylus avellana L.), peanut ( Arachis hypogaea ), and soybean ( Glycine max ) in foods. After DNA extraction, multiplex PCR was set up using 5'-labeled specific primers for Cor a 1, Ar h 2, and Le genes, respectively. Digoxin-labeled PCR products were detected by hybridization with 5'-biotinylated probes immobilized on a streptavidin-modified DVD surface. The reaction product attenuates the signal intensity of the laser that reached the DVD drive used as detector, correlating well with the amount of amplified sequence. Analytical performances showed a detection limit of 1 μg/g and good assay reproducibility (RSD 8%), suitable for the simultaneous detection of the three targeted allergens. The developed methodology was tested with several commercially available foodstuffs, demonstrating its applicability. The results were in good agreement, in terms of sensitivity and reproducibility, with those obtained with ELISA, PCR-gel agarose electrophoresis, and RT-PCR.

Safe Energy Source in Battery-operated Toys for Children.

PubMed

Rossi, Alfredo; Vignola, Silvia; Nason, Francesca; Boschetti, Federica; Bramerio, Manuela; Bailini, Alessandro; Pinarello, Giordano

2017-11-01

Serious and even fatal consequences of disk batteries ingestion in children are well known. Among other applications, disk batteries are used to power small toys, from which they can be unexpectedly extracted and swallowed. We tested a new cell intended for little toys (green cell [GC]), after 6 and 12 hours of in vitro close contact with esophageal swine mucosa. The GC was compared with lithium and silver button batteries under the same experimental conditions. Tissues in contact with the GC did not show pH variations nor histological alterations after 6 and 12 hours. In such conditions, statistically significant differences were found between the GC and the lithium and silver batteries. So far, multidisciplinary medical effort has been driven to both emergency approach and subsequent operative strategies in children with ingested batteries. Our trial demonstrates the possibility to primarily prevent battery-induced damages by designing new-generation safe cells with no tissue toxicity to power little toys intended for children.

Screening of plant resources with anti-ice nucleation activity for frost damage prevention.

PubMed

Suzuki, Shingo; Fukuda, Satoshi; Fukushi, Yukiharu; Arakawa, Keita

2017-11-01

Previous studies have shown that some polyphenols have anti-ice nucleation activity (anti-INA) against ice-nucleating bacteria that contribute to frost damage. In the present study, leaf disk freezing assay, a test of in vitro application to plant leaves, was performed for the screening of anti-INA, which inhibits the ice nucleation activity of an ice-nucleating bacterium Erwinia ananas in water droplets on the leaf surfaces. The application of polyphenols with anti-INA, kaempferol 7-O-β-glucoside and (-)-epigallocatechin gallate, to the leaf disk freezing assay by cooling at -4--6 °C for 3 h, revealed that both the compounds showed anti-INAs against E. ananas in water droplets on the leaf surfaces. Further, this assay also revealed that the extracts of five plant leaves showed high anti-INA against E. ananas in water droplets on leaf surfaces, indicating that they are the candidate resources to protect crops from frost damage.

Elucidation of Metallic Plume and Spatter Characteristics Based on SVM During High-Power Disk Laser Welding

NASA Astrophysics Data System (ADS)

Gao, Xiangdong; Liu, Guiqian

2015-01-01

During deep penetration laser welding, there exist plume (weak plasma) and spatters, which are the results of weld material ejection due to strong laser heating. The characteristics of plume and spatters are related to welding stability and quality. Characteristics of metallic plume and spatters were investigated during high-power disk laser bead-on-plate welding of Type 304 austenitic stainless steel plates at a continuous wave laser power of 10 kW. An ultraviolet and visible sensitive high-speed camera was used to capture the metallic plume and spatter images. Plume area, laser beam path through the plume, swing angle, distance between laser beam focus and plume image centroid, abscissa of plume centroid and spatter numbers are defined as eigenvalues, and the weld bead width was used as a characteristic parameter that reflected welding stability. Welding status was distinguished by SVM (support vector machine) after data normalization and characteristic analysis. Also, PCA (principal components analysis) feature extraction was used to reduce the dimensions of feature space, and PSO (particle swarm optimization) was used to optimize the parameters of SVM. Finally a classification model based on SVM was established to estimate the weld bead width and welding stability. Experimental results show that the established algorithm based on SVM could effectively distinguish the variation of weld bead width, thus providing an experimental example of monitoring high-power disk laser welding quality.

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

Xiang, N. B.; Qu, Z. N., E-mail: znqu@ynao.ac.cn

The ensemble empirical mode decomposition (EEMD) analysis is utilized to extract the intrinsic mode functions (IMFs) of the solar mean magnetic field (SMMF) observed at the Wilcox Solar Observatory of Stanford University from 1975 to 2014, and then we analyze the periods of these IMFs as well as the relation of IMFs (SMMF) with some solar activity indices. The two special rotation cycles of 26.6 and 28.5 days should be derived from different magnetic flux elements in the SMMF. The rotation cycle of the weak magnetic flux element in the SMMF is 26.6 days, while the rotation cycle of themore » strong magnetic flux element in the SMMF is 28.5 days. The two rotation periods of the structure of the interplanetary magnetic field near the ecliptic plane are essentially related to weak and strong magnetic flux elements in the SMMF, respectively. The rotation cycle of weak magnetic flux in the SMMF did not vary over the last 40 years because the weak magnetic flux element derived from the weak magnetic activity on the full disk is not influenced by latitudinal migration. Neither the internal rotation of the Sun nor the solar magnetic activity on the disk (including the solar polar fields) causes the annual variation of SMMF. The variation of SMMF at timescales of a solar cycle is more related to weak magnetic activity on the full solar disk.« less

Anti-Helicobacter pylori activity of plant extracts traditionally used for the treatment of gastrointestinal disorders

PubMed Central

Cogo, Laura Lúcia; Monteiro, Cristina Leise Bastos; Miguel, Marilis Dallarmi; Miguel, Obdulio Gomes; Cunico, Miriam Machado; Ribeiro, Marcelo Lima; de Camargo, Eloá Ramalho; Kussen, Gislene Maria Botão; Nogueira, Keite da Silva; Costa, Libera Maria Dalla

2010-01-01

The antibacterial activity of plant extracts obtained from Bixa orellana L., Chamomilla recutita L., Ilex paraguariensis A. St.-Hil., Malva sylvestris L., Plantago major L. and Rheum rhaponticum L. has been evaluated against two reference strains and eleven clinical isolates of Helicobacter pylori. All the plant species chosen are used in popular Brazilian cuisine and folk medicine in the treatment of gastrointestinal disorders. Initial screening was made by the disk diffusion test and then minimum inhibitory concentration was determined by the agar dilution method. The results presented in this work demonstrated that among the plant preparations analyzed, B. orellana L., C. recutita L., I. paraguariensis A. St.-Hil. and M. sylvestris L. were capable of inhibiting the in vitro growth of H. pylori. PMID:24031496

Aurora on Uranus - A Faraday disc dynamo mechanism

NASA Technical Reports Server (NTRS)

Hill, T. W.; Rassbach, M. E.; Dessler, A. J.

1983-01-01

A mechanism is proposed whereby the solar wind flowing past the magnetosphere of Uranus causes a Faraday disk dynamo topology to be established and power to be extracted from the kinetic energy of rotation of Uranus. An immediate consequence of this dynamo is the generation of Birkeland currents that flow in and out of the sunlit polar cap with the accompanying production of polar aurora. The power extracted from planetary rotation is calculated as a function of planetary dipole magnetic moment and the ionospheric conductivity of Uranus. For plausible values of ionospheric conductivity, the observed auroral power requires a magnetic moment corresponding to a surface equatorial field of the order of 4 Gauss, slightly larger than the value 1.8 Gauss given by the empirical 'magnetic Bodes law'.

Insecticidal components from field pea extracts: soyasaponins and lysolecithins.

