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Sample records for extract dilution analysis

  1. Extended aroma extract dilution analysis profile of Shiikuwasha (Citrus depressa Hayata pulp essential oil

    Directory of Open Access Journals (Sweden)

    Yonathan Asikin

    2018-01-01

    Full Text Available Shiikuwasha pulp is an important raw material for producing citrus essential oils. The volatile aroma composition of pulp essential oil was evaluated using gas chromatography (GC methods, and its aroma profile was assessed using GC-olfactometry with an extended aroma extract dilution analysis (AEDA technique in regard to alterations of odor strength and sensorial perception throughout serial dilution steps. The essential oil comprised a mixture of 55 aroma compounds, including monoterpene hydrocarbon, sesquiterpene hydrocarbon, alcohol, aldehyde, ester, and oxide compounds. The predominant compounds were limonene [57.36% (4462.80 mg/100 g of pulp] and γ-terpinene [25.14% (1956.21 mg/100 g of pulp]. However, linalool was identified as one of the key aroma components providing the highest flavor dilution factor in AEDA, whilst three sesquiterpene hydrocarbons (δ-elemene, germacrene B, and bicyclosesquiphellandrene and two esters (heptyl acetate and decyl acetate had superior relative flavor activities. The extended AEDA profile identified variations in assessed odor perceptions, intensity, and duration of aroma components over dilution, whereas the 12 most odor-active compounds showed comparable odor strengths.

  2. Cellular Lipid Extraction for Targeted Stable Isotope Dilution Liquid Chromatography-Mass Spectrometry Analysis

    Science.gov (United States)

    Gelhaus, Stacy L.; Mesaros, A. Clementina; Blair, Ian A.

    2011-01-01

    The metabolism of fatty acids, such as arachidonic acid (AA) and linoleic acid (LA), results in the formation of oxidized bioactive lipids, including numerous stereoisomers1,2. These metabolites can be formed from free or esterified fatty acids. Many of these oxidized metabolites have biological activity and have been implicated in various diseases including cardiovascular and neurodegenerative diseases, asthma, and cancer3-7. Oxidized bioactive lipids can be formed enzymatically or by reactive oxygen species (ROS). Enzymes that metabolize fatty acids include cyclooxygenase (COX), lipoxygenase (LO), and cytochromes P450 (CYPs)1,8. Enzymatic metabolism results in enantioselective formation whereas ROS oxidation results in the racemic formation of products. While this protocol focuses primarily on the analysis of AA- and some LA-derived bioactive metabolites; it could be easily applied to metabolites of other fatty acids. Bioactive lipids are extracted from cell lysate or media using liquid-liquid (l-l) extraction. At the beginning of the l-l extraction process, stable isotope internal standards are added to account for errors during sample preparation. Stable isotope dilution (SID) also accounts for any differences, such as ion suppression, that metabolites may experience during the mass spectrometry (MS) analysis9. After the extraction, derivatization with an electron capture (EC) reagent, pentafluorylbenzyl bromide (PFB) is employed to increase detection sensitivity10,11. Multiple reaction monitoring (MRM) is used to increase the selectivity of the MS analysis. Before MS analysis, lipids are separated using chiral normal phase high performance liquid chromatography (HPLC). The HPLC conditions are optimized to separate the enantiomers and various stereoisomers of the monitored lipids12. This specific LC-MS method monitors prostaglandins (PGs), isoprostanes (isoPs), hydroxyeicosatetraenoic acids (HETEs), hydroxyoctadecadienoic acids (HODEs), oxoeicosatetraenoic

  3. Isotope dilution analysis

    Energy Technology Data Exchange (ETDEWEB)

    Fudge, A.

    1978-12-15

    The following aspects of isotope dilution analysis are covered in this report: fundamental aspects of the technique; elements of interest in the nuclear field, choice and standardization of spike nuclide; pre-treatment to achieve isotopic exchange and chemical separation; sensitivity; selectivity; and accuracy.

