Sample records for plasma sample preparation

  1. LC-MS analysis of the plasma metabolome–a novel sample preparation strategy

    DEFF Research Database (Denmark)

    Skov, Kasper; Hadrup, Niels; Smedsgaard, Jørn


    of plasma samples: The first is protein precipitation; the second is protein precipitation followed by solid phase extraction with sub-fractionation into three sub-samples; a phospholipid, a lipid and a polar sub-fraction. Molecular feature extraction of the data files from LC-qTOF analysis of the samples......Blood plasma is a well-known body fluid often analyzed in studies on the effects of toxic compounds as physiological or chemical induced changes in the mammalian body are reflected in the plasma metabolome. Sample preparation prior to LC-MS based analysis of the plasma metabolome is a challenge...... as plasma contains compounds with very different properties. Besides, proteins, which usually are precipitated with organic solvent, phospholipids, are known to cause ion suppression in electrospray mass spectrometry. We have compared two different sample preparation techniques prior to LC-qTOF analysis...

  2. A simple sample preparation method for measuring amoxicillin in human plasma by hollow fiber centrifugal ultrafiltration. (United States)

    Dong, Wei-Chong; Hou, Zi-Li; Jiang, Xin-Hui; Jiang, Ye


    A simple sample preparation method has been developed for the determination of amoxicillin in human plasma by hollow fiber centrifugal ultrafiltration (HF-CF-UF). A 400-μL plasma sample was placed directly into the HF-CF-UF device, which consisited of a slim glass tube and a U-shaped hollow fiber. After centrifugation at 1.25 × 10(3) g for 10 min, the filtrate was withdrawn from the hollow fiber and 20 µL was directly injected into the high-performance liquid chromatography (HPLC) for analysis. The calibration curve was linear over the range of 0.1-20 µg/mL (r = 0.9996) and the limit of detection was as low as 0.025 µg/mL. The average recovery and absolute recovery were 99.9% and 84.5%, respectively. Both the intra-day and inter-day precisions (relative standard deviation) were less than 3.1% for three concentrations (0.25, 2.5 and 10 µg/mL). The sample preparation process was simplified. Only after a single centrifugal ultrafiltration can the filtrate be injected directly into HPLC. The present method is simple, sensitive and accurate. It could be effective for the analysis of biological samples with high protein contents, especially for the biopharmaceutical analysis of drugs that use traditional isolation techniques for sample preparation such as the protein precipitation method.

  3. pH adjustment of human blood plasma prior to bioanalytical sample preparation

    NARCIS (Netherlands)

    Hendriks, G.; Uges, D. R. A.; Franke, J. P.


    pH adjustment in bioanalytical sample preparation concerning ionisable compounds is one of the most common sample treatments. This is often done by mixing an aliquot of the sample with a proper buffer adjusted to the proposed pH. The pH of the resulting mixture however, does not necessarily have to

  4. Demonstration of a frozen sample aliquotter to prepare plasma and serum aliquots without thawing frozen parent samples. (United States)

    Ellis, Helena Judge; Venturini, Deborah S


    Human biospecimens represent invaluable resources to advance molecular medicine, epidemiology, and biomarker discovery/validation, among other biomedical research. Biobanks typically cryopreserve biospecimens to safeguard their biochemical composition. However, exposing specimens repeatedly to freeze/thaw cycles can degrade their integrity in unforeseen ways. Those biobanks storing liquid samples, thus, regularly make a fundamental compromise at collection time between freezing samples in many small volumes (e.g., 0.5 mL or smaller) or in fewer, larger volumes (e.g., 1.8 mL). The former eliminates the need to expose samples to repeated freeze/thaw cycling, although increasing up-front labor costs, consumables used, and cold storage space requirements. The latter decreases up-front labor costs, consumables, and cold storage requirements, yet exposes samples repeatedly to damaging freeze/thaw cycles when smaller aliquots are needed for analysis. The Rhode Island BioBank at Brown University (RIBB) thoroughly evaluated the performance of an original technology that minimizes a sample's exposure to freeze/thaw cycling by enabling the automated extraction of frozen aliquots from one single frozen parent sample without thawing it. A technology that eliminates unnecessary sample exposures to freeze/thaw cycles could help protect sample integrity, extend its useful life, and effectively rectify and eliminate the aforementioned need to compromise. This report presents the results of the evaluation, and conclusively demonstrates the technology's ability to extract multiple uniform frozen aliquots from a single cryotube of never-thawed frozen human plasma, which faithfully represent the parent sample when analyzed for typical biochemical analytes, showing a coefficient of variability lower than 5.5%.

  5. Determination of protein carbonyls in plasma, cell extracts, tissue homogenates, isolated proteins: Focus on sample preparation and derivatization conditions. (United States)

    Weber, Daniela; Davies, Michael J; Grune, Tilman


    Protein oxidation is involved in regulatory physiological events as well as in damage to tissues and is thought to play a key role in the pathophysiology of diseases and in the aging process. Protein-bound carbonyls represent a marker of global protein oxidation, as they are generated by multiple different reactive oxygen species in blood, tissues and cells. Sample preparation and stabilization are key steps in the accurate quantification of oxidation-related products and examination of physiological/pathological processes. This review therefore focuses on the sample preparation processes used in the most relevant methods to detect protein carbonyls after derivatization with 2,4-dinitrophenylhydrazine with an emphasis on measurement in plasma, cells, organ homogenates, isolated proteins and organelles. Sample preparation, derivatization conditions and protein handling are presented for the spectrophotometric and HPLC method as well as for immunoblotting and ELISA. An extensive overview covering these methods in previously published articles is given for researchers who plan to measure protein carbonyls in different samples.

  6. Plasma, blood and liver tissue sample preparation methods for the separate quantification of liposomal-encapsulated prednisolone phosphate and non-encapsulated prednisolone

    NARCIS (Netherlands)

    Smits, Evelien A W; Soetekouw, José A; Bakker, Peter F A; Baijens, Bart J H; Vromans, Herman


    Besides the development of sample preparation methods for the determination of separate liposomal-encapsulated prednisolone phosphate and non-encapsulated prednisolone concentrations in murine plasma and blood, this article also presents the first description of an accurate sample preparation method

  7. Automated Sample Preparation Platform for Mass Spectrometry-Based Plasma Proteomics and Biomarker Discovery

    Directory of Open Access Journals (Sweden)

    Vilém Guryča


    Full Text Available The identification of novel biomarkers from human plasma remains a critical need in order to develop and monitor drug therapies for nearly all disease areas. The discovery of novel plasma biomarkers is, however, significantly hampered by the complexity and dynamic range of proteins within plasma, as well as the inherent variability in composition from patient to patient. In addition, it is widely accepted that most soluble plasma biomarkers for diseases such as cancer will be represented by tissue leakage products, circulating in plasma at low levels. It is therefore necessary to find approaches with the prerequisite level of sensitivity in such a complex biological matrix. Strategies for fractionating the plasma proteome have been suggested, but improvements in sensitivity are often negated by the resultant process variability. Here we describe an approach using multidimensional chromatography and on-line protein derivatization, which allows for higher sensitivity, whilst minimizing the process variability. In order to evaluate this automated process fully, we demonstrate three levels of processing and compare sensitivity, throughput and reproducibility. We demonstrate that high sensitivity analysis of the human plasma proteome is possible down to the low ng/mL or even high pg/mL level with a high degree of technical reproducibility.

  8. Sample preparation and biopharmaceutical analysis


    Farrelly, Gillian


    In chapter 1, an overview is given of sample preparation methods and analytical techniques in use today. Each one is discussed, and relevant examples are given. In chapter 2, the development of a method for the HPLC analysis of taurine in human plasma using acetonitrile precipitation and pre-column derivatisation with fluorescamine is presented. This procedure was found to be faster and easier to use than previous taurine assays. In chapter 3, the evaluation of novel aspirin derivativ...

  9. An efficient sample preparation method for high-throughput analysis of 15(S)-8-iso-PGF2α in plasma and urine by enzyme immunoassay. (United States)

    Bielecki, A; Saravanabhavan, G; Blais, E; Vincent, R; Kumarathasan, P


    Although several methods have been reported on the analysis of the oxidative stress marker 15(S)-8-iso-prostaglandin-F2alpha (8-iso-PGF2α) in biological fluids, they either involve extensive sample preparation and costly technology or require high sample volume. This study presents a sample preparation method that utilizes low sample volume for 8-iso-PGF2α analysis in plasma and urine by an enzyme immunoassay (EIA). In brief, 8-iso-PGF2α in deproteinized plasma or native urine sample is complexed with an antibody and then captured by molecular weight cut-off filtration. This method was compared with two other sample preparation methods that are typically used in the analysis of 8-iso-PGF2α by EIA: Cayman's affinity column purification method and solid-phase extraction on C-18. The immunoaffinity purification method described here was superior to the other two sample preparation methods and yielded recovery values of 99.8 and 54.1% for 8-iso-PGF2α in plasma and urine, respectively. Analytical precision (relative standard deviation) was ±5% for plasma and ±15% for urine. The analysis of healthy human plasma and urine resulted in basal 8-iso-PGF2α levels of 31.8 ± 5.5 pg/mL and 2.9 ± 2.0 ng/mg creatinine, respectively. The robustness and analytical performance of this method makes it a promising tool for high-throughput screening of biological samples for 8-iso-PGF2α.

  10. Increased levels of HIV RNA detected in samples with viral loads close to the detection limit collected in Plasma Preparation Tubes (PPT). (United States)

    Griffith, Brigitte P; Mayo, Donald R


    The accurate and reliable quantification of HIV RNA is an essential part of the management of HIV infected individuals, and elucidation of factors that may affect HIV RNA measurements, such as the use of Vacutainer Plasma Preparation Tubes (PPT), is crucial. The objective of this study was to determine if plasma samples with viral loads close to the lower limit of the dynamic range of the assay collected in PPT tubes had increased levels of HIV RNA as compared to samples collected in standard EDTA tubes. HIV RNA levels were compared in 112 paired plasma samples collected in PPT and standard EDTA tubes. All samples had been frozen prior to testing. Discrepancies between PPT and EDTA tubes did not occur for samples with high viral loads. However, in samples with viral loads close to the lower limit of the dynamic range, levels of HIV RNA detected were higher in a large proportion of PPT as compared to the corresponding EDTA plasma samples. Forty percent of plasma pairs had no detectable HIV RNA in the EDTA aliquot, but had low levels of HIV RNA in the corresponding PPT aliquot. This prospective study underlines the need for cautious interpretation of small transient viral load changes in samples with values close to the detection limit.

  11. Development of a high throughput 96-well plate sample preparation method for the determination of trileptal (oxcarbazepine) and its metabolites in human plasma. (United States)

    Souppart, C; Decherf, M; Humbert, H; Maurer, G


    A high throughput preparation method for the determination of trileptal (oxcarbazepine, OXC) and its mono (MHD) and dihydroxy (DHD) metabolites in human plasma, using 96-well plate technology, has been developed and validated according to international regulatory requirements. Preparation of plasma samples (50 microl) containing the compounds to be analysed involved solid-phase extraction (SPE) on Empore C18 96-well SPE plates. Eluates from the plate were injected onto a reversed-phase column (Hypersil C18,3 microm) with UV detection at 210 nm. Detector response was linear over the ranges 0.2-10, 0.1-200 and 0.1-20 micromol/l, for OXC, MHD and DHD, respectively, with relative standard deviations from 1 to 10% and mean accuracies within 4% of the nominal values (number of standard curves=3 in duplicate). The limits of quantitation were 0.2, 0.1 and 0.1 micromol/l, respectively. The overall mean accuracies ranged from 96 to 106% and precision was in the range 4 to 11%. Cross validation indicated no significant difference between plasma concentrations obtained using the 96-well method and the previous method using a traditional SPE method with a 50 mg C18 cartridge. About a threefold increase in sample throughput and a twofold decrease of plasma volume required for the assays, were the main advantages obtained from the previous method. The method was applied for the determination of 3000 plasma samples from clinical studies.

  12. Comparison of sample preparation methods for the quantitative analysis of eicosanoids and other oxylipins in plasma by means of LC-MS/MS. (United States)

    Ostermann, Annika I; Willenberg, Ina; Schebb, Nils Helge


    Oxylipins are potent lipid mediators. For the evaluation of their biological roles, several LC-MS based methods have been developed. While these methods are similar, the described sample preparation procedures for the extraction of oxylipins differ considerably. In order to deduce the most appropriate method for the analysis of non-esterified oxylipins in human plasma, we evaluated the performance of seven established sample preparation procedures. Six commonly used solid phase extraction (SPE) and one liquid-liquid extraction (LLE) protocol were compared based on the recovery of 13 added internal standards, extraction efficacy of oxylipins from plasma and reduction of ion-suppressing matrix. Dramatic differences in the performance in all three parameters were found. LLE with ethyl acetate was overall not a sufficient sample preparation strategy. The protocols using Oasis- and StrataX-material insufficiently removed interfering matrix compounds. Extraction efficacy of oxylipins on anion-exchanging BondElut cartridges was low, while removal of matrix was nearly perfect. None of the protocols led to a high extraction efficacy of analytes while removing all interfering matrix components. However, SPE on a C18-material with removal of matrix by water and n-hexane prior elution with methyl formate showed the best performance for the analysis of a broad spectrum of oxylipins in plasma.

  13. Multicomponent kinetic spectrophotometric determination of pefloxacin and norfloxacin in pharmaceutical preparations and human plasma samples with the aid of chemometrics (United States)

    Ni, Yongnian; Wang, Yong; Kokot, Serge


    A spectrophotometric method for the simultaneous determination of the important pharmaceuticals, pefloxacin and its structurally similar metabolite, norfloxacin, is described for the first time. The analysis is based on the monitoring of a kinetic spectrophotometric reaction of the two analytes with potassium permanganate as the oxidant. The measurement of the reaction process followed the absorbance decrease of potassium permanganate at 526 nm, and the accompanying increase of the product, potassium manganate, at 608 nm. It was essential to use multivariate calibrations to overcome severe spectral overlaps and similarities in reaction kinetics. Calibration curves for the individual analytes showed linear relationships over the concentration ranges of 1.0-11.5 mg L -1 at 526 and 608 nm for pefloxacin, and 0.15-1.8 mg L -1 at 526 and 608 nm for norfloxacin. Various multivariate calibration models were applied, at the two analytical wavelengths, for the simultaneous prediction of the two analytes including classical least squares (CLS), principal component regression (PCR), partial least squares (PLS), radial basis function-artificial neural network (RBF-ANN) and principal component-radial basis function-artificial neural network (PC-RBF-ANN). PLS and PC-RBF-ANN calibrations with the data collected at 526 nm, were the preferred methods—%RPE T ˜ 5, and LODs for pefloxacin and norfloxacin of 0.36 and 0.06 mg L -1, respectively. Then, the proposed method was applied successfully for the simultaneous determination of pefloxacin and norfloxacin present in pharmaceutical and human plasma samples. The results compared well with those from the alternative analysis by HPLC.

  14. Solid Matrix Transformation and Tracer Addition using Molten Ammonium Bifluoride Salt as a Sample Preparation Method for Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grate, Jay W.; Gonzalez, Jhanis J.; O' Hara, Matthew J.; Kellogg, Cynthia M.; Morrison, Samuel S.; Koppenaal, David W.; Chan, George C.; Mao, Xianglei; Zorba, Vassilia; Russo, Richard


    Laser ablation (LA) is a means of sample introduction to inductively coupled plasma (ICP) mass spectrometry (MS) that avoids acid dissolution and chemical separation steps conventionally associated with solid sample analysis. At the same time, certain features of LA-ICP-MS are often mentioned in critical reviews including solid matrix variability and its influence on the ablation process, matrix dependent elemental fractionation, lack of matrix matched standards for external calibration, and limitations to internal calibration because it is challenging to add and distribute spikes into solid samples. In this paper we introduce the concept of a synergistic minimal sample preparation method that is used in combination with LA-ICP-MS as a means to overcome these limitations. The aim of this minimal sample preparation procedure is to reactively transform the original matrix to a more consistent matrix for LA-based analysis, thus reducing the effects of matrix variability, while enabling the addition of tracers. In conjunction with ICP-MS, we call this MTR-LA-ICP-MS, where MTR is derived from matrix transformation including the option to add tracers

  15. Ferromagnetic particles as a rapid and robust sample preparation for the absolute quantification of seven eicosanoids in human plasma by UHPLC-MS/MS. (United States)

    Suhr, Anna Catharina; Bruegel, Mathias; Maier, Barbara; Holdt, Lesca Miriam; Kleinhempel, Alisa; Teupser, Daniel; Grimm, Stefanie H; Vogeser, Michael


    We used ferromagnetic particles as a novel technique to deproteinize plasma samples prior to quantitative UHPLC-MS/MS analysis of seven eicosanoids [thromboxane B2 (TXB2), prostaglandin E2 (PGE2), PGD2, 5-hydroxyeicosatetraenoic acid (5-HETE), 11-HETE, 12-HETE, arachidonic acid (AA)]. A combination of ferromagnetic particle enhanced deproteination and subsequent on-line solid phase extraction (on-line SPE) realized quick and convenient semi-automated sample preparation-in contrast to widely used manual SPE techniques which are rather laborious and therefore impede the investigation of AA metabolism in larger patient cohorts. Method evaluation was performed according to a protocol based on the EMA guideline for bioanalytical method validation, modified for endogenous compounds. Calibrators were prepared in ethanol. The calibration curves were found to be linear in a range of 0.1-80ngmL(-1) (TXB2, PGE2, PGD2), 0.05-40ngmL(-1) (5-HETE, 11-HETE), 0.5-400ngmL(-1) (12-HETE) and 25-9800ngmL(-1) (AA). Regarding all analytes and all quality controls, the resulting precision data (inter-assay 2.6 %-15.5 %; intra-assay 2.5 %-15.1 %, expressed as variation coefficient) as well as the accuracy results (inter-assay 93.3 %-125 %; intra-assay 91.7 %-114 %) were adequate. Further experiments addressing matrix effect, recovery and robustness, yielded also very satisfying results. As a proof of principle, the newly developed LC-MS/MS assay was employed to determine the capacity of AA metabolite release after whole blood stimulation in healthy blood donors. For this purpose, whole blood specimens of 5 healthy blood donors were analyzed at baseline and after a lipopolysaccharide (LPS) induced blood cell activation. In several baseline samples some eicosanoids levels were below the Lower Limit of Quantification. However, in the stimulated samples all chosen eicosanoids (except PGD2) could be quantified. These results, in context with those obtained in validation, demonstrate the

  16. Analytical sample preparation strategies for the determination of antimalarial drugs in human whole blood, plasma and urine

    DEFF Research Database (Denmark)

    Casas, Monica Escolà; Hansen, Martin; Krogh, Kristine A;


    Antimalarial drugs commonly referred to as antimalarials, include a variety of compounds with different physicochemical properties. There is a lack of information on antimalarial distribution in the body over time after administration, e.g. the drug concentrations in whole blood, plasma, and urin...... summarized. Finally, the main problems that the researchers have dealt with are highlighted. This information will aid analytical chemists in the development of novel methods for determining existing antimalarials and upcoming new drugs.......Antimalarial drugs commonly referred to as antimalarials, include a variety of compounds with different physicochemical properties. There is a lack of information on antimalarial distribution in the body over time after administration, e.g. the drug concentrations in whole blood, plasma, and urine...

  17. Monitoring of cefepime in human serum and plasma by micellar electrokinetic capillary chromatography: Improvement of sample preparation and validation by liquid chromatography coupled to mass spectrometry. (United States)

    Šestáková, Nela; Theurillat, Regula; Sendi, Parham; Thormann, Wolfgang


    Cefepime monitoring in deproteinized human serum and plasma by micellar electrokinetic capillary chromatography and liquid chromatography coupled to mass spectrometry in presence of other drugs is reported. For micellar electrokinetic capillary chromatography, sample preparation comprised dodecylsulfate protein precipitation at pH 4.5 using an increased buffer concentration compared to that of a previous assay and removal of hydrophobic compounds with dichloromethane. This provided robust conditions for cefepime analysis in the presence of sulfamethoxazole and thus enabled its determination in samples of patients that receive co-trimoxazole. The liquid chromatography assay is based upon use of a column with a pentafluorophenyl-propyl modified and multi-endcapped stationary phase and the coupling to electrospray ionization with a single quadrupole detector. The performances of both assays with multi-level internal calibration were assessed with calibration and control samples and both assays were determined to be robust. Cefepime levels monitored by micellar electrokinetic capillary chromatography in samples from patients that were treated with cefepime only and with cefepime and co-trimoxazole were found to compare well with those obtained by liquid chromatography coupled to mass spectrometry. Cefepime drug levels determined by micellar electrokinetic capillary chromatography could thereby be validated. This article is protected by copyright. All rights reserved.

  18. Microfluidic Sample Preparation for Immunoassays

    Energy Technology Data Exchange (ETDEWEB)

    Visuri, S; Benett, W; Bettencourt, K; Chang, J; Fisher, K; Hamilton, J; Krulevitch, P; Park, C; Stockton, C; Tarte, L; Wang, A; Wilson, T


    Researchers at Lawrence Livermore National Laboratory are developing means to collect and identify fluid-based biological pathogens in the forms of proteins, viruses, and bacteria. to support detection instruments, they are developing a flexible fluidic sample preparation unit. The overall goal of this Microfluidic Module is to input a fluid sample, containing background particulates and potentially target compounds, and deliver a processed sample for detection. They are developing techniques for sample purification, mixing, and filtration that would be useful to many applications including immunologic and nucleic acid assays. Many of these fluidic functions are accomplished with acoustic radiation pressure or dielectrophoresis. They are integrating these technologies into packaged systems with pumps and valves to control fluid flow through the fluidic circuit.

  19. Sample Preparation for Bioanalytical and Pharmaceutical Analysis. (United States)

    Clark, Kevin D; Zhang, Cheng; Anderson, Jared L


    Biological and pharmaceutical samples represent formidable challenges in sample preparation that hold important consequences for bioanalysis and genotoxic impurity quantification. This Feature will emphasize significant advances toward the development of rapid, sensitive, and selective sample preparation methods.

  20. Biofouling development on plasma treated samples versus layers coated samples (United States)

    Hnatiuc, B.; Exnar, P.; Sabau, A.; Spatenka, P.; Dumitrache, C. L.; Hnatiuc, M.; Ghita, S.


    Biofouling is the most important cause of naval corrosion. In order to reduce the Biofouling development on naval materials as steel or resin, different new methods have been tested. These methods could help to follow the new IMO environment reglementations and they could replace few classic operations before the painting of the small ships. The replacement of these operations means a reduction in maintenance costs. Their action must influence especially the first two steps of the Biofouling development, called Microfouling, that demand about 24 hours. This work presents the comparative results of the Biofouling development on two different classic naval materials, steel and resin, for three treated samples, immersed in sea water. Non-thermal plasma, produced by GlidArc technology, is applied to the first sample, called GD. The plasma treatment was set to 10 minutes. The last two samples, called AE9 and AE10 are covered by hydrophobic layers, prepared from a special organic-inorganic sol synthesized by sol-gel method. Theoretically, because of the hydrophobic properties, the Biofouling formation must be delayed for AE9 and AE10. The Biofouling development on each treated sample was compared with a witness non-treated sample. The microbiological analyses have been done for 24 hours by epifluorescence microscopy, available for one single layer.


    Directory of Open Access Journals (Sweden)

    AVRAM Florin Timotei


    Full Text Available In this paper we propose to present the issues involved in the case of the constructive conception of a station for metallographic sample preparation. This station is destined for laboratory work. The metallographic station is composed of a robot ABB IRB1600, a metallographic microscope, a gripping device, a manipulator, a laboratory grinding and polishing machine. The robot will be used for manipulation of the sample preparation and the manipulator take the sample preparation for processing.

  2. Final Report BW Sample Collection& Preparation Device

    Energy Technology Data Exchange (ETDEWEB)

    Koopman, R P; Belgrader, P; Meyer, G; Benett, W J; Richards, J B; Hadley, D R; Stratton, P L; Milanovich, F P


    The objective of this project was to develop the technique needed to prepare a field collected sample for laboratory analysis and build a portable integrated biological detection instrument with new miniaturized and automated sample purification capabilities. The device will prepare bacterial spores, bacterial vegetative cells, and viral particles for PCR amplification.

  3. Modular microfluidic system for biological sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Rose, Klint A.; Mariella, Jr., Raymond P.; Bailey, Christopher G.; Ness, Kevin Dean


    A reconfigurable modular microfluidic system for preparation of a biological sample including a series of reconfigurable modules for automated sample preparation adapted to selectively include a) a microfluidic acoustic focusing filter module, b) a dielectrophoresis bacteria filter module, c) a dielectrophoresis virus filter module, d) an isotachophoresis nucleic acid filter module, e) a lyses module, and f) an isotachophoresis-based nucleic acid filter.

  4. Automated sample preparation for CE-SDS. (United States)

    Le, M Eleanor; Vizel, Alona; Hutterer, Katariina M


    Traditionally, CE with SDS (CE-SDS) places many restrictions on sample composition. Requirements include low salt content, known initial sample concentration, and a narrow window of final sample concentration. As these restrictions require buffer exchange for many sample types, sample preparation is often tedious and yields poor sample recoveries. To improve capacity and streamline sample preparation, an automated robotic platform was developed using the PhyNexus Micro-Extractor Automated Instrument (MEA) for both the reduced and nonreduced CE-SDS assays. This automated sample preparation normalizes sample concentration, removes salts and other contaminants, and adds the required CE-SDS reagents, essentially eliminating manual steps during sample preparation. Fc-fusion proteins and monoclonal antibodies were used in this work to demonstrate benefits of this approach when compared to the manual method. With optimized conditions, this application has demonstrated decreased analyst "hands on" time and reduced total assay time. Sample recovery greater than 90% can be achieved, regardless of initial composition and concentration of analyte.

  5. Sample preparation in biological mass spectrometry

    CERN Document Server

    Ivanov, Alexander R


    The aim of this book is to provide the researcher with important sample preparation strategies in a wide variety of analyte molecules, specimens, methods, and biological applications requiring mass spectrometric analysis as a detection end-point.

  6. Combined supercritical fluid extraction/solid-phase extraction with octadecylsilane cartridges as a sample preparation technique for the ultratrace analysis of a drug metabolite in plasma. (United States)

    Liu, H; Cooper, L M; Raynie, D E; Pinkston, J D; Wehmeyer, K R


    Supercritical fluid extraction was coupled with solid-phase extraction using octadecylsilane cartridges for the selective isolation of ultratrace levels of a drug metabolite, mebeverine alcohol, from plasma. Plasma was directly applied to the extraction cartridge, the cartridge was washed to remove protein and then extracted under supercritical conditions using CO2/5% methanol. The effluent from the extraction cell was bubbled through a small volume of 2-propanol to trap the extracted mebeverine alcohol. The effects of extraction pressure and temperature on analyte recovery were examined. The absolute recovery, selectivity, precision, and accuracy of the combined supercritical fluid extraction/solid-phase extraction approach were compared to those of conventional solid-phase extraction using gas chromatography/mass spectrometry in the selected-ion monitoring mode. Mebeverine alcohol was used as a model compound, and dog plasma was employed as the biological matrix for these studies.

  7. Molecularly imprinted polymers for bioanalytical sample preparation. (United States)

    Gama, Mariana Roberto; Bottoli, Carla Beatriz Grespan


    Molecularly imprinted polymers (MIP) are stable polymers with molecular recognition abilities, provided by the presence of a template during their synthesis, and are excellent materials with high selectivity for sample preparation in bioanalytical methods. This short review discusses aspects of MIP preparation and its applications as a sorbent material in pharmaceutical and biomedical analysis. MIP in different extraction configurations, including classical solid-phase extraction, solid-phase microextraction, magnetic molecularly imprinted solid-phase extraction, microextraction by packed sorbent and solid-phase extraction in pipette tips, are used to illustrate the good performance of this type of sorbent for sample preparation procedures of complex matrices, especially prior to bioanalytical approaches.

  8. Surface studies of plasma processed Nb samples

    Energy Technology Data Exchange (ETDEWEB)

    Tyagi, Puneet V. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Doleans, Marc [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Hannah, Brian S. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Afanador, Ralph [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Stewart, Stephen [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Mammosser, John [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Howell, Matthew P [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Saunders, Jeffrey W [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Degraff, Brian D [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS); Kim, Sang-Ho [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source (SNS)


    Contaminants present at top surface of superconducting radio frequency (SRF) cavities can act as field emitters and restrict the cavity accelerating gradient. A room temperature in-situ plasma processing technology for SRF cavities aiming to clean hydrocarbons from inner surface of cavities has been recently developed at the Spallation Neutron Source (SNS). Surface studies of the plasma-processed Nb samples by Secondary ion mass spectrometry (SIMS) and Scanning Kelvin Probe (SKP) showed that the NeO2 plasma processing is very effective to remove carbonaceous contaminants from top surface and improves the surface work function by 0.5 to 1.0 eV.

  9. Sample preparation for SEM of plant surfaces


    A.K. Pathan; Bond, J.; R.E. Gaskin


    Plant tissues must be dehydrated for observation in most electron microscopes. Although a number of sample processing techniques have been developed for preserving plant tissues in their original form and structure, none of them are guaranteed artefact-free. The current paper reviews common scanning electron microscopy techniques and the sample preparation methods employed for visualisation of leaves under specific types of electron microscopes. Common artefacts introduced by specific techniq...

  10. Sample preparation method for scanning force microscopy

    CERN Document Server

    Jankov, I R; Szente, R N; Carreno, M N P; Swart, J W; Landers, R


    We present a method of sample preparation for studies of ion implantation on metal surfaces. The method, employing a mechanical mask, is specially adapted for samples analysed by Scanning Force Microscopy. It was successfully tested on polycrystalline copper substrates implanted with phosphorus ions at an acceleration voltage of 39 keV. The changes of the electrical properties of the surface were measured by Kelvin Probe Force Microscopy and the surface composition was analysed by Auger Electron Spectroscopy.

  11. Sample Preparation Report of the Fourth OPCW Confidence Building Exercise on Biomedical Sample Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Udey, R. N. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Corzett, T. H. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Alcaraz, A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)


    Following the successful completion of the 3rd biomedical confidence building exercise (February 2013 – March 2013), which included the analysis of plasma and urine samples spiked at low ppb levels as part of the exercise scenario, another confidence building exercise was targeted to be conducted in 2014. In this 4th exercise, it was desired to focus specifically on the analysis of plasma samples. The scenario was designed as an investigation of an alleged use of chemical weapons where plasma samples were collected, as plasma has been reported to contain CWA adducts which remain present in the human body for several weeks (Solano et al. 2008). In the 3rd exercise most participants used the fluoride regeneration method to analyze for the presence of nerve agents in plasma samples. For the 4th biomedical exercise it was decided to evaluate the analysis of human plasma samples for the presence/absence of the VX adducts and aged adducts to blood proteins (e.g., VX-butyrylcholinesterase (BuChE) and aged BuChE adducts using a pepsin digest technique to yield nonapeptides; or equivalent). As the aging of VX-BuChE adducts is relatively slow (t1/2 = 77 hr at 37 °C [Aurbek et al. 2009]), soman (GD), which ages much more quickly (t1/2 = 9 min at 37 °C [Masson et al. 2010]), was used to simulate an aged VX sample. Additional objectives of this exercise included having laboratories assess novel OP-adducted plasma sample preparation techniques and analytical instrumentation methodologies, as well as refining/designating the reporting formats for these new techniques.

  12. Scanning Electron Microscopy Sample Preparation and Imaging. (United States)

    Nguyen, Jenny Ngoc Tran; Harbison, Amanda M


    Scanning electron microscopes allow us to reach magnifications of 20-130,000× and resolve compositional and topographical images with intense detail. These images are created by bombarding a sample with electrons in a focused manner to generate a black and white image from the electrons that bounce off of the sample. The electrons are detected using positively charged detectors. Scanning electron microscopy permits three-dimensional imaging of desiccated specimens or wet cells and tissues by using variable pressure chambers. SEM ultrastructural analysis and intracellular imaging supplement light microscopy for molecular profiling of prokaryotes, plants, and mammals. This chapter demonstrates how to prepare and image samples that are (a) desiccated and conductive, (b) desiccated and nonconductive but coated with an electron conductive film using a gold sputter coater, and (c) wet and maintained in a hydrated state using a Deben Coolstage.

  13. HASE - The Helsinki adaptive sample preparation line

    Energy Technology Data Exchange (ETDEWEB)

    Palonen, V., E-mail: [Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 (Finland); Pesonen, A. [Laboratory of Chronology, Finnish Museum of Natural History, P.O. Box 64, FI-00014 (Finland); Herranen, T.; Tikkanen, P. [Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 (Finland); Oinonen, M. [Laboratory of Chronology, Finnish Museum of Natural History, P.O. Box 64, FI-00014 (Finland)


    We have designed and built an adaptive sample preparation line with separate modules for combustion, molecular sieve handling, CO{sub 2} gas cleaning, CO{sub 2} storage, and graphitization. The line is also connected to an elemental analyzer. Operation of the vacuum equipment, a flow controller, pressure sensors, ovens, and graphitization reactors are automated with a reliable NI-cRIO real-time system. Stepped combustion can be performed in two ovens at temperatures up to 900 Degree-Sign C. Depending on the application, CuO or O{sub 2}-flow combustion can be used. A flow controller is used to adjust the O{sub 2} flow and pressure during combustion. For environmental samples, a module for molecular sieve regeneration and sample desorption is attached to the line replacing the combustion module. In the storage module, CO{sub 2} samples can be stored behind a gas-tight diaphragm valve and either stored for later graphitization or taken for measurements with separate equipment (AMS gas ion source or a separate mass spectrometer). The graphitization module consists of four automated reactors, capable of graphitizing samples with masses from 3 mg down to 50 {mu}g.

  14. Sample preparation for SEM of plant surfaces

    Directory of Open Access Journals (Sweden)

    A.K. Pathan


    Full Text Available Plant tissues must be dehydrated for observation in most electron microscopes. Although a number of sample processing techniques have been developed for preserving plant tissues in their original form and structure, none of them are guaranteed artefact-free. The current paper reviews common scanning electron microscopy techniques and the sample preparation methods employed for visualisation of leaves under specific types of electron microscopes. Common artefacts introduced by specific techniques on different leaf types are discussed. Comparative examples are depicted from our lab using similar techniques; the pros and cons for specific techniques are discussed. New promising techniques and microscopes, which can alleviate some of the problems encountered in conventional methods of leaf sample processing and visualisation, are also discussed. It is concluded that the choice of technique for a specific leaf sample is dictated by the surface features that need to be preserved (such as trichomes, epidermal cells or wax microstructure, the resolution to be achieved, availability of the appropriate processing equipment and the technical capabilities of the available electron microscope.

  15. Corrosion behavior of magnetic ferrite coating prepared by plasma spraying

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Yi; Wei, Shicheng, E-mail:; Tong, Hui; Tian, Haoliang; Liu, Ming; Xu, Binshi


    Graphical abstract: The saturation magnetization (M{sub s}) of the ferrite coating is 34.417 emu/g while the M{sub s} value of the ferrite powder is 71.916 emu/g. It can be seen that plasma spray process causes deterioration of the room temperature soft magnetic properties. - Highlights: • Spinel ferrite coatings have been prepared by plasma spraying. • The coating consists of nanocrystalline grains. • The saturation magnetization of the ferrite coating is 34.417 emu/g. • Corrosion behavior of the ferrite coating was examined in NaCl solution. - Abstract: In this study, spray dried spinel ferrite powders were deposited on the surface of mild steel substrate through plasma spraying. The structure and morphological studies on the ferrite coatings were carried out using X-ray diffraction, scanning electron microscope and Raman spectroscopy. It was showed that spray dried process was an effective method to prepare thermal spraying powders. The coating showed spinel structure with a second phase of LaFeO{sub 3}. The magnetic property of the ferrite samples were measured by vibrating sample magnetometer. The saturation magnetization (M{sub s}) of the ferrite coating was 34.417 emu/g. The corrosion behavior of coating samples was examined by electrochemical impedance spectroscopy. EIS diagrams showed three corrosion processes as the coating immersed in 3.5 wt.% NaCl solution. The results suggested that plasma spraying was a promising technology for the production of magnetic ferrite coatings.

  16. Recent advances in sample preparation techniques for effective bioanalytical methods. (United States)

    Kole, Prashant Laxman; Venkatesh, Gantala; Kotecha, Jignesh; Sheshala, Ravi


    This paper reviews the recent developments in bioanalysis sample preparation techniques and gives an update on basic principles, theory, applications and possibilities for automation, and a comparative discussion on the advantages and limitation of each technique. Conventional liquid-liquid extraction (LLE), protein precipitation (PP) and solid-phase extraction (SPE) techniques are now been considered as methods of the past. The last decade has witnessed a rapid development of novel sample preparation techniques in bioanalysis. Developments in SPE techniques such as selective sorbents and in the overall approach to SPE, such as hybrid SPE and molecularly imprinted polymer SPE, have been addressed. Considerable literature has been published in the area of solid-phase micro-extraction and its different versions, e.g. stir bar sorptive extraction, and their application in the development of selective and sensitive bioanalytical methods. Techniques such as dispersive solid-phase extraction, disposable pipette extraction and micro-extraction by packed sorbent offer a variety of extraction phases and provide unique advantages to bioanalytical methods. On-line SPE utilizing column-switching techniques is rapidly gaining acceptance in bioanalytical applications. PP sample preparation techniques such as PP filter plates/tubes offer many advantages like removal of phospholipids and proteins in plasma/serum. Newer approaches to conventional LLE techniques (salting-out LLE) are also covered in this review article.

  17. FISHprep: A Novel Integrated Device for Metaphase FISH Sample Preparation

    DEFF Research Database (Denmark)

    Shah, Pranjul Jaykumar; Vedarethinam, Indumathi; Kwasny, Dorota;


    We present a novel integrated device for preparing metaphase chromosomes spread slides (FISHprep). The quality of cytogenetic analysis from patient samples greatly relies on the efficiency of sample pre-treatment and/or slide preparation. In cytogenetic slide preparation, cell cultures are routin...... with minimal handling for metaphase FISH slide preparation....

  18. Congener Production in Blood Samples During Preparation and Storage

    DEFF Research Database (Denmark)

    Felby, Søren; Nielsen, Erik


    Retsmedicin, congener production, preparation, head space GC, acetone, isobutanol, storage, blood samples, n-propanol, methanol, methylethylketone......Retsmedicin, congener production, preparation, head space GC, acetone, isobutanol, storage, blood samples, n-propanol, methanol, methylethylketone...

  19. Plasma preparation and storage for African elephants (Loxodonta africana). (United States)

    Knauf, Sascha; Blad-Stahl, Julia; Lawrenz, Arne; Schuerer, Ulrich; Wehrend, Axel


    The use of plasma as a life-saving tool for neonatal African elephants (Loxodonta africana) that failed passive transfer of immunoglobulins is proposed. The methodology of blood sampling, plasma extraction, and plasma storage is described. Values for cellular component sedimentation and biochemical parameters of extracted plasma that was collected from 2 female elephants is presented. The proposal for a central plasma bank for elephants in European zoos is suggested.

  20. Method of 14C Sample Preparation for AMS Measurement

    Directory of Open Access Journals (Sweden)

    YANG Xu-ran


    Full Text Available In order to carry out the application research of 14C by accelerator mass spectrometry (AMS, the principle of sample preparation were systematically studied and more attention was paid to improve the preparation process efficiently. The set of integrated system of sample preparation was built up on the research. The experimental results showed that the sample preparation scheme was able to meet the demand of AMS measurement.

  1. Preparation of spherical hollow alumina particles by thermal plasma

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Wonkyung [Department of Chemical Engineering, INHA University, 253 Yonghyun-dong, Nam-gu, Incheon 402‐751 (Korea, Republic of); Regional Innovation Center for Environmental Technology of Thermal Plasma (RIC-ETTP), INHA University, 253 Yonghyun-dong, Nam-gu, Incheon 402‐751 (Korea, Republic of); Choi, Sooseok [Center for Advance Research in Fusion Reactor Engineering, Seoul National University, 599 Gwanak-ro, Gwanak-gu, Seoul 151‐742 (Korea, Republic of); Oh, Seung-Min [Daejoo Electronic Materials Co., 1236‐10 Jeongwang-dong, Siheung-si, Kyunggi-do 429‐848 (Korea, Republic of); Park, Dong-Wha, E-mail: [Department of Chemical Engineering, INHA University, 253 Yonghyun-dong, Nam-gu, Incheon 402‐751 (Korea, Republic of); Regional Innovation Center for Environmental Technology of Thermal Plasma (RIC-ETTP), INHA University, 253 Yonghyun-dong, Nam-gu, Incheon 402‐751 (Korea, Republic of)


    Spherical hollow particles were prepared from solid alumina powders using DC arc thermal plasma, and then spray coating was performed with the as-prepared particles. Operating variables for the hollow particle preparation process were additional plasma gas, input power, and carrier gas flow rate. The spherical hollow alumina particles were produced in the case of using additive gas of H{sub 2} or N{sub 2}, while alumina surface was hardly molten in the pure argon thermal plasma. In addition, the hollow particles were well produced in high power and low carrier gas conditions due to high melting point of alumina. Hollow structure was confirmed by focused ion beam-scanning electron microscopy analysis. Morphology and size distribution of the prepared particles that were examined by field emission-scanning electron microscopy and phase composition of the particles was characterized by X-ray diffraction. In the spray coating process, the as-prepared hollow particles showed higher deposition rate. - Highlights: ► Spherical hollow alumina powder was prepared by non-transferred DC arc plasma. ► Diatomic gasses were added in Ar plasma for high power. ► Prepared hollow alumina powder was efficient for the plasma spray coating.

  2. Optimization and validation of sample preparation for metagenomic sequencing of viruses in clinical samples. (United States)

    Lewandowska, Dagmara W; Zagordi, Osvaldo; Geissberger, Fabienne-Desirée; Kufner, Verena; Schmutz, Stefan; Böni, Jürg; Metzner, Karin J; Trkola, Alexandra; Huber, Michael


    Sequence-specific PCR is the most common approach for virus identification in diagnostic laboratories. However, as specific PCR only detects pre-defined targets, novel virus strains or viruses not included in routine test panels will be missed. Recently, advances in high-throughput sequencing allow for virus-sequence-independent identification of entire virus populations in clinical samples, yet standardized protocols are needed to allow broad application in clinical diagnostics. Here, we describe a comprehensive sample preparation protocol for high-throughput metagenomic virus sequencing using random amplification of total nucleic acids from clinical samples. In order to optimize metagenomic sequencing for application in virus diagnostics, we tested different enrichment and amplification procedures on plasma samples spiked with RNA and DNA viruses. A protocol including filtration, nuclease digestion, and random amplification of RNA and DNA in separate reactions provided the best results, allowing reliable recovery of viral genomes and a good correlation of the relative number of sequencing reads with the virus input. We further validated our method by sequencing a multiplexed viral pathogen reagent containing a range of human viruses from different virus families. Our method proved successful in detecting the majority of the included viruses with high read numbers and compared well to other protocols in the field validated against the same reference reagent. Our sequencing protocol does work not only with plasma but also with other clinical samples such as urine and throat swabs. The workflow for virus metagenomic sequencing that we established proved successful in detecting a variety of viruses in different clinical samples. Our protocol supplements existing virus-specific detection strategies providing opportunities to identify atypical and novel viruses commonly not accounted for in routine diagnostic panels.

  3. Polysilicon Prepared from SIC14 by Atmospheric-Pressure Non-Thermal Plasma%Polysilicon Prepared from SIC14 by Atmospheric-Pressure Non-Thermal Plasma

    Institute of Scientific and Technical Information of China (English)

    李小松; 王楠; 杨晋华; 王友年; 朱爱民


    Non-thermal plasma at atmospheric pressure was explored for the preparation of polysilicon from SiCl4. The power supply sources of positive pulse and alternating current (8 kHz and 100 kHz) were compared for polysilicon preparation. The samples prepared by using the 100 kHz power source were crystalline silicon. The effects of H2 and SiCl4 volume fractions were investigated. The optical emission spectra showed that silicon species played an important role in polysilicon deposition

  4. Homogeneous sample preparation of raw shrimp using dry ice. (United States)

    Bunch, E A; Altwein, D M; Johnson, L E; Farley, J R; Hammersmith, A A


    Sample homogeneity is critical to accurate and reproducible analysis of trace residues in foods. A method of uniform sample preparation using dry ice is described for shrimp. Other sample preparation techniques for raw shrimp produce nonhomogeneous samples. Sample homogeneity was determined through analysis of chloramphenicol added to intact tiger or white shrimp prior to sample preparation. Simulated chloramphenicol residue levels were 50, 15, 10, and 5 ppb. No significant differences were noted when analyses of shrimp inoculated with chlor-amphenicol prior to sample preparation with dry ice were compared with analyses of shrimp spiked after grinding with dry ice. Grinding shrimp with dry ice produced samples with homogeneous chloramphenicol residues. This technique should be applicable to other tissues and vegetable products.

  5. Universal Sample Preparation Module for Molecular Analysis in Space Project (United States)

    National Aeronautics and Space Administration — Lynntech proposes to develop and demonstrate the ability of a compact, light-weight, and automated universal sample preparation module (USPM) to process samples from...

  6. Preparation of protein samples for gel electrophoresis by sequential extraction

    Institute of Scientific and Technical Information of China (English)

    钟伯雄; 翁宏飚; 等


    Since preparation and solubilization of protein samples are crucial factors in proteome research,the authors established a sequential extraction technique to prepare protein samples from the body wall of the 5th instar larvae of silkworm.Bombyx mori.Two kinds of protein samples were obtained from the body wall using the method.Between the two types of samples only about 15% proteins were identical;the majority were different,indicating that more species of proteins could be obtained with the sequential extraction method;which will be useful for preparation of protein samples for proteome study.

  7. Preparation of protein samples for gel electrophoresis by sequential extraction

    Institute of Scientific and Technical Information of China (English)

    钟伯雄; 翁宏飚; 方维焕


    Since preparation and solubilization of protein samples are crucial factors in proteome research, the authors established a sequential extraction technique to prepare protein samples from the body wall of the 5th instar larvae of silkworm, Bombyx mori. Two kinds of protein samples were obtained from the body wall using the method. Between the two types of samples only about 15% proteins were identical; the majority were different, indicating that more species of proteins could be obtained with the sequential extraction method; which will be useful for preparation of protein samples for proteome study.

  8. Separation of proteins from human plasma by sample displacement chromatography in hydrophobic interaction mode


    Josic, Djuro; Breen, Lucas; Clifton, James; Gajdosik, Martina Srajer; Gaso-Sokac, Dajana; Rucevic, Marijana; Müller, Egbert


    Sample displacement chromatography (SDC) in reversed-phase and ion-exchange modes was introduced approximately twenty years ago. This method was first used for the preparative purification of peptides and proteins. Recently, SDC in ion-exchange mode was also successfully used for enrichment of low abundance proteins from human plasma. In this paper, the use of SDC for the separation of plasma proteins in hydrophobic interaction mode is demonstrated. By use of two or more columns coupled in se...

  9. Alternative sample preparation methods for MALDI-MS

    Energy Technology Data Exchange (ETDEWEB)

    Hurst, G.B.; Buchanan, M.V. [Oak Ridge National Lab., TN (United States); Czartoski, T.J. [Kenyon College, Gambier, OH (United States)


    Since the introduction of matrix-assisted laser desorption and ionization (MALDI), sample preparation has been a limiting step in the applicability of this important technique for mass spectrometric analysis of biomolecules. A number of variations on the original sample preparation method for have been described. The {open_quotes}standard{close_quotes} method of MALDI sample preparation requires mixing a solution containing the analyte and a large excess of matrix, and allowing a small volume of this solution to dry on a probe tip before insertion into the mass spectrometer. The resulting sample can fairly inhomogeneous. As a result, the process of aiming the desorption laser at a favorable spot on the dried sample can be tedious and time-consuming. The authors are evaluating several approaches to MALDI sample preparation, with the goal of developing a faster and more reproducible method.

  10. Snow White Trench Prepared for Sample Collection (United States)


    The informally named 'Snow White' trench is the source for the next sample to be acquired by NASA's Phoenix Mars Lander for analysis by the wet chemistry lab. The Surface Stereo Imager on Phoenix took this shadow-enhanced image of the trench, on the eastern end of Phoenix's work area, on Sol 103, or the 103rd day of the mission, Sept. 8, 2008. The trench is about 23 centimeters (9 inches) wide. The wet chemistry lab is part of Phoenix's Microscopy, Electrochemistry and Conductivity suite of instruments. The Phoenix Mission is led by the University of Arizona, Tucson, on behalf of NASA. Project management of the mission is by NASA's Jet Propulsion Laboratory, Pasadena, Calif. Spacecraft development is by Lockheed Martin Space Systems, Denver.

  11. Preparing Magnetocaloric LaFeSi Uniform Microstructures by Spark Plasma Sintering

    DEFF Research Database (Denmark)

    Vicente, N.; Ocanã, J.; Neves Bez, Henrique


    Spark Plasma Sintering (SPS) of LaFeSi alloy powders was conducted to prepare magnetocaloric La-Fe-Si-based uniform microstructures. Two electrically insulating discs made of alumina were interposed between the punches and powder sample inhibiting the flow of electric current across the powder......’s microhardness by means of ANOVA statistics....

  12. Sample preparation for atomic spectroscopy: evolution and future trends

    Directory of Open Access Journals (Sweden)

    Oliveira Elisabeth de


    Full Text Available Sample preparation is the critical step of any analytical protocol, and involves steps from simple dilution to partial or total dissolution. The methods include dry or wet decomposition of the samples in open or closed systems, using thermal, ultrasonic or radiant (infrared, ultraviolet and microwaves energy. This review emphasizes sample preparation for atomic spectroscopy. The present and future tendencies for sample preparation also involve on-line dissolution, extraction of the analytes, speciation, solid sample and slurry analysis, in situ and in vivo procedures, etc. Nowadays the goals are the best result, in the shortest time, with minimum contamination, using the smallest quantities of reagents and samples, and having low residue and waste generation, as well as maintaining the integrity of the sample and the traceability of the results, to have quality and confidence in the measurements as the primordial attributes required by the community and by the users.

  13. γ-ray spectrometry results versus sample preparation methods

    Institute of Scientific and Technical Information of China (English)


    According to recommended conditions two bio-samples, tea leave and flour, are prepared with different methods: grounding into powder and reducing to ash, then they were analyzed by γ ray spectrometry. Remarkable difference was shown between the measured values of tea samples prepared with these different methods. One of the reasons may be that the method of reducing to ash makes some nuclides lost. Compared with the "non-destructive"method of grounding into powder, the method of reducing to ash can be much more sensible to the loss of some nuclides. The probable reasons are discussed for the varied influences of different preparation methods of tea leave and flour samples.

  14. Microscale sample preparation for PCR of C. difficile infected stool (United States)

    Gillers, Sara; Atkinson, Christopher D.; Bartoo, Aaron C.; Mahalanabis, Madhumita; Boylan, Michael O.; Schwartz, John H.; Klapperich, Catherine; Singh, Satish K.


    In this paper, we describe the design of a microfluidic sample preparation chip for human stool samples infected with Clostridium difficile. We established a polymerase chain reaction able to distinguish C. difficile in the presence of several other organisms found in the normal intestinal flora. A protocol for on-chip extraction of nucleic acids from clinical samples is described that can detect target DNA down to 5.0×10−3 ng of template. The assay and sample preparation chip were then validated using known positive and known negative clinical samples. The work presented has potential applications in both the developed and developing world. PMID:19505511

  15. Electric-Arc Plasma Installation for Preparing Nanodispersed Carbon Structures

    Institute of Scientific and Technical Information of China (English)



    An electric-arc plasma installation operated in the hidden anode arrangement is constructed and used for the preparation of carbon nanostructures. A contracted plasma arc gen-erated by a plasma torch using an inert gas is used as heat source. The average mass temperature of arc is higher than 104 K, while its power density, which is directly transferred onto the electrode (anode), is ~ 2 kW/mm2. The anode contact area formed on the electrode moves against the arc by way of shifting the electrode and is hidden completely in the interior of plasma gas stream moving towards it. As a result of both the direct plasma attack and the opposite movement of streams in the hidden anode contact area, a temperature higher than 6000 K is reached. Thus, intensive vaporization takes place, which forms a saturated plasma-gas-aerosol phase of the initial material of electrode (anode). This gas phase is mixed in and carried by the plasma stream. Over that mixed plasma stream, a controlled process of quenching (fixation) is carried out by twisted turbulent fluid streams. After the fixation, the resultant carbon nano-structures are caught by a filter and collected in a bunker.

  16. The effect of sample preparation and testing procedure on the ...

    African Journals Online (AJOL)

    The effect of sample preparation and testing procedure on the geotechnical ... of conventional laboratory testing, classification and evaluation systems, which were ... It should not be used to classify them based on conventional methods ...

  17. Preparation of Cytology Samples: Tricks of the Trade. (United States)

    Moore, A Russell


    General principles and techniques for collection, preparation, and staining of cytologic samples in the general practice setting are reviewed. Tips for collection of digital images are also discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  18. Modern methods of sample preparation for GC analysis


    de Koning; Janssen, H.-G.; Brinkman, U.A.T.


    Today, a wide variety of techniques is available for the preparation of (semi-) solid, liquid and gaseous samples, prior to their instrumental analysis by means of capillary gas chromatography (GC) or, increasingly, comprehensive two-dimensional GC (GC × GC). In the past two decades, a large number of ‘modern’ sample-preparation techniques has been introduced, which have partly superseded their ‘classical’ counterparts. These novel techniques include off-line and on-line (sometimes semi- or f...

  19. Curatorial Works for the Hayabusa-Returned Sample and Preparation for Hayabusa2 Sample Curation (United States)

    Yada, T.; Abe, M.; Okada, T.; Yurimoto, H.; Uesugi, M.; Karouji, Y.; Nakato, A.; Hashiguchi, M.; Nishimura, M.; Kumagai, K.; Matsui, S.; Yoshitake, M.; Sakamoto, K.; Nakano, Y.; Kawasaki, N.; Fujimoto, M.


    We continue describing Hayabusa-returned samples after its return in 2010. The number of described particles reaches around 650 and >540 of them are identified as Itokawa origin. We also start preparation for Hayabusa2 sample curation.

  20. Blood sampling and hemolysis affect concentration of plasma metabolites

    DEFF Research Database (Denmark)

    Theil, Peter Kappel; Pedersen, Lene Juul; Jensen, Margit Bak;


    , a subset of samples from 24 sows fed twice daily in Exp. 1 was combined with data obtained from 30 sows sampled using jugular vein catheters. All sows in Exp. 2 were fed twice daily (0800 h and 1500 h) and blood samples collected repeatedly 1, 4, 11, and 23 h after morning feeding (other conditions were......Two experiments were carried out to reveal and quantify plasma metabolites that are sensitive to hemolysis and animal stress due to the blood sampling procedure (vein puncture vs. catheter). In Exp. 1, 48 sows were fed 4 diets either once (0800 h) or twice daily (0800 h and 1500 h) in a crossover...... design and blood was collected after restraint via vein puncture 1, 4, 11, and 23 h after morning feeding. Plasma samples were categorized as without or with minor or major hemolysis [clear (n = 218), yellow (n = 97), or red (n = 37)] upon centrifugation. Plasma NEFA (P

  1. Sample Preparation (SS): SE51_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available e Master NEO, BMS, Tokyo, Japan), and the seed powder was extracted with 1 mL of extraction buffer (0.1% HCO...trifugation (4 ℃, 10,000 rpm, 5 min), the sample tubes were subjected to sample preparation (buffer transfer

  2. A 96-well screen filter plate for high-throughput biological sample preparation and LC-MS/MS analysis. (United States)

    Peng, Sean X; Cousineau, Martin; Juzwin, Stephen J; Ritchie, David M


    A novel 96-well screen filter plate (patent pending) has been invented to eliminate a time-consuming and labor-intensive step in preparation of in vivo study samples--to remove blood or plasma clots. These clots plug the pipet tips during a manual or automated sample-transfer step causing inaccurate pipetting or total pipetting failure. Traditionally, these blood and plasma clots are removed by picking them out manually one by one from each sample tube before any sample transfer can be made. This has significantly slowed the sample preparation process and has become a bottleneck for automated high-throughput sample preparation using robotic liquid handlers. Our novel screen filter plate was developed to solve this problem. The 96-well screen filter plate consists of 96 stainless steel wire-mesh screen tubes connected to the 96 openings of a top plate so that the screen filter plate can be readily inserted into a 96-well sample storage plate. Upon insertion, the blood and plasma clots are excluded from entering the screen tube while clear sample solutions flow freely into it. In this way, sample transfer can be easily completed by either manual or automated pipetting methods. In this report, three structurally diverse compounds were selected to evaluate and validate the use of the screen filter plate. The plasma samples of these compounds were transferred and processed in the presence and absence of the screen filter plate and then analyzed by LC-MS/MS methods. Our results showed a good agreement between the samples prepared with and without the screen filter plate, demonstrating the utility and efficiency of this novel device for preparation of blood and plasma samples. The device is simple, easy to use, and reusable. It can be employed for sample preparation of other biological fluids that contain floating particulates or aggregates.

  3. Ion sampling and transport in Inductively Coupled Plasma Mass Spectrometry (United States)

    Farnsworth, Paul B.; Spencer, Ross L.


    Quantitative accuracy and high sensitivity in inductively coupled plasma mass spectrometry (ICP-MS) depend on consistent and efficient extraction and transport of analyte ions from an inductively coupled plasma to a mass analyzer, where they are sorted and detected. In this review we examine the fundamental physical processes that control ion sampling and transport in ICP-MS and compare the results of theory and computerized models with experimental efforts to characterize the flow of ions through plasma mass spectrometers' vacuum interfaces. We trace the flow of ions from their generation in the plasma, into the sampling cone, through the supersonic expansion in the first vacuum stage, through the skimmer, and into the ion optics that deliver the ions to the mass analyzer. At each stage we consider idealized behavior and departures from ideal behavior that affect the performance of ICP-MS as an analytical tool.

  4. New materials for sample preparation techniques in bioanalysis. (United States)

    Nazario, Carlos Eduardo Domingues; Fumes, Bruno Henrique; da Silva, Meire Ribeiro; Lanças, Fernando Mauro


    The analysis of biological samples is a complex and difficult task owing to two basic and complementary issues: the high complexity of most biological matrices and the need to determine minute quantities of active substances and contaminants in such complex sample. To succeed in this endeavor samples are usually subject to three steps of a comprehensive analytical methodological approach: sample preparation, analytes isolation (usually utilizing a chromatographic technique) and qualitative/quantitative analysis (usually with the aid of mass spectrometric tools). Owing to the complex nature of bio-samples, and the very low concentration of the target analytes to be determined, selective sample preparation techniques is mandatory in order to overcome the difficulties imposed by these two constraints. During the last decade new chemical synthesis approaches has been developed and optimized, such as sol-gel and molecularly imprinting technologies, allowing the preparation of novel materials for sample preparation including graphene and derivatives, magnetic materials, ionic liquids, molecularly imprinted polymers, and much more. In this contribution we will review these novel techniques and materials, as well as their application to the bioanalysis niche. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Experimental breakdown of selected anodized aluminum samples in dilute plasmas (United States)

    Grier, Norman T.; Domitz, Stanley


    Anodized aluminum samples representative of Space Station Freedom structural material were tested for electrical breakdown under space plasma conditions. In space, this potential arises across the insulating anodized coating when the spacecraft structure is driven to a negative bias relative to the external plasma potential due to plasma-surface interaction phenomena. For anodized materials used in the tests, it was found that breakdown voltage varied from 100 to 2000 volts depending on the sample. The current in the arcs depended on the sample, the capacitor, and the voltage. The level of the arc currents varied from 60 to 1000 amperes. The plasma number density varied from 3 x 10 exp 6 to 10 exp 3 ions per cc. The time between arcs increased as the number density was lowered. Corona testing of anodized samples revealed that samples with higher corona inception voltage had higher arcing inception voltages. From this it is concluded that corona testing may provide a method of screening the samples.

  6. Microfluidic Sample Preparation Methods for the Analysis of Milk Contaminants

    Directory of Open Access Journals (Sweden)

    Andrea Adami


    Full Text Available In systems for food analysis, one of the major challenges is related to the quantification of specific species into the complex chemical and physical composition of foods, that is, the effect of “matrix”; the sample preparation is often the key to a successful application of biosensors to real measurements but little attention is traditionally paid to such aspects in sensor research. In this critical review, we discuss several microfluidic concepts that can play a significant role in sample preparation, highlighting the importance of sample preparation for efficient detection of food contamination. As a case study, we focus on the challenges related to the detection of aflatoxin M1 in milk and we evaluate possible approaches based on inertial microfluidics, electrophoresis, and acoustic separation, compared with traditional laboratory and industrial methods for phase separation as a baseline of thrust and well-established techniques.

  7. Fluidics platform and method for sample preparation and analysis

    Energy Technology Data Exchange (ETDEWEB)

    Benner, W. Henry; Dzenitis, John M.; Bennet, William J.; Baker, Brian R.


    Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

  8. Metabolomic Quality Assessment of EDTA Plasma and Serum Samples. (United States)

    Malm, Linus; Tybring, Gunnel; Moritz, Thomas; Landin, Britta; Galli, Joakim


    Handling and processing of blood can significantly alter the molecular composition and consistency of biobank samples and can have a major impact on the identification of biomarkers. It is thus crucial to identify tools to determine the quality of samples to be used in biomarker discovery studies. In this study, a non-targeted gas chromatography/time-of-flight mass spectrometry (GC-TOFMS) metabolomic strategy was used with the aim of identifying quality markers for serum and plasma biobank collections lacking proper documentation of preanalytical handling. The effect of postcentrifugation delay was examined in serum stored in tubes with gel separation plugs and ethylenediaminetetraacetic acid (EDTA) plasma in tubes with or without gel separation plugs. The change in metabolic pattern was negligible in all sample types processed within 3 hours after centrifugation regardless of whether the samples were kept at 4°C or 22°C. After 8 and 24 hours postcentrifugation delay before aliquoting, there was a pronounced increase in the number of affected metabolites, as well as in the magnitude of the observed changes. No protective effect on the metabolites was observed in gel-separated EDTA plasma samples. In a separate series of experiments, lactate and glucose levels were determined in plasma to estimate the effect of precentrifugation delay. This separate experiment indicates that the lactate to glucose ratio may serve as a marker to identify samples with delayed time to centrifugation. Although our data from the untargeted GC-TOFMS analysis did not identify any specific markers, we conclude that plasma and serum metabolic profiles remain quite stable when plasma and serum are centrifuged and separated from the blood cells within 3 hours.

  9. Sample preparation for quantitation of tritium by accelerator mass spectrometry. (United States)

    Chiarappa-Zucca, Marina L; Dingley, Karen H; Roberts, Mark L; Velsko, Carol A; Love, Adam H


    The capability to prepare samples accurately and reproducibly for analysis of tritium (3H) content by accelerator mass spectrometry (AMS) greatly facilitates isotopic tracer studies in which attomole levels of 3H can be measured in milligram-sized samples. A method has been developed to convert the hydrogen of organic samples to a solid, titanium hydride, which can be analyzed by AMS. Using a two-step process, the sample is first oxidized to carbon dioxide and water. In the second step, the water is transferred within a heated manifold into a quartz tube, reduced to hydrogen gas using zinc, and reacted with titanium powder. The 3H/1H ratio of the titanium hydride is measured by AMS and normalized to standards whose ratios were determined by decay counting to calculate the amount of 3H in the original sample. Water, organic compounds, and biological samples with 3H activities measured by liquid scintillation counting were utilized to develop and validate the method. The 3H/1H ratios were quantified in samples that spanned 5 orders of magnitude, from 10(-10) to 10(-15), with a detection limit of 3.0 x 10(-15), which is equivalent to 0.02 dpm tritium/mg of material. Samples smaller than 2 mg were analyzed following addition of 2 mg of a tritium-free-hydrogen carrier. Preparation of organic standards containing both 14C and 3H in 2-mg organic samples demonstrated that this sample preparation methodology can also be applied to quantify both of these isotopes from a single sample.

  10. Inductively coupled plasma mass spectrometry in the analysis of biological samples and pharmaceutical drugs (United States)

    Ossipov, K.; Seregina, I. F.; Bolshov, M. A.


    Inductively coupled plasma mass spectrometry (ICP-MS) is widely used in the analysis of biological samples (whole blood, serum, blood plasma, urine, tissues, etc.) and pharmaceutical drugs. The shortcomings of this method related to spectral and non-spectral interferences are manifested in full measure in determination of the target analytes in these complex samples strongly differing in composition. The spectral interferences are caused by similarity of masses of the target component and sample matrix components. Non-spectral interferences are related to the influence of sample matrix components on the physicochemical processes taking place during formation and transportation of liquid sample aerosols into the plasma, on the value and spatial distribution of plasma temperature and on the transmission of the ion beam from the interface to mass spectrometer detector. The review is devoted to analysis of different mechanisms of appearance of non-spectral interferences and to ways for their minimization or elimination. Special attention is paid to the techniques of biological sample preparation, which largely determine the mechanisms of the influence of sample composition on the results of element determination. The ways of lowering non-spectral interferences by instrumental parameter tuning and application of internal standards are considered. The bibliography includes 189 references.

  11. Basic tree-ring sample preparation techniques for aging aspen (United States)

    Lance A. Asherin; Stephen A. Mata


    Aspen is notoriously difficult to age because of its light-colored wood and faint annual growth rings. Careful preparation and processing of aspen ring samples can overcome these problems, yield accurate age and growth estimates, and concisely date disturbance events present in the tree-ring record. Proper collection of aspen wood is essential in obtaining usable ring...

  12. Preparation of artificial plasma membrane mimicking vesicles with lipid asymmetry.

    Directory of Open Access Journals (Sweden)

    Qingqing Lin

    Full Text Available Lipid asymmetry, the difference in lipid distribution across the lipid bilayer, is one of the most important features of eukaryotic cellular membranes. However, commonly used model membrane vesicles cannot provide control of lipid distribution between inner and outer leaflets. We recently developed methods to prepare asymmetric model membrane vesicles, but facile incorporation of a highly controlled level of cholesterol was not possible. In this study, using hydroxypropyl-α-cyclodextrin based lipid exchange, a simple method was devised to prepare large unilamellar model membrane vesicles that closely resemble mammalian plasma membranes in terms of their lipid composition and asymmetry (sphingomyelin (SM and/or phosphatidylcholine (PC outside/phosphatidylethanolamine (PE and phosphatidylserine (PS inside, and in which cholesterol content can be readily varied between 0 and 50 mol%. We call these model membranes "artificial plasma membrane mimicking" ("PMm" vesicles. Asymmetry was confirmed by both chemical labeling and measurement of the amount of externally-exposed anionic lipid. These vesicles should be superior and more realistic model membranes for studies of lipid-lipid and lipid-protein interaction in a lipid environment that resembles that of mammalian plasma membranes.