PubMed

Taylor, Wesley G; Fields, Paul G; Sutherland, Daniel H

2004-12-15

Extracts from field peas (Pisum sativum L.) have previously been shown to have a utility to control insect pests. To identify potentially new bioinsecticides in field crops, we describe the fractionation of impure extracts (C8 extracts) derived from protein-rich fractions of commercial pea flour. The activity of separated fractions was determined by a flour disk antifeedant bioassay with the rice weevil [Sitophilus oryzae (L.)], an insect pest of stored products. Bioassay-guided fractionation showed that the triterpenoid saponin fractions were partly responsible for the antifeedant activity of C8 extracts. Soyasaponin I (soyasaponin Bb), isolated from peas and soybeans, and mixtures of soyasaponins, comprised of soyasaponins I-III and isolated from soybeans, were inactive antifeedants, but dehydrosoyasaponin I (the C-22 ketone derivative of soyasaponin I), a minor component found in C8 extracts, was shown to be an active component. Dehydrosoyasaponin I (soyasaponin Be) and soyasaponin VI (soyasaponin betag) coeluted under conditions of silica gel thin-layer chromatography and C18 high-performance liquid chromatography. However, dehydrosoyasaponin I could be isolated from saponin-enriched fractions with a reversed phase column of styrene/divinylbenzene operated at alkaline pH. Phospholipids of the lysolecithin type were also identified in saponin fractions of C8 extracts from peas. Three of the lysolecithins were inactive alone against rice weevils, but mixtures of these phospholipids enhanced the insecticidal activity of dehydrosoyasaponin I.

Semiautomatic sequential extraction of polycyclic aromatic hydrocarbons and elemental bio-accessible fraction by accelerated solvent extraction on a single particulate matter sample.

PubMed

Astolfi, Maria Luisa; Di Filippo, Patrizia; Gentili, Alessandra; Canepari, Silvia

2017-11-01

We describe the optimization and validation of a sequential extractive method for the determination of the polycyclic aromatic hydrocarbons (PAHs) and elements (Al, As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Se, V and Zn) that are chemically fractionated into bio-accessible and mineralized residual fractions on a single particulate matter filter. The extraction is performed by automatic accelerated solvent extraction (ASE); samples are sequentially treated with dichloromethane/acetone (4:1) for PAHs extraction and acetate buffer (0.01M; pH 4.5) for elements extraction (bio-accessible fraction). The remaining solid sample is then collected and subjected to acid digestion with HNO 3 :H 2 O 2 (2:1) to determine the mineralized residual element fraction. We also describe a homemade ASE cell that reduces the blank values for most elements; in this cell, the steel frit was replaced by a Teflon pierced disk and a Teflon cylinder was used as the filler. The performance of the proposed method was evaluated in terms of recovery from standard reference material (SRM 1648 and SRM 1649a) and repeatability. The equivalence between the new ASE method and conventional methods was verified for PAHs and for bio-accessible and mineralized residual fractions of elements on PM 10 twin filters. Copyright © 2017 Elsevier B.V. All rights reserved.

Bifunctional anion-exchange resins with improved selectivity and exchange kinetics

DOEpatents

Alexandratos, Spiro D.; Brown, Gilbert M.; Bonnesen, Peter V.; Moyer, Bruce A.

2000-01-01

Disclosed herein are a class of anion exchange resins containing two different exchange sites with improved selectivity and sorptive capability for chemical species in solution, such as heptavalent technetium (as pertechnetate anion, TcO.sub.4.sup.-). The resins are prepared by first reacting haloalkylated crosslinked copolymer beads with a large tertiary amine in a solvent in which the resin beads can swell, followed by reaction with a second, smaller, tertiary amine to more fully complete the functionalization of the resin. The resins have enhanced selectivity, capacity, and exchange kinetics.

Effect of wind turbine wakes on summer-time wind profiles in the US Great Plains

NASA Astrophysics Data System (ADS)

Rhodes, M. E.; Lundquist, J. K.; Aitken, M.

2011-12-01

Wind energy is steadily becoming a significant source of grid electricity in the United States, and the Midwestern United States provides one of the nation's richest wind resources. This study examines the effect of wind turbine wakes on the wind profile in central Iowa. Data were collected using a coherent Doppler LiDAR system located approximately 2.5 rotor diameters north of a row of modern multi-MW wind turbine generators. The prevailing wind direction was from the South allowing the LiDAR to capture wind turbine wake properties; however, a number of periods existed where the LiDAR captured undisturbed flow. The LiDAR system reliably obtained readings up to 200 m above ground level (AGL), spanning the entire rotor disk (~40 m to 120 m AGL) which far surpasses the information provided by traditional wind resource assessment instrumentation. We extract several relevant parameters from the lidar data including: horizontal wind speed, vertical velocity, horizontal turbulence intensity, wind shear, and turbulent kinetic energy (TKE). Each time period at a particular LiDAR measurement height was labeled "wake" or "undisturbed" based on the wind direction at that height. Wake and undisturbed data were averaged separately to create a time-height cross-section averaged day for each parameter. Significant differences between wake and undisturbed data emerge. During the day, wake conditions experience larger values of TKE within the altitudes of the turbine rotor disk while TKE values above the rotor disk are similar between waked and undisturbed conditions. Furthermore, the morning transition of TKE in the atmospheric boundary layer commences earlier during wake conditions than in undisturbed conditions, and the evening decay of TKE persists longer during wake conditions. Waked wind shear is consistently greater than undisturbed periods at the edges of the wind turbine rotor disk (40m & 120m AGL), but especially so during the night where wind shear values during wake conditions are three times larger than in undisturbed conditions. Waked conditions show an increased rate of nocturnal subsidence over that of undisturbed conditions, likely due to the momentum deficit as a result of energy extraction by the turbine. Turbulent intensity shows increased levels and longevity in the waked rotor region when compared to the undisturbed conditions. The presentation will present these differences between waked and undisturbed conditions, and compare these observations to the phenomena accounted for in traditional wind turbine wake models.

The potential of achiral sponge-derived and synthetic bromoindoles as selective cytotoxins against PANC-1 tumor cells.

PubMed

Lorig-Roach, Nicholas; Hamkins-Indik, Frances; Johnson, Tyler A; Tenney, Karen; Valeriote, Frederick A; Crews, Phillip

2018-01-11

Our quest to isolate and characterize natural products with in vitro solid tumor selectivity is driven by access to repositories of Indo-Pacific sponge extracts. In this project an extract of a species of Haplosclerida sponge obtained from the US NCI Natural Products Repository displayed, by in vitro disk diffusion assay (DDA) and IC 50 determinations, selective cytotoxicity with modest potency to a human pancreatic cancer cell line (PANC-1) relative to the human lymphoblast leukemia cell line (CCRF-CEM). Two brominated indoles, the known 6-bromo conicamin ( 1 ) and the new derivative, 6-Br-8-keto-conicamin A ( 2 ), were identified and 2 (IC 50 1.5 μM for the natural product vs 4.1 μM for the synthetic material) was determined to be responsible for the cytotoxic activity of the extract against the PANC-1 tumor cell line. The new natural product and ten additional analogs were prepared for further SAR testing.

Antibacterial activity of Phyllantus emblica, Coriandrum sativum, Culinaris medic, Lawsonia alba and Cucumis sativus.

PubMed

Khan, Dawood Ali; Hassan, Fouzia; Ullah, Hanif; Karim, Sabiha; Baseer, Abdul; Abid, Mobasher Ali; Ubaidi, Muhammad; Khan, Shujaat Ali; Murtaza, Ghulam

2013-01-01

Present study deals with the demonstration of the antibacterial activity of very common medicinal plants of Pakistani origin i.e., Phyllantus emblica, Coriandrum sativum, Culinaris medic, Lawsonia alba and Cucumis sativus. The extracts were prepared in crude form by the use of hydro-alcoholic solution and were screened for antibacterial activity against various bacterial species by disk diffusion method. Assay was performed using clinical isolates of B. cereus, S. aureus, P. aeruginosa and E. coli. Crude extract of Phyllantus emblica fruit exhibited strong activity against standard cultures of all studied bacteria. Lawsonia alba showed good activity against standard cultures of all the used microorganisms. Coriandrum sativum was effective only against Bacillus cereus, while Cucumis sativus and Culinaris medic showed poor activity against Pseudomonas aeruginosa only. Hence, Phyllantus emblica exhibited strong antibacterial activity against a wide range of bacteria it means that Phyllantus emblica extract contains some compounds which have broad spectrum of bactericidal activity.