  4. Spectroscopic analysis of hot-water- and dilute-acid-extracted hardwood and softwood chips

    Science.gov (United States)

    Lehto, Joni; Louhelainen, Jarmo; Huttunen, Marko; Alén, Raimo

    2017-09-01

    Hot-water and dilute sulfuric acid pretreatments were performed prior to chemical pulping for silver/white birch (Betula pendula/B. pubescens) and Scots pine (Pinus sylvestris) chips to determine if varying pretreatment conditions on the original wood material were detectable via attenuated total reflectance (ATR) infrared spectroscopy. Pretreatment conditions varied with respect to temperature (130 °C and 150 °C) and treatment time (from 30 min to 120 min). The effects of the pretreatments on the composition of wood chips were determined by ATR infrared spectroscopy. The spectral data were compared to those determined by common wood chemistry analyses to evaluate the suitability of ATR spectroscopy method for rapid detection of changes in the wood chemical composition caused by different pretreatment conditions. In addition to determining wood species-dependent differences in the wood chemical composition, analytical results indicated that most essential lignin- and carbohydrates-related phenomena taking place during hot-water and acidic pretreatments could be described by applying this simple spectral method requiring only a small sample amount and sample preparation. Such information included, for example, the cleavage of essential lignin bonds (i.e., mainly β-O-4 linkages in guaiacyl and syringyl lignin) and formation of newly condensed lignin structures under different pretreatment conditions. Carbohydrate analyses indicated significant removal of hemicelluloses (especially hardwood xylan) and hemicelluloses-derived acetyl groups during the pretreatments, but they also confirmed the highly resistant nature of cellulose towards mild pretreatments.

  5. Aroma extraction dilution analysis of Sauternes wines. Key role of polyfunctional thiols.

    Science.gov (United States)

    Bailly, Sabine; Jerkovic, Vesna; Marchand-Brynaert, Jacqueline; Collin, Sonia

    2006-09-20

    The aim of the present work was to investigate Sauternes wine aromas. In all wine extracts, polyfunctional thiols were revealed to have a huge impact. A very strong bacon-petroleum odor emerged at RI = 845 from a CP-Sil5-CB column. Two thiols proved to participate in this perception: 3-methyl-3-sulfanylbutanal and 2-methylfuran-3-thiol. A strong synergetic effect was evidenced between the two compounds. The former, never mentioned before in wines, and not found in the musts of this study, is most probably synthesized during fermentation. 3-Methylbut-2-ene-1-thiol, 3-sulfanylpropyl acetate, 3-sulfanylhexan-1-ol, and 3-sulfanylheptanal also contribute to the global aromas of Sauternes wines. Among other key odorants, the presence of a varietal aroma (alpha-terpineol), sotolon, fermentation alcohols (3-methylbutan-1-ol and 2-phenylethanol) and esters (ethyl butyrate, ethyl hexanoate, and ethyl isovalerate), carbonyls (trans-non-2-enal and beta-damascenone), and wood flavors (guaiacol, vanillin, eugenol, beta-methyl-gamma-octalactone, and Furaneol) is worth stressing.

  6. Approaches of aroma extraction dilution analysis (AEDA) for headspace solid phase microextraction and gas chromatography-olfactometry (HS-SPME-GC-O): Altering sample amount, diluting the sample or adjusting split ratio?

    Science.gov (United States)

    Feng, Yunzi; Cai, Yu; Sun-Waterhouse, Dongxiao; Cui, Chun; Su, Guowan; Lin, Lianzhu; Zhao, Mouming

    2015-11-15

    Aroma extract dilution analysis (AEDA) is widely used for the screening of aroma-active compounds in gas chromatography-olfactometry (GC-O). In this study, three aroma dilution methods, (I) using different test sample volumes, (II) diluting samples, and (III) adjusting the GC injector split ratio, were compared for the analysis of volatiles by using HS-SPME-AEDA. Results showed that adjusting the GC injector split ratio (III) was the most desirable approach, based on the linearity relationships between Ln (normalised peak area) and Ln (normalised flavour dilution factors). Thereafter this dilution method was applied in the analysis of aroma-active compounds in Japanese soy sauce and 36 key odorants were found in this study. The most intense aroma-active components in Japanese soy sauce were: ethyl 2-methylpropanoate, ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, ethyl 4-methylpentanoate, 3-(methylthio)propanal, 1-octen-3-ol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2-methoxy-4-vinylphenol, 2-phenylethanol, and 4-hydroxy-5-ethyl-2-methyl-3(2H)-furanone. Copyright © 2015. Published by Elsevier Ltd.

  7. Substoichiometric isotope dilution analysis of arsenic in biological and environmental standard reference materials by solvent extraction using toluene-3,4-dithiol in benzene

    International Nuclear Information System (INIS)

    Chutke, N.L.; Ambulkar, Ms.M.N.; Weginwar, R.G.; Garg, A.N.