  13. Preparation of artificial plasma membrane mimicking vesicles with lipid asymmetry. (United States)

    Lin, Qingqing; London, Erwin


    Lipid asymmetry, the difference in lipid distribution across the lipid bilayer, is one of the most important features of eukaryotic cellular membranes. However, commonly used model membrane vesicles cannot provide control of lipid distribution between inner and outer leaflets. We recently developed methods to prepare asymmetric model membrane vesicles, but facile incorporation of a highly controlled level of cholesterol was not possible. In this study, using hydroxypropyl-α-cyclodextrin based lipid exchange, a simple method was devised to prepare large unilamellar model membrane vesicles that closely resemble mammalian plasma membranes in terms of their lipid composition and asymmetry (sphingomyelin (SM) and/or phosphatidylcholine (PC) outside/phosphatidylethanolamine (PE) and phosphatidylserine (PS) inside), and in which cholesterol content can be readily varied between 0 and 50 mol%. We call these model membranes "artificial plasma membrane mimicking" ("PMm") vesicles. Asymmetry was confirmed by both chemical labeling and measurement of the amount of externally-exposed anionic lipid. These vesicles should be superior and more realistic model membranes for studies of lipid-lipid and lipid-protein interaction in a lipid environment that resembles that of mammalian plasma membranes.

  14. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen


    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  15. 51Cr-EDTA plasma clearance in severe renal failure determined by one plasma sample

    DEFF Research Database (Denmark)

    Kamper, A L; Nielsen, S L


    at zero-time was derived from injected dose and body surface area. This method might provide values 1.5 ml/min below or 0.8 ml/min above the established method of 51Cr-EDTA plasma clearance, which would be acceptable for clinical purposes. It is concluded that exact plasma clearance of 51Cr-EDTA in severe......Two hundred and thirty-four measurements of standard 51Cr-EDTA plasma clearance were made in 50 patients with severe chronic renal failure. Based on these data two calculation methods were attempted using one plasma sample drawn 24 h after injection of 51Cr-EDTA. One of the methods used the 'one...... sample clearance' formulas disregarding exact time of plasma sampling. This method might provide values 3.1 ml/min below or 2.9 ml/min above the established method of total 51Cr-EDTA plasma clearance, and would thus provide insufficient agreement. In the other method an estimate of plasma activity...

  16. Applications of reversible covalent chemistry in analytical sample preparation. (United States)

    Siegel, David


    Reversible covalent chemistry (RCC) adds another dimension to commonly used sample preparation techniques like solid-phase extraction (SPE), solid-phase microextraction (SPME), molecular imprinted polymers (MIPs) or immuno-affinity cleanup (IAC): chemical selectivity. By selecting analytes according to their covalent reactivity, sample complexity can be reduced significantly, resulting in enhanced analytical performance for low-abundance target analytes. This review gives a comprehensive overview of the applications of RCC in analytical sample preparation. The major reactions covered include reversible boronic ester formation, thiol-disulfide exchange and reversible hydrazone formation, targeting analyte groups like diols (sugars, glycoproteins and glycopeptides, catechols), thiols (cysteinyl-proteins and cysteinyl-peptides) and carbonyls (carbonylated proteins, mycotoxins). Their applications range from low abundance proteomics to reversible protein/peptide labelling to antibody chromatography to quantitative and qualitative food analysis. In discussing the potential of RCC, a special focus is on the conditions and restrictions of the utilized reaction chemistry.

  17. Liquid chromatography-mass spectrometric determination of rufinamide in low volume plasma samples. (United States)

    Gáll, Zsolt; Vancea, Szende; Dogaru, Maria T; Szilágyi, Tibor


    Quantification of rufinamide in plasma was achieved using a selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method. The chromatographic separation was achieved on a reversed phase column (Zorbax SB-C18 100mm×3mm, 3.5μm) under isocratic conditions. The mobile phase consisted of a mixture of water containing 0.1% formic acid and methanol (50:50, v/v). The mass spectrometric detection of the analyte was in multiple reaction monitoring mode (MRM) using an electrospray positive ionization (ESI positive). The monitored ions were 127m/z derived from 239m/z rufinamide and 108m/z derived from 251m/z the internal standard (lacosamide). Protein precipitation with methanol was applied for sample preparation using only 50μl aliquots. The concentration range was 40-2000ng/ml for rufinamide in plasma. The limit of detection was 1.25ng/ml and the lower limit of quantification was established at 5ng/ml rufinamide concentration. Selectivity and matrix effect was verified using individual human, rat and rabbit plasma samples. Short-term, post-preparative and freeze-thaw stability was also investigated. The proposed method provides accuracy, precision and high-throughput (short runtime 4.5min) for quantitative determination of rufinamide in plasma. This is the first reported liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for analysis of rufinamide from low volume plasma samples. The LC-MS/MS method was validated according to the current official guidelines and can be applied to accurately measure rufinamide level of large number of plasma samples from clinical studies or therapeutic drug monitoring.

  18. [Optimized sample preparation for metabolome studies on Streptomyces coelicolor]. (United States)

    Li, Yihong; Li, Shanshan; Ai, Guomin; Wang, Weishan; Zhang, Buchang; Yang, Keqian


    Streptomycetes produce many antibiotics and are important model microorgansims for scientific research and antibiotic production. Metabolomics is an emerging technological platform to analyze low molecular weight metabolites in a given organism qualitatively and quantitatively. Compared to other Omics platform, metabolomics has greater advantage in monitoring metabolic flux distribution and thus identifying key metabolites related to target metabolic pathway. The present work aims at establishing a rapid, accurate sample preparation protocol for metabolomics analysis in streptomycetes. In the present work, several sample preparation steps, including cell quenching time, cell separation method, conditions for metabolite extraction and metabolite derivatization were optimized. Then, the metabolic profiles of Streptomyces coelicolor during different growth stages were analyzed by GC-MS. The optimal sample preparation conditions were as follows: time of low-temperature quenching 4 min, cell separation by fast filtration, time of freeze-thaw 45 s/3 min and the conditions of metabolite derivatization at 40 degrees C for 90 min. By using this optimized protocol, 103 metabolites were finally identified from a sample of S. coelicolor, which distribute in central metabolic pathways (glycolysis, pentose phosphate pathway and citrate cycle), amino acid, fatty acid, nucleotide metabolic pathways, etc. By comparing the temporal profiles of these metabolites, the amino acid and fatty acid metabolic pathways were found to stay at a high level during stationary phase, therefore, these pathways may play an important role during the transition between the primary and secondary metabolism. An optimized protocol of sample preparation was established and applied for metabolomics analysis of S. coelicolor, 103 metabolites were identified. The temporal profiles of metabolites reveal amino acid and fatty acid metabolic pathways may play an important role in the transition from primary to

  19. Microstructure characterization of PAN preoxidation fibers prepared with radio frequency plasma

    Institute of Scientific and Technical Information of China (English)

    FU Weibiao; XU Haiping; GONG Jingsong; SUN Yanping; HOU Lingyun; CHEN Xinmou


    The microstructures of preoxidation fibers prepared with radio frequency plasma were characterized in terms of micron, nano and atomic scales through scanning electron microscopy (SEM), high resolving transmission electron microscopy (HRTEM), scanning tunneling microscopy (STM), X-ray diffraction (XRD), etc. The polyacrylonitrile (PAN) precursors were first soaked in the oxygen-enriched solvent and polarized in radio frequency electric field, and then were oxidized in the atmosphere of oxygen plasma. The morphology of SEM at micron scales shows that the wrinkles on the surface of preoxidation fibers prepared with plasma are shallower, and the surfaces are more tidy and smoother than the unsoaked samples prepared with usual electric furnace, and the uneven radial structure is improved. The results of XRD calculation show that the graphitization degree and microcrystalline size get larger and the interlayer spacing gets smaller. Also, the lattice stripe and edge of bedding plane (002) can be observed from HRTEM at nano scales. From STM images at nano and atom scales, the microfibrils were found to be composed of ultrafibrils that closely twined and arranged, forming the left spiral structures spreading to fiber axis, and the carbon atoms on the surface of microcrystalline were found to have the trend of directional arrangement. All the above characterization results indicate that the plasma method effectively makes the internal and external oxidation of PAN precursors at the same level, so that the radial structure difference of preoxidation fibers is reduced.

  20. Preparation of SELEX Samples for Next-Generation Sequencing. (United States)

    Tolle, Fabian; Mayer, Günter


    Fuelled by massive whole genome sequencing projects such as the human genome project, enormous technological advancements and therefore tremendous price drops could be achieved, rendering next-generation sequencing very attractive for deep sequencing of SELEX libraries. Herein we describe the preparation of SELEX samples for Illumina sequencing, based on the already established whole genome sequencing workflow. We describe the addition of barcode sequences for multiplexing and the adapter ligation, avoiding associated pitfalls.

  1. Sample preparation of metal alloys by electric discharge machining (United States)

    Chapman, G. B., II; Gordon, W. A.


    Electric discharge machining was investigated as a noncontaminating method of comminuting alloys for subsequent chemical analysis. Particulate dispersions in water were produced from bulk alloys at a rate of about 5 mg/min by using a commercially available machining instrument. The utility of this approach was demonstrated by results obtained when acidified dispersions were substituted for true acid solutions in an established spectrochemical method. The analysis results were not significantly different for the two sample forms. Particle size measurements and preliminary results from other spectrochemical methods which require direct aspiration of liquid into flame or plasma sources are reported.

  2. Reproducibility of Circulating MicroRNAs in Stored Plasma Samples.

    Directory of Open Access Journals (Sweden)

    Monica L Bertoia

    Full Text Available Most studies of microRNA (miRNA and disease have examined tissue-specific expression in limited numbers of samples. The presence of circulating miRNAs in plasma samples provides the opportunity to examine prospective associations between miRNA expression and disease in initially healthy individuals. However, little data exist on the reproducibility of miRNAs in stored plasma.We used Real-Time PCR to measure 61 pre-selected microRNA candidates in stored plasma. Coefficients of variation (CVs were used to assess inter-assay reliability (n = 15 and within-person stability over one year (n = 80. Intraclass correlation coefficients (ICCs and polychoric correlation coefficients were used to assess within-person stability and delayed processing reproducibility (whole blood stored at 4°C for 0, 24 and 48 hours; n = 12 samples.Of 61 selected miRNAs, 23 were detected in at least 50% of samples and had average CVs below 20% for inter-assay reproducibility and 31 for delayed processing reproducibility. Ten miRNAs were detected in at least 50% of samples, had average CVs below 20% and had ICCs above 0.4 for within-person stability over 1-2 years, six of which satisfied criteria for both interassay reproducibility and short-term within-person stability (miR-17-5p, -191-5p, -26a-5p, -27b-3p, -320a, and -375 and two all three types of reproducibility (miR-27b-3p and -26a-5p. However, many miRNAs with acceptable average CVs had high maximum CVs, most had low expression levels, and several had low ICCs with delayed processing.About a tenth of miRNAs plausibly related to chronic disease were reliably detected in stored samples of healthy adults.

  3. Optimization for Peptide Sample Preparation for Urine Peptidomics

    Energy Technology Data Exchange (ETDEWEB)

    Sigdel, Tara K.; Nicora, Carrie D.; Hsieh, Szu-Chuan; Dai, Hong; Qian, Weijun; Camp, David G.; Sarwal, Minnie M.


    Analysis of native or endogenous peptides in biofluids can provide valuable insights into disease mechanisms. Furthermore, the detected peptides may also have utility as potential biomarkers for non-invasive monitoring of human diseases. The non-invasive nature of urine collection and the abundance of peptides in the urine makes analysis by high-throughput ‘peptidomics’ methods , an attractive approach for investigating the pathogenesis of renal disease. However, urine peptidomics methodologies can be problematic with regards to difficulties associated with sample preparation. The urine matrix can provide significant background interference in making the analytical measurements that it hampers both the identification of peptides and the depth of the peptidomics read when utilizing LC-MS based peptidome analysis. We report on a novel adaptation of the standard solid phase extraction (SPE) method to a modified SPE (mSPE) approach for improved peptide yield and analysis sensitivity with LC-MS based peptidomics in terms of time, cost, clogging of the LC-MS column, peptide yield, peptide quality, and number of peptides identified by each method. Expense and time requirements were comparable for both SPE and mSPE, but more interfering contaminants from the urine matrix were evident in the SPE preparations (e.g., clogging of the LC-MS columns, yellowish background coloration of prepared samples due to retained urobilin, lower peptide yields) when compared to the mSPE method. When we compared data from technical replicates of 4 runs, the mSPE method provided significantly improved efficiencies for the preparation of samples from urine (e.g., mSPE peptide identification 82% versus 18% with SPE; p = 8.92E-05). Additionally, peptide identifications, when applying the mSPE method, highlighted the biology of differential activation of urine peptidases during acute renal transplant rejection with distinct laddering of specific peptides, which was obscured for most proteins

  4. Radiocarbon accelerator mass spectrometry (AMS) sample preparation laboratory in Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Macario, Kita D.; Gomes, Paulo R. S.; Anjos, Roberto M. dos; Linares, Roberto; Queiroz, Eduardo; Oliveira, Fabiana M. de; Cardozo, Laio [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil); Carvalho, Carla R.A. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil)


    Full text: For decades Accelerator Mass Spectrometry has been widely used for radiocarbon measurements all over the world with application in several fields of science from archaeology to geosciences. This technique provides ultrasensitive analysis of reduced size samples or even specific compounds since sample atoms are accelerated to high energies and measured using nuclear particle detectors. Sample preparation is extremely important for accurate radiocarbon measurement and includes chemical pre-treatment to remove all possible contaminants. For beam extraction in the accelerator ion source, samples are usually converted to graphite. In this work we report a new radiocarbon sample preparation facility installed at the Physics Institute of Universidade Federal Fluminense (UFF), in Brazil. At the Nuclear Chronology Laboratory (LACRON) samples are chemically treated and converted to carbon dioxide by hydrolysis or combustion. A stainless steel based vacuum line was constructed for carbon dioxide separation and graphitization is performed in sealed quartz tubes in a muffle oven. Successful graphite production is important to provide stable beam currents and to minimize isotopic fractionation. Performance tests for graphite production are currently under way and isotopic analysis will soon be possible with the acquisition of a Single Stage AMS System by our group. The Single Stage Accelerator produced by National Electrostatic Corporation is a 250 kV air insulated accelerator especially constructed to measure the amount of {sup 14}C in small modern graphite samples to a precision of 0.3 % or better. With the installation of such equipment in the first half of 2012, UFF will be ready to perform the 14C -AMS technique. (author)

  5. Amorphous semiconductor sample preparation for transmission EXAFS measurements

    Energy Technology Data Exchange (ETDEWEB)

    Ridgway, M.C.; Glover, C.J.; Tan, H.H. [Australian National Univ., Canberra (Australia). Dept. of Electronic Materials Engineering] [and others


    A novel methodology has been developed for the preparation of amorphous semiconductor samples for use in transmission extended x-ray absorption fine structure (EXAFS) measurements. Epitaxial heterostructures were fabricated by metal organic chemical vapor deposition (group III-Vs) or molecular beam epitaxy (group IVs). An epitaxial layer of {approximately} 2 {micro}m thickness was separated from the underlying substrate by selective chemical etching of an intermediate sacrificial layer. Ion implantation was utilized to amorphize the epitaxial layer either before or after selective chemical etching. The resulting samples were both stoichiometric and homogeneous in contrast to those produced by conventional techniques. The fabrication of amorphous GaAs, InP, In{sub 0.53}Ga{sub 0.47}As and Si{sub x}Ge{sub 1{minus}x} samples is described. Furthermore, EXAFS measurements comparing both fluorescence and transmission detection, and crystalline and amorphized GaAs, are shown.

  6. Hands-free sample preparation platform for nucleic acid analysis. (United States)

    Baier, T; Hansen-Hagge, T E; Gransee, R; Crombé, A; Schmahl, S; Paulus, C; Drese, K S; Keegan, H; Martin, C; O'Leary, J J; Furuberg, L; Solli, L; Grønn, P; Falang, I M; Karlgård, A; Gulliksen, A; Karlsen, F


    A Lab-On-Chip system with an instrument is presented which is capable of performing total sample preparation and automated extraction of nucleic acid from human cell samples fixed in a methanol based solution. The target application is extraction of mRNA from cervical liquid based cytology specimens for detection of transformed HPV-infections. The device accepts 3 ml of sample and performs the extraction in a disposable polymer chip of credit card size. All necessary reagents for cell lysis, washing, and elution are stored on-chip and the extraction is performed in two filter stages; one for cell pre-concentration and the other for nucleic acid capture. Tests performed using cancer cell lines and cervical liquid based cytology specimens confirm the extraction of HPV-mRNA by the system.

  7. A fast method to prepare water samples for 15N analysis

    Institute of Scientific and Technical Information of China (English)

    肖化云; 刘丛强


    Automatic element analyser is often used to prepare organic matters tor 15N analysis. It is seldom used to prepare water samples. Water samples are conventionally dealt with by Kjeldahl-Rittenberg technique. But it requires tedious and labor-intensive sample preparation. A fast and reliable method is proposed in this paper to prepare water samples for 15N analysis.

  8. Evaluation of two human plasma pools as candidate international standard preparations for syphilitic antibodies. (United States)

    Rigsby, Peter; Ison, Catherine; Brierley, Matthew; Ballard, Ron; Hagedorn, Hans-Jochen; Lewis, David A; Notermans, Daan W; Riis, Jørn; Robertson, Peter; Seppälä, Ilkka J T; Rijpkema, Sjoerd


    A collaborative study was designed to asses two freeze-dried human plasma preparations containing anti-Treponema pallidum antibodies, 05/132 and 05/122, for their suitability as international reference reagents for syphilis serology. Both preparations are intended as replacements of the first international standard (IS) for syphilitic serum antibodies (HS). Samples were tested by eight laboratories using the T. pallidum passive particle agglutination assay (TPPA), the venereal disease research laboratory test (VDRL) and the rapid plasma reagin test (RPR). In addition a range of immunoassays was also used. The outcome of the collaborative study revealed that candidate standard 05/132 contains T. pallidum-specific IgG and IgM and is reactive in VDRL or RPR, and that 05/122 contains T. pallidum-specific IgG but is not reactive in either the VDRL or RPR test. Both 05/132 and 05/122 are reactive in the TPPA. On the basis of these results the Expert Committee on Biological Standardization of the World Health Organization designated 05/132 as the 1st IS for human syphilitic plasma IgG and IgM with a unitage of 3 IU per ampoule relative to HS and 05/122 as the 1st IS for human syphilitic plasma IgG with a unitage of 300 mIU per ampoule relative to 05/132.

  9. Sample Preparation (SS) - Metabolonote | LSDB Archive [Life Science Database Archive metadata

    Lifescience Database Archive (English)

    Full Text Available 908/lsdba.nbdc01324-008 Description of data contents Detailed information regarding sample preparations comm...ed to by S (Sample information). Data file File name: File URL: File size: 13 KB Simple search URL Preparation ID are merged into ID in the Simple search.) Sample Preparation ID The sample preparation detai

  10. On sample preparation and dielectric breakdown in nanostructured epoxy resins

    Energy Technology Data Exchange (ETDEWEB)

    Reading, M; Xu, Z; Lewin, P L; Vaughan, A S, E-mail: [Tony Davies High Voltage Laboratory, University of Southampton (United Kingdom)


    There are many methods available to achieve a good dispersion of fillers within a polymeric matrix. This investigation considered several methods of dispersing three chosen fillers within an epoxy resin; the same processes were also performed on unfilled materials to investigate any effects they may have on the host material. For this investigation, the epoxy system (EP) was combined with sodium montmorillonite (MMT), micrometric silicon dioxide (SD) or nanometric silicon dioxide (NSD) as fillers. The effect of the different sample preparation routes on breakdown behaviour was then evaluated. While more thorough mixing protocols were found to lead to improved breakdown behaviour in the case of the various filled systems, surprisingly, an entirely equivalent form of behaviour was also seen in the unfilled epoxy. The influence of changes in sample geometry on the breakdown strength was established.

  11. Preparation to manufacturing of ITER plasma facing components in Russia

    Energy Technology Data Exchange (ETDEWEB)

    Mazul, I.V., E-mail: [Efremov Institute, St. Petersburg, 196641 (Russian Federation); Belyakov, V.A.; Giniatulin, R.N.; Gervash, A.A.; Kuznetsov, V.E.; Makhankov, A.N. [Efremov Institute, St. Petersburg, 196641 (Russian Federation); Sizenev, V.S. [Corporation ' Kompozit' , Korolev, 141070 (Russian Federation)


    The preparation of the procurement activities for the ITER plasma-facing-components (PFC) is currently well underway. Three ITER procurement packages associated with PFCs are currently allocated to the Russian Federation (RF): delivery of the central assembly of the divertor (dome and reflector plates assemblies), delivery of 40% of the first-wall (FW) panels and high heat flux testing of divertor components during the qualification and subsequent manufacturing phases. The results of the qualification process for these tasks undertaken by RF industry are presented. Qualification mockups of the dome divertor structure were successfully manufactured in accordance with the ITER specifications and tested at heat fluxes exceeding operational ones. The maturity and reliability of the proposed design and manufacturing technologies, proposed by RF industry, was therefore demonstrated. To confirm the manufacturing readiness of technologies proposed for the fabrication of the ITER first wall, three qualification mockups were fabricated. Two were heat flux tested in two facilities abroad. In addition to launching the qualification process, the PFC team at Efremov Institute is preparing the industrial facilities for serial production of above mentioned components. A brief description of such facilities is presented in this paper, together with the manufacturing technologies to be used. Two electron beam facilities (Tsefey and IDTF) for various high heat flux testing of PFC components are also described.

  12. Preparation of tissue samples for X-ray fluorescence microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Chwiej, Joanna [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland)]. E-mail:; Szczerbowska-Boruchowska, Magdalena [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Lankosz, Marek [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Wojcik, Slawomir [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Falkenberg, Gerald [Hamburger Synchrotronstrahlungslabor at Deutsches Elektronen-Synchrotron, Notkestr. 85, Hamburg (Germany); Stegowski, Zdzislaw [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Setkowicz, Zuzanna [Department of Neuroanatomy, Institute of Zoology, Jagiellonian University, Ingardena 6, 30-060 Cracow (Poland)


    As is well-known, trace elements, especially metals, play an important role in the pathogenesis of many disorders. The topographic and quantitative elemental analysis of pathologically changed tissues may shed some new light on processes leading to the degeneration of cells in the case of selected diseases. An ideal and powerful tool for such purpose is the Synchrotron Microbeam X-ray Fluorescence technique. It enables the carrying out of investigations of the elemental composition of tissues even at the single cell level. The tissue samples for histopathological investigations are routinely fixed and embedded in paraffin. The authors try to verify the usefulness of such prepared tissue sections for elemental analysis with the use of X-ray fluorescence microscopy. Studies were performed on rat brain samples. Changes in elemental composition caused by fixation in formalin or paraformaldehyde and embedding in paraffin were examined. Measurements were carried out at the bending magnet beamline L of the Hamburger Synchrotronstrahlungslabor HASYLAB in Hamburg. The decrease in mass per unit area of K, Br and the increase in P, S, Fe, Cu and Zn in the tissue were observed as a result of the fixation. For the samples embedded in paraffin, a lower level of most elements was observed. Additionally, for these samples, changes in the composition of some elements were not uniform for different analyzed areas of rat brain.

  13. Nanoliter viscometer for analyzing blood plasma and other liquid samples. (United States)

    Srivastava, Nimisha; Davenport, Robertson D; Burns, Mark A


    We have developed a microfabricated nanoliter capillary viscometer that quickly, easily, and inexpensively measures the viscosity of liquids. The measurement of viscosity is based on capillary pressure-driven flow inside microfluidic channels (depth approximately 30 microm and width approximately 300 microm). Accurate and precise viscosity measurements can be made in less than 100 s while using only 600 nL of liquid sample. The silicon-glass hybrid device (18 mm by 15 mm) contains on-chip components that measure the driving capillary pressure difference and the relevant geometrical parameters; these components make the nanoliter viscometer completely self-calibrating, robust, and easy to use. Several different microfabricated viscometers were tested using solutions with viscosities ranging from 1 to 5 cP, a range relevant to biological fluids (urine, blood, blood plasma, etc.). Blood plasma samples collected from patients with the symptoms of hyperviscosity syndrome were tested on the nanoliter capillary viscometer to an accuracy of 3%. Such self-calibrating nanoliter viscometers may have widespread applications in chemical, biological, and medical laboratories as well as in personal health care.

  14. Challenges of biological sample preparation for SIMS imaging of elements and molecules at subcellular resolution

    Energy Technology Data Exchange (ETDEWEB)

    Chandra, Subhash [Cornell SIMS Laboratory, Department of Earth and Atmospheric Sciences, Snee Hall, Cornell University, Ithaca, NY 14853 (United States)], E-mail:


    Secondary ion mass spectrometry (SIMS) based imaging techniques capable of subcellular resolution characterization of elements and molecules are becoming valuable tools in many areas of biology and medicine. Due to high vacuum requirements of SIMS, the live cells cannot be analyzed directly in the instrument. The sample preparation, therefore, plays a critical role in preserving the native chemical composition for SIMS analysis. This work focuses on the evaluation of frozen-hydrated and frozen freeze-dried sample preparations for SIMS studies of cultured cells with a CAMECA IMS-3f dynamic SIMS ion microscope instrument capable of producing SIMS images with a spatial resolution of 500 nm. The sandwich freeze-fracture method was used for fracturing the cells. The complimentary fracture planes in the plasma membrane were characterized by field-emission secondary electron microscopy (FESEM) in the frozen-hydrated state. The cells fractured at the dorsal surface were used for SIMS analysis. The frozen-hydrated SIMS analysis of individual cells under dynamic primary ion beam (O{sub 2}{sup +}) revealed local secondary ion signal enhancements correlated with the water image signals of {sup 19}(H{sub 3}O){sup +}. A preferential removal of water from the frozen cell matrix in the Z-axis was also observed. These complications render the frozen-hydrated sample type less desirable for subcellular dynamic SIMS studies. The freeze-drying of frozen-hydrated cells, either inside the instrument or externally in a freeze-drier, allowed SIMS imaging of subcellular chemical composition. Morphological evaluations of fractured freeze-dried cells with SEM and confocal laser scanning microscopy (CLSM) revealed well-preserved mitochondria, Golgi apparatus, and stress fibers. SIMS analysis of fractured freeze-dried cells revealed well-preserved chemical composition of even the most highly diffusible ions like K{sup +} and Na{sup +} in physiologically relevant concentrations. The high K

  15. Sample preparation strategies for food and biological samples prior to nanoparticle detection and imaging

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Löschner, Katrin


    fractionation (AFFF, or AF4) coupled on-line to various detectors including static and dynamic light scattering (LS), UV or fluorescence (FL) spectroscopies and ICP-MS have proven useful and powerful [1, 2, 3]. Furthermore, additional information obtained by an imaging method such as transmission electron...... microscopy (TEM) proved to be necessary for trouble shooting of results obtained from AFFF-LS-ICP-MS. Aqueous and enzymatic extraction strategies were tested for thorough sample preparation aiming at degrading the sample matrix and to liberate the AgNPs from chicken meat into liquid suspension. The resulting...

  16. Preparation of carbon-nitride bulk samples in the presence of seed carbon-nitride films

    Energy Technology Data Exchange (ETDEWEB)

    Kim, J. I. [Korea University of Technology and Education, Chonan (Korea, Republic of); Zorov, N. B. [Moscow State University, Moscow (Russian Federation)


    A procedure was developed for preparing bulk carbon-nitride crystals from polymeric alpha-C{sub 3}N{sub 4.2} at high pressure and high temperature in the presence of seeds of crystalline carbon-nitride films prepared by using a high-voltage discharge plasma combined with pulsed laser ablation of a graphite target. The samples were evaluated by using X-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, Auger electron spectroscopy (AES), secondary-ion mass spectrometry (SIMS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Notably, XPS studies of the film composition before and after thermobaric treatments demonstrated that the nitrogen composition in the alpha-C{sub 3}N{sub 4.2} material, which initially contained more than 58 % nitrogen, decreased during the annealing process and reached a common, stable composition of approx 45 %. The thermobaric experiments were performed at 10 - 77 kbar and 350 - 1200 .deg. C.

  17. Plasma chemical reduction of model corrosion brass layers prepared in soil (United States)

    Radkova, Lucie; Mikova, Petra; Prikryl, Radek; Krcma, Frantisek


    The brass plates of (50 × 10 × 1) mm3 were prepared with model corrosion layer because the real archaeological artifacts could be damaged during the method optimization. Samples corroded naturally more than 2 years in the soil. Excavated samples were treated in the low pressure (150 Pa) quartz glass plasma reactor (90 cm long and 9.5 cm in diameter) which was surrounded by two external copper electrodes supplied by radio-frequency generator (13.56 MHz). The experiments were carried out in a hydrogen-argon gas mixture at mass flows of 30 sccm for hydrogen and 20 sccm for argon for 90 min. The plasma power was 100, 200, 300 and 400 W in continuous and pulsed mode. Maximum sample temperature was set at 120 °C. The whole process was monitored by optical emission spectroscopy and the obtained data were used to calculate the relative intensity of OH radicals and rotational temperature. The results showed that the higher power had the greater maximum intensity of the OH radicals and rapidly degraded the corrosion layer. Corrosion layer was not completely removed during the reduction, but due to the reactions which occur in the plasma corrosion layer became brittle and after plasma chemical treatment can be removed easily. Finally, the SEM-EDX analysis of the surface composition confirmed removal of chlorine and oxygen from the corrosion products layers. Contribution to the topical issue "6th Central European Symposium on Plasma Chemistry (CESPC-6)", edited by Nicolas Gherardi, Ester Marotta and Cristina Paradisi

  18. Automated processing of whole blood samples into microliter aliquots of plasma



    A rotor that accepts and automatically processes a bulk aliquot of a single blood sample into multiple aliquots of plasma has been designed and built. The rotor consists of a central processing unit, which includes a disk containing eight precision-bore capillaries. By varying the internal diameters of the capillaries, aliquot volumes ranging 1 to 10 μl can be prepared. In practice, an unmeasured volume of blood is placed in a centre well, and, as the rotor begins to spin, is moved radially i...

  19. Preparation of Biological Samples Containing Metoprolol and Bisoprolol for Applying Methods for Quantitative Analysis

    Directory of Open Access Journals (Sweden)

    Corina Mahu Ştefania


    Full Text Available Arterial hypertension is a complex disease with many serious complications, representing a leading cause of mortality. Selective beta-blockers such as metoprolol and bisoprolol are frequently used in the management of hypertension. Numerous analytical methods have been developed for the determination of these substances in biological fluids, such as liquid chromatography coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, high performance liquid chromatography. Due to the complex composition of biological fluids a biological sample pre-treatment before the use of the method for quantitative determination is required in order to remove proteins and potential interferences. The most commonly used methods for processing biological samples containing metoprolol and bisoprolol were identified through a thorough literature search using PubMed, ScienceDirect, and Willey Journals databases. Articles published between years 2005-2015 were reviewed. Protein precipitation, liquid-liquid extraction and solid phase extraction are the main techniques for the extraction of these drugs from plasma, serum, whole blood and urine samples. In addition, numerous other techniques have been developed for the preparation of biological samples, such as dispersive liquid-liquid microextraction, carrier-mediated liquid phase microextraction, hollow fiber-protected liquid phase microextraction, on-line molecularly imprinted solid phase extraction. The analysis of metoprolol and bisoprolol in human plasma, urine and other biological fluids provides important information in clinical and toxicological trials, thus requiring the application of appropriate extraction techniques for the detection of these antihypertensive substances at nanogram and picogram levels.

  20. Characterization of Green-Emitting Translucent Zinc Oxide Ceramics Prepared Via Spark Plasma Sintering

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Mei [University of California; DeVito, David M [ORNL; Howe, Jane Y [ORNL; Yang, Xiaocheng [West Virginia University; Giles, Nancy C. [Air Force Institute of Technology; Neal, John S [ORNL; Munir, Zuhair [University of California


    Translucent, green-emitting zinc oxide (ZnO) bodies, 19 mm in diameter and 0.72 mm in thickness, have been prepared via spark plasma sintering method. The consolidation of ZnO powders was investigated over the temperature range of 550-1050 C and the pressure range of 55-530 MPa. Samples sintered at temperatures >850 C and pressures of {approx}120 MPa were translucent and had densities of {approx}100%. Samples sintered at 950 C and 130 MPa showed a higher maximum transmittance than the samples sintered at higher or lower temperatures or pressures, with an excellent in-line transmission of 70% in the IR region around 2330 nm. The dense ZnO ceramics exhibited a strong green emission and a weak ultraviolet emission, and the relative intensity of the green emission increased with increasing sintering temperature.

  1. Microstructure and mechanical strength of near- and sub-micrometre grain size copper prepared by spark plasma sintering

    DEFF Research Database (Denmark)

    Zhu, K. N.; Godfrey, A.; Hansen, Niels


    Spark plasma sintering (SPS) has been used to prepare fully dense samples of copper in a fully recrystallized condition with grain sizes in the near- and sub-micrometre regime. Two synthesis routes have been investigated to achieve grain size control: (i) SPS at different temperatures from 800 to...... been probed using hardness measurements and tensile testing, revealing an enhanced strength for samples with grain sizes less than ≈ 1 μm....

  2. Preparation and Characterization of Plasma Cu Surface Modified Stainless Steel

    Institute of Scientific and Technical Information of China (English)

    ZHANG Xiangyu; TANG Bin; FAN Ailan; MA Yong; TIAN Linhai


    Cu modified layer was prepared on the surface of AISI304 stainless steel by plasma surface alloying technique.The effects of processing parameters on the thickness,surface topography,microstructure and chemical composition of Cu modified layer were characterized using glow discharge optical emission spectroscopy (GDOES),scanning electron microscopy (SEM) and X-ray diffraction (XRD).The experimental results show that the surface modified layer is a duplex layer (deposited + diffused layer) with thickness of about 26 μm under the optimum process parameters.The modified layer is mainly composed of a mixture of Cu and expanded austenite phase.The ball-on-disk results show that the modified layer possesses low friction coefficients (0.25) and excellent wear resistance (wear volume 0.005× 109 μm3).The Cu modified layer is very effective in killing the bacteria S.aureus.Meanwhile,no viable S.aureus is found after 3 h (100% killed) by contact with the Cu alloyed surface.

  3. Chimeric External Control to Quantify Cell Free DNA in Plasma Samples by Real Time PCR (United States)

    Eini, Maryam; Behzad-Behbahani, Abbas; Takhshid, Mohammad Ali; Ramezani, Amin; Rafiei Dehbidi, Gholam Reza; Okhovat, Mohammad Ali; Farhadi, Ali; Alavi, Parniyan


    Background: DNA isolation procedure can significantly influence the quantification of DNA by real time PCR specially when cell free DNA (cfDNA) is the subject. To assess the extraction efficiency, linearity of the extraction yield, presence of co-purified inhibitors and to avoid problems with fragment size relevant to cfDNA, development of appropriate External DNA Control (EDC) is challenging. Using non-human chimeric nucleotide sequences, an EDC was developed for standardization of qPCR for monitoring stability of cfDNA concentration in blood samples over time. Methods: A0 DNA fragment of 167 bp chimeric sequence of parvovirus B19 and pBHA designated as EDC fragment was designed. To determine the impact of different factors during DNA extraction processing on quantification of cfDNA, blood samples were collected from normal subjects and divided into aliquots with and without specific treatment. In time intervals, the plasma samples were isolated. The amplicon of 167 bp EDC fragment in final concentration of 1.1 pg/500 μl was added to each plasma sample and total DNA was extracted by an in house method. Relative and absolute quantification real time PCR was performed to quantify both EDC fragment and cfDNA in extracted samples. Results: Comparison of real time PCR threshold cycle (Ct) for cfDNA fragment in tubes with and without specific treatment indicated a decrease in untreated tubes. In contrast, the threshold cycle was constant for EDC fragment in treated and untreated tubes, indicating the difference in Ct values of the cfDNA is because of specific treatments that were made on them. Conclusions: Spiking of DNA fragment size relevant to cfDNA into the plasma sample can be useful to minimize the bias due to sample preparation and extraction processing. Therefore, it is highly recommended that standard external DNA control be employed for the extraction and quantification of cfDNA for accurate data analysis. PMID:27141267

  4. Effect of sample preparation on charged impurities in graphene substrates (United States)

    Burson, K. M.; Dean, C. R.; Watanabe, K.; Taniguchi, T.; Hone, J.; Kim, P.; Cullen, W. G.; Fuhrer, M. S.


    The mobility of graphene as fabricated on SiO2 has been found to vary widely depending on sample preparation conditions. Additionally, graphene mobility on SiO2 appears to be limited to ~20,000 cm2/Vs, likely due to charged impurities in the substrate. Here we present a study of the effect of fabrication procedures on substrate charged impurity density (nimp) utilizing ultrahigh-vacuum Kelvin probe force microscopy. We conclude that even minimal SEM exposure, as from e-beam lithography, induces an increased impurity density, while heating reduces the number of charges for sample substrates which already exhibit a higher impurity density. We measure both SiO2 and h-BN and find that all nimp values observed for SiO2 are higher than those observed for h-BN; this is consistent with the observed improvement in mobility for graphene devices fabricated on h-BN over those fabricated on SiO2 substrates. This work was supported by the US ONR MURI program, and the University of Maryland NSF-MRSEC under Grant No. DMR 05-20471.

  5. Miniaturized sample preparation method for determination of amphetamines in urine. (United States)

    Nishida, Manami; Namera, Akira; Yashiki, Mikio; Kimura, Kojiro


    A simple and miniaturized sample preparation method for determination of amphetamines in urine was developed using on-column derivatization and gas chromatography-mass spectrometry (GC-MS). Urine was directly applied to the extraction column that was pre-packed with Extrelut and sodium carbonate. Amphetamine (AP) and methamphetamine (MA) in urine were adsorbed on the surface of Extrelut. AP and MA were then converted to a free base and derivatized to N-propoxycarbonyl derivatives using propylchloroformate on the column. Pentadeuterated MA was used as an internal standard. The recoveries of AP and MA from urine were 100 and 102%, respectively. The calibration curves showed linearity in the range of 0.50-50 microg/mL for AP and MA in urine. When urine samples containing two different concentrations (0.50 and 5.0 microg/mL) of AP and MA were determined, the intra-day and inter-day coefficients of variation were 1.4-7.7%. This method was applied to 14 medico-legal cases of MA intoxication. The results were compared and a good agreement was obtained with a HPLC method.

  6. Ultrasound: a subexploited tool for sample preparation in metabolomics. (United States)

    Luque de Castro, M D; Delgado-Povedano, M M


    Metabolomics, one of the most recently emerged "omics", has taken advantage of ultrasound (US) to improve sample preparation (SP) steps. The metabolomics-US assisted SP step binomial has experienced a dissimilar development that has depended on the area (vegetal or animal) and the SP step. Thus, vegetal metabolomics and US assisted leaching has received the greater attention (encompassing subdisciplines such as metallomics, xenometabolomics and, mainly, lipidomics), but also liquid-liquid extraction and (bio)chemical reactions in metabolomics have taken advantage of US energy. Also clinical and animal samples have benefited from US assisted SP in metabolomics studies but in a lesser extension. The main effects of US have been shortening of the time required for the given step, and/or increase of its efficiency or availability for automation; nevertheless, attention paid to potential degradation caused by US has been scant or nil. Achievements and weak points of the metabolomics-US assisted SP step binomial are discussed and possible solutions to the present shortcomings are exposed. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Automated acoustic matrix deposition for MALDI sample preparation. (United States)

    Aerni, Hans-Rudolf; Cornett, Dale S; Caprioli, Richard M


    Novel high-throughput sample preparation strategies for MALDI imaging mass spectrometry (IMS) and profiling are presented. An acoustic reagent multispotter was developed to provide improved reproducibility for depositing matrix onto a sample surface, for example, such as a tissue section. The unique design of the acoustic droplet ejector and its optimization for depositing matrix solution are discussed. Since it does not contain a capillary or nozzle for fluid ejection, issues with clogging of these orifices are avoided. Automated matrix deposition provides better control of conditions affecting protein extraction and matrix crystallization with the ability to deposit matrix accurately onto small surface features. For tissue sections, matrix spots of 180-200 microm in diameter were obtained and a procedure is described for generating coordinate files readable by a mass spectrometer to permit automated profile acquisition. Mass spectral quality and reproducibility was found to be better than that obtained with manual pipet spotting. The instrument can also deposit matrix spots in a dense array pattern so that, after analysis in a mass spectrometer, two-dimensional ion images may be constructed. Example ion images from a mouse brain are presented.

  8. Preparation of carbon nanotubes with different morphology by microwave plasma enhanced chemical vapour deposition

    Energy Technology Data Exchange (ETDEWEB)

    Duraia, El-Shazly M. [Suez Canal University, Faculty of Science, Physics Department, Ismailia (Egypt); Al-Farabi Kazakh National University, 71 Al-Farabi av., 050038 Almaty (Kazakhstan); Institute of Physics and Technology, Ibragimov Street 11, 050032 Almaty (Kazakhstan); Mansurov, Zulkhair [Al-Farabi Kazakh National University, 71 Al-Farabi av., 050038 Almaty (Kazakhstan); Tokmoldin, S.Zh. [Institute of Physics and Technology, Ibragimov Street 11, 050032 Almaty (Kazakhstan)


    In this work we present a part of our results about the preparation of carbon nanotube with different morphologies by using microwave plasma enhanced chemical vapour deposition MPECVD. Well aligned, curly, carbon nanosheets, coiled carbon sheets and carbon microcoils have been prepared. We have investigated the effect of the different growth condition parameters such as the growth temperature, pressure and the hydrogen to methane flow rate ratio on the morphology of the carbon nanotubes. The results showed that there is a great dependence of the morphology of carbon nanotubes on these parameters. The yield of the carbon microcoils was high when the growth temperature was 700 C. There is a linear relation between the growth rate and the methane to hydrogen ratio. The effect of the gas pressure on the CNTs was also studied. Our samples were investigated by scanning electron microscope and Raman spectroscopy (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  9. Aqueous Plasma Pharmacy: Preparation Methods, Chemistry, and Therapeutic Applications (United States)

    Joslin, Jessica M.; McCall, James R.; Bzdek, Justin P.; Johnson, Derek C.; Hybertson, Brooks M.


    Plasma pharmacy is a subset of the broader field of plasma medicine. Although not strictly defined, the term aqueous plasma pharmacy (APP) is used to refer to the generation and distribution of reactive plasma-generated species in an aqueous solution followed by subsequent administration for therapeutic benefits. APP attempts to harness the therapeutic effects of plasma-generated oxidant species within aqueous solution in various applications, such as disinfectant solutions, cell proliferation related to wound healing, and cancer treatment. The subsequent use of plasma-generated solutions in the APP approach facilitates the delivery of reactive plasma species to internal locations within the body. Although significant efforts in the field of plasma medicine have concentrated on employing direct plasma plume exposure to cells or tissues, here we focus specifically on plasma discharge in aqueous solution to render the solution biologically active for subsequent application. Methods of plasma discharge in solution are reviewed, along with aqueous plasma chemistry and the applications for APP. The future of the field also is discussed regarding necessary research efforts that will enable commercialization for clinical deployment. PMID:28428835

  10. Spectrochemical analysis of powdered biological samples using transversely excited atmospheric carbon dioxide laser plasma excitation (United States)

    Zivkovic, Sanja; Momcilovic, Milos; Staicu, Angela; Mutic, Jelena; Trtica, Milan; Savovic, Jelena


    The aim of this study was to develop a simple laser induced breakdown spectroscopy (LIBS) method for quantitative elemental analysis of powdered biological materials based on laboratory prepared calibration samples. The analysis was done using ungated single pulse LIBS in ambient air at atmospheric pressure. Transversely-Excited Atmospheric pressure (TEA) CO2 laser was used as an energy source for plasma generation on samples. The material used for the analysis was a blue-green alga Spirulina, widely used in food and pharmaceutical industries and also in a few biotechnological applications. To demonstrate the analytical potential of this particular LIBS system the obtained spectra were compared to the spectra obtained using a commercial LIBS system based on pulsed Nd:YAG laser. A single sample of known concentration was used to estimate detection limits for Ba, Ca, Fe, Mg, Mn, Si and Sr and compare detection power of these two LIBS systems. TEA CO2 laser based LIBS was also applied for quantitative analysis of the elements in powder Spirulina samples. Analytical curves for Ba, Fe, Mg, Mn and Sr were constructed using laboratory produced matrix-matched calibration samples. Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used as the reference technique for elemental quantification, and reasonably well agreement between ICP and LIBS data was obtained. Results confirm that, in respect to its sensitivity and precision, TEA CO2 laser based LIBS can be successfully applied for quantitative analysis of macro and micro-elements in algal samples. The fact that nearly all classes of materials can be prepared as powders implies that the proposed method could be easily extended to a quantitative analysis of different kinds of materials, organic, biological or inorganic.

  11. Design and Demonstration of a Material-Plasma Exposure Target Station for Neutron Irradiated Samples

    Energy Technology Data Exchange (ETDEWEB)

    Rapp, Juergen [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Aaron, A. M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bell, Gary L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Burgess, Thomas W. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ellis, Ronald James [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Giuliano, D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Howard, R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Kiggans, James O. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Lessard, Timothy L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ohriner, Evan Keith [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Perkins, Dale E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Varma, Venugopal Koikal [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)


    -state heat fluxes of 5–20 MW/m2 and ion fluxes up to 1024 m-2s-1. Since PFCs will have to withstand neutron irradiation displacement damage up to 50 dpa, the target station design must accommodate radioactive specimens (materials to be irradiated in HFIR or at SNS) to enable investigations of the impact of neutron damage on materials. Therefore, the system will have to be able to install and extract irradiated specimens using equipment and methods to avoid sample modification, control contamination, and minimize worker dose. Included in the design considerations will be an assessment of all the steps between neutron irradiation and post-exposure materials examination/characterization, as well as an evaluation of the facility hazard categorization. In particular, the factors associated with the acquisition of radioactive specimens and their preparation, transportation, experimental configuration at the plasma-specimen interface, post-plasma-exposure sample handling, and specimen preparation will be evaluated. Neutronics calculations to determine the dose rates of the samples were carried out for a large number of potential plasma-facing materials.



    Itagaki, K.; Lemieux, G.


    Since most commonly used sample preparation methods for ice dielectric studies involve rather heavy mechanical straining, the effects of straining were studied and compared with more strain-free sample preparation methods.

  13. Sample preparation issues in NMR-based plant metabolomics: optimisation for Vitis wood samples. (United States)

    Halabalaki, Maria; Bertrand, Samuel; Stefanou, Anna; Gindro, Katia; Kostidis, Sarantos; Mikros, Emmanuel; Skaltsounis, Leandros A; Wolfender, Jean-Luc


    Nuclear magnetic resonance (NMR) is one of the most commonly used analytical techniques in plant metabolomics. Although this technique is very reproducible and simple to implement, sample preparation procedures have a great impact on the quality of the metabolomics data. Investigation of different sample preparation methods and establishment of an optimised protocol for untargeted NMR-based metabolomics of Vitis vinifera L. wood samples. Wood samples from two different cultivars of V. vinifera with well-defined phenotypes (Gamaret and 2091) were selected as reference materials. Different extraction solvents (successively, dichloromethane, methanol and water, as well as ethyl acetate and 7:3 methanol-water (v/v)) and deuterated solvents (methanol-d4, 7:3 chloroform-d-methanol-d4 (v/v), dimethylsulphoxide-d6 and 9:1 dimethylsulphoxide-d6-water-d2 (v/v)) were evaluated for NMR acquisition, and the spectral quality was compared. The optimal extract concentration, chemical shift stability and peak area repeatability were also investigated. Ethyl acetate was found to be the most satisfactory solvent for the extraction of all representative chemical classes of secondary metabolites in V. vinifera wood. The optimal concentration of dried extract was 10 mg/mL and 7:3 chloroform-d-methanol-d4 (v/v) was the most suitable solvent system for NMR analysis. Multivariate data analysis was used to estimate the biological variation and clustering between different cultivars. Close attention should be paid to all required procedures before NMR analysis, especially to the selection of an extraction solvent and a deuterated solvent system to perform an extensive metabolomic survey of the specific matrix. Copyright © 2014 John Wiley & Sons, Ltd.

  14. A standardized research protocol for platelet- rich plasma (PRP preparation in rats

    Directory of Open Access Journals (Sweden)

    Michel Reis Messora


    Full Text Available Introduction: The urgent need for studies using standardized protocols to evaluate the real biological effects of PRP has been emphasized by several authors. Objective: The purpose of this study was to standardize a methodology for autologous Platelet-Rich Plasma (PRP preparation in rats. Material and methods: Twenty-four, 5 to 6-month-old, male rats, weighing 450 to 500 g were used. After general anesthesia, 3.15 ml of blood was collected from each animal, via cannulation of the jugular vein. A standardized technique of double centrifugation was used to prepare PRP. PRP samples and peripheral blood platelets were then manually counted using a Neubauer chamber. Student’s t-test was used to compare the differences between the number of platelets in peripheral blood and PRP samples (p < 0.05. In addition, PRP and peripheral blood smears were stained to see platelets’ morphology. Results: All surgical procedures were well tolerated by the animals and they were healthy during the entire experimental period. PRP samples showed higher significantly platelet concentrations than peripheral blood samples (2,677,583 and 683,680 respectively. Conclusion: Within the limits of this study, it can be concluded that the method used produced autologous PRP with appropriated platelet quantity and quality, in rats.

  15. Dynamic Fracture Toughness of TaC/CNTs/SiC CMCs Prepared by Spark Plasma Sintering

    Directory of Open Access Journals (Sweden)

    Qiaoyun Xie


    Full Text Available This study focuses on the fracture toughness of TaC and carbon nanotubes (CNTs reinforced SiC ceramic matrix composites (CMCs, prepared by spark plasma sintering (SPS technique. A high densification of 98.4% was achieved under the sintering parameter of 133°C/min, 1800°C, and 90 MPa pressure. Vickers indentation was employed to measure the indentation toughness on the polished surface of ceramic samples, SEM was applied to directly observe the crack propagation after indentation, and split Hopkinson pressure bar (SHPB was developed to determine the dynamic fracture toughness within the ceramic samples subjected to an impact in a three-point bending configuration.

  16. Preparation of Ti3SiC2 with Aluminum by Means of Spark Plasma Sintering

    Institute of Scientific and Technical Information of China (English)


    Polycrystalline bulk Ti3SiC2 material with a high purity and density was fabricated by spark plasma sintering from the elemental powder mixture with starting composition of Ti3Si1-xAlxC2,where x=0.05-0.2.X-ray diffraction patterns and scanning electron microscopy photographs of the fully dense samples show that a proper addition of aluminum promotes the formation,and accelerates the crystal growth rate of Ti3SiC2,consequently results in a high purity of the prepared samples.The synthesized Ti3SiC2 is in plane-shape with a size of about 10-25μm in the elongated dimension.Solid solution of aluminum decreases the thermal stability of Ti3SiC2,and lowers the temperature of Ti3SiC2 decomposeing to be 1300 ℃.

  17. Characterization of doped hydrogenated nanocrystalline silicon films prepared by plasma enhanced chemical vapour deposition

    Institute of Scientific and Technical Information of China (English)

    Wang Jin-Liang; Wu Er-Xing


    The B-and P-doped hydrogenated nanocrystalline silicon films (nc-Si:H) are prepared by plasma-enhanced chemical vapour deposition (PECVD) .The microstructures of doped nc-Si:H films are carefully and systematically char acterized by using high resolution electron microscopy (HREM) ,Raman scattering,x-ray diffraction (XRD) ,Auger electron spectroscopy (AES) ,and resonant nucleus reaction (RNR) .The results show that as the doping concentration of PH3 increases,the average grain size (d) tends to decrease and the crystalline volume percentage (Xc) increases simultaneously.For the B-doped samples,as the doping concentration of B2H6 increases,no obvious change in the value of d is observed,but the value of Xc is found to decrease.This is especially apparent in the case of heavy B2H6 doped samples,where the films change from nanocrystalline to amorphous.

  18. Preparation of thermal barrier coatings by ultrasonic plasma spraying

    Institute of Scientific and Technical Information of China (English)

    WEN Xiong-wei; LI Lu-ming; ZHANG Hua-tang; HAO Hong-wei; LU Zhi-qing


    Modulated plasma arc not only can heat the powder, but also can excite ultrasonic of different frequencies and different powers. The principles and characters of the plasma arc-excited ultrasonic were described, and the ultrasonic plasma spraying was compared with normal plasma spraying. Zirconia thermal barrier coatings (TBCs) were fabricated with two kinds of method. The TBCs were studied by the optical microscope observation, SEM observation and bonding strength experiment. The results show that suitable ultrasonic changes the performance and microstructure of TBCs in evidence. And the mechanism of ultrasonic influencing the TBCs was also discussed.

  19. Cell proliferation on modified DLC thin films prepared by plasma enhanced chemical vapor deposition. (United States)

    Stoica, Adrian; Manakhov, Anton; Polčák, Josef; Ondračka, Pavel; Buršíková, Vilma; Zajíčková, Renata; Medalová, Jiřina; Zajíčková, Lenka


    Recently, diamondlike carbon (DLC) thin films have gained interest for biological applications, such as hip and dental prostheses or heart valves and coronary stents, thanks to their high strength and stability. However, the biocompatibility of the DLC is still questionable due to its low wettability and possible mechanical failure (delamination). In this work, DLC:N:O and DLC: SiOx thin films were comparatively investigated with respect to cell proliferation. Thin DLC films with an addition of N, O, and Si were prepared by plasma enhanced CVD from mixtures of methane, hydrogen, and hexamethyldisiloxane. The films were optically characterized by infrared spectroscopy and ellipsometry in UV-visible spectrum. The thickness and the optical properties were obtained from the ellipsometric measurements. Atomic composition of the films was determined by Rutherford backscattering spectroscopy combined with elastic recoil detection analysis and by x-ray photoelectron spectroscopy. The mechanical properties of the films were studied by depth sensing indentation technique. The number of cells that proliferate on the surface of the prepared DLC films and on control culture dishes were compared and correlated with the properties of as-deposited and aged films. The authors found that the level of cell proliferation on the coated dishes was high, comparable to the untreated (control) samples. The prepared DLC films were stable and no decrease of the biocompatibility was observed for the samples aged at ambient conditions.

  20. The preparation of albumin as a biological drug from human plasma by fiber filtration

    Directory of Open Access Journals (Sweden)

    Mousavi Hosseini K


    Full Text Available "nBackground: In recent years, consumption of whole-blood for the treatment of patients has decreased but use of biological plasma-derived medicines such as albumin, immunoglobulin and coagulation factors have increased instead. Paying attention to albumin molecular structure is important for its isolation from human plasma. Albumin is a single-chain protein consisting of about 585 amino acids and a molecular weight of 66500 Daltons. Albumin is a stable molecule and it is spherical in shape. There are different methods for human albumin preparation. Considering the large consumption of this biological drug in clinical settings, methods with fewer steps in production line are of big advantage in saving time and manufacturing more products."n "nMethods: In this project, we prepared human albumin using hollow fiber cartridges in order to omit the rework on fraction V+VI. Human albumin is usually produced by the application of cold ethanol method, where albumin is obtained from fraction V by doing a rework on fraction V+VI to separate fraction V."n "nResults: In the current work, human albumin was prepared from fraction V+VI by the help of hollow fiber cartridges. With a concentration of 20%, the obtained albumin had 96.5% of monomer and 3.5% of polymer and polymer aggregate."n "nConclusion: Comparing the obtained human albumin with a number of commercial human albumin samples by the use of SDS-page, the results were satisfactory regarding the 3.5 percent polymer and aggregate rate for the prepared albumin.

  1. Analysis of bioethanol samples through Inductively Coupled Plasma Mass Spectrometry with a total sample consumption system (United States)

    Sánchez, Carlos; Lienemann, Charles-Philippe; Todolí, Jose-Luis


    Bioethanol real samples have been directly analyzed through ICP-MS by means of the so called High Temperature Torch Integrated Sample Introduction System (hTISIS). Because bioethanol samples may contain water, experiments have been carried out in order to determine the effect of ethanol concentration on the ICP-MS response. The ethanol content studied went from 0 to 50%, because higher alcohol concentrations led to carbon deposits on the ICP-MS interface. The spectrometer default spray chamber (double pass) equipped with a glass concentric pneumatic micronebulizer has been taken as the reference system. Two flow regimes have been evaluated: continuous sample aspiration at 25 μL min- 1 and 5 μL air-segmented sample injection. hTISIS temperature has been shown to be critical, in fact ICP-MS sensitivity increased with this variable up to 100-200 °C depending on the solution tested. Higher chamber temperatures led to either a drop in signal or a plateau. Compared with the reference system, the hTISIS improved the sensitivities by a factor included within the 4 to 8 range while average detection limits were 6 times lower for the latter device. Regarding the influence of the ethanol concentration on sensitivity, it has been observed that an increase in the temperature was not enough to eliminate the interferences. It was also necessary to modify the torch position with respect to the ICP-MS interface to overcome them. This fact was likely due to the different extent of ion plasma radial diffusion encountered as a function of the matrix when working at high chamber temperatures. When the torch was moved 1 mm plasma down axis, ethanolic and aqueous solutions provided statistically equal sensitivities. A preconcentration procedure has been applied in order to validate the methodology. It has been found that, under optimum conditions from the point of view of matrix effects, recoveries for spiked samples were close to 100%. Furthermore, analytical concentrations for real

  2. Non-thermal plasma as preparative technique to evaluate olive oil adulteration. (United States)

    Van Durme, Jim; Vandamme, Jeroen


    In recent years adulteration of pure extra virgin olive oil (EVOO) with other types of vegetable oils has become an important issue. In this study, non-thermal plasma (NTP) is investigated as an innovative preparative analytical technique enabling classification of adulterated olive oil from an ascertained authentic batch of olive oil in a more sensitive manner. Non-thermal plasma discharges are a source of highly oxidative species such as singlet oxygen, and atomic oxygen. It was assumed that NTP-induced oxidation triggers unique lipid oxidation mechanisms depending on the specific composition of the oil matrix and minor constituents. In this work EVOO samples were adulterated with sunflower oil (1-3%) and submitted to NTP treatment. Results showed that while untreated samples could not be classified from the authentic olive oil reference, NTP treatments of 60min (Ar/O2 0.1%) on the oil batches resulted in the formation of a unique set of secondary volatile lipid oxidation products enabling classification of adulterated oil samples.

  3. Design and Demonstration of a Material-Plasma Exposure Target Station for Neutron Irradiated Samples

    Energy Technology Data Exchange (ETDEWEB)

    Rapp, Juergen [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Aaron, A. M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bell, Gary L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Burgess, Thomas W. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ellis, Ronald James [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Giuliano, D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Howard, R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Kiggans, James O. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Lessard, Timothy L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ohriner, Evan Keith [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Perkins, Dale E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Varma, Venugopal Koikal [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)


    -state heat fluxes of 5–20 MW/m2 and ion fluxes up to 1024 m-2s-1. Since PFCs will have to withstand neutron irradiation displacement damage up to 50 dpa, the target station design must accommodate radioactive specimens (materials to be irradiated in HFIR or at SNS) to enable investigations of the impact of neutron damage on materials. Therefore, the system will have to be able to install and extract irradiated specimens using equipment and methods to avoid sample modification, control contamination, and minimize worker dose. Included in the design considerations will be an assessment of all the steps between neutron irradiation and post-exposure materials examination/characterization, as well as an evaluation of the facility hazard categorization. In particular, the factors associated with the acquisition of radioactive specimens and their preparation, transportation, experimental configuration at the plasma-specimen interface, post-plasma-exposure sample handling, and specimen preparation will be evaluated.

  4. Monte Carlo Sampling of Negative-temperature Plasma States

    Energy Technology Data Exchange (ETDEWEB)

    John A. Krommes; Sharadini Rath


    A Monte Carlo procedure is used to generate N-particle configurations compatible with two-temperature canonical equilibria in two dimensions, with particular attention to nonlinear plasma gyrokinetics. An unusual feature of the problem is the importance of a nontrivial probability density function R0(PHI), the probability of realizing a set {Phi} of Fourier amplitudes associated with an ensemble of uniformly distributed, independent particles. This quantity arises because the equilibrium distribution is specified in terms of {Phi}, whereas the sampling procedure naturally produces particles states gamma; {Phi} and gamma are related via a gyrokinetic Poisson equation, highly nonlinear in its dependence on gamma. Expansion and asymptotic methods are used to calculate R0(PHI) analytically; excellent agreement is found between the large-N asymptotic result and a direct numerical calculation. The algorithm is tested by successfully generating a variety of states of both positive and negative temperature, including ones in which either the longest- or shortest-wavelength modes are excited to relatively very large amplitudes.

  5. Structure and strength of aluminum with sub-micrometer/micrometer grain size prepared by spark plasma sintering

    DEFF Research Database (Denmark)

    Le, G.M.; Godfrey, A.; Hansen, Niels


    A spark plasma sintering (SPS) technique has been applied to prepare fully dense Al samples from Al powder. By applying a sintering temperature of 600°C and a loading pressure of 50MPa, fully recrystallized samples of nearly 100% density with average grain sizes of 5.2μm, 1.3μm and 0.8μm have been...... the initial powder particle size. The SPS samples show higher strength than Al samples with an identical grain size prepared using thermo-mechanical processing, and a better strength-ductility combination, with the 1.3μm grain size sample showing a yield strength (σ0.2%) of 140MPa and a uniform elongation...

  6. Preparation of silver-carbon nanotubes composites with plasma electrochemistry (United States)

    Hoefft, Oliver; Lohmann, Lara; Olschewski, Mark; Endres, Frank


    Plasma electrochemistry is a powerful tool to generate free nanoparticles in aqueous solutions and especially in ionic liquids (ILs). Due to their very low vapour pressure, ionic liquids can be employed under vacuum conditions as fluid substrates or solvents. Thus, ionic liquids are well suitable electrolytes for plasma electrochemical processes delivering stable and homogeneous plasmas. We have shown that free copper and germanium nanoparticles can be obtained in ILs by applying a plasma as a mechanically contact-free electrode. Here we present our results using an argon plasma for the electrochemical synthesis of silver on pure and pre-treated multiwall carbon nanotubes (MWCNTs) in 1-ethyl-3-methylimidazolium dicyanamide. For the pre-treatment of the MWCNTS we have used a dielectric barrier discharge plasma (DBD) at atmospheric pressure. For the untreated MWCNTs we have found a formation of free silver nanoparticles between, on and in the vicinity of the carbon nanotubes. In case of the plasma treated MWCNTs a silver-carbon nanotubes composite is formed. Thus, the treatment of the MWCNTs obviously has a great influence on the deposit. Therefore we additionally have investigated the influence of the DBD on the chemical composition of the MWCNTs surface with X-Ray Photoelectron Spectroscopy.

  7. A comparison of sample preparation strategies for biological tissues and subsequent trace element analysis using LA-ICP-MS. (United States)

    Bonta, Maximilian; Török, Szilvia; Hegedus, Balazs; Döme, Balazs; Limbeck, Andreas


    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is one of the most commonly applied methods for lateral trace element distribution analysis in medical studies. Many improvements of the technique regarding quantification and achievable lateral resolution have been achieved in the last years. Nevertheless, sample preparation is also of major importance and the optimal sample preparation strategy still has not been defined. While conventional histology knows a number of sample pre-treatment strategies, little is known about the effect of these approaches on the lateral distributions of elements and/or their quantities in tissues. The technique of formalin fixation and paraffin embedding (FFPE) has emerged as the gold standard in tissue preparation. However, the potential use for elemental distribution studies is questionable due to a large number of sample preparation steps. In this work, LA-ICP-MS was used to examine the applicability of the FFPE sample preparation approach for elemental distribution studies. Qualitative elemental distributions as well as quantitative concentrations in cryo-cut tissues as well as FFPE samples were compared. Results showed that some metals (especially Na and K) are severely affected by the FFPE process, whereas others (e.g., Mn, Ni) are less influenced. Based on these results, a general recommendation can be given: FFPE samples are completely unsuitable for the analysis of alkaline metals. When analyzing transition metals, FFPE samples can give comparable results to snap-frozen tissues. Graphical abstract Sample preparation strategies for biological tissues are compared with regard to the elemental distributions and average trace element concentrations.

  8. Oxygen bomb combustion of biological samples for inductively coupled plasma optical emission spectrometry (United States)

    Souza, Gilberto B.; Carrilho, Elma Neide V. M.; Oliveira, Camila V.; Nogueira, Ana Rita A.; Nóbrega, Joaquim A.


    A rapid sample preparation method is proposed for decomposition of milk powder, corn bran, bovine and fish tissues, containing certified contents of the analytes. The procedure involves sample combustion in a commercial stainless steel oxygen bomb operating at 25 bar. Most of the samples were decomposed within 5 min. Diluted nitric acid or water-soluble tertiary amines 10% v/v were used as absorption solutions. Calcium, Cu, K, Mg, Na, P, S and Zn were recovered with the bomb washings and determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Ethanol mixed with paraffin was used as a combustion aid to allow complete combustion. A cooling step prior releasing of the bomb valve was employed to increase the efficiency of sample combustion. Iodine was also determined in milk samples spiked with potassium iodide to evaluate the volatilization and collection of iodine in amine CFA-C medium and the feasibility of its determination by ICP-OES with axial view configuration. Most of the element recoveries in the samples were between 91 and 105% and the certified and found contents exhibited a fair agreement at a 95% confidence level.