System and Method for High-Speed Data Recording

NASA Technical Reports Server (NTRS)

Taveniku, Mikael B. (Inventor)

2017-01-01

A system and method for high speed data recording includes a control computer and a disk pack unit. The disk pack is provided within a shell that provides handling and protection for the disk packs. The disk pack unit provides cooling of the disks and connection for power and disk signaling. A standard connection is provided between the control computer and the disk pack unit. The disk pack units are self sufficient and able to connect to any computer. Multiple disk packs are connected simultaneously to the system, so that one disk pack can be active while one or more disk packs are inactive. To control for power surges, the power to each disk pack is controlled programmatically for the group of disks in a disk pack.

Phytochemical profiles and antimicrobial activity of aromatic Malaysian herb extracts against food-borne pathogenic and food spoilage microorganisms.

PubMed

Aziman, Nurain; Abdullah, Noriham; Noor, Zainon Mohd; Kamarudin, Wan Saidatul Syida Wan; Zulkifli, Khairusy Syakirah

2014-04-01

Preliminary phytochemical and flavonoid compounds of aqueous and ethanolic extracts of 6 aromatic Malaysian herbs were screened and quantified using Reverse-Phase High Performance Liquid Chromatography (RP-HPLC). The herbal extracts were tested for their antimicrobial activity against 10 food-borne pathogenic and food spoilage microorganisms using disk diffusion assay. The minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC)/minimum fungicidal concentration (MFC) of herbal extracts were determined. In the phytochemical screening process, both aqueous and ethanolic extracts of P. hydropiper exhibited presence of all 7 tested phytochemical compounds. Among all herbal extracts, the aqueous P. hydropiper and E. elatior extracts demonstrated the highest antibacterial activity against 7 tested Gram-positive and Gram-negative bacteria with diameter ranging from 7.0 to 18.5 mm and 6.5 to 19 mm, respectively. The MIC values for aqueous and ethanolic extracts ranged from 18.75 to 175 mg/mL and 0.391 to 200 mg/mL, respectively while the MBC/MFC values for aqueous and ethanolic extracts ranged from 25 to 200 mg/mL and 3.125 to 50 mg/mL, respectively. Major types of bioactive compounds in aqueous P. hydropiper and E. elatior extracts were identified using RP-HPLC instrument. Flavonoids found in these plants were epi-catechin, quercetin, and kaempferol. The ability of aqueous Persicaria hydropiper (L.) H. Gross and Etlingera elatior (Jack) R.M. Sm. extracts to inhibit the growth of bacteria is an indication of its broad spectrum antimicrobial potential. Hence these herbal extracts may be used as natural preservative to improve the safety and shelf-life of food and pharmaceutical products. © 2014 Institute of Food Technologists®

On the decay of outbursts in dwarf novae nad X-ray novae

NASA Technical Reports Server (NTRS)

Cannizzo, John K.

1994-01-01

We perform computations using a time-dependent model for the accretion disk limit-cycle mechanism to examine the decay of the optical light following the peak of a dwarf nova outburst. We present the results of a parameter study of the physical input variables which affect the decay rate. In the model, the decay is brought about by a cooling transition front which begins at large radii in the disk and moves inward. The nature of the decay is strongly influenced by the radial dependence of the accretion disk viscosity parameter alpha. To obtain exponential decays for typical dwarf nova parameters, we require alpha proportional to r(exp epsilon(sub 0)), where epsilon(sub 0) approximately = 0.3-0.4. The exact value of epsilon(sub 0) which produces exponential decays depends on factors such as the mass of the accreting star and the inner radius of the accretion disk. Therefore, the observed ubiquity of exponential decays in two different types of systems (dwarf novae and X-ray novae) leads us to believe that alpha is an unnatural scaling for the viscosity. The physics of the cooling transition front must be self-regulating in that the timescale (-parital derivative of lnSigma(r)/partial derivative +)(exp -1) (where Sigma is the surface density) for mass extraction across the front remains constant. This may be consistent with a scaling alpha proportional to (h/r)(exp n), where h is the local disk semi-thickness and n approximately 1-2. As regards the speed of the cooling front, we find v(sub F)(r) proportional to r(exp p), where p approximately 3 at large radii, with an abrupt transition to p approximately 0 at some smaller radius. The r(exp 3) dependence is much steeper than has been found by previous workers and appears to result from the strong variation of specific heat within the cooling front when the front resides at a large radius in the disk. The outflow of disk material across the cooling front causes a significant departure of dln T(sub dff0/dln r from the standard value of -0.75 (expected from steady state accretion) within about 0.2 dex in radius of the break associated with the cooling front -- T(sub eff) aproximately 10(exp 3.9) K (r/10(exp 10 cm)) (exp -0.1). These effects should be observable with eclipse mapping. Finally, it appears that the relatively slow decay rate for the optical flux in the 1975 outburst of A0620-00 can be accounted for if the primary is a approximately 10 Solar mass black hole.

Colours of minor bodies in the outer solar system. II. A statistical analysis revisited

NASA Astrophysics Data System (ADS)

Hainaut, O. R.; Boehnhardt, H.; Protopapa, S.

2012-10-01

We present an update of the visible and near-infrared colour database of Minor Bodies in the Outer Solar System (MBOSSes), which now includes over 2000 measurement epochs of 555 objects, extracted from over 100 articles. The list is fairly complete as of December 2011. The database is now large enough to enable any dataset with a large dispersion to be safely identified and rejected from the analysis. The selection method used is quite insensitive to individual outliers. Most of the rejected datasets were observed during the early days of MBOSS photometry. The individual measurements are combined in a way that avoids possible rotational artifacts. The spectral gradient over the visible range is derived from the colours, as well as the R absolute magnitude M(1,1). The average colours, absolute magnitude, and spectral gradient are listed for each object, as well as the physico-dynamical classes using a classification adapted from Gladman and collaborators. Colour-colour diagrams, histograms, and various other plots are presented to illustrate and investigate class characteristics and trends with other parameters, whose significances are evaluated using standard statistical tests. Except for a small discrepancy for the J-H colour, the largest objects, with M(1,1) < 5, are indistinguishable from the smaller ones. The larger ones are slightly bluer than the smaller ones in J-H. Short-period comets, Plutinos and other resonant objects, hot classical disk objects, scattered disk objects and detached disk objects have similar properties in the visible, while the cold classical disk objects and the Jupiter Trojans form two separate groups of their spectral properties in the visible wavelength range. The well-known colour bimodality of Centaurs is confirmed. The hot classical disk objects with large inclinations, or large orbital excitations are found to be bluer than the others, confirming a previously known result. Additionally, the hot classical disk objects with a smaller perihelion distance are bluer than those that do not come as close to the Sun. The bluer hot classical disk objects and resonant objects have fainter absolute magnitudes than the redder ones of the same class. Finally, we discuss possible scenarios for the origin of the colour diversity observed in MBOSSes, i.e. colouration caused by evolutionary or formation processes. The colour tables and all plots are also available on the MBOSS colour web page, which will be updated when new measurements are published Full Tables 2 and 3 are only available at the CDS via anonymous ftp to cdsarc.u-strasbg.fr (130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/546/A115

Tutorial: Performance and reliability in redundant disk arrays

NASA Technical Reports Server (NTRS)

Gibson, Garth A.