    1994-01-01

    A radiochemical solvent extraction procedure has been developed for the determination of As(III) using 76 As tracer. It is based on the complexation of As(III) with toluene-3,4-dithiol (TDT) at pH 2 and subsequent extraction in benzene. The effect of various parameters such as pH, time of equilibration, nature of solvent, quantitative character and interferences have been studied. The method has been further developed into substoichiometric isotope dilution analysis for the determination of As at < 1μg level and employed for the analysis of several environmental and biological standard Reference Materials from NIST (USA), IAEA (Vienna) and NIES (Japan). (author) 39 refs.; 4 figs.; 4 tabs

  8. Primary system boron dilution analysis

    International Nuclear Information System (INIS)

    Crump, R.J.; Naretto, C.J.; Borgen, R.A.; Rockhold, H.C.

    1978-01-01

    The results are presented for an analysis conducted to determine the potential paths through which nonborated water or water with insufficient boron concentration might enter the LOFT primary coolant piping system or reactor vessel to cause dilution of the borated primary coolant water. No attempt was made in the course of this analysis to identify possible design modifications nor to suggest changes in administrative procedures or controls

  9. Characterization of the Major Odor-Active Compounds in the Leaves of the Curry Tree Bergera koenigii L. by Aroma Extract Dilution Analysis.

    Science.gov (United States)

    Steinhaus, Martin

    2015-04-29

    Curry leaves are a popular seasoning herb with a pronounced sulfury and burnt odor, the molecular background of which was yet unclear. Application of an aroma extract dilution analysis to the volatile fraction of curry leaves isolated by solvent extraction and solvent-assisted flavor evaporation afforded 23 odor-active compounds with flavor dilution (FD) factors ranging from 1 to 8192. On the basis of the comparison of their retention indices, mass spectra, and odor properties with data of reference compounds, the structures of 22 odorants could be assigned, 15 of which had not been reported in curry leaves before. Odorants with high FD factors included 1-phenylethanethiol (FD factor 8192), linalool (4096), α-pinene (2048), 1,8-cineole (1024), (3Z)-hex-3-enal (256), 3-(methylsulfanyl)propanal (128), myrcene (64), (3Z)-hex-3-en-1-ol (32), and (2E,6Z)-nona-2,6-dienal (32). The unique sulfury and burnt odor exhibited by 1-phenylethanethiol in combination with its high FD factor suggested that it constitutes the character impact compound of fresh curry leaf aroma.

  10. Verification of key odorants in rose oil by gas chromatography-olfactometry/aroma extract dilution analysis, odour activity value and aroma recombination.

    Science.gov (United States)

    Xiao, Zuobing; Li, Jing; Niu, Yunwei; Liu, Qiang; Liu, Junhua

    2017-10-01

    Rose oil is much too expensive but very popular. It's well known that the flower oil's aroma profile hasn't been intensively investigated. In order to verify the aroma profile of rose oil, the synthetic blend of odorants was prepared and then compared with the original rose oil using electronic nose analysis (ENA) combined with quantitative descriptive analysis (QDA). The odorants from rose oils were screened out by Gas Chromatography-Olfactometry/aroma extract dilution analysis (GC-O/AEDA) combined with odour activity value (OAV). Both ENA and QDA indicated the recombination model derived from OAV and GC-O/AEDA closely resembled the original rose oil. The experiment results show that rose oxide, linalool, α-pinene, β-pinene, nonanal, heptanal citronellal, phenyl ethyl alcohol, benzyl alcohol, eugenol, methyl eugenol, β-citronellol, hexyl acetate, β-ionone, nerol, etc. are very important constituent to rose oil aroma profile.

  11. Characterization of Key Aroma Compounds in Raw and Thermally Processed Prawns and Thermally Processed Lobsters by Application of Aroma Extract Dilution Analysis.

    Science.gov (United States)

    Mall, Veronika; Schieberle, Peter

    2016-08-24

    Application of aroma extract dilution analysis (AEDA) to an aroma distillate of blanched prawn meat (Litopenaeus vannamei) (BPM) revealed 40 odorants in the flavor dilution (FD) factor range from 4 to 1024. The highest FD factors were assigned to 2-acetyl-1-pyrroline, 3-(methylthio)propanal, (Z)-1,5-octadien-3-one, trans-4,5-epoxy-(E)-2-decenal, (E)-3-heptenoic acid, and 2-aminoacetophenone. To understand the influence of different processing conditions on odorant formation, fried prawn meat was investigated by means of AEDA in the same way, revealing 31 odorants with FD factors between 4 and 2048. Also, the highest FD factors were determined for 2-acetyl-1-pyrroline, 3-(methylthio)propanal, and (Z)-1,5-octadien-3-one, followed by 4-hydroxy-2,5-dimethyl-3(2H)-furanone, (E)-3-heptenoic acid, and 2-aminoacetophenone. As a source of the typical marine, sea breeze-like odor attribute of the seafood, 2,4,6-tribromoanisole was identified in raw prawn meat as one of the contributors. Additionally, the aroma of blanched prawn meat was compared to that of blanched Norway and American lobster meat, respectively (Nephrops norvegicus and Homarus americanus). Identification experiments revealed the same set of odorants, however, with differing FD factors. In particular, 3-hydroxy-4,5-dimethyl-2(5H)-furanone was found as the key aroma compound in blanched Norway lobster, whereas American lobster contained 3-methylindole with a high FD factor.