  9. Determination of trace elements in refined gold samples by inductively coupled plasma atomic emission spectrometry

    Directory of Open Access Journals (Sweden)

    Steharnik Mirjana


    Full Text Available This paper presents a method for determination the trace contents of silver, copper, iron, palladium, zinc and platinum in refined gold samples. Simultaneous inductively coupled plasma atomic emission spectrometer with radial torch position and cross flow nebulizer was used for determination. In order to compare the different calibration strategies, two sets of calibration standards were prepared. The first set was based on matrix matched calibration standards and the second was prepared without the addition of matrix material. Detection limits for matrix matching calibrations were higher for some elements than those without matrix matching. In addition, the internal standardization method was applied and experiments indicated that indium was the best option as internal standard. The obtained results for gold sample by matrix matching and matrix free calibrations were compared with the obtained results by standard addition method. The accuracy of the methods was tested performing recovery test. Recoveries for spiked sample were in the range of 90-115 %. The accuracy of the methods was also tested by analysis of certified reference material of high pure goldAuGHP1. The best results were achieved by matrix free calibration and standard addition method using indium as internal standard at wavelength of 230 nm. [Projekat Ministarstva nauke Republike Srbije, br. 34024: Development of Technologies for Recycling of Precious, Rare and Associated Metals from Solid Waste in Serbia to High Purity Products

  10. Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Taflik, Ticiane; Antes, Fabiane G.; Paniz, Jose N.G.; Flores, Erico M.M.; Dressler, Valderi L., E-mail: [Departamento de Quimica, Universidade Federal de Santa Maria, RS (Brazil); Duarte, Fabio A. [Escola de Quimica e Alimentos, Universidade Federal do Rio Grande, Rio Grande, RS (Brazil); Flores, Eder L.M. [Coordenacao de Engenharia de Alimentos, Universidade Tecnologica Federal do Parana, Medianeira, PR (Brazil)


    Pyrohydrolysis was employed for mineral supplements decomposition prior to F, Br and I determination. Fluoride determination was carried out by potentiometry using a fluoride-ion selective electrode, whereas Br and I were determined by inductively coupled plasma mass spectrometry. The main parameters that influence on pyrohydrolysis were investigated. After evaluation, the following conditions were established: reactor temperature of 1000 deg C during 10 min; sample plus accelerator mass ratio of 1 + 5 and carrier gas (air) flow rate of 200 mL min{sup -1} . The accuracy of the proposed method was evaluated by analyte recovery tests and analysis of certified reference materials of phosphate rock and soil. Commercial mineral supplement samples were analyzed. The limits of quantification were 16, 0.3 and 0.07 {mu}g g{sup -1} for F, Br and I, respectively. By using a relatively simple and low cost pyrohydrolysis system up to 5 samples can be processed per hour. The developed sample preparation procedure can be routinely employed for F, Br and I determination in mineral supplements. (author)

  11. [Indications for fresh frozen plasma: evaluation of virus inactivating preparations]. (United States)

    Pindur, G; Kiesewetter, H; Seyfert, U T; Wenzel, E


    When no specific factor concentrate is available fresh-frozen plasma (FFP) is indicated in the treatment of clinically relevant hemorrhagic diathesis. These disorders include congenital factor V and XI deficiencies, multiple factor defects, as disseminated intravascular coagulation and severe liver disease, and patients receiving massive transfusions, when bleeding occurs and severe abnormalities on coagulation testing are evident. FFP is beneficial when used with plasma exchange in thrombotic thrombocytopenic purpura and related disorders. Various virucidal treatments including solvent-detergent (SD), photoactivated dyes (methylene blue) or pasteurization have been evolved to improve virus safety of human plasma. More extensive studies to demonstrate efficient virus inactivation in plasma have been performed with SD compared to other methods. On the other hand, the use of single-donor FFP in methylene blue treatment is possibly superior to pooled plasma which is processed according to the SD procedure. Pasteurization enables the inactivation not only of lipid-enveloped but also of non-lipid-enveloped viruses. Virucidal treatment of plasma may cause alterations in clotting factors, fibrinolysis and protease inhibitors; however, the currently achieved recovery of procoagulant activities is approximately comparable with that found in untreated FFP. The toxicity of virucidal additives is reported to be negligible since manufacturing includes a removal procedure (SD) or comparably low amounts (methylene blue) are used in inactivation treatment.

  12. Amphiphilic mediated sample preparation for micro-flow cytometry

    Energy Technology Data Exchange (ETDEWEB)

    Clague, David S. (Livermore, CA); Wheeler, Elizabeth K. (Livermore, CA); Lee, Abraham P. (Irvine, CA)


    A flow cytometer includes a flow cell for detecting the sample, an oil phase in the flow cell, a water phase in the flow cell, an oil-water interface between the oil phase and the water phase, a detector for detecting the sample at the oil-water interface, and a hydrophobic unit operatively connected to the sample. The hydrophobic unit is attached to the sample. The sample and the hydrophobic unit are placed in an oil and water combination. The sample is detected at the interface between the oil phase and the water phase.

  13. Final LDRD report : development of sample preparation methods for ChIPMA-based imaging mass spectrometry of tissue samples.

    Energy Technology Data Exchange (ETDEWEB)

    Maharrey, Sean P.; Highley, Aaron M.; Behrens, Richard, Jr.; Wiese-Smith, Deneille


    The objective of this short-term LDRD project was to acquire the tools needed to use our chemical imaging precision mass analyzer (ChIPMA) instrument to analyze tissue samples. This effort was an outgrowth of discussions with oncologists on the need to find the cellular origin of signals in mass spectra of serum samples, which provide biomarkers for ovarian cancer. The ultimate goal would be to collect chemical images of biopsy samples allowing the chemical images of diseased and nondiseased sections of a sample to be compared. The equipment needed to prepare tissue samples have been acquired and built. This equipment includes an cyro-ultramicrotome for preparing thin sections of samples and a coating unit. The coating unit uses an electrospray system to deposit small droplets of a UV-photo absorbing compound on the surface of the tissue samples. Both units are operational. The tissue sample must be coated with the organic compound to enable matrix assisted laser desorption/ionization (MALDI) and matrix enhanced secondary ion mass spectrometry (ME-SIMS) measurements with the ChIPMA instrument Initial plans to test the sample preparation using human tissue samples required development of administrative procedures beyond the scope of this LDRD. Hence, it was decided to make two types of measurements: (1) Testing the spatial resolution of ME-SIMS by preparing a substrate coated with a mixture of an organic matrix and a bio standard and etching a defined pattern in the coating using a liquid metal ion beam, and (2) preparing and imaging C. elegans worms. Difficulties arose in sectioning the C. elegans for analysis and funds and time to overcome these difficulties were not available in this project. The facilities are now available for preparing biological samples for analysis with the ChIPMA instrument. Some further investment of time and resources in sample preparation should make this a useful tool for chemical imaging applications.

  14. Preparation of ion-exchange thin film using plasma processes. Plasma process wo mochiita ion kokansei usumaku no sakusei

    Energy Technology Data Exchange (ETDEWEB)

    Ogumi, Z.; Uchimoto, Y. (Kyoto University, Kyoto (Japan). Faculty of Engineering)


    The present report describes a study which aims at preparation of a new functional film by plasma polymerization. For this purpose, 4-vinylpyridine monomer is plasma-polymerized to obtain a thin film, which is quaternarized with 1-bromopropane to produce an anion exchange thin film, which is laminated on the surface of a cation-exchange film to make a mono-valent cation perm-selective film. In plasma-polymerization, the relations of polymerizing pressure, as parameter, to the deposition rate of the polymerizerd film and the characteristics of compound were clarified. In preparing the anion-exchange thin film, the preparation of uniform ultrathin films with no pinhole was attempted. For this purpose, the transference number of Cl[sup -] was measured so as to confirm that Cl[sup -] is uniformly distributed and fixed cation groups are distributed uniformly in the film. The perm-selective film exhibited a high mono-valent cation perm-selectivity while its film resistance was increased. This increase is found to be broken down to the resistance of the plasma-polymerization film layer and the resistance of the film interface. The latter arises from the implantation of nitrogen-cointaining species in the plasma onto the surface of the cation exchange film. 26 refs., 10 figs., 2 tabs.

  15. Protein adsorption on gradient surfaces on polyethylene prepared in a shielded gas plasma

    NARCIS (Netherlands)

    Spijker, Hendrikje; Bos, Roelof; van Oeveren, Willem; de Vries, Jacob; Busscher, Hendrik


    In this study, a new and simple method is described to prepare wettability gradients on polymers by means of glow discharge in a partly shielded argon plasma. The surface characteristics of thus prepared gradients on low density polyethylene were determined by contact angle measurements and electron

  16. Analysis of liquid samples using dried-droplet laser ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Do, Trong-Mui; Hsieh, Hui-Fang; Chang, Wei-Ciang [Department of Biomedical Engineering and Environmental Sciences, National Tsing Hua University, Hsinchu, 30013 Taiwan (China); Chang, E.-E. [Department of Biochemistry, Taipei Medical University, Taipei City, 11031 Taiwan (China); Wang, Chu-Fang, E-mail: [Department of Biomedical Engineering and Environmental Sciences, National Tsing Hua University, Hsinchu, 30013 Taiwan (China); Institute of Nuclear Engineering and Science, National Tsing Hua University, Hsinchu 30013, Taiwan (China)


    In this study we developed a dried-droplet method for laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method provides accurate and precise results when building calibration curves and determining elements of interest in real liquid samples. After placing just 1 {mu}L of a liquid standard solution or a real sample onto the filter surface and then converting the solution into a very small, thin dry spot, the sample could be applied as an analytical subject for LA. To demonstrate the feasibility of this proposed method, we used LA-ICP-MS and conventional ICP-MS to determine the levels of 13 elements (Li, V, Mn, Co, Ni, Cu, Zn, As, Mo, Cd, Sb, Tl, and Pb) in five water samples. The correlation coefficients obtained from the various calibration curves ranged from 0.9920 ({sup 205}Tl) to 0.9998 ({sup 51}V), sufficient to allow the determination of a wide range of elements in the samples. We also investigated the effects of Methylene Blue (MB) and the NaCl concentration on the elemental analyses. MB could be used as an indicator during the ablation process; its presence in the samples only negligibly influenced the intensities of the signals of most of the tested elements. Notably, high NaCl contents led to signal suppression for some of the elements. In comparison with the established sample introduction by nebulization, our developed technique abrogates the need for time-consuming sample preparation and reduces the possibility of sample contamination.

  17. Selecting Sample Preparation Workflows for Mass Spectrometry-Based Proteomic and Phosphoproteomic Analysis of Patient Samples with Acute Myeloid Leukemia

    Directory of Open Access Journals (Sweden)

    Maria Hernandez-Valladares


    Full Text Available Global mass spectrometry (MS-based proteomic and phosphoproteomic studies of acute myeloid leukemia (AML biomarkers represent a powerful strategy to identify and confirm proteins and their phosphorylated modifications that could be applied in diagnosis and prognosis, as a support for individual treatment regimens and selection of patients for bone marrow transplant. MS-based studies require optimal and reproducible workflows that allow a satisfactory coverage of the proteome and its modifications. Preparation of samples for global MS analysis is a crucial step and it usually requires method testing, tuning and optimization. Different proteomic workflows that have been used to prepare AML patient samples for global MS analysis usually include a standard protein in-solution digestion procedure with a urea-based lysis buffer. The enrichment of phosphopeptides from AML patient samples has previously been carried out either with immobilized metal affinity chromatography (IMAC or metal oxide affinity chromatography (MOAC. We have recently tested several methods of sample preparation for MS analysis of the AML proteome and phosphoproteome and introduced filter-aided sample preparation (FASP as a superior methodology for the sensitive and reproducible generation of peptides from patient samples. FASP-prepared peptides can be further fractionated or IMAC-enriched for proteome or phosphoproteome analyses. Herein, we will review both in-solution and FASP-based sample preparation workflows and encourage the use of the latter for the highest protein and phosphorylation coverage and reproducibility.

  18. Sample preparation for the analysis of complex carbohydrates by multicapillary gel electrophoresis with light-emitting diode induced fluorescence detection. (United States)

    Olajos, Marcell; Hajós, Péter; Bonn, Guenther K; Guttman, András


    This paper evaluates various sample preparation methods for multicapillary gel electrophoresis based glycan analysis to support electrokinetic injection. First the removal of excess derivatization reagent is discussed. Although the Sephadex G10 filled multiscreen 96-well filter plate and Sephadex G10 filled pipet tips enabled increased analysis sensitivity, polyamide DPA-6S pipet tips worked particularly well. In this latter case an automated liquid handling system was used to increase purification throughput, necessary to feed the multicapillary electrophoresis unit. Problems associated with the high glucose content of such biological samples as normal human plasma were solved by applying ultrafiltration. Finally, a volatile buffer system was developed for exoglycosidase-based carbohydrate analysis.


    Institute of Scientific and Technical Information of China (English)


    CuO/γ-Al2O3 catalysts were prepared by plasma treatment and conventional impregnation methods. The catalytic combustion of two kinds of volatile organic compounds (VOCs), toluene and benzene, were carried out over these CuO/γ-Al2O3 catalysts. The surface properties of these catalysts were characterized by X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The experimental results showed that in catalytic combustion the activity of the CuO/γ-Al2O3 catalyst prepared via plasma was much higher than that of the CuO/γ-Al2O3 catalyst prepared by conventional impregnation method. XRD results showed that an enhanced dispersion had been achieved with the plasma treatment. SEM results indicated that the size became much smaller and the surface became more uniform with the plasma treatment.

  20. Using Exclusion-Based Sample Preparation (ESP to Reduce Viral Load Assay Cost.

    Directory of Open Access Journals (Sweden)

    Scott M Berry

    Full Text Available Viral load (VL measurements are critical to the proper management of HIV in developing countries. However, access to VL assays is limited by the high cost and complexity of existing assays. While there is a need for low cost VL assays, performance must not be compromised. Thus, new assays must be validated on metrics of limit of detection (LOD, accuracy, and dynamic range. Patient plasma samples from the Joint Clinical Research Centre in Uganda were de-identified and measured using both an existing VL assay (Abbott RealTime HIV-1 and our assay, which combines low cost reagents with a simplified method of RNA isolation termed Exclusion-Based Sample Preparation (ESP.71 patient samples with VLs ranging from 3,000,000 copies/mL were used to compare the two methods. We demonstrated equivalent LOD (~50 copies/mL and high accuracy (average difference between methods of 0.08 log, R2 = 0.97. Using expenditures from this trial, we estimate that the cost of the reagents and consumables for this assay to be approximately $5 USD. As cost is a significant barrier to implementation of VL testing, we anticipate that our assay will enhance access to this critical monitoring test in developing countries.

  1. Using Exclusion-Based Sample Preparation (ESP) to Reduce Viral Load Assay Cost. (United States)

    Berry, Scott M; Pezzi, Hannah M; Williams, Eram D; Loeb, Jennifer M; Guckenberger, David J; Lavanway, Alex J; Puchalski, Alice A; Kityo, Cissy M; Mugyenyi, Peter N; Graziano, Franklin M; Beebe, David J


    Viral load (VL) measurements are critical to the proper management of HIV in developing countries. However, access to VL assays is limited by the high cost and complexity of existing assays. While there is a need for low cost VL assays, performance must not be compromised. Thus, new assays must be validated on metrics of limit of detection (LOD), accuracy, and dynamic range. Patient plasma samples from the Joint Clinical Research Centre in Uganda were de-identified and measured using both an existing VL assay (Abbott RealTime HIV-1) and our assay, which combines low cost reagents with a simplified method of RNA isolation termed Exclusion-Based Sample Preparation (ESP).71 patient samples with VLs ranging from 3,000,000 copies/mL were used to compare the two methods. We demonstrated equivalent LOD (~50 copies/mL) and high accuracy (average difference between methods of 0.08 log, R2 = 0.97). Using expenditures from this trial, we estimate that the cost of the reagents and consumables for this assay to be approximately $5 USD. As cost is a significant barrier to implementation of VL testing, we anticipate that our assay will enhance access to this critical monitoring test in developing countries.

  2. Porous membrane ultrafiltration-A novel method for enrichment of the active compounds from micro-plasma samples (United States)

    Liu, Qingshan; Yin, Xiaoying; Sha, Biying; You, Jingjing


    To enrich the active compounds from plasma samples, a novel and simple method has been developed using a porous membrane envelope based on the ultrafiltration technique combining with high-performance liquid chromatography. The ultrafiltration device is a sealed porous membrane envelope prepared with a polypropylene sheet to effectively separate the active small molecules and large biomolecules, and a sample carrier is held inside the envelope to load plasma samples. The enrichment of hyperoside and isoquercitrin from rat plasma was used as an example. Significant factors of this method, such as membrane types, the desorption solvent, and the desorption time were optimized for the ultrafiltration method. Under the optimal conditions, correlation coefficients of 0.999 and 0.998 were obtained for hyperoside and isoquercitrin, respectively, with a linear range between 0.5 and 100 μg/mL. The absolute extraction recoveries from 83.2% to 86.8% were achieved. The detection limits of the method for hyperoside and isoquercitrin were 0.22 and 0.20 μg/mL, respectively. Compared with protein precipitation, solid-phase extraction and commercial ultrafiltration membrane methods, our proposed method demonstrates lower detection limits and lower cost for extraction. Also, it consumes less plasma samples and is found to be applicable to biological samples.

  3. Studies on the preparation and plasma spherodization of yttrium aluminosilicate glass microspheres for their potential application in liver brachytherapy (United States)

    Sreekumar, K. P.; Saxena, S. K.; Kumar, Yogendra; Thiyagarajan, T. K.; Dash, Ashutosh; Ananthapadmanabhan, P. V.; Venkatesh, Meera


    Plasma spheroidization exploits the high temperature and high enthalpy available in the thermal plasma jet to melt irregularly shaped powder particles and quench them to get dense spherical particles. Plasma spheroidization is a versatile process and can be applied to metals, ceramics, alloys and composites to obtain fine spherical powders. Radioactive microspheres incorporated with high energetic beta emitting radioisotopes have been reported to be useful in the palliative treatment of liver cancer. These powders are to be prepared in closer range of near spherical morphology in the size range 20-35 microns. Inactive glass samples were prepared by heating the pre-calculated amount of glass forming ingredients in a recrystallized alumina crucible. The glass was formed by keeping the glass forming ingredients at 1700°C for a period of three hours to form a homogeneous melt. After cooling, the glass was recovered from the crucible by crushing and was subsequently powdered mechanically with the help of mortar and pestle. This powder was used as the feed stock for plasma spheroidization using an indigenously developed 40 kW plasma spray system. Experiments were carried out at various operating parameters. The operating parameters were optimised to get spheroidised particles. The powder was sieved to get the required size range before irradiation.

  4. Studies on the preparation and plasma spherodization of yttrium aluminosilicate glass microspheres for their potential application in liver brachytherapy

    Energy Technology Data Exchange (ETDEWEB)

    Sreekumar, K P; Saxena, S K; Kumar, Yogendra; Thiyagarajan, T K; Dash, Ashutosh; Ananthapadmanabhan, P V; Venkatesh, Meera, E-mail: [Laser and Plasma Technology Division, Radiopharmaceuticals Division, Bhabha Atomic Research Centre, Trombay, Mumbai - 400 085 (India)


    Plasma spheroidization exploits the high temperature and high enthalpy available in the thermal plasma jet to melt irregularly shaped powder particles and quench them to get dense spherical particles. Plasma spheroidization is a versatile process and can be applied to metals, ceramics, alloys and composites to obtain fine spherical powders. Radioactive microspheres incorporated with high energetic beta emitting radioisotopes have been reported to be useful in the palliative treatment of liver cancer. These powders are to be prepared in closer range of near spherical morphology in the size range 20-35 microns. Inactive glass samples were prepared by heating the pre-calculated amount of glass forming ingredients in a recrystallized alumina crucible. The glass was formed by keeping the glass forming ingredients at 1700{sup 0}C for a period of three hours to form a homogeneous melt. After cooling, the glass was recovered from the crucible by crushing and was subsequently powdered mechanically with the help of mortar and pestle. This powder was used as the feed stock for plasma spheroidization using an indigenously developed 40 kW plasma spray system. Experiments were carried out at various operating parameters. The operating parameters were optimised to get spheroidised particles. The powder was sieved to get the required size range before irradiation.

  5. [Deep frozen fresh plasma in blood component therapy: preparation--quality control--indications]. (United States)

    Koerner, K; Stampe, D; Kubanek, B


    Fresh frozen plasma is prepared within 6 hrs after collection in a double bag system. A second centrifugation at 4600 x g is necessary to obtain a platelet poor plasma. A special bag freezing system fitted to a conventional cryostat and cooled with ethanol to -50 degrees C was developed to reach the required cooling rate. It is possible to freeze 25 plasma bags simultaneously within 30 min in this new apparatus. Fresh frozen plasma prepared in this manner contains all coagulation factors and inhibitors with almost normal activities. Freezing at -40 degrees C in the air, prolonged storage of the starting material, or insufficient cooling of the frozen product deteriorate its quality. The influence of these variables with the discussed in detail. Indications of fresh frozen plasma, especially for dilution- and posttraumatic consumption coagulopathy as well as liver disease, are presented.

  6. LacaScore: a novel plasma sample quality control tool based on ascorbic acid and lactic acid levels. (United States)

    Trezzi, Jean-Pierre; Bulla, Alexandre; Bellora, Camille; Rose, Michael; Lescuyer, Pierre; Kiehntopf, Michael; Hiller, Karsten; Betsou, Fay

    Metabolome analysis is complicated by the continuous dynamic changes of metabolites in vivo and ex vivo. One of the main challenges in metabolomics is the robustness and reproducibility of results, partially driven by pre-analytical variations. The objective of this study was to analyse the impact of pre-centrifugation time and temperature, and to determine a quality control marker in plasma samples. Plasma metabolites were measured by gas chromatography-mass spectrometry (GC-MS) and analysed with the MetaboliteDetector software. The metabolites, which were the most labile to pre-analytical variations, were further measured by enzymatic assays. A score was calculated for their use as quality control markers. The pre-centrifugation temperature was shown to be critical in the stability of plasma samples and had a significant impact on metabolite concentration profiles. In contrast, pre-centrifugation delay had only a minor impact. Based on the results of this study, whole blood should be kept on wet ice and centrifuged within maximum 3 h as a prerequisite for preparing EDTA plasma samples fit for the purpose of metabolome analysis. We have established a novel blood sample quality control marker, the LacaScore, based on the ascorbic acid to lactic acid ratio in plasma, which can be used as an indicator of the blood pre-centrifugation conditions, and hence the suitability of the sample for metabolome analyses. This method can be applied in research institutes and biobanks, enabling assessment of the quality of their plasma sample collections.

  7. Characterization of Plasma Polymerized Hexamethyldisiloxane Films Prepared by Arc Discharge

    NARCIS (Netherlands)

    Lazauskas, A.; Baltrusaitis, Jonas; Grigaliunas, V.; Jucius, D; Guobiene, A.; Prosycevas, I.; Narmontas, P.


    Herein, we present a simple method for fabricating plasma polymerized hexamethyldisiloxane films (pp-HMDSO) possessing superhydrophobic characteristics via arc discharge. The pp-HMDSO films were deposited on a soda–lime–silica float glass using HMDSO monomer vapor as a precursor. A detailed surface

  8. Preview of the NASA NNWG NDE Sample Preparation Handbook (United States)


    This viewgraph presents a step-by-step how-to fabrication documentation of every kind of sample that is fabricated for MSFC by UA Huntsville, including photos and illustrations. The tabulation of what kind of samples are being fabricated for what NDE method, detailed instructions/documentation of the inclusion/creation of defects, detailed specifications for materials, processes, and equipment, case histories and/or experiences with the different fabrication methods and defect inclusion techniques, discussion of pitfalls and difficulties associated with sample fabrication and defect inclusion techniques, and a discussion of why certain fabrication techniques are needed as related to the specific NDE methods are included in this presentation.

  9. Sample Preparation (SS): SE45_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available tration of 15 ng µl-1 for each 1-µl injection. After 5-min centrifugation at 15,1...0 mg/ml in pyridine) was added to the sample. After 24 h of derivatization at room temperature, the sample w...µl of methoxyamine hydrochloride (20 mg ml-1 in pyridine) were added to the sample. After 24 h of derivatiza...f MSTFA at 37°C with shaking. After silylation 30 µl of n-heptane were added. All derivatization steps were

  10. Controls to validate plasma samples for cell free DNA quantification

    DEFF Research Database (Denmark)

    Pallisgaard, Niels; Spindler, Karen-Lise Garm; Andersen, Rikke Fredslund;


    Recent research has focused on the utility of cell free DNA (cfDNA) in serum and plasma for clinical application, especially in oncology. The literature holds promise of cfDNA as a valuable tumour marker to be used for treatment selection, monitoring and follow-up. The results, however, are diver...

  11. Nanostructured Sulfide Composite Coating Prepared by Atmospheric Plasma Spraying

    Institute of Scientific and Technical Information of China (English)



    Nanostructured FeS-SiC coating was deposited by atmospheric plasma spraying (APS). The microstructure and phase composition of the coating were characterized with SEM and XRD, respectively. In addition, the size distribution of the reconstituted powders and the porosity of the coating have been measured. It was found that the reconstitiuted powers with sizes in the range of 20 to 80 μm had excellent flowability and were suitable for plasma spraying process. The assprayed FeS-SiC composite coating exhibited a bimodal distribution with small grains (30~80nm) and large grains (100~200nm). The coating was mainly composed of FeS and SiC, a small quantity of Fe1-x S and oxide were also found. The porosity of the coating was approximately 19 %.

  12. Sample Preparation (SS): SE55_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available 80℃ until analysis. The frozen tissues were homogenized in five volumes of 80% aqueous methanol containing 0...SE55_SS01 Metabolic profiling Collected sample tissues were weighed and stored at -

  13. Sample Preparation for Monolithic Refractories Part 1: Refractory Castables

    Institute of Scientific and Technical Information of China (English)

    Zhang Xiaohui; Peng Xigao


    @@ 1 Scope This standard specifies the definition and test methods of flowability of dense and insulating refractory castables,and moulding equipment,moulding methods,curing and drying conditions of castables samples.

  14. Sample Preparation (SS): SE52_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available Tokyo, Japan) using a mixer mill (MM 300, Retsch) with a zirconia bead for 6 min... at 20 Hz. Next, the samples were centrifuged at 15,000 g for 10 min and filtered (Ultrafree-MC filter, 0.2 μm; Mil...lipore, Bedford, MA, USA). The sample extracts were then applied to an HLB μElution plate (Waters, Mil

  15. Analysis of efficiency of the double- centrifugation protocol to prepare platelet rich plasma (PRP – an experimental study in rabbits

    Directory of Open Access Journals (Sweden)

    Michel Reis MESSORA


    Full Text Available Introduction and objective:The purpose of this study was to evaluatethe concentrations of platelets obtained from platelet rich plasma (PRP prepared according to the double-centrifugation protocol. Material and methods: Eight adult male rabbits (White New Zealand weighing 2.8 to 4 kg were used.After general anesthesia, 10 ml of blood were drawn from each animal via cardiac puncture. Each blood sample was centrifuged according to the protocol of Sonnleitner et al.(2000.The peripheral blood (total from each animal and the PRP samples platelets were counted manually. Data were submitted to statistical analysis.The normality of the data was confirmed and the Student’s t test was applied (p < 0.05.Results: PRP samples presented an average platele count significantly higher than that of peripheral blood.Conclusion Within the limits of this study, it was concluded that the double centrifugation protocol was adequate to prepare PRP .

  16. Particle Size and Pore Structure Characterization of Silver Nanoparticles Prepared by Confined Arc Plasma

    Directory of Open Access Journals (Sweden)

    Mingru Zhou


    Full Text Available In the protecting inert gas, silver nanoparticles were successfully prepared by confined arc plasma method. The particle size, microstructure, and morphology of the particles by this process were characterized via X-ray powder diffraction (XRD, transmission electron microscopy (TEM and the corresponding selected area electron diffraction (SAED. The N2 absorption-desorption isotherms of the samples were measured by using the static volumetric absorption analyzer, the pore structure of the sample was calculated by Barrett-Joyner-Halenda (BJH academic model, and the specific surface area was calculated from Brunauer-Emmett-Teller (BET adsorption equation. The experiment results indicate that the crystal structure of the samples is face-centered cubic (FCC structure the same as the bulk materials, the particle size distribution ranging from 5 to 65 nm, with an average particle size about 26 nm obtained by TEM and confirmed by XRD and BET results. The specific surface area is 23.81 m2/g, pore volumes are 0.09 cm3/g, and average pore diameter is 18.7 nm.

  17. Preparation of Crystallized Carbon Nitride Based on Microwave Plasma CVD

    National Research Council Canada - National Science Library

    Masatoshi INOUE; Yukihiro SAKAMOTO; Matsufumi TAKAYA


    ... on. To obtain this material, generally CH4 is used as a carbon source. Therefore, to make clear the effects of the reaction gas on the preparation of carbon nitride, we tried to use C2H4 as a carbon source instead of CH4...

  18. Development of Al2O3 electrospun fibers prepared by conventional sintering method or plasma assisted surface calcination (United States)

    Mudra, E.; Streckova, M.; Pavlinak, D.; Medvecka, V.; Kovacik, D.; Kovalcikova, A.; Zubko, P.; Girman, V.; Dankova, Z.; Koval, V.; Duzsa, J.


    In this paper, the electrospinning method was used for preparation of α-Al2O3 microfibers from PAN/Al(NO3)3 precursor solution. The precursor fibers were thermally treated by conventional method in furnace or low-temperature plasma induced surface sintering method in ambient air. The four different temperatures of PAN/Al(NO3)3 precursors were chosen for formation of α-Al2O3 phase by conventional sintering way according to the transition features observed in the TG/DSC analysis. In comparison, the low-temperature plasma treatment at atmospheric pressure was used as an alternative sintering method at the exposure times of 5, 10 and 30 min. FTIR analysis was used for evaluation of residual polymer after plasma induced calcination and for studying the mechanism of polymer degradation. The polycrystalline alumina fibers arranged with the nanoparticles was created continuously throughout the whole volume of the sample. On the other side the low temperature approach, high density of reactive species and high power density of plasma generated at atmospheric pressure by used plasma source allowed rapid removal of polymer in preference from the surface of fibers leading to the formation of composite ceramic/polymer fibers. This plasma induced sintering of PAN/Al(NO3)3 can have obvious importance in industrial applications where the ceramic character of surface with higher toughness of the fibers are required.

  19. Multiple stage MS in analysis of plasma, serum, urine and in vitro samples relevant to clinical and forensic toxicology. (United States)

    Meyer, Golo M; Maurer, Hans H; Meyer, Markus R


    This paper reviews MS approaches applied to metabolism studies, structure elucidation and qualitative or quantitative screening of drugs (of abuse) and/or their metabolites. Applications in clinical and forensic toxicology were included using blood plasma or serum, urine, in vitro samples, liquids, solids or plant material. Techniques covered are liquid chromatography coupled to low-resolution and high-resolution multiple stage mass analyzers. Only PubMed listed studies published in English between January 2008 and January 2015 were considered. Approaches are discussed focusing on sample preparation and mass spectral settings. Comments on advantages and limitations of these techniques complete the review.



    O'Geen, Henriette; Nicolet, Charles M.; Blahnik, Kim; Green, Roland; Farnham, Peggy J.


    A single ChIP sample does not provide enough DNA for hybridization to a genomic tiling array. A commonly used technique for amplifying the DNA obtained from ChIP assays is linker-mediated PCR (LMPCR). However, using this amplification method, we could not identify Oct4 binding sites on genomic tiling arrays representing 1% of the human genome (ENCODE arrays). In contrast, hybridization of a pool of 10 ChIP samples to the arrays produced reproducible binding patterns and low background signals...

  1. Quantitating morphological changes in biological samples during scanning electron microscopy sample preparation with correlative super-resolution microscopy. (United States)

    Zhang, Ying; Huang, Tao; Jorgens, Danielle M; Nickerson, Andrew; Lin, Li-Jung; Pelz, Joshua; Gray, Joe W; López, Claudia S; Nan, Xiaolin


    Sample preparation is critical to biological electron microscopy (EM), and there have been continuous efforts on optimizing the procedures to best preserve structures of interest in the sample. However, a quantitative characterization of the morphological changes associated with each step in EM sample preparation is currently lacking. Using correlative EM and superresolution microscopy (SRM), we have examined the effects of different drying methods as well as osmium tetroxide (OsO4) post-fixation on cell morphology during scanning electron microscopy (SEM) sample preparation. Here, SRM images of the sample acquired under hydrated conditions were used as a baseline for evaluating morphological changes as the sample went through SEM sample processing. We found that both chemical drying and critical point drying lead to a mild cellular boundary retraction of ~60 nm. Post-fixation by OsO4 causes at least 40 nm additional boundary retraction. We also found that coating coverslips with adhesion molecules such as fibronectin prior to cell plating helps reduce cell distortion from OsO4 post-fixation. These quantitative measurements offer useful information for identifying causes of cell distortions in SEM sample preparation and improving current procedures.

  2. Effects of blood sample handling procedures on measurable inflammatory markers in plasma, serum and dried blood spot samples

    DEFF Research Database (Denmark)

    Skogstrand, K.; Thorsen, P.; Vogel, I.


    of whole blood samples at low temperatures and rapid isolation of plasma and serum. Effects of different handling procedures for all markers studied are given. DBSS proved to be a robust and convenient way to handle samples for immunoassay analysis of inflammatory markers in whole blood Udgivelsesdato......The interests in monitoring inflammation by immunoassay determination of blood inflammatory markers call for information on the stability of these markers in relation to the handling of blood samples. The increasing use of stored biobank samples for such ventures that may have been collected...... and stored for other purposes, justifies the study hereof. Blood samples were stored for 0, 4, 24, and 48 h at 4 degrees C, room temperature (RT), and at 35 degrees C, respectively, before they were separated into serum or plasma and frozen. Dried blood spot samples (DBSS) were stored for 0, 1, 2, 3, 7...

  3. A needle extraction utilizing a molecularly imprinted-sol-gel xerogel for on-line microextraction of the lung cancer biomarker bilirubin from plasma and urine samples. (United States)

    Moein, Mohammad Mahdi; Jabbar, Dunia; Colmsjö, Anders; Abdel-Rehim, Mohamed


    In the present work, a needle trap utilizing a molecularly imprinted sol-gel xerogel was prepared for the on-line microextraction of bilirubin from plasma and urine samples. Each prepared needle could be used for approximately one hundred extractions before it was discarded. Imprinted and non-imprinted sol-gel xerogel were applied for the extraction of bilirubin from plasma and urine samples. The produced molecularly imprinted sol-gel xerogel polymer showed high binding capacity and fast adsorption/desorption kinetics for bilirubin in plasma and urine samples. The adsorption capacity of molecularly imprinted sol-gel xerogel polymer was approximately 60% higher than that of non-imprinted polymer. The effect of the conditioning, washing and elution solvents, pH, extraction time, adsorption capacity and imprinting factor were investigated. The limit of detection and the lower limit of quantification were set to 1.6 and 5nmolL(-1), respectively using plasma or urine samples. The standard calibration curves were obtained within the concentration range of 5-1000nmolL(-1) in both plasma and urine samples. The coefficients of determination values (R(2)) were ≥0.998 for all runs. The extraction recovery was approximately 80% for BR in the human plasma and urine samples.

  4. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.


    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  5. Microfluidic desalination. Capacitive deionization on chip for microfluidic sample preparation

    NARCIS (Netherlands)

    Roelofs, Susan Helena


    The main aim of the work described in this thesis is to implement the desalination technique capacitive deionization (CDI) on a microfluidic chip to improve the reproducibility in the analysis of biological samples for drug development. Secondly, microfluidic CDI allows for the in situ study of ion

  6. Microsystem strategies for sample preparation in biological detection.

    Energy Technology Data Exchange (ETDEWEB)

    James, Conrad D.; Galambos, Paul C.; Bennett, Dawn Jonita (University of Maryland Baltimore County, Baltimore, MD); Manginell, Monica; Okandan, Murat; Acrivos, Andreas (The City College of New York, NY); Brozik, Susan Marie; Khusid, Boris (New Jersey Institute of Technology, Newark, NJ)


    The objective of this LDRD was to develop microdevice strategies for dealing with samples to be examined in biological detection systems. This includes three sub-components: namely, microdevice fabrication, sample delivery to the microdevice, and sample processing within the microdevice. The first component of this work focused on utilizing Sandia's surface micromachining technology to fabricate small volume (nanoliter) fluidic systems for processing small quantities of biological samples. The next component was to develop interfaces for the surface-micromachined silicon devices. We partnered with Micronics, a commercial company, to produce fluidic manifolds for sample delivery to our silicon devices. Pressure testing was completed to examine the strength of the bond between the pressure-sensitive adhesive layer and the silicon chip. We are also pursuing several other methods, both in house and external, to develop polymer-based fluidic manifolds for packaging silicon-based microfluidic devices. The second component, sample processing, is divided into two sub-tasks: cell collection and cell lysis. Cell collection was achieved using dielectrophoresis, which employs AC fields to collect cells at energized microelectrodes, while rejecting non-cellular particles. Both live and dead Staph. aureus bacteria have been collected using RF frequency dielectrophoresis. Bacteria have been separated from polystyrene microspheres using frequency-shifting dielectrophoresis. Computational modeling was performed to optimize device separation performance, and to predict particle response to the dielectrophoretic traps. Cell lysis is continuing to be pursued using microactuators to mechanically disrupt cell membranes. Novel thermal actuators, which can generate larger forces than previously tested electrostatic actuators, have been incorporated with and tested with cell lysis devices. Significant cell membrane distortion has been observed, but more experiments need to be

  7. Preparation of Ultra-fine Aluminum Nitride in Thermal Plasma

    Institute of Scientific and Technical Information of China (English)

    漆继红; 罗义文; 印永祥; 代晓雁


    Ultra-fine aluminum nitride has been synthesized by the evaporation of aluminum powder at atmospheric-pressure nitrogen plasma in a hot-wall reactor. The average size of aluminum nitride particle is 0.11μm measured by scanning electric mirror (SEM), and the purity is at least over 90% evaluated by X-Ray diffraction (XRD). The conversion of Al powder to aluminum nitride is strongly depended on the injection of NH3. Typical experimental parameters such as the feed rate of raw material, the flow rate of ammonia and the position of injecting aluminum powder into the reactor are given.

  8. Accurate and precise plasma clearance measurement using four 99mTc-DTPA plasma samples over 4 h


    Wanasundara, Surajith N.; Wesolowski, Michal J.; Barnfield, Mark C.; Waller, Michael L.; Murray, Anthony W.; Burniston, Maria T.; Babyn, Paul S.; Wesolowski, Carl A.


    Objectives Glomerular filtration rate can be measured as the plasma clearance (CL) of a glomerular filtration rate marker despite body fluid disturbances using numerous, prolonged time samples. We desire a simplified technique without compromised accuracy and precision. Materials and methods We compared CL values derived from two plasma concentration curve area methods – (a) biexponential fitting [CL (E2)] and (b) Tikhonov adaptively regularized gamma variate fitting [CL (Tk-GV)] – for 4 vers...

  9. Effects of Sample Preparation on the Infrared Reflectance Spectra of Powders

    Energy Technology Data Exchange (ETDEWEB)

    Brauer, Carolyn S.; Johnson, Timothy J.; Myers, Tanya L.; Su, Yin-Fong; Blake, Thomas A.; Forland, Brenda M.


    While reflectance spectroscopy is a useful tool in identifying molecular compounds, laboratory measurement of solid (particularly powder) samples often is confounded by sample preparation methods. For example, both the packing density and surface roughness can have an effect on the quantitative reflectance spectra of powdered samples. Recent efforts in our group have focused on developing standard methods for measuring reflectance spectra that accounts for sample preparation, as well as other factors such as particle size and provenance. In this work, the effect of preparation method on sample reflectivity was investigated by measuring the directional-hemispherical spectra of samples that were hand-packed as well as pressed into pellets using an integrating sphere attached to a Fourier transform infrared spectrometer. The results show that the methods used to prepare the sample have a substantial effect on the measured reflectance spectra, as do other factors such as particle size.

  10. Titanium carbide/carbon composite nanofibers prepared by a plasma process

    Energy Technology Data Exchange (ETDEWEB)

    El Mel, A A; Gautron, E; Angleraud, B; Granier, A; Tessier, P Y [Universite de Nantes, CNRS, Institut des Materiaux Jean Rouxel, UMR 6502, 2 rue de la Houssiniere BP 32229-44322 Nantes cedex 3 (France); Choi, C H [Department of Mechanical Engineering, Stevens Institute of Technology, Hoboken, NJ 07030 (United States)


    The incorporation of metal or metal carbide nanoparticles into carbon nanofibers modifies their properties and enlarges their field of application. The purpose of this work is to report a new non-catalytic and easy method to prepare organized metal carbide-carbon composite nanofibers on nanopatterned silicon substrates prepared by laser interference lithography coupled with deep reactive ion etching. Titanium carbide-carbon composite nanofibers were grown on the top of the silicon lines parallel to the substrate by a hybrid plasma process combining physical vapor deposition and plasma enhanced chemical vapor deposition. The prepared nanofibers were analyzed by scanning electron microscopy, x-ray photoelectron spectroscopy, Raman spectroscopy and transmission electron microscopy. We demonstrate that the shape, microstructure and the chemical composition of the as-grown nanofibers can be tuned by changing the plasma conditions.

  11. Titanium carbide/carbon composite nanofibers prepared by a plasma process. (United States)

    El Mel, A A; Gautron, E; Choi, C H; Angleraud, B; Granier, A; Tessier, P Y


    The incorporation of metal or metal carbide nanoparticles into carbon nanofibers modifies their properties and enlarges their field of application. The purpose of this work is to report a new non-catalytic and easy method to prepare organized metal carbide-carbon composite nanofibers on nanopatterned silicon substrates prepared by laser interference lithography coupled with deep reactive ion etching. Titanium carbide-carbon composite nanofibers were grown on the top of the silicon lines parallel to the substrate by a hybrid plasma process combining physical vapor deposition and plasma enhanced chemical vapor deposition. The prepared nanofibers were analyzed by scanning electron microscopy, x-ray photoelectron spectroscopy, Raman spectroscopy and transmission electron microscopy. We demonstrate that the shape, microstructure and the chemical composition of the as-grown nanofibers can be tuned by changing the plasma conditions.

  12. Study on acetylene preparation from coal conversion directly by plasma

    Energy Technology Data Exchange (ETDEWEB)

    Bao, W.; Lu, Y.; Cao, Q.; Xie, K. [Taiyuan University of Technology, Taiyuan (China)


    To develop an innovative method for directly converting coal into an important chemical acetylene, arc plasma technology was applied to the direct conversion of coal. The powdered coal from Datong was injected into a hydrogen-enriched plasma reactor for pyrolysis. The results show that the coal conversion and the acetylene yield and the special energy consumption (SEC) of acetylene are decreased as coal feed rate is increased, but the concentration of acetylene in production gas is increased. The yield of acetylene is not obviously affected by the formation of CO in production gas. Since oxygen can compete with the active atomic carbon, therefore, the high content oxygen in coal is disadvantageous to the formation of acetylene. Under the experimental conditions selected, the coal conversion rate reach 38.42%, the concentration of acetylene in product gas is 9.30% and the selectivity of acetylene in hydrocarbon is above 70% when the coal fed is 5.0 g/s. 10 refs., 3 figs., 1 tab.

  13. Sample preparation and assay refinements for pathogen detection platforms (United States)

    Lim, Daniel V.; Kearns, Elizabeth A.; Leskinen, Stephaney D.; Magaña, Sonia; Stroot, Joyce M.; Hunter, Dawn M.; Schlemmer, Sarah M.


    Food-borne and waterborne microbial pathogens are a potential problem in biowarfare and public health. Such pathogens can affect the health, combat readiness, and effectiveness of the warfighter in a battlefield environment and present potential threats to the civilian population through intentional or natural contamination of food and water. Conventional procedures to detect and identify microbial pathogens in food, water, and other materials can take days to perform and may provide inconclusive information. Research at the University of South Florida's Advanced Biosensors Laboratory (ABL) focuses on development of sample processing procedures and biosensor-based assays for rapid detection of biothreat agents. Rapid processing methods, including use of an automated concentrator of microorganisms in water, have been developed for complex matrix samples including ground beef, apple juice, produce, potable water and recreational water, enabling such samples to be directly tested by biosensor assays for target analytes. Bacillus atrophaeus spores and other bacteria can be concentrated from potable and recreational water at low levels with a dead-end hollow-fiber ultrafiltration concentration system. Target bacteria recovered by these processing procedures can be identified by evanescent wave, fiber optic biosensors or other detection platforms. Fiber optic biosensor assays have been improved to include subsequent PCR analysis and viability determination of captured target bacteria using broth enrichment and/or ATP luminescence.

  14. Quantitative analysis of intermediately and infinitely thick samples with thin sample approach without sample preparation using confocal X-ray fluorescence

    CERN Document Server

    Sun, Xue-Peng; Sun, Tian-Xi; Peng, Song; Sun, Wei-Yuan; Li, Fang-Zuo; Jiang, Bo-Wen; Ma, Yong-Zhong; Ding, Xun-Liang


    In order to validate that the confocal X-ray fluorescence had potential applications in analyzing the intermediately and infinitely thick samples with thin sample approach without sample preparations, as an example, the confocal X-ray fluorescence based on polycapillary X-ray optics was used to analyze multi elements solutions.

  15. Plasma etching of polystyrene latex particles for the preparation of graphene oxide nanowalls

    Directory of Open Access Journals (Sweden)

    Bon Bittolo Silvia


    Full Text Available Graphene oxide nanowalls were prepared by casting a water dispersion of polystyrene latex particles onto a graphene oxide film followed by tetrafluoromethane plasma etching. Mild plasma etching conditions allow one to retain the oxygen functional groups on the graphene oxide nanowalls. It was found that the exposure to a xenon light source of such graphene oxide nanowalls coated with a gold thin film results in an increase of the electrical conductivity.

  16. Preparation of Hollow Spherical and Core/shell Structured Powders by Plasma Processing

    Institute of Scientific and Technical Information of China (English)

    ZHANG; Xiaofeng; ZHOU; Kesong; DENG; Changguang; SONG; Jinbing; ZHANG; Jifu; DONG; Shujuan


    Four types of hollow spherical micro- and nano-szied powders of ZrO2-7wt.%Y2O3(7YSZ), ZrO2-7wt.%Y2O3, Al2O3-13 wt.% TiO2(AT) and WC as well as one type of core/shell structured powder of ZrB2-30 wt.%Mo Si2 were prepared via plasma processing. In addition, the formation mechanisms of hollow spherical and core/shell structured powders prepared via plasma processing were also proposed.

  17. Global metabolite analysis of yeast: evaluation of sample preparation methods

    DEFF Research Database (Denmark)

    Villas-Bôas, Silas Granato; Højer-Pedersen, Jesper; Åkesson, Mats Fredrik;


    , which is the analysis of a large number of metabolites with very diverse chemical and physical properties. This work reports the leakage of intracellular metabolites observed during quenching yeast cells with cold methanol solution, the efficacy of six different methods for the extraction...... of intracellular metabolites, and the losses noticed during sample concentration by lyophilization and solvent evaporation. A more reliable procedure is suggested for quenching yeast cells with cold methanol solution, followed by extraction of intracellular metabolites by pure methanol. The method can be combined...

  18. Heat treatment process of new NdFeB magnet prepared by spark plasma sintering

    Institute of Scientific and Technical Information of China (English)

    李涛; 岳明; 张久兴; 王公平; 肖耀福; 王润


    In recent years, spark plasma sintering technique(SPS) has been a focus in the field of material preparation due to its advantages. SPS technique is first introduced for preparation of high quality NdFeB magnets. The effects of heat treatment process on the magnetic properties of SPS NdFeB magnet were investigated. Meanwhile, the effects of heat treatment process on the microstructure, tropism and dimensional precision of the SPS NdFeB magnets were also studied. The high quality NdFeB magnets with fine grains were prepared under proper heat treatment process. The results show that the magnetic properties of SPS NdFeB can be further improved through proper heat treatment process. Meanwhile, the experiment also demonstrates that it is feasible to prepare near-net-shape NdFeB magnets with fine grains and high magnetic property by spark plasma sintering.

  19. Current advances and strategies towards fully automated sample preparation for regulated LC-MS/MS bioanalysis. (United States)

    Zheng, Naiyu; Jiang, Hao; Zeng, Jianing


    Robotic liquid handlers (RLHs) have been widely used in automated sample preparation for liquid chromatography-tandem mass spectrometry (LC-MS/MS) bioanalysis. Automated sample preparation for regulated bioanalysis offers significantly higher assay efficiency, better data quality and potential bioanalytical cost-savings. For RLHs that are used for regulated bioanalysis, there are additional requirements, including 21 CFR Part 11 compliance, software validation, system qualification, calibration verification and proper maintenance. This article reviews recent advances in automated sample preparation for regulated bioanalysis in the last 5 years. Specifically, it covers the following aspects: regulated bioanalysis requirements, recent advances in automation hardware and software development, sample extraction workflow simplification, strategies towards fully automated sample extraction, and best practices in automated sample preparation for regulated bioanalysis.

  20. Electroluminescence and photoluminescence of conjugated polymer films prepared by plasma enhanced chemical vapor deposition of naphthalene

    CERN Document Server

    Rajabi, Mojtaaba; Firouzjah, Marzieh Abbasi; Hosseini, Seyed Iman; Shokri, Babak


    Polymer light-emitting devices were fabricated utilizing plasma polymerized thin films as emissive layers. These conjugated polymer films were prepared by RF Plasma Enhanced Chemical Vapor Deposition (PECVD) using naphthalene as monomer. The effect of different applied powers on the chemical structure and optical properties of the conjugated polymers was investigated. The fabricated devices with structure of ITO/PEDOT:PSS/ plasma polymerized Naphthalene/Alq3/Al showed broadband Electroluminescence (EL) emission peaks with center at 535-550 nm. Using different structural and optical tests, connection between polymers chemical structure and optical properties under different plasma powers has been studied. Fourier transform infrared (FTIR) and Raman spectroscopies confirmed that a conjugated polymer film with a 3-D cross-linked network was developed. By increasing the power, products tended to form as highly cross-linked polymer films. Photoluminescence (PL) spectra of plasma polymers showed different excimerc ...

  1. Structure and properties of nanocrystalline rare earth bulks prepared by spark plasma sintering

    Institute of Scientific and Technical Information of China (English)

    卢年端; 宋晓艳; 刘雪梅; 张久兴


    A series of rare earth bulks with the ultrafine nanocrystalline structure were prepared by applying an "oxygen-free" (an environmental oxygen concentration less than 0.5 ppm) in-situ synthesis system, where the inert-gas condensation was combined with the spark plasma sintering technology into an entirely closed system. The thermal and mechanical properties of the prepared ultrafine nanocrystalline bulks were characterized and compared with those of the raw polycrystalline bulks. It was found that the speci...

  2. Preparation of Al-SiC{sub p} composite coating by plasma thermal spray

    Energy Technology Data Exchange (ETDEWEB)

    Min, J.W. [Chungnam National University, Taejeon (Korea); Yoo, S.E. [Korea Automotive Technology Institute, Chonan (Korea); Kim, Y.J. [Sunmoon University, Asan (Korea); Kim, J.S.; Suhr, D.S. [Chungnam National University, Taejeon (Korea)


    Al-SiC{sub p} composite layer was prepared by plasma thermal spray on aluminum substrate using composite powder prepared by mechanical alloying. Mechanically alloyed powder was achieved after 24 h milling, which was used for thermal spray coating. The correlations between process conditions and thickness/porosity were analyzed, and increase of hardness was confirmed. The presence of Al-Si-C-O compound was detected by TEM analysis. (author). 16 refs., 6 tabs., 11 figs.

  3. Status report of AMS sample preparation laboratory at GADAM Centre, Gliwice, Poland

    Energy Technology Data Exchange (ETDEWEB)

    Piotrowska, N., E-mail: [GADAM Centre of Excellence, Department of Radioisotopes, Institute of Physics, Silesian University of Technology, Gliwice (Poland)


    The laboratory for {sup 14}C AMS sample preparation in the Gliwice Radiocarbon Laboratory has gradually evolved since its start in 1999 to cater for an increase in volume and variety of radiocarbon dating samples. To date, nearly 2000 graphite targets have been produced from materials such as plant macrofossils, charcoal, peat, bones, shells and wood. The equipment comprises a station for chemical preparation and high vacuum lines for production, purification and graphitization of sample carbon dioxide. The present capacity allows preparation of up to 400 targets annually for the needs of scientific projects and external orders for radiocarbon dating continuously received by the GADAM Centre of Excellence. The laboratory's sample preparation protocols and recent improvements are described and its performance during the 10 years of activity is discussed in terms of parameters obtained from reference materials prepared in this laboratory and demonstrated with a few science applications.

  4. Sample Preparation and Staining Methods for Two-Dimensional Polyacrylamide Gel Electrophoresis of Proteins from Animal Tissues

    Directory of Open Access Journals (Sweden)

    Levente Czegledi


    Full Text Available Proteomics in animal science as well as in other biological sciences is a significant tool in the post-genomic era. In proteomic studies the presence and relative abundance of expressed proteins of a cell, tissue or biological fluid is studied. Recently, the whole genome of more and more domestic animal species is known, but genes and the transcribed mRNA have no direct effect on biological systems as they are regulated by proteins, which explain the importance of proteomics. The most common tool in proteomic approach is the two-dimensional polyacrylamide gel electrophoresis (2D PAGE, when proteins are separated by their isoelectric point followed by their mass separation as a second dimension. In this study authors used different sample preparation and protein staining methods on meat,  liver and blood plasma and carried out 2D PAGE experiments. The most appropriate sample preparation methods are described in this paper. We concluded that depletion of major proteins in plasma is required but not necessary for meat and liver samples.

  5. Trace Elements Analysis of Geological Samples by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)


    This paper describes recent work applying a taser ablation system (LSX-200) hyphenated with POEMS Ⅲ inductively coupled plasma mass spectrometry (LA-ICP-MS) for the in situ analysis of 22 trace elements of solid geological materials. It demonstrates the potential of LA-ICP-MS for the determination of geochemically important trace and ultra-trace elements following XRF routine sample preparation. Signal drift, difference in transport efficiency and sampling yield are well corrected with NIST SRM 612 as external calibration standard and Ca as internal standard. The obtained results agree to the recommended values with relative error better than 15 % and RSD less than 15 % for most determined trace elemems. LOD ranges from 0.021 × 10-6 to 0. 23 × 10-6 and less than 0.10 × 10-6 for majority trace elements determined. In addition, home-made macro functions including filter and calculator compiled by VBA language under Excel software greatly enhanced off-line data reduction efficiency.``

  6. Study of sample preparation for quantitative analysis of amino acids in human sweat by liquid chromatography-tandem mass spectrometry. (United States)

    Delgado-Povedano, M M; Calderón-Santiago, M; Priego-Capote, F; Luque de Castro, M D


    The determination of physiological levels of amino acids is important to aid in the diagnosis and treatment of several diseases and nutritional status of individuals. Amino acids are frequently determined in biofluids such as blood (serum or plasma) and urine; however, there are less common biofluids with different concentration profiles of amino acids that could be of interest. One of these biofluids is sweat that can be obtained in a non-invasive manner and is characterized by low complex composition. The analysis of amino acids in human sweat requires the development of sample preparation strategies according to the sample matrix and small collected volume. The influence of sample preparation on the quantitative analysis of amino acids in sweat by LC-MS/MS has been assessed through a comparison between two strategies: dilution of sweat and centrifugal microsolid-phase extraction (c-μSPE). In both cases, several dilution factors were assayed for in-depth knowledge of the matrix effects, and the use of c-μSPE provided the best results in terms of accuracy. The behavior of the target analytes was a function of the dilution factor, thus providing a pattern for sample preparation that depended on the amino acid to be determined. The concentration of amino acids in sweat ranges between 6.20 ng mL(-1) (for homocysteine) and 259.77 µg mL(-1) (for serine) with precision, expressed as relative standard deviation, within 1.1-21.4%.

  7. Impact of hemolysis during sample collection: how different is drug concentration in hemolyzed plasma from that of normal plasma? (United States)

    Tan, Aimin; Gagné, Sébastien; Lévesque, Isabelle A; Lachance, Sylvain; Boudreau, Nadine; Lévesque, Ann


    Hemolysis is a common phenomenon in clinical studies. Despite the growing interest in hemolysis matrix effect, how hemolysis impacts the representability of hemolyzed plasma samples was rarely evaluated. The purpose of this research is to perform such an evaluation by theoretical consideration and experiment. A formula for estimating the impact is proposed, which includes the degree of hemolysis and the drug's red blood cell (RBC): plasma concentration ratio. The impact of hemolysis on the representability of hemolyzed plasma samples is compound-dependant. Given the same degree of hemolysis, the stronger a drug binds to RBCs, the more significant the impact of hemolysis. For a drug with high affinity to RBCs, the results of hemolyzed plasma samples may not be useful even though they are accurate. There is an overall agreement between theoretical predication and experimental results. Among the ten different drug compounds tested, only methazolamide, which binds strongly to RBCs, showed significant change in plasma concentration due to hemolysis. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. Sample preparation for atomic-resolution STEM at low voltages by FIB

    Energy Technology Data Exchange (ETDEWEB)

    Schaffer, Miroslava, E-mail: [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Department of Engineering, George Holt Building, Ashton Street, Liverpool L69 3BX (United Kingdom); Schaffer, Bernhard [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Kelvin Nanocharacterisation Centre, SUPA School of Physics and Astronomy, University of Glasgow, Glasgow G12 8QQ, Scotland (United Kingdom); Ramasse, Quentin [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Department of Engineering, George Holt Building, Ashton Street, Liverpool L69 3BX (United Kingdom)


    While FIB sample preparation for transmission electron microscopy is a well established technique, few examples exist of samples of sufficient quality for atomic resolution imaging by aberration corrected (scanning) transmission electron microscopy (STEM). In this work we demonstrate the successful preparation of such samples from five different materials and present the refined lift-out preparation technique, which was applied here. Samples with parallel surfaces and a general thickness between 20 and 40 nm over a range of several {mu}m were repeatedly prepared and analyzed by Cs-corrected STEM at 60 and 100 kV. Here, a novel 'wedge pre-milling' step helps to keep the protective surface layers intact during the whole milling process, allowing features close to or at the sample surface to be analyzed without preparation damage. Another example shows the cross-sectional preparation of a working thin film solar cell device to a final thickness of 10 to 20 nm over {mu}m sized areas in the region of interest, enabling atomic resolution imaging and elemental mapping across general grain boundaries without projection artefacts. All sample preparation has been carried out in modern Dual-Beam FIB microscopes capable of low-kV Ga{sup +} ion milling, but without additional preparation steps after the FIB lift-out procedure. -- Highlights: Black-Right-Pointing-Pointer Suitability of stand-alone FIB preparation for atomic resolution STEM is shown. Black-Right-Pointing-Pointer Reproducible preparation of 10-40 nm thick samples from 5 different materials. Black-Right-Pointing-Pointer Low-kV milling and adjusted procedure for crystalline, homogeneously thin specimen. Black-Right-Pointing-Pointer Wedge pre-milling to protect surface-near features.

  9. Proteomic biomarker discovery in 1000 human plasma samples with mass spectrometry

    DEFF Research Database (Denmark)

    Cominetti, Ornella; Núñez Galindo, Antonio; Corthésy, John


    the quality of the MS data and provided descriptive statistics. The data set was interrogated for proteins with most stable expression levels in that set of plasma samples. We evaluated standard clinical variables that typically impact forthcoming results and assessed body mass index-associated and gender......-specific proteins at two time points. We demonstrate that analyzing a large number of human plasma samples for biomarker discovery with MS using isobaric tagging is feasible, providing robust and consistent biological results....

  10. Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging (United States)

    Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee


    Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed.

  11. Effect of sample preparation methods on photometric determination of the tellurium and cobalt content in the samples of copper concentrates

    Directory of Open Access Journals (Sweden)

    Viktoriya Butenko


    Full Text Available Methods of determination of cobalt and nickel in copper concentrates currently used in factory laboratories are very labor intensive and time consuming. The limiting stage of the analysis is preliminary chemical sample preparation. Carrying out the decomposition process of industrial samples with concentrated mineral acids in open systems does not allow to improve the metrological characteristics of the methods, for this reason improvement the methods of sample preparation is quite relevant and has a practical interest. The work was dedicated to the determination of the optimal conditions of preliminary chemical preparation of copper concentrate samples for the subsequent determination of cobalt and tellurium in the obtained solution using tellurium-spectrophotometric method. Decomposition of the samples was carried out by acid dissolving in individual mineral acids and their mixtures by heating in an open system as well as by using ultrasonification and microwave radiation in a closed system. In order to select the optimal conditions for the decomposition of the samples in a closed system the phase contact time and ultrasonic generator’s power were varied. Intensification of the processes of decomposition of copper concentrates with nitric acid (1:1, ultrasound and microwave radiation allowed to transfer quantitatively cobalt and tellurium into solution spending 20 and 30 min respectively. This reduced the amount of reactants used and improved the accuracy of determination by running the process in strictly identical conditions.

  12. Preparation and investigation of bulk and thin film samples of strontium ferrite

    Directory of Open Access Journals (Sweden)

    A Poorbafrani


    Full Text Available   In this article, bulk and thin film samples of strontium ferrite have been studied. Due to the high electrical resistivity in strontium ferrite, energy loss due to eddy currents reduces and because of this, it can be used in high frequency magnetic circuits. On the other hand, strontium ferrite has attracted much attention as a permanent magnet. At first, we study the preparation process of bulk samples of strontium ferrite by a solid state reaction technique. In preparation of samples, to optimize the magnetic properties, we have used the stoichiometry factor (n = Fe2O3 / SrO of 5.25. In addition, we have used additives such as CaO and SiO2 to control grain growth. The samples have been prepared in two series: Isotropic and Anisotropic. For preparation of anisotropic samples, the magnetic field of 1T has been used for orientation of the grains during the press. Then, X-ray diffraction, Scanning Electron Microscopy (SEM, EDAX analysis and Magnetometer, was used for analyzing and comparing of structural and magnetic properties of isotropic and anisotropic samples. The results indicate that, due to the applied magnetic field, the structural and Magnetic properties of anisotropic samples improved efficiently because of the orientation of the grains during the press. In the next stage, we used bulk samples to prepare strontium ferrite thin films by Pulsed Laser Deposition technique (PLD. The Si (111 substrate has been used to prepare the thin films. Then we have studied the microstructure of thin films by X-ray diffraction, SEM and EDAX analysis. These studies on different samples show that for the preparation of crystalline phase of strontium ferrite thin films, the substrate temperature must be higher than 800˚C. The optimum conditions for preparation of strontium, ferrite thin films have been achieved on the substrate temperature of 840˚C and oxygen pressure of 75 mtorr.

  13. Preparation and modification of carbon nanotubes electrodes by cold plasmas processes toward the preparation of amperometric biosensors

    Energy Technology Data Exchange (ETDEWEB)

    Luais, E. [CEISAM, Universite de Nantes, CNRS, 2 rue de la Houssiniere, 44322 Nantes cedex 3 (France); IMN, Universite de Nantes, CNRS, 2 rue de la Houssiniere, 44322 Nantes cedex 3 (France); PCI, Universite du Maine, CNRS, rue Aristote, 72085 Le Mans cedex 9 (France); Thobie-Gautier, C. [CEISAM, Universite de Nantes, CNRS, 2 rue de la Houssiniere, 44322 Nantes cedex 3 (France); Tailleur, A.; Djouadi, M.-A.; Granier, A.; Tessier, P.Y. [IMN, Universite de Nantes, CNRS, 2 rue de la Houssiniere, 44322 Nantes cedex 3 (France); Debarnot, D.; Poncin-Epaillard, F. [PCI, Universite du Maine, CNRS, rue Aristote, 72085 Le Mans cedex 9 (France); Boujtita, M., E-mail: mohammed.boujtita@univ-nantes.f [CEISAM, Universite de Nantes, CNRS, 2 rue de la Houssiniere, 44322 Nantes cedex 3 (France)


    An electrochemical transducer based on vertically aligned carbon nanotubes (CNT) was prepared as a platform for biosensor development. Prior to enzyme immobilization, the CNT were treated using a microwave plasma system (CO{sub 2} and N{sub 2}/H{sub 2}) in order to functionalize the CNT surface with oxygenated and aminated groups. The morphological aspect of the electrode surface was examined by SEM and its chemical structure was also elucidated by XPS analysis. It was found out that microwave plasma system (CO{sub 2} and N{sub 2}/H{sub 2}) not only functionalizes the CNT but also permits to avoid the collapse phenomena retaining thus the alignment structure of the electrode surface. The electrochemical properties of the resulting new material based on CNT were carried out by cyclic voltammetry and were found suitable to develop high sensitive enzyme (HRP) biosensors operating on direct electron transfer process.

  14. Equipment for Topographical Preparation and Analysis of Various Semiconductor Infrared Detector Samples (United States)


    Approved for Public Release; Distribution Unlimited Final Report: Equipment for Topographical Preparation and Analysis of Various Semiconductor Infrared...Final Report: Equipment for Topographical Preparation and Analysis of Various Semiconductor Infrared Detector Samples Report Title A used will reinitialize and the video settings have to be reset. 6 Figure 4. This will open the both video overlay and the Dektak

  15. Advanced Curation Activities at NASA: Preparing for the Next Waves of Astromaterials Sample Return (United States)

    Zeigler, R. A.; Allton, J. H.; Evans, C. A.; Fries, M. D.; McCubbin, F. M.; Nakamura-Messenger, K.; Righter, K.; Zolensky, M.; Stansbery, E. K.


    We discuss the current curatorial efforts for NASA's astromaterials collections, as well as efforts that are underway (or need to be undertaken) to prepare for the challenging curation conditions required by future sample return missions.

  16. Simple and Reproducible Sample Preparation for Single-Shot Phosphoproteomics with High Sensitivity

    DEFF Research Database (Denmark)

    Jersie-Christensen, Rosa R.; Sultan, Abida; Olsen, Jesper V


    The traditional sample preparation workflow for mass spectrometry (MS)-based phosphoproteomics is time consuming and usually requires multiple steps, e.g., lysis, protein precipitation, reduction, alkylation, digestion, fractionation, and phosphopeptide enrichment. Each step can introduce chemica...

  17. Robotic, MEMS-based Multi Utility Sample Preparation Instrument for ISS Biological Workstation Project (United States)

    National Aeronautics and Space Administration — This project will develop a multi-functional, automated sample preparation instrument for biological wet-lab workstations on the ISS. The instrument is based on a...

  18. Surface modified polypropylene pipette tips packed with a monolithic plug of adsorbent for high-throughput sample preparation. (United States)

    Altun, Zeki; Hjelmström, Anette; Abdel-Rehim, Mohamed; Blomberg, Lars G


    UV-initiated poly(butyl methacrylate-ethylene glycol dimethacrylate) porous polymer monoliths were prepared in situ in polypropylene-based pipette tips for high-throughput sample preparation. Prior to the in situ polymerization, the surface of the PP tips was modified. In this work, two different surface modification approaches were tested for this purpose. First the photoinitiator benzophenone was used to generate radicals at the surface of PP by hydrogen abstraction. In the second modification approach, a thin layer of a polymer was directly grafted to the surface. The effect of surface modification was measured by contact angle measurements of a drop of water at the surface. As a result of the surface modification, scan electron microscopy images indicate a covalent attachment of the monolith to the wall of the pipette tip. Pipette tips modified with 5% BP in methanol and packed with a plug of monolith were further evaluated for high-throughput sample preparation. Using a liquid handling system, the extraction performance of packed pipette tips was tested for the analysis of ropivacaine in plasma samples. The recovery and reproducibility results were in accordance with internationally accepted criteria for qualitative and quantitative analysis of the test substance, ropivacaine.