1993-01-01

A disk array is a collection of physically small magnetic disks that is packaged as a single unit but operates in parallel. Disk arrays capitalize on the availability of small-diameter disks from a price-competitive market to provide the cost, volume, and capacity of current disk systems but many times their performance. Unfortunately, relative to current disk systems, the larger number of components in disk arrays leads to higher rates of failure. To tolerate failures, redundant disk arrays devote a fraction of their capacity to an encoding of their information. This redundant information enables the contents of a failed disk to be recovered from the contents of non-failed disks. The simplest and least expensive encoding for this redundancy, known as N+1 parity is highlighted. In addition to compensating for the higher failure rates of disk arrays, redundancy allows highly reliable secondary storage systems to be built much more cost-effectively than is now achieved in conventional duplicated disks. Disk arrays that combine redundancy with the parallelism of many small-diameter disks are often called Redundant Arrays of Inexpensive Disks (RAID). This combination promises improvements to both the performance and the reliability of secondary storage. For example, IBM's premier disk product, the IBM 3390, is compared to a redundant disk array constructed of 84 IBM 0661 3 1/2-inch disks. The redundant disk array has comparable or superior values for each of the metrics given and appears likely to cost less. In the first section of this tutorial, I explain how disk arrays exploit the emergence of high performance, small magnetic disks to provide cost-effective disk parallelism that combats the access and transfer gap problems. The flexibility of disk-array configurations benefits manufacturer and consumer alike. In contrast, I describe in this tutorial's second half how parallelism, achieved through increasing numbers of components, causes overall failure rates to rise. Redundant disk arrays overcome this threat to data reliability by ensuring that data remains available during and after component failures.

Effects of microstructure on water imbibition in sandstones using X-ray computed tomography and neutron radiography

NASA Astrophysics Data System (ADS)

Zhao, Yixin; Xue, Shanbin; Han, Songbai; Chen, Zhongwei; Liu, Shimin; Elsworth, Derek; He, Linfeng; Cai, Jianchao; Liu, Yuntao; Chen, Dongfeng

2017-07-01

Capillary imbibition in variably saturated porous media is important in defining displacement processes and transport in the vadose zone and in low-permeability barriers and reservoirs. Nonintrusive imaging in real time offers the potential to examine critical impacts of heterogeneity and surface properties on imbibition dynamics. Neutron radiography is applied as a powerful imaging tool to observe temporal changes in the spatial distribution of water in porous materials. We analyze water imbibition in both homogeneous and heterogeneous low-permeability sandstones. Dynamic observations of the advance of the imbibition front with time are compared with characterizations of microstructure (via high-resolution X-ray computed tomography (CT)), pore size distribution (Mercury Intrusion Porosimetry), and permeability of the contrasting samples. We use an automated method to detect the progress of wetting front with time and link this to square-root-of-time progress. These data are used to estimate the effect of microstructure on water sorptivity from a modified Lucas-Washburn equation. Moreover, a model is established to calculate the maximum capillary diameter by modifying the Hagen-Poiseuille and Young-Laplace equations based on fractal theory. Comparing the calculated maximum capillary diameter with the maximum pore diameter (from high-resolution CT) shows congruence between the two independent methods for the homogeneous silty sandstone but less effectively for the heterogeneous sandstone. Finally, we use these data to link observed response with the physical characteristics of the contrasting media—homogeneous versus heterogeneous—and to demonstrate the sensitivity of sorptivity expressly to tortuosity rather than porosity in low-permeability sandstones.

Sealing of cracks in cement using microencapsulated sodium silicate

NASA Astrophysics Data System (ADS)

Giannaros, P.; Kanellopoulos, A.; Al-Tabbaa, A.

2016-08-01

Cement-based materials possess an inherent autogenous self-healing capability allowing them to seal, and potentially heal, microcracks. This can be improved through the addition of microencapsulated healing agents for autonomic self-healing. The fundamental principle of this self-healing mechanism is that when cracks propagate in the cementitious matrix, they rupture the dispersed capsules and their content (cargo material) is released into the crack volume. Various healing agents have been explored in the literature for their efficacy to recover mechanical and durability properties in cementitious materials. In these materials, the healing agents are most commonly encapsulated in macrocontainers (e.g. glass tubes or capsules) and placed into the material. In this work, microencapsulated sodium silicate in both liquid and solid form was added to cement specimens. Sodium silicate reacts with the calcium hydroxide in hydrated cement paste to form calcium-silicate-hydrate gel that fills cracks. The effect of microcapsule addition on rheological and mechanical properties of cement is reported. It is observed that the microcapsule addition inhibits compressive strength development in cement and this is observed through a plateau in strength between 28 and 56 days. The improvement in crack-sealing for microcapsule-containing specimens is quantified through sorptivity measurements over a 28 day healing period. After just seven days, the addition of 4% microcapsules resulted in a reduction in sorptivity of up to 45% when compared to specimens without any microcapsule addition. A qualitative description of the reaction between the cargo material and the cementitious matrix is also provided using x-ray diffraction analysis.

Gas-phase organics in environmental tobacco smoke. 1. Effects of smoking rate, ventilation, and furnishing level on emission factors.

PubMed

Singer, Brett C; Hodgson, Alfred T; Guevarra, Karla S; Hawley, Elisabeth L; Nazaroff, William W

2002-03-01

We measured the emissions of 26 gas-phase organic compounds in environmental tobacco smoke (ETS) using a model room that simulates realistic conditions in residences and offices. Exposure-relevant emission factors (EREFs), which include the effects of sorption and re-emission over a 24-h period, were calculated by mass balance from measured compound concentrations and chamber ventilation rates in a 50-m3 room constructed and furnished with typical materials. Experiments were conducted at three smoking rates (5, 10, and 20 cigarettes day(-1)), three ventilation rates (0.3, 0.6, and 2 h(-1)), and three furnishing levels (wallboard with aluminum flooring, wallboard with carpet, and full furnishings). Smoking rate did not affect EREFs, suggesting that sorption was linearly related to gas-phase concentration. Furnishing level and ventilation rate in the model room had little effect on EREFs of several ETS compounds including 1,3-butadiene, acrolein, acrylonitrile, benzene, toluene, and styrene. However, sorptive losses at low ventilation with full furnishings reduced EREFs for the ETS tracers nicotine and 3-ethenylpyridine by as much as 90 and 65% as compared to high ventilation, wallboard/aluminum experiments. Likewise, sorptive losses were 40-70% for phenol, cresols, naphthalene, and methylnaphthalenes. Sorption persisted for many compounds; for example, almost all of the sorbed nicotine and most of the sorbed cresol remained sorbed 3 days after smoking. EREFs can be used in models and with ETS tracer-based methods to refine and improve estimates of exposures to ETS constituents.

Application of biochar from food and wood waste as green admixture for cement mortar.

PubMed

Gupta, Souradeep; Kua, Harn Wei; Koh, Hui Jun

2018-04-01

Landfilling of food waste due to its low recycling rate is raising serious concerns because of associated soil and water contamination, and emission of methane and other greenhouse gases during the degradation process. This paper explores feasibility of using biochar derived from mixed food waste (FWBC), rice waste (RWBC) and wood waste (mixed wood saw dust, MWBC) as carbon sequestering additive in mortar. RWBC is prepared from boiled plain rice, while FWBC is prepared from combination of rice, meat, and vegetables in fixed proportion. Carbon content in FWBC, RWBC and MWBC were found to be 71%, 66% and 87% by weight respectively. Results show that addition of 1-2wt% of FWBC and RWBC in mortar results in similar mechanical strength as control mix (without biochar). 1wt% of FWBC led to 40% and 35% reduction in water penetration and sorptivity respectively, indicating higher impermeability of mortar. Biochar from mixed wood saw dust performed better in terms of mechanical and permeability properties. Increase in compressive strength and tensile strength by up to 20% was recorded, while depth of water penetration and sorptivity was reduced by about 60% and 38% respectively compared to control. Both FWBC and MWBC were found to act as reinforcement to mortar paste, which resulted in higher ductility than control at failure under flexure. This study suggests that biochar from food waste and mixed wood saw dust has the potential to be successfully deployed as additive in cement mortar, which would also promote waste recycling, and sequester high volume carbon in civil infrastructure. Copyright © 2017 Elsevier B.V. All rights reserved.

Automated on-line renewable solid-phase extraction-liquid chromatography exploiting multisyringe flow injection-bead injection lab-on-valve analysis.