  12. Analysis of trace metals (Cu, Cd, Pb, and Fe) in seawater using single batch nitrilotriacetate resin extraction and isotope dilution inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jong-Mi [Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States); Boyle, Edward A., E-mail: eaboyle@mit.edu [Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States); Echegoyen-Sanz, Yolanda; Fitzsimmons, Jessica N. [Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States); Zhang Ruifeng [State Key Laboratory of Estuarine and Coastal Research, East China Normal University, Shanghai 200062 (China); Kayser, Richard A. [Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States)

    2011-02-07

    A simple and accurate low-blank method has been developed for the analysis of total dissolved copper, cadmium, lead, and iron in a small volume (1.3-1.5 mL per element) of seawater. Pre-concentration and salt-separation of a stable isotope spiked sample are achieved by single batch extraction onto nitrilotriacetate (NTA)-type Superflow chelating resin beads (100-2400 beads depending on the element). Metals are released into 0.1-0.5 M HNO{sub 3}, and trace metal isotope ratios are determined by ICPMS. The benefit of this method compared to our previous Mg(OH){sub 2} coprecipitation method is that the final matrix is very dilute so cone-clogging and matrix sensitivity suppression are minimal, while still retaining the high accuracy of the isotope dilution technique. Recovery efficiencies are sensitive to sample pH, number of resin beads added, and the length of time allowed for sample-resin binding and elution; these factors are optimized for each element to yield the highest recovery. The method has a low procedural blank and high sensitivity sufficient for the analysis of pM-nM open-ocean trace metal concentrations. Application of this method to samples from the Bermuda Atlantic Time-Series Study station provides oceanographically consistent Cu, Cd, Pb, and Fe profiles that are in good agreement with other reliable data for this site. In addition, the method can potentially be modified for the simultaneous analysis of multiple elements, which will be beneficial for the analysis of large number of samples.

  13. Analysis of trace metals (Cu, Cd, Pb, and Fe) in seawater using single batch nitrilotriacetate resin extraction and isotope dilution inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Lee, Jong-Mi; Boyle, Edward A.; Echegoyen-Sanz, Yolanda; Fitzsimmons, Jessica N.; Zhang Ruifeng; Kayser, Richard A.

    2011-01-01

    A simple and accurate low-blank method has been developed for the analysis of total dissolved copper, cadmium, lead, and iron in a small volume (1.3-1.5 mL per element) of seawater. Pre-concentration and salt-separation of a stable isotope spiked sample are achieved by single batch extraction onto nitrilotriacetate (NTA)-type Superflow chelating resin beads (100-2400 beads depending on the element). Metals are released into 0.1-0.5 M HNO 3 , and trace metal isotope ratios are determined by ICPMS. The benefit of this method compared to our previous Mg(OH) 2 coprecipitation method is that the final matrix is very dilute so cone-clogging and matrix sensitivity suppression are minimal, while still retaining the high accuracy of the isotope dilution technique. Recovery efficiencies are sensitive to sample pH, number of resin beads added, and the length of time allowed for sample-resin binding and elution; these factors are optimized for each element to yield the highest recovery. The method has a low procedural blank and high sensitivity sufficient for the analysis of pM-nM open-ocean trace metal concentrations. Application of this method to samples from the Bermuda Atlantic Time-Series Study station provides oceanographically consistent Cu, Cd, Pb, and Fe profiles that are in good agreement with other reliable data for this site. In addition, the method can potentially be modified for the simultaneous analysis of multiple elements, which will be beneficial for the analysis of large number of samples.

  14. Characterization of the major odor-active compounds in Thai durian ( Durio zibethinus L. 'Monthong') by aroma extract dilution analysis and headspace gas chromatography-olfactometry.