  19. Analysis of whole blood samples with low gas flow inductively coupled plasma-optical emission spectrometry. (United States)

    Nowak, Sascha; Künnemeyer, Jens; Terborg, Lydia; Trümpler, Stefan; Günsel, Andreas; Wiesmüller, Gerhard A; Karst, Uwe; Buscher, Wolfgang


    Low gas flow ICP-OES with a total argon consumption below 0.7 L/min is introduced for the analysis of trace elements in blood samples to investigate the influence of samples containing an organic solvent in a demanding matrix on the performance of this plasma for the first time. Therefore, gadolinium was determined in human plasma samples and mercury in red blood cells, human plasma, and precipitated plasma protein fraction. Limits of detection (LOD) were determined to be in the low microgram per liter range for the analytes and the accuracy of the method was assessed by comparison with a conventional Fassel-type torch-based ICP-OES. It was proven that the low gas flow ICP-OES leads to comparable results with the instrument based on the Fassel-type torch.

  20. Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 2, Sample preparation methods

    Energy Technology Data Exchange (ETDEWEB)


    This volume contains the interim change notice for sample preparation methods. Covered are: acid digestion for metals analysis, fusion of Hanford tank waste solids, water leach of sludges/soils/other solids, extraction procedure toxicity (simulate leach in landfill), sample preparation for gamma spectroscopy, acid digestion for radiochemical analysis, leach preparation of solids for free cyanide analysis, aqueous leach of solids for anion analysis, microwave digestion of glasses and slurries for ICP/MS, toxicity characteristic leaching extraction for inorganics, leach/dissolution of activated metal for radiochemical analysis, extraction of single-shell tank (SST) samples for semi-VOC analysis, preparation and cleanup of hydrocarbon- containing samples for VOC and semi-VOC analysis, receiving of waste tank samples in onsite transfer cask, receipt and inspection of SST samples, receipt and extrusion of core samples at 325A shielded facility, cleaning and shipping of waste tank samplers, homogenization of solutions/slurries/sludges, and test sample preparation for bioassay quality control program.

  1. Simulated Irradiation of Samples in HFIR for use as Possible Test Materials in the MPEX (Material Plasma Exposure Experiment) Facility

    Energy Technology Data Exchange (ETDEWEB)

    Ellis, Ronald James [ORNL; Rapp, Juergen [ORNL


    The importance of Plasma Material Interaction (PMI) is a major concern in fusion reactor design and analysis. The Material-Plasma Exposure eXperiment (MPEX) facility will explore PMI under fusion reactor plasma conditions. Samples with accumulated displacements per atom (DPA) damage produced by irradiations in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) will be studied in the MPEX facility. The project presented in this paper involved performing assessments of the induced radioactivity and resulting radiation fields of a variety of potential fusion reactor materials. The scientific code packages MCNP and SCALE were used to simulate irradiation of the samples in HFIR; generation and depletion of nuclides in the material and the subsequent composition, activity levels, gamma radiation fields, and resultant dose rates as a function of cooling time. These state-of-the-art simulation methods were used in addressing the challenge of the MPEX project to minimize the radioactive inventory in the preparation of the samples for inclusion in the MPEX facility.

  2. Preparation for the operation of ITER: EU study on the plasma control system

    Energy Technology Data Exchange (ETDEWEB)

    Cavinato, M., E-mail: [Fusion for Energy, Barcelona (Spain); Ambrosino, G. [CREATE/ENEA/Euratom Association, Università di Napoli Federico II, Naples (Italy); Figini, L.; Granucci, G. [Associazione EURATOM-ENEA sulla Fusione, IFP-CNR, Via R. Cozzi 53, 20125 Milano (Italy); Gribov, Y. [ITER Organization, Route de Vinon sur Verdon, 13115 St Paul Lez Durance (France); Koechl, F. [Association EURATOM-ÖAW/ATI, Atominstitut, TU Wien, 1020 Vienna (Austria); Mattei, M. [CREATE/ENEA/Euratom Association, Seconda Università di Napoli, Naples (Italy); Parail, V. [Euratom/CCFE Fusion Association, Culham Science Centre, Abingdon OX14 3DB (United Kingdom); Pironti, A. [CREATE/ENEA/Euratom Association, Università di Napoli Federico II, Naples (Italy); Ricci, D. [Associazione EURATOM-ENEA sulla Fusione, IFP-CNR, Via R. Cozzi 53, 20125 Milano (Italy); Saibene, G.; Sartori, R. [Fusion for Energy, Barcelona (Spain); Zabeo, L. [ITER Organization, Route de Vinon sur Verdon, 13115 St Paul Lez Durance (France)


    In view of the preparation for the operation of the ITER tokamak it is necessary to develop the plasma scenarios taking into account all engineering constraints coming from the plant and including a realistic control system. It is important to consider that, due to the high energy of ITER plasmas, much more stringent requirements are posed on the control of transients in order to avoid machine damage. Several activities are performed in the EU focusing on one side on the scenario optimization from a physics point of view and on the other side on the design and modeling of a realistic plasma control system driving the plasma configuration throughout the whole pulse and suitable for implementation on a real machine. The issues related to the computation of the control feed-forward component are addressed. In particular, the possibility to trigger a feed-forward component to solve controllability problems arising in the transitions from plasma L to H and H to L modes is studied in detail with the support of linear and non-linear simulations. A control strategy is designed and tested on non-linear simulations of the whole pulse, including linear and non-linear effects due to controller switching, plasma shape reconstruction and power supplies. The paper reports on the results of the studies performed and discuss the proposed design of the plasma control system.

  3. Preparation of testate amoebae samples affects water table depth reconstructions in peatland palaeoecological studies

    Directory of Open Access Journals (Sweden)

    Eve Avel


    Full Text Available In peatland palaeoecological studies, the preparation of peat samples for testate amoebae (TA analysis involves boiling of samples and microsieving them through a 15-μm sieve. We studied the effect of these preparation stages on the estimation of TA assemblages and on the reconstruction of water table depths (WTD. Our results indicate that the TA assemblages of boiled and unboiled samples are not significantly different, while microsieving reduces the concentration of small TA taxa and results in significantly different TA assemblages. The differences between microsieved and unsieved TA assemblages were reflected also in predicted values of WTD, which indicated drier conditions in case of unsieved samples than in microsieved samples. We conclude that the boiling of samples might be omitted if TA are extracted from the fresh peat samples. Microsieving may lead to erroneous palaeoecological WTD reconstructions and should be avoided if small TA taxa are present in samples.

  4. On radiation damage in FIB-prepared softwood samples measured by scanning X-ray diffraction. (United States)

    Storm, Selina; Ogurreck, Malte; Laipple, Daniel; Krywka, Christina; Burghammer, Manfred; Di Cola, Emanuela; Müller, Martin


    The high flux density encountered in scanning X-ray nanodiffraction experiments can lead to severe radiation damage to biological samples. However, this technique is a suitable tool for investigating samples to high spatial resolution. The layered cell wall structure of softwood tracheids is an interesting system which has been extensively studied using this method. The tracheid cell has a complex geometry, which requires the sample to be prepared by cutting it perpendicularly to the cell wall axis. Focused ion beam (FIB) milling in combination with scanning electron microscopy allows precise alignment and cutting without splintering. Here, results of a scanning X-ray diffraction experiment performed on a biological sample prepared with a focused ion beam of gallium atoms are reported for the first time. It is shown that samples prepared and measured in this way suffer from the incorporation of gallium atoms up to a surprisingly large depth of 1 µm.

  5. Radionuclide Determination In Surface Water Samples By Inductively Coupled Plasma With Sector Field Mass Spectrometry (ICP-SFMS

    Directory of Open Access Journals (Sweden)

    E. T. Romero-Guzmán


    Full Text Available The determination of naturally occurring radionuclides in the environment by inductively coupled plasma mass spectrometry of high resolution (ICP-SFMS has gained recognition over the last fifteen years, relative to the radiometric techniques, as the result of improvement in instrumental performance, sample introduction equipment and sample preparation. With the increase in instrumental sensitivity, it is now possible to measure ultratrace levels of many radioisotopes. The aim of this work was to determined the natural radionuclides (232Th, 234U, 235U and 238U in surface water using Inductively Coupled PlasmaSector Field Mass Spectrometry (ICP-SFMS. The samples were sampling from Lerma river, State of Mexico at february to april 2015. The process of treatment of sample consisted in perform an acid digestion according to the 3015A USEPA method followed of the direct measurement in ICP-SFMS. Results obtained were: a identify the presence of 232Th, 234U, 235U and 238U isotopes in water, b isotopic ratios were for 234U/238U=1.133 ± 0.016. ICPSFMS has gained popularity in the field of radiochemistry, particularly as a method of detection for long lived-actinides.

  6. Plasma processes in the preparation of lithium-ion battery electrodes and separators (United States)

    Nava-Avendaño, J.; Veilleux, J.


    Lithium-ion batteries (LIBs) are the energy storage devices that dominate the portable electronic market. They are now also considered and used for electric vehicles and are foreseen to enable the smart grid. Preparing batteries with high energy and power densities, elevated cycleability and improved safety could be achieved by controlling the microstructure of the electrode materials and the interaction they have with the electrolyte over the working potential window. Selecting appropriate precursors, reducing the preparation steps and selecting more efficient synthesis methods could also significantly reduce the costs of LIB components. Implementing plasma technologies can represent a high capital investment, but the versatility of the technologies allows the preparation of powdered nanoparticles with different morphologies, as well as with carbon and metal oxide coatings. Plasma technologies can also enable the preparation of binder-free thin films and coatings for LIB electrodes, and the treatment of polymeric membranes to be used as separators. This review paper aims at highlighting the different thermal and non-thermal plasma technologies recently used to synthesize coated and non-coated active materials for LIB cathodes and anodes, and to modify the surface of separators.

  7. Sample preparation for thermo-gravimetric determination and thermo-gravimetric characterization of refuse derived fuel. (United States)

    Robinson, T; Bronson, B; Gogolek, P; Mehrani, P


    Thermo-gravimetric analysis (TGA) is a useful method for characterizing fuels. In the past it has been applied to the study of refuse derived fuel (RDF) and related materials. However, the heterogeneity of RDF makes the preparation of small representative samples very difficult and this difficulty has limited the effectiveness of TGA for characterization of RDF. A TGA method was applied to a variety of materials prepared from a commercially available RDF using a variety of procedures. Applicability of TGA method to the determination of the renewable content of RDF was considered. Cryogenic ball milling was found to be an effective means of preparing RDF samples for TGA. When combined with an effective sample preparation, TGA could be used as an alternative method for assessing the renewable content of RDF.

  8. Expanding the application of the tablet processing workstation to support the sample preparation of oral suspensions. (United States)

    Opio, Alex Manuel; Nickerson, Beverly; Xue, Gang; Warzeka, John; Norris, Ken


    Sample preparation is the most time-consuming part of the analytical method for powder for oral suspension (POS) assay, purity, and preservative analysis, as this involves multiple dilution and filtration steps. The Tablet Processing Workstation (TPW) was used to automate the sample preparation of a POS formulation. Although the TPW is typically used to automate the preparation of solid oral dosage forms and powders, it contains all of the necessary components to perform POS sample preparation. The TPW exhibited acceptable repeatability in testing 3 lots using 10 replicate preparations per lot. Acceptable linearity of the drug and preservative in the presence of excipients was demonstrated over the range corresponding to 50-150% of intent. Accuracy showed suitable recoveries for all points evaluated. TPW results were shown to correlate to results obtained with the manual method. The TPW method was used to prepare samples in support of manufacturing scale-up efforts. With the efficiencies gained using the TPW, it was possible to analyze a large number of samples generated during process development activities for the POS formulation with minimal human intervention. The extensive data enabled trending of the manufacturing development runs and helped to identify optimization strategies for the process.

  9. Chemical Structure of Carbon Nitride Films Prepared by MW-ECR Plasma Enhanced Magnetron Sputtering

    Institute of Scientific and Technical Information of China (English)

    XUJun,GAOPeng; DINGWan-yu; LIXin; DENGXin-lu; DONGChuang


    Amorphous carbon nitride thin films were prepared by plasma-enhanced DC magnetron sputtering using twinned microwave electron cyclotron resonance plasma sources. Chemical structure of deposited films was investigated using X-ray photoelectron spectroscopy and Fourier transtorm infrared spectroscopy. The results indicate that the deposition rate is strongly affected by direct current bias, and the films are mainly composed of a single amorphous carbon nitride phase with N/C ratio close to C3N4, and the bonding is predominantly of C-N type.

  10. Pretreatment of plasma samples by a novel hollow fiber centrifugal ultrafiltrate device for the determination of cefaclor concentrations in human plasma. (United States)

    Li, Jun-Mei; Li, Cen; Jiang, Ye; Ren, Shu-Meng


    A simple sample preparation method was developed by using a centrifugal ultrafiltration (CF-UF) device with hollow fiber (HF) for the determination of cefaclor in plasma by HPLC. Samples were placed into a homemade device, which was consisted of a glass tube and a U-shaped hollow fiber. The filtrate was withdrawn from the hollow fiber into a syringe after centrifugation and 20 μL was directly injected into the HPLC for analysis. The HPLC method had a linear calibration curve in the concentration range of 6.00×10(-2)-30.7 μg mL(-1)(r=0.9996). The limit of detection (LOD) and limit of quantitation (LOQ) were 0.02 and 0.06 μg mL(-1), respectively. The intra and inter-day precisions (RSD) were 1.7%, 1.2%, 1.0% and 3.6%, 2.5%, 1.9%, respectively, for three concentrations. Assay accuracy was higher than 99.2% and the absolute recovery was 86.8-92.5%. It is feasible to use this novel and low cost device for sample pretreatment for the analysis of cefaclor in plasma.

  11. Cytotoxicity of Light-Cured Dental Materials according to Different Sample Preparation Methods (United States)

    Lee, Myung-Jin; Kim, Mi-Joo; Kwon, Jae-Sung; Lee, Sang-Bae; Kim, Kwang-Mahn


    Dental light-cured resins can undergo different degrees of polymerization when applied in vivo. When polymerization is incomplete, toxic monomers may be released into the oral cavity. The present study assessed the cytotoxicity of different materials, using sample preparation methods that mirror clinical conditions. Composite and bonding resins were used and divided into four groups according to sample preparation method: uncured; directly cured samples, which were cured after being placed on solidified agar; post-cured samples were polymerized before being placed on agar; and “removed unreacted layer” samples had their oxygen-inhibition layer removed after polymerization. Cytotoxicity was evaluated using an agar diffusion test, MTT assay, and confocal microscopy. Uncured samples were the most cytotoxic, while removed unreacted layer samples were the least cytotoxic (p cytotoxicity. Clinicians should remove unreacted monomers on the resin surface immediately after restoring teeth with light-curing resin to improve the restoration biocompatibility. PMID:28772647

  12. Preparation and characterization of microporous fibers for sample preparation and LC-MS determination of drugs. (United States)

    Buszewski, Boguslaw; Nowaczyk, Jacek; Ligor, Tomasz; Olszowy, Pawel; Ligor, Magdalena; Wasiniak, Bartlomiej; Miekisch, Wolfram; Schubert, Jochen K; Amann, Anton


    The aim of this study was the preparation of polypyrrole (PPy) fibers for solid phase microextraction (SPME). PPy coatings were obtained during the electrochemical polymerization process. The utility of various metal wires (Fe, Cu, Ag, Cu/Ag, kanthal and medical stainless steel) as a support for polymers was compared. Various experimental conditions of the synthesis process such as scan rate, voltage limits and number of scans and deposition time were applied. The average polymer thickness was in the range of 7-125 microm and its weight was in the scope of 0.65-5.6 mg. Different techniques, mainly elemental analysis, Fourier transform infrared spectroscopy, microscopy, and chromatography were performed for the characterization of obtained fibers with microporous structure. The extraction efficiency of cardiovascular drugs (metoprolol, propranolol, oxprenolol, propafenone and mexiletine) by means of fibers was tested. The concentration of mentioned compounds in standard solution was in the span of 10-150 ng/mL. LC-MS was employed for determination of drugs in desorption solution. LODs varied from 0.013 to 1.51 ng/mL for metoprolol and mexiletine respectively. The repeatability of extraction was obtained with the RSD values lower than 10%.

  13. The effect of sample size on fresh plasma thromboplastin ISI determination

    DEFF Research Database (Denmark)

    Poller, L; Van Den Besselaar, A M; Jespersen, J;


    The possibility of reduction of numbers of fresh coumarin and normal plasmas has been studied in a multicentre manual prothrombin (PT) calibration of high international sensitivity index (ISI) rabbit and low ISI human reference thromboplastins at 14 laboratories. The number of calibrant plasmas...... was reduced progressively by a computer program which generated random numbers to provide 1000 different selections for each reduced sample at each participant laboratory. Results were compared with those of the full set of 20 normal and 60 coumarin plasma calibrations. With the human reagent, 20 coumarins...... and seven normals still achieved the W.H.O. precision limit (3% CV of the slope), but with the rabbit reagent reduction coumarins with 17 normal plasmas led to unacceptable CV. Little reduction of numbers from the full set of 80 fresh plasmas appears advisable. For maximum confidence, when calibrating...

  14. Simulation of rarefied low pressure RF plasma flow around the sample (United States)

    Zheltukhin, V. S.; Shemakhin, A. Yu


    The paper describes a mathematical model of the flow of radio frequency plasma at low pressure. The hybrid mathematical model includes the Boltzmann equation for the neutral component of the RF plasma, the continuity and the thermal equations for the charged component. Initial and boundary conditions for the corresponding equations are described. The electron temperature in the calculations is 1-4 eV, atoms temperature in the plasma clot is (3-4) • 103 K, in the plasma jet is (3.2-10) • 102 K, the degree of ionization is 10-7-10-5, electron density is 1015-1019 m-3. For calculations plasma parameters is developed soft package on C++ program language, that uses the OpenFOAM library package. Simulations for the vacuum chamber in the presence of a sample and the free jet flow were carried out.

  15. Reducing Spatial Heterogeneity of MALDI Samples with Marangoni Flows During Sample Preparation (United States)

    Lai, Yin-Hung; Cai, Yi-Hong; Lee, Hsun; Ou, Yu-Meng; Hsiao, Chih-Hao; Tsao, Chien-Wei; Chang, Huan-Tsung; Wang, Yi-Sheng


    This work demonstrates a method to prepare homogeneous distributions of analytes to improve data reproducibility in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS). Natural-air drying processes normally result in unwanted heterogeneous spatial distributions of analytes in MALDI crystals and make quantitative analysis difficult. This study demonstrates that inducing Marangoni flows within drying droplets can significantly reduce the heterogeneity problem. The Marangoni flows are accelerated by changing substrate temperatures to create temperature gradients across droplets. Such hydrodynamic flows are analyzed semi-empirically. Using imaging mass spectrometry, changes of heterogeneity of molecules with the change of substrate temperature during drying processes are demonstrated. The observed heterogeneities of the biomolecules reduce as predicted Marangoni velocities increase. In comparison to conventional methods, drying droplets on a 5 °C substrate while keeping the surroundings at ambient conditions typically reduces the heterogeneity of biomolecular ions by 65%-80%. The observation suggests that decreasing substrate temperature during droplet drying processes is a simple and effective means to reduce analyte heterogeneity for quantitative applications.

  16. Repeating cytological preparations on liquid-based cytology samples: A methodological advantage? (United States)

    Pinto, Alvaro P; Maia, Henrique Felde; di Loretto, Celso; Krunn, Patrícia; Túlio, Siumara; Collaço, Luis Martins


    This study investigates the rule that repeating cytological preparations on liquid-based cytology improves sample adequacy, diagnosis, microbiological, and hormonal evaluations. We reviewed 156 cases of pap-stained preparations of exfoliated cervical cells in two slides processed by DNA-Cytoliq System. After sample repeat/dilution, limiting factors affecting sample adequacy were removed in nine cases and three unsatisfactory cases were reclassified as satisfactory. Diagnosis was altered in 24 cases. Of these, the original diagnosis in 15 was atypical squamous cells of undetermined significance; after the second slide examination, diagnosis in 5 of the 15 cases changed to low-grade squamous intraepithelial lesion, 3 to high-grade squamous intraepithelial lesion, and 7 to absence of lesion. Microbiological evaluation was altered, with Candida sp. detected in two repeated slides. Repeat slide preparation or dilution of residual samples enhances cytological diagnosis and decreases effects of limiting factors in manually processed DIGENE DCS LBC.

  17. Plasma treatment of bulk niobium surface for superconducting rf cavities: Optimization of the experimental conditions on flat samples

    Directory of Open Access Journals (Sweden)

    M. Rašković


    Full Text Available Accelerator performance, in particular the average accelerating field and the cavity quality factor, depends on the physical and chemical characteristics of the superconducting radio-frequency (SRF cavity surface. Plasma based surface modification provides an excellent opportunity to eliminate nonsuperconductive pollutants in the penetration depth region and to remove the mechanically damaged surface layer, which improves the surface roughness. Here we show that the plasma treatment of bulk niobium (Nb presents an alternative surface preparation method to the commonly used buffered chemical polishing and electropolishing methods. We have optimized the experimental conditions in the microwave glow discharge system and their influence on the Nb removal rate on flat samples. We have achieved an etching rate of 1.7  μm/min⁡ using only 3% chlorine in the reactive mixture. Combining a fast etching step with a moderate one, we have improved the surface roughness without exposing the sample surface to the environment. We intend to apply the optimized experimental conditions to the preparation of single cell cavities, pursuing the improvement of their rf performance.

  18. Preparation and properties of plasma-polymerized thiophene (PPT) conducting films

    Energy Technology Data Exchange (ETDEWEB)

    Sadhir, R.K. (Westinghouse Science and Tech. Center, Pittsburgh, PA (United States)); Schoch, K.F. Jr. (Westinghouse Science and Tech. Center, Pittsburgh, PA (United States))


    This paper presents, for the first time, conducting films of polythiophene prepared by plasma-polymerization. In this technique, ionized argon is the initiating species for the polymerization of thiophene in a region away from the high RF flux-density. These films displayed a conductivity of 1.8 x 10[sup -4] S cm[sup -1] after doping with iodine. The surface morphology of the films deposited away from the high RF flux-density region showed topology similar to the films prepared by electrochemical methods. The films deposited near the high RF flux-density region showed a platelet structure. (orig.)

  19. Development of a high vacuum sample preparation system for helium mass spectrometer (United States)

    Kumar, P.; Das, N. K.; Mallik, C.; Bhandari, R. K.


    A high vacuum sample preparation system for the 3He/4He ratio mass spectrometer (Helix SFT) has been developed to remove all the gaseous constituents excluding helium from the field gases. The sample preparation system comprises of turbo molecular pump, ion pump, zirconium getter, pipettes and vacuum gauges with controller. All these are fitted with cylindrical SS chamber using all metal valves. The field samples are initially treated with activated charcoal trap immersed in liquid nitrogen to cutoff major impurities and moisture present in the sample gas. A sample of 5 ml is collected out of this stage at a pressure of 10-2 mbar. This sample is subsequently purified at a reduced pressure of 10-7 mbar before it is injected into the ion source of the mass spectrometer. The sample pressure was maintained below 10-7 mbar with turbo molecular vacuum pumps and ion pumps. The sample gas passes through several getter elements and a cold finger with the help of manual high vacuum valves before it is fed to the mass spectrometer. Thus the high vacuum sample preparation system introduces completely clean, dry and refined helium sample to the mass spectrometer for best possible analysis of isotopic ratio of helium.

  20. Plasma sintering of ferritic steel reinforced with niobium carbide prepared by high energy milling; Sinterizacao a plasma de aco ferritico reforcado com carbeto de niobio preparado por moagem de alta energia

    Energy Technology Data Exchange (ETDEWEB)

    Silva Junior, J.F. da; Almeida, E.O.; Gomes, U.U.; Alves Junior, C.; Messias, A.P. [Universidade Federal do Rio Grande do Norte (UFRN), Natal (Brazil). Lab. de Materiais Ceramicos e Metais Especiais; Universidade Federal do Rio Grande do Norte (UFRN), Natal (Brazil). Lab. de Processamento de Materiais por Plasma


    Plasma is an ionized gas where ions are accelerated from anode to cathode surface, where the sample is placed. There are a lot of collisions on cathode surface by ions heating and sintering the sample. High energy milling (HEM) is often used to produce composite particles to be used on powder metallurgy. These particles can exhibit fine particles and high phase dispersion. This present work aim to study ferritic steels reinforced with 3%NbC prepared by HEM and sintered on plasma furnace. Ferritic steel and NbC powders were milled during 5 hours and characterized by SEM, XRD and laser scattering. Then, these composite powders were compacted in a cylindrical steel die and then sintered in a plasma furnace. Vickers microhardness tests and SEM and XRD analysis were performed on sintered samples. (author)

  1. Effects of anesthesia and blood sampling techniques on plasma metabolites and corticosterone in the rat. (United States)

    Arnold, Myrtha; Langhans, Wolfgang


    Blood is routinely sampled from laboratory animals in biomedical research, and many of the commonly applied sampling techniques require anesthesia. Acute effects of many sampling and anesthesia procedures may confound the results, but those effects are incompletely characterized. We here compare the effects of four common anesthesia procedures (inhalation anesthesia with ether (EA) or isoflurane (IA) and intraperitoneal injection anesthesia with xylazin/ketamine (XKA) or medetomidine/midazolam/fentanyl (MMFA)) on plasma concentrations of glucose, lactate, non-esterified fatty acids (NEFAs), and corticosterone in blood obtained from a previously implanted jugular vein (JV) catheter with the effect of JV blood sampling from non-anesthetized, freely-moving rats (JV-NA). Also, we included in the comparison two other blood sampling procedures usually performed without anesthesia (NA), i.e., puncture of the saphenic vein (SV) and tail incision (TI). Whereas the control procedure (JV-NA) did not significantly affect any of the target parameters, plasma glucose increased from 14 (JV-IA) to 44 (JV-MMFA) % (all Ps=0.05 when compared with the control procedure) in all blood samples collected in anesthesia and was 12 and 14% lower (both Pssamples, respectively. Plasma lactate increased from 74 (JV-IA) to 226% (SV-NA) (all Pssampling and anesthesia procedures except for JV-XKA and JV-MMF. Plasma NEFAs increased to 52% (P0.05). Finally, only the JV-EA and the JV-MMFA procedures increased plasma corticosterone (+525 and +353%, respectively, both Pssampling procedures can have profound acute effects on plasma metabolite and hormone concentrations. This must be considered for the design and interpretation of blood sampling experiments in laboratory animals. (c) 2010. Published by Elsevier Inc.

  2. Preparation of Spherical Bi2O3 Powder by Plasma and Precipitation Processes

    Institute of Scientific and Technical Information of China (English)

    Chen Peirong; Ji Youzhang; Feng Shifen


    Spherical Bi2O3 powder prepared by plasma chemical vapor reaction and aqueous chemical precipitation is studied. The superfine spherical Bi2O3 powder with an average diameter of 1 μm is made by plasma process. During the precipitation process, the micrograph of the Bi2O3 powder can be controlled through the reaction temperature, the rate of addition of the precipitation reagent, the reaction time and the amount of the dispersant. Accordingly, spherical Bi2O3 powder with diameters ranging from 2 μm to 3 μm is prepared. The spherical Bi2 O3particles have such advantages as uniform size distribution and excellent dispersing property.ZnO varistors made from the resultant powder exhibit properties of a low discharge voltage ratio,great eligibility coefficient measured by a rectangle wave of 2 ms 800 A and good stability in the above characteristics.

  3. Preparation and Characterization of Plasma-Sprayed Ultrafine Chromium Oxide Coatings

    Institute of Scientific and Technical Information of China (English)

    LIN Feng; JIANG Xianliang; YU Yueguang; ZENG Keli; REN Xianjing; LI Zhenduo


    Ultrafine chromium oxide coatings were prepared by plasma spraying with ultrafine feedstock. Processing parameters of plasma spraying were optimized. Optical microscope (OM) was used to observe the microstructure of the ultrafine chromium oxide coatings. Scanning electron microscopy (SEM) was used to observe the morphology and particle size of ultrafine powder feedstock as well as to examine the microstructure of the chromium oxide coating. In addition, hardness and bonding strength of the ultrafine chromium oxide coatings were measured.The results showed that the optimized plasma spraying parameters were suitable for ultrafine chromium oxide coating and the properties and microstructure of the optimized ultrafine chromium oxide coating were superior compared to conventional chromium oxide wear resistant coatings.

  4. Preparation and Adsorption Properties of PAM Based Adsorbents for Plasma Lipoproteins

    Institute of Scientific and Technical Information of China (English)

    Hai Tao LI; Zhi YUAN; Xin Fu CHEN; Bin LIU; Bin SHEN; Bing Lin HE


    Crosslinked macroporous polyacrylamide(PAM)was prepared with inverse phase suspension polymerization technique.After treatment with hydrazine,the polymer was functionalized with chloroacetic acid,trifluoroacetic acid diethylenetriaminepentaacetic acid (DEPAA), and maleic acid, respectively,and PAM based adsorbents bearing carboxyl functional groups for low density lipoprotein(LDL)apheresis use were obtained.The blood compatibility and the adsorption properties for plasma lipoproteins of PAM based adsorbents were investigated.

  5. Electromembrane extraction as a rapid and selective miniaturized sample preparation technique for biological fluids

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Pedersen-Bjergaard, Stig; Seip, Knut Fredrik


    This special report discusses the sample preparation method electromembrane extraction, which was introduced in 2006 as a rapid and selective miniaturized extraction method. The extraction principle is based on isolation of charged analytes extracted from an aqueous sample, across a thin film....... Technical aspects of electromembrane extraction, important extraction parameters as well as a handful of examples of applications from different biological samples and bioanalytical areas are discussed in the paper....

  6. TruSeq Stranded mRNA and Total RNA Sample Preparation Kits (United States)

    Total RNA-Seq enabled by ribosomal RNA (rRNA) reduction is compatible with formalin-fixed paraffin embedded (FFPE) samples, which contain potentially critical biological information. The family of TruSeq Stranded Total RNA sample preparation kits provides a unique combination of unmatched data quality for both mRNA and whole-transcriptome analyses, robust interrogation of both standard and low-quality samples and workflows compatible with a wide range of study designs.

  7. Influence of mechanical alloying time on the properties of Fe3Al intermetallics prepared by spark plasma sintering

    Institute of Scientific and Technical Information of China (English)

    Chengchang Jia; Qing He; Jie Meng; Lina Guo


    The Fe3Al-based intermetallics were prepared by mechanical alloying and spark plasma sintering (SPS), and the influence of milling time on the properties of materials was investigated. The phase identification was investigated by X-ray, and the surface morphology and fractography were observed by scanning electron microscope (SEM). The mechanical properties such as bending strength, strain, and microhardness were tested. The results show that Fe reacts with Al completely to form Fe3Al during short SPS processing time. The relative densities of the sintered samples were nearly 100%. The mechanical properties of the sintered samples can be improved along with the milling time. The representative values are the bend strength of 1327 MPa and the microhardness of 434.

  8. Surface characterization and platelet adhesion studies on fluorocarbons prepared by plasma-induced graft polymerization. (United States)

    Lin, J C; Tiong, S L; Chen, C Y


    It is believed that the interactions between the biological environment and biomaterial surface are the key factors influencing its biocompatibility. Therefore, plasma processing, which can vary the surface properties without altering the bulk properties, has been considered as one of the important techniques for improving a materials' biocompatibility. In this investigation, plasma-induced grafting polymerization of vinylidene fluoride (VDF) and chlorotrifluoroethylene (CTFE), instead of direct plasma polymerization, was attempted with an aim to improve the substrate blood compatibility. Contact angle measurement indicated both fluorocarbon-grafted Pdyethylenes (PEs) are hydrophobic. Due to the additional fluorine and chlorine atoms on the CTFE chain, the PCTFE-grafted PE exhibited a higher hydrophobicity than the PVDF-grafted one. ESCA analysis has revealed that these two plasma-induced fluorocarbon deposits contain almost no CFx (x > 2) binding on the surface layer, indicating the grafting polymerization mainly follows the free radical mechanism instead of the molecule-highly-fragmented reaction steps commonly seen in the direct plasma polymerization treatment. In addition, ATR-FTIR has shown the surface chemical configuration of these PVDF- and PCTFE-grafted PEs to be very similar to those of the bulk samples of PVDF and PCTFE. The surface roughness decreased after oxygen plasma treatment and was further reduced by VDF and CTFE grafting polymerization. In vitro platelet adhesion testing indicated these two fluorocarbon grafted PEs are less platelet-activating than the nontreated PE control and oxygen plasma activated one.

  9. Determination of metformin in mouse, rat, dog and human plasma samples by laser diode thermal desorption/atmospheric pressure chemical ionization tandem mass spectrometry. (United States)

    Swales, John G; Gallagher, Richard; Peter, Raimund M


    A simple, rapid and robust high-throughput assay for the quantitative analysis of metformin in plasma from different species using laser diode thermal desorption interfaced with atmospheric chemical pressure ionization tandem mass spectrometry (LDTD-APCI-MSMS) was developed for use in a pharmaceutical discovery environment. In order to minimize sample preparation a generic protein precipitation method was used to extract metformin from the plasma. Laser diode thermal desorption is a relatively new sample introduction method, the optimization of the instrumental parameters are presented. The method was successfully applied to spiked mouse, rat, dog and human plasma samples and was subsequently used to determine the oral pharmacokinetics of metformin after dosing to male rats in order to support drug discovery projects. The deviations for intra-assay accuracy and precision across the four species were less than 30% at all calibration and quality control levels.

  10. A rapid, accurate and robust particle-based assay for the simultaneous screening of plasma samples for the presence of five different anti-cytokine autoantibodies

    DEFF Research Database (Denmark)

    Guldager, Daniel Kring Rasmussen; von Stemann, Jakob Hjorth; Larsen, Rune


    PURPOSE: To establish and validate a rapid, cost-effective and accurate screening assay for the simultaneous testing of human naturally occurring anti-cytokine autoantibodies (c-aAb) targeting interleukin-1α (IL-1α), interleukin-6 (IL-6), interleukin-10 (IL-10), granulocyte-macrophage colony...... plasma samples and pooled normal immunoglobulin preparations were used to validate the assay. Plasma samples from 98 transfusion recipients, half of whom presented with febrile reactions, were tested by the assay. RESULTS: The assay detected specific and saturable immunoglobulin G (IgG) binding to each...... cytokine autoantibodies quantities in the negative plasma samples ranged between 80% and 125%. The analytical intra- and inter-assay variations were 4% and 11%, respectively. Varying c-aAb levels were detectable in the transfusion recipients. There was no difference in c-aAb frequency between the patients...

  11. Measurement and Comparison of Organic Compound Concentrations in Plasma, Whole Blood, and Dried Blood Spot Samples. (United States)

    Batterman, Stuart A; Chernyak, Sergey; Su, Feng-Chiao


    The preferred sampling medium for measuring human exposures of persistent organic compounds (POPs) is blood, and relevant sample types include whole blood, plasma, and dried blood spots (DBS). Because information regarding the performance and comparability of measurements across these sample types is limited, it is difficult to compare across studies. This study evaluates the performance of POP measurements in plasma, whole blood and DBS, and presents the distribution coefficients needed to convert concentrations among the three sample types. Blood samples were collected from adult volunteers, along with demographic and smoking information, and analyzed by GC/MS for organochlorine pesticides (OCPs), chlorinated hydrocarbons (CHCs), polychlorinated biphenyls (PCBs), and brominated diphenyl ethers (PBDEs). Regression models were used to evaluate the relationships between the sample types and possible effects of personal covariates. Distribution coefficients also were calculated using physically-based models. Across all compounds, concentrations in plasma were consistently the highest; concentrations in whole blood and DBS samples were comparable. Distribution coefficients for plasma to whole blood concentrations ranged from 1.74 to 2.26 for pesticides/CHCs, averaged 1.69 ± 0.06 for the PCBs, and averaged 1.65 ± 0.03 for the PBDEs. Regression models closely fit most chemicals (R (2) > 0.80), and whole blood and DBS samples generally showed very good agreement. Distribution coefficients estimated using biologically-based models were near one and did not explain the observed distribution. Among the study population, median concentrations of several pesticides/CHCs and PBDEs exceeded levels reported in the 2007-2008 National Health and Nutrition Examination Survey, while levels of other OCPs and PBDEs were comparable or lower. Race and smoking status appeared to slightly affect plasma/blood concentration ratios for several POPs. The experimentally

  12. Measurement and Comparison of Organic Compound Concentrations in Plasma, Whole Blood and Dried Blood Spot Samples

    Directory of Open Access Journals (Sweden)

    Stuart A Batterman


    Full Text Available The preferred sampling medium for measuring human exposures of persistent organic compounds (POPs is blood, and relevant sample types include whole blood, plasma, and dried blood spots (DBS. Because information regarding the performance and comparability of measurements across these sample types is limited, it is difficult to compare across studies. This study evaluates the performance of POP measurements in plasma, whole blood and DBS, and presents the distribution coefficients needed to convert concentrations among the three sample types. Blood samples were collected from adult volunteers, along with demographic and smoking information, and analyzed by GC/MS for organochlorine pesticides (OCPs, chlorinated hydrocarbons (CHCs, polychlorinated biphenyls (PCBs, and brominated diphenyl ethers (PBDEs. Regression models were used to evaluate the relationships between the sample types and possible effects of personal covariates. Distribution coefficients also were calculated using physically-based models.Across all compounds, concentrations in plasma were consistently the highest; concentrations in whole blood and DBS samples were comparable. Distribution coefficients for plasma to whole blood concentrations ranged from 1.74 to 2.26 for pesticides/CHCs, averaged 1.69 ± 0.06 for the PCBs, and averaged 1.65 ± 0.03 for the PBDEs. Regression models closely fit most chemicals (R2 > 0.80, and whole blood and DBS samples generally showed very good agreement. Distribution coefficients estimated using biologically-based models were near one and did not explain the observed distribution. Among the study population, median concentrations of several pesticides/CHCs and PBDEs exceeded levels reported in the 2007-2008 National Health and Nutrition Examination Survey, while levels of other OCPs and PBDEs were comparable or lower. Race and smoking status appeared to slightly affect plasma/blood concentration ratios for several POPs. The experimentally

  13. Radiochemical Separation and Measurement by Mass Spectrometry with Magnetic Sector with Inductively Coupled Plasma source (ICP-SFMS of Plutonium Isotopes in Soil Samples

    Directory of Open Access Journals (Sweden)

    C. O. Torres-Cortés


    Full Text Available The aim of this work is twofold: to optimize the radiochemical separation of Plutonium (Pu from soil samples, and to measure the Pu concentration. Soil samples were prepared using acid digestion assisted by microwaves; then, Pu purification was carried out with Pu AG1X8 resin. Pu isotopes were measured using Mass Spectrometry with Magnetic Sector with Inductively Coupled Plasma source (ICP-SFMS. In order to reduce the interference due to the presence of 238UH+ in the samples a desolvation system (Apex was used. The limit of detection (LOD of Pu was determined. The efficiency of Pu recovery from soil samples varies from 70 to 93%.

  14. Direct analysis of samples by mass spectrometry: From elements to bio-molecules using laser ablation inductively couple plasma mass spectrometry and laser desorption/ionization mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Perdian, David C. [Iowa State Univ., Ames, IA (United States)


    Mass spectrometric methods that are able to analyze solid samples or biological materials with little or no sample preparation are invaluable to science as well as society. Fundamental research that has discovered experimental and instrumental parameters that inhibit fractionation effects that occur during the quantification of elemental species in solid samples by laser ablation inductively coupled plasma mass spectrometry is described. Research that determines the effectiveness of novel laser desorption/ionization mass spectrometric methods for the molecular analysis of biological tissues at atmospheric pressure and at high spatial resolution is also described. A spatial resolution is achieved that is able to analyze samples at the single cell level.

  15. High-throughput automated microfluidic sample preparation for accurate microbial genomics (United States)

    Kim, Soohong; De Jonghe, Joachim; Kulesa, Anthony B.; Feldman, David; Vatanen, Tommi; Bhattacharyya, Roby P.; Berdy, Brittany; Gomez, James; Nolan, Jill; Epstein, Slava; Blainey, Paul C.


    Low-cost shotgun DNA sequencing is transforming the microbial sciences. Sequencing instruments are so effective that sample preparation is now the key limiting factor. Here, we introduce a microfluidic sample preparation platform that integrates the key steps in cells to sequence library sample preparation for up to 96 samples and reduces DNA input requirements 100-fold while maintaining or improving data quality. The general-purpose microarchitecture we demonstrate supports workflows with arbitrary numbers of reaction and clean-up or capture steps. By reducing the sample quantity requirements, we enabled low-input (∼10,000 cells) whole-genome shotgun (WGS) sequencing of Mycobacterium tuberculosis and soil micro-colonies with superior results. We also leveraged the enhanced throughput to sequence ∼400 clinical Pseudomonas aeruginosa libraries and demonstrate excellent single-nucleotide polymorphism detection performance that explained phenotypically observed antibiotic resistance. Fully-integrated lab-on-chip sample preparation overcomes technical barriers to enable broader deployment of genomics across many basic research and translational applications. PMID:28128213

  16. A proteomics sample preparation method for mature, recalcitrant leaves of perennial plants.

    Directory of Open Access Journals (Sweden)

    Deng Gang

    Full Text Available Sample preparation is key to the success of proteomics studies. In the present study, two sample preparation methods were tested for their suitability on the mature, recalcitrant leaves of six representative perennial plants (grape, plum, pear, peach, orange, and ramie. An improved sample preparation method was obtained: Tris and Triton X-100 were added together instead of CHAPS to the lysis buffer, and a 20% TCA-water solution and 100% precooled acetone were added after the protein extraction for the further purification of protein. This method effectively eliminates nonprotein impurities and obtains a clear two-dimensional gel electrophoresis array. The method facilitates the separation of high-molecular-weight proteins and increases the resolution of low-abundance proteins. This method provides a widely applicable and economically feasible technology for the proteomic study of the mature, recalcitrant leaves of perennial plants.

  17. Automatic coal sample preparation system%煤炭自动制样系统

    Institute of Scientific and Technical Information of China (English)



    To solve the problems occurred during manual coal sample preparation,such as low work efficien-cy,high labor intensity,poor working environment,harmful to human beings and poor representativeness of the sample due to large error,the auto coal sample preparation system was designed.Performance tests like residue sample mass,fuel size,residue sample precision and sample preparation bias verified this system has met the requirements of GB/T 1 9494.3-2004 and GB 474-2008 on precision and bias.Its application not only improves the automation degree of sample preparation,but also reduces human disturbance factors in the sample preparation process.%为了解决电厂燃煤人工制样存在的工作效率低,劳动强度大,工作环境差,有害人体健康,误差大影响样品的代表性等问题,设计了煤炭自动制样系统.通过留样质量、出料粒径、留样精密度及制样偏倚等性能试验,证明该系统精密度和偏倚达到了 GB 474—2008和 GB/T 19494.3—2004规定的要求,其应用提高了样品制备的自动化程度,减少了制样过程人为因素的干扰.

  18. Direct determination of mercury in cosmetic samples by isotope dilution inductively coupled plasma mass spectrometry after dissolution with formic acid

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Ying; Shi, Zeming; Zong, Qinxia; Wu, Peng; Su, Jing [Sichuan Provincial Key Laboratory of Nuclear Technology in Geology, College of Nuclear Technology and Automation Engineering, Chengdu University of Technology, Chengdu 610059 (China); Liu, Rui, E-mail: [Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu 610059 (China)


    Graphical abstract: -- Highlights: •Simple, sensitive, and accurate method is established for mercury determination in cosmetics. •The sample preparation procedure is highly simplified. •Isotope dilution efficiently eliminates matrix effect. •First report of using formic acid based method in combination with PVG-ID-ICP MS for mercury quantitation in cosmetics. -- Abstract: A new method was proposed for the accurate determination of mercury in cosmetic samples based on isotopic dilution (ID)-photochemical vapor generation (PVG)-inductively coupled plasma mass spectrometry (ICP MS) measurement. Cosmetic samples were directly dissolved in formic acid solution and subsequently subjected to PVG for the reduction of mercury into vapor species following by ICP MS detection. Therefore, the risks of analyte contamination and loss were avoided. Highly enriched {sup 201}Hg isotopic spike is added to cosmetics and the isotope ratios of {sup 201}Hg/{sup 202}Hg were measured for the quantitation of mercury. With ID calibration, the influences originating from sample matrixes for the determination of mercury in cosmetic samples have been efficiently eliminated. The effects of several experimental parameters, such as the concentration of the formic acid, and the flow rates of carrier gas and sample were investigated. The method provided good reproducibility and the detection limits were found to be 0.6 pg mL{sup −1}. Finally, the developed method was successfully applied for the determination of mercury in six cosmetic samples and a spike test was performed to verify the accuracy of the method.

  19. Electric transport measurements on bulk, polycrystalline MgB2 samples prepared at various reaction temperatures (United States)

    Wiederhold, A.; Koblischka, M. R.; Inoue, K.; Muralidhar, M.; Murakami, M.; Hartmann, U.


    A series of disk-shaped, bulk MgB2 superconductors (sample diameter up to 4 cm) was prepared in order to improve the performance for superconducting super-magnets. Several samples were fabricated using a solid state reaction in pure Ar atmosphere from 750 to 950oC in order to determine the optimum processing parameters to obtain the highest critical current density as well as large trapped field values. Additional samples were prepared with added silver (up to 10 wt.-%) to the Mg and B powder. Magneto-resistance data and I/V-characteristics were recorded using an Oxford Instruments Teslatron system. From Arrhenius plots, we determine the TAFF pinning potential, U 0. The I/V-characteristics yield detailed information on the current flow through the polycrystalline samples. The current flow is influenced by the presence of pores in the samples. Our analysis of the achieved critical currents together with a thorough microstructure investigation reveals that the samples prepared at temperatures between 775°C and 805°C exhibit the smallest grains and the best connectivity between them, while the samples fabricated at higher reaction temperatures show a reduced connectivity and lower pinning potential. Doping the samples with silver leads to a considerable increase of the pinning potential and hence, the critical current densities.

  20. [Sample preparation methods for chromatographic analysis of organic components in atmospheric particulate matter]. (United States)

    Hao, Liang; Wu, Dapeng; Guan, Yafeng


    The determination of organic composition in atmospheric particulate matter (PM) is of great importance in understanding how PM affects human health, environment, climate, and ecosystem. Organic components are also the scientific basis for emission source tracking, PM regulation and risk management. Therefore, the molecular characterization of the organic fraction of PM has become one of the priority research issues in the field of environmental analysis. Due to the extreme complexity of PM samples, chromatographic methods have been the chief selection. The common procedure for the analysis of organic components in PM includes several steps: sample collection on the fiber filters, sample preparation (transform the sample into a form suitable for chromatographic analysis), analysis by chromatographic methods. Among these steps, the sample preparation methods will largely determine the throughput and the data quality. Solvent extraction methods followed by sample pretreatment (e. g. pre-separation, derivatization, pre-concentration) have long been used for PM sample analysis, and thermal desorption methods have also mainly focused on the non-polar organic component analysis in PM. In this paper, the sample preparation methods prior to chromatographic analysis of organic components in PM are reviewed comprehensively, and the corresponding merits and limitations of each method are also briefly discussed.

  1. Preparation and Performance of Plasma/Polymer Composite Coatings on Magnesium Alloy (United States)

    Bakhsheshi-Rad, H. R.; Hamzah, E.; Bagheriyan, S.; Daroonparvar, M.; Kasiri-Asgarani, M.; Shah, A. M.; Medraj, M.


    A triplex plasma (NiCoCrAlHfYSi/Al2O3·13%TiO2)/polycaprolactone composite coating was successfully deposited on a Mg-1.2Ca alloy by a combination of atmospheric plasma spraying and dip-coating techniques. The NiCoCrAlHfYSi (MCrAlHYS) coating, as the first layer, contained a large number of voids, globular porosities, and micro-cracks with a thickness of 40-50 μm, while the Al2O3·13%TiO2 coating, as the second layer, presented a unique bimodal microstructure with a thickness of 70-80 μm. The top layer was a hydrophobic polymer, which effectively sealed the porosities of plasma layers. The results of micro-hardness and bonding strength tests showed that the plasma coating presented excellent hardness (870 HV) and good bonding strength (14.8 MPa). However, the plasma/polymer coatings interface exhibited low bonding strength (8.6 MPa). The polymer coating formed thick layer (100-110 μm) that homogeneously covered the surface of the plasma layers. Contact angle measurement showed that polymer coating over plasma layers significantly decreased surface wettability. The corrosion current density ( i corr) of an uncoated sample (262.7 µA/cm2) decreased to 76.9 µA/cm2 after plasma coatings were applied. However, it was found that the i corr decreased significantly to 0.002 µA/cm2 after polymer sealing of the porous plasma layers.

  2. Synthesis and Characterization of Nanofibrous Polyaniline Thin Film Prepared by Novel Atmospheric Pressure Plasma Polymerization Technique

    Directory of Open Access Journals (Sweden)

    Choon-Sang Park


    Full Text Available This work presents a study on the preparation of plasma-polymerized aniline (pPANI nanofibers and nanoparticles by an intense plasma cloud type atmospheric pressure plasma jets (iPC-APPJ device with a single bundle of three glass tubes. The nano size polymer was obtained at a sinusoidal wave with a peak value of 8 kV and a frequency of 26 kHz under ambient air. Discharge currents, photo-sensor amplifier, and optical emission spectrometer (OES techniques were used to analyze the plasma produced from the iPC-APPJ device. Field emission scanning electron microscopy (FE-SEM, transmission electron microscopy (TEM, Fourier transform infrared spectroscopy (FT-IR, gas chromatography-mass spectrometry (GC-MS, and gel permeation chromatography (GPC techniques were used to analyze the pPANI. FE-SEM and TEM results show that pPANI has nanofibers, nanoparticles morphology, and polycrystalline characteristics. The FT-IR and GC-MS analysis show the characteristic polyaniline peaks with evidence that some quinone and benzene rings are broken by the discharge energy. GPC results show that pPANI has high molecular weight (Mw, about 533 kDa with 1.9 polydispersity index (PDI. This study contributes to a better understanding on the novel growth process and synthesis of uniform polyaniline nanofibers and nanoparticles with high molecular weights using the simple atmospheric pressure plasma polymerization technique.

  3. Electrochemical Evaluation of Thin-Film Li-Si Anodes Prepared by Plasma Spraying

    Energy Technology Data Exchange (ETDEWEB)



    Thin-film electrodes of a plasma-sprayed Li-Si alloy were evaluated for use as anodes in high-temperature thermally activated (thermal) batteries. These anodes were prepared using 44% Li/56% Si (w/w) material as feed material in a special plasma-spray apparatus under helium or hydrogen, to protect this air- and moisture-sensitive material during deposition. Anodes were tested in single cells using conventional pressed-powder separators and lithiated pyrite cathodes at temperatures of 400 to 550 C at several different current densities. A limited number of 5-cell battery tests were also conducted. The data for the plasma-sprayed anodes was compared to that for conventional pressed-powder anodes. The performance of the plasma-sprayed anodes was inferior to that of conventional pressed-powder anodes, in that the cell emfs were lower (due to the lack of formation of the desired alloy phases) and the small porosity of these materials severely limited their rate capability. Consequently, plasma-sprayed Li-Si anodes would not be practical for use in thermal batteries.

  4. Fibrin glue from stored human plasma. An inexpensive and efficient method for local blood bank preparation. (United States)

    Spotnitz, W D; Mintz, P D; Avery, N; Bithell, T C; Kaul, S; Nolan, S P


    European surgeons have used fibrin glue extensively during thoracic, cardiovascular, and general surgical operations. Until now, however, it has been available only as a commercial preparation made from pooled human plasma, and it has not been approved by the U.S. Food and Drug Administration for use in the United States because of a high associated risk of hepatitis and acquired immune deficiency syndrome. Methods of obtaining fibrinogen, an essential component of fibrin glue, from cryoprecipitate or fresh frozen plasma have been published recently. However, the cryoprecipitate method results in relatively low concentrations of fibrinogen, which can reduce glue effectiveness. The fresh frozen plasma method is more expensive and does not meet the standards of the American Association of Blood Banks for the "closed" system required for safe handling and management of blood component products. Both the cryoprecipitate and the fresh frozen plasma methods result in waste of unstable clotting factors. These factors are necessary to replace human plasma clotting deficiencies but are not necessary for the production of fibrin glue. The authors have developed an efficient, high-concentration blood bank method for producing and maintaining a local supply of a safer and less expensive but equally effective material derived from stored human plasma. This material is produced using approved blood bank techniques for a "closed" system in blood component production, thus reducing the risks of contamination and infection, and its fibrinogen concentration is higher than that of standard cryoprecipitate. The cost of 1 unit of this fibrin glue is comparable to that for 1 unit of cryoprecipitate and less than that for 1 unit of fresh frozen plasma.(ABSTRACT TRUNCATED AT 250 WORDS)

  5. Molecularly imprinted polymers for sample preparation and biosensing in food analysis: Progress and perspectives

    DEFF Research Database (Denmark)

    Ashley, Jon; Shahbazi, Mohammad-Ali; Kant, Krishna


    Molecularly imprinted polymers (MIPs) are biomimetics which can selectively bind to analytes of interest. One of the most interesting areas where MIPs have shown the biggest potential is food analysis. MIPs have found use as sorbents in sample preparation attributed to the high selectivity and high...... the imprinting methods which are applicable for imprinting food templates, summarize the recent progress in using MIPs for preparing and analysing food samples, and discuss the current limitations in the commercialisation of MIPs technology. Finally, future perspectives will be given....

  6. Analysis of aroma compounds of Roselle by Dynamic Headspace Sampling using different preparation methods

    DEFF Research Database (Denmark)

    Juhari, Nurul Hanisah Binti; Varming, Camilla; Petersen, Mikael Agerlin


    The influence of different methods of sample preparation on the aroma profiles of dried Roselle (Hibiscus sabdariffa) was studied. Least amounts of aroma compounds were recovered by analysis of whole dry calyxes (WD) followed by ground dry (GD), blended together with water (BTW), and ground...... and then mixed with water (GMW). The highest number of aroma compounds was found in Roselle treated in water bath (2hr/40°C) (GMWKB). GMW was chosen as the preparation method because it was shown to be an efficient extraction method without the possibility of excessive chemical changes of the sample....

  7. HPLC analysis of oxindole alkaloids in Uncaria tomentosa: sample preparation and analysis optimisation by factorial design. (United States)

    Bertol, Gustavo; Franco, Luzia; Oliveira, Brás Heleno de


    Uncaria tomentosa ("cat's claw") is widely used for the treatment of some infectious and inflammatory diseases. Oxindole alkaloids are regarded as the most important components responsible for the biological activities attributed to the plant. Their analysis require efficient sample preparation and suitable reference standards but few are commercially available. To develop and validate a HPLC analytical method for oxindole alkaloids in Uncaria tomentosa with emphasis on sample preparation. Factorial experimental designs were used for the optimisation of both sample preparation and chromatographic separation. The optimised sample preparation involved extraction with aqueous ethanol, and the granulometry of the powdered plant material significantly influenced extraction yields. Mitraphylline was used as a calibration reference for the determination of total alkaloids. The method was fully validated and showed good selectivity, linearity (r²  ≥ 0.9996), accuracy (≥ 96%) and precision (RSD < 2.4%). Detection and quantification limits for mitraphylline were 0.8 and 2.4 ppm, respectively. The optimised chromatographic method, using organic buffer in the mobile phase, provided baseline separation of tetracyclic and pentacyclic alkaloids in the samples. Calibration using mitraphylline provided more accurate estimates of total alkaloid content when compared to other available reference alkaloids. Copyright © 2011 John Wiley & Sons, Ltd.

  8. Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation (United States)

    Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)


    An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

  9. Validation of a fully automated robotic setup for preparation of whole blood samples for LC-MS toxicology analysis

    DEFF Research Database (Denmark)

    Andersen, David Wederkinck; Rasmussen, Brian; Linnet, Kristian


    A fully automated setup was developed for preparing whole blood samples using a Tecan Evo workstation. By integrating several add-ons to the robotic platform, the flexible setup was able to prepare samples from sample tubes to a 96-well sample plate ready for injection on liquid chromatography...

  10. Recent advances in sample preparation techniques and methods of sulfonamides detection - A review. (United States)

    Dmitrienko, Stanislava G; Kochuk, Elena V; Apyari, Vladimir V; Tolmacheva, Veronika V; Zolotov, Yury A


    Sulfonamides (SAs) have been the most widely used antimicrobial drugs for more than 70 years, and their residues in foodstuffs and environmental samples pose serious health hazards. For this reason, sensitive and specific methods for the quantification of these compounds in numerous matrices have been developed. This review intends to provide an updated overview of the recent trends over the past five years in sample preparation techniques and methods for detecting SAs. Examples of the sample preparation techniques, including liquid-liquid and solid-phase extraction, dispersive liquid-liquid microextraction and QuEChERS, are given. Different methods of detecting the SAs present in food and feed and in environmental, pharmaceutical and biological samples are discussed.

  11. Efficient discrimination and removal of phospholipids during electromembrane extraction from human plasma samples

    DEFF Research Database (Denmark)

    Vårdal, Linda; Gjelstad, Astrid; Huang, Chuixiu


    AIM: For the first time, extracts obtained from human plasma samples by electromembrane extraction (EME) were investigated comprehensively with particular respect to phospholipids using ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Thhe purpose was to invest...

  12. Measurement of glomerular filtration rate in adults: accuracy of five single-sample plasma clearance methods

    DEFF Research Database (Denmark)

    Rehling, M; Rabøl, A


    After an intravenous injection of a tracer that is removed from the body solely by filtration in the kidneys, the glomerular filtration rate (GFR) can be determined from its plasma clearance. The method requires a great number of blood samples but collection of urine is not needed. In the present...

  13. Author Contribution to the Pu Handbook II: Chapter 37 LLNL Integrated Sample Preparation Glovebox (TEM) Section

    Energy Technology Data Exchange (ETDEWEB)

    Wall, Mark A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)


    The development of our Integrated Actinide Sample Preparation Laboratory (IASPL) commenced in 1998 driven by the need to perform transmission electron microscopy studies on naturally aged plutonium and it’s alloys looking for the microstructural effects of the radiological decay process (1). Remodeling and construction of a laboratory within the Chemistry and Materials Science Directorate facilities at LLNL was required to turn a standard radiological laboratory into a Radiological Materials Area (RMA) and Radiological Buffer Area (RBA) containing type I, II and III workplaces. Two inert atmosphere dry-train glove boxes with antechambers and entry/exit fumehoods (Figure 1), having a baseline atmosphere of 1 ppm oxygen and 1 ppm water vapor, a utility fumehood and a portable, and a third double-walled enclosure have been installed and commissioned. These capabilities, along with highly trained technical staff, facilitate the safe operation of sample preparation processes and instrumentation, and sample handling while minimizing oxidation or corrosion of the plutonium. In addition, we are currently developing the capability to safely transfer small metallographically prepared samples to a mini-SEM for microstructural imaging and chemical analysis. The gloveboxes continue to be the most crucial element of the laboratory allowing nearly oxide-free sample preparation for a wide variety of LLNL-based characterization experiments, which includes transmission electron microscopy, electron energy loss spectroscopy, optical microscopy, electrical resistivity, ion implantation, X-ray diffraction and absorption, magnetometry, metrological surface measurements, highpressure diamond anvil cell equation-of-state, phonon dispersion measurements, X-ray absorption and emission spectroscopy, and differential scanning calorimetry. The sample preparation and materials processing capabilities in the IASPL have also facilitated experimentation at world-class facilities such as the

  14. Preparing to Receive and Handle Martian Samples When They Arrive on Earth (United States)

    McCubbin, Francis M.


    The Astromaterials Acquisition and Curation Office at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10F+ derivative NPR 'Curation of Extraterrestrial Materials', JSC is charged with 'The curation of all extraterrestrial material under NASA control, including future NASA missions. 'The Directive goes on to define Curation as including'...documentation, preservation, preparation, and distribution of samples for research, education, and public outreach."

  15. Crystal structure, microstructure, and thermoelectric properties of GeSb{sub 6}Te{sub 10} prepared by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Kosuga, Atsuko, E-mail: [Nanoscience and Nanotechnology Research Center, Research Organization for the 21st Century, Osaka Prefecture University, Sakai 599-8570 (Japan); Nakai, Kazuki [Nanoscience and Nanotechnology Research Center, Research Organization for the 21st Century, Osaka Prefecture University, Sakai 599-8570 (Japan); Department of Physical Science, Graduate School of Science, Osaka Prefecture University, Sakai 599-8531 (Japan); Matsuzawa, Mie; Fujii, Yousuke [Nanoscience and Nanotechnology Research Center, Research Organization for the 21st Century, Osaka Prefecture University, Sakai 599-8570 (Japan); Funahashi, Ryoji [Research Institute for Ubiquitous Energy Devices, National Institute of Advanced Industrial Science and Technology, Ikeda 563-8577 (Japan); Tachizawa, Takuya; Kubota, Yoshiki [Department of Physical Science, Graduate School of Science, Osaka Prefecture University, Sakai 599-8531 (Japan); Kifune, Kouichi [Department of Physical Science, Graduate School of Science, Osaka Prefecture University, Sakai 599-8531 (Japan); Faculty of Engineering, Hiroshima Institute of Technology, Hiroshima 731-5193 (Japan)


    Highlights: • Spark plasma sintering effects on GeSb{sub 6}Te{sub 10} properties are described. • Sintered GeSb{sub 6}Te{sub 10} contains homologous GeSb{sub 6}Te{sub 10} and Sb{sub 2}Te{sub 3} tetradymite structures. • Spark plasma sintering causes elemental compositional deviations from GeSb{sub 6}Te{sub 10}. • SPS-consolidated and melt-prepared samples have similar ZT{sub max} values. • Spark plasma sintering significantly changes crystal structure and microstructure. - Abstract: We report the effects of spark plasma sintering (SPS) and subsequent annealing on the crystal structure, microstructure, and thermoelectric properties of polycrystalline GeSb{sub 6}Te{sub 10}. GeSb{sub 6}Te{sub 10} consolidated using SPS consisted of a mixture of GeSb{sub 6}Te{sub 10}-type homologous and Sb{sub 2}Te{sub 3}-type tetradymite structures, whereas the sample prepared by melting had a single homologous structure. SPS produced small amounts of Ge-rich precipitates with a few micrometers in size. Even excluding these precipitates, the elemental compositional deviation from the nominal composition was wider than that for the sample prepared by melting. This implies that SPS promoted atomic diffusion and rearrangement of elements, leading to a substantial change in the crystal structure and elemental distribution of GeSb{sub 6}Te{sub 10}. SPS improved the power factor but also increased the thermal conductivity, as a result of the increased electrical conductivity, yielding a maximum dimensionless figure of merit, ZT{sub max}, of 0.33 at 710 K, which is similar to the value for the sample prepared by melting (0.39 at 710 K)

  16. Nanocomposite metal/plasma polymer films prepared by means of gas aggregation cluster source

    Energy Technology Data Exchange (ETDEWEB)

    Polonskyi, O.; Solar, P.; Kylian, O.; Drabik, M.; Artemenko, A.; Kousal, J.; Hanus, J.; Pesicka, J.; Matolinova, I. [Charles University in Prague, Faculty of Mathematics and Physics, V Holesovickach 2, 18000 Prague 8 (Czech Republic); Kolibalova, E. [Tescan, Libusina trida 21, 632 00 Brno (Czech Republic); Slavinska, D. [Charles University in Prague, Faculty of Mathematics and Physics, V Holesovickach 2, 18000 Prague 8 (Czech Republic); Biederman, H., E-mail: [Charles University in Prague, Faculty of Mathematics and Physics, V Holesovickach 2, 18000 Prague 8 (Czech Republic)


    Nanocomposite metal/plasma polymer films have been prepared by simultaneous plasma polymerization using a mixture of Ar/n-hexane and metal cluster beams. A simple compact cluster gas aggregation source is described and characterized with emphasis on the determination of the amount of charged clusters and their size distribution. It is shown that the fraction of neutral, positively and negatively charged nanoclusters leaving the gas aggregation source is largely influenced by used operational conditions. In addition, it is demonstrated that a large portion of Ag clusters is positively charged, especially when higher currents are used for their production. Deposition of nanocomposite Ag/C:H plasma polymer films is described in detail by means of cluster gas aggregation source. Basic characterization of the films is performed using transmission electron microscopy, ultraviolet-visible and Fourier-transform infrared spectroscopies. It is shown that the morphology, structure and optical properties of such prepared nanocomposites differ significantly from the ones fabricated by means of magnetron sputtering of Ag target in Ar/n-hexane mixture.

  17. Optimization of sample preparation for accurate results in quantitative NMR spectroscopy (United States)

    Yamazaki, Taichi; Nakamura, Satoe; Saito, Takeshi


    Quantitative nuclear magnetic resonance (qNMR) spectroscopy has received high marks as an excellent measurement tool that does not require the same reference standard as the analyte. Measurement parameters have been discussed in detail and high-resolution balances have been used for sample preparation. However, the high-resolution balances, such as an ultra-microbalance, are not general-purpose analytical tools and many analysts may find those balances difficult to use, thereby hindering accurate sample preparation for qNMR measurement. In this study, we examined the relationship between the resolution of the balance and the amount of sample weighed during sample preparation. We were able to confirm the accuracy of the assay results for samples weighed on a high-resolution balance, such as the ultra-microbalance. Furthermore, when an appropriate tare and amount of sample was weighed on a given balance, accurate assay results were obtained with another high-resolution balance. Although this is a fundamental result, it offers important evidence that would enhance the versatility of the qNMR method.