PubMed

Quintana, José Benito; Miró, Manuel; Estela, José Manuel; Cerdà, Víctor

2006-04-15

In this paper, the third generation of flow injection analysis, also named the lab-on-valve (LOV) approach, is proposed for the first time as a front end to high-performance liquid chromatography (HPLC) for on-line solid-phase extraction (SPE) sample processing by exploiting the bead injection (BI) concept. The proposed microanalytical system based on discontinuous programmable flow features automated packing (and withdrawal after single use) of a small amount of sorbent (<5 mg) into the microconduits of the flow network and quantitative elution of sorbed species into a narrow band (150 microL of 95% MeOH). The hyphenation of multisyringe flow injection analysis (MSFIA) with BI-LOV prior to HPLC analysis is utilized for on-line postextraction treatment to ensure chemical compatibility between the eluate medium and the initial HPLC gradient conditions. This circumvents the band-broadening effect commonly observed in conventional on-line SPE-based sample processors due to the low eluting strength of the mobile phase. The potential of the novel MSFI-BI-LOV hyphenation for on-line handling of complex environmental and biological samples prior to reversed-phase chromatographic separations was assessed for the expeditious determination of five acidic pharmaceutical residues (viz., ketoprofen, naproxen, bezafibrate, diclofenac, and ibuprofen) and one metabolite (viz., salicylic acid) in surface water, urban wastewater, and urine. To this end, the copolymeric divinylbenzene-co-n-vinylpyrrolidone beads (Oasis HLB) were utilized as renewable sorptive entities in the micromachined unit. The automated analytical method features relative recovery percentages of >88%, limits of detection within the range 0.02-0.67 ng mL(-1), and coefficients of variation <11% for the column renewable mode and gives rise to a drastic reduction in operation costs ( approximately 25-fold) as compared to on-line column switching systems.

Considerations on ultra-trace analysis of phthalates in drinking water.

PubMed

Serôdio, P; Nogueira, J M F

2006-07-01

Stir bar sorptive extraction with liquid desorption followed by large volume injection and capillary gas chromatography coupled to mass spectrometry (SBSE-LD/LVI-GC-MS), had been applied for the determination of ultra-traces of seven-phthalates (dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, butyl benzyl phthalate, bis(2-ethylhexyl) adipate, bis(2-ethylhexyl) phthalate and bis(1-octyl) phthalate) in drinking water samples, which are included in the priority lists set by several international regulatory organizations. Instrumental calibration under the selected-ion monitoring mode acquisition (LVI-GC-MS(SIM)), experimental parameters that could affect the SBSE-LD efficiency, as well as, the control of the contamination profile are fully discussed. Throughout systematic assays on 30 mL water samples spiked at the 0.40 microg/L level, it had been established that stir bars coated with 47 microL of polydimethylsiloxane, an equilibrium time of 60 min (1,000 rpm) and methanol as back extraction solvent, allowed the best analytical performance to monitor phthalates in water matrices. From the data obtained, good accuracy and a remarkable reproducibility (< 14.8%) were attained, providing experimental recovery data in agreement with the theoretical equilibrium described by the octanol-water partition coefficients (K(PDMS/W) approximately K(O/W)), with the exception of bis(2-ethylhexyl) adipate, bis(2-ethylhexyl) phthalate and bis(1-octyl) phthalate, for which lower yields were measured. Additionally, a remarkable linear dynamic range between 25 and 2,000 ng/L (r(2)>0.99) and low detection limits (3-40 ng/L) were also achieved for the seven-phthalates studied. The application of the present method to monitor phthalates in tap and bottled mineral water samples, allowed convenient selectivity and high sensitivity up to 1.0 microg/L level, using the standard addition methodology. The proposed method showed to be feasible and sensitive with a low sample volume requirement to monitor phthalates in drinking water matrices at the ultra-trace level, in compliance with international regulatory directives on water quality.

Improvements on bar adsorptive microextraction (BAμE) technique--application for the determination of insecticide repellents in environmental water matrices.

PubMed

Almeida, C; Strzelczyk, Rafał; Nogueira, J M F

2014-03-01

Bar adsorptive microextraction combined with micro-liquid desorption followed by large volume injection-gas chromatography-mass spectrometry operating in the selected-ion monitoring acquisition mode (BAµE-µLD/LVI-GC-MS(SIM)), is proposed for the determination of trace levels of three insecticide repellents (N,N-diethyl-meta-toluamide (DEET), cis and trans permethrin (PERM)) in environmental water matrices. By comparing different sorbent coatings (five activated carbons and six polymers) through BAµE, an activated carbon (AC2) proved to be the best compromise between selectivity and efficiency, even against polydimethylsiloxane through stir bar sorptive extraction. The novel improvement proposed on the back-extraction stage performed in a single step, by reducing the desorption solvent volume at the microliter level, demonstrated remarkable performance turning possible to save time, making easier the practical manipulation and more environmentally friendly. Assays performed by BAµE(AC2)-µLD/LVI-GC-MS(SIM) on 25 mL of ultrapure water samples spiked at the 1.0 μg/L level, yielded recoveries ranging from 73.8±8.8% (trans-PERM) to 96.4±9.9% (DEET), under optimised experimental conditions. The analytical performance showed convenient detection limits (8-20 ng/L) and good linear dynamic ranges (0.04-4.0 µg/L) with suitable determination coefficients (r(2)>0.9963, DEET). Excellent repeatability were also achieved through intraday (RSD<14.9%) and interday (RSD<11.9%) experiments. The novel improvement on downsizing the BAµE device to half-size proved to be either a promising option in forthcoming to reduce still more the desorption solvent volume without losing microextraction efficiency. By using the standard addition methodology, the application of the present analytical approach on tap, ground, river, swimming-pool and estuary water samples revealed good sensitivity at trace level and absence of matrix effects. © 2013 Elsevier B.V. All rights reserved.

The effect of homogenization pressure on the flavor and flavor stability of whole milk powder.

PubMed

Park, Curtis W; Drake, MaryAnne

2017-07-01

Flavor is one of the key factors that can limit the application and shelf life of dried dairy ingredients. Many off-flavors are caused during ingredient manufacture that carry through into ingredient applications and decrease consumer acceptance. The objective of this research was to investigate the effect of homogenization pressure on the flavor and flavor stability of whole milk powder (WMP). Whole milk powder was produced from standardized pasteurized whole milk that was evaporated to 50% solids (wt/wt), homogenized in 2 stages with varying pressures (0/0, 5.5/1.4, 11.0/2.8, or 16.5/4.3 MPa), and spray dried. Whole milk powder was evaluated at 0, 3, and 6 mo of storage at 21°C. Sensory properties were evaluated by descriptive analysis. Volatile compounds were analyzed by sorptive stir bar extraction with gas chromatography-mass spectrometry. Fat globule size in condensed whole milk and particle size of powders were measured by laser diffraction. Surface free fat, inner free fat, and encapsulated fat of WMP were measured by solvent extractions. Phospholipid content was measured by ultra-high-performance liquid chromatography-evaporative light scattering. Furosine in WMP was analyzed by ultra-high-performance liquid chromatography-mass spectrometry. Increased homogenization pressure decreased cardboard and painty flavors, volatile lipid oxidation compound concentrations, fat globule size in condensed milk, surface free fat, and inner free fat in WMP. Encapsulated fat increased and phospholipid-to-encapsulated fat ratio decreased with higher homogenization pressure. Surface free fat in powders increased cardboard flavor and lipid oxidation. These results indicate that off-flavors were decreased with increased homogenization pressures in WMP due to the decrease in free fat. To decrease off-flavor intensities in WMP, manufacturers should carefully evaluate these parameters during ingredient manufacture. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Flavor and flavor chemistry differences among milks processed by high-temperature, short-time pasteurization or ultra-pasteurization.