    Science.gov (United States)

    Li, Jia-Xiao; Schieberle, Peter; Steinhaus, Martin

    2012-11-14

    An aroma extract dilution analysis applied on the volatile fraction isolated from Thai durian by solvent extraction and solvent-assisted flavor evaporation resulted in 44 odor-active compounds in the flavor dilution (FD) factor range of 1-16384, 41 of which could be identified and 24 that had not been reported in durian before. High FD factors were found for ethyl (2S)-2-methylbutanoate (fruity; FD 16384), ethyl cinnamate (honey; FD 4096), and 1-(ethylsulfanyl)ethanethiol (roasted onion; FD 1024), followed by 1-(ethyldisulfanyl)-1-(ethylsulfanyl)ethane (sulfury, onion), 2(5)-ethyl-4-hydroxy-5(2)-methylfuran-3(2H)-one (caramel), 3-hydroxy-4,5-dimethylfuran-2(5H)-one (soup seasoning), ethyl 2-methylpropanoate (fruity), ethyl butanoate (fruity), 3-methylbut-2-ene-1-thiol (skunky), ethane-1,1-dithiol (sulfury, durian), 1-(methylsulfanyl)ethanethiol (roasted onion), 1-(ethylsulfanyl)propane-1-thiol (roasted onion), and 4-hydroxy-2,5-dimethylfuran-3(2H)-one (caramel). Among the highly volatile compounds screened by static headspace gas chromatography-olfactometry, hydrogen sulfide (rotten egg), acetaldehyde (fresh, fruity), methanethiol (rotten, cabbage), ethanethiol (rotten, onion), and propane-1-thiol (rotten, durian) were found as additional potent odor-active compounds. Fourteen of the 41 characterized durian odorants showed an alkane-1,1-dithiol, 1-(alkylsulfanyl)alkane-1-thiol, or 1,1-bis(alkylsulfanyl)alkane structure derived from acetaldehyde, propanal, hydrogen sulfide, and alkane-1-thiols. Among these, 1-(propylsulfanyl)ethanethiol, 1-{[1-(methylsulfanyl)ethyl]sulfanyl}ethanethiol, and 1-{[1-(ethylsulfanyl)ethyl]sulfanyl}ethanethiol were reported for the first time in a natural product.

  15. Characterization of the aroma-active compounds in pink guava (Psidium guajava, L.) by application of the aroma extract dilution analysis.

    Science.gov (United States)

    Steinhaus, Martin; Sinuco, Diana; Polster, Johannes; Osorio, Coralia; Schieberle, Peter

    2008-06-11

    The volatiles present in fresh, pink-fleshed Colombian guavas ( Psidium guajava, L.), variety regional rojo, were carefully isolated by solvent extraction followed by solvent-assisted flavor evaporation, and the aroma-active areas in the gas chromatogram were screened by application of the aroma extract dilution analysis. The results of the identification experiments in combination with the FD factors revealed 4-methoxy-2,5-dimethyl-3(2 H)-furanone, 4-hydroxy-2,5-dimethyl-3(2 H)-furanone, 3-sulfanylhexyl acetate, and 3-sulfanyl-1-hexanol followed by 3-hydroxy-4,5-dimethyl-2(5 H)-furanone, ( Z)-3-hexenal, trans-4,5-epoxy-( E)-2-decenal, cinnamyl alcohol, ethyl butanoate, hexanal, methional, and cinnamyl acetate as important aroma contributors. Enantioselective gas chromatography revealed an enantiomeric distribution close to the racemate in 3-sulfanylhexyl acetate as well as in 3-sulfanyl-1-hexanol. In addition, two fruity smelling diastereomeric methyl 2-hydroxy-3-methylpentanoates were identified as the ( R,S)- and the ( S,S)-isomers, whereas the ( S,R)- and ( R,R)-isomers were absent. Seven odorants were identified for the first time in guavas, among them 3-sulfanylhexyl acetate, 3-sulfanyl-1-hexanol, 3-hydroxy-4,5-dimethyl-2(5 H)-furanone, trans-4,5-epoxy-( E)-2-decenal, and methional were the most odor-active.

  16. Analysis of halogenated and priority pesticides at different concentration levels. Automated SPE extraction followed by isotope dilution-GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Planas, C.; Saulo, J.; Rivera, J.; Caixach, J. [Institut Investigacions Quimiques i Ambientals (IIQAB-CSIC), Barcelona (Spain)

    2004-09-15

    In this work, automatic SPE extraction of 16 pesticides and metabolites with the automated Power-Prep trademark system is evaluated at different concentration levels using polymeric (ENV+) and C{sub 18} sorbent phases. The method was optimised by comparing recoveries obtained using different eluting solvents. The optimised procedure was then applied to spiked water samples at concentration levels of 0.1{mu}g/L (quality standard for individual pesticides in drinking water) and 0.02{mu}g/L (close to the detection limit of most pesticides).

  17. Characterization of the key aroma compounds in beef and pork vegetable gravies á la chef by application of the aroma extract dilution analysis.