  18. A novel method for sample preparation of fresh lung cancer tissue for proteomics analysis by tumor cell enrichment and removal of blood contaminants

    Directory of Open Access Journals (Sweden)

    Orre Lotta


    Full Text Available Abstract Background In-depth proteomics analyses of tumors are frequently biased by the presence of blood components and stromal contamination, which leads to large experimental variation and decreases the proteome coverage. We have established a reproducible method to prepare freshly collected lung tumors for proteomics analysis, aiming at tumor cell enrichment and reduction of plasma protein contamination. We obtained enriched tumor-cell suspensions (ETS from six lung cancer cases (two adenocarcinomas, two squamous-cell carcinomas, two large-cell carcinomas and from two normal lung samples. The cell content of resulting ETS was evaluated with immunocytological stainings and compared with the histologic pattern of the original specimens. By means of a quantitative mass spectrometry-based method we evaluated the reproducibility of the sample preparation protocol and we assessed the proteome coverage by comparing lysates from ETS samples with the direct lysate of corresponding fresh-frozen samples. Results Cytological analyses on cytospin specimens showed that the percentage of tumoral cells in the ETS samples ranged from 20% to 70%. In the normal lung samples the percentage of epithelial cells was less then 10%. The reproducibility of the sample preparation protocol was very good, with coefficient of variation at the peptide level and at the protein level of 13% and 7%, respectively. Proteomics analysis led to the identification of a significantly higher number of proteins in the ETS samples than in the FF samples (244 vs 109, respectively. Albumin and hemoglobin were among the top 5 most abundant proteins identified in the FF samples, showing a high contamination with blood and plasma proteins, whereas ubiquitin and the mitochondrial ATP synthase 5A1 where among the top 5 most abundant proteins in the ETS samples. Conclusion The method is feasible and reproducible. We could obtain a fair enrichment of cells but the major benefit of the method

  19. Soil and Water – What is Detectable through Microbiological Sample Preparation Techniques (United States)

    The concerns of a potential terrorist’s use of biological agents in soil and ground water are articulated by comparisons to major illnesses in this Country involving contaminated drinking water sources. Objectives are focused on the importance of sample preparation in the rapid, ...

  20. Analysis of biopharmaceutical proteins in biological matrices by LC-MS/MS I. Sample preparation

    NARCIS (Netherlands)

    Bischoff, Rainer; Bronsema, Kees J.; van de Merbel, Nico C.


    Part I of this review discusses sample-preparation aspects of quantifying biopharmaceutical proteins in complex biological matrices by LC-MS/MS with a focus on blood-derived body fluids. We conclude Part I with a short overview over options for automating the entire analytical procedure, which is

  1. Analysis of biopharmaceutical proteins in biological matrices by LC-MS/MS I. Sample preparation

    NARCIS (Netherlands)

    Bischoff, Rainer; Bronsema, Kees J.; van de Merbel, Nico C.


    Part I of this review discusses sample-preparation aspects of quantifying biopharmaceutical proteins in complex biological matrices by LC-MS/MS with a focus on blood-derived body fluids. We conclude Part I with a short overview over options for automating the entire analytical procedure, which is in

  2. Challenges of sample preparation for cross sectional EBSD analysis of electrodeposited nickel films

    DEFF Research Database (Denmark)

    Alimadadi, Hossein; Pantleon, Karen


    . Different procedures for sample preparation including mechanical grinding and polishing, electropolishing and focused ion beam milling have been applied to a nickel film electrodeposited on top of an amorphous Ni-P layer on a Cu-substrate. Reliable EBSD analysis of the whole cross section can be obtained...

  3. Standardized Sample Preparation Using a Drop-on-Demand Printing Platform

    Directory of Open Access Journals (Sweden)

    Paul M. Pellegrino


    Full Text Available Hazard detection systems must be evaluated with appropriate test material concentrations under controlled conditions in order to accurately identify and quantify unknown residues commonly utilized in theater. The existing assortment of hazard reference sample preparation methods/techniques presents a range of variability and reproducibility concerns, making it increasingly difficult to accurately assess optically- based detection technologies. To overcome these challenges, we examined the optimization, characterization, and calibration of microdroplets from a drop-on-demand microdispenser that has a proven capability for the preparation of energetic reference materials. Research presented herein focuses on the development of a simplistic instrument calibration technique and sample preparation protocol for explosive materials testing based on drop-on-demand technology. Droplet mass and reproducibility were measured using ultraviolet-visible (UV-Vis absorption spectroscopy. The results presented here demonstrate the operational factors that influence droplet dispensing for specific materials (e.g., energetic and interferents. Understanding these parameters permits the determination of droplet and sample uniformity and reproducibility (typical R2 values of 0.991, relative standard deviation or RSD ≤ 5%, and thus the demonstrated maturation of a successful and robust methodology for energetic sample preparation.

  4. Sample preparation composite and replicate strategy case studies for assay of solid oral drug products. (United States)

    Nickerson, Beverly; Harrington, Brent; Li, Fasheng; Guo, Michele Xuemei


    Drug product assay is one of several tests required for new drug products to ensure the quality of the product at release and throughout the life cycle of the product. Drug product assay testing is typically performed by preparing a composite sample of multiple dosage units to obtain an assay value representative of the batch. In some cases replicate composite samples may be prepared and the reportable assay value is the average value of all the replicates. In previously published work by Harrington et al. (2014) [5], a sample preparation composite and replicate strategy for assay was developed to provide a systematic approach which accounts for variability due to the analytical method and dosage form with a standard error of the potency assay criteria based on compendia and regulatory requirements. In this work, this sample preparation composite and replicate strategy for assay is applied to several case studies to demonstrate the utility of this approach and its application at various stages of pharmaceutical drug product development. Copyright © 2017. Published by Elsevier B.V.

  5. A novel sample preparation method to avoid influence of embedding medium during nano-indentation (United States)

    Yujie Meng; Siqun Wang; Zhiyong Cai; Timothy M. Young; Guanben Du; Yanjun Li


    The effect of the embedding medium on the nano-indentation measurements of lignocellulosic materials was investigated experimentally using nano-indentation. Both the reduced elastic modulus and the hardness of nonembedded cell walls were found to be lower than those of the embedded samples, proving that the embedding medium used for specimen preparation on cellulosic...

  6. Sample preparation for combined chemical analysis and bioassay application in water quality assessment

    NARCIS (Netherlands)

    Kolkman, A.; Schriks, M.; Brand, W; Bäuerlein, P.S.; van der Kooi, M.M.E.; van Doorn, R.H.; Emke, E.; Reus, A.; van der Linden, S.; de Voogt, P.; Heringa, M.B.


    The combination of in vitro bioassays and chemical screening can provide a powerful toolbox to determine biologically relevant compounds in water extracts. In this study, a sample preparation method is evaluated for the suitability for both chemical analysis and in vitro bioassays. A set of 39 chemi

  7. Durable antibacterial Ag/polyacrylonitrile (Ag/PAN) hybrid nanofibers prepared by atmospheric plasma treatment and electrospinning (United States)

    Durable antibacterial Ag/polyacrylonitrile (Ag/PAN) hybrid nanofibers were prepared by atmospheric plasma treatment and electrospinning. Atmospheric helium plasma treatment was first used to reduce the silver nitrate precursor in pre-electrospinning solutions into metallic silver nanoparticles, foll...

  8. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry (United States)

    Montaser, A.

    This research follows a multifaceted approach, from theory to practice, to the investigation and development of novel helium plasmas, sample introduction systems, and diagnostic techniques for atomic and mass spectrometries. During the period January 1994 - December 1994, four major sets of challenging research programs were addressed that each included a number of discrete but complementary projects: (1) The first program is concerned with fundamental and analytical investigations of novel atmospheric-pressure helium inductively coupled plasmas (He ICPS) that are suitable for the atomization-excitation-ionization of elements, especially those possessing high excitation and ionization energies, for the purpose of enhancing sensitivity and selectivity of analytical measurements. (2) The second program includes simulation and computer modeling of He ICPS. The aim is to ease the hunt for new helium plasmas by predicting their structure and fundamental and analytical properties, without incurring the enormous cost for extensive experimental studies. (3) The third program involves spectroscopic imaging and diagnostic studies of plasma discharges to instantly visualize their prevailing structures, to quantify key fundamental properties, and to verify predictions by mathematical models. (4) The fourth program entails investigation of new, low-cost sample introduction systems that consume micro- to nanoliter quantity of sample solution in plasma spectrometries. A portion of this research involves development and applications of novel diagnostic techniques suitable for probing key fundamental properties of aerosol prior to and after injection into high-temperature plasmas. These efforts, still in progress, collectively offer promise of solving singularly difficult analytical problems that either exist now or are likely to arise in the future in the various fields of energy generation, environmental pollution, material science, biomedicine and nutrition.

  9. The role of sample preparation in interpretation of trace element concentration variability in moss bioindication studies (United States)

    Migaszewski, Z.M.; Lamothe, P.J.; Crock, J.G.; Galuszka, A.; Dolegowska, S.


    Trace element concentrations in plant bioindicators are often determined to assess the quality of the environment. Instrumental methods used for trace element determination require digestion of samples. There are different methods of sample preparation for trace element analysis, and the selection of the best method should be fitted for the purpose of a study. Our hypothesis is that the method of sample preparation is important for interpretation of the results. Here we compare the results of 36 element determinations performed by ICP-MS on ashed and on acid-digested (HNO3, H2O2) samples of two moss species (Hylocomium splendens and Pleurozium schreberi) collected in Alaska and in south-central Poland. We found that dry ashing of the moss samples prior to analysis resulted in considerably lower detection limits of all the elements examined. We also show that this sample preparation technique facilitated the determination of interregional and interspecies differences in the chemistry of trace elements. Compared to the Polish mosses, the Alaskan mosses displayed more positive correlations of the major rock-forming elements with ash content, reflecting those elements' geogenic origin. Of the two moss species, P. schreberi from both Alaska and Poland was also highlighted by a larger number of positive element pair correlations. The cluster analysis suggests that the more uniform element distribution pattern of the Polish mosses primarily reflects regional air pollution sources. Our study has shown that the method of sample preparation is an important factor in statistical interpretation of the results of trace element determinations. ?? 2010 Springer-Verlag.

  10. Preparation and characterisation of magnetic nanostructured samples for inelastic neutron scattering experiments

    Energy Technology Data Exchange (ETDEWEB)

    Kreuzpaintner, Wolfgang


    Recent advances in thin-film structuring techniques have generated significant interest in the dynamics of spin waves in magnetic nanostructures and the possible use of inelastic neutron scattering (INS) for their investigation. This thesis describes the design and implementation, at GKSS Research Centre, of equipment for preparation of large and laterally submicron and nanometre structured magnetic samples for such future INS experiments. After a brief resume on spin waves in nanostructures, the development work on new purpose-designed equipment, including high vacuum (HV) argon ion beam milling and ultra high vacuum (UHV) e-beam evaporation setups, is described. Ni nanodot as well as Ni and novel Gd nanowire samples were prepared using combinations of sputter deposition, laser interference lithography, argon ion beam milling, e-beam evaporation and self organisation techniques. With reference to sample preparation, epitaxial growth studies for Ni on Si(100) substrate were performed, resulting in the development of a new deposition process, which by thermal tuning allows for the direct epitaxial growth of Ni on Si with unprecedented crystalline quality. The results of various characterisation experiments on the prepared nanostructured samples, including Scanning Electron Microscopy (SEM), microprobe analysis, Atomic and Magnetic Force Microscopy (AFM/MFM), Vibrating Sample Magnetometry (VSM), X-ray Diffraction (XRD) and Reflectivity (XRR), unpolarised and Polarised Neutron Scattering (PNR) and off-specular scattering by X-rays and neutrons using rocking scans and Time-Of-Flight Grazing Incidence Small Angle Neutron Scattering (TOF-GISANS), together with various analysis procedures such as Distorted-Wave Born Approximation (DWBA), are reported. The analysis of a Gd nanowire sample by TOF-GISANS led to a novel evaluation technique which in comparison with single wavelength methods allows portions of reciprocal space to be scanned without changing the angle of

  11. Preparation of magnetized nanodusty plasmas in a radio frequency-driven parallel-plate reactor

    Energy Technology Data Exchange (ETDEWEB)

    Tadsen, Benjamin, E-mail:; Greiner, Franko; Piel, Alexander [IEAP, Christian-Albrechts-Universität, D-24098 Kiel (Germany)


    Nanodust is produced in an rf-driven push-pull parallel-plate reactor using argon with an acetylene admixture at 5–30 Pa. A scheme for the preparation of nanodust clouds with particle radii up to 400 nm for investigations in magnetized plasmas is proposed. The confinement that keeps the nanodust of different radii inside a moderately magnetized discharge (B ≤ 500 mT) is investigated by a comparison of 2d-Langmuir probe measurements in the dust-free plasma without and with a magnetic field and by the analysis of scattered light of nanodust clouds. It is shown that the dust cloud changes its shape when the dust density changes. This results in a reversed α-γ{sup ′} transition from a dense dust cloud with a central disk-like void to a dilute dust cloud with a toroidal void. When the dust density is further reduced, filaments are observed in the central part of the cloud, which were absent in the high-density phase. It is concluded that the dense nanodust cloud is able to suppress plasma filamentation in magnetized plasmas.

  12. Effects of fruit and vegetable consumption on total antioxidant capacity of fasting and postprandial plasma samples

    DEFF Research Database (Denmark)

    Ravn-Haren, Gitte; Dragsted, L. O.; Pedersen, A.


    Fruits and vegetables are known to protect against cancer and heart disease. This is often ascribed to their high content of antioxidants. We have therefore tested whether a daily intake of fruits and vegetables corresponding to the recommended 600 g had any effect on the antioxidant activity of ...... of fasting and postprandial plasma samples. Antioxidant activity was determined by the Trolox Equivalent Antioxidant Capacity (TEAC) assay and the Ferric Reducing Ability of Plasma (FRAP) assay, which have been reported to be affected by the presence of dietary antioxidants....

  13. Gas Diffusion Barriers Prepared by Spatial Atmospheric Pressure Plasma Enhanced ALD. (United States)

    Hoffmann, Lukas; Theirich, Detlef; Pack, Sven; Kocak, Firat; Schlamm, Daniel; Hasselmann, Tim; Fahl, Henry; Räupke, André; Gargouri, Hassan; Riedl, Thomas


    In this work, we report on aluminum oxide (Al2O3) gas permeation barriers prepared by spatial ALD (SALD) at atmospheric pressure. We compare the growth characteristics and layer properties using trimethylaluminum (TMA) in combination with an Ar/O2 remote atmospheric pressure plasma for different substrate velocities and different temperatures. The resulting Al2O3 films show ultralow water vapor transmission rates (WVTR) on the order of 10(-6) gm(-2)d(-1). In notable contrast, plasma based layers already show good barrier properties at low deposition temperatures (75 °C), while water based processes require a growth temperature above 100 °C to achieve equally low WVTRs. The activation energy for the water permeation mechanism was determined to be 62 kJ/mol.

  14. Analysis of inflammatory response in human plasma samples by an automated multicapillary electrophoresis system. (United States)

    Larsson, Anders; Hansson, Lars-Olof


    A new automated multicapillary zone electrophoresis instrument with a new high-resolution (HR) buffer (Capillarys with HR buffer) for analysis of human plasma proteins was evaluated. Albumin, alpha(1)-antitrypsin, alpha(1)-acid glycoprotein, haptoglobin, fibrinogen, immunoglobulin (Ig)A, IgG and IgM were determined nephelometrically in 200 patient plasma samples. The same samples were then analyzed on the Capillarys system (Sebia, Paris, France). The albumin concentration from the nephelometric determination was used for quantification of the individual peaks in the capillary electrophoresis (CE) electropherogram. There was strong linear correlation between the nephelometric and electrophoretic determination of alpha(1)-antitrypsin (R(2) = 0.906), alpha(1)-acid glycoprotein (R(2) =0.894) and haptoglobin (R(2) = 0.913). There was also good correlation between the two determinations of gamma-globulins (R(2) = 0.883), while the correlation was weaker for fibrinogen (R(2) = 0.377). The Capillarys instrument is a reliable system for plasma protein analysis, combining the advantages of full automation, good analytical performance and high throughput. The HR buffer in combination with albumin quantification allows the simultaneous quantification of inflammatory markers in plasma samples without the need for nephelometric determination of these proteins.

  15. TiC0.5N0.5-Based Cermets with Varied Amounts of Si3N4 Nanopowders Prepared by Spark Plasma Sintering

    Directory of Open Access Journals (Sweden)

    Changchun Lv


    Full Text Available TiCN-based cermets with varied fractions of Si3N4 nanopowder (0–5 wt.% were prepared by spark plasma sintering. The microstructural and mechanical properties of these cermets were investigated. In general, with increasing addition amount of Si3N4 nanopowder the relative density as well as mechanical properties of the as-prepared TiCN cermets increased first and then decreased. The samples containing 2 wt.% Si3N4 nanopowder presented the best performance with the relative density of about 98%, bending strength of 1000 MPa, and Vickers microhardness of about 1810 HV10.

  16. Community-Level Physiological Profiling of Microbial Communities in Constructed Wetlands: Effects of Sample Preparation. (United States)

    Button, Mark; Weber, Kela; Nivala, Jaime; Aubron, Thomas; Müller, Roland Arno


    Community-level physiological profiling (CLPP) using BIOLOG® EcoPlates™ has become a popular method for characterizing and comparing the functional diversity, functional potential, and metabolic activity of heterotrophic microbial communities. The method was originally developed for profiling soil communities; however, its usage has expanded into the fields of ecotoxicology, agronomy, and the monitoring and profiling of microbial communities in various wastewater treatment systems, including constructed wetlands for water pollution control. When performing CLPP on aqueous samples from constructed wetlands, a wide variety of sample characteristics can be encountered and challenges may arise due to excessive solids, color, or turbidity. The aim of this study was to investigate the impacts of different sample preparation methods on CLPP performed on a variety of aqueous samples covering a broad range of physical and chemical characteristics. The results show that using filter paper, centrifugation, or settling helped clarify samples for subsequent CLPP analysis, however did not do so as effectively as dilution for the darkest samples. Dilution was able to provide suitable clarity for the darkest samples; however, 100-fold dilution significantly affected the carbon source utilization patterns (CSUPs), particularly with samples that were already partially or fully clear. Ten-fold dilution also had some effect on the CSUPs of samples which were originally clear; however, the effect was minimal. Based on these findings, for this specific set of samples, a 10-fold dilution provided a good balance between ease of use, sufficient clarity (for dark samples), and limited effect on CSUPs. The process and findings outlined here can hopefully serve future studies looking to utilize CLPP for functional analysis of microbial communities and also assist in comparing data from studies where different sample preparation methods were utilized.

  17. Isolation and purification of heroin from heroin street samples by preparative high performance liquid chromatography. (United States)

    Guo, Zhen; Zheng, Hui; Lu, Yanzhen; Wei, Yun


    The present study established a novel method using preparative high performance liquid chromatography to isolate and purify heroin·HCl from heroin street samples to be used as a reference standard. Different kinds of mobile phases and columns were used, ultimately the mobile phase consisting of hexane-isopropanol-methanol (65:28:7, v/v) and the SIL preparative column prepared in laboratory were selected as the final condition. Heroin was further purified by the drowning-out crystallization method using isopropanol-methanol (50:1, v/v) and hexane as drowning-out anti-solvents and salting-out agents, respectively. The purity was assessed by analytical high performance liquid chromatography and the confirmation of the chemical structure was performed by IR and NMR. About 110.7mg of heroin·HCl at a purity of over 99.52% was obtained from 180mg of heroin street samples which contained 156.15mg of heroin·HCl component by preparative high performance liquid chromatography. This method is suitable for preparing heroin standards in forensic science area.

  18. Membrane biofouling characterization: effects of sample preparation procedures on biofilm structure and the microbial community

    KAUST Repository

    Xue, Zheng


    Ensuring the quality and reproducibility of results from biofilm structure and microbial community analysis is essential to membrane biofouling studies. This study evaluated the impacts of three sample preparation factors (ie number of buffer rinses, storage time at 4°C, and DNA extraction method) on the downstream analysis of nitrifying biofilms grown on ultrafiltration membranes. Both rinse and storage affected biofilm structure, as suggested by their strong correlation with total biovolume, biofilm thickness, roughness and the spatial distribution of EPS. Significant variations in DNA yields and microbial community diversity were also observed among samples treated by different rinses, storage and DNA extraction methods. For the tested biofilms, two rinses, no storage and DNA extraction with both mechanical and chemical cell lysis from attached biofilm were the optimal sample preparation procedures for obtaining accurate information about biofilm structure, EPS distribution and the microbial community. © 2014 © 2014 Taylor & Francis.

  19. Membrane biofouling characterization: effects of sample preparation procedures on biofilm structure and the microbial community. (United States)

    Xue, Zheng; Lu, Huijie; Liu, Wen-Tso


    Ensuring the quality and reproducibility of results from biofilm structure and microbial community analysis is essential to membrane biofouling studies. This study evaluated the impacts of three sample preparation factors (ie number of buffer rinses, storage time at 4°C, and DNA extraction method) on the downstream analysis of nitrifying biofilms grown on ultrafiltration membranes. Both rinse and storage affected biofilm structure, as suggested by their strong correlation with total biovolume, biofilm thickness, roughness and the spatial distribution of EPS. Significant variations in DNA yields and microbial community diversity were also observed among samples treated by different rinses, storage and DNA extraction methods. For the tested biofilms, two rinses, no storage and DNA extraction with both mechanical and chemical cell lysis from attached biofilm were the optimal sample preparation procedures for obtaining accurate information about biofilm structure, EPS distribution and the microbial community.

  20. An enzyme-based DNA preparation method for application to forensic biological samples and degraded stains. (United States)

    Lounsbury, Jenny A; Coult, Natalie; Miranian, Daniel C; Cronk, Stephen M; Haverstick, Doris M; Kinnon, Paul; Saul, David J; Landers, James P


    Extraction of DNA from forensic samples typically uses either an organic extraction protocol or solid phase extraction (SPE) and these methods generally involve numerous sample transfer, wash and centrifugation steps. Although SPE has been successfully adapted to the microdevice, it can be problematic because of lengthy load times and uneven packing of the solid phase. A closed-tube enzyme-based DNA preparation method has recently been developed which uses a neutral proteinase to lyse cells and degrade proteins and nucleases [14]. Following a 20 min incubation of the buccal or whole blood sample with this proteinase, DNA is polymerase chain reaction (PCR)-ready. This paper describes the optimization and quantitation of DNA yield using this method, and application to forensic biological samples, including UV- and heat-degraded whole blood samples on cotton or blue denim substrates. Results demonstrate that DNA yield can be increased from 1.42 (±0.21)ng/μL to 7.78 (±1.40)ng/μL by increasing the quantity of enzyme per reaction by 3-fold. Additionally, there is a linear relationship between the amount of starting cellular material added and the concentration of DNA in the solution, thereby allowing DNA yield estimations to be made. In addition, short tandem repeat (STR) profile results obtained using DNA prepared with the enzyme method were comparable to those obtained with a conventional SPE method, resulting in full STR profiles (16 of 16 loci) from liquid samples (buccal swab eluate and whole blood), dried buccal swabs and bloodstains and partial profiles from UV or heat-degraded bloodstains on cotton or blue denim substrates. Finally, the DNA preparation method is shown to be adaptable to glass or poly(methyl methacrylate) (PMMA) microdevices with little impact on STR peak height but providing a 20-fold reduction in incubation time (as little as 60 s), leading to a ≥1 h reduction in DNA preparation time.

  1. Plasma-enhanced preparation of graphene composites with polyaniline and polypyrrole (United States)

    Uygun Oksuz, Aysegul; Cogal, Sadik; Celik Cogal, Gamze; Uygun, Emre; Oksuz, Lutfi


    This study presents the preparation of graphene (GR) nanocomposites with polyaniline (PANI) and polypyrrole (PPy) through the fast, versatile and environmentally friendly process of radiofrequency (RF) -plasma polymerization. Morphological characterization of nanocomposites was performed using scanning electron microscopy (SEM) and showed that the PANI and PPy conducting polymers coated the GR surface. The surface properties of the GR nanocomposites were determined using Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) analysis. This work has been supported by Tubitak with 114M867 project number.

  2. Physical, mechanical, and tribological properties of quasicrystalline Al-Cu-Fe coatings prepared by plasma spraying (United States)

    Lepeshev, A. A.; Rozhkova, E. A.; Karpov, I. V.; Ushakov, A. V.; Fedorov, L. Yu.


    The physical, mechanical, and tribological properties of quasicrystalline coatings based on the Al65Cu23Fe12 alloy prepared by plasma spraying have been investigated. The specific features of the phase formation due to the competitive interactions of the icosahedral ψ and cubic β phases have been elucidated. A correlation between the microhardness and the content of the icosahedral phase in the coating has been determined. The decisive role of the quasicrystalline phase in the formation of high tribological characteristics of the coatings has been revealed and tested.

  3. MALDI MS sample preparation by using paraffin wax film: systematic study and application for peptide analysis. (United States)

    Wang, Junhua; Chen, Ruibing; Ma, Mingming; Li, Lingjun


    Recently developed sample preparation techniques employing hydrophobic sample support have improved the detection sensitivity and mass spectral quality of matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). These methods concentrate the samples on target by minimizing the sample area via the solvent repellent effect of the target surface. In the current study, we employed the use of paraffin wax film (Parafilm M) for improved MALDI MS analysis of low-abundance peptide mixtures, including neuronal tissue releasate and protein tryptic digests. This thin film was found to strongly repel polar solvents including water, methanol, and acetonitrile, which enabled the application of a wide range of sample preparation protocols that involved the use of various organic solvents. A "nanoliter-volume deposition" technique employing a capillary column has been used to produce tiny ( approximately 400 microm) matrix spots of 2,5-dihydroxybenzoic acid on the film. By systematically optimizing the sample volume, solvent composition, and film treatment, the Parafilm M substrate in combination with the nanoliter-volume matrix deposition method allowed dilute sample to be concentrated on the film for MALDI MS analysis. Peptide mixtures with nanomolar concentrations have been detected by MALDI time-of-flight and MALDI Fourier transform ion cyclotron resonance mass spectrometers. Overall, the use of Parafilm M enabled improved sensitivity and spectral quality for the analysis of complex peptide mixtures.

  4. Plasma preparation and low-temperature sintering of spherical TiC-Fe composite powder

    Institute of Scientific and Technical Information of China (English)

    Jian-jun Wang; Jun-jie Hao; Zhi-meng Guo; Song Wang


    A spherical Fe matrix composite powder containing a high volume fraction (82vol%) of fine TiC reinforcement was produced us-ing a novel process combining in situ synthesis and plasma techniques. The composite powder exhibited good sphericity and a dense struc-ture, and the fine sub-micron TiC particles were homogeneously distributed in theα-Fe matrix. A TiC–Fe cermet was prepared from the as-prepared spherical composite powder using powder metallurgy at a low sintering temperature;the product exhibited a hardness of HRA 88.5 and a flexural strength of 1360 MPa. The grain size of the fine-grained TiC and special surface structure of the spherical powder played the key roles in the fabrication process.

  5. Overestimation of canine albumin concentration with the bromcresol green method in heparinized plasma samples. (United States)

    Stokol, Tracy; Tarrant, Jacqueline M.; Scarlett, Janet M.


    Albumin concentrations are routinely measured in dogs with bromcresol green (BCG)-binding assays on automated chemistry analyzers. Several variables affect this assay, including the length of reaction time, sample type, and lack of specificity of BCG for albumin. We observed that albumin concentrations measured with BCG appeared higher in heparinized plasma samples in sick dogs. The objective of this study was to determine the effect of anticoagulant and assay procedure on BCG albumin concentrations in clinically ill dogs. We hypothesized that albumin concentrations would be overestimated in heparinized plasma compared with serum because of the combination of heparin and fibrinogen. Furthermore, we hypothesized that the overestimation would be influenced by assay parameters. Blood was collected from 32 clinically ill dogs into tubes containing heparin, citrate, or no anticoagulant. Citrate was chosen to assess the effect of fibrinogen in the absence of heparin. Albumin concentration was measured in all 3 sample types from each dog using 2 different BCG procedures on an automated chemistry analyzer. The BCG procedures (standard and modified) differed in the wavelengths used for absorbance readings (standard, 600/700; modified, 570/505) and the time point at which absorbance was measured (standard, 100 seconds; modified, 40 seconds). In addition, the modified method incorporated a sample blank. Globulin fractions, fibrinogen concentration, and indices of lipemia, hemolysis, and icterus were evaluated for their contribution to the overestimation of albumin concentration in heparinized plasma compared with serum samples. Albumin concentrations were significantly higher (P plasma (mean +/- SE, 3.8 +/- 0.1 g/dL) than in serum (3.6 +/- 0.2 g/dL) or citrated plasma (3.2 +/- 0.1 g/dL). Overestimation was evident only with the standard BCG procedure. Multiple linear regression analysis indicated that fibrinogen was largely responsible for the higher

  6. Determination of quinolones in plasma samples by capillary electrophoresis using solid-phase extraction. (United States)

    Hernández, M; Borrull, F; Calull, M


    The potential of capillary zone electrophoresis (CZE) and micellar electrokinetic capillary chromatography (MEKC) have been investigated for the separation and quantitative determination of 10 quinolone antibiotics. The influence of different conditions, such as the buffer and pH of the electrolyte, the surfactant and the ion-pairing agents added to the electrolyte and the organic modifier were studied. A buffer consisting of 40 mM sodium tetraborate at pH 8.1 containing 10% (v/v) methanol was found to be a highly efficient electrophoretic system for separating lomefloxacin, enoxacin, norfloxacin, pipemidic acid, ofloxacin, piromidic acid, flumequine, oxolinic acid, cinoxacin and nalidixic acid. A solid-phase extraction method to remove the sample matrix (pig plasma samples) was developed on a C(18) cartridge using a mixture of methanol-water (70:30, v/v). The method is specific and reproducible and mean recoveries were in the range 94.0+/-4.2% and 123.3+/-4.1% for pig plasma samples over the range used. A linear relationship between concentration and peak area for each compound in pig plasma samples was obtained in the concentration range 5-20 mg l(-1) and detection limits were between 1.1 and 2.4 mg l(-1).

  7. Development of a simple device for processing whole-blood samples into measured aliquots of plasma. (United States)

    Burtis, C A; Johnson, W F; Walker, W A


    A capillary processor and aliquoter has been designed and fabricated that is capable of accepting aliquots of whole blood and automatically processing them into discrete aliquots of plasma. The device consists of two disks, each of which contains 16 individual capillaries and a processing rotor. One disk accepts larger capillaries that hold approximately 100 microL of whole blood each. The second disk accepts 2.54-cm-long precision capillaries of various internal diameters, which provide exact sample volumes from 1 to 10 microL. The processing rotor contains 16 individual compartments and chambers to accept both disks. Applying centrifugal force transfers the aliquots of whole blood into their respective compartments, where they are separated into cellular and plasma fractions. As the rotor speed is slowly decreased, an aliquot of plasma is withdrawn by capillary action into each measuring capillary. The disk containing the 16 measured aliquots of plasma is then removed and placed into a modified rotor for conventional centrifugal analysis. This device can entrain and deliver microliter volumes of liquids with precision and accuracy (1-2%) near that of mechanical pipettes. Assays of the separated plasma aliquots also have acceptable precision (e.g., CVs approximately 3% for measurements of serum enzymes).

  8. Compact low temperature scanning tunneling microscope with in-situ sample preparation capability (United States)

    Kim, Jungdae; Nam, Hyoungdo; Qin, Shengyong; Kim, Sang-ui; Schroeder, Allan; Eom, Daejin; Shih, Chih-Kang


    We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

  9. Experimental improvements in sample preparation for the track registration technique from dry and solution media

    Energy Technology Data Exchange (ETDEWEB)

    Suarez-Navarro, M.J. [Universidad Politecnica de Madrid (UPM), E.T.S.I de Caminos, Canales y Puertos, Profesor Aranguren s/n, 28040 Madrid (Spain)]. E-mail:; Pujol, Ll. [Centro de Estudios y Experimentacion de Obras Publicas (CEDEX), Alfonso XII, 3, 28014 Madrid (Spain); Gonzalez-Gonzalez, J.A. [Universidad Politecnica de Madrid (UPM), E.T.S.I de Caminos, Canales y Puertos, Profesor Aranguren s/n, 28040 Madrid (Spain)


    This paper describes the sample preparation studies carried out to determine gross alpha activities in waste materials by means of alpha-particle track counting using CR-39 detector. Sample preparation for the track registration technique using evaporation or electroplating methods (also known as conventional 'dry methods') has a number of drawbacks. The distribution of tracks in different areas of the detector surface is non-uniform, so accurate quantitative determinations depend on tedious and time-consuming counting of tracks under an optical microscope. In this paper, we propose the use of tensioactives in sample preparation to achieve uniform track distribution over the entire detector surface, which enables track density to be evaluated by scanning a small representative area. Under our counting conditions, uniform distribution was achieved with 0.2 ml of Teg from a planchetted source. Furthermore, track registration techniques using solution media (also known as the 'wet methods') and conventional 'dry methods' were analysed and compared with the proposed method. The reproducibility of the procedure described in the study was tested by analysing gross alpha activity in two low-level nuclear waste samples at two different laboratories.

  10. Molecularly imprinted polymers for sample preparation and biosensing in food analysis: Progress and perspectives. (United States)

    Ashley, Jon; Shahbazi, Mohammad-Ali; Kant, Krishna; Chidambara, Vinayaka Aaydha; Wolff, Anders; Bang, Dang Duong; Sun, Yi


    Molecularly imprinted polymers (MIPs) are biomimetics which can selectively bind to analytes of interest. One of the most interesting areas where MIPs have shown the biggest potential is food analysis. MIPs have found use as sorbents in sample preparation attributed to the high selectivity and high loading capacity. MIPs have been intensively employed in classical solid-phase extraction and solid-phase microextraction. More recently, MIPs have been combined with magnetic bead extraction, which greatly simplifies sample handling procedures. Studies have consistently shown that MIPs can effectively minimize complex food matrix effects, and improve recoveries and detection limits. In addition to sample preparation, MIPs have also been viewed as promising alternatives to bio-receptors due to the inherent molecular recognition abilities and the high stability in harsh chemical and physical conditions. MIPs have been utilized as receptors in biosensing platforms such as electrochemical, optical and mass biosensors to detect various analytes in food. In this review, we will discuss the current state-of-the-art of MIP synthesis and applications in the context of food analysis. We will highlight the imprinting methods which are applicable for imprinting food templates, summarize the recent progress in using MIPs for preparing and analysing food samples, and discuss the current limitations in the commercialisation of MIPs technology. Finally, future perspectives will be given.

  11. Comparison of sample preparation methods for the recovery of foodborne pathogens from fresh produce. (United States)

    Kim, Se-Ri; Yoon, Yohan; Kim, Won-Il; Park, Kyeong-Hun; Yun, Hye-Jeong; Chung, Duck Hwa; Yun, Jong Chul; Ryu, Kyoung Yul


    Sample preparation methods (pummeling, pulsifying, sonication, and shaking by hand) were compared for achieving maximum recovery of foodborne pathogens from iceberg lettuce, perilla leaves, cucumber, green pepper, and cherry tomato. Antimicrobial and dehydration effects also were examined to investigate causes of poor recovery of pathogens. Each produce type was inoculated with Escherichia coli O157:H7, Salmonella Typhimurium, Listeria monocytogenes, Staphylococcus aureus, and Bacillus cereus at 6.0 log CFU/cm(2), and samples were prepared using the four methods. Bacterial populations recovered from the five types of produce were significantly different (P cucumber, and green pepper had no antimicrobial activity, the populations of E. coli O157:H7, Salmonella Typhimurium, B. cereus, and L. monocytogenes in cherry tomato extract were slightly reduced after these treatments (P 2 log CFU/cm(2) after exposure to 40% relative humidity for 1 h. No reduction was observed when the five pathogens were exposed to 90% relative humidity. These data suggest that pummeling and pulsifying are optimal sample preparation methods for detection of microorganisms. Acidic produce such as cherry tomato should be treated with a method that does not cause sample breakdown so that acid stress on the bacteria can be minimized. Dehydration stress also affects recovery of pathogens from produce.

  12. Should the mass of a nanoferrite sample prepared by autocombustion method be considered as a realistic preparation parameter? (United States)

    Wahba, Adel Maher; Mohamed, Mohamed Bakr


    Detectable variations in structural, elastic and magnetic properties have been reported depending on the mass of the cobalt nanoferrite sample prepared by citrate autocombustion method. Heat released during the autocombustion process and its duration are directly proportional to the mass to be prepared, and is thus expected to affect both the crystallite size and the cation distribution giving rise to the reported variations in microstrain, magnetization, and coercivity. Formation of a pure spinel phase has been validated using X-ray diffraction patterns (XRD) and Fourier-transform infrared (FTIR) spectra. Crystallite sizes obtained from Williamson-Hall (W-H) method range from 28-87 nm, being further supported by images of high-resolution transmission electron microscope (HRTEM). Saturation magnetization and coercivity deduced from M-H hysteresis loops show a clear correlation with the cation distribution, which was proposed on the basis of experimentally obtained data of XRD, VSM, and IR. Elastic parameters have been estimated using the cation distribution and FTIR data, with a resulting trend quite opposite to that of the lattice parameter.

  13. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Karina B. de [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Farmacia; Oliveira, Bras H. de, E-mail: [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Quimica


    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C{sub 18} column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min-1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 {+-} 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  14. Macro- and micro-element analysis in milk samples by inductively coupled plasma-optical emission spectrometry

    Directory of Open Access Journals (Sweden)

    Petrović Sanja M.


    Full Text Available The paper describes the determination of Ag, Al, B, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Na, Ni, Pb, Sr, Tl and Zn, as well as total fat content of milk samples, originated from different sources. The analyzed milk samples were: human milk, fresh cow milk, pasteurized cow milk from a local market, and reconstituted powder milk. The milk samples were obtained from Jablanica District (Serbia territory. Preparation of samples for macro- and micro-analyses was done by wet digestion. Concentrations of the elements after digestion were determined by inductively coupled plasma optical emission spectrometry (ICP-OES. Total fat content of milk samples was determinate by the Weibull and Stoldt method. The results showed that potassium and calcium concentrations were the highest in all samples: 1840.64 - 2993.26 mg/L and 456.05 - 1318.08 mg/L, respectively. Of all heavy metals from the examined milk samples (copper, zinc, manganese, nickel, cadmium, and lead, the most common were zinc and copper, with approximately similar content in the range of 5 - 12 mg/l, while cadmium nickel and manganese were not detected at all. Samples of fresh cow milk and human milk showed the highest fat content of 3.6 and 4.2 %, respectively. Results for total fat and macro- and micro-analyses showed that fresh cow milk has the highest contents of fat and calcium, making it the most nutritious. [Projekat Ministarstva nauke Republike Srbije, br. TR 34012

  15. Analysis of iodine in food samples by inductively coupled plasma-mass spectrometry. (United States)

    Todorov, Todor I; Gray, Patrick J


    This work shows a method for the determination of iodine in a variety of food samples and reference materials using inductively coupled plasma-mass spectrometry (ICP-MS) following alkaline extraction. Optimisation of the addition of organic carbon showed that a minimum of 3% 2-propanol was necessary for a constant ratio of iodine to internal standard. The limit of quantification (LOQ), calculated as 30σ for the method, was 36 ng g(-1) in solid food samples. For method validation, seven standard reference materials (SRM) and 21 fortified food samples were used. The precision (%RSD) of the measurements was in the 2-7% range. Accuracies for the SRMs were 85-105%, while the fortified food samples showed 81-119% recoveries, including a number of samples fortified at 50% of the LOQ.

  16. Long-term performance and stability of molecular shotgun lipidomic analysis of human plasma samples. (United States)

    Heiskanen, Laura A; Suoniemi, Matti; Ta, Hung Xuan; Tarasov, Kirill; Ekroos, Kim


    The stability of the lipid concentration levels in shotgun lipidomics analysis was tracked over a period of 3.5 years. Concentration levels in several lipid classes, such as phospholipids, were determined in human plasma lipid extracts. Impact of the following factors on the analysis was investigated: sample amount, internal standard amount, and sample dilution factor. Moreover, the reproducibility of lipid profiles obtained in both polarity modes was evaluated. Total number of samples analyzed was approximately 6800 and 7300 samples in negative and positive ion modes, respectively, out of which 610 and 639 instrument control samples were used in stability calculations. The assessed shotgun lipidomics approach showed to be remarkably robust and reproducible, requiring no batch corrections. Coefficients of variation (CVs) of lipid mean concentration measured with optimized analytical parameters were typically less than 15%. The high reproducibility indicated that no lipid degradation occurred during the monitored time period.

  17. Antibiotic plasma levels in dogs with otitis externa treated routinely with various topical preparations. (United States)

    Voget, Michael; Armbruster, Martin; Meyer, Michael


    We aimed to determine whether, and at what levels, topical antibiotics applied to treat Otitis externa in dogs are absorbed systemically, leading to an increased risk of antibiotic resistance. 75 dogs brought to a veterinarian for Otitis externa were recruited for a non-interventional study. Selection criteria included diagnosis of Otitis externa and owner consent.The animals were divided into five groups of 15 dogs each. Each group received one of five commonly prescribed topical medications for up to 14 days according to the labeled instructions. Development and validation of low residue detection methods (HPLC-MS/MS) for all active substances studied was performed. Plasma concentrations were evaluated for gentamicin (Otomax, Easotic), marbofloxacin (Aurizon), orbifloxacin (Posatex) and polymyxin B (Surolan). Low-level plasma concentrations of the topically applied antibiotics were detected after multiple administrations. In several samples, the concentrations detected were less than the limit of detection (LOD) of the corresponding analytical method. However, at the end of the treatment period, mean plasma concentrations were in the low pmol/ml range and exceeded the LOD for gentamicin, marbofloxacin and orbifloxacin. None of the plasma samples examined for polymyxin showed levels above the LOD. After routine topical antibiotic use in the treatment of Otitis externa in dogs, low systemic plasma concentrations are likely to develop.This low-level exposure may facilitate cellular changes that lead to an increased possibility for antibiotic resistance. These findings should provoke veterinary clinicians to optimise therapy for Otitis externa in light of minimising the development of antibiotic resistance.

  18. One-step preparation of hydrogenated ZrO2 microspheres by cathode plasma electrolysis (United States)

    Liu, Chenxu; Xiang, Qingyun; Yang, Mu; Wang, Shengdian; Wang, Linxiu; Zhang, Jin; He, Yedong


    Hydrogenated ZrO2 microspheres were directly prepared by cathode plasma electrolysis (CPE) in an aqueous solution of Zr(NO3)4•5H2O. Owing to the energy of plasma and the cathodic hydrogen evolution reactions, the CPE method combined the preparation of ZrO2 ceramic and the hydrogen treatment into only one step. The results showed regular microspheres consisting of tetragonal-ZrO2 and monoclinic-ZrO2 with 1-10 µm in diameter were formed at relatively high concentration of Zr(NO3)3•5H2O. These ZrO2 microspheres contained about 52.54 µg g-1 hydrogen which caused a narrow band gap (3.10 eV). Thus, the microspheres showed good photocatalytic activity under simulated sunlight, and the degradation of RhB dye reached nearly 58% for 3 h of irradiation, much better than the ZrO2 microspheres after dehydrogenation treatment.

  19. Indentations on Air Plasma Sprayed Thermal Barrier Coatings Prepared by Different Starting Granules

    Directory of Open Access Journals (Sweden)

    Yong Suk Heo


    Full Text Available The effect of starting granules on the indentation properties of air plasma sprayed thermal barrier coatings (TBCs is investigated in this paper. Various kinds of spray-dried granules are prepared from different processing conditions, especially varying solvent and dispersant, showing a deformed hollow-typed and a filled spherical-typed granule. The similar coating thicknesses are prepared by adjusting process parameters during air plasma spray. All XRD peaks in phase analysis are tetragonal and cubic phases without any monoclinic phase after the starting granules were heat-treated. A relatively porous microstructure of the coating layer could be obtained from the monodisperse granules, while a relatively dense microstructure resulted from the hollow-typed granules. The morphology and distribution of the granules crucially affect the microstructure of thermal barrier coatings and thus have influences on indentation properties such as indentation stress-strain curves, contact damage, and hardness. The implication concerning microstructure design of TBCs for gas turbine applications is considered.

  20. Bio-sample preparation and gas chromatographic determination of benzodiazepines--a review. (United States)

    Uddin, Mohammad Nasir; Samanidou, Victoria F; Papadoyannis, Ioannis N


    Benzodiazepines have become commonly prescribed medicines worldwide in the therapy of anxiety, sleep disorders and convulsive attacks because they are relatively safe, with mild side effects. The availability of rapid, sensitive and selective analytical methods is essential for the determination of these drugs in clinical and forensic cases. Benzodiazepines are usually present at trace levels (μg/mL or ng/mL) in a complex biological matrix, and the potentially interfering compounds need to be removed before analysis. Therefore, a sample preparation technique is often mandatory, both to extract the drugs of interest from the matrices and to increase their concentration. An extended and comprehensive review is presented herein, focusing on bio-sample preparation (pretreatment, extraction and derivatization) and gas chromatographic methods applied for the quantification of 1,4-benzodiazepines.

  1. DIII-D Upgrade to Prepare the Basis for Steady-State Burning Plasmas (United States)

    Buttery, R. J.; Guo, H. Y.; Taylor, T. S.; Wade, M. R.; Hill, D. N.


    Future steady-state burning plasma facilities will access new physics regimes and modes of plasma behavior. It is vital to prepare for this both experimentally using existing facilities, and theoretically in order to develop the tools to project to and optimize these devices. An upgrade to DIII-D is proposed to address the three critical aspects where research must go beyond what we can do now: (i) torque free electron heating to address the energy, particle and momentum transport mechanisms of burning plasmas using electron cyclotron (EC) heating and full power balanced neutral beams; (ii) off-axis heating and current drive to develop the path to true fusion steady state by reorienting neutral beams and deploying EC and helicon current drive; (iii) a new divertor with hot walls and reactor relevant materials to develop the basis for benign detached divertor operation compatible with wall materials and a high performance fusion core. These elements with modest incremental cost and enacted as a user facility for the whole US program will enable the US to lead on ITER and take a decision to proceed with a Fusion Nuclear Science Facility. Work supported by the US Department of Energy under DE-FC02-04ER54698 and DE-AC52-07NA27344.

  2. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR. (United States)

    Mandal, Abhishek; Boatz, Jennifer C; Wheeler, Travis B; van der Wel, Patrick C A


    A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

  3. Sample preparation for the analysis of flavors and off-flavors in foods. (United States)

    Wilkes, J G; Conte, E D; Kim, Y; Holcomb, M; Sutherland, J B; Miller, D W


    Off-flavors in foods may originate from environmental pollutants, the growth of microorganisms, oxidation of lipids, or endogenous enzymatic decomposition in the foods. The chromatographic analysis of flavors and off-flavors in foods usually requires that the samples first be processed to remove as many interfering compounds as possible. For analysis of foods by gas chromatography (GC), sample preparation may include mincing, homogenation, centrifugation, distillation, simple solvent extraction, supercritical fluid extraction, pressurized-fluid extraction, microwave-assisted extraction, Soxhlet extraction, or methylation. For high-performance liquid chromatography of amines in fish, cheese, sausage and olive oil or aldehydes in fruit juice, sample preparation may include solvent extraction and derivatization. Headspace GC analysis of orange juice, fish, dehydrated potatoes, and milk requires almost no sample preparation. Purge-and-trap GC analysis of dairy products, seafoods, and garlic may require heating, microwave-mediated distillation, purging the sample with inert gases and trapping the analytes with Tenax or C18, thermal desorption, cryofocusing, or elution with ethyl acetate. Solid-phase microextraction GC analysis of spices, milk and fish can involve microwave-mediated distillation, and usually requires adsorption on poly(dimethyl)siloxane or electrodeposition on fibers followed by thermal desorption. For short-path thermal desorption GC analysis of spices, herbs, coffee, peanuts, candy, mushrooms, beverages, olive oil, honey, and milk, samples are placed in a glass-lined stainless steel thermal desorption tube, which is purged with helium and then heated gradually to desorb the volatiles for analysis. Few of the methods that are available for analysis of food flavors and off-flavors can be described simultaneously as cheap, easy and good.

  4. Fast detection of Noroviruses using a real-time PCR assay and automated sample preparation

    Directory of Open Access Journals (Sweden)

    Schmid Michael


    Full Text Available Abstract Background Noroviruses (NoV have become one of the most commonly reported causative agents of large outbreaks of non-bacterial acute gastroenteritis worldwide as well as sporadic gastroenteritis in the community. Currently, reverse transcriptase polymerase chain reaction (RT-PCR assays have been implemented in NoV diagnosis, but improvements that simplify and standardize sample preparation, amplification, and detection will be further needed. The combination of automated sample preparation and real-time PCR offers such refinements. Methods We have designed a new real-time RT-PCR assay on the LightCycler (LC with SYBR Green detection and melting curve analysis (Tm to detect NoV RNA in patient stool samples. The performance of the real-time PCR assay was compared with that obtained in parallel with a commercially available enzyme immunoassay (ELISA for antigen detection by testing a panel of 52 stool samples. Additionally, in a collaborative study with the Baden-Wuerttemberg State Health office, Stuttgart (Germany the real-time PCR results were blindly assessed using a previously well-established nested PCR (nPCR as the reference method, since PCR-based techniques are now considered as the "gold standard" for NoV detection in stool specimens. Results Analysis of 52 clinical stool samples by real-time PCR yielded results that were consistent with reference nPCR results, while marked differences between the two PCR-based methods and antigen ELISA were observed. Our results indicate that PCR-based procedures are more sensitive and specific than antigen ELISA for detecting NoV in stool specimens. Conclusions The combination of automated sample preparation and real-time PCR provided reliable diagnostic results in less time than conventional RT-PCR assays. These benefits make it a valuable tool for routine laboratory practice especially in terms of rapid and appropriate outbreak-control measures in health-care facilities and other settings.

  5. Development of an automated sample preparation module for environmental monitoring of biowarfare agents. (United States)

    Hindson, Benjamin J; Brown, Steve B; Marshall, Graham D; McBride, Mary T; Makarewicz, Anthony J; Gutierrez, Dora M; Wolcott, Duane K; Metz, Thomas R; Madabhushi, Ramakrishna S; Dzenitis, John M; Colston, Billy W


    An automated sample preparation module, based upon sequential injection analysis (SIA), has been developed for use within an autonomous pathogen detection system. The SIA system interfaced aerosol sampling with multiplexed microsphere immunoassay-flow cytometric detection. Metering and sequestering of microspheres using SIA was found to be reproducible and reliable, over 24-h periods of autonomous operation. Four inbuilt immunoassay controls showed excellent immunoassay and system stability over five days of unattended continuous operation. Titration curves for two biological warfare agents, Bacillus anthracis and Yersinia pestis, obtained using the automated SIA procedure were shown to be similar to those generated using a manual microtiter plate procedure.

  6. Optimization of Proteomic Sample Preparation Procedures for Comprehensive Protein Characterization of Pathogenic Systems (United States)

    Mottaz-Brewer, Heather M.; Norbeck, Angela D.; Adkins, Joshua N.; Manes, Nathan P.; Ansong, Charles; Shi, Liang; Rikihisa, Yasuko; Kikuchi, Takane; Wong, Scott W.; Estep, Ryan D.; Heffron, Fred; Pasa-Tolic, Ljiljana; Smith, Richard D.


    Mass spectrometry-based proteomics is a powerful analytical tool for investigating pathogens and their interactions within a host. The sensitivity of such analyses provides broad proteome characterization, but the sample-handling procedures must first be optimized to ensure compatibility with the technique and to maximize the dynamic range of detection. The decision-making process for determining optimal growth conditions, preparation methods, sample analysis methods, and data analysis techniques in our laboratory is discussed herein with consideration of the balance in sensitivity, specificity, and biomass losses during analysis of host-pathogen systems. PMID:19183792

  7. Preparation of Plant 41Ca Tracer Samples for Accelerator Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    ZHAO Qing-zhang1;JANG Ping-ping3;LIN De-yu4;YANG Xian-lin1;DOU Liang1;PANG Yi-jun1;WANG Xiao-ming1;ZHANG Hui1,5;YANG Xu-ran1;WU Shao-yong1;GAO Dong-sheng2;LI Ling2;WANG Lei2;SUN Ke-peng2;ZHOU Jun2;DONG Ke-jun1;HE Ming1


    Full Text Available Calcium plays an important role in the metabolism of plants and animals. In this paper, the preparation method of plant 41Ca for accelerator mass spectrometry (AMS measurement was developed for the first time in China. AMS, with its advantages of high sensitivity, small dose of radioactivity, high accuracy, large measuring range, and long tracer cycle, can be used to measure cosmogenic nuclide 41Ca , which has long half-life. The intensity of the beam in ion source is an important parameter for the sensitivity of AMS measurement. The high beam current can improve the sensitivity of AMS. The preparation methods of plant samples of 41Ca tracer were systematically studied to obtain high beam current using wet, dry and a combining method with wet and dry re-fluoride. A reliable preparation procedure of plant samples for 41Ca tracer and its optimization parameters were determined by testing beam currents of various samples and lay a foundation for the 41Ca-AMS technology at plant tracer applications.

  8. Sample preparation: a critical step in the analysis of cholesterol oxidation products. (United States)

    Georgiou, Christiana A; Constantinou, Michalis S; Kapnissi-Christodoulou, Constantina P


    In recent years, cholesterol oxidation products (COPs) have drawn scientific interest, particularly due to their implications on human health. A big number of these compounds have been demonstrated to be cytotoxic, mutagenic, and carcinogenic. The main source of COPs is through diet, and particularly from the consumption of cholesterol-rich foods. This raises questions about the safety of consumers, and it suggests the necessity for the development of a sensitive and a reliable analytical method in order to identify and quantify these components in food samples. Sample preparation is a necessary step in the analysis of COPs in order to eliminate interferences and increase sensitivity. Numerous publications have, over the years, reported the use of different methods for the extraction and purification of COPs. However, no method has, so far, been established as a routine method for the analysis of COPs in foods. Therefore, it was considered important to overview different sample preparation procedures and evaluate the different preparative parameters, such as time of saponification, the type of organic solvents for fat extraction, the stationary phase in solid phase extraction, etc., according to recovery, precision and simplicity.

  9. Preparation and Properties of Ag-Containing Diamond-Like Carbon Films by Magnetron Plasma Source Ion Implantation

    Directory of Open Access Journals (Sweden)

    K. Baba


    Full Text Available The doping effect of silver on the structure and properties of diamond-like carbon (DLC films was investigated. The samples were prepared by a process combining acetylene plasma source ion implantation (high-voltage pulses of −10 kV with reactive magnetron sputtering of an Ag disc. A mixture of two gases, argon, and acetylene was introduced into the discharge chamber as working gas for plasma formation. A negative high-voltage pulse was applied to the substrate holder, thus, accelerating ions towards the substrate. The chemical composition of the deposited films was modified by the respective gas flows and determined using X-ray photoelectron spectroscopy and secondary ion mass spectrometry. The silver concentration within the DLC films influenced the structure and the tribological properties. The surface roughness, as observed by scanning electron microscopy, increased with silver concentration. The film structure was characterized by Raman spectroscopy and X-ray diffractometry (XRD. The DLC films were mainly amorphous, containing crystalline silver, with the amount of silver depending on the process conditions. The tribological properties of the films were improved by the silver doping. The lowest friction coefficient of around 0.06 was derived at a low silver content.

  10. Electric and mechanical performances of Bi0.5Sb1.5Te3 prepared by spark plasma sintering

    Institute of Scientific and Technical Information of China (English)

    XIAO Bo; CHEN Hui; WU Borong; ZHU Lei; LIU Mingyi; JIAN Xuyu; LI Lin


    Thermoelectric (TE) materials are a kind of functional materials which can be used to convert directly heat energy to electricity or reversely.The thermoelectric effects hold great potential for application in power generation and refrigeration.Bi2Te3 and its alloys are well known as best TE materials currently available near room temperature.This paper studies respectively the effects of spark plasma sintering (SPS) on electric performance of Bi0.5Sb1.5Te3 thermoelectric materials that are prepared through vacuum melting and ball milling.Through X-ray Diffraction and cold field emission scanning electric microscope s4800, the phase constituent and microstructure of the TE materials samples were analyzed.Electric conductivity and power factor can be improved with the rise of Spark Plasma Sintering temperature (from 300 to 500 ℃) and pressure(from 30 to 60 MPa), and the density and mechanical strength of Bi0.5Sb1.5Te3 thermoelectric material increase, too.

  11. DNA isolation and sample preparation for quantification of adduct levels by accelerator mass spectrometry. (United States)

    Dingley, Karen H; Ubick, Esther A; Vogel, John S; Ognibene, Ted J; Malfatti, Michael A; Kulp, Kristen; Haack, Kurt W


    Accelerator mass spectrometry (AMS) is a highly sensitive technique used for the quantification of adducts following exposure to carbon-14- or tritium-labeled chemicals, with detection limits in the range of one adduct per 10(11)-10(12) nucleotides. The protocol described in this chapter provides an optimal method for isolating and preparing DNA samples to measure isotope-labeled DNA adducts by AMS. When preparing samples, special precautions must be taken to avoid cross-contamination of isotope among samples and produce a sample that is compatible with AMS. The DNA isolation method described is based upon digestion of tissue with proteinase K, followed by extraction of DNA using Qiagen isolation columns. The extracted DNA is precipitated with isopropanol, washed repeatedly with 70 % ethanol to remove salt, and then dissolved in water. DNA samples are then converted to graphite or titanium hydride and the isotope content measured by AMS to quantify adduct levels. This method has been used to reliably generate good yields of uncontaminated, pure DNA from animal and human tissues for analysis of adduct levels.

  12. On-chip sample preparation for complete blood count from raw blood. (United States)

    Nguyen, John; Wei, Yuan; Zheng, Yi; Wang, Chen; Sun, Yu


    This paper describes a monolithic microfluidic device capable of on-chip sample preparation for both RBC and WBC measurements from whole blood. For the first time, on-chip sample processing (e.g. dilution, lysis, and filtration) and downstream single cell measurement were fully integrated to enable sample preparation and single cell analysis from whole blood on a single device. The device consists of two parallel sub-systems that perform sample processing and electrical measurements for measuring RBC and WBC parameters. The system provides a modular environment capable of handling solutions of various viscosities by adjusting the length of channels and precisely controlling mixing ratios, and features a new 'offset' filter configuration for increased duration of device operation. RBC concentration, mean corpuscular volume (MCV), cell distribution width, WBC concentration and differential are determined by electrical impedance measurement. Experimental characterization of over 100,000 cells from 10 patient blood samples validated the system's capability for performing on-chip raw blood processing and measurement.

  13. Improved sample preparation and counting techniques for enhanced tritium measurement sensitivity (United States)

    Moran, J.; Aalseth, C.; Bailey, V. L.; Mace, E. K.; Overman, C.; Seifert, A.; Wilcox Freeburg, E. D.


    Tritium (T) measurements offer insight to a wealth of environmental applications including hydrologic tracking, discerning ocean circulation patterns, and aging ice formations. However, the relatively short half-life of T (12.3 years) limits its effective age dating range. Compounding this limitation is the decrease in atmospheric T content by over two orders of magnitude (from 1000-2000 TU in 1962 to low background proportional counters which, when combined, offer improved T measurement sensitivity (~4.5 mmoles of H2 equivalent) and will help expand the application of T age dating to smaller sample sizes linked to persistent environmental questions despite the limitations above. For instance, this approach can be used to T date ~ 2.2 mmoles of CH4 collected from sample-limited systems including microbial communities, soils, or subsurface aquifers and can be combined with radiocarbon dating to distinguish the methane's formation age from C age in a system. This approach can also expand investigations into soil organic C where the improved sensitivity will permit resolution of soil C into more descriptive fractions and provide direct assessments of the stability of specific classes of organic matter in soils environments. We are employing a multiple step sample preparation system whereby organic samples are first combusted with resulting CO2 and H2O being used as a feedstock to synthesize CH4. This CH4 is mixed with Ar and loaded directly into an ultra-low background proportional counter for measurement of T β decay in a shallow underground laboratory. Analysis of water samples requires only the addition of geologic CO2 feedstock with the sample for methane synthesis. The chemical nature of the preparation techniques enable high sample throughput with only the final measurement requiring T decay with total sample analysis time ranging from 2 -5 weeks depending on T content.

  14. Processing, Mechanical and Optical Properties of Additive-Free ZrC Ceramics Prepared by Spark Plasma Sintering

    Directory of Open Access Journals (Sweden)

    Clara Musa


    Full Text Available In the present study, nearly fully dense monolithic ZrC samples are produced and broadly characterized from microstructural, mechanical and optical points of view. Specifically, 98% dense products are obtained by Spark Plasma Sintering (SPS after 20 min dwell time at 1850 °C starting from powders preliminarily prepared by Self-propagating High-temperature Synthesis (SHS followed by 20 min ball milling. A prolonged mechanical treatment up to 2 h of SHS powders does not lead to appreciable benefits. Vickers hardness of the resulting samples (17.5 ± 0.4 GPa is reasonably good for monolithic ceramics, but the mechanical strength (about 250 MPa up to 1000 °C could be further improved by suitable optimization of the starting powder characteristics. The very smoothly polished ZrC specimen subjected to optical measurements displays high absorption in the visible-near infrared region and low thermal emittance at longer wavelengths. Moreover, the sample exhibits goodspectral selectivity (2.1–2.4 in the 1000–1400 K temperature range. These preliminary results suggest that ZrC ceramics produced through the two-step SHS/SPS processing route can be considered as attractive reference materials for the development of innovative solar energy absorbers.

  15. Reducing time and increasing sensitivity in sample preparation for adherent mammalian cell metabolomics. (United States)

    Lorenz, Matthew A; Burant, Charles F; Kennedy, Robert T


    A simple, fast, and reproducible sample preparation procedure was developed for relative quantification of metabolites in adherent mammalian cells using the clonal β-cell line INS-1 as a model sample. The method was developed by evaluating the effect of different sample preparation procedures on high performance liquid chromatography- mass spectrometry quantification of 27 metabolites involved in glycolysis and the tricarboxylic acid cycle on a directed basis as well as for all detectable chromatographic features on an undirected basis. We demonstrate that a rapid water rinse step prior to quenching of metabolism reduces components that suppress electrospray ionization thereby increasing signal for 26 of 27 targeted metabolites and increasing total number of detected features from 237 to 452 with no detectable change of metabolite content. A novel quenching technique is employed which involves addition of liquid nitrogen directly to the culture dish and allows for samples to be stored at -80 °C for at least 7 d before extraction. Separation of quenching and extraction steps provides the benefit of increased experimental convenience and sample stability while maintaining metabolite content similar to techniques that employ simultaneous quenching and extraction with cold organic solvent. The extraction solvent 9:1 methanol: chloroform was found to provide superior performance over acetonitrile, ethanol, and methanol with respect to metabolite recovery and extract stability. Maximal recovery was achieved using a single rapid (∼1 min) extraction step. The utility of this rapid preparation method (∼5 min) was demonstrated through precise metabolite measurements (11% average relative standard deviation without internal standards) associated with step changes in glucose concentration that evoke insulin secretion in the clonal β-cell line INS-1.

  16. Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry (United States)

    Todorov, Todor I.; Wolf, Ruth E.; Adams, Monique


    Typically, 27 major, minor, and trace elements are determined in natural waters, acid mine drainage, extraction fluids, and leachates of geological and environmental samples by inductively coupled plasma-optical emission spectrometry (ICP-OES). At the discretion of the analyst, additional elements may be determined after suitable method modifications and performance data are established. Samples are preserved in 1–2 percent nitric acid (HNO3) at sample collection or as soon as possible after collection. The aqueous samples are aspirated into the ICP-OES discharge, where the elemental emission signals are measured simultaneously for 27 elements. Calibration is performed with a series of matrix-matched, multi-element solution standards.

  17. Preparation and Microstructure of Porous ZrB2 Ceramics Using Reactive Spark Plasma Sintering Method

    Institute of Scientific and Technical Information of China (English)

    YUAN Huiping; LI Junguo; SHEN Qiang; ZHANG Lianmeng


    Zirconium oxide (ZrO2) and boron carbide (B4C) were added to ZrB2 raw powders to prepare ZrB2 porous ceramics by reactive spark plasma sintering (RSPS). The reactions between ZrO2 and B4C which produce ZrB2 and gas (such as CO and B2O3) result in pore formation. X-Ray Diffraction results indicated that the products phase was ZrB2 and the reaction was completed after the RSPS process. The porosity could be controlled by changing the ratio of synthesized ZrB2 to raw ZrB2 powders. The porosity of porous ceramics with 20 wt% and 40 wt% synthsized ZrB2 are 0.185 and 0.222, respectivly. And dense ZrB2-SiC ceramic with a porosity of 0.057 was prepared under the same conditions for comparison. The pores were homogeneously distributed within the microstructure of the porous ceramics. The results indicate a promising method for preparing porous ZrB2-based ceramics.

  18. Soybean and lactose in meat products and preparations sampled at retail

    Directory of Open Access Journals (Sweden)

    Filomena Piccolo


    Full Text Available Food allergies and intolerances have increased during the last decades and regulatory authorities have taken different measures to prevent and manage consumers’ adverse reactions, including correct labelling of foods. Aim of this work was to search for soybean and lactose in meat products and meat preparations taken from retail in some provinces of Campania Region (Southern Italy and to evaluate the food labels compliance with Regulation (EU n.1169/2011. Soybean and lactose were searched using commercial kits in n. 58 samples of meat products produced in or distributed by 19 establishments, and in n. 55 samples of meat products and n. 8 of meat preparations produced in 21 plants. All samples were selected on the basis of the absence of any information on the labels about the presence of the two searched allergens, with the exception of n. 5 samples tested for lactose. Traces of soybean were detected in 50 out of the 58 examined samples, at concentrations up to 0.93 mg kg–1. Only two samples contained levels above the detection limit of 0.31 mg kg–1. Lactose levels ranging from 0.11 to 2.95 g/100 g, i.e. above the detection limit, were found in all the tested samples (n. 63. The results of the present research underline the need for careful controls and planning by operators as part of the self-control plans, and deserve attention from the competent authorities considering not only the consumers’ health but also the great attention media pay to regulations providing consumers with information on food.

  19. Effect of particle size on the polycrystalline CeB6 cathode prepared by spark plasma sintering

    Institute of Scientific and Technical Information of China (English)

    BAO Lihong; ZHANG Jiuxing; ZHOU Shenlin


    The full densification polycrystalline cerium hexaboride (CeB6) cathode material was prepared by using the spark plasma sintering (SPS) method in an oxygen free system. The starting precursor nanopowders with an average grain size of 50 nm were prepared by high-energy ball milling. The ball-milled nanopowder was fully densified at 1550 ℃ under 50 MPa, which was about 350 ℃ lower than the conventional hot-pressing method and it was also lower than that of coarse powder under the same sintering condition. The mechanical properties of nanopowder sintered samples were significantly better than that of coarse powder, e.g., the flexural strength and Vickers hardness were 211% and 51% higher than that of coarse powder, respectively. The electron backscattered diffraction (EBSD) result showed that the (100) fiber texture could be fabricated by the ball-milled nanopowder sintered at 1550 ℃ and the thermionic emission current density was measured to be 16.04 A/cm2 at a cathode temperature of 1873 K.