PubMed

Jo, Y; Benoist, D M; Barbano, D M; Drake, M A

2018-05-01

Typical high-temperature, short-time (HTST) pasteurization encompasses a lower heat treatment and shorter refrigerated shelf life compared with ultra-pasteurization (UP) achieved by direct steam injection (DSI-UP) or indirect heat (IND-UP). A greater understanding of the effect of different heat treatments on flavor and flavor chemistry of milk is required to characterize, understand, and identify the sources of flavors. The objective of this study was to determine the differences in the flavor and volatile compound profiles of milk subjected to HTST, DSI-UP, or IND-UP using sensory and instrumental techniques. Raw skim and raw standardized 2% fat milks (50 L each) were processed in triplicate and pasteurized at 78°C for 15 s (HTST) or 140°C for 2.3 s by DSI-UP or IND-UP. Milks were cooled and stored at 4°C, then analyzed at d 0, 3, 7, and 14. Sensory attributes were determined using a trained panel, and aroma active compounds were evaluated by solid-phase micro-extraction or stir bar sorptive extraction followed by gas chromatography-mass spectrometry, gas chromatography-olfactometry, and gas chromatography-triple quad mass spectrometry. The UP milks had distinct cooked and sulfur flavors compared with HTST milks. The HTST milks had less diversity in aroma active compounds compared with UP milks. Flavor intensity of all milks decreased by d 14 of storage. Aroma active compound profiles were affected by heat treatment and storage time in both skim and 2% milk. High-impact aroma active compounds were hydrogen sulfide, dimethyl trisulfide, and methional in DSI-UP and 2 and 3-methylbutanal, furfural, 2-heptanone, 2-acetyl-1-pyrroline, 2-aminoacetophenone, benzaldehyde, and dimethyl sulfide in IND-UP. These results provide a foundation knowledge of the effect of heat treatments on flavor development and differences in sensory quality of UP milks. Copyright © 2018 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Herschel evidence for disk flattening or gas depletion in transitional disks

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

Keane, J. T.; Pascucci, I.; Espaillat, C.

Transitional disks are protoplanetary disks characterized by reduced near- and mid-infrared emission, with respect to full disks. This characteristic spectral energy distribution indicates the presence of an optically thin inner cavity within the dust disk believed to mark the disappearance of the primordial massive disk. We present new Herschel Space Observatory PACS spectra of [O I] 63.18 μm for 21 transitional disks. Our survey complements the larger Herschel GASPS program ({sup G}as in Protoplanetary Systems{sup )} by quadrupling the number of transitional disks observed with PACS in this wavelength. [O I] 63.18 μm traces material in the outer regions ofmore » the disk, beyond the inner cavity of most transitional disks. We find that transitional disks have [O I] 63.18 μm line luminosities ∼2 times fainter than their full disk counterparts. We self-consistently determine various stellar properties (e.g., bolometric luminosity, FUV excess, etc.) and disk properties (e.g., disk dust mass, etc.) that could influence the [O I] 63.18 μm line luminosity, and we find no correlations that can explain the lower [O I] 63.18 μm line luminosities in transitional disks. Using a grid of thermo-chemical protoplanetary disk models, we conclude that either transitional disks are less flared than full disks or they possess lower gas-to-dust ratios due to a depletion of gas mass. This result suggests that transitional disks are more evolved than their full disk counterparts, possibly even at large radii.« less

Antimicrobial, antibiofilm and cytotoxic activities of Hakea sericea Schrader extracts

PubMed Central

Luís, Ângelo; Breitenfeld, Luiza; Ferreira, Susana; Duarte, Ana Paula; Domingues, Fernanda

2014-01-01

Background: Hakea sericea Schrader is an invasive shrub in Portuguese forests. Objective: The goal of this work was to evaluate the antimicrobial activity of H. sericea extracts against several strains of microorganisms, including the ability to inhibit the formation of biofilms. Additionally the cytotoxic properties of these extracts, against human cells, were assessed. Materials and Methods: The antimicrobial activity of the methanolic extracts of H. sericea was assessed by disk diffusion assay and Minimum Inhibitory Concentration (MIC) value determination. The antibiofilm activity was determined by quantification of total biofilm biomass with crystal violet. Cytotoxicity was evaluated by hemolysis assay and 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) test. Results: For Gram-positive bacteria, MIC values of H. sericea methanolic extracts ranged between 0.040 and 0.625 mg/mL, whereas the fruits extract yielded the lowest MIC for several strains of microorganisms, namely, S. aureus, B. cereus, L. monocytogenes and clinical methicillin-resistant S. aureus (MRSA). Stems and fruits extract at 2.5 mg/mL effectively eradicated the biofilm of S. aureus ATCC 25923, SA 01/10 and MRSA 12/10. Regarding leaves extract, hemolysis was not observed, and in the case of stems and fruits, hemolysis was verified only for higher concentrations, suggesting its low toxicity. Fruits extract presented no toxic effect to normal human dermal fibroblasts (NHDF) cells however for concentrations of 0.017 and 0.008 mg/mL this extract was able to decrease human breast adenocarcinoma cells (MCF-7) viability in about 60%, as MTT test results had confirmed. This is a clearly demonstrator of the cytotoxicity of this extract against MCF-7 cells. PMID:24914310

Phytochemical analysis and antibacterial activities extracts of mangrove leaf against the growth of some pathogenic bacteria.

PubMed

Alizadeh Behbahani, Behrooz; Tabatabaei Yazdi, Farideh; Shahidi, Fakhri; Noorbakhsh, Hamid; Vasiee, Alireza; Alghooneh, Ali

2018-01-01

In this study, the effects of water, ethanol, methanol and glycerin at five levels (0, 31.25, 83.33, 125 and 250 ml) were investigated on the efficiency of mangrove leaf extraction using mixture optimal design. The antimicrobial effect of the extracts on Streptococcus pneumoniae, Enterococcus faecium and Klebsiella pneumoniae was evaluated using disk diffusion, minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) methods. The mangrove leaf extraction components were identified through gas chromatography/mass spectrometry (GC/MS). Phytochemical analysis (alkaloids, tannins, saponins, flavone and glycosides) were evaluated based on qualitative methods. Antioxidant activity of extracts was measured using 2,2-diphenyl-1-picrylhydrazyl (DPPH), ferric reducing antioxidant potential (FRAP) methods. Maximum antimicrobial effect was observed in Enterococcus faecium and highest resistance against mangrove leaf extract in Enterococcus faecium and Klebsiella pneumoniae, respectively. Increasing concentration of mangrove extracts had a significant effect (p ≤ 0.05) on inhibition zone diameter. The MICs of the mangrove leaf extraction varied from 4 mg/ml to 16 mg/ml. The optimum formulation was found to contain glycerin (0 ml), water (28.22 ml), methanol (59.83 ml) and ethanol (161.95 ml). The results showed that the highest antioxidant activity was related to optimum extract of mangrove leaf and ethanolic extract respectively. The results of phytochemical screening of Avicennia marina leaves extract showed the existence of alkaloids, tannins, saponins, flavone and glycosides. 2-Propenoic acid, 3-phenyl- was the major compound of Avicennia marina. The results of non-significant lack of fit tests, and F value (14.62) indicated that the model was sufficiently accurate. In addition, the coefficient of variations (16.8%) showed an acceptable reproducibility. Copyright © 2017 Elsevier Ltd. All rights reserved.

Antimicrobial activity of Marcetia DC species (Melastomataceae) and analysis of its flavonoids by reverse phase-high performance liquid chromatography coupled-diode array detector.

PubMed

Leite, Tonny Cley Campos; de Sena, Amanda Reges; Dos Santos Silva, Tânia Regina; Dos Santos, Andrea Karla Almeida; Uetanabaro, Ana Paula Trovatti; Branco, Alexsandro

2012-07-01

Marcetia genera currently comprises 29 species, with approximately 90% inhabiting Bahia (Brazil), and most are endemic to the highlands of the Chapada Diamantina (Bahia). Among the species, only M. taxifolia (A.St.-Hil.) DC. populates Brazil (state of Roraima to Paraná) and also Venezuela, Colombia, and Guyana. This work evaluated the antimicrobial activity of hexane, ethyl acetate, and methanol extracts of three species of Marcetia (Marcetia canescens Naud., M. macrophylla Wurdack, and M. taxifolia A.StHil) against several microorganism. In addition, the flavonoids were analyzed in extracts by HPLC-DAD. The tests were made using Gram-positive (three strains of Staphylococcus aureus) and Gram-negative (two strains of Escherichia coli, a strain of Pseudomonas aeruginosa and another of Salmonella choleraesius) bacteria resistant and nonresistant to antibiotics and yeasts (two strains of Candida albicans and one of C. parapsilosis) by the disk diffusion method. Solid-phase extraction (SPE) was performed on the above extracts to isolate flavonoids, which were subsequently analyzed by high performance liquid chromatography coupled diode array detector (HPLC-DAD). Results showed that extracts inhibited the Gram-positive bacteria and yeast. The hexane extracts possessed the lowest activity, while the ethyl acetate and methanolic extracts were more active. Marcetia taxifolia was more effective (active against 10 microorganisms studied), and only its methanol extract inhibited Gram-negative bacteria (P. aeruginosa and S. choleraesius). SPE and HPLC-DAD analysis showed that M. canescens and M. macrophylla contain glycosylated flavonoids, while the majority of extracts from M. taxifolia were aglycone flavonoids.