    Science.gov (United States)

    Christlbauer, Monika; Schieberle, Peter

    2009-10-14

    By application of the aroma extract dilution analysis (AEDA) on an aroma distillate isolated from a freshly prepared, stewed beef/vegetable gravy, 52 odor-active compounds were detected in the flavor dilution (FD) factor range of 4-4096. On the basis of high FD factors in combination with the results of the identification experiments, 3-(methylthio)propanal (cooked potato), 3-mercapto-2-methylpentan-1-ol (gravy-like), (E,E)-2,4-decadienal (deep-fried, fatty), 3-hydroxy-4,5-dimethyl-2(5H)-furanone (lovage-like), vanillin (vanilla-like), (E,E)-2,4-nonadienal (deep-fried), and (E)-2-undecenal (metallic) are suggested as key contributors to the aroma of the gravy. To get an insight into the role of the vegetables as sources of gravy odorants, a beef gravy was prepared without vegetables. The AEDA results revealed that, in particular, onions and leek are important sources of gravy aroma compounds, adding particularly the very potent, gravy-like smelling 3-mercapto-2-methylpentan-1-ol to the overall aroma profile. Further compounds that were clearly derived from the vegetables and, thus, are important modifiers of the overall aroma were 4-vinyl-2-methoxyphenol, (E)-beta-damascenone, beta-ionone, 2-isopropyl-3-methoxypyrazine, and 2-(sec-butyl)-3-methoxypyrazine. Interestingly, none of the key odorants detected in the gravy can be assumed to be formed from a reaction between beef and vegetable constituents. A comparison of the odorants in the beef/vegetable gravy with a gravy prepared according to the same procedure, but substituting beef by pork meat, indicated that most of the aroma compounds were identical-although different in FD factors-but the tallowy smelling 12-methyltridecanal was detected as key odorant only in the beef/vegetable gravy.

  18. Chemical characterization of the aroma of Grenache rosé wines: aroma extract dilution analysis, quantitative determination, and sensory reconstitution studies.

    Science.gov (United States)

    Ferreira, Vicente; Ortín, Natalia; Escudero, Ana; López, Ricardo; Cacho, Juan

    2002-07-03

    The aroma of a Grenache rosé wine from Calatayud (Zaragoza, Spain) has been elucidated following a strategy consisting of an aroma extract dilution analysis (AEDA), followed by the quantitative analysis of the main odorants and the determination of odor activities values (OAVs) and, finally, by a series of reconstitution and omission tests with synthetic aroma models. Thirty-eight aroma compounds were found in the AEDA study, 35 of which were identified. Twenty-one compounds were at concentrations higher than their corresponding odor thresholds. An aroma model prepared by mixing the 24 compounds with OAV > 0.5 in a synthetic wine showed a high qualitative similarity with the aroma of the rosé wine. The addition of compounds with OAV 10 was very different from that of the wine. Omission tests revealed that the most important odorant of this Grenache rosé wine was 3-mercapto-1-hexanol, with a deep impact on the wine fruity and citric notes. The synergic action of Furaneol and homofuraneol also had an important impact on wine aroma, particularly in its fruity and caramel notes. The omission of beta-damascenone, which had the second highest OAV, caused only a slight decrease on the intensity of the aroma model. Still weaker was the sensory effect caused by the omission of 10 other compounds, such as fatty acids and their ethyl esters, isoamyl acetate, and higher alcohols.

  19. Characterization and comparison of key aroma compounds in raw and dry porcini mushroom (Boletus edulis) by aroma extract dilution analysis, quantitation and aroma recombination experiments.

    Science.gov (United States)

    Zhang, Huiying; Pu, Dandan; Sun, Baoguo; Ren, Fazheng; Zhang, Yuyu; Chen, Haitao

    2018-08-30

    A study was carried out to determine and compare the key aroma compounds in raw and dry porcini mushroom (Boletus edulis). The volatile fractions were prepared by solvent-assisted flavor evaporation (SAFE), and aroma extract dilution analysis (AEDA) combined with gas chromatography-mass spectrometry (GC-MS) was employed to identify the odorants. Selected aroma compounds were quantitated and odor activity values (OAVs) were calculated revealing OAVs ≥ 1 for 12 compounds in raw porcini, among which 1-octen-3-one showed the highest OAV. In addition to compounds with eight carbon atoms, 3-methylbutanal, (E,E)-2,4-decadienal and (E,E)-2,4-nonadienal were also responsible for the unique aroma profile. In dry mushroom OAVs ≥ 1 were obtained for 20 odorants. Among them, 3-(methylthio)propanal, 1-octen-3-one and pyrazines were determined as predominant odorants. Overall, drying increased complexity of volatile compounds, thus significantly changing the aroma profile of porcini, providing more desirable roasted and seasoning-like flavor and less grass-like and earthy notes. Copyright © 2018 Elsevier Ltd. All rights reserved.