  20. Optically- and thermally-stimulated luminescences of Ce-doped SiO2 glasses prepared by spark plasma sintering (United States)

    Okada, Go; Kasap, Safa; Yanagida, Takayuki


    Rare-earth doped phosphors have been used in many applications including radiation measurements. In the latter applications, the radiation photons are converted to light so that we can indirectly detect the radiation using a conventional photodetector. In this work, we have prepared and characterized a Ce-doped SiO2 glass for dosimeter applications. Unlike conventional techniques such as sol-gel synthesis, the sample was prepared by spark plasma sintering. Although the PL emission seems to be only from the Ce3+ ions in the structure, due to the X-ray induced luminescence, we have also observed optically-stimulated luminescence (OSL), and thermally-stimulated luminescence (TSL), owing to a pair of silylenes and a set of dioxasilirane and silylene in addition to Ce3+. We have measured the detector response vs irradiation dose for both the OSL and TSL. The detector response in both cases is linear over the dose range from at least 1 mGy to 2 Gy. Particularly, the sensitivity of TSL is so high that it should be considered to be a good candidate for practical applications.

  1. Rapid Measurement of Food Adulteration with Minimal Sample Preparation and No Chromatography Using Ambient Ionization Mass Spectrometry. (United States)

    Dalmia, Avinash


    A rapid method, with minimal sample preparation and no chromatography, was developed for analyzing food samples such as olive oil and pomegranate juice to measure adulteration with cheaper ingredients using the novel Direct Sample Analysis™ (DSA) ion source in conjunction with a time-of-flight (TOF)-MS. In less than 30 s, with minimal sample preparation and method development, adulteration of olive oil and pomegranate juice with cheaper seed oils and fruit juices, respectively, was measured with DSA/TOF-MS.

  2. Membrane-based sample preparation for ion chromatography-Techniques, instrumental configurations and applications. (United States)

    Frenzel, Wolfgang; Markeviciute, Inga


    Sample preparation is the bottleneck of many analytical methods, including ion chromatography (IC). Procedures based on the application of membranes are important, yet not well appreciated means for clean-up and analyte preconcentration of liquid samples. Filtration, ultrafiltration, the variety of dialysis techniques, i.e. passive dialysis, Donnan dialysis and electrodialysis, as well as gas-diffusion are being reviewed here with respect to their application in combination with IC. Instrumental aspects including hardware requirements, configuration of membrane separation units and membrane characteristics are presented. Operation in batch and flow-through mode is described with emphasis on the latter to in-line coupling with IC, permitting fully automated operation. Attention is also drawn to dialysis probes and microdialysis both providing options for in-situ measurements with inherent selective sampling of analytes and sample preparation. The respective features of the various techniques are outlined with respect to the possibilities of matrix removal and selectivity enhancement. In this article, we provide examples of application of the diverse membrane separation techniques and discuss the benefits and limitations thereof.

  3. Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

    Directory of Open Access Journals (Sweden)

    Vuković Gorica L.


    Full Text Available In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns. The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec­ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf­finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2 for the first method of sample preparation and 101% (%RSD = 2.2 for the second method. Values of LOQ for OTA were 0.25 and 1.00 μg/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

  4. Removal of interfering substances in samples prepared for two-dimensional (2-D) electrophoresis. (United States)

    Berkelman, Tom


    Biological samples may contain contaminants that interfere with analysis by two-dimensional (2-D) electrophoresis. Lysates or biological fluids are complex mixtures that contain a wide variety of nonprotein substances in addition to the proteins to be analyzed. These substances often interfere with the resolution of the electrophoretic separation or the visualization of the result. Macromolecules (e.g., polysaccharides and DNA) can interfere with electrophoretic separation by clogging gel pores. Small ionic molecules can impair isoelectric focusing (IEF) separation by rendering the sample too conductive. Other substances (e.g., phenolics and lipids) can bind to proteins, influencing their electrophoretic properties or solubility. In many cases, measures to remove interfering substances can result in significantly clearer 2-D patterns with more visible spots and better resolution. It should be borne in mind, however, that analysis of samples by 2-D electrophoresis is usually most successful and informative when performed with minimally processed samples, so it is important that any steps taken to remove interfering substance be appropriate to the sample and only performed when necessary. Procedures for the removal of interfering substances therefore represent a compromise between removing nonprotein contaminants, and minimizing interference with the integrity and relative abundances of the sample proteins. This chapter presents a number of illustrative examples of optimized sample preparation methods in which specific interfering substances are removed by a variety of different strategies.

  5. Elevated phospholipase A2 activities in plasma samples from multiple cancers.

    Directory of Open Access Journals (Sweden)

    Hui Cai

    Full Text Available Only in recent years have phospholipase A2 enzymes (PLA2s emerged as cancer targets. In this work, we report the first detection of elevated PLA2 activities in plasma from patients with colorectal, lung, pancreatic, and bladder cancers as compared to healthy controls. Independent sets of clinical plasma samples were obtained from two different sites. The first set was from patients with colorectal cancer (CRC; n = 38 and healthy controls (n = 77. The second set was from patients with lung (n = 95, bladder (n = 31, or pancreatic cancers (n = 38, and healthy controls (n = 79. PLA2 activities were analyzed by a validated quantitative fluorescent assay method and subtype PLA2 activities were defined in the presence of selective inhibitors. The natural PLA2 activity, as well as each subtype of PLA2 activity was elevated in each cancer group as compared to healthy controls. PLA2 activities were increased in late stage vs. early stage cases in CRC. PLA2 activities were not influenced by sex, smoking, alcohol consumption, or body-mass index (BMI. Samples from the two independent sites confirmed the results. Plasma PLA2 activities had approximately 70% specificity and sensitivity to detect cancer. The marker and targeting values of PLA2 activity have been suggested.

  6. Determination of trovafloxacin and marbofloxacin in sheep plasma samples by HPLC using UV detection. (United States)

    Mahmood, Adnan H; Medley, Gregory A; Grice, Jeffrey E; Liu, Xin; Roberts, Michael S


    A simple and rapid high performance liquid chromatographic method was developed, validated and applied for the simultaneous determination of marbofloxacin (MBX) and trovafloxacin (TVX) in sheep plasma. Samples were extracted with 20% perchloric acid and MBX and TVX were separated on a C(18) column using a gradient mobile phase system consisting of 17.5mM of NaH(2)PO(4) and 1.5mM of tetrabutylammonium hydroxide aqueous solution, pH 3 (A) and 50% acetonitrile and 50% methanol (B), with UV detection at 293 and 270 nm. The retention times of MBX and TVX were 4.9 and 6.6 min respectively. The detection and quantification limits for MBX and TVX were 2 ng/mL and 10 ng/mL respectively for both compounds. The calibration curves were linear over a concentration range of 10-50,000 ng/mL for both antibiotics. The linearity, precision, accuracy, recovery and stability of the assay were evaluated from spiked sheep plasma. The method was successfully applied to sheep plasma samples obtained from MBX and TVX pharmacokinetic studies.

  7. A developed wedge fixtures assisted high precision TEM samples pre-thinning method: Towards the batch lamella preparation

    Directory of Open Access Journals (Sweden)

    Dandan Wang


    Full Text Available Ion milling, wedge cutting or polishing, and focused ion beam (FIB milling are widely-used techniques for the transmission electron microscope (TEM sample preparation. Especially, the FIB milling provides a site-specific analysis, deposition, and ablation of materials in the micrometer and nanometer scale. However, the cost of FIB tools has been always a significant concern. Since it is inevitable to use the FIB technique, the improvement of efficiency is a key point. Traditional TEM sample preparation with FIB was routinely implemented on a single sample each time. Aiming at cost efficiency, a new pre-thinning technique for batch sample preparation was developed in this paper. The present proposal combines the sample preparation techniques with multi-samples thinning, cross-section scanning electron microscopy (SEM, wedge cutting, FIB and other sample pre-thinning techniques. The new pre-thinning technique is to prepare an edge TEM sample on a grinding and polishing fixture with a slant surface. The thickness of the wedges sample can be measured to 1∼2 μm under optical microscope. Therefore, this fixture is superior to the traditional optical method of estimating the membrane thickness. Moreover, by utilizing a multi-sample holding fixture, more samples can be pre-thinned simultaneously, which significantly improved the productivity of TEM sample preparation.

  8. Evaluation of neon focused ion beam milling for TEM sample preparation. (United States)

    Pekin, T C; Allen, F I; Minor, A M


    Gallium-based focused ion beams generated from liquid-metal sources are widely used in micromachining and sample preparation for transmission electron microscopy, with well-known drawbacks such as sample damage and contamination. In this work, an alternative (neon) focused ion beam generated by a gas field-ionization source is evaluated for the preparation of electron-transparent specimens. To do so, electron-transparent sections of Si and an Al alloy are prepared with both Ga and Ne ion beams for direct comparison. Diffraction-contrast imaging and energy dispersive x-ray spectroscopy are used to evaluate the relative damage induced by the two beams, and cross-sections of milled trenches are examined to compare the implantation depth with theoretical predictions from Monte Carlo simulations. Our results show that for the beam voltages and materials systems investigated, Ne ion beam milling does not significantly reduce the focused ion beam induced artefacts. However, the Ne ion beam does enable more precise milling and may be of interest in cases where Ga contamination cannot be tolerated.

  9. A Novel Sample Preparation for Shotgun Proteomics Characterization of HCPs in Antibodies. (United States)

    Huang, Lihua; Wang, Ning; Mitchell, Charles E; Brownlee, Tammy; Maple, Steven R; De Felippis, Michael R


    Residual host cell proteins (HCPs) in biopharmaceuticals derived from recombinant DNA technology can present potential safety risks to patients or compromise product stability. Thus, the downstream purification process is designed to demonstrate robust removal of these impurities. ELISA using polyclonal anti-HCP antibodies as reagents for capture, detection, and quantitation purposes is most commonly used to monitor HCP removal during process development, but this technique has limitations. More recently, LC-MS for residual HCP characterization has emerged as a powerful tool to support purification process development. However, mass spectrometry needs to overcome the enormous dynamic range to detect low ppm levels of residual HCPs in biopharmaceutical samples. We describe a simple and powerful methodology to characterize residual HCPs in (monoclonal) antibodies by combining a novel sample preparation procedure using trypsin digestion and a shotgun proteomics approach. Differing from the traditional methodology, the sample preparation approach maintains nearly intact antibody while HCPs are digested. Thus, the dynamic range for HCP detection by MS is 1 to 2 orders of magnitude less than the traditional trypsin digestion sample preparation procedure. HCP spiking experiments demonstrated that our method could detect 0.5 ppm of HCP with molecular weight >60 kDa, such as rPLBL2. Application of our method to analyze a high-purity NIST monoclonal antibody standard RM 8670 derived from a murine cell line expression system resulted in detection of 60 mouse HCPs; twice as many as previously reported with 2D-UPLC/IM/MS(E) method. A control monoclonal antibody used for 70 analyses over 450 days demonstrated that our method is robust.

  10. Novel sample preparation method for surfactant containing suppositories: effect of micelle formation on drug recovery. (United States)

    Kalmár, Éva; Ueno, Konomi; Forgó, Péter; Szakonyi, Gerda; Dombi, György


    Rectal drug delivery is currently at the focus of attention. Surfactants promote drug release from the suppository bases and enhance the formulation properties. The aim of our work was to develop a sample preparation method for HPLC analysis for a suppository base containing 95% hard fat, 2.5% Tween 20 and 2.5% Tween 60. A conventional sample preparation method did not provide successful results as the recovery of the drug failed to fulfil the validation criterion 95-105%. This was caused by the non-ionic surfactants in the suppository base incorporating some of the drug, preventing its release. As guidance for the formulation from an analytical aspect, we suggest a well defined surfactant content based on the turbidimetric determination of the CMC (critical micelle formation concentration) in the applied methanol-water solvent. Our CMC data correlate well with the results of previous studies. As regards the sample preparation procedure, a study was performed of the effects of ionic strength and pH on the drug recovery with the avoidance of degradation of the drug during the procedure. Aminophenazone and paracetamol were used as model drugs. The optimum conditions for drug release from the molten suppository base were found to be 100 mM NaCl, 20-40 mM NaOH and a 30 min ultrasonic treatment of the final sample solution. As these conditions could cause the degradation of the drugs in the solution, this was followed by NMR spectroscopy, and the results indicated that degradation did not take place. The determined CMCs were 0.08 mM for Tween 20, 0.06 mM for Tween 60 and 0.04 mM for a combined Tween 20, Tween 60 system. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Sample preparation methods for beeswax characterization by gas chromatography with flame ionization detection. (United States)

    Jiménez, J J; Bernal, J L; del Nozal, M A J; Martín, M A T; Bernal, J


    New and simpler methods of sample preparation to determine several families of compounds in beeswax by conventional and high temperature gas chromatography are proposed. To analyze hydrocarbons and palmitates, a dilution of sample is enough whereas for the total acid content, a hydrolysis and simultaneous methylation with BF3-methanol results more effective than the usual methods; for the total content of alcohols, a further acetylation with acetic anhydride is necessary. Free alcohols are directly acetylated in a sample dissolution but for free acids and monoesterified 1,2,3-propanetriols analysis, a previous extraction with acetonitrile is required. The concentrations of all the compounds studied are expressed in weight percentage referred only to one standard: octadecyl octadecanoate. The precision of the analytical methods has been evaluated showing its importance in the analysis of beeswaxes used in apiculture.

  12. Development of a chromatographic method for the determination of saquinavir in plasma samples of HIV patients. (United States)

    Campanero, M A; Escolar, M; Arangoa, M A; Sádaba, B; Azanza, J R


    A simple, sensitive and reproducible high-performance liquid chromatographic method for detecting and quantifying saquinavir in human plasma is described. Verapamil was used as internal standard. The method employes a single liquid-liquid extraction step with tert-butil methyl ether followed by chromatography on a Lichrospher 60 Select B C8 reversed-phase column. Ultraviolet detection was used to identify the compounds of interest. The quantitation limit of saquinavir was 1 ng/mL and only 0.5 mL of plasma sample was required for the determination. The average saquinavir recoveries over a concentration range of 2.5-500 ng/mL ranged from 86 to 95%. Precision and accuracy did not exceed 5%.

  13. Analysis of surface chemistry of boronized TZM samples in NSTX-U between plasma exposures (United States)

    Schamis, Hanna; Bedoya, Felipe; Allain, Jean Paul; Kaita, Robert; Koel, Bruce


    In the National Spherical Torus Experiment Upgrade (NSTX-U) a new plasma facing component diagnostic, the Material Analysis and Particle Probe (MAPP), was installed. MAPP has the capability of conducting XPS studies on materials without exposing them to atmospheric conditions. MAPP was used to conduct XPS studies of TZM (99% Mo, 0.5% Ti, 0.08% Zr) samples. XPS gives information about the chemical composition of up to about 5 nm of the surface, and can be conducted on a day-to-day basis or at higher temporal resolutions e.g. close to in-between plasma shots. MAPP characterization gives insight on boron deposition and fuel retention by following the evolution of atomic concentrations and oxidation states. The data shows that the boron deposited layer was thicker than 5 nm. Additionally, the data shows evidence of sputtering of the boron layers following tens of plasma shots. The data also shows an increase in the oxygen concentration with plasma exposure. The next NSTX-U experimental campaign will feature TZM tiles in the lower divertor region, while the rest of the first wall will continue to be ATJ graphite. Our data provides the basis to analyze how the surface chemistry of the new set of tiles will be influenced by plasma operations, boron conditioning and carbon migration. Work supported by US DOE Contract No. DE-AC02-09CH11466, US DOE Contract No. DE-SC0010717, Award No. DE-SC0012890, and the DOE Science Undergraduate Laboratory Internship (SULI) Program.

  14. Practical Guide to Using Cryoprotectants in Biological Sample Preparation at Cryogenic temperature for Electron Microscopic Studies

    Directory of Open Access Journals (Sweden)

    A-Reum Je


    Full Text Available Cryo-fixation enables the preservation of the fine structures of intracellular organelles in a condition that is as close to their native state as possible compared with chemical fixation and room temperature processing. Fixation is the initial step for biological sample preparation in electron microscopy. This step is critically important because the goals of electron microscopic observation are fundamentally dependent on well-preserved specimens resulting from this fixation. In the present work, key components of cryo-fixation, cryoprotectants, are tested with various cell types of interest. The results show that dextran can be easily adapted for use with animal cells and cyanobacteria, whereas 1-hexadecene is applicable to plant and yeast cells. The current report provides useful information on the preparation of cryo-fixed biological specimens using high pressure freezing and freeze-substitution aimed at electron microscopic observation.

  15. Laboratory Investigation of Rivers State Clay Samples for Drilling Mud Preparation

    Directory of Open Access Journals (Sweden)

    Nmegbu, Chukwuma Godwin Jacob


    Full Text Available Drilling fluids are an integral part of any oil and gas industry, providing the ease to which wells are drilled to access subsurface reservoir fluids. Certain rheology and mineralogical properties of the clay material used for drilling mud preparation must be critically investigated since clay deposits in different location exhibits different characteristics. Clay samples were collected from three different geographical locations namely; Egbamini (Emolga, Afam Street (Port Harcourt and Oboboru (onelga local government areas in Rivers state. Their rheological and wall building properties were measured in the laboratory to determine their suitability for drilling mud formulation. Results showed that in their respective native states, they proved unsuitable for drilling mud preparation when compared to standard Bentonite because they were observed to show responses far below the required API standards for mud formulation.

  16. Improved sample preparation for CE-LIF analysis of plant N-glycans. (United States)

    Nagels, Bieke; Santens, Francis; Weterings, Koen; Van Damme, Els J M; Callewaert, Nico


    In view of glycomics studies in plants, it is important to have sensitive tools that allow one to analyze and characterize the N-glycans present on plant proteins in different species. Earlier methods combined plant-based sample preparations with CE-LIF N-glycan analysis but suffered from background contaminations, often resulting in non-reproducible results. This publication describes a reproducible and sensitive protocol for the preparation and analysis of plant N-glycans, based on a combination of the 'in-gel release method' and N-glycan analysis on a multicapillary DNA sequencer. Our protocol makes it possible to analyze plant N-glycans starting from low amounts of plant material with highly reproducible results. The developed protocol was validated for different plant species and plant cells.

  17. An attempt to validate serum and plasma as sample matrices for analyses of polychlorobiphenylols

    Energy Technology Data Exchange (ETDEWEB)

    Weiss, J.; Bergman, Aa. [Stockholm Univ. (Sweden). Dept. of Environmental Chemistry; Bignert, A. [Museum of Natural History (Sweden)


    Polychlorinated biphenyls (PCBs) form hydroxylated metabolites (OH-PCBs), as reported both from wildlife and from experimental animal studies already in the early 1970s'. However, the interest increased in OH-PCBs from the mid 1990s' depending on the discovery that some OHPCB congeners are strongly retained in the blood of birds, fish and mammals, including humans. The interest is linked to the fact that OH-PCBs is strongly, but reversibly, bound to the blood protein transthyretin (TTR). It is reasonable to believe that the strong TTR binding may have toxicological impact, probably related to endocrine type effects. Importantly, OH-PCBs are present in blood at far higher concentrations than in any other compartment in the body, which is dependent on the physico-chemical characteristics of the phenols. Analyses of OH-PCBs have thus been concentrated to whole blood, plasma or serum. Still there is no comparison between the three sample types even though it is clear that whole blood is not optimal due to the large proportion of haemoglobin in the sample that make the clean up more difficult than if plasma or serum is selected for analysis. In the present study we have addressed two questions: First we have looked at any potential differences in the analytical results of OH-PCBs when using serum and plasma for extraction and clean up; Second, the serum and plasma applied in the validation has been unfrozen, frozen (at -20 C) for two months and frozen for twenty months, respectively.

  18. Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection. (United States)

    Huber, Charles S; Vale, Maria Goreti R; Dessuy, Morgana B; Svoboda, Milan; Musil, Stanislav; Dědina, Jiři


    A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO3, HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL(-1) HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg(-1) for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg(-1) which were below the limits of 300, 200 and 100µgkg(-1) set by the Brazilian, Chinese and European legislation, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Atmospheric-Pressure DBD Cold Plasma for Preparation of High Active Au/P25 Catalysts for Low-Temperature CO Oxidation

    Institute of Scientific and Technical Information of China (English)

    DI Lanbo; ZHAN Zhibin; ZHANG Xiuling; QI Bin; XU Weijie


    Cold plasma generated by dielectric barrier discharge (DBD) at atmospheric pressure was adopted for preparation of commercial TiO2 Degussa P25 supported Au catalysts (Au/P25-P) with the assistance of the deposition-precipitation procedure.The influences of the plasma reduction time and calcination on the performance of the Au/P25-P catalysts were investigated.CO oxidation was performed to investigate the catalytic activity of thc Au/P25 catalysts.The results show that DBD cold plasma for the fabrication of Au/P25-P catalysts is a fast process,and Au/P25-P (4 min) exhibited the highest CO oxidation activity due to the complete reduction of Au compounds and less consumption of oxygen vacancies.In order to form more oxygen vacancies active species,Au/P25-P was calcined to obtain Au/P25-PC catalysts.Interestingly,Au/P25-PC exhibited the highest activity for CO oxidation among the Au/P25 samples.The results of transmission electron microscopy (TEM) indicated that the smaller size and high distribution of Au nanoparticles are the mean reasons for a high performance of Au/P25-PC.Atmospheric-pressure DBD cold plasma was proved to be of great efficiency in preparing high performance supported Au catalysts.

  20. Preparation and Characterization of NiO Nanoparticles by Anodic Arc Plasma Method

    Directory of Open Access Journals (Sweden)

    Hongxia Qiao


    Full Text Available NiO nanoparticles with average particle size of 25 nm were successfully prepared by anodic arc plasma method. The composition, morphology, crystal microstructure, specific surface area, infrared spectra, and particle size distribution of product were analyzed by using X-ray diffraction (XRD, transmission electron microscopy (TEM and the corresponding selected area electron diffraction (SAED, Fourier transform infrared (FTIR spectrum, and Brunauer-Emmett-Teller (BET N2 adsorption. The experiment results show that the NiO nanoparticles are bcc structure with spherical shape and well dispersed, the particle size distribution ranging from 15 to 45 nm with the average particle size is about 25 nm, and the specific surface area is 33 m2/g. The infrared absorption band of NiO nanoparticles shows blue shifts compared with that of bulk NiO.


    Institute of Scientific and Technical Information of China (English)



    The micro-Raman spectroscopy and infrared (IR) spectroscopy have been performed for the study of the microstructure of amorphous hydrogenated oxidized silicon (a-SiOx:H) films prepared by Plasma Enhanced Chemical Vapor Deposition technique. It is found that a-SiOx :H consists of two phases: an amorphous silicon-rich phase and an oxygen-rich phase mainly comprised of HSi-SiO2 and HSi-O3. The Raman scattering results exhibit that the frequency of TO-like mode of amorphous silicon red-shifts with decreasing size of silicon-rich region. This is related to the quantum confinement effects, similar to the nanocrystalline silicon.

  2. Graphene-reinforced aluminum matrix composites prepared by spark plasma sintering

    Institute of Scientific and Technical Information of China (English)

    Wen-ming Tian; Song-mei Li; Bo Wang; Xin Chen; Jian-hua Liu; Mei Yu


    Graphene-reinforced 7055 aluminum alloy composites with different contents of graphene were prepared by spark plasma sinter-ing (SPS). The structure and mechanical properties of the composites were investigated. Testing results show that the hardness, compressive strength, and yield strength of the composites are improved with the addition of 1wt% graphene. A clean, strong interface is formed between the metal matrix and graphene via metallurgical bonding on atomic scale. Harmful aluminum carbide (Al4C3) is not formed during SPS processing. Further addition of graphene (above 1wt%) results in the deterioration in mechanical properties of the composites. The agglomeration of graphene plates is exacerbated with increasing graphene content, which is the main reason for this deterioration.

  3. Titanium carbonitride thick coating prepared by plasma spray synthesis and its tribological properties

    Institute of Scientific and Technical Information of China (English)

    ZHU Lin; HE JiNing; YAN DianRan; XIAO LiSong; DONG YanChun; XUE DingChuan; MENG DeLiang


    TiCN coating,owing to its superior wear-resistance,has been frequently applied in many fields. TiCN thick coating was first prepared by reactive plasma spraying. The phase composition,microstructure and tribological properties of the TiCN coating were investigated in this research. Experimental results show that the microstructure of the TiCN coating was quite dense,and there was also a little amount of titanium oxides within the coating. By XPS analysis,Ti-C and Ti-N bonds were detected in the coating. The TiCN coating exhibited superior wear-resistance. The failure mechanism was attributed to the adhesive wear,the grinding of TiCN hard-grain,as well as the coating failure by oxidation. There were more Fe,Cr,O,etc. in the failure zone,suggesting that the corrosion propagated gradually from surface to interior.

  4. Preparation and characterization of molybdenum disilicide coating on molybdenum substrate by air plasma spraying

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yi [Key Laboratory of Ministry of Education for Non-ferrous Materials Science and Engineering, Central South University, Changsha 410083 (China); Key Laboratory of Hunan Province for Metallurgy and Material Processing of Rare Metals, Central South University, Changsha 410083 (China); School of Materials Science and Engineering, Central South University, Changsha 410083 (China); Wang, Dezhi, E-mail: [Key Laboratory of Ministry of Education for Non-ferrous Materials Science and Engineering, Central South University, Changsha 410083 (China); Key Laboratory of Hunan Province for Metallurgy and Material Processing of Rare Metals, Central South University, Changsha 410083 (China); School of Materials Science and Engineering, Central South University, Changsha 410083 (China); Yan, Jianhui [Advanced Materials Synthesis and Application Technology Laboratory, Hunan University of Science and Technology, Xiangtan 411201 (China); Sun, Aokui [Key Laboratory of Ministry of Education for Non-ferrous Materials Science and Engineering, Central South University, Changsha 410083 (China); Key Laboratory of Hunan Province for Metallurgy and Material Processing of Rare Metals, Central South University, Changsha 410083 (China); School of Materials Science and Engineering, Central South University, Changsha 410083 (China)


    MoSi{sub 2} oxidation protective coatings on molybdenum substrate were prepared by air plasma spraying technique (APS). Microstructure, phase composition, porosity, microhardness and bonding strength of the coatings were investigated and determined. Oxidation behavior of the coating at high temperature was also examined. Results show that composition of the coatings is constituted with MoSi{sub 2} and Mo{sub 5}Si{sub 3}, the surface morphology is described as flattened lamellar features, insufficiently flattened protuberance with some degree of surface roughness, a certain quantity of spherical particles, microcracks and pores. Testing results reveal that microhardness and bonding strength of the coatings increase, and porosity decreases with increasing power or decreasing Ar gas flow rate. Moreover, with decreasing the porosity, the microhardness of the coatings increases. The bonding strength of the coatings also increases with increasing spray distance. The MoSi{sub 2} coated Mo substrate exhibited a good oxidation resistance at 1200 °C.

  5. Preparation of silicon carbide nitride films on Si substrate by pulsed high-energy density plasma

    Institute of Scientific and Technical Information of China (English)


    Thin films of silicon carbide nitride (SiCN) were prepared on (111) oriented silicon substrates by pulsed high-energy density plasma (PHEDP). The evolution of the chemical bonding states between silicon, nitrogen and carbon was investigated as a function of discharge voltage using X-ray photoelectron spectroscopy. With an increase in discharge voltage both the C1s and N 1s spectra shift to lower binding energy due to the formation of C-Si and N-Si bonds. The Si-C-N bonds were observed in the deconvolved C1s and N 1s spectra. The X-ray diffractometer (XRD) results show that there were no crystals in the films. The thickness of the films was approximately 1-2 μm with scanning electron microscopy (SEM).

  6. Determination of metals in composite diet samples by inductively coupled plasma-mass spectrometry. (United States)

    Melnyk, Lisa Jo; Morgan, Jeffrey N; Fernando, Reshan; Pellizzari, Edo D; Akinbo, Olujide


    A study was conducted to evaluate the applicability of inductively coupled plasma-mass spectrometry (ICP-MS) techniques for determination of metals in composite diets. Aluminum, cadmium, chromium, copper, lead, manganese, nickel, vanadium, and zinc were determined by this method. Atmospheric pressure microwave digestion was used to solubilize analytes in homogenized composite diet samples, and this procedure was followed by ICP-MS analysis. Recovery of certified elements from standard reference materials ranged from 92 to 119% with relative standard deviations (RSDs) of 0.4-1.9%. Recovery of elements from fortified composite diet samples ranged from 75 to 129% with RSDs of 0-11.3%. Limits of detection ranged from 1 to 1700 ng/g; high values were due to significant amounts of certain elements naturally present in composite diets. Results of this study demonstrate that low-resolution quadrupole-based ICP-MS provides precise and accurate measurements of the elements tested in composite diet samples.

  7. Human genomic DNA analysis using a semi-automated sample preparation, amplification, and electrophoresis separation platform. (United States)

    Raisi, Fariba; Blizard, Benjamin A; Raissi Shabari, Akbar; Ching, Jesus; Kintz, Gregory J; Mitchell, Jim; Lemoff, Asuncion; Taylor, Mike T; Weir, Fred; Western, Linda; Wong, Wendy; Joshi, Rekha; Howland, Pamela; Chauhan, Avinash; Nguyen, Peter; Petersen, Kurt E


    The growing importance of analyzing the human genome to detect hereditary and infectious diseases associated with specific DNA sequences has motivated us to develop automated devices to integrate sample preparation, real-time PCR, and microchannel electrophoresis (MCE). In this report, we present results from an optimized compact system capable of processing a raw sample of blood, extracting the DNA, and performing a multiplexed PCR reaction. Finally, an innovative electrophoretic separation was performed on the post-PCR products using a unique MCE system. The sample preparation system extracted and lysed white blood cells (WBC) from whole blood, producing DNA of sufficient quantity and quality for a polymerase chain reaction (PCR). Separation of multiple amplicons was achieved in a microfabricated channel 30 microm x 100 microm in cross section and 85 mm in length filled with a replaceable methyl cellulose matrix operated under denaturing conditions at 50 degrees C. By incorporating fluorescent-labeled primers in the PCR, the amplicons were identified by a two-color (multiplexed) fluorescence detection system. Two base-pair resolution of single-stranded DNA (PCR products) was achieved. We believe that this integrated system provides a unique solution for DNA analysis.

  8. Sample preparation for laser-microdissection of soybean shoot apical meristem

    Directory of Open Access Journals (Sweden)

    Chui E. Wong


    Full Text Available The shoot apical meristem houses stem cells responsible for the continuous formation of aerial plant organs including leaves and stems throughout the life of plants. Laser-microdissection in combination with high-throughput technology such as next generation sequencing permits an in-depth analysis of molecular events associated with specific cell type of interest. Sample preparation is the most critical step in ensuring good quality RNA to be extracted from samples following laser-microdissection. Here, we optimized the sample preparation for a major legume crop, soybean. We used Farmer’s solution as a fixative and paraffin as the embedding medium for soybean shoot apical meristem tissue without the use of any specialized equipment. Shorter time for tissue fixation (two days was found to be critical for the preservation of RNA in soybean shoot apical meristem. We further demonstrated the utility of this method for different tissues derived from soybean and rice. The method outlined here shall facilitate studies on crop plants involving laser-microdissection.

  9. Application of a Dual-Arm Robot in Complex Sample Preparation and Measurement Processes. (United States)

    Fleischer, Heidi; Drews, Robert Ralf; Janson, Jessica; Chinna Patlolla, Bharath Reddy; Chu, Xianghua; Klos, Michael; Thurow, Kerstin


    Automation systems with applied robotics have already been established in industrial applications for many years. In the field of life sciences, a comparable high level of automation can be found in the areas of bioscreening and high-throughput screening. Strong deficits still exist in the development of flexible and universal fully automated systems in the field of analytical measurement. Reasons are the heterogeneous processes with complex structures, which include sample preparation and transport, analytical measurements using complex sensor systems, and suitable data analysis and evaluation. Furthermore, the use of nonstandard sample vessels with various shapes and volumes results in an increased complexity. The direct use of existing automation solutions from bioscreening applications is not possible. A flexible automation system for sample preparation, analysis, and data evaluation is presented in this article. It is applied for the determination of cholesterol in biliary endoprosthesis using gas chromatography-mass spectrometry (GC-MS). A dual-arm robot performs both transport and active manipulation tasks to ensure human-like operation. This general robotic concept also enables the use of manual laboratory devices and equipment and is thus suitable in areas with a high standardization grade.

  10. Preparation of SrZrO3 Thermal Barrier Coating by Solution Precursor Plasma Spray (United States)

    Li, Xinhui; Ma, Wen; Wen, Jing; Bai, Yu; Sun, Li; Chen, Baodong; Dong, Hongying; Shuang, Yingchai


    The solution precursor plasma spray (SPPS) process is capable of depositing highly durable thermal barrier coatings (TBCs). In this study, an aqueous chemical precursor feedstock was injected into the plasma jet to deposit SrZrO3 thermal barrier coating on metal substrate. Taguchi design of experiments was employed to optimize the SPPS process. The thermal characteristics and phase evolution of the SrZrO3 precursor, as well as the influence of various spray parameters on the coating deposition rate, microhardness, microstructure, and phase stability, were investigated. The experimental results showed that, at given spray distance, feedstock flow rate, and atomization pressure, the optimized spray parameters were arc current of 600 A, argon flow rate of 40 L/min, and hydrogen flow rate of 10 L/min. The SrZrO3 coating prepared using the optimized spray parameters had single-pass thickness of 6.0 μm, porosity of 18%, and microhardness of 6.8 ± 0.1 GPa. Phase stability studies indicated that the as-sprayed SrZrO3 coating had good phase stability in the temperature range from room temperature to 1400 °C, gradually exhibiting a phase transition from t'-ZrO2 to m-ZrO2 in the SrZrO3 coating at 1450 °C with increasing time, while the SrZrO3 phase did not change.

  11. Studies on Nanocrystalline TiN Coatings Prepared by Reactive Plasma Spraying

    Directory of Open Access Journals (Sweden)

    Dong Yanchun


    Full Text Available Titanium nitride (TiN coatings with nanostructure were prepared on the surface of 45 steel (Fe-0.45%C via reactive plasma spraying (denoted as RPS Ti powders using spraying gun with self-made reactive chamber. The microstructural characterization, phases constitute, grain size, microhardness, and wear resistance of TiN coatings were systematically investigated. The grain size was obtained through calculation using the Scherrer formula and observed by TEM. The results of X-ray diffraction and electron diffraction indicated that the TiN is main phase of the TiN coating. The forming mechanism of the nano-TiN was characterized by analyzing the SEM morphologies of surface of TiN coating and TiN drops sprayed on the surface of glass, and observing the temperature and velocity of plasma jet using Spray Watch. The tribological properties of the coating under nonlubricated condition were tested and compared with those of the AISI M2 high-speed steel and Al2O3 coating. The results have shown that the RPS TiN coating presents better wear resistance than the M2 high-speed steel and Al2O3 coating under nonlubricated condition. The microhardness of the cross-section and longitudinal section of the TiN coating was tested. The highest hardness of the cross-section of TiN coating is 1735.43HV100 g.

  12. Preparative soft and reactive landing of gas-phase ions on plasma-treated metal surfaces. (United States)

    Volný, Michael; Elam, W Timothy; Ratner, Buddy D; Turecek, Frantisek


    Soft landing of singly charged gas-phase ions on dry metal surfaces that were pretreated in situ by oxygen plasma results in 0.1-2% total yields of recovered intact compounds. Lysine, peptides, crystal violet dye, and a biotin conjugate are found to survive soft landing of hyperthermal ions of up to 50-eV kinetic energy. Soft landing at 40-50-eV ion kinetic energies of a fluorescence-labeled biotin conjugate results in an immobilized fraction that cannot be washed from the surface and is found to contain an intact biotin moiety. The present results represent an approximately 10(4) fold improvement in soft-landing efficiency and indicate that plasma-treated metal surfaces can be useful for preparative separation of organic and biological molecules by mass spectrometry. The substantial improvement in soft-landing yields results from a high transmission of electrosprayed ions into the vacuum system, efficient and nondestructive discharge of ions on the metal oxide surface, and facile analyte recovery in the absence of a matrix.

  13. Plasma concentrations resulting from florfenicol preparations given to pigs in their drinking water. (United States)

    Gutiérrez, L; Vargas, D; Ocampo, L; Sumano, H; Martinez, R; Tapia, G


    Florfenicol administered through the drinking water has been recommended as a metaphylactic antibacterial drug to control outbreaks of respiratory diseases in pigs caused by strains of Actinobacillus pleuropneumoniae and Pasteurella multocida, yet it is difficult to pinpoint in practice when the drug is given metaphylactically or therapeutically. Further, pigs are likely to reject florfenicol-medicated water, and plasma concentrations of the drug are likely to be marginal for diseases caused by Escherichia coli, Klebsiella pneumoniae, and Staphylococcus aureus. The reported minimal inhibitory concentration (MIC) values for these organisms show a breakpoint of 2 to 3 μg/mL. An experiment was conducted during September and October 2009. One hundred twenty healthy crossbred pigs (Landrace-Yorkshire), weighing 23 ± 6.2 kg, were used in this trial. They were randomly assigned to 5 groups, with 3 replicates of 8 animals/group. Two commercial preparations of florfenicol were administered through the drinking water at 2 concentrations (0.01 and 0.015%). Water intake was measured before and after medication, and plasma concentrations of florfenicol were determined by HPLC. Considerable rejection of florfenicol-medicated water was observed. However, plasma florfenicol concentrations were of a range sufficient for a methaphylaxis approach to preventing disease by bacteria, with MIC breakpoints of ≤ 0.25 μg/mL. Decreased efficacy as a metaphylactic medication should be expected for bacteria with MIC >0.25 μg/mL, considering the reported existence of bacteria resistant to florfenicol and the natural resistance of Streptococcus suis or E. coli to this drug.

  14. Observation of asymmetrically imploded core plasmas with a two-dimensional sampling image x-ray streak camera. (United States)

    Shiraga, Hiroyuki; Lee, Myongdok; Mahigashi, Norimitsu; Fujioka, Shinsuke; Azechi, Hiroshi


    A shell target with a cone for guiding the heating beam has been proposed for the fast ignition scheme. Implosion of such target is no longer symmetric because of the cone. A fast two-dimensional x-ray imaging technique, two-dimensional (2D) sampling image x-ray streak camera was applied for the first time to observation of the dynamics of implosion and core plasma. X-ray emission image of the plasma was sampled with two-dimensionally distributed image sampling points, streaked with the tube, and the recorded signals were reconstructed as sequential 2D frame images. Shape and movement of the core plasma were clearly observed.

  15. Gel-aided sample preparation (GASP)--a simplified method for gel-assisted proteomic sample generation from protein extracts and intact cells. (United States)

    Fischer, Roman; Kessler, Benedikt M


    We describe a "gel-assisted" proteomic sample preparation method for MS analysis. Solubilized protein extracts or intact cells are copolymerized with acrylamide, facilitating denaturation, reduction, quantitative cysteine alkylation, and matrix formation. Gel-aided sample preparation has been optimized to be highly flexible, scalable, and to allow reproducible sample generation from 50 cells to milligrams of protein extracts. This methodology is fast, sensitive, easy-to-use on a wide range of sample types, and accessible to nonspecialists. © 2014 The Authors. PROTEOMICS published by Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Error baseline rates of five sample preparation methods used to characterize RNA virus populations (United States)

    Kugelman, Jeffrey R.; Wiley, Michael R.; Nagle, Elyse R.; Reyes, Daniel; Pfeffer, Brad P.; Kuhn, Jens H.; Sanchez-Lockhart, Mariano; Palacios, Gustavo F.


    Individual RNA viruses typically occur as populations of genomes that differ slightly from each other due to mutations introduced by the error-prone viral polymerase. Understanding the variability of RNA virus genome populations is critical for understanding virus evolution because individual mutant genomes may gain evolutionary selective advantages and give rise to dominant subpopulations, possibly even leading to the emergence of viruses resistant to medical countermeasures. Reverse transcription of virus genome populations followed by next-generation sequencing is the only available method to characterize variation for RNA viruses. However, both steps may lead to the introduction of artificial mutations, thereby skewing the data. To better understand how such errors are introduced during sample preparation, we determined and compared error baseline rates of five different sample preparation methods by analyzing in vitro transcribed Ebola virus RNA from an artificial plasmid-based system. These methods included: shotgun sequencing from plasmid DNA or in vitro transcribed RNA as a basic “no amplification” method, amplicon sequencing from the plasmid DNA or in vitro transcribed RNA as a “targeted” amplification method, sequence-independent single-primer amplification (SISPA) as a “random” amplification method, rolling circle reverse transcription sequencing (CirSeq) as an advanced “no amplification” method, and Illumina TruSeq RNA Access as a “targeted” enrichment method. The measured error frequencies indicate that RNA Access offers the best tradeoff between sensitivity and sample preparation error (1.4−5) of all compared methods. PMID:28182717

  17. Simple, Expendable, 3D-Printed Microfluidic Systems for Sample Preparation of Petroleum. (United States)

    Kataoka, Érica M; Murer, Rui C; Santos, Jandyson M; Carvalho, Rogério M; Eberlin, Marcos N; Augusto, Fabio; Poppi, Ronei J; Gobbi, Angelo L; Hantao, Leandro W


    In this study, we introduce a simple protocol to manufacture disposable, 3D-printed microfluidic systems for sample preparation of petroleum. This platform is produced with a consumer-grade 3D-printer, using fused deposition modeling. Successful incorporation of solid-phase extraction (SPE) to microchip was ensured by facile 3D element integration using proposed approach. This 3D-printed μSPE device was applied to challenging matrices in oil and gas industry, such as crude oil and oil-brine emulsions. Case studies investigated important limitations of nonsilicon and nonglass microchips, namely, resistance to nonpolar solvents and conservation of sample integrity. Microfluidic features remained fully functional even after prolonged exposure to nonpolar solvents (20 min). Also, 3D-printed μSPE devices enabled fast emulsion breaking and solvent deasphalting of petroleum, yielding high recovery values (98%) without compromising maltene integrity. Such finding was ascertained by high-resolution molecular analyses using comprehensive two-dimensional gas chromatography and gas chromatography/mass spectrometry by monitoring important biomarker classes, such as C10 demethylated terpanes, ααα-steranes, and monoaromatic steroids. 3D-Printed chips enabled faster and reliable preparation of maltenes by exhibiting a 10-fold reduction in sample processing time, compared to the reference method. Furthermore, polar (oxygen-, nitrogen-, and sulfur-containing) analytes found in low-concentrations were analyzed by Fourier transform ion cyclotron resonance mass spectrometry. Analysis results demonstrated that accurate characterization may be accomplished for most classes of polar compounds, except for asphaltenes, which exhibited lower recoveries (82%) due to irreversible adsorption to sorbent phase. Therefore, 3D-printing is a compelling alternative to existing microfabrication solutions, as robust devices were easy to prepare and operate.

  18. Review of sample preparation strategies for MS-based metabolomic studies in industrial biotechnology. (United States)

    Causon, Tim J; Hann, Stephan


    Fermentation and cell culture biotechnology in the form of so-called "cell factories" now play an increasingly significant role in production of both large (e.g. proteins, biopharmaceuticals) and small organic molecules for a wide variety of applications. However, associated metabolic engineering optimisation processes relying on genetic modification of organisms used in cell factories, or alteration of production conditions remain a challenging undertaking for improving the final yield and quality of cell factory products. In addition to genomic, transcriptomic and proteomic workflows, analytical metabolomics continues to play a critical role in studying detailed aspects of critical pathways (e.g. via targeted quantification of metabolites), identification of biosynthetic intermediates, and also for phenotype differentiation and the elucidation of previously unknown pathways (e.g. via non-targeted strategies). However, the diversity of primary and secondary metabolites and the broad concentration ranges encompassed during typical biotechnological processes means that simultaneous extraction and robust analytical determination of all parts of interest of the metabolome is effectively impossible. As the integration of metabolome data with transcriptome and proteome data is an essential goal of both targeted and non-targeted methods addressing production optimisation goals, additional sample preparation steps beyond necessary sampling, quenching and extraction protocols including clean-up, analyte enrichment, and derivatisation are important considerations for some classes of metabolites, especially those present in low concentrations or exhibiting poor stability. This contribution critically assesses the potential of current sample preparation strategies applied in metabolomic studies of industrially-relevant cell factory organisms using mass spectrometry-based platforms primarily coupled to liquid-phase sample introduction (i.e. flow injection, liquid

  19. Absorption kinetics and steady-state plasma concentrations of theophylline following therapeutic doses of two sustained-release preparations

    DEFF Research Database (Denmark)

    Andersen, O; Nielsen, M K; Eriksen, P B;


    Ten healthy volunteers received two sustained-release preparations as a single and multiple dose regimen in an open crossover study. Plasma theophylline concentrations were measured by an enzyme immunoassay. The limited fluctuation of the theophylline levels at steady state, with twice daily...... formulation, whereas this was not the case for the other (r = 0.27 and 0.49). The daily dose necessary to keep the plasma concentration within the therapeutic range of 55-110 mumole/liter varied from 7.9 to 22.9 mg/kg. Only mild side effects were recorded, but they were not correlated to the plasma...... theophylline concentration....

  20. Determination of the neutral oxygen atom density in a plasma reactor loaded with metal samples

    Energy Technology Data Exchange (ETDEWEB)

    Mozetic, Miran; Cvelbar, Uros [Jozef Stefan Institute, Jamova cesta 39, 1000 Ljubljana (Slovenia)], E-mail:


    The density of neutral oxygen atoms was determined during processing of metal samples in a plasma reactor. The reactor was a Pyrex tube with an inner diameter of 11 cm and a length of 30 cm. Plasma was created by an inductively coupled radiofrequency generator operating at a frequency of 27.12 MHz and output power up to 500 W. The O density was measured at the edge of the glass tube with a copper fiber optics catalytic probe. The O atom density in the empty tube depended on pressure and was between 4 and 7 x 10{sup 21} m{sup -3}. The maximum O density was at a pressure of about 150 Pa, while the dissociation fraction of O{sub 2} molecules was maximal at the lowest pressure and decreased with increasing pressure. At about 300 Pa it dropped below 10%. The measurements were repeated in the chamber loaded with different metallic samples. In these cases, the density of oxygen atoms was lower than that in the empty chamber. The results were explained by a drain of O atoms caused by heterogeneous recombination on the samples.

  1. Determination by high-performance liquid chromatography of phenylbutazone in samples of plasma from fighting bulls. (United States)

    Marti, M I González; Sánchez, González C I; Jiménez, Hernández; Cachán, García; Castro, de Cabo M J; Cuadrado, A L Garzón


    The purpose of this study was to investigate the possible presence of phenylbutazone in plasma samples from fighting bulls killed in 2nd and 3rd category bullrings in the province of Salamanca (Spain) in 1998, 1999 and 2000. For quantitative and qualitative determination, a high-performance liquid chromatograph was used, equipped with a photodiode-array detector and setting wavelengths at 240, 254 and 284 nm. The mobile phase optimized for the simultaneous detection of dexamethasone, betamethasone, flunixin and phenylbutazone, was 0.01 M acetic acid pH 3 in methanol (35:65 v/v) at a flow rate of 1 ml/min. Plasma samples were deproteinized with 400 microl of acetonitrile and 20 microl of the supernatant were injected directly into the chromatographic system equipped with a Lichrospher 60 RP select B column and guard column. For the quantitative analysis, standard calibration curves were made in a concentration range between 0.25 and 30 microg/ml, using betamethasone as internal standard. The retention time of phenylbutazone was 8.7 +/- 0.2 min and recovery was 83%. The detection and quantification limits were 0.016 and 0.029, respectively for A=240 nm. The study results show that 17 of the 74 samples analyzed in 1998, 18 of those from 1999 and 10 of those from 2000 were positive for phenylbutazone.

  2. Etching of Niobium Sample Placed on Superconducting Radio Frequency Cavity Surface in Ar/CL2 Plasma

    Energy Technology Data Exchange (ETDEWEB)

    Janardan Upadhyay, Larry Phillips, Anne-Marie Valente


    Plasma based surface modification is a promising alternative to wet etching of superconducting radio frequency (SRF) cavities. It has been proven with flat samples that the bulk Niobium (Nb) removal rate and the surface roughness after the plasma etchings are equal to or better than wet etching processes. To optimize the plasma parameters, we are using a single cell cavity with 20 sample holders symmetrically distributed over the cell. These holders serve the purpose of diagnostic ports for the measurement of the plasma parameters and for the holding of the Nb sample to be etched. The plasma properties at RF (100 MHz) and MW (2.45 GHz) frequencies are being measured with the help of electrical and optical probes at different pressures and RF power levels inside of this cavity. The niobium coupons placed on several holders around the cell are being etched simultaneously. The etching results will be presented at this conference.

  3. Effects of sample preparation conditions on biomolecular solid-state NMR lineshapes

    Energy Technology Data Exchange (ETDEWEB)

    Jakeman, David L.; Mitchell, Dan J.; Shuttleworth, Wendy A.; Evans, Jeremy N.S. [Washington State University, Department of Biochemistry and Biophysics (United States)


    Sample preparation conditions with the 46 kDa enzyme complex of 5-enolpyruvyl-shikimate-3-phosphate (EPSP) synthase, shikimate-3-phosphate (S3P) and glyphosate (GLP) have been examined in an attempt to reduce linewidths in solid-state NMR spectra. The linewidths of {sup 13}P resonances associated with enzyme bound S3P and GLP in the lyophilized ternary complex have been reduced to 150 {+-} 12 Hz and 125 {+-} 7 Hz respectively, by a variety of methods involving additives and freezing techniques.

  4. The Structure and Mechanical Properties of High-Strength Bulk Ultrafine-Grained Cobalt Prepared Using High-Energy Ball Milling in Combination with Spark Plasma Sintering

    Directory of Open Access Journals (Sweden)

    Ivo Marek


    Full Text Available In this study, bulk ultrafine-grained and micro-crystalline cobalt was prepared using a combination of high-energy ball milling and subsequent spark plasma sintering. The average grain sizes of the ultrafine-grained and micro-crystalline materials were 200 nm and 1 μm, respectively. Mechanical properties such as the compressive yield strength, the ultimate compressive strength, the maximum compressive deformation and the Vickers hardness were studied and compared with those of a coarse-grained as-cast cobalt reference sample. The bulk ultrafine-grained sample showed an ultra-high compressive yield strength that was greater than 1 GPa, which is discussed with respect to the preparation technique and a structural investigation.

  5. Nanocrystalline Al7075 + 1 wt % Zr Alloy Prepared Using Mechanical Milling and Spark Plasma Sintering. (United States)

    Molnárová, Orsolya; Málek, Přemysl; Veselý, Jozef; Šlapáková, Michaela; Minárik, Peter; Lukáč, František; Chráska, Tomáš; Novák, Pavel; Průša, Filip


    The microstructure, phase composition, and microhardness of both gas-atomized and mechanically milled powders of the Al7075 + 1 wt % Zr alloy were investigated. The gas-atomized powder exhibited a cellular microstructure (grain size of a few µm) with layers of intermetallic phases along the cell boundaries. Mechanical milling (400 revolutions per minute (RPM)/8 h) resulted in a grain size reduction to the nanocrystalline range (20 to 100 nm) along with the dissolution of the intermetallic phases. Milling led to an increase in the powder's microhardness from 97 to 343 HV. Compacts prepared by spark plasma sintering (SPS) exhibited negligible porosity. The grain size of the originally gas-atomized material was retained, but the continuous layers of intermetallic phases were replaced by individual particles. Recrystallization led to a grain size increase to 365 nm in the SPS compact prepared from the originally milled powder. Small precipitates of the Al₃Zr phase were observed in the SPS compacts, and they are believed to be responsible for the retainment of the sub-microcrystalline microstructure during SPS. A more intensive precipitation in this SPS compact can be attributed to a faster diffusion due to a high density of dislocations and grain boundaries in the milled powder.

  6. Nanocrystalline Al7075 + 1 wt % Zr Alloy Prepared Using Mechanical Milling and Spark Plasma Sintering

    Directory of Open Access Journals (Sweden)

    Orsolya Molnárová


    Full Text Available The microstructure, phase composition, and microhardness of both gas-atomized and mechanically milled powders of the Al7075 + 1 wt % Zr alloy were investigated. The gas-atomized powder exhibited a cellular microstructure (grain size of a few µm with layers of intermetallic phases along the cell boundaries. Mechanical milling (400 revolutions per minute (RPM/8 h resulted in a grain size reduction to the nanocrystalline range (20 to 100 nm along with the dissolution of the intermetallic phases. Milling led to an increase in the powder’s microhardness from 97 to 343 HV. Compacts prepared by spark plasma sintering (SPS exhibited negligible porosity. The grain size of the originally gas-atomized material was retained, but the continuous layers of intermetallic phases were replaced by individual particles. Recrystallization led to a grain size increase to 365 nm in the SPS compact prepared from the originally milled powder. Small precipitates of the Al3Zr phase were observed in the SPS compacts, and they are believed to be responsible for the retainment of the sub-microcrystalline microstructure during SPS. A more intensive precipitation in this SPS compact can be attributed to a faster diffusion due to a high density of dislocations and grain boundaries in the milled powder.

  7. Corrosion behaviors of NdFeB magnets prepared by spark plasma sintering

    Institute of Scientific and Technical Information of China (English)

    Tao Li; Ming Yue; Aizhi Sun; Baoqin Qiu; Yaofu Xiao; Jiuxing Zhang


    The spark plasma sintering (SPS) technique was introduced into the field of NdFeB preparation due to its own advantages.High property NdFeB magnets with fine grains were prepared by SPS method. The corrosion behaviors of SPS NdFeB were studied by electrochemical measurements and 92% RH hyther tests at 353 K. The results were compared with those of the traditional sintered NdFeB magnets. It shows that both the SPS NdFeB and the traditional sintered NdFeB have good corrosion resistance in alkaline environment due to surface passivation; while, the fine grain microstructure of SPS NdFeB results in a more homogeneous phase composition distribution and thus reduces the electrochemical inhomogenity between the ferromagnetic phase and the Nd-rich intergranular phase in the magnet. Therefore, the SPS NdFeB exhibits better corrosion resistance than the traditional sintered NdFeB in neutral and weak acidic environment.

  8. Measurement of glomerular filtration rate in adults: accuracy of five single-sample plasma clearance methods

    DEFF Research Database (Denmark)

    Rehling, M; Rabøl, A


    After an intravenous injection of a tracer that is removed from the body solely by filtration in the kidneys, the glomerular filtration rate (GFR) can be determined from its plasma clearance. The method requires a great number of blood samples but collection of urine is not needed. In the present......-acetate) was determined simultaneously. Using these clearance values as reference the accuracy of six simplified methods were studied: five single-sample methods and one five-sample method. The standard error of estimate (SEE) of the single-sample methods ranged from 4.2 to 7.5 ml min-1 using EDTA, and from 3.8 to 6.3 ml...... min-1 using DTPA. SEE of the five-samples method was 3.0 ml min-1 (EDTA) and 3.1 ml min-1 (DTPA). The single-sample methods given by Christensen & Groth (1986) and by Tauxe (1986) are recommended for daily use, as SEE was small even at low GFR values. In patients with GFR less than 80 ml min-1...

  9. Effects of Long-Term Storage Time and Original Sampling Month on Biobank Plasma Protein Concentrations. (United States)

    Enroth, Stefan; Hallmans, Göran; Grankvist, Kjell; Gyllensten, Ulf


    The quality of clinical biobank samples is crucial to their value for life sciences research. A number of factors related to the collection and storage of samples may affect the biomolecular composition. We have studied the effect of long-time freezer storage, chronological age at sampling, season and month of the year and on the abundance levels of 108 proteins in 380 plasma samples collected from 106 Swedish women. Storage time affected 18 proteins and explained 4.8-34.9% of the observed variance. Chronological age at sample collection after adjustment for storage-time affected 70 proteins and explained 1.1-33.5% of the variance. Seasonal variation had an effect on 15 proteins and month (number of sun hours) affected 36 proteins and explained up to 4.5% of the variance after adjustment for storage-time and age. The results show that freezer storage time and collection date (month and season) exerted similar effect sizes as age on the protein abundance levels. This implies that information on the sample handling history, in particular storage time, should be regarded as equally prominent covariates as age or gender and need to be included in epidemiological studies involving protein levels.

  10. Tantalum-Tungsten Oxide Thermite Composite Prepared by Sol-Gel Synthesis and Spark Plasma Sintering

    Energy Technology Data Exchange (ETDEWEB)

    Cervantes, O; Kuntz, J; Gash, A; Munir, Z


    Energetic composite powders consisting of sol-gel derived nanostructured tungsten oxide were produced with various amounts of micrometer-scale tantalum fuel metal. Such energetic composite powders were ignition tested and results show that the powders are not sensitive to friction, spark and/or impact ignition. Initial consolidation experiments, using the High Pressure Spark Plasma Sintering (HPSPS) technique, on the sol-gel derived nanostructured tungsten oxide produced samples with higher relative density than can be achieved with commercially available tungsten oxide. The sol-gel derived nanostructured tungsten oxide with immobilized tantalum fuel metal (Ta - WO{sub 3}) energetic composite was consolidated to a density of 9.17{sup -3} or 93% relative density. In addition those parts were consolidated without significant pre-reaction of the constituents, thus the sample retained its stored chemical energy.

  11. Quantitative analysis of Tenecteplase in rat plasma samples using LC-MS/MS as an alternative for ELISA

    NARCIS (Netherlands)

    Buscher, B.A.P.; Gerritsen, H.; Schöll, I. van; Cnubben, N.H.P.; Brüll, L.P.


    An LC-MS/MS method has been developed for the quantitative determination of a protein drug (Tenecteplase; MW 58,777 Da) in rat plasma. The protein was digested with trypsin without prior clean-up of the plasma sample, without the use of a label nor internal standard. A limited validation was perform

  12. Quantitative analysis of Tenecteplase in rat plasma samples using LC-MS/MS as an alternative for ELISA

    NARCIS (Netherlands)

    Buscher, B.A.P.; Gerritsen, H.; Schöll, I. van; Cnubben, N.H.P.; Brüll, L.P.


    An LC-MS/MS method has been developed for the quantitative determination of a protein drug (Tenecteplase; MW 58,777 Da) in rat plasma. The protein was digested with trypsin without prior clean-up of the plasma sample, without the use of a label nor internal standard. A limited validation was perform

  13. Sample preparation and separation techniques for bioanalysis of morphine and related substances. (United States)

    Hansen, Steen Honoré


    In present time the use or misuse of morphine and its derivatives are monitored by assaying the presence of the drug and its metabolites in biofluids. In the present review, focus is placed on the sample preparation and on the separation techniques used in the current best practices of bioanalysis of morphine and its major metabolites. However, as methods for testing the misuse of heroin, a morphine derivative, often involve bioanalytical methods that cover a number of other illicit drug substances, such methods are also included in the review. Furthermore, the review also includes bioanalysis in a broader perspective as analysis of plant materials, cell cultures and environmental samples. The review is not intended to cover all publications that include bioanalysis of morphine but is more to be considered a view into the current best practices of bioanalysis of morphine, its metabolites and other related substances.

  14. Capacitive deionization on-chip as a method for microfluidic sample preparation. (United States)

    Roelofs, Susan H; Kim, Bumjoo; Eijkel, Jan C T; Han, Jongyoon; van den Berg, Albert; Odijk, Mathieu


    Desalination as a sample preparation step is essential for noise reduction and reproducibility of mass spectrometry measurements. A specific example is the analysis of proteins for medical research and clinical applications. Salts and buffers that are present in samples need to be removed before analysis to improve the signal-to-noise ratio. Capacitive deionization is an electrostatic desalination (CDI) technique which uses two porous electrodes facing each other to remove ions from a solution. Upon the application of a potential of 0.5 V ions migrate to the electrodes and are stored in the electrical double layer. In this article we demonstrate CDI on a chip, and desalinate a solution by the removal of 23% of Na(+) and Cl(-) ions, while the concentration of a larger molecule (FITC-dextran) remains unchanged. For the first time impedance spectroscopy is introduced to monitor the salt concentration in situ in real-time in between the two desalination electrodes.

  15. Crednerite-CuMnO{sub 2} thin films prepared using atmospheric pressure plasma annealing

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Hong-Ying, E-mail: [Department of Chemical and Materials Engineering, National Kaohsiung University of Applied Sciences, 415 Chiken Kuang Road, Kaohsiung 807, Taiwan, ROC (China); Lin, Yu-Chang [Department of Chemical and Materials Engineering, National Kaohsiung University of Applied Sciences, 415 Chiken Kuang Road, Kaohsiung 807, Taiwan, ROC (China); Lee, Jiann-Shing [Department of Applied Physics, National Pingtung University, 4-18 Minsheng Road, Pingtung City 900, Taiwan, ROC (China)


    Highlights: • Crednerite-CuMnO{sub 2} thin films were formed at atmospheric pressure plasma with N{sub 2}–(5–10)%O{sub 2}. • The binding energy of Cu-2p spectrum of the crednerite-CuMnO{sub 2} thin films was 932.3 eV (Cu{sup +}). • The binding energies of Mn-3p spectrum were 48.1 ± 0.2 eV (Mn{sup 3+}) and 50.0 ± 0.2 eV (Mn{sup 4+}). • The cation distribution in the crednerite-CuMnO{sub 2} thin films was Cu{sub 1.0}{sup +}(Mn{sub 0.6}{sup 3+}Mn{sub 0.4}{sup 4+})O{sub 2}. • The electrical conductivity of CuMnO{sub 2} thin films was (2.61–2.65) × 10{sup 4} Ω cm. - Abstract: This study reports the preparation of crednerite-CuMnO{sub 2} thin films using atmospheric pressure plasma annealing. The pristine thin films were deposited onto a quartz substrate using the sol–gel process. The specimens were then annealed using atmospheric pressure plasma at N{sub 2}–(0–20%)O{sub 2} for 20 min. Crednerite-CuMnO{sub 2} thin films were obtained using atmospheric pressure plasma annealing at N{sub 2}–5%O{sub 2} and N{sub 2}–10%O{sub 2}. The lattice parameters of the thin films were a = 0.5574–0.5580 nm, b = 0.2874–0.2879 nm, c = 0.5878–0.5881 nm, and β = 104.15–104.25°, which agree well with previous reports. The Raman shifts of the crednerite-CuMnO{sub 2} thin films were 688 ± 2 cm{sup −1}, 381 ± 2 cm{sup −1}, and 314 ± 2 cm{sup −1}. The binding energy of Cu-2p spectrum of the crednerite-CuMnO{sub 2} thin films was 932.3 ± 0.2 eV representing the Cu{sup +} in the thin films. The binding energies of Mn-3p spectrum were 48.1 ± 0.2 eV (Mn{sup 3+}) and 50.0 ± 0.2 eV (Mn{sup 4+}). Furthermore, the cation distribution in the thin films was Cu{sup +}{sub 1.0}(Mn{sup 3+}{sub 0.6}Mn{sup 4+}{sub 0.4})O{sub 2} from the X-ray photoelectron spectroscopy measurement. When the crednerite-CuMnO{sub 2} phase was formed, the surface morphology exhibited a compact/dense granular morphology. The optical bandgap of the crednerite-CuMnO{sub 2} thin

  16. Determination of Cu, Mn, Ni and Sn in gasoline by electrothermal vaporization inductively coupled plasma mass spectrometry, and emulsion sample introduction (United States)

    Saint'Pierre, Tatiana D.; Dias, Lúcia Felicidade; Pozebon, Dirce; Aucélio, Ricardo Q.; Curtius, Adilson J.; Welz, Bernhard


    Trace metals in fuels, except in the case of additives, are usually undesirable and normally they occur in very low concentrations in gasoline, requiring sensitive techniques for their determination. Coupling of electrothermal vaporization with inductively coupled plasma mass spectrometry minimizes the problems related to the introduction of organic solvents into the plasma. Furthermore, sample preparation as oil-in-water emulsions reduces problems related to gasoline analysis. In this work, a method for determination of Cu, Mn, Ni and Sn in gasoline is proposed. Samples were prepared by forming a 10-fold diluted emulsion with a surfactant (Triton X-100), after treatment with concentrated HNO 3. The sample emulsion was pre-concentrated in the graphite tube by repeated pipetting and drying. External calibration was used with aqueous standards in a purified gasoline emulsion. Six samples from different gas stations were analyzed, and the analyte concentrations were found to be in the μg l -1 range or below. The limits of detection were 0.22, 0.02, 0.38 and 0.03 μg l -1 for Cu, Mn, Ni and Sn, respectively. The accuracy of the method was estimated using a recovery test.

  17. Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater (United States)

    Yokochi, Reika


    Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

  18. Matrix compatible solid phase microextraction coating, a greener approach to sample preparation in vegetable matrices. (United States)

    Naccarato, Attilio; Pawliszyn, Janusz


    This work proposes the novel PDMS/DVB/PDMS fiber as a greener strategy for analysis by direct immersion solid phase microextraction (SPME) in vegetables. SPME is an established sample preparation approach that has not yet been adequately explored for food analysis in direct immersion mode due to the limitations of the available commercial coatings. The robustness and endurance of this new coating were investigated by direct immersion extractions in raw blended vegetables without any further sample preparation steps. The PDMS/DVB/PDMS coating exhibited superior features related to the capability of the external PDMS layer to protect the commercial coating, and showed improvements in terms of extraction capability and in the cleanability of the coating surface. In addition to having contributed to the recognition of the superior features of this new fiber concept before commercialization, the outcomes of this work serve to confirm advancements in the matrix compatibility of the PDMS-modified fiber, and open new prospects for the development of greener high-throughput analytical methods in food analysis using solid phase microextraction in the near future.

  19. Performance Evaluation of Fast Microfluidic Thermal Lysis of Bacteria for Diagnostic Sample Preparation

    Directory of Open Access Journals (Sweden)

    Evangelyn C. Alocilja


    Full Text Available Development of new diagnostic platforms that incorporate lab-on-a-chip technologies for portable assays is driving the need for rapid, simple, low cost methods to prepare samples for downstream processing or detection. An important component of the sample preparation process is cell lysis. In this work, a simple microfluidic thermal lysis device is used to quickly release intracellular nucleic acids and proteins without the need for additional reagents or beads used in traditional chemical or mechanical methods (e.g., chaotropic salts or bead beating. On-chip lysis is demonstrated in a multi-turn serpentine microchannel with external temperature control via an attached resistive heater. Lysis was confirmed for Escherichia coli by fluorescent viability assay, release of ATP measured with bioluminescent assay, release of DNA measured by fluorometry and qPCR, as well as bacterial culture. Results comparable to standard lysis techniques were achievable at temperatures greater than 65 °C and heating durations between 1 and 60 s.