Supercritical carbon dioxide extraction of compounds with antimicrobial activity from Origanum vulgare L.: determination of optimal extraction parameters.

PubMed

Santoyo, S; Cavero, S; Jaime, L; Ibañez, E; Señoráns, F J; Reglero, G

2006-02-01

Oregano leaves were extracted using a pilot-scale supercritical fluid extraction plant under a wide range of extraction conditions, with the goal of determining the extraction and fractionation conditions to obtain extracts with optimal antimicrobial activity. In this investigation, the essential oil-rich fractions were selectively precipitated in the second separator, and their chemical composition and antimicrobial activity were investigated. Gas chromatography-mass spectrometry analysis of the various fractions resulted in the identification of 27 compounds of the essential oil. The main components of these fractions were carvacrol, trans-sabinene hydrate, cis-piperitol, borneol, terpinen-4-ol, and linalool. Antimicrobial activity was investigated by the disk diffusion and broth dilution methods against six different microbial species, including two gram-positive bacteria (Staphylococcus aureus and Bacillus subtilis), two gram-negative bacteria (Escherichia coli and Pseudomonas aeruginosa), a yeast (Candida albicans), and a fungus (Aspergillus niger). All of the supercritical fluid extraction fractions obtained showed antimicrobial activity against all of the microorganisms tested, although the most active fraction was the one obtained in experiment 5 (fraction was obtained with 7% ethanol at 150 bar and 40 degrees C). C. albicans was the most sensitive microorganism to the oregano extracts, whereas the least susceptible was A. niger. Carvacrol, sabinene hydrate, borneol, and linalool standards also showed antimicrobial activity against all of the microorganisms tested, with carvacrol being the most effective. Consequently, it was confirmed that essential oil from experiment 5, with the best antimicrobial activity, also presented the highest quantity of carvacrol.

Carbon nanotube coatings as chemical absorbers

DOEpatents

Tillotson, Thomas M.; Andresen, Brian D.; Alcaraz, Armando

2004-06-15

Airborne or aqueous organic compound collection using carbon nanotubes. Exposure of carbon nanotube-coated disks to controlled atmospheres of chemical warefare (CW)-related compounds provide superior extraction and retention efficiencies compared to commercially available airborne organic compound collectors. For example, the carbon nanotube-coated collectors were four (4) times more efficient toward concentrating dimethylmethyl-phosphonate (DMMP), a CW surrogate, than Carboxen, the optimized carbonized polymer for CW-related vapor collections. In addition to DMMP, the carbon nanotube-coated material possesses high collection efficiencies for the CW-related compounds diisopropylaminoethanol (DIEA), and diisopropylmethylphosphonate (DIMP).

Turbine Design for Energy Extraction from Dust Devils

NASA Astrophysics Data System (ADS)

Malaya, Nicholas; Moser, Robert

2016-11-01

Columnar vortices ("Dust-Devils") arise naturally in the atmosphere, over a wide range of scales in many different locations across the Earth, as well as on Mars. A new energy harvesting approach makes use of this ubiquitous process by creating and anchoring the vortices artificially and extracting energy from them. However, any analysis of the power that can be extracted is complicated by the presence of considerable vertical and azimuthal flow in the vortex, and so the design considerations are different from those for a classical wind turbine. This talk presents a modeling approach to estimate the upper limit on the power that could be extracted from such a flow. This method is based on the actuator disk model common to turbine design, but with generalized drag polars permitting exploration of a broader design space. This model can be fully coupled to the flow, which ensures the results do not violate any Betz-like considerations that might similarly arise in an analysis of frozen flow fields. The results of this model demonstrate a limit on how much of the energy can be extracted before disrupting the flow so greatly that the vortex cannot be maintained. This work supported by the Department of Energy [ARPA-E] un- der Award Number [DE-FOA-0000670].

Diabetic retinopathy grading by digital curvelet transform.

PubMed

Hajeb Mohammad Alipour, Shirin; Rabbani, Hossein; Akhlaghi, Mohammad Reza

2012-01-01

One of the major complications of diabetes is diabetic retinopathy. As manual analysis and diagnosis of large amount of images are time consuming, automatic detection and grading of diabetic retinopathy are desired. In this paper, we use fundus fluorescein angiography and color fundus images simultaneously, extract 6 features employing curvelet transform, and feed them to support vector machine in order to determine diabetic retinopathy severity stages. These features are area of blood vessels, area, regularity of foveal avascular zone, and the number of micro-aneurisms therein, total number of micro-aneurisms, and area of exudates. In order to extract exudates and vessels, we respectively modify curvelet coefficients of color fundus images and angiograms. The end points of extracted vessels in predefined region of interest based on optic disk are connected together to segment foveal avascular zone region. To extract micro-aneurisms from angiogram, first extracted vessels are subtracted from original image, and after removing detected background by morphological operators and enhancing bright small pixels, micro-aneurisms are detected. 70 patients were involved in this study to classify diabetic retinopathy into 3 groups, that is, (1) no diabetic retinopathy, (2) mild/moderate nonproliferative diabetic retinopathy, (3) severe nonproliferative/proliferative diabetic retinopathy, and our simulations show that the proposed system has sensitivity and specificity of 100% for grading.

Efficacy of methanolic extract of green and black teas against extended-spectrum β-Lactamase-producing Pseudomonas aeruginosa.

PubMed

Taherpour, Arezou; Hashemi, Ali; Erfanimanesh, Soroor; Taki, Elahe

2016-07-01

Pseudomonas aeruginosa is one of the major bacteria causing acute infections. β-Lactamase production is the principal defense mechanism in gram-negative bacteria. The aim of our study was to evaluate the antibacterial activity of Methanolic Extracts of Green and Black Teas on P. aeruginosa Extended Spectrum-β-Lactamases (ESBLs) production. This research was carried out on burn wounds of 245 hospitalized patients in Kerman, Iran. P. aeruginosa ESBLs and MBL producing strains were detected by Combination Disk Diffusion Test (CDDT) and Epsilometer test (E-test) strips, respectively. Minimum inhibitory concentration (MIC) was measured for Ceftazidime, Meropenem, Imipenem, Aztreonam, Cefotaxime and methanollic extracts of Camellia Sinensis (Green Tea). From 245 patients in the burn ward, 120 cases were infected with P. aeruginosa. 41 isolates contained ESBL while MBL was not detected. P. aeruginosa were resistant to Cefotaxime, Aztreonam, Ceftazidime, Meropenem and Imipenem, 72 (60%), 50 (41.66%), 79 (65.83%), 33 (27.5%) and 24 (20%), respectively. Green tea extract had the highest anti-bacterial effect on standard and P. aeruginosa strains in 1.25mg/ml concentration. This study determined that the methanolic extract of green tea has a higher effect against ESBL producing P. aeruginosa than Cefotaxime, Aztreonam and Ceftazidime.