  20. Comparison of GC-ICP-MS and HPLC-ICP-MS for species-specific isotope dilution analysis of tributyltin in sediment after accelerated solvent extraction

    International Nuclear Information System (INIS)

    Wahlen, Raimund; Wolff-Briche, Celine

    2003-01-01

    This study describes a direct comparison of GC and HPLC hyphenated to ICP-MS determination of tributyltin (TBT) in sediment by species-specific isotope dilution analysis (SS-IDMS). The certified reference sediment PACS-2 (NRC, Canada) and a candidate reference sediment (P-18/HIPA-1) were extracted using an accelerated solvent extraction (ASE) procedure. For comparison of GC and LC methods an older bottle of PACS-2 was used, whilst a fresh bottle was taken for demonstration of the accuracy of the methods. The data obtained show good agreement between both methods for both the PACS-2 sediment (LC-ICP-IDMS 828±87 ng g -1 TBT as Sn, GC-ICP-IDMS 848±39 ng g -1 TBT as Sn) and the P-18/ HIPA-1 sediment (LC-ICP-IDMS 78.0±9.7 ng g -1 TBT as Sn, GC-ICP-IDMS 79.2±3.8 ng g -1 TBT as Sn). The analysis by GC-ICP-IDMS offers a greater signal-to-noise ratio and hence a superior detection limit of 0.03 pg TBT as Sn, in the sediment extracts compared to HPLC-ICP-IDMS (3 pg TBT as Sn). A comparison of the uncertainties associated with both methods indicates superior precision of the GC approach. This is related to the better reproducibility of the peak integration, which affects the isotope ratio measurements used for IDMS. The accuracy of the ASE method combined with HPLC-ICP-IDMS was demonstrated during the international interlaboratory comparison P-18 organised by the Comite Consultatif pour la Quantite de Matiere (CCQM). The results obtained by GC-ICP-IDMS for a newly opened bottle of PACS-2 were 1087±77 ng g -1 Sn for DBT and 876±51 ng g -1 Sn for TBT (expanded uncertainties with a coverage factor of 2), which are in good agreement with the certified values of 1090±150 ng g -1 Sn and 980±130 ng g -1 Sn, respectively. (orig.)

  1. Isotope dilution analysis of environmental samples

    International Nuclear Information System (INIS)

    Tolgyessy, J.; Lesny, J.; Korenova, Z.; Klas, J.; Klehr, E.H.

    1986-01-01

    Isotope dilution analysis has been used for the determination of several trace elements - especially metals - in a variety of environmental samples, including aerosols, water, soils, biological materials and geological materials. Variations of the basic concept include classical IDA, substoichiometric IDA, and more recently, sub-superequivalence IDA. Each variation has its advantages and limitations. A periodic chart has been used to identify those elements which have been measured in environmental samples using one or more of these methods. (author)

  2. ISOTOPE-DILUTION AMMONIA CHEMICAL-IONIZATION MASS FRAGMENTOGRAPHIC ANALYSIS OF URINARY 3-O-METHYLATED CATECHOLAMINE METABOLITES - RAPID SAMPLE CLEANUP BY DERIVATIZATION AND EXTRACTION OF LYOPHILIZED SAMPLES

    NARCIS (Netherlands)

    KEMA, IP; MEIBORG, G; NAGEL, GT; STOB, GJ; MUSKIET, FAJ

    1993-01-01

    We developed a method for simultaneous quantification of the urinary 3-O-methylated catecholamine metabolites 3-methoxytyramine, normetanephrine and metanephrine by stable isotope-dilution ammonia chemical ionization mass fragmentography. Prepurification of lyophilized samples was done by

  3. Characterization of the major aroma-active compounds in mango (Mangifera indica L.) cultivars Haden, White Alfonso, Praya Sowoy, Royal Special, and Malindi by application of a comparative aroma extract dilution analysis.