  20. Semiautomated Sample Preparation for Protein Stability and Formulation Screening via Buffer Exchange. (United States)

    Ying, William; Levons, Jaquan K; Carney, Andrea; Gandhi, Rajesh; Vydra, Vicky; Rubin, A Erik


    A novel semiautomated buffer exchange process workflow was developed to enable efficient early protein formulation screening. An antibody fragment protein, BMSdab, was used to demonstrate the workflow. The process afforded 60% to 80% cycle time and scientist time savings and significant material efficiencies. These efficiencies ultimately facilitated execution of this stability work earlier in the drug development process, allowing this tool to inform the developability of potential candidates for development from a formulation perspective. To overcome the key technical challenges, the protein solution was buffer-exchanged by centrifuge filtration into formulations for stability screening in a 96-well plate with an ultrafiltration membrane, leveraging automated liquid handling and acoustic volume measurements to allow several cycles of exchanges. The formulations were transferred into a vacuum manifold and sterile filtered into a rack holding 96 glass vials. The vials were sealed with a capmat of individual caps and placed in stability stations. Stability of the samples prepared by this process and by the standard process was demonstrated to be comparable. This process enabled screening a number of formulations of a protein at an early pharmaceutical development stage with a short sample preparation time.

  1. Stable isotope dilution analysis of hydrologic samples by inductively coupled plasma mass spectrometry (United States)

    Garbarino, J.R.; Taylor, H.E.


    Inductively coupled plasma mass spectrometry is employed in the determination of Ni, Cu, Sr, Cd, Ba, Ti, and Pb in nonsaline, natural water samples by stable isotope dilution analysis. Hydrologic samples were directly analyzed without any unusual pretreatment. Interference effects related to overlapping isobars, formation of metal oxide and multiply charged ions, and matrix composition were identified and suitable methods of correction evaluated. A comparability study snowed that single-element isotope dilution analysis was only marginally better than sequential multielement isotope dilution analysis. Accuracy and precision of the single-element method were determined on the basis of results obtained for standard reference materials. The instrumental technique was shown to be ideally suited for programs associated with certification of standard reference materials.

  2. Aqueous two phase system based on ionic liquid for isolation of quinine from human plasma sample. (United States)

    Flieger, J; Czajkowska-Żelazko, A


    Aqueous two phase system was applied for selective extraction of quinine from human plasma. Bi-phase was constructed from ionic liquid: butyl-methyl-imidazolium chloride after addition kosmotropic salts K₃PO₄ or KH₂PO₄. Quinine was determined in plasma samples after drinking of tonic containing quinine. Determination was performed by HPLC on 5-μm Zorbax SB-CN column and eluent containing 40% acetonitrile (v/v), 20 mM phosphate buffer at pH 3 and 40 mM NaPF₆ using external standard method. The spectrophotometric detection was set λ=214 nm. Selective fluorescence detection was performed at excitation of 325 nm and emission of 375 nm. Proposed strategy provides suitable sample purification and gives extraction yields in the range of 89-106%. The determination coefficient (R(2)) has a value ≥0.997 in the range of 50-800 ng/ml quinine concentration. The limit of quantification was set at 27.9 ng/ml and the detection limit was found to be 8.4 ng/ml under fluorescence detection.

  3. Preparation of solid-state samples of a transition metal coordination compound for synchrotron radiation photoemission studies

    CERN Document Server

    Crotti, C; Celestino, T; Fontana, S


    The aim of this research was to identify a sample preparation method suitable for the study of transition metal complexes by photoemission spectroscopy with synchrotron radiation as the X-ray source, even in the case where the compound is not evaporable. Solid-phase samples of W(CO) sub 4 (dppe) [dppe=1,2-bis(diphenylphosphino)ethane] were prepared according to different methods and their synchrotron radiation XPS spectra measured. The spectra acquired from samples prepared by spin coating show core level peaks only slightly broader than the spectrum recorded from UHV evaporated samples. Moreover, for these samples the reproducibility of the binding energy values is excellent. The dependence of the spin coating technique on parameters such as solvent and solution concentration, spinning speed and support material was studied. The same preparation method also allowed the acquisition of valence band spectra, the main peaks of which were clearly resolved. The results suggest that use of the spin coating techniqu...

  4. Catecholamines in plasma from artery, cubital vein, and femoral vein in patients with cirrhosis. Significance of sampling site

    DEFF Research Database (Denmark)

    Henriksen, J H; Ring-Larsen, H; Christensen, N J


    The concentration of noradrenaline (NA) and adrenaline (A) was measured in arterial, cubital venous and femoral venous plasma in order to determine possible differences in different vascular beds in the peripheral circulation. In patients with cirrhosis, arterial plasma NA (median 2.54 nmol/l, n ...... the skin of forearm and hand). To assess circulating levels of catecholamines, the importance of arterial sampling is stressed as peripheral venous samples may also reflect local factors....

  5. Evaluation of sample preparation methods and optimization of nickel determination in vegetable tissues

    Directory of Open Access Journals (Sweden)

    Rodrigo Fernando dos Santos Salazar


    Full Text Available Nickel, although essential to plants, may be toxic to plants and animals. It is mainly assimilated by food ingestion. However, information about the average levels of elements (including Ni in edible vegetables from different regions is still scarce in Brazil. The objectives of this study were to: (a evaluate and optimize a method for preparation of vegetable tissue samples for Ni determination; (b optimize the analytical procedures for determination by Flame Atomic Absorption Spectrometry (FAAS and by Electrothermal Atomic Absorption (ETAAS in vegetable samples and (c determine the Ni concentration in vegetables consumed in the cities of Lorena and Taubaté in the Vale do Paraíba, State of São Paulo, Brazil. By means of the analytical technique for determination by ETAAS or FAAS, the results were validated by the test of analyte addition and recovery. The most viable method tested for quantification of this element was HClO4-HNO3 wet digestion. All samples but carrot tissue collected in Lorena contained Ni levels above the permitted by the Brazilian Ministry of Health. The most disturbing results, requiring more detailed studies, were the Ni concentrations measured in carrot samples from Taubaté, where levels were five times higher than permitted by Brazilian regulations.

  6. Preparation of Magnetic Hollow Molecularly Imprinted Polymers for Detection of Triazines in Food Samples. (United States)

    Wang, Aixiang; Lu, Hongzhi; Xu, Shoufang


    Novel magnetic hollow molecularly imprinted polymers (M-H-MIPs) were proposed for highly selective recognition and fast enrichment of triazines in food samples. M-H-MIPs were prepared on the basis of multi-step swelling polymerization, followed by in situ growth of magnetic Fe3O4 nanoparticles on the surface of hollow molecularly imprinted polymers (H-MIPs). Transmission electron microscopy and scanning electron microscopy confirmed the successful immobilization of Fe3O4 nanoparticles on the surface of H-MIPs. M-H-MIPs could be separated simply using an external magnet. The binding adsorption results indicated that M-H-MIPs displayed high binding capacity and fast mass transfer property and class selective property for triazines. Langmuir isotherm and pseudo-second-order kinetic models fitted the best adsorption models for M-H-MIPs. M-H-MIPs were used to analyze atrazine, simazine, propazine, and terbuthylazine in corn, wheat, and soybean samples. Satisfactory recoveries were in the range of 80.62-101.69%, and relative standard deviation was lower than 5.2%. Limits of detection from 0.16 to 0.39 μg L(-1) were obtained. When the method was applied to test positive samples that were contaminated with triazines, the results agree well with those obtained from an accredited method. Thus, the M-H-MIP-based dispersive solid-phase extraction method proved to be a convenient and practical platform for detection of triazines in food samples.

  7. Optimized sample preparation of endoscopic collected pancreatic fluid for SDS-PAGE analysis. (United States)

    Paulo, Joao A; Lee, Linda S; Wu, Bechien; Repas, Kathryn; Banks, Peter A; Conwell, Darwin L; Steen, Hanno


    The standardization of methods for human body fluid protein isolation is a critical initial step for proteomic analyses aimed to discover clinically relevant biomarkers. Several caveats have hindered pancreatic fluid proteomics, including the heterogeneity of samples and protein degradation. We aim to optimize sample handling of pancreatic fluid that has been collected using a safe and effective endoscopic collection method (endoscopic pancreatic function test). Using SDS-PAGE protein profiling, we investigate (i) precipitation techniques to maximize protein extraction, (ii) auto-digestion of pancreatic fluid following prolonged exposure to a range of temperatures, (iii) effects of multiple freeze-thaw cycles on protein stability, and (iv) the utility of protease inhibitors. Our experiments revealed that TCA precipitation resulted in the most efficient extraction of protein from pancreatic fluid of the eight methods we investigated. In addition, our data reveal that although auto-digestion of proteins is prevalent at 23 and 37 degrees C, incubation on ice significantly slows such degradation. Similarly, when the sample is maintained on ice, proteolysis is minimal during multiple freeze-thaw cycles. We have also determined the addition of protease inhibitors to be assay-dependent. Our optimized sample preparation strategy can be applied to future proteomic analyses of pancreatic fluid.

  8. Preparative divergent flow IEF without carrier ampholytes for separation of complex biological samples. (United States)

    Stastna, Miroslava; Slais, Karel


    Efficient separation method is a crucial part of the process in which components of highly complex biological sample are identified and characterized. Based on the principles of recently newly established electrophoretic method called divergent flow IEF (DF IEF), we have tested the DF IEF instrument which is able to operate without the use of background carrier ampholytes. We have verified that during separation and focusing of sample consisting of high numbers of proteins (yeast lysate and wheat flour extract), the pH gradient of preparative DF IEF can be created by autofocusing of the sample components themselves without any addition of carrier ampholytes. In DF IEF, the proteins are separated, desalted and concentrated in one step. The fractions of yeast lysate sample, collected at the DF IEF output and subjected to gel IEF, contained the zones of proteins gradually covering the pI values from 3.7 to 8.5. In our experimental arrangement, the highest number of proteins has been found in fractions with pI values around 5.3 as detected by polyacrylamide gel IEF with CBB staining. During DF IEF, the selected protein bands have been concentrated up to 16.8-fold.

  9. Sample preparation for scanning electron microscopy of plant surfaces--horses for courses. (United States)

    Pathan, A K; Bond, J; Gaskin, R E


    Plant tissues must be dehydrated for observation in most electron microscopes. Although a number of sample processing techniques have been developed for preserving plant tissues in their original form and structure, none of them are guaranteed artefact-free. The current paper reviews common scanning electron microscopy techniques and the sample preparation methods employed for visualisation of leaves under specific types of electron microscopes. Common artefacts introduced by specific techniques on different leaf types are discussed. Comparative examples are depicted from our lab using similar techniques; the pros and cons for specific techniques are discussed. New promising techniques and microscopes, which can alleviate some of the problems encountered in conventional methods of leaf sample processing and visualisation, are also discussed. It is concluded that the choice of technique for a specific leaf sample is dictated by the surface features that need to be preserved (such as trichomes, epidermal cells or wax microstructure), the resolution to be achieved, availability of the appropriate processing equipment and the technical capabilities of the available electron microscope.


    Bailly-Chouriberry, Ludovic; Baudoin, Florent; Cormant, Florence; Glavieux, Yohan; Loup, Benoit; Garcia, Patrice; Popot, Marie-Agnès; Bonnaire, Yves


    The improvement of doping control is an on-going race. Techniques to fight against doping are usually based on the direct detection of drugs or their metabolites by analytical methods such as chromatography hyphenated to mass spectrometry after ad hoc sample preparation. Nowadays, omic methods constitute an attractive development and advances have been achieved particularly by application of molecular biology tools for detection of anabolic androgenic steroids (AAS), erythropoiesis-stimulating agent (ESA) or to control human growth hormone misuses. These interesting results across different animal species have suggested that modification of gene expression offers promising new methods of improving the window of detection of banned substances by targeting their effects on blood cell gene expression. In this context, the present study describes the possibility of using a modified version of the dedicated Human IVD (in vitro Diagnostics) PAXgene® Blood RNA Kit for horse gene expression analysis in blood collected on PAXgene® tubes applied to the Horse Biological Passport. The commercial kit was only approved for human blood samples and has required an optimization of specific technical requirements for equine blood samples. Improvements and recommendations were achieved for sample collection, storage and RNA extraction procedure. Following these developments, RNA yield and quality were demonstrated to be suitable for downstream gene expression analysis by qPCR techniques.

  11. Platelet-rich plasma preparation using three devices : Implications for platelet activation and platelet growth factor release

    NARCIS (Netherlands)

    Everts, Peter A. M.; Mahoney, Christine Brown; Hoffmann, Johannes J. M. L.; Schonberger, Jacques P. A. M.; Box, Henk A. M.; Van Zundert, Andre; Knape, Johannes T. A.


    Background: In this study, three commercial systems for the preparation of platelet-rich plasma (PRP) were compared and platelet growth factors release was measured. Methods: Ten healthy volunteers donated whole blood that was fractionated by a blood cell separator, and a table-top centrifuge to pre

  12. Partially crystallized Pd nanoparticles decorated TiO2 prepared by atmospheric-pressure cold plasma and its enhanced photocatalytic performance

    Institute of Scientific and Technical Information of China (English)

    Zhijian Xu; Bin Qi; Lanbo Di; Xiuling Zhang


    TiO2 decorated with partially crystallized Pd nanoparticles (Pd/TiO2-P) was successfully prepared by atmospheric-pressure dielectric barrier discharge cold plasma. The XRD and XPS analyses proved that Pd ions were reduced to partially crystallized metallic Pd nanoparticles in Pd/TiO2-P. The XPS spectra also indicated that an enhanced metal-support interaction was formed due to the existence of partially crystallized Pd nanoparticles with lower coordination number in Pd/TiO2-P. Photocatalytic activity of Pd/TiO2-P was much higher than that of TiO2 samples decorated with well crystallized Pd nanoparticles.

  13. Preparation and analysis of dust samples for medical examinations; Praeparation und Analytik der Staubproben fuer medizinische Untersuchungen

    Energy Technology Data Exchange (ETDEWEB)

    Armbruster, L. [Deutsche Montan Technologie GmbH, Essen (Germany). Gas and Fire Div.


    For medical research within this project three respirable dust samples have been prepared and analysed. The original bulk material came from three different stratigraphic horizons, for the preparation a multiplex classifier was used. The respirable samples showed the same size distribution as the samples used in former projects. The quartz content was rather low, but within the normal variability. Pure quartz particles without surface contamination are not present in the three samples. Nickel, lead, cobalt, and arsenic are the most significant trace elements in the samples. (orig.)

  14. Preparing and measuring ultra-small radiocarbon samples with the ARTEMIS AMS facility in Saclay, France

    Energy Technology Data Exchange (ETDEWEB)

    Delque-Kolic, E., E-mail: [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France); Comby-Zerbino, C.; Ferkane, S.; Moreau, C.; Dumoulin, J.P.; Caffy, I.; Souprayen, C.; Quiles, A.; Bavay, D.; Hain, S.; Setti, V. [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France)


    The ARTEMIS facility in Saclay France measures, on average, 4500 samples a year for French organizations working in an array of fields, including environmental sciences, archeology and hydrology. In response to an increasing demand for the isolation of specific soil compounds and organic water fractions, we were motivated to evaluate our ability to reduce microgram samples using our standard graphitization lines and to measure the graphite thus obtained with our 3MV NEC Pelletron AMS. Our reduction facility consists of two fully automated graphitization lines. Each line has 12 reduction reactors with a reduction volume of 18 ml for the first line and 12 ml for the second. Under routine conditions, we determined that we could reduce the samples down to 10 {mu}g of carbon, even if the graphitization yield is consequently affected by the lower sample mass. Our results when testing different Fe/C ratios suggest that an amount of 1.5 mg of Fe powder was ideal (instead of lower amounts of catalyst) to prevent the sample from deteriorating too quickly under the Cs+ beam, and to facilitate pressing procedures. Several sets of microsamples produced from HOxI standard, international references and backgrounds were measured. When measuring {sup 14}C-free wood charcoal and HOxI samples we determined that our modern and dead blanks, due to the various preparation steps, were of 1.1 {+-} 0.8 and 0.2 {+-} 0.1 {mu}g, respectively. The results presented here were obtained for IAEA-C1, {sup 14}C-free wood, IAEA-C6, IAEA-C2 and FIRI C.

  15. Automation of sample preparation for mass cytometry barcoding in support of clinical research: protocol optimization. (United States)

    Nassar, Ala F; Wisnewski, Adam V; Raddassi, Khadir


    Analysis of multiplexed assays is highly important for clinical diagnostics and other analytical applications. Mass cytometry enables multi-dimensional, single-cell analysis of cell type and state. In mass cytometry, the rare earth metals used as reporters on antibodies allow determination of marker expression in individual cells. Barcode-based bioassays for CyTOF are able to encode and decode for different experimental conditions or samples within the same experiment, facilitating progress in producing straightforward and consistent results. Herein, an integrated protocol for automated sample preparation for barcoding used in conjunction with mass cytometry for clinical bioanalysis samples is described; we offer results of our work with barcoding protocol optimization. In addition, we present some points to be considered in order to minimize the variability of quantitative mass cytometry measurements. For example, we discuss the importance of having multiple populations during titration of the antibodies and effect of storage and shipping of labelled samples on the stability of staining for purposes of CyTOF analysis. Data quality is not affected when labelled samples are stored either frozen or at 4 °C and used within 10 days; we observed that cell loss is greater if cells are washed with deionized water prior to shipment or are shipped in lower concentration. Once the labelled samples for CyTOF are suspended in deionized water, the analysis should be performed expeditiously, preferably within the first hour. Damage can be minimized if the cells are resuspended in phosphate-buffered saline (PBS) rather than deionized water while waiting for data acquisition.

  16. Preparation and examination of monolithic in-needle extraction (MINE) device for the direct analysis of liquid samples

    Energy Technology Data Exchange (ETDEWEB)

    Pietrzyńska, Monika, E-mail:; Voelkel, Adam; Bielicka-Daszkiewicz, Katarzyna


    Graphical abstract: -- Highlights: •MINE device for isolation of analytes from water samples. •Nine polymer poly(styrene-divinylbenzene) monoliths prepared in stainless steel needles. •High efficiency of in-needle extraction systems based on monolithic materials. •New possibilities in sample preparation area. -- Abstract: Combination of extraction and chromatographic techniques opens NEW possibilities in sample preparation area. Macroporous poly(styrene-divinylbenzene) (PS-DVB) monoliths were prepared by in situ polymerization in stainless steel needles. The surface of stainless steel needle was modified earlier by the silane coupling agent. Monolithic materials located inside needles were used as the in-needle extraction device. Scanning electron microscope (SEM) images were obtained for nine monoliths. Spectra of prepared materials were also performed with the use of two techniques: Attenuated Total Reflectance (ATR) and Fourier Transform Infrared Spectroscopy (FTIR). The new monolithic in-needle extraction (MINE) devices were used in the preparation of a series of test water samples for chromatographic analysis. The extraction of phenolic compounds from water samples was carried out by pumping liquid samples through the MINE device. Obtained results indicate a high efficiency of in-needle extraction systems based on monolithic materials. Breakthrough volume and the sorption efficiency of prepared monolithic in-needle extraction devices were determined experimentally. The achieved recovery was close to 90%, and determined LOQ values varied between 0.4 and 6 μg.

  17. Quantitative analysis of Tenecteplase in rat plasma samples using LC-MS/MS as an alternative for ELISA. (United States)

    Buscher, B A P; Gerritsen, H; van Schöll, I; Cnubben, N H P; Brüll, L P


    An LC-MS/MS method has been developed for the quantitative determination of a protein drug (Tenecteplase; M(W) 58,777 Da) in rat plasma. The protein was digested with trypsin without prior clean-up of the plasma sample, without the use of a label nor internal standard. A limited validation was performed to assess the linearity, the sensitivity and the specificity of the method. In addition, the developed method was applied to the quantitative analysis of Tenecteplase in rat plasma samples originating from a single-dose study in rats.

  18. Quantitative analysis of plasma proteins in whole blood-derived fresh frozen plasma prepared with three pathogen reduction technologies. (United States)

    Larrea, Luis; Ortiz-de-Salazar, María-Isabel; Martínez, Patricia; Roig, Roberto


    Several plasma pathogen reduction technologies (PRT) are currently available. We evaluated three plasma PRT processes: Cerus Amotosalen (AM), Terumo BCT riboflavin (RB) and Macopharma methylene blue (MB). RB treatment resulted in the shortest overall processing time and in the smallest volume loss (1%) and MB treatment in the largest volume loss (8%). MB treatment retained the highest concentrations of factors II, VII, X, IX, Protein C, and Antithrombin and the AM products of factor V and XI. Each PRT process evaluated offered distinct advantages such as procedural simplicity and volume retention (RB) and overall plasma protein retention (MB).

  19. Comparison of sample preparation methods for reliable plutonium and neptunium urinalysis using automatic extraction chromatography. (United States)

    Qiao, Jixin; Xu, Yihong; Hou, Xiaolin; Miró, Manuel


    This paper describes improvement and comparison of analytical methods for simultaneous determination of trace-level plutonium and neptunium in urine samples by inductively coupled plasma mass spectrometry (ICP-MS). Four sample pre-concentration techniques, including calcium phosphate, iron hydroxide and manganese dioxide co-precipitation and evaporation were compared and the applicability of different techniques was discussed in order to evaluate and establish the optimal method for in vivo radioassay program. The analytical results indicate that the various sample pre-concentration approaches afford dissimilar method performances and care should be taken for specific experimental parameters for improving chemical yields. The best analytical performances in terms of turnaround time (6h) and chemical yields for plutonium (88.7 ± 11.6%) and neptunium (94.2 ± 2.0%) were achieved by manganese dioxide co-precipitation. The need of drying ashing (≥ 7h) for calcium phosphate co-precipitation and long-term aging (5d) for iron hydroxide co-precipitation, respectively, rendered time-consuming analytical protocols. Despite the fact that evaporation is also somewhat time-consuming (1.5d), it endows urinalysis methods with better reliability and repeatability compared with co-precipitation techniques. In view of the applicability of different pre-concentration techniques proposed previously in the literature, the main challenge behind relevant method development is pointed to be the release of plutonium and neptunium associated with organic compounds in real urine assays. In this work, different protocols for decomposing organic matter in urine were investigated, of which potassium persulfate (K2S2O8) treatment provided the highest chemical yield of neptunium in the iron hydroxide co-precipitation step, yet, the occurrence of sulfur compounds in the processed sample deteriorated the analytical performance of the ensuing extraction chromatographic separation with chemical

  20. Validated microbiological and HPLC methods for the determination of moxifloxacin in pharmaceutical preparations and human plasma

    Directory of Open Access Journals (Sweden)

    Ahmed A. Abdelaziz


    Full Text Available The article presents a comparison between microbiological and high performance liquid chromatographic (HPLC assays for quantification of moxifloxacin in tablets, ophthalmic solutions and human plasma. The microbiological method employed a cylinder-plate agar diffusion assay using a strain of Esherichia coli ATCC 25922 as the test organism and phosphate buffer (pH8 as the diluent. The calibration curves were linear (R²> 0.98 over a concentration range of 0.125 to 16 µgml-1. The within day and between days precisions were 0.999 over the range of 0.125 to 16 µg ml-1. The within day and between days precisions were < 4.07% and < 5.09% respectively. Recovery values were between 97.7 and 107.6%. Similar potencies were obtained after the analysis of moxifloxacin tablets and ophthalmic solutions by both methods. Also pharmacokinetic parameters were calculated after the analysis of plasma samples of six male healthhy volunteers by both validated methods.

  1. Properties of sintered glass-ceramics prepared from plasma vitrified air pollution control residues. (United States)

    Roether, J A; Daniel, D J; Rani, D Amutha; Deegan, D E; Cheeseman, C R; Boccaccini, A R


    Air pollution control (APC) residues, obtained from a major UK energy from waste (EfW) plant, processing municipal solid waste, have been blended with silica and alumina and melted using DC plasma arc technology. The glass produced was crushed, milled, uni-axially pressed and sintered at temperatures between 750 and 1150 degrees C, and the glass-ceramics formed were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Mechanical properties assessed included Vickers's hardness, flexural strength, Young's modulus and thermal shock resistance. The optimum sintering temperature was found to be 950 degrees C. This produced a glass-ceramic with high density (approximately 2.58 g/cm(3)), minimum water absorption (approximately 2%) and relatively high mechanical strength (approximately 81+/-4 MPa). Thermal shock testing showed that 950 degrees C sintered samples could withstand a 700 degrees C quench in water without micro-cracking. The research demonstrates that glass-ceramics can be readily formed from DC plasma treated APC residues and that these have comparable properties to marble and porcelain. This novel approach represents a technically and commercially viable treatment option for APC residues that allow the beneficial reuse of this problematic waste.

  2. Studies of lithium deposition and D retention on tungsten samples exposed to Li-seeded plasmas in PISCES-A (United States)

    Tabarés, F. L.; Alegre, D.; Baldwin, M.; Nishijima, D.; Simmonds, M.; Doerner, R.; Alves, E.; Mateus, R.


    The interaction between lithium-seeded deuterium plasmas and tungsten targets has been studied in the PISCES-A divertor plasma simulator. Tungsten samples, of ITER-grade, with a diameter of 25 and 2 mm thick, were held at temperatures ranging from 403 to 873 K and exposed to Li/D plasmas under different plasma conditions and fixed total fluences of 5 ×1025 m‑2, with typical particle flux values of (1–5) × 1022 m‑2 s‑1. The deuterium and lithium contents of the samples after irradiation were analyzed by thermal desorption spectroscopy and nuclear reaction analysis (NRA). No lithium deposition was found within the sensitivity range of NRA, except for the cold (403 K) sample on which a layer with Li atomic density below 2 × 1022 m‑2 was detected. Deuterium retention values in the range of 1018 m‑2 were measured, even for the Li deposition conditions.

  3. Microwave processing for sample preparation to evaluate mitochondrial ultrastructural damage in hemorrhagic shock. (United States)

    Josephsen, Gary D; Josephsen, Kelly A; Beilman, Greg J; Taylor, Jodie H; Muiler, Kristine E


    This is a report of the adaptation of microwave processing in the preparation of liver biopsies for transmission electron microscopy (TEM) to examine ultrastructural damage of mitochondria in the setting of metabolic stress. Hemorrhagic shock was induced in pigs via 35% total blood volume bleed and a 90-min period of shock followed by resuscitation. Hepatic biopsies were collected before shock and after resuscitation. Following collection, biopsies were processed for TEM by a rapid method involving microwave irradiation (Giberson, 2001). Samples pre- and postshock of each of two animals were viewed and scored using the mitochondrial ultrastructure scoring system (Crouser et al., 2002), a system used to quantify the severity of ultrastructural damage during shock. Results showed evidence of increased ultrastructural damage in the postshock samples, which scored 4.00 and 3.42, versus their preshock controls, which scored 1.18 and 1.27. The results of this analysis were similar to those obtained in another model of shock (Crouser et al., 2002). However, the amount of time used to process the samples was significantly shortened with methods involving microwave irradiation.

  4. Modular approach to customise sample preparation procedures for viral metagenomics: a reproducible protocol for virome analysis. (United States)

    Conceição-Neto, Nádia; Zeller, Mark; Lefrère, Hanne; De Bruyn, Pieter; Beller, Leen; Deboutte, Ward; Yinda, Claude Kwe; Lavigne, Rob; Maes, Piet; Van Ranst, Marc; Heylen, Elisabeth; Matthijnssens, Jelle


    A major limitation for better understanding the role of the human gut virome in health and disease is the lack of validated methods that allow high throughput virome analysis. To overcome this, we evaluated the quantitative effect of homogenisation, centrifugation, filtration, chloroform treatment and random amplification on a mock-virome (containing nine highly diverse viruses) and a bacterial mock-community (containing four faecal bacterial species) using quantitative PCR and next-generation sequencing. This resulted in an optimised protocol that was able to recover all viruses present in the mock-virome and strongly alters the ratio of viral versus bacterial and 16S rRNA genetic material in favour of viruses (from 43.2% to 96.7% viral reads and from 47.6% to 0.19% bacterial reads). Furthermore, our study indicated that most of the currently used virome protocols, using small filter pores and/or stringent centrifugation conditions may have largely overlooked large viruses present in viromes. We propose NetoVIR (Novel enrichment technique of VIRomes), which allows for a fast, reproducible and high throughput sample preparation for viral metagenomics studies, introducing minimal bias. This procedure is optimised mainly for faecal samples, but with appropriate concentration steps can also be used for other sample types with lower initial viral loads.

  5. Investigation of microstructure and irradiation behavior of W–Nb/Ti composites prepared by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Jing-Bo [School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China); Luo, Lai-Ma, E-mail: [School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China); National–Local Joint Engineering Research Centre of Nonferrous Metals and Processing Technology, Hefei 230009 (China); Zhao, Mei-Ling [School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China); Xu, Qiu [Research Reactor Institute, Kyoto University, Osaka-Fu 590-0494 (Japan); Zan, Xiang [School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China); National–Local Joint Engineering Research Centre of Nonferrous Metals and Processing Technology, Hefei 230009 (China); Wu, Yu-Cheng, E-mail: [School of Materials Science and Engineering, Hefei University of Technology, Hefei 230009 (China); National–Local Joint Engineering Research Centre of Nonferrous Metals and Processing Technology, Hefei 230009 (China)


    W–Nb/Ti composites were prepared by machine milling and spark plasma sintering. Field–emission scanning electron microscopy, high–resolution transmission electron microscopy, and X-ray diffraction analyses were used to characterize the samples. Thermal desorption spectroscopy (TDS) was used to measure the deuterium retention after only deuterium irradiation. The deuterium retention in W–4wt%Ti–wt1%Nb was lower than that in pure W (D{sub 2}{sup +} flux ∼10{sup 22} ions/(m{sup 2} s), ion energy ∼5 keV), Nb and Ti will improve the deuterium irradiation resistance of tungsten composite. In addition, transgranular and intergranular fractures were observed on the surface of the W–4 wt% Ti–1 wt% Nb composite. A Ti{sub (X)}W{sub (1−X)} solid solution was formed during sintering. The maximum tensile strength (410.53 MPa) was detected in the W–4wt%Ti–1wt%Nb composite at 600 °C.

  6. Thermal analysis of the influence of the support in the superficial treatment by plasma of cylindrical samples

    Energy Technology Data Exchange (ETDEWEB)

    Belisio, A.S.; Lima, J.A.; Alves Junior, C. [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil). Programa de Pos-Graduacao em Engenharia Mecanica]. E-mails:;;


    Different of the conventional processes of heating, that is, transport, convection, and radiation, heat transfer in heating process by plasma also occur also by collisions of particles, in other words, through the transfer heat motion ions for the surface of the sample, the kinetic energy, and potential those particles, as well as the enthalpy of the chemical reactions involved in the surface. In thermal plasmas, that transfer can to be simplified initially through general energy balance between plasma and samples. However, existent models of temperature distribution are in its majority unidimensional and it do not analyze, mainly, support influence on sample in the heating process by r plasma. In that way, with the mark of analyzing the temperature distribution in the samples submitted to polarization voltage of 706 V, 744 V and 790 V, as well as process heating support influence analysis those samples, the present work developed a code computational for a transient (2D-t) two-dimensional model, destined to the simulation of the heat transfer during heating phases and cooling in superficial process of treatment by plasma in cylindrical samples of copper, being considered the configuration of hollow cathode and the presence of a support. The model computational serves as a tool in the predict of the final properties of treated samples, well as in the specification of the parameters of the heating processes by plasma. In the developed model was considered that the physical samples properties were variable, functions of the temperature field. The results obtained through simulation are leaning and validated in experimental and theoretical data available in the literature, as well as, in information of tests accomplished in Lab Plasma/ UFRN. (author)

  7. Preparation of Ag-containing diamond-like carbon films on the interior surface of tubes by a combined method of plasma source ion implantation and DC sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Hatada, R., E-mail: [Technische Universität Darmstadt, Department of Materials Science, 64287 Darmstadt (Germany); Flege, S.; Bobrich, A.; Ensinger, W.; Dietz, C. [Technische Universität Darmstadt, Department of Materials Science, 64287 Darmstadt (Germany); Baba, K. [Industrial Technology Center of Nagasaki, Applied Technology Division, Omura, Nagasaki 856-0026 (Japan); Sawase, T.; Watamoto, T. [Nagasaki University, Department of Applied Prosthodontics, Nagasaki 852-8523 (Japan); Matsutani, T. [Technische Universität Darmstadt, Department of Materials Science, 64287 Darmstadt (Germany); Kinki University, Department of Electric and Electronic Engineering, Higashi-osaka 577-2332 (Japan)


    Highlights: • Deposition of Ag-containing diamond-like carbon films inside of tubes. • Combination of plasma source ion implantation and DC sputtering. • Antibacterial effect against S. aureus bacteria. - Abstract: Adhesive diamond-like carbon (DLC) films can be prepared by plasma source ion implantation (PSII), which is also suitable for the treatment of the inner surface of a tube. Incorporation of a metal into the DLC film provides a possibility to change the characteristics of the DLC film. One source for the metal is DC sputtering. In this study PSII and DC sputtering were combined to prepare DLC films containing low concentrations of Ag on the interior surfaces of stainless steel tubes. A DLC film was deposited using a C{sub 2}H{sub 4} plasma with the help of an auxiliary electrode inside of the tube. This electrode was then used as a target for the DC sputtering. A mixture of the gases Ar and C{sub 2}H{sub 4} was used to sputter the silver. By changing the gas flow ratios and process time, the resulting Ag content of the films could be varied. Sample characterizations were performed by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, atomic force microscopy and Raman spectroscopy. Additionally, a ball-on-disk test was performed to investigate the tribological properties of the films. The antibacterial activity was determined using Staphylococcus aureus bacteria.

  8. Effects of sample preparation on the optical properties of breast tissue (United States)

    Marks, Fay A.


    The optical properties of biological tissue should be determined in vivo whenever possible. However, for those instances when in vivo studies are impractical, too expensive or inappropriate, and when blood flow is not an issue, the ability to perform in vitro studies then becomes invaluable. Optical absorption spectroscopy shows that it may be possible to obtain meaningful information about the optical properties of human breast tissue from in vitro samples if strict preparation and measuring protocols are used. That a strict protocol for storing and handling tissue is critical can be seen from our observations of changes in the optical absorption spectra that occur in response to formalin fixation, the passage of time, application of stains and dyes, and storage in growth medium of the excised tissue. In vivo optical absorption spectroscopy measurements have been made on human breast cancer xenografts and compared with in vitro measurements on breast biopsies prepared according to precise collection and treatment protocols. There is a 'window of opportunity' before time dependent changes in the UV optical absorption spectra of the excised tissue specimens occur. This time window of opportunity widens at longer wavelengths with the least changes occurring in the optical spectra in the NIR.

  9. Lights Will Guide You : Sample Preparation and Applications for Integrated Laser and Electron Microscopy (United States)

    Karreman, M. A.


    Correlative microscopy is the combined use of two different forms of microscopy in the study of a specimen, allowing for the exploitation of the advantages of both imaging tools. The integrated Laser and Electron Microscope (iLEM), developed at Utrecht University, combines a fluorescence microscope (FM) and a transmission electron microscope (TEM) in a single set-up. The region of interest in the specimen is labeled or tagged with a fluorescent probe and can easily be identified within a large field of view with the FM. Next, this same area is retraced in the TEM and can be studied at high resolution. The iLEM demands samples that can be imaged with both FM and TEM. Biological specimen, typically composed of light elements, generate low image contrast in the TEM. Therefore, these samples are often ‘contrasted’ with heavy metal stains. FM, on the other hand, images fluorescent samples. Sample preparation for correlative microscopy, and iLEM in particular, is complicated by the fact that the heavy metals stains employed for TEM quench the fluorescent signal of the probe that is imaged with FM. The first part of this thesis outlines preparation procedures for biological material yielding specimen that can be imaged with the iLEM. Here, approaches for the contrasting of thin sections of cells and tissue are introduced that do not affect the fluorescence signal of the probe that marks the region of interest. Furthermore, two novel procedures, VIS2FIXH and VIS2FIX­FS are described that allow for the chemical fixation of thin sections of cryo-immobilized material. These procedures greatly expedite the sample preparation process, and open up novel possibilities for the immuno-labeling of difficult antigens, eg. proteins and lipids that are challenging to preserve. The second part of this thesis describes applications of iLEM in research in the field of life and material science. The iLEM was employed in the study of UVC induced apoptosis (programmed cell death) of

  10. Sample Preparation for Headspace GC Analysis of Residual Solvents in Hyaluronic Acid Derivative Fiber

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hoon Joo; Kim, Dong Min; Yang, Jeong Soo [LG life Sciences, Ltd./R and D Park, Daejeon (Korea, Republic of); Kim, Chan Wha [Korea University, Seoul (Korea, Republic of)


    The aim of this study is to develop efficient sample preparation method for HS-GC analysis of residual solvents in HA derivative fiber. Compared to direct extraction of residual solvents from HA derivative fiber, the extraction through the hydrolysis of HA derivative fiber by HAse gave more complete and higher reproducible quantification of residual solvent. To validate HS-GC analysis method of residual solvents, specificity, limits of detection and quantification, linearity, accuracy and precision are investigated in the study. HA derivative fiber was hydrolyzed using HAse for headspace gas chromatographic analysis of residual solvents of ethanol, acetone and isopropanol in HA derivative fiber. This study showed that the developed method had specificity, linearity, accuracy and precision. In addition, it demonstrated that HS-GC coupled with matrix-breaking method such as hydrolysis was available for the determination of residual solvents in a matrix like HA derivative fiber.

  11. Applied Study on Magnetic Nanometer Beads in Preparation of Genechip Samples

    Institute of Scientific and Technical Information of China (English)

    陈慧; 高华方; 谢欣; 马雪梅; 杨渝珍


    Summary: A protocol for enrichment and adsorption of karyocyte from whole blood by using magnetic nanometer beads as solid-phase absorbents was presented. The PCR amplification could be accomplished by using the nanobeads with karyocyte as template directly and the PCR products were applied on an oligonucleotide array to do gene typing. The HLA-A PCR amplification system and a small HLA-A oligonucleotide microarray were applied as the platform and an experiment protocol of separating karyocyte from whole blood using the magnetic nanometer beads (Fe2O3) were set up.The experimental conditions were also discussed. It showed that pH level of PBS eluent, Taq enzyme quantity and fragment length of products could influent the amplification results, and the magnetic nano-beads could succeed in sample preparation in microarray to provide a promising way in automatic detection and lab-on-a-chip.

  12. NGSI FY15 Final Report. Innovative Sample Preparation for in-Field Uranium Isotopic Determinations

    Energy Technology Data Exchange (ETDEWEB)

    Yoshida, Thomas M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Meyers, Lisa [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)


    Our FY14 Final Report included an introduction to the project, background, literature search of uranium dissolution methods, assessment of commercial off the shelf (COTS) automated sample preparation systems, as well as data and results for dissolution of bulk quantities of uranium oxides, and dissolution of uranium oxides from swipe filter materials using ammonium bifluoride (ABF). Also, discussed were reaction studies of solid ABF with uranium oxide that provided a basis for determining the ABF/uranium oxide dissolution mechanism. This report details the final experiments for optimizing dissolution of U3O8 and UO2 using ABF and steps leading to development of a Standard Operating Procedure (SOP) for dissolution of uranium oxides on swipe filters.

  13. Agarose- and alginate-based biopolymers for sample preparation: Excellent green extraction tools for this century. (United States)

    Sanagi, Mohd Marsin; Loh, Saw Hong; Wan Ibrahim, Wan Nazihah; Pourmand, Neda; Salisu, Ahmed; Wan Ibrahim, Wan Aini; Ali, Imran


    Recently, there has been considerable interest in the use of miniaturized sample preparation techniques before the chromatographic monitoring of the analytes in unknown complex compositions. The use of biopolymer-based sorbents in solid-phase microextraction techniques has achieved a good reputation. A great variety of polysaccharides can be extracted from marine plants or microorganisms. Seaweeds are the major sources of polysaccharides such as alginate, agar, agarose, as well as carrageenans. Agarose and alginate (green biopolymers) have been manipulated for different microextraction approaches. The present review is focused on the classification of biopolymer and their applications in multidisciplinary research. Besides, efforts have been made to discuss the state-of-the-art of the new microextraction techniques that utilize commercial biopolymer interfaces such as agarose in liquid-phase microextraction and solid-phase microextraction.


    Directory of Open Access Journals (Sweden)

    M. I. Egorova


    Full Text Available Summary. Molasses is characterized as sugar production by-product from primary or secondary sacchariferous raw materials. The features of the appearance, the chemical composition, molasses and exit directions of its use, depending on the type of production, in which it is formed. The value of molasses is demonstrated according to its total composition as well as its use directions. Statistics on beet molasses amounts in Russia is presented. Described consumer market molasses in Russia and abroad with its exports. Shown regulations contain requirements for the quality and safety of molasses, including sulfur dioxide. The data on sulfur allergenic properties are presented. Showing source of the sulfur dioxide in the residual molasses number of processing aids and the impact of its level in the value of raw molasses for use in biotechnological processes and fodder production. The necessity to develop methodology for determining the sulfur dioxide content in the molasses to control its security. The iodometric method, which is used in practice for determination of sulphur dioxide in foods are characterized. Differences molasses and sugar as objects of iodometric determination of sulfur dioxide, which leads to the inability to ascertain the equivalence point. The variants eliminate interfering background of dark-colored foods common in analytical chemistry. Advantages and disadvantages of the background masking and stripping the determination of sulfur dioxide in the darkcolored products. It was characterized by clarifying sugar solutions in optical control methods. The hypothesis about preferability of its use in sample molasses preparation for equivalence point fixation in iodometric titration is suggested. The tasks of experimental research for the development of sample preparation algorithm molasses in determining the content of sulphurous acid.


    Directory of Open Access Journals (Sweden)

    D. I. Samal


    Full Text Available The algorithm of preparation and sampling for training of the multiclass qualifier of support vector machines (SVM is provided. The described approach based on the modeling of possible changes of the face features of recognized person. Additional features like perspectives of shooting, conditions of lighting, tilt angles were introduced to get improved identification results. These synthetic generated changes have some impact on the classifier learning expanding the range of possible variations of the initial image. The classifier learned with such extended example is ready to recognize unknown objects better. The age, emotional looks, turns of the head, various conditions of lighting, noise, and also some combinations of the listed parameters are chosen as the key considered parameters for modeling. The third-party software ‘FaceGen’ allowing to model up to 150 parameters and available in a demoversion for free downloading is used for 3D-modeling.The SVM classifier was chosen to test the impact of the introduced modifications of training sample. The preparation and preliminary processing of images contains the following constituents like detection and localization of area of the person on the image, assessment of an angle of rotation and an inclination, extension of the range of brightness of pixels and an equalization of the histogram to smooth the brightness and contrast characteristics of the processed images, scaling of the localized and processed area of the person, creation of a vector of features of the scaled and processed image of the person by a Principal component analysis (algorithm NIPALS, training of the multiclass SVM-classifier.The provided algorithm of expansion of the training selection is oriented to be used in practice and allows to expand using 3D-models the processed range of 2D – photographs of persons that positively affects results of identification in system of face recognition. This approach allows to compensate

  16. Surface modification of silicon-containing fluorocarbon films prepared by plasma-enhanced chemical vapor deposition (United States)

    Jin, Yoonyoung; Desta, Yohannes; Goettert, Jost; Lee, G. S.; Ajmera, P. K.


    Surface modification of silicon-containing fluorocarbon (SiCF) films achieved by wet chemical treatments and through x-ray irradiation is examined. The SiCF films were prepared by plasma-enhanced chemical vapor deposition, using gas precursors of tetrafluoromethane and disilane. As-deposited SiCF film composition was analyzed by x-ray photoelectron spectroscopy. Surface modification of SiCF films utilizing n-lithiodiaminoethane wet chemical treatment is discussed. Sessile water-drop contact angle changed from 95°+/-2° before treatment to 32°+/-2° after treatment, indicating a change in the film surface characteristics from hydrophobic to hydrophilic. For x-ray irradiation on the SiCF film with a dose of 27.4 kJ/cm3, the contact angle of the sessile water drop changed from 95°+/-2° before radiation to 39°+/-3° after x-ray exposure. The effect of x-ray exposure on chemical bond structure of SiCF films is studied using Fourier transform infrared measurements. Electroless Cu deposition was performed to test the applicability of the surface modified films. The x-ray irradiation method offers a unique advantage in making possible surface modification in a localized area of high-aspect-ratio microstructures. Fabrication of a Ti-membrane x-ray mask is introduced here for selective surface modification using x-ray irradiation.

  17. Preparation of carbon nanoparticles by plasma arc discharge under fluidized dynamic equilibrium (United States)

    Wang, F.; Sun, D. L.; Hong, R. Y.; Kumar, M. R.


    Continuous preparation of carbon nanoparticles by dielectric barrier discharge (DBD)-induced non-thermal plasma arc discharge with large spacing in a modified fluidized bed is presented. Discharge arc is generated via the inducement of DBD which provides conductive media in order to realize a large spacing arc discharge. Three kinds of flow conditions defined as full circulation, fluidized dynamic equilibrium, and full collection are determined by the relationship of critical fluidized velocity and the real gas velocity after some modification of the fluidized bed. Movement model of carbon nanoparticles has been proposed to illustrate the flow conditions. A visualized and comprehensive refinement of aggregating processes has been exhibited and proved by high-resolution transmission electron microscopy. Simplified equivalent electrical conductive model of the arc discharge system is successful to generally and perspicuously figure out the discharge process which is impeded by the generated carbon nanoparticles. Effects of flow conditions and flow ratio of carrier gas/carbon source on morphology and yield of nanoparticles have been analyzed by morphology observation and yield calculation along with modeling the process.

  18. Characterization of Ni ferrites powders prepared by plasma arc discharge process (United States)

    Safari, A.; Gheisari, Kh.; Farbod, M.


    The aim of this work was to synthesize a single-phase spinel structure from a mixture of zinc, iron and nickel powders by plasma arc discharge method. A mixture of zinc, iron and nickel powders with the appropriate molar ratio was prepared and formed into a cylindrical shape. The synthesis process was performed in air, oxygen and argon atmospheres with the applied arc current of 400 A and pressure of 1 atm. After establishing an arc between the electrodes, the produced powders were collected and their structure and magnetic properties were examined by XRD and VSM, respectively. ZnO as an impurity was appeared in the as-produced powders owing to the high reactivity of zinc atoms, preventing the formation of Ni-Zn ferrite. A pure spinel structure with the highest saturation magnetization (43.8 emu/g) was observed as zinc powders removed completely from the initial mixture. Morphological evaluations using field emission scanning electron microscopy showed that the mean size of fabricated nanoparticles was in the range 100-200 nm and was dependent on the production conditions.

  19. Advanced sample preparation for the molecular quantification of Staphylococcus aureus in artificially and naturally contaminated milk. (United States)

    Aprodu, Iuliana; Walcher, Georg; Schelin, Jenny; Hein, Ingeborg; Norling, Börje; Rådström, Peter; Nicolau, Anca; Wagner, Martin


    Sample treatment is an essential element when using real-time PCR for quantification of pathogens directly on food samples. This study comparatively evaluated three different principles of sample treatment, i.e. immunomagnetic separation based on phage-derived cell wall binding molecules, matrix solubilization and flotation, in order to establish their suitability for quantifying low numbers of Staphylococcus aureus in milk. All three procedures succeeded to remove S. aureus from the milk matrix, either raw or pasteurized, and, as a result of the concentration of the target cells, minimized the effect of milk associated PCR inhibitors. Sample preparation based on immunomagnetic separation albeit of being user friendly, specific and rapid, failed to allow quantification of low and medium numbers (<10(4)CFU) of S. aureus. In a mastitic milk model cell wall binding domain (CBD)-based target cell extraction revealed results most closely matching those derived from culture-based quantification. Both matrix lysis and flotation allowed quantification of S. aureus at a level of 1-10 cells per ml. Both methods resulted in higher numbers of bacterial cell equivalents (bce) than plating could reveal. Since both methods harvest cells that have been subjected to either mechanical and chemical stresses before quantification, we concluded that the higher bce numbers resulted from a disaggregation of S. aureus clusters initially present in the inoculum. Conclusively, since likely each S. aureus cell of a toxigenic strain contributes to enterotoxin production, molecular quantification could provide an even more realistic impact assessment in outbreak investigations than plating does.

  20. Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples (United States)

    Yang, Bin; Smith, A. M.; Long, S.


    We present construction details and test results for two second-generation laser-heated microfurnaces (LHF-II) used to prepare graphite samples for Accelerator Mass Spectrometry (AMS) at ANSTO. Based on systematic studies aimed at optimising the performance of our prototype laser-heated microfurnace (LHF-I) (Smith et al., 2007 [1]; Smith et al., 2010 [2,3]; Yang et al., 2014 [4]), we have designed the LHF-II to have the following features: (i) it has a small reactor volume of 0.25 mL allowing us to completely graphitise carbon dioxide samples containing as little as 2 μg of C, (ii) it can operate over a large pressure range (0-3 bar) and so has the capacity to graphitise CO2 samples containing up to 100 μg of C; (iii) it is compact, with three valves integrated into the microfurnace body, (iv) it is compatible with our new miniaturised conventional graphitisation furnaces (MCF), also designed for small samples, and shares a common vacuum system. Early tests have shown that the extraneous carbon added during graphitisation in each LHF-II is of the order of 0.05 μg, assuming 100 pMC activity, similar to that of the prototype unit. We use a 'budget' fibre packaged array for the diode laser with custom built focusing optics. The use of a new infrared (IR) thermometer with a short focal length has allowed us to decrease the height of the light-proof safety enclosure. These innovations have produced a cheaper and more compact device. As with the LHF-I, feedback control of the catalyst temperature and logging of the reaction parameters is managed by a LabVIEW interface.

  1. Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Bin; Smith, A.M.; Long, S.


    We present construction details and test results for two second-generation laser-heated microfurnaces (LHF-II) used to prepare graphite samples for Accelerator Mass Spectrometry (AMS) at ANSTO. Based on systematic studies aimed at optimising the performance of our prototype laser-heated microfurnace (LHF-I) (Smith et al., 2007 [1]; Smith et al., 2010 [2,3]; Yang et al., 2014 [4]), we have designed the LHF-II to have the following features: (i) it has a small reactor volume of 0.25 mL allowing us to completely graphitise carbon dioxide samples containing as little as 2 μg of C, (ii) it can operate over a large pressure range (0–3 bar) and so has the capacity to graphitise CO{sub 2} samples containing up to 100 μg of C; (iii) it is compact, with three valves integrated into the microfurnace body, (iv) it is compatible with our new miniaturised conventional graphitisation furnaces (MCF), also designed for small samples, and shares a common vacuum system. Early tests have shown that the extraneous carbon added during graphitisation in each LHF-II is of the order of 0.05 μg, assuming 100 pMC activity, similar to that of the prototype unit. We use a ‘budget’ fibre packaged array for the diode laser with custom built focusing optics. The use of a new infrared (IR) thermometer with a short focal length has allowed us to decrease the height of the light-proof safety enclosure. These innovations have produced a cheaper and more compact device. As with the LHF-I, feedback control of the catalyst temperature and logging of the reaction parameters is managed by a LabVIEW interface.

  2. A Movable Mass Spectroscopy Sampling Apparatus for Measuring Spatial Distribution of Neutral Radicals in Silane Plasma

    Institute of Scientific and Technical Information of China (English)

    WANG Zhao-Kui; LIN Kui-Xun; LIN Xuan-Ying; QIU Gui-Ming; ZHU Zu-Song


    @@ A movable mass spectroscopy gas sampling apparatus has been established and a straight-line fit ofsilane depletion fraction f is proposed.The spatial density distributions of SiHn (n = 0-3) radicals in silane radio frequency glow discharge have been measured by a mass spectrometer.The experimental results demonstrate that the densities of the neutral radicals have the peak value near the middle position of electrodes, and the densities of SiH2 and SiHs are higher than those of Si and SiH in silane plasma.This reveals that SiH2 and SiH3 may be the primary precursors in forming the a-Si:H film.

  3. Glow Discharge Plasma-Assisted Preparation of Nickel-Based Catalyst for Carbon Dioxide Reforming of Methane

    Institute of Scientific and Technical Information of China (English)

    Fang Guo; Wei Chu; Jun-qiang Xu; Lin Zhong


    A plasma-assisted method was employed to prepare Ni/γ-Al2O3 catalyst for carbon dioxide reforming of methane reaction. The novel catalyst possessed higher activity and better coke-suppression performance than those of the conventional calcination catalyst. To achieve the same CH4 conversion, the conventional catalyst needed higher reaction temperature, about 50 ℃ higher than that of the N2 plasma-treated catalyst.After the evaluation test, the deactivation rate of the novel catalyst was 1.7%, compared with 15.2% for the conventional catalyst. Different from the characterization results of the calcined catalyst, a smaller average pore diameter and a higher specific surface area were obtained for the plasma-treated catalyst.The variations of the reduction peak temperatures and areas indicated that the catalyst reducibility was promoted by plasma assistance. The dispersion of nickel was also remarkably improved, which was helpful for controlling the ensemble size of metal atoms on the catalyst surface. The modification effect of plasmaassisted preparation on the surface property of alumina supported catalyst was speculated to account for the concentration increase of absorbed CO2. An enhancement of CO2 adsorption was propitious to the inhibition of carbon formation. The coke amount deposited on plasma treated catalyst was much smaller than that on the conventional catalyst.

  4. Optimization of a miniaturized DBD plasma chip for mercury detection in water samples. (United States)

    Abdul-Majeed, Wameath S; Parada, Jaime H Lozano; Zimmerman, William B


    In this work, an optimization study was conducted to investigate the performance of a custom-designed miniaturized dielectric barrier discharge (DBD) microplasma chip to be utilized as a radiation source for mercury determination in water samples. The experimental work was implemented by using experimental design, and the results were assessed by applying statistical techniques. The proposed DBD chip was designed and fabricated in a simple way by using a few microscope glass slides aligned together and held by a Perspex chip holder, which proved useful for miniaturization purposes. Argon gas at 75-180 mL/min was used in the experiments as a discharge gas, while AC power in the range 75-175 W at 38 kHz was supplied to the load from a custom-made power source. A UV-visible spectrometer was used, and the spectroscopic parameters were optimized thoroughly and applied in the later analysis. Plasma characteristics were determined theoretically by analysing the recorded spectroscopic data. The estimated electron temperature (T(e) = 0.849 eV) was found to be higher than the excitation temperature (T(exc) = 0.55 eV) and the rotational temperature (T(rot) = 0.064 eV), which indicates non-thermal plasma is generated in the proposed chip. Mercury cold vapour generation experiments were conducted according to experimental plan by examining four parameters (HCl and SnCl(2) concentrations, argon flow rate, and the applied power) and considering the recorded intensity for the mercury line (253.65 nm) as the objective function. Furthermore, an optimization technique and statistical approaches were applied to investigate the individual and interaction effects of the tested parameters on the system performance. The calculated analytical figures of merit (LOD = 2.8 μg/L and RSD = 3.5%) indicates a reasonable precision system to be adopted as a basis for a miniaturized portable device for mercury detection in water samples.

  5. Influence of sample temperature on the expansion dynamics and the optical emission of laser-induced plasma

    Energy Technology Data Exchange (ETDEWEB)

    Eschlböck-Fuchs, S.; Haslinger, M.J.; Hinterreiter, A.; Kolmhofer, P.; Huber, N. [Christian Doppler Laboratory for Laser-Assisted Diagnostics, Institute of Applied Physics, Johannes Kepler University Linz, A-4040 Linz (Austria); Rössler, R. [voestalpine Stahl GmbH, A-4031 Linz (Austria); Heitz, J. [Christian Doppler Laboratory for Laser-Assisted Diagnostics, Institute of Applied Physics, Johannes Kepler University Linz, A-4040 Linz (Austria); Pedarnig, J.D., E-mail: [Christian Doppler Laboratory for Laser-Assisted Diagnostics, Institute of Applied Physics, Johannes Kepler University Linz, A-4040 Linz (Austria)


    We investigate the influence of sample temperature on the dynamics and optical emission of laser induced plasma for various solid materials. Bulk aluminum alloy, silicon wafer, and metallurgical slag samples are heated to temperature T{sub S} ≤ 500 °C and ablated in air by Nd:YAG laser pulses (wavelength 1064 nm, pulse duration approx. 7 ns). The plasma dynamics is investigated by fast time-resolved photography. For laser-induced breakdown spectroscopy (LIBS) the optical emission of plasma is measured by Echelle spectrometers in combination with intensified CCD cameras. For all sample materials the temporal evolution of plume size and broadband plasma emission vary systematically with T{sub S}. The size and brightness of expanding plumes increase at higher T{sub S} while the mean intensity remains independent of temperature. The intensity of emission lines increases with temperature for all samples. Plasma temperature and electron number density do not vary with T{sub S}. We apply the calibration-free LIBS method to determine the concentration of major oxides in slag and find good agreement to reference data up to T{sub S} = 450 °C. The LIBS analysis of multi-component materials at high temperature is of interest for technical applications, e.g. in industrial production processes. - Highlights: • Size and emission of laser-induced plasma increase with sample temperature Ts. • Mean optical intensity of plasma is independent of Ts. • Plasma temperature and electron number density do not vary with Ts. • Major oxides in steel slag are quantified up to Ts = 450 °C. • Industrial steel slags are analyzed by calibration-free LIBS method.

  6. First steps towards a generic sample preparation scheme for inorganic engineered nanoparticles in a complex matrix for detection, characterization, and quantification by asymmetric flow-field flow fractionation coupled to multi-angle light scattering and ICP-MS

    DEFF Research Database (Denmark)

    Wagner, Stephan; Legros, Samuel; Löschner, Katrin


    The applicability of a multi-step generic procedure to systematically develop sample preparation methods for the detection, characterization, and quantification of inorganic engineered nanoparticles (ENPs) in a complex matrix was successfully demonstrated. The research focused on the optimization...... content by asymmetric flow-field flow fractionation coupled to a multi-angle light scattering detector and an inductively coupled plasma mass spectrometer. Following the proposed generic procedure SiO2-ENPs were separated from a tomato soup. Two potential sample preparation methods were tested these being...

  7. Optical biosensor system with integrated microfluidic sample preparation and TIRF based detection (United States)

    Gilli, Eduard; Scheicher, Sylvia R.; Suppan, Michael; Pichler, Heinz; Rumpler, Markus; Satzinger, Valentin; Palfinger, Christian; Reil, Frank; Hajnsek, Martin; Köstler, Stefan


    There is a steadily growing demand for miniaturized bioanalytical devices allowing for on-site or point-of-care detection of biomolecules or pathogens in applications like diagnostics, food testing, or environmental monitoring. These, so called labs-on-a-chip or micro-total analysis systems (μ-TAS) should ideally enable convenient sample-in - result-out type operation. Therefore, the entire process from sample preparation, metering, reagent incubation, etc. to detection should be performed on a single disposable device (on-chip). In the early days such devices were mainly fabricated using glass or silicon substrates and adapting established fabrication technologies from the electronics and semiconductor industry. More recently, the development focuses on the use of thermoplastic polymers as they allow for low-cost high volume fabrication of disposables. One of the most promising materials for the development of plastic based lab-on-achip systems are cyclic olefin polymers and copolymers (COP/COC) due to their excellent optical properties (high transparency and low autofluorescence) and ease of processing. We present a bioanalytical system for whole blood samples comprising a disposable plastic chip based on TIRF (total internal reflection fluorescence) optical detection. The chips were fabricated by compression moulding of COP and microfluidic channels were structured by hot embossing. These microfluidic structures integrate several sample pretreatment steps. These are the separation of erythrocytes, metering of sample volume using passive valves, and reagent incubation for competitive bioassays. The surface of the following optical detection zone is functionalized with specific capture probes in an array format. The plastic chips comprise dedicated structures for simple and effective coupling of excitation light from low-cost laser diodes. This enables TIRF excitation of fluorescently labeled probes selectively bound to detection spots at the microchannel surface

  8. Fast determination of paraquat in plasma and urine samples by solid-phase microextraction and gas chromatography-mass spectrometry. (United States)

    Gao, Lina; Liu, Junting; Wang, Chunyuan; Liu, Guojie; Niu, Xiaodong; Shu, Cuixia; Zhu, Juan


    A simple, sensitive and reliable gas chromatographic-mass spectrometric method (GC-MS) for quantifying paraquat concentration in biological samples has been developed, using ethyl paraquat as an internal standard. The method involved the procedures of sodium borohydride-nickel chloride (NaBH4-NiCl2) reduction and solid-phase microextraction (SPME) of the perhydrogenated products. GC-MS was used to identify and quantify the analytes in selected ion monitoring (SIM) mode. Under the optimal conditions, recoveries in plasma and urine samples were 94.00-99.85% and 95.00-100.34%, respectively. Excellent sample clean-up was observed and good linearities (r=0.9982 for plasma sample and 0.9987 for urine sample) were obtained in the range of 0.1-50μg/mL. The limits of detection (S/N=3) were 0.01μg/mL in plasma and urine samples. The intra-day precision was less than 8.43%, 4.19% (n=3), and inter-day precision was less than 10.90%, 10.49% (n=5) for plasma and urine samples, respectively. This method was successfully applied to the analysis of the biological samples collected from a victim who died as a result of ingestion of paraquat.

  9. Sample preparation for metalloprotein analysis: A case study using horse chestnuts. (United States)

    de Magalhães, Cristiana Schmidt; Arruda, Marco Aurélio Zezzi


    In the present work, 11 different procedures for protein and metalloprotein extraction from horse chestnuts (Aescullus hippocastanum L.) in natura were tested. After each extraction, total protein was determined and, after protein separation through sodium dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE), those metals belonging to the protein structure were mapped by synchrotron radiation X-ray fluorescence (SRXRF). After mapping the elements (Cr, Fe and Mn) in the protein bands (ca. 33 and 23.7kDa), their concentrations were determined using atomic absorption spectrometry (ET AAS). Good results were obtained for protein extraction using a combination of grinding and sonication. However, this strategy was not suitable to preserve metal ions in the protein structure. In fact, there was 42% decrease on Mn concentration using this procedure, compared to that performed with sample agitation in water (taken as reference). On the other hand, when grinding and agitation with an extracting buffer was used, there was a 530% increase of Mn concentration, when compared to the reference procedure. These results indicate agreement between metal identification and determination in proteins as well as the great influence of the extraction procedure (i.e., the sample preparation step) for preserving metals in the protein structures.

  10. Sample preparation and in situ hybridization techniques for automated molecular cytogenetic analysis of white blood cells

    Energy Technology Data Exchange (ETDEWEB)

    Rijke, F.M. van de; Vrolijk, H.; Sloos, W. [Leiden Univ. (Netherlands)] [and others


    With the advent in situ hybridization techniques for the analysis of chromosome copy number or structure in interphase cells, the diagnostic and prognostic potential of cytogenetics has been augmented considerably. In theory, the strategies for detection of cytogenetically aberrant cells by in situ hybridization are simple and straightforward. In practice, however, they are fallible, because false classification of hybridization spot number or patterns occurs. When a decision has to be made on molecular cytogenetic normalcy or abnormalcy of a cell sample, the problem of false classification becomes particularly prominent if the fraction of aberrant cells is relatively small. In such mosaic situations, often > 200 cells have to be evaluated to reach a statistical sound figure. The manual enumeration of in situ hybridization spots in many cells in many patient samples is tedious. Assistance in the evaluation process by automation of microscope functions and image analysis techniques is, therefore, strongly indicated. Next to research and development of microscope hardware, camera technology, and image analysis, the optimization of the specimen for the (semi)automated microscopic analysis is essential, since factors such as cell density, thickness, and overlap have dramatic influences on the speed and complexity of the analysis process. Here we describe experiments that have led to a protocol for blood cell specimen that results in microscope preparations that are well suited for automated molecular cytogenetic analysis. 13 refs., 4 figs., 1 tab.

  11. Suspension trapping (STrap) sample preparation method for bottom-up proteomics analysis. (United States)

    Zougman, Alexandre; Selby, Peter J; Banks, Rosamonde E


    Despite recent developments in bottom-up proteomics, the need still exists in a fast, uncomplicated, and robust method for comprehensive sample processing especially when applied to low protein amounts. The suspension trapping method combines the advantage of efficient SDS-based protein extraction with rapid detergent removal, reactor-type protein digestion, and peptide cleanup. Proteins are solubilized in SDS. The sample is acidified and introduced into the suspension trapping tip incorporating the depth filter and hydrophobic compartments, filled with the neutral pH methanolic solution. The instantly formed fine protein suspension is trapped in the depth filter stack-this crucial step is aimed at separating the particulate matter in space. SDS and other contaminants are removed in the flow-through, and a protease is introduced. Following the digestion, the peptides are cleaned up using the tip's hydrophobic part. The methodology allows processing of protein loads down to the low microgram/submicrogram levels. The detergent removal takes about 5 min, whereas the tryptic proteolysis of a cellular lysate is complete in as little as 30 min. We have successfully utilized the method for analysis of cellular lysates, enriched membrane preparations, and immunoprecipitates. We expect that due to its robustness and simplicity, the method will become an essential proteomics tool.

  12. Determination of uranium from nuclear fuel in environmental samples using inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, S.F. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen]|[Radiation Physics and Chemistry Problems Inst., Minsk (Belarus); Becker, J.S. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen


    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The {sup 236}U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on inductively coupled plasma quadrupole mass spectrometry with a hexapole collision cell (HEX-ICP-QMS). The figures of merit of the HEX-ICP-QMS were studied with a plasma-shielded torch using different nebulizers (such as an ultrasonic nebulizer (USN) and Meinhard nebulizer) for solution introduction. A {sup 238}U{sup +} ion intensity of up to 27000 MHz/ppm in HEX-ICP-QMS with USN was observed by introducing helium into the hexapole collision cell as the collision gas at a flow rate of 10 ml min{sup -1}. The formation rate of uranium hydride ions UH{sup +}/U{sup +} of 2 x 10{sup -6} was obtained by using USN with a membrane desolvator. The limit of {sup 236}U/{sup 238}U ratio determination in 10 {mu}g 1{sup -1} uranium solution was 3 x 10{sup -7} corresponding to the detection limit for {sup 236}U of 3 pg 1{sup -1}. The precision of uranium isotopic ratio measurements in 10 {mu}g 1{sup -1} laboratory uranium isotopic standard solution was 0.13% ({sup 235}U/{sup 238}U) and 0.33% ({sup 236}U/{sup 238}U) using a Meinhard nebulizer and 0.45% ({sup 235}U/{sup 238}U) and 0.88% ({sup 236}U/{sup 238}U) using a USN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the {sup 236}U/{sup 238}U ratio ranged from 10{sup -5} to 10{sup -3}. (orig.)