Evaluation of Preclinical Assays to Investigate an Anthroposophic Pharmaceutical Process Applied to Mistletoe (Viscum album L.) Extracts

PubMed Central

Flückiger, Heidi

2014-01-01

Extracts from European mistletoe (Viscum album L.) developed in anthroposophic medicine are based on specific pharmaceutical procedures to enhance remedy efficacy. One such anthroposophic pharmaceutical process was evaluated regarding effects on cancer cell toxicity in vitro and on colchicine tumor formation in Lepidium sativum. Anthroposophically processed Viscum album extract (APVAE) was produced by mixing winter and summer mistletoe extracts in the edge of a high-speed rotating disk and was compared with manually mixed Viscum album extract (VAE). The antiproliferative effect of VAE/APVAE was determined in five cell lines (NCI-H460, DU-145, HCC1143, MV3, and PA-TU-8902) by WST-1 assay in vitro; no difference was found between VAE and APVAE in any cell line tested (P > 0.14). Incidence of colchicine tumor formation was assessed by measurement of the root/shoot-ratio of seedlings of Lepidium sativum treated with colchicine as well as VAE, APVAE, or water. Colchicine tumor formation decreased after application of VAE (−5.4% compared to water, P < 0.001) and was even stronger by APVAE (−8.8% compared to water, P < 0.001). The high-speed mistletoe extract mixing process investigated thus did not influence toxicity against cancer cells but seemed to sustain morphostasis and to enhance resistance against external noxious influences leading to phenomenological malformations. PMID:24876872

Quantification of the association between intervertebral disk calcification and disk herniation in Dachshunds.

PubMed

Jensen, Vibeke F; Beck, Sarah; Christensen, Knud A; Arnbjerg, Jens

2008-10-01

To quantify the association between intervertebral disk calcification and disk herniation in Dachshunds. Longitudinal study. 61 Dachshunds that had been radiographically screened for calcification of intervertebral disks at 2 years of age in other studies. Thirty-seven of the dogs had survived to the time of the present study and were > or = 8 years of age; 24 others had not survived. Radiographic examination of 36 surviving dogs was performed, and information on occurrence of disk calcification at 2 years of age were obtained from records of all 61 Dachshunds. Information on occurrence of disk herniation between 2 and 8 years of age was obtained from owners via questionnaire. Associations between numbers of calcified disks and disk herniation were analyzed via maximum likelihood logistic regression. Disk calcification at 2 years of age was a significant predictor of clinical disk herniation (odds ratio per calcified disk, 1.42; 95% confidence interval, 1.19 to 1.81). Number of calcified disks in the full vertebral column was a better predictor than number of calcified disks between vertebrae T10 and L3. Numbers of calcified disks at > or = 8 years of age and at 2 years of age were significantly correlated. Number of calcified disks at 2 years of age was a good predictor of clinical disk herniation in Dachshunds. Because of the high heritability of disk calcification, it is possible that an effective reduction in occurrence of severe disk herniation in Dachshunds could be obtained by selective breeding against high numbers of calcified disks at 2 years of age.

Aerodynamic and torque characteristics of enclosed Co/counter rotating disks

NASA Astrophysics Data System (ADS)

Daniels, W. A.; Johnson, B. V.; Graber, D. J.

1989-06-01

Experiments were conducted to determine the aerodynamic and torque characteristics of adjacent rotating disks enclosed in a shroud, in order to obtain an extended data base for advanced turbine designs such as the counterrotating turbine. Torque measurements were obtained on both disks in the rotating frame of reference for corotating, counterrotating and one-rotating/one-static disk conditions. The disk models used in the experiments included disks with typical smooth turbine geometry, disks with bolts, disks with bolts and partial bolt covers, and flat disks. A windage diaphragm was installed at mid-cavity for some experiments. The experiments were conducted with various amounts of coolant throughflow injected into the disk cavity from the disk hub or from the disk OD with swirl. The experiments were conducted at disk tangential Reynolds number up to 1.6 x 10 to the 7th with air as the working fluid. The results of this investigation indicated that the static shroud contributes a significant amount to the total friction within the disk system; the torque on counterrotating disks is essentially independent of coolant flow total rate, flow direction, and tangential Reynolds number over the range of conditions tested; and a static windage diaphragm reduces disk friction in counterrotating disk systems.

Structural valve deterioration in a starr-edwards mitral caged-disk valve prosthesis.

PubMed

Aoyagi, Shigeaki; Tayama, Kei-Ichiro; Okazaki, Teiji; Shintani, Yusuke; Kono, Michitaka; Wada, Kumiko; Kosuga, Ken-Ichi; Mori, Ryusuke; Tanaka, Hiroyuki

2013-01-01

The durability of the Starr-Edwards (SE) mitral caged-disk valve, model 6520, is not clearly known, and structural valve deterioration in the SE disk valve is very rare. Replacement of the SE mitral disk valve was performed in 7 patients 23-40 years after implantation. Macroscopic examination of the removed disk valves showed no structural abnormalities in 3 patients, in whom the disk valves were removed at <26 years after implantation. Localized disk wear was found at the sites where the disk abutted the struts of the cage, in disk valves excised >36 years after implantation in 4 patients. Disk fracture, a longitudinal split in the disk along its circumference at the site of incorporation of the titanium ring, was detected in the valves removed 36 and 40 years after implantation, respectively, and many cracks were also observed on the outflow aspect of the disk removed 40 years after implantation. Disk fracture and localized disk wear were found in the SE mitral disk valves implanted >36 years previously. The present results suggest that SE mitral caged-disk valves implanted >20 years previously should be carefully followed up, and that those implanted >30 years previously should be electively replaced with modern prosthetic valves

Improved turbine disk design to increase reliability of aircraft jet engines

NASA Technical Reports Server (NTRS)

Alver, A. S.; Wong, J. K.

1975-01-01

An analytical study was conducted on a bore entry cooled turbine disk for the first stage of the JT8D-17 high pressure turbine which had the potential to improve disk life over existing design. The disk analysis included the consideration of transient and steady state temperature, blade loading, creep, low cycle fatigue, fracture mechanics and manufacturing flaws. The improvement in life of the bore entry cooled turbine disk was determined by comparing it with the existing disk made of both conventional and advanced (Astroloy) disk materials. The improvement in crack initiation life of the Astroloy bore entry cooled disk is 87% and 67% over the existing disk made of Waspaloy and Astroloy, respectively. Improvement in crack propagation life is 124% over the Waspaloy and 465% over the Astroloy disks. The available kinetic energies of disk fragments calculated for the three disks indicate a lower fragment energy level for the bore entry cooled turbine disk.

Determination of pharmaceutical residues in drinking water in Poland using a new SPE-GC-MS(SIM) method based on Speedisk extraction disks and DIMETRIS derivatization.

PubMed

Caban, Magda; Lis, Ewa; Kumirska, Jolanta; Stepnowski, Piotr

2015-12-15

The presence of pharmaceuticals in drinking water, even at very low concentrations, has raised concerns among stakeholders such as drinking-water regulators, governments, water suppliers and the public, with regard to the potential risks to humans. Despite this, the occurrence and the fate of pharmaceuticals in drinking waters of many countries (e.g. in Poland) remains unknown. There is a lack of sufficiently sensitive and reliable analytical methods for such analyses and a need for more in-depth hydrogeological analysis of the possible sources of drug residues in drinking water. In this paper, a multi-residual method for the simultaneous determination of seventeen human pharmaceuticals in drinking waters has been developed. Large-volume extractions using Speedisk extraction disks, and derivatization prior to GC-MS-SIM analysis using a new silylating agent DIMETRIS were applied. The method detection limits (MDLs) ranged from 0.9 to 5.7ng/L and the absolute recoveries of the target compounds were above 80% for most analytes. The developed method was successfully applied in the analysis of the target compounds in drinking water collected in Gdansk (Poland), and of the 17 pharmaceuticals, 6 compounds were detected at least once. During the investigation, the geomorphology of the site region was taken into account, possible sources of pharmaceuticals in the analysed drinking water samples were investigated, and the presence of the drugs in ground and surface waters, raw and treated drinking waters was determined. Concentrations were also compared with those observed in other countries. As a result, this study has not only developed a new analytical method for determining pharmaceuticals in drinking waters as well as rendering missing information for Poland (a country with one of the highest consumptions of pharmaceuticals in Europe), but it also presents a modelled in-depth hydrogeological analysis of the real sources of drugs in drinking waters. Copyright © 2015 Elsevier B.V. All rights reserved.