  13. Geopolymers prepared from DC plasma treated air pollution control (APC) residues glass: properties and characterisation of the binder phase. (United States)

    Kourti, Ioanna; Devaraj, Amutha Rani; Bustos, Ana Guerrero; Deegan, David; Boccaccini, Aldo R; Cheeseman, Christopher R


    Air pollution control (APC) residues have been blended with glass-forming additives and treated using DC plasma technology to produce a high calcium aluminosilicate glass (APC glass). This has been used to form geopolymer-glass composites that exhibit high strength and density, low porosity, low water absorption, low leaching and high acid resistance. The composites have a microstructure consisting of un-reacted residual APC glass particles imbedded in a complex geopolymer and C-S-H gel binder phase, and behave as particle reinforced composites. The work demonstrates that materials prepared from DC plasma treated APC residues have potential to be used to form high quality pre-cast products.

  14. Investigation into Alternative Sample Preparation Techniques for the Determination of Heavy Metals in Stationary Source Emission Samples Collected on Quartz Filters

    Directory of Open Access Journals (Sweden)

    Sharon L. Goddard


    Full Text Available Monitoring stationary source emissions for heavy metals generally requires the use of quartz filters to collect samples because of the high temperature and high moisture sampling environment. The documentary standard method sample preparation technique in Europe, EN 14385, uses digestion in hydrofluoric acid and nitric acid (HF/HNO3 followed by complexing with boric acid (H3BO3 prior to analysis. However, the use of this method presents a number of problems, including significant instrumental drift during analysis caused by the matrix components, often leading to instrument breakdown and downtime for repairs, as well as posing significant health and safety risks. The aim of this work was to develop an alternative sample preparation technique for emissions samples on quartz filters. The alternative techniques considered were: (i acid digestion in a fluoroboric acid (HBF4 and HNO3 mixture and (ii acid extraction in an aqua regia (AR mixture (HCl and HNO3. Assessment of the effectiveness of these options included determination of interferences and signal drift, as well as validating the different methods by measurement of matrix certified reference materials (CRMs, and comparing the results obtained from real test samples and sample blanks to determine limits of detection. The results showed that the HBF4/HNO3 mixture provides the most viable alternative to the documentary standard preparation technique.

  15. State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review. (United States)

    Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C


    Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed.

  16. Preparation of a high-performance multi-lectin affinity chromatography (HP-M-LAC) adsorbent for the analysis of human plasma glycoproteins. (United States)

    Kullolli, Majlinda; Hancock, William S; Hincapie, Marina


    We report on the preparation of an improved multi-lectin affinity support for HPLC separations. We combined the selectivity of three different lectins: concanavalin A (ConA), wheat germ agglutinin (WGA), and jacalin (JAC). Each lectin was first covalently immobilized onto a polymeric matrix and then the three lectin media were combined in equal ratios. The beads were packed into a column to produce a mixed-bed multi-lectin HPLC column (high-performance multi-lectin affinity chromatography (HP-M-LAC)) for fast chromatographic affinity separations. The support was characterized with respect to kinetics of immobilization, ligand density, and binding capacity for human plasma glycoproteins. A high lectin density (15 mg/mL of beads) was found to be optimal for the binding of glycoproteins from human plasma. A single clinical sample can be fractionated in less than 10 min per run, making this a useful sample preparation tool for proteomics/glycoproteomics studies associated with disease abnormalities.

  17. Sample selection algorithm to improve quality of genotyping from plasma-derived DNA: to separate the wheat from the chaff. (United States)

    Schoenborn, Veit; Gohlke, Henning; Heid, Iris M; Illig, Thomas; Utermann, Gerd; Kronenberg, Florian


    Plasma and serum samples were often the only biological material collected for earlier epidemiological studies. These studies have a huge informative content, especially due to their long follow-up and would be an invaluable treasure for genetic investigations. However, often no banked DNA is available. To use the small amounts of DNA present in plasma, in a first step, we applied magnetic bead technology to extract this DNA, followed by a whole-genome amplification (WGA) using phi29-polymerase. We assembled 88 sample pairs, each consisting of WGA plasma DNA and the corresponding whole-blood DNA. We genotyped nine highly polymorphic short tandem repeats (STRs) and 23 SNPs in both DNA sources. The average within-pair discordance was 3.8% for SNPs and 15.9% for STR genotypes, respectively. We developed an algorithm based on one-half of the sample pairs and validated on the other one-half to identify the samples with high WGA plasma DNA quality to assure low genotyping error and to exclude plasma DNA samples with insufficient quality: excluding samples showing homozygosity at five or more of the nine STR loci yielded exclusion of 22.7% of all samples and decreased average discordance for STR and SNP markers to 3.92% and 0.63%, respectively. For SNPs, this is very close to the error observed for genomic DNA in many laboratories. Our workflow and sample selection algorithm offers new opportunities to recover reliable DNA from stored plasma material. This algorithm is superior to testing the amount of input DNA.

  18. Pregnancy-associated glycoprotein (PAG) concentration in plasma and milk samples for early pregnancy diagnosis in Lacaune dairy sheep. (United States)

    El Amiri, B; Sousa, N M; Alvarez Oxiley, A; Hadarbach, D; Beckers, J F


    In the present study, four RIA systems (RIA-1 to -4) based on two antisera raised against ovine pregnancy-associated glycoproteins (ovPAGs), combined with an ovine or a bovine PAG tracer were used to measure PAG concentrations in plasma and milk samples of dairy ewes. Blood and milk samples were collected on different days of gestation: 0, 18, 20, 22, 25, 28, 32, 42, and 49. From day 20 onward, the PAG in plasma could be detected in all pregnant ewes using the four RIA systems. By using milk, except for RIA-1, the other systems showed a sensitivity of 100% from day 28 of gestation onward. In plasma, PAG concentrations were higher in multiple than in single pregnancies, while no clear relationship was observed in milk. In conclusion, milk is a good alternative to plasma for early pregnancy diagnosis in sheep from day 28 to day 42.

  19. An evaluation of multiplex bead-based analysis of cytokines and soluble proteins in archived lithium heparin plasma, EDTA plasma and serum samples

    DEFF Research Database (Denmark)

    Brøndum, Line; Sørensen, Brita Singers; Eriksen, Jesper Grau


    in plasma and serum from 86 head and neck cancer patients and 33 controls were evaluated: EGFR, leptin, OPN, VEGFR-1, VEGFR-2, IL-2, IL-13, PDGF-bb, TNF, PAI-1, SDF-1a, IL-4, IL-6, IL-8, eotaxin, G-CSF, VEGF, GRO-a, and HGF. RESULTS: The correlation between measurements of the same samples analyzed...

  20. Toward a Fieldable Atomic Mass Spectrometer for Safeguards Applications: Sample Preparation and Ionization

    Energy Technology Data Exchange (ETDEWEB)

    Barinaga, Charles J.; Hager, George J.; Hart, Garret L.; Koppenaal, David W.; Marcus, R. Kenneth; Jones, Sarah MH; Manard, Benjamin T.


    The International Atomic Energy Agency’s (IAEA’s) long-term research and development plan calls for the development of new methods to detect misuse at nuclear fuel cycle facilities such as reprocessing and enrichment plants. At enrichment plants, for example, the IAEA’s contemporary safeguards approaches are based on a combination of routine and random inspections that include collection of UF6 samples from in-process material and selected cylinders for subsequent analyses. These analyses include destructive analysis (DA) in a laboratory (typically by mass spectrometry [MS]) for isotopic characterization, and environmental sampling (ES) for subsequent laboratory elemental and isotopic analysis (also both typically by MS). One area of new method development includes moving this kind of isotope ratio analytical capability for DA and ES activities into the field. Some of the reasons for these developments include timeliness of results, avoidance of hazardous material shipments, and guidance for additional sample collecting. However, this capability does not already exist for several reasons, such as that most lab-based chemical and instrumental methods rely on laboratory infrastructure (highly trained staff, power, space, hazardous material handling, etc.) and require significant amounts of consumables (power, compressed gases, etc.). In addition, there are no currently available, fieldable instruments for atomic or isotope ratio analysis. To address these issues, Pacific Northwest National Laboratory (PNNL) and collaborator, Clemson University, are studying key areas that limit the fieldability of isotope ratio mass spectrometry for atomic ions: sample preparation and ionization, and reducing the physical size of a fieldable mass spectrometer. PNNL is seeking simple and robust techniques that could be effectively used by inspectors who may have no expertise in analytical MS. In this report, we present and describe the preliminary findings for three candidate

  1. Comparative study of TEM sample preparation techniques for plasma-sprayed ceramic coatings


    Ramírez de Arellano López, Antonio; Chiou, W-A.; Faber, K. T.


    El desarrollo de materiales avanzados, con microestructuras cada vez más complejas, supone un reto constante de desarrollo y aplicación de técnicas que permitan el análisis de la microestructura de forma eficiente. En el caso de los recubrimientos cerámicos sobre substrato metálico, la diferente velocidad de adelgazamiento iónico que suelen mostrar ambos sistemas supone, en principio, una limitación sustancial. En este trabajo, presentamos un estudio comparativo de la fabricación de lámina...

  2. Preparation of edible wild fruit and plant samples for analysis and some difficulties encountered in such analyses

    CSIR Research Space (South Africa)

    Strydom, ESP


    Full Text Available Freeze-dried samples are used for analysis and the methods of preparation of samples for freeze-drying are discussed. Freeze-drying has obvious advantages but has also a few minor disadvantages. Difficulties encountered in the determination of some...

  3. Selectivity in the sample preparation for the analysis of drug residues in products of animal origin using LC-MS

    NARCIS (Netherlands)

    Berendsen, B.J.A.; Stolker, A.A.M.; Nielen, M.W.F.


    Sample preparation is critical in relation to analysis time, sample throughput and therefore analysis costs. Due to recent advances in liquid chromatography-mass spectrometry (LC-MS) instrumentation, the detection of many compounds within one run became possible, and methods for the simultaneous ana

  4. New Sample Preparation Method for Quantification of Phenolic Compounds of Tea (Camellia sinensis L. Kuntze: A Polyphenol Rich Plant

    Directory of Open Access Journals (Sweden)

    P. A. Nimal Punyasiri


    Full Text Available Chemical analysis of the Sri Lankan tea (Camellia sinensis, L. germplasm would immensely contribute to the success of the tea breeding programme. However, the polyphenols, particularly catechins (flavan-3-ols, are readily prone to oxidation in the conventional method of sample preparation. Therefore, optimization of the present sample preparation methodology for the profiling of metabolites is much important. Two sample preparation methodologies were compared, fresh leaves (as in the conventional procedures and freeze-dried leaves (a new procedure, for quantification of major metabolites by employing two cultivars, one is known to be high quality black tea and the other low quality black tea. The amounts of major metabolites such as catechins, caffeine, gallic acid, and theobromine, recorded in the new sampling procedure via freeze-dried leaves, were significantly higher than those recorded in the conventional sample preparation procedure. Additionally new method required less amount of leaf sample for analysis of major metabolites and facilitates storage of samples until analysis. The freeze-dried method would be useful for high throughput analysis of large number of samples in shorter period without chemical deterioration starting from the point of harvest until usage. Hence, this method is more suitable for metabolite profiling of tea as well as other phenol rich plants.


    The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.


    The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.

  7. ENO1 Protein Levels in the Tumor Tissues and Circulating Plasma Samples of Non-small Cell Lung Cancer Patients

    Directory of Open Access Journals (Sweden)

    Ying ZHANG


    Full Text Available Background and objective Proper tumor markers are useful to diagnosis, prognosis and treatment for lung cancer. The aim of this study is to examine the levels of alpha-enolase (ENO1 protein in the tumor tissues and peripheral plasma samples obtained from non-small cell lung cancer (NSCLC patients, and evaluate its potential clinical significance. Methods The ENO1 protein levels in the tumor tissues and corresponding normal tissues from 16 cases of lung squamous cell carcinoma were analyzed by Western blot. The ENO1 protein levels in the plasma samples from 42 healthy individuals, 34 patients with lung benign disease and 84 patients with NSCLC were measured by double antibody sandwich enzyme-linked immunosorbent assay. Results For 87.5% (14/16 of the patients with lung squamous cell carcinoma, the ENO1 protein level in the tumor tissues was higher than that in the corresponding normal lung tissues. The ENO1 protein level in the plasma of NSCLC patients was significantly higher than that in the plasma of healthy individuals (P=0.031 and patients with lung benign disease (P=0.019. Furthermore, the ENO1 protein level was significantly higher in the plasma of patients with lung adenocarcinoma than that of patients with lung squamous cell carcinoma. Conclusion The elevated levels of ENO1 protein in the tumor tissues and the plasma samples from NSCLC patients indicate ENO1 may be a candidate biomarker of lung cancer.

  8. A lab-on-a-chip system with integrated sample preparation and loop-mediated isothermal amplification for rapid and quantitative detection of Salmonella spp. in food samples

    DEFF Research Database (Denmark)

    Sun, Yi; Than Linh, Quyen; Hung, Tran Quang


    and usually take a few hours to days to complete. In response to the demand for rapid on line or at site detection of pathogens, in this study, we describe for the first time an eight-chamber lab-on-a-chip (LOC) system with integrated magnetic beads-based sample preparation and loop-mediated isothermal...

  9. Characteristics and properties of metal aluminum thin films prepared by electron cyclotron resonance plasma-assisted atomic layer deposition technology

    Institute of Scientific and Technical Information of China (English)

    Xiong Yu-Qing; Li Xing-Cun; Chen Qiang; Lei Wen-Wen; Zhao Qiao; Sang Li-Jun; Liu Zhong-Wei; Wang Zheng-Duo; Yang Li-Zhen


    Metal aluminum (Al) thin films are prepared by 2450 MHz electron cyclotron resonance plasma-assisted atomic layer deposition on glass and p-Si substrates using trimethylaluminum as the precursor and hydrogen as the reductive gas.We focus our attention on the plasma source for the thin-film preparation and annealing of the as-deposited films relative to the surface square resistivity.The square resistivity of as-deposited Al films is greatly reduced after annealing and almost reaches the value of bulk metal.Through chemical and structural analysis,we conclude that the square resistivity is determined by neither the contaminant concentration nor the surface morphology,but by both the crystallinity and crystal size in this process.

  10. Development of microwave-assisted drying methods for sample preparation for dried spot micro-X-ray fluorescence analysis. (United States)

    Link, Dirk D; Kingston, H M; Havrilla, George J; Colletti, Lisa P


    Although dried spot micro X-ray fluorescence (MXRF) is an effective analytical technique for trace elemental analysis, the sample preparation procedures currently used suffer from a number of drawbacks. These drawbacks include relatively long preparation times, lack of control of the sample preparation environment, and possibility of loss of volatile analytes during the drying process. Microwave-assisted drying offers several advantages for dried spot preparation, including control of the environment and minimized volatility because of the differences between microwave heating and conventional heating. A microwave-assisted drying technique has been evaluated for use in preparing dried spots for trace analysis. Two apparatus designs for microwave drying were constructed and tested using multielement standard solutions, a standard reference material, and a "real-world" semiconductor cleaning solution. Following microwave-assisted drying of these aqueous samples, the residues were redissolved and analyzed by ICPMS. Effective recovery was obtained using the microwave drying methods, demonstrating that the microwave drying apparatus and methods described here may be more efficient alternatives for dried spot sample preparation.

  11. Atmospheric-Pressure DBD Cold Plasma for Preparation of High Active Au/P25 Catalysts for Low-Temperature CO Oxidation (United States)

    Di, Lanbo; Zhan, Zhibin; Zhang, Xiuling; Qi, Bin; Xu, Weijie


    Cold plasma generated by dielectric barrier discharge (DBD) at atmospheric pressure was adopted for preparation of commercial TiO2 Degussa P25 supported Au catalysts (Au/P25-P) with the assistance of the deposition-precipitation procedure. The influences of the plasma reduction time and calcination on the performance of the Au/P25-P catalysts were investigated. CO oxidation was performed to investigate the catalytic activity of the Au/P25 catalysts. The results show that DBD cold plasma for the fabrication of Au/P25-P catalysts is a fast process, and Au/P25-P (4 min) exhibited the highest CO oxidation activity due to the complete reduction of Au compounds and less consumption of oxygen vacancies. In order to form more oxygen vacancies active species, Au/P25-P was calcined to obtain Au/P25-PC catalysts. Interestingly, Au/P25-PC exhibited the highest activity for CO oxidation among the Au/P25 samples. The results of transmission electron microscopy (TEM) indicated that the smaller size and high distribution of Au nanoparticles are the mean reasons for a high performance of Au/P25-PC. Atmospheric-pressure DBD cold plasma was proved to be of great efficiency in preparing high performance supported Au catalysts. supported by National Natural Science Foundation of China (Nos. 11505019, 21173028), the Science and Technology Research Project of Liaoning Provincial Education Department (No. L2013464), the Scientific Research Foundation for the Doctor of Liaoning Province (No. 20131004), and the Dalian Jinzhou New District Science and Technology Plan Project (No. KJCX-ZTPY-2014-0001)

  12. A lipemia-independent NanoDrop(®)-based score to identify hemolysis in plasma and serum samples. (United States)

    Appierto, Valentina; Callari, Maurizio; Cavadini, Elena; Morelli, Daniele; Daidone, Maria Grazia; Tiberio, Paola


    The identification and management of hemolyzed samples are crucial issues in the development of new blood-based biomarkers. Using experiments of controlled hemolysis and lipemia and two plasma series from cancer patients, we developed and validated a lipemia-independent hemolysis score (HS). HS resulted strictly associated with the amount of lysed erythrocytes and with serum index measurement (reference method), highly reproducible, and able to identify as hemolyzed plasma/serum samples containing ≥6.1 mg/dl of free hemoglobin. We developed a simple, robust, sensitive, cost-effective, spectrophotometrically-based system to identify hemolyzed plasma/serum specimens. The procedure requires only 2 μl of sample, thus representing a useful tool for research studies and an essential pre-analytical quality control for an optimal biobanking of liquid biopsies.

  13. Vehicle Exhaust Gas Clearance by Low Temperature Plasma-Driven Nano-Titanium Dioxide Film Prepared by Radiofrequency Magnetron Sputtering


    Shuang Yu; Yongdong Liang; Shujun Sun; Kai Zhang; Jue Zhang; Jing Fang


    A novel plasma-driven catalysis (PDC) reactor with special structure was proposed to remove vehicle exhaust gas. The PDC reactor which consisted of three quartz tubes and two copper electrodes was a coaxial dielectric barrier discharge (DBD) reactor. The inner and outer electrodes firmly surrounded the outer surface of the corresponding dielectric barrier layer in a spiral way, respectively. Nano-titanium dioxide (TiO2) film prepared by radiofrequency (RF) magnetron sputtering was coated on t...

  14. Humidity-controlled preparation of frozen-hydrated biological samples for cryogenic coherent x-ray diffraction microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Takayama, Yuki; Nakasako, Masayoshi [Department of Physics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Kanagawa 223-8522 (Japan); RIKEN Harima Institute/SPring-8, 1-1-1 Kouto, Mikaduki, Sayo, Hyogo 679-5148 (Japan)


    Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, we report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.

  15. Rapid Preparation Methods of Biological Samples for Ionic Compounds Using Ion Exchange Type Monolithic Silica Spin Column


    宮崎, 将太; 山田, 智子; 太田, 茂徳; 斉藤, 剛; 奈女良, 昭; 大平, 真義


    We developed a device comprising a spin column packed with ion exchange type (SCX and SAX) monolithic silica for extracting ionic compounds from biological samples. The methods involving the use of these spin column are not useful for the extraction of ionic analytes, but are highly reproducible for the analysis in serum and urine. This spin column enabled sample preparation in less than 10 min. Handling such as sample loading, washing, and elution of analytes, was exhibited by the centrifuga...

  16. Quality analysis of salmon calcitonin in a polymeric bioadhesive pharmaceutical formulation: sample preparation optimization by DOE. (United States)

    D'Hondt, Matthias; Van Dorpe, Sylvia; Mehuys, Els; Deforce, Dieter; DeSpiegeleer, Bart


    A sensitive and selective HPLC method for the assay and degradation of salmon calcitonin, a 32-amino acid peptide drug, formulated at low concentrations (400 ppm m/m) in a bioadhesive nasal powder containing polymers, was developed and validated. The sample preparation step was optimized using Plackett-Burman and Onion experimental designs. The response functions evaluated were calcitonin recovery and analytical stability. The best results were obtained by treating the sample with 0.45% (v/v) trifluoroacetic acid at 60 degrees C for 40 min. These extraction conditions did not yield any observable degradation, while a maximum recovery for salmon calcitonin of 99.6% was obtained. The HPLC-UV/MS methods used a reversed-phase C(18) Vydac Everest column, with a gradient system based on aqueous acid and acetonitrile. UV detection, using trifluoroacetic acid in the mobile phase, was used for the assay of calcitonin and related degradants. Electrospray ionization (ESI) ion trap mass spectrometry, using formic acid in the mobile phase, was implemented for the confirmatory identification of degradation products. Validation results showed that the methodology was fit for the intended use, with accuracy of 97.4+/-4.3% for the assay and detection limits for degradants ranging between 0.5 and 2.4%. Pilot stability tests of the bioadhesive powder under different storage conditions showed a temperature-dependent decrease in salmon calcitonin assay value, with no equivalent increase in degradation products, explained by the chemical interaction between salmon calcitonin and the carbomer polymer.

  17. Growth and characterization of nanodiamond layers prepared using the plasma-enhanced linear antennas microwave CVD system

    Energy Technology Data Exchange (ETDEWEB)

    Fendrych, Frantisek; Taylor, Andrew; Peksa, Ladislav; Kratochvilova, Irena; Kluiber, Zdenek; Fekete, Ladislav [Institute of Physics, Academy of Sciences of the Czech Republic, v.v.i, Na Slovance 2, CZ-18221 Prague 8 (Czech Republic); Vlcek, Jan [Department of Physics and Measurement, Institute of Chemical Technology Prague, Technicka 5, CZ-16628 Prague 6 (Czech Republic); Rezacova, Vladimira; Petrak, Vaclav [Faculty of Biomedical Engineering, Czech Technical University, Sitna 3105, CZ-27201 Kladno 2 (Czech Republic); Liehr, Michael [Leybold Optics Dresden GmbH, Zur Wetterwarte 50, D-01109 Dresden (Germany); Nesladek, Milos, E-mail: fendrych@fzu.c [IMOMEC division, IMEC, Institute for Materials Research, University Hasselt, Wetenschapspark 1, B-3590 Diepenbeek (Belgium)


    Industrial applications of plasma-enhanced chemical vapour deposition (CVD) diamond grown on large area substrates, 3D shapes, at low substrate temperatures and on standard engineering substrate materials require novel plasma concepts. Based on the pioneering work of the group at AIST in Japan, the high-density coaxial delivery type of plasmas has been explored (Tsugawa et al 2006 New Diamond Front. Carbon Technol. 16 337-46). However, an important challenge is to obtain commercially interesting growth rates at very low substrate temperatures. In this work we introduce the concept of novel linear antenna sources, designed at Leybold Optics Dresden, using high-frequency pulsed MW discharge with a high plasma density. This type of pulse discharges leads to the preparation of nanocrystalline diamond (NCD) thin films, compared with ultra-NCD thin films prepared in (Tsugawa et al 2006 New Diamond Front. Carbon Technol. 16 337-46). We present optical emission spectroscopy data for the CH{sub 4}-CO{sub 2}-H{sub 2} gas chemistry and we discuss the basic properties of the NCD films grown.

  18. Ni/MgO catalyst prepared using atmospheric high-frequency discharge plasma for CO2 reforming of methane

    Institute of Scientific and Technical Information of China (English)

    Pan Qin; Huiyuan Xu; Huali Long; Yi Ran; Shuyong Shang; Yongxiang Yin; Xiaoyan Dai


    A new type of Ni/MgO catalyst was prepared using atmospheric high-frequency discharge cold plasma.The influences of conventional method,plasma method,and plasma plus calcination method on the catalytic activity were studied and the CO2 reforming of methane was chosen as the probe reaction.The catalysts were characterized by X-ray diffraction (XRD),transmission electron microscope (TEM),X-ray photoelectron spectroscopy,and CO2 temperature-programmed surface reaction techniques.The results suggested that the nickel-based catalyst prepared by plasma plus calcination method possessed a smaller particle size and a higher dispersion of active component,better low-temperature activity and enhanced anti-coking ability.The conversion of CO2 and CH4 was 90.70% and 89.37%,respectively,and the reaction lasted for 36 h without obvious deactivation under 101.325 kPa and 750 ℃ with CO2/CH4 =1/1.

  19. Adjustable virtual pore-size filter for automated sample preparation using acoustic radiation force

    Energy Technology Data Exchange (ETDEWEB)

    Jung, B; Fisher, K; Ness, K; Rose, K; Mariella, R


    We present a rapid and robust size-based separation method for high throughput microfluidic devices using acoustic radiation force. We developed a finite element modeling tool to predict the two-dimensional acoustic radiation force field perpendicular to the flow direction in microfluidic devices. Here we compare the results from this model with experimental parametric studies including variations of the PZT driving frequencies and voltages as well as various particle sizes and compressidensities. These experimental parametric studies also provide insight into the development of an adjustable 'virtual' pore-size filter as well as optimal operating conditions for various microparticle sizes. We demonstrated the separation of Saccharomyces cerevisiae and MS2 bacteriophage using acoustic focusing. The acoustic radiation force did not affect the MS2 viruses, and their concentration profile remained unchanged. With optimized design of our microfluidic flow system we were able to achieve yields of > 90% for the MS2 with > 80% of the S. cerevisiae being removed in this continuous-flow sample preparation device.

  20. Dynamic simulation tools for the analysis and optimization of novel collection, filtration and sample preparation systems

    Energy Technology Data Exchange (ETDEWEB)

    Clague, D; Weisgraber, T; Rockway, J; McBride, K


    The focus of research effort described here is to develop novel simulation tools to address design and optimization needs in the general class of problems that involve species and fluid (liquid and gas phases) transport through sieving media. This was primarily motivated by the heightened attention on Chem/Bio early detection systems, which among other needs, have a need for high efficiency filtration, collection and sample preparation systems. Hence, the said goal was to develop the computational analysis tools necessary to optimize these critical operations. This new capability is designed to characterize system efficiencies based on the details of the microstructure and environmental effects. To accomplish this, new lattice Boltzmann simulation capabilities where developed to include detailed microstructure descriptions, the relevant surface forces that mediate species capture and release, and temperature effects for both liquid and gas phase systems. While developing the capability, actual demonstration and model systems (and subsystems) of national and programmatic interest were targeted to demonstrate the capability. As a result, where possible, experimental verification of the computational capability was performed either directly using Digital Particle Image Velocimetry or published results.

  1. Methodologies and perspectives of proteomics applied to filamentous fungi: from sample preparation to secretome analysis. (United States)

    Bianco, Linda; Perrotta, Gaetano


    Filamentous fungi possess the extraordinary ability to digest complex biomasses and mineralize numerous xenobiotics, as consequence of their aptitude to sensing the environment and regulating their intra and extra cellular proteins, producing drastic changes in proteome and secretome composition. Recent advancement in proteomic technologies offers an exciting opportunity to reveal the fluctuations of fungal proteins and enzymes, responsible for their metabolic adaptation to a large variety of environmental conditions. Here, an overview of the most commonly used proteomic strategies will be provided; this paper will range from sample preparation to gel-free and gel-based proteomics, discussing pros and cons of each mentioned state-of-the-art technique. The main focus will be kept on filamentous fungi. Due to the biotechnological relevance of lignocellulose degrading fungi, special attention will be finally given to their extracellular proteome, or secretome. Secreted proteins and enzymes will be discussed in relation to their involvement in bio-based processes, such as biomass deconstruction and mycoremediation.

  2. Atmospheric pressure microwave sample preparation procedure for the combined analysis of total phosphorus and kjeldahl nitrogen. (United States)

    Collins, L W; Chalk, S J; Kingston, H M


    An atmospheric pressure microwave digestion method has been developed for the combined analysis of total phosphorus and Kjeldahl nitrogen in complex matrices. In comparison to the digestion steps in EPA Methods 365.4 (total phosphorus) and 351.x (Kjeldahl nitrogen), this method requires less time, eliminates the need for a catalyst, and reduces the toxicity of the waste significantly. It employs a microwave-assisted digestion step, using refluxing borosilicate glass vessels at atmospheric pressure. Traditionally, this method has a time-consuming sample preparation step and generates toxic waste through the use of heavy metal catalysts. These advantages are gained by the combination of a high boiling point acid (sulfuric acid) and the application of focused microwave irradiation, which enhances the digestion process by direct energy coupling. NIST standard reference materials 1572 (citrus leaves), 1577a (bovine liver), and 1566 (oyster tissue) and tryptophan were analyzed to validate the method. Phosphorus concentrations were determined by the colorimetric ascorbic acid method outlined in EPA Method 365.3. Kjeldahl nitrogen concentrations were determined using EPA Method 351.1. The results of the analyses showed good precision and are in excellent agreement with the NIST published values for both elements.

  3. Small scale experiment on the plasma assisted thermal chemical preparation and combustion of pulverized coal

    Energy Technology Data Exchange (ETDEWEB)

    Masaya, Sugimoto; Koichi, Takeda [Akita Prefectural University (Japan); Solonenko, O.P. [Institute of Theoretical and Applied Mechanics, Novosibirsk (Russian Federation); Sakashita, M.; Nakamura, M. [Japan Technical Information Service, Tokyo (Japan)


    Ignition and stable combustion of pulverized coal with Nitrogen and Air plasmas are investigated experimentally for some different types of coal. The experimental results show that air plasma has strong effect for ignition and stabilization of coal combustion. In addition, suppression of NO{sub x} production could be possible even in air plasma. It is possible to ignite and burn stably for the inferior coal that contains volatile matter in the ratio of only 10% of dry total mass. (authors)

  4. Comparison of ESR1 Mutations in Tumor Tissue and Matched Plasma Samples from Metastatic Breast Cancer Patients

    Directory of Open Access Journals (Sweden)

    Takashi Takeshita


    Full Text Available BACKGROUND: ESR1 mutation in circulating cell-free DNA (cfDNA is emerging as a noninvasive biomarker of acquired resistance to endocrine therapy, but there is a paucity of data comparing the status of ESR1 gene in cfDNA with that in its corresponding tumor tissue. The objective of this study is to validate the degree of concordance of ESR1 mutations between plasma and tumor tissue. METHODS: ESR1 ligand-binding domain mutations Y537S, Y537N, Y537C, and D538G were analyzed using droplet digital PCR in 35 patients with metastatic breast cancer (MBC (35 tumor tissue samples and 67 plasma samples. RESULTS: Of the 35 paired samples, 26 (74.3% were concordant: one patient had detectable ESR1 mutations both plasma (ESR1 Y537S/Y537N and tumor tissue (ESR1 Y537S/Y537C, and 25 had WT ESR1 alleles in both. Nine (25.7% had discordance between the plasma and tissue results: five had mutations detected only in their tumor tissue (two Y537S, one Y537C, one D538G, and one Y537S/Y537N/D538G, and four had mutations detected only in their plasma (one Y537S, one Y537N, and two Y537S/Y537N/D538G. Furthermore, longitudinal plasma samples from 19 patients were used to assess changes in the presence of ESR1 mutations during treatment. Eleven patients had cfDNA ESR1 mutations over the course of treatment. A total of eight of 11 patients with MBC with cfDNA ESR1 mutations (72.7% had the polyclonal mutations. CONCLUSION: We have shown the independent distribution of ESR1 mutations between plasma and tumor tissue in 35 patients with MBC.

  5. Comparison of a new blood sampling device with the vacuum tube system for plasma and hematological analyses in healthy dogs. (United States)

    Reynolds, Brice S; Boudet, Karine G; Faucher, Mathieu R; Geffre, Anne; Germain, Claude; Lefebvre, Hervé P


    Pediatric devices based on a capillary system may provide an alternative to vacuum tubes for canine blood sampling. The potential advantages are absence of vein collapse, limited blood volume sampled, and improved safety. The aim of this study was to compare routine plasma and hematological variables in seven healthy dogs using both techniques. Five biochemical analytes were measured, and a complete hematological examination and plasma exogenous creatinine clearance test were performed. No clinically relevant difference between the two techniques was observed for any variable or functional test assessed.

  6. Development of a sample preparation procedure for the simultaneous determination of Np and Pu in clay samples

    Energy Technology Data Exchange (ETDEWEB)

    Renz, Tobias; Quinto, Francesca; Lagos, Markus; Plaschke, Markus; Bauer, Andreas; Geckeis, Horst [INE, KIT, Eggenstein-Leopoldshafen (Germany); Taubald, Heinrich [Eberhard Karls Universitaet, Tuebingen (Germany)


    Neptunium (Np) and plutonium (Pu) are two key radionuclides for the long-term disposal of nuclear waste. Within this context Opalinus Clay formations are considered as a potential location for disposal of high-level radioactive waste. In the framework of experiments studying the diffusion behavior and retention of actinides under repository conditions, the present work focuses on the development of an analytical-chemical procedure for the determination of Np and Pu in clay (or clay-rich soil) samples. The procedure aims at the simultaneous determination of Np and Pu at femto- to attogram levels with AMS. Fields of application are the investigation of global fallout actinides in environmental clay-rich samples or the diffusion behavior of actinides in compacted clay liners used as technical barriers in nuclear waste repositories. Clay samples are spiked with certified standards of Pu-242 and Np-237. The analytical method, including a) leaching of the spiked clay samples, b) redox adjustments of Np and Pu, c) chromatographic separation of Np and Pu from the sample matrix and d) measurement of the actinides with Sector Field (SF)-ICP-MS will be presented. The suitability of a Pu isotope as non-isotopic tracer for determination of Np-237 is evaluated by determining the chemical yield using SF-ICP-MS.

  7. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    Directory of Open Access Journals (Sweden)

    Christina Schreier


    Full Text Available Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after 1H NMR spectroscopy. Results. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at −20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Conclusion. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  8. Reproducibility of NMR analysis of urine samples: impact of sample preparation, storage conditions, and animal health status. (United States)

    Schreier, Christina; Kremer, Werner; Huber, Fritz; Neumann, Sindy; Pagel, Philipp; Lienemann, Kai; Pestel, Sabine


    Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining (1)H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing) and the health status of the animals, which may influence urine pH and osmolarity. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after (1)H NMR spectroscopy. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at -20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  9. Automated Sample Preparation for Radiogenic and Non-Traditional Metal Isotopes: Removing an Analytical Barrier for High Sample Throughput (United States)

    Field, M. Paul; Romaniello, Stephen; Gordon, Gwyneth W.; Anbar, Ariel D.; Herrmann, Achim; Martinez-Boti, Miguel A.; Anagnostou, Eleni; Foster, Gavin L.


    MC-ICP-MS has dramatically improved the analytical throughput for high-precision radiogenic and non-traditional isotope ratio measurements, compared to TIMS. The generation of large data sets, however, remains hampered by tedious manual drip chromatography required for sample purification. A new, automated chromatography system reduces the laboratory bottle neck and expands the utility of high-precision isotope analyses in applications where large data sets are required: geochemistry, forensic anthropology, nuclear forensics, medical research and food authentication. We have developed protocols to automate ion exchange purification for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U) using the new prepFAST-MC™ (ESI, Nebraska, Omaha). The system is not only inert (all-flouropolymer flow paths), but is also very flexible and can easily facilitate different resins, samples, and reagent types. When programmed, precise and accurate user defined volumes and flow rates are implemented to automatically load samples, wash the column, condition the column and elute fractions. Unattended, the automated, low-pressure ion exchange chromatography system can process up to 60 samples overnight. Excellent reproducibility, reliability, recovery, with low blank and carry over for samples in a variety of different matrices, have been demonstrated to give accurate and precise isotopic ratios within analytical error for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U). This illustrates the potential of the new prepFAST-MC™ (ESI, Nebraska, Omaha) as a powerful tool in radiogenic and non-traditional isotope research.

  10. Isotope labeled internal standards (ILIS) as a basis for quality control in clinical studies using plasma samples. (United States)

    Rezeli, Melinda; Végvári, Akos; Marko-Varga, György; Laurell, Thomas


    For clinical proteomic studies, the quality of the biofluid samples such as human blood plasma is extremely important. In this study we have investigated the stability of human plasma samples by spiking stable isotope-labeled peptides into the plasma and monitoring their degradation under different storage conditions. FPA-1, C4A and C3f were synthesized with isotopically labeled amino acids, and used as reference peptides. The mixture of internal calibrants was spiked into plasma at the starting point of investigation, mimicking the time of collection for future biobanking efforts, and their qualitative and quantitative changes were analyzed over time by using both MALDI-MS (LTQ Orbitrap XL) and nanoLC-ESI-MS (LTQ XL ETD). We have found that all three synthetic peptides were stable in plasma at -20 and -80 degrees C during the examined 2-month period. However, different proteolytic degradation profiles of the peptides were observed at room temperature. We anticipate that the use of these isotope-labeled peptides as internal standards (ILIS) provides a quality control for long-term storage and proteomic plasma analysis.

  11. Separation and Determination of Methylnaltrexone in Human Plasma Samples After Oral Administration by HPLC Coupled with Electrochemical Detection

    Institute of Scientific and Technical Information of China (English)

    WANG An-bao; Joseph F. Foss; YUAN Chun-su; Joachim Osinski


    A high performance liquid chromatography(HPLC) method coupled with electrochemical detection and solid phase extraction is described for the separation and determination of methylnaltrexone(MNTX), a quaternary opioid antagonist, in human clinical plasma samples after oral administration. Linearity of the standard curve for MNTX was found in the range of 4.0_150 ng/mL and was statistically conformed. The correlation coefficient(r2) and calibration equation obtained from linear regression analysis are 0.9999 and Y=54.27X-0.22, where Y and X represent the peak area and concentration of MNTX, respectively. The detection limit of MNTX under the present experimental conditions is 2.0 ng/mL by estimating at a ratio of 3 of signal to noise. The mean recovery of MNTX in human plasma is higher than 97%. The analytical method was applied to the pharmacokinetic determination of MNTX after single dose oral administration. These data demonstrate that the change of MNTX plasma concentration versus time is obvious. MNTX level of plasma reaches to a plateau between 45 to 120 minutes and then falls slowly. The content of MNTX in plasma sample maintains at an obviously detectable level after twelve hours of oral administration. The pharmacokinetic parameters for a single dose of 19.2 mg/kg in plasma are cmax=206.42(±16.53) ng/mL and tmax=60 min.

  12. Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents. (United States)

    Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew


    We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents.

  13. Automated Gel Size Selection to Improve the Quality of Next-generation Sequencing Libraries Prepared from Environmental Water Samples. (United States)

    Uyaguari-Diaz, Miguel I; Slobodan, Jared R; Nesbitt, Matthew J; Croxen, Matthew A; Isaac-Renton, Judith; Prystajecky, Natalie A; Tang, Patrick


    Next-generation sequencing of environmental samples can be challenging because of the variable DNA quantity and quality in these samples. High quality DNA libraries are needed for optimal results from next-generation sequencing. Environmental samples such as water may have low quality and quantities of DNA as well as contaminants that co-precipitate with DNA. The mechanical and enzymatic processes involved in extraction and library preparation may further damage the DNA. Gel size selection enables purification and recovery of DNA fragments of a defined size for sequencing applications. Nevertheless, this task is one of the most time-consuming steps in the DNA library preparation workflow. The protocol described here enables complete automation of agarose gel loading, electrophoretic analysis, and recovery of targeted DNA fragments. In this study, we describe a high-throughput approach to prepare high quality DNA libraries from freshwater samples that can be applied also to other environmental samples. We used an indirect approach to concentrate bacterial cells from environmental freshwater samples; DNA was extracted using a commercially available DNA extraction kit, and DNA libraries were prepared using a commercial transposon-based protocol. DNA fragments of 500 to 800 bp were gel size selected using Ranger Technology, an automated electrophoresis workstation. Sequencing of the size-selected DNA libraries demonstrated significant improvements to read length and quality of the sequencing reads.

  14. Microstructure, bonding strength and thermal shock resistance of ceramic coatings on steels prepared by plasma electrolytic oxidation (United States)

    Wang, Yunlong; Jiang, Zhaohua; Yao, Zhongping


    Ceramic coatings were successfully prepared on steel by plasma electrolytic oxidation (PEO) in aluminate electrolyte and silicate electrolyte, respectively. The microstructure of the coatings including surface morphology, phase and element composition were studied by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. The bonding strength between the ceramic coating and the substrate was tested using different methods including tensile tests and shearing tests. The thermal shock resistance of the coatings was also evaluated. The results indicated that coatings obtained in both electrolytes were porous and coarse. The average diameters of the pores were below 10 μm. PEO coatings obtained in aluminate electrolyte were composed of Fe 3O 4 and FeAl 2O 4, while those obtained in silicate electrolyte were in a noncrystal state. PEO coatings obtained in aluminate electrolyte showed similar change trend of tensile strength and shearing strength with increasing treating time, namely, a relatively high values with middle time treating and low value with short and long time treating. The best coating was the samples treated with 30 min, whose tensile strength was 20.6 MPa and shearing strength was 16 MPa. The tensile strength and shearing strength of coatings obtained in silicate electrolyte were not strongly influenced by the treating time, the values of which were range in 14 ± 2 MPa and 11 ± 2 MPa, respectively. Coatings obtained in both electrolytes showed the best thermal shock resistance with middle time treating. Coatings obtained in silicate electrolyte show a little better thermal shock resistance than those obtained in aluminate electrolyte.

  15. Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis. (United States)

    Wang, Xuan; Ye, Nengsheng


    In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  16. A Plasma-Assisted Route to the Rapid Preparation of Transition-Metal Phosphides for Energy Conversion and Storage

    KAUST Repository

    Liang, Hanfeng


    Transition-metal phosphides (TMPs) are important materials that have been widely used in catalysis, supercapacitors, batteries, sensors, light-emitting diodes, and magnets. The physical and chemical structure of a metal phosphide varies with the method of preparation as the electronic, catalytic, and magnetic properties of the metal phosphides strongly depend on their synthesis routes. Commonly practiced processes such as solid-state synthesis and ball milling have proven to be reliable routes to prepare TMPs but they generally require high temperature and long reaction time. Here, a recently developed plasma-assisted conversion route for the preparation of TMPs is reviewed, along with their applications in energy conversion and storage, including water oxidation electrocatalysis, sodium-ion batteries, and supercapacitors. The plasma-assisted synthetic route should open up a new avenue to prepare TMPs with tailored structure and morphology for various applications. In fact, the process may be further extended to the synthesis of a wide range of transition-metal compounds such as borides and fluorides at low temperature and in a rapid manner.

  17. Polymer monolithic capillary microextraction on-line coupled with inductively coupled plasma-mass spectrometry for the determination of trace Au and Pd in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xiaolan; He, Man; Chen, Beibei; Hu, Bin, E-mail:


    A novel method based on on-line polymer monolithic capillary microextraction (CME)-inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Au and Pd in biological samples. For this purpose, poly(glycidyl methacrylate-ethylene dimethacrylate) monolith was prepared and functionalized with mercapto groups. The prepared monolith exhibited good selectivity to Au and Pd, and good resistance to strong acid with a long life span. Factors affecting the extraction efficiency of CME, such as sample acidity, sample flow rate, eluent conditions and coexisting ion interference were investigated in detail. Under the optimal conditions, the limits of detection (LODs, 3σ) were 5.9 ng L{sup −1} for Au and 8.3 ng L{sup −1} for Pd, and the relative standard deviations (RSDs, c = 50 ng L{sup −1}, n = 7) were 6.5% for Au and 1.1% for Pd, respectively. The developed method was successfully applied to the determination of Au and Pd in human urine and serum samples with the recovery in the range of 84–118% for spiked samples. The developed on-line polymer monolithic CME-ICP-MS method has the advantages of rapidity, simplicity, low sample/reagent consumption, high sensitivity and is suitable for the determination of trace Au and Pd in biological samples with limited amount available and complex matrix. - Highlights: • An on-line CME-ICP-MS method was developed for Au and Pd analysis in human fluids. • Poly(GMA-EDMA-SH) monolith exhibited good selectivity for Au/Pd and acid-resistance. • The method is rapid, simple, and sensitive with low sample/reagents consumption.

  18. An On-Target Desalting and Concentration Sample Preparation Protocol for MALDI-MS and MS/MS Analysis

    DEFF Research Database (Denmark)

    Zhang, Xumin; Wang, Quanhui; Lou, Xiaomin;


    2DE coupled with MALDI-MS is one of the most widely used and powerful analytic technologies in proteomics study. The MALDI sample preparation method has been developed and optimized towards the combination of simplicity, sample-cleaning, and sample concentration since its introduction. Here we...... present a protocol of the so-called Sample loading, Matrix loading, and on-target Wash (SMW) method which fulfills the three criteria by taking advantage of the AnchorChip™ targets. Our method is extremely simple and no pre-desalting or concentration is needed when dealing with samples prepared from 2DE....... The protocol is amendable for automation and would pave the road for high-throughput MALDI-MS or MS/MS-based proteomics studies with guaranteed sensitivity and high identification rate. The method has been successfully applied to mouse liver proteome study and so far has been employed in other proteome studies...

  19. Fe{sub 2}O{sub 3} nanopowders prepared by a thermal plasma process for water oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Dongeun; Choi, Yong-Wook; Na, Ye-Seul; Choi, Soo-Suk; Park, Dong-Wha; Choi, Jinsub, E-mail:


    Highlights: • Hematite nanopowders with a high purity were synthesized by a DC thermal plasma process. • Fe{sub 3}O{sub 4} is formed during the formation of Fe{sub 2}O{sub 3} by thermal plasma with iron and oxygen sources. • Hematite nanopowders with a high purity show higher PEC performance compared to mixed oxides. - Abstract: Hematite (Fe{sub 2}O{sub 3}) nanopowders were synthesized from commercially available micro-sized iron powders by a DC thermal plasma process at atmospheric pressure. The micro-sized iron powders were vaporized in the plasma region, after which the plasma processing equipment was rapidly quenched, resulting in the formation of iron nanopowders with a size of less than 100 nm. Subsequently, the iron nanopowders were heated to convert hematite with a high purity, which was then formed into a thin film with a binder for preparation of electrodes for photoelectrochemical water oxidation. Iron oxide nanopowders were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), particle size analysis (PSA) and transmission electron microscopy (TEM). The photoelectrochemical properties of the Fe{sub 2}O{sub 3} film were characterized in 1 M NaOH under AM 1.5 conditions.

  20. Preparation

    Directory of Open Access Journals (Sweden)

    M.M. Dardir


    Full Text Available Some hexanamide-mono and di-linoleniate esters were prepared by the reaction of linolenic acid and hexanamide (derived from the reaction of hexanoic acid and diethanolamine. The chemical structure for the newly prepared hexanamide-mono and di-linoleniate esters were elucidated using elemental analysis, (FTIR, H 1NMR and chemical ionization mass spectra (CI/Ms spectroscopic techniques. The results of the spectroscopic analysis indicated that they were prepared through the right method and they have high purity. The new prepared esters have high biodegradability and lower toxicity (environmentally friendly so they were evaluated as a synthetic-based mud (ester-based mud for oil-well drilling fluids. The evaluation included study of the rheological properties, filtration and thermal properties of the ester based-muds formulated with the newly prepared esters compared to the reference commercial synthetic-based mud.

  1. Effect of piperine on pharmacokinetics of sodium valproate in plasma samples of rats using gas chromatography-mass spectrometry method

    Directory of Open Access Journals (Sweden)

    Bushra Parveen


    Full Text Available Piperine (PIP is used as anticonvulsant in traditional Chinese medicine. Co-administration of low-dose sodium valproate with PIP has been regarded to have potential anticonvulsant activity. Aim: This study was intended to investigate the effect of PIP on the pharmacokinetics of sodium valproate (SVP in the plasma samples of rats using gas chromatography-mass spectrometry (GC-MS method. Materials and Methods: The plasma samples obtained after oral administration of SVP, 150 mg/kg and SVP, 150 mg/kg + PIP, and 5 mg/kg to male Wistar rats were used to quantify the concentrations in plasma using GC-MS method. Results: A simple and accurate method developed in-house was applied for the analysis of plasma samples of Wistar rats after oral administration of SVP and PIP + sodium valproate, respectively. The pharmacokinetic parameters reported 14.8-fold increase in plasma concentration (maximum observed concentration in the concentration-time profile, 4.6-fold increase in area under the curve and slightly prolonged time to reach that concentration (1 h of SVP in presence of PIP. Conclusion: The study reaffirms the bioenhancing effect of PIP suggesting possibility of dose reduction of SVP while co-adminstering with PIP.

  2. Determination of stable cesium and strontium in rice samples by inductively coupled plasma mass spectrometry (United States)

    Srinuttrakul, W.; Yoshida, S.


    For long-term radiation dose assessment models, food ingestion is one of the major exposure pathways to human. In general, the stable isotopes can serve as analogues of radioisotopes. In this study, rice samples were collected from 30 paddy fields in Si Sa Ket, Yasothon and Roi Et in the northeast of Thailand in November 2014. The concentrations of stable cesium (Cs-133) and strontium (Sr-88) in polished rice were determined by inductively coupled plasma mass spectrometry (ICP-MS). The standard reference material of rice flour (NIST 1568a) with spiked Cs and Sr was used to validate the analytical method. The concentration of Cs in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.158 ± 0.167 mg kg-1, 0.090 ± 0.117 mg kg-1 and 0.054 ± 0.031 mg kg-1, respectively. The concentration of Sr in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.351 ± 0.108 mg kg-1, 0.364 ± 0.215 mg kg-1 and 0.287 ± 0.102 mg kg-1, respectively. Comparison of the results with Japanese data before the Fukushima Di-ichi nuclear power plant accident showed that the concentrations of both Cs and Sr for Thai rice were higher than those for Japanese rice.

  3. Heat Transfer in the Anode Region in Plasma-Electrolytic Heating of a Cylindrical Sample (United States)

    Zhirov, A. V.; Belkin, P. N.; Shadrin, S. Yu.


    The energy balance in a three-phase system "anode-vapor/gas envelope-electrolyte" and the results of experimental determination of the heat fluxes acting in the vapor-gas envelope are considered. To determine the fluxes quantitatively, the calorimetric method and the theory of inverse problems of the thermal conductivity of solid bodies are used. It is shown that heat fluxes into the anode and electrolyte increase with the voltage delivered to the electrochemical cell, whereas the heat flux associated with the vapor release to the atmosphere remains practically unchanged. An increase in the concentration of the current-conducting component in the electrolyte leads to a certain growth of the heat flux into the anode and to a decrease of the flux into the electrolyte. The stages of a nonstationary period of the process of plasma-electrolytic heating have been revealed, and it has been established that the time of heating the vapor-gas envelope is several times shorter than the time of heating a sample.

  4. Comparison of different sample preparation methods for platinum determination in cultured cells by graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Man Xiao


    Full Text Available Background Platinum-based agents are widely used in chemotherapy against solid tumors and insufficient intracellular drug accumulation is one of the leading causes of platinum resistance which is associated with poor survival of tumor patients. Thus, the detection of intracellular platinum is pivotal for studies aiming to overcome platinum resistance. In the present study, we aimed to establish a reliable graphite furnace atomic absorption spectrometry (GFAAS-based assay to quantify the intracellular platinum content for cultured cells. Methods Several most commonly applied cell preparation methods, including 0.2% HNO3, 0.2% Triton X-100, concentrated nitric acid, RIPA combined with concentrated nitric acid and hydroxide, followed by GFAAS for platinum detection were compared in ovarian, cervical and liver cancer cell lines to obtain the optimal one, and parameters regarding linearity, accuracy, precision and sensitivity were evaluated. Influence of other metals on platinum detection and the storage conditions of samples were also determined. Results The treatment of cells with 0.2% HNO3 was superior to other approaches with fewer platinum loss and better repeatability. The recovery rate and precision of this method were 97.3%–103.0% and 1.4%–3.8%, respectively. The average recoveries in the presence of other metals were 95.1%–103.1%. The detection limit was 13.23 ug/L. The recovery rate of platinum remained acceptable even in cell samples stored in −20 °C or −80 °C for two months. Discussion After comparison, we found that 0.2% HNO3 was optimal for intracellular platinum quantification based on GFAAS, which presented values compatible with that of inductively-coupled plasma mass-spectrometry (ICP-MS, and this is partially attributed to the simplicity of this method. Moreover, the assay was proved to be accurate, sensitive, cost-effective and suitable for the research of platinum-based antitumor therapy.

  5. Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate (United States)

    Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo


    The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

  6. Purification of Pregnancy-associated Plasma Protein-A and Preparation of Its Antibodies

    Institute of Scientific and Technical Information of China (English)

    CHENG; Bin-yan; LI; Zi-ying; YUAN; Zhi-gang; ZHANG; Xue-feng; LIU; Yi-bing


    Pregnancy-associated plasma protein-A(PAPP-A)is isolated from the plasma of pregnant women.It is producted by the syntrophoblast tissue of the placenta and decidual cells.PAPP-A belongs to macromolecular glycoprotein.As a sensitive serum marker,the decreased PAPP-A levels during the first

  7. Preparation and properties of HA coating hydrothermally synthesized from plasma sprayed CaHPO4 coating

    Institute of Scientific and Technical Information of China (English)

    FU Tao; HAN Yong; ZHANG Yu-mei; XU Ke-wei


    @@ INTRODUCTION Hydroxyapatite (HA) biocoatings can form osseointegration at a shorter time than metallic implants, and plasma sprayed (PS) HA coating has received the widest studies and is now used clinically. However, due to the high temperature of plasma flame, soluble impurity phases and amorphous calcium phosphate were contained which declined the bonding strength of the coating, and spoiled the excellent biological properties of HA.

  8. Preparation of Ag-containing diamond-like carbon films on the interior surface of tubes by a combined method of plasma source ion implantation and DC sputtering (United States)

    Hatada, R.; Flege, S.; Bobrich, A.; Ensinger, W.; Dietz, C.; Baba, K.; Sawase, T.; Watamoto, T.; Matsutani, T.


    Adhesive diamond-like carbon (DLC) films can be prepared by plasma source ion implantation (PSII), which is also suitable for the treatment of the inner surface of a tube. Incorporation of a metal into the DLC film provides a possibility to change the characteristics of the DLC film. One source for the metal is DC sputtering. In this study PSII and DC sputtering were combined to prepare DLC films containing low concentrations of Ag on the interior surfaces of stainless steel tubes. A DLC film was deposited using a C2H4 plasma with the help of an auxiliary electrode inside of the tube. This electrode was then used as a target for the DC sputtering. A mixture of the gases Ar and C2H4 was used to sputter the silver. By changing the gas flow ratios and process time, the resulting Ag content of the films could be varied. Sample characterizations were performed by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, atomic force microscopy and Raman spectroscopy. Additionally, a ball-on-disk test was performed to investigate the tribological properties of the films. The antibacterial activity was determined using Staphylococcus aureus bacteria.

  9. Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nomura, Cassiana S. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil); Silva, Cintia S. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil); Nogueira, Ana R.A. [Embrapa Pecuaria Sudeste, CP 339, Sao Carlos, SP 13560-970 (Brazil); Oliveira, Pedro V. [Instituto de Quimica, Universidade de Sao Paulo, CP 26077, Sao Paulo, SP 05513-970 (Brazil)]. E-mail:


    This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 deg. C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 deg. C and 2300 deg. C for Cu, and 700 deg. C and 1700 deg. C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 {mu}g of W + 200 {mu}g of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 {mu}g for Cu and 30 {mu}g for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg{sup -} {sup 1} and 128 mg kg{sup -} {sup 1}, respectively. The relative standard deviations were lower

  10. Evaluation of Electrospray as a Sample Preparation Tool for Electron Microscopic Investigations: Toward Quantitative Evaluation of Nanoparticles. (United States)

    Mielke, Johannes; Dohányosová, Pavla; Müller, Philipp; López-Vidal, Silvia; Hodoroaba, Vasile-Dan


    The potential of electrospray deposition, for the controlled preparation of particles for imaging in electron microscopes, is evaluated on various materials: from mono-modal suspensions of spherical particles to multimodal suspensions and to real-world industrial materials. It is shown that agglomeration is reduced substantially on the sample carrier, compared with conventional sample preparation techniques. For the first time, it is possible to assess the number concentration of a tri-modal polystyrene suspension by electron microscopy, due to the high deposition efficiency of the electrospray. We discovered that some suspension stabilizing surfactants form artifact particles during electrospraying. These can be avoided by optimizing the sprayed suspension.

  11. Simultaneous quantification of VX and its toxic metabolite in blood and plasma samples and its application for in vivo and in vitro toxicological studies. (United States)

    Reiter, Georg; Mikler, John; Hill, Ira; Weatherby, Kendal; Thiermann, Horst; Worek, Franz


    The present study was initiated to develop a sensitive and highly selective method for the simultaneous quantification of the nerve agent VX (O-ethyl S-[2(diisopropylamino)ethyl] methylphosphonothioate) and its toxic metabolite (EA-2192) in blood and plasma samples in vivo and in vitro. For the quantitative detection of VX and EA-2192 the resolution was realized on a HYPERCARB HPLC phase. A specific procedure was developed to isolate both toxic analytes from blood and plasma samples. The limit of detection was 0.1 pg/ml and the absolute recovery of the overall sample preparation procedure was 74% for VX and 69% for EA-2192. After intravenous and percutaneous administration of a supralethal doses of VX in anaesthetised swine both VX and EA-2192 could be quantified over 540 min following exposure. This study is the first to verify the in vivo formation of the toxic metabolite EA-2192 after poisoning with the nerve agent VX. Further toxicokinetic and therapeutic studies are required in order to determine the impact of EA-2192 on the treatment of acute VX poisoning.

  12. Pretreatment of plasma samples by a novel hollow fiber centrifugal ultrafiltration technique for the determination of plasma protein binding of three coumarins using acetone as protein binding releasing agent. (United States)

    Li, Junmei; Shi, Qingwen; Jiang, Ye; Liu, Yan


    A novel and practical sample pretreatment method based on hollow fiber centrifugal ultrafiltration (HFCF-UF) was developed to determine plasma protein binding by using HPLC. The samples for analyzing unbound and total concentrations could be prepared in parallel simultaneously by the same device. It only required centrifugation for a short time and the filtrate could be injected directly for HPLC analysis without further treatment. Coumarins were selected as the model drugs. Acetone was chosen as the releasing agent to free the binding drug from the drug-protein complex for the total drug concentration determination. Non-specific bindings (NSBs) between the analytes and hollow fiber membrane materials were investigated. The type and volume of protein binding releaser were optimized. Additionally, centrifugal speed and centrifugal time were considered. Under the optimized conditions, the absolute recovery rates of the unbound and total concentrations were in the range of 97.5-100.9% for the three analytes. The limits of detection were in the range of 0.0135-0.0667μgmL(-1). In vitro plasma protein binding of the three coumarins was determined at three concentrations using the validated method and the relative standard deviations (RSDs) were less than 3.4%. Compared with traditional method, the HFCF-UF method is simple to run, no specialized equipment requirement and is a more accurate plasma pretreatment procedure with almost excellent drug-protein binding equilibrium. Therefore, this method can be applied to determine the plasma protein binding in clinical practice. It also provides a reliable alternative for accurate monitoring of unbound or total drug concentration in therapeutic drug monitoring (TDM).

  13. Preparation of anti-adhesion surfaces on aluminium substrates of rubber plastic moulds using a coupling method of liquid plasma and electrochemical machining

    Directory of Open Access Journals (Sweden)

    Jianbing Meng


    Full Text Available Hard anti-adhesion surfaces, with low roughness and wear resistance, on aluminium substrates of rubber plastic moulds were fabricated via a new coupling method of liquid plasma and electrochemical machining. With the aid of liquid plasma thermal polishing and electrochemical anodic dissolution, micro/nano-scale binary structures were prepared as the base of the anti-adhesion surfaces. The anti-adhesion behaviours of the resulting aluminium surfaces were analysed by a surface roughness measuring instrument, a scanning electron microscope (SEM, a Fourier-transform infrared spectrophotometer (FTIR, an X-ray diffractometer (XRD, an optical contact angle meter, a digital Vickers micro-hardness (Hv tester, and electronic universal testing. The results show that, after the liquid plasma and electrochemical machining, micro/nano-scale binary structures composed of micro-scale pits and nano-scale elongated boss structures were present on the sample surfaces. As a result, the anti-adhesion surfaces fabricated by the above coupling method have good anti-adhesion properties, better wear resistance and lower roughness.

  14. Recovery of Salmonella from internally and externally contaminated whole tomatoes using several different sample preparation procedures. (United States)

    Wang, Hua; Gill, Vikas S; Irvin, Kari A; Byrd, Mindi; Bolger, Cathryn M; Zheng, Jie; Dickey, Erin E; Duvall, Robert E; Jacobson, Andrew P; Hammack, Thomas S


    Studies were conducted to determine the relative effectiveness of whole soak [current Bacteriological Analytical Manual-(BAM) Salmonella method], quarter, stomach, and blend methods for the recovery of Salmonella organisms from internally and externally contaminated tomatoes. Tomatoes were subjected to three inoculation methods: surface inoculation, internal inoculation by injection, and immersion with single Salmonella serovars. The inoculation levels ranged from 1 to 100 CFU/tomato for surface and injection inoculation or 1 to 100 CFU/mL for immersion inoculation. Tomatoes were held for 3 days after inoculation at 2-6 degrees C prior to initiation of analysis. Contaminated tomatoes were soaked, quartered, stomached, and blended in appropriate portions of Universal Pre-enrichment broth, and incubated for 24 h at 35 +/- 2 degrees C. The BAM Salmonella culture method was followed thereafter, and tomatoes were treated as a low-microbial-load food. The stomaching procedure was significantly (P < 0.05) more effective than the whole soak procedure for recovery of internalized Salmonella from tomatoes (by injection). The blending procedure was arithmetically superior to the stomaching procedure for detection of internalized Salmonella from tomatoes (by immersion). The blending procedure showed the same effectiveness as the whole soak procedure for the detection of Salmonella on tomato surfaces. Comparisons between test portion-to-broth ratios (weight to volume) showed that a 1:3 test portion-to-broth ratio had a better buffering capacity for blended tomatoes than a 1:1 test portion-to-broth ratio. It is recommended that the current whole soak BAM tomato sample preparation procedure be replaced with a blending procedure and a 1:3 test portion-to-broth ratio.

  15. Partial characterization of low density lipoprotein preparations isolated from fresh and frozen plasma after radiolabeling by seven different methods

    Energy Technology Data Exchange (ETDEWEB)

    Atsma, D.E.; Kempen, H.J.; Nieuwenhuizen, W.; van ' t Hooft, F.M.; Pauwels, E.K. (Gaubius Institute TNO, Leiden (Netherlands))


    Four {sup 99m}Tc and three {sup 123}I labeling methods were evaluated for their suitability to label low density lipoproteins (LDL) for the purpose of scintigraphic biodistribution studies. For {sup 99m}Tc these methods were: direct incorporation in LDL of {sup 99m}TcO4- using sodium dithionite (dithionite method); a method using first N,N-dimethylformamide to prepare a {sup 99m}Tc-complex reacting with LDL in a subsequent step (DMF method); a technique in which {sup 99m}TcO4- is first coupled to a diamide dithiolate derivative of pentanoic acid by reduction with dithionite, followed by coupling of this ligand to LDL (N2S2 method); and a method using sodium borohydride and stannous chloride as reducing agents (borohydride method). The iodination techniques were based on oxidation of I(-)----I+, using iodine monochloride (ICl method), 1,3,4,6-tetrachloro-3,6-diphenylglycoluril (Iodogen method), and N-bromosuccinimide (NBS method) as oxidants. We studied labeling yields, modification of LDL caused by the labeling procedures using agarose-gel electrophoresis, and radiochemical stability of the labeled LDL complex upon incubation in plasma at 37 degrees C for 15 h. We used Sepharose CL6B chromatography to separate LDL from other plasma proteins. We also examined whether LDL isolated from frozen plasma (Pool-LDL) gave results similar to LDL obtained from freshly prepared plasma (Fresh-LDL). Pool-LDL radiolabeled by the dithionite, DMF, NBS, and Iodogen methods lost its label upon incubation with plasma. This also happened with Fresh-LDL when the DMF, NBS and Iodogen methods were used. Upon agarose-gel electrophoresis, no modification of LDL was observed with all methods when the radionuclide/LDL ratio was kept low.

  16. Preparative chromatography for specific δ13C isotopic analysis of individual carbohydrates in environmental samples (United States)

    Nouara, Amel; Panagiotopoulos, Christos; Balesdent, Jérôme; Sempéré, Richard


    Carbohydrates are among the most abundant organic molecules on the Earth and are present in all geochemical systems. Despite their high abundance in the environment, very few studies assessed their origin using molecular carbohydrate isotopic analyses. In contrast with bulk stable isotope analysis (BSIA), which gives the isotopic signature of the entire sample without any specification about its chemical composition, compound specific 13C isotopic analysis of individual sugars (CSIA) offers valuable information about the origin of single molecules. Previous investigations used gas or liquid chromatography coupled with isotope ratio mass spectroscopy (GC-IRMS; HPLC-IRMS) for CSIA of sugars however the former requires δ13C corrections due to the carbon added to the sugar (derivatization) while the later does not provide always adequate separations among monosaccharides. Here we used cation preparative chromatography (Ca2+, Pb2+ and Na+) with refractive index detection in order to produce pure monosaccharide targets for subsequent EA-IRMS analyses. Milli-Q water was used as eluant at a flow rate 0.6 ml min-1. In general, three successive purifications (Ca2+, Pb2+, Ca2+) were sufficient to produce pure compounds. Pure monosaccharides were compared with authentic monosaccharide standards using 1H NMR and/or mass spectroscopy. The detection limit of our technique was about 1µM/sugar with a precision of 10% (n=6). Blanks run with Milli-Q water after three successive purifications resulted in carbon content of 0.13 to 2.77 µgC per collected sugar. These values are much lower than the minimum required amount (5 µgC) of the EA-IRSMS system with a precision of ± 0.35 ‰. Application of our method to environmental samples resulted in δ13C values of glucose, fructose, and levoglucosan in the range of -24 to -26 ‰ (PM10 atmospheric particles), and -15‰ to -22 ‰ for arabinose, glucose, and xylose (marine high molecular dissolved organic matter). These results fall in

  17. Closer to the native state. Critical evaluation of cryo-techniques for Transmission Electron Microscopy: preparation of biological samples. (United States)

    Mielanczyk, Lukasz; Matysiak, Natalia; Michalski, Marek; Buldak, Rafal; Wojnicz, Romuald


    Over the years Transmission Electron Microscopy (TEM) has evolved into a powerful technique for the structural analysis of cells an