    Science.gov (United States)

    Munafo, John P; Didzbalis, John; Schnell, Raymond J; Schieberle, Peter; Steinhaus, Martin

    2014-05-21

    The aroma-active compounds present in tree-ripened fruits of the five mango (Mangifera indica L.) cultivars Haden, White Alfonso, Praya Sowoy, Royal Special, and Malindi were isolated by solvent extraction followed by solvent-assisted flavor evaporation (SAFE) and analyzed by gas chromatography-olfactometery (GC-O). Application of a comparative aroma extract dilution analysis (cAEDA) afforded 54 aroma-active compounds in the flavor dilution (FD) factor range from 4 to ≥2048, 16 of which are reported for the first time in mango. The results of the identification experiments in combination with the FD factors revealed 4-hydroxy-2,5-dimethyl-3(2H)-furanone as an important aroma compound in all cultivars analyzed. Twenty-seven aroma-active compounds were present in at least one mango cultivar at an FD factor ≥128. Clear differences in the FD factors of these odorants between each of the mango cultivars suggested that they contributed to the unique sensory profiles of the individual cultivars.

  4. Redox substoichiometry in isotope dilution analysis Pt. 2

    International Nuclear Information System (INIS)

    Kambara, T.; Suzuki, J.; Yoshioka, H.; Nakajima, N.

    1978-01-01

    Isotope dilution analysis using the redox substoichiometric principle has been applied to the determination of antimony content in metallic zinc. As the substoichiometric reaction, the oxidation of trivalent to pentavalent antimony with potassium permanganate was used, followed by separation of these species by the BHPA extraction of trivalent antimony. Determination of antimony contents less than 0.5 μg was found to be possible with good accuracy, without separation of zinc ions. The antimony content in a metallic zinc sample was determined to be 19.7+-0.8 ppm, in good agreement with the results obtained by the other analytical methods. (author)

  5. Redox substoichiometric isotope dilution analysis of metallic arsenic for antimony

    International Nuclear Information System (INIS)

    Kambara, Tomihisa; Yoshioka, Hiroe; Suzuki, Junsuke; Shibata, Yasue.

    1979-01-01

    In 1 M HCl solution Sb(III) reacts with N-benzoyl-N-phenylhydroxylamine (BPHA) to form a complex extractable into chloroform while the extraction of Sb(V) is negligible. The redox substoichiometric isotope dilution analysis based on this reaction was applied to the determination of antimony in metallic arsenic. After the dissolution of metallic arsenic, Sb(V) was separated from As(V) by a tribenzylamine extraction from 8 M HCl solution and the extracted Sb(V) was stripped into 0.5 M NaOH solution. Thereafter, all the Sb(V) were completely reduced to Sb(III) by bubbling SO 2 gas through 3 M HCl solution. As the substoichiometric reaction, the oxidation of Sb(III) to Sb(V) by a substoichiometric amount of potassium dichromate was used, followed by separation of these species by the BPHA extraction of Sb(III). The substoichiometric oxidation of Sb(III) was found to be quantitative over HCl concentration range from 0.8 to 1.2 M. The amount of antimony was determined by isotope dilution analysis using the method of carrier amount variation. By the present method the determination of as small as 0.36 μg antimony was accomplished with a good accuracy (relative error; 5.6%) and also the method was successfully applied to the determination of antimony in arsenic samples containing known amounts of Sb(III) and in metallic arsenic. The present method gives reliable results with the good accuracy and precision. (author)

  6. Molecular analysis of two mouse dilute locus deletion mutations: Spontaneous dilute lethal20J and radiation-induced dilute prenatal lethal Aa2 alleles

    International Nuclear Information System (INIS)

    Strobel, M.C.; Seperack, P.K.; Copeland, N.G.; Jenkins, N.A.

    1990-01-01

    The dilute (d) coat color locus of mouse chromosome 9 has been identified by more than 200 spontaneous and mutagen-induced recessive mutations. With the advent of molecular probes for this locus, the molecular lesion associated with different dilute alleles can be recognized and precisely defined. In this study, two dilute mutations, dilute-lethal20J (dl20J) and dilute prenatal lethal Aa2, have been examined. Using a dilute locus genomic probe in Southern blot analysis, we detected unique restriction fragments in dl20J and Aa2 DNA. Subsequent analysis of these fragments showed that they represented deletion breakpoint fusion fragments. DNA sequence analysis of each mutation-associated deletion breakpoint fusion fragment suggests that both genomic deletions were generated by nonhomologous recombination events. The spontaneous dl20J mutation is caused by an interstitial deletion that removes a single coding exon of the dilute gene. The correlation between this discrete deletion and the expression of all dilute-associated phenotypes in dl20J homozygotes defines the dl20J mutation as a functional null allele of the dilute gene. The radiation-induced Aa2 allele is a multilocus deletion that, by complementation analysis, affects both the dilute locus and the proximal prenatal lethal-3 (pl-3) functional unit. Molecular analysis of the Aa2 deletion breakpoint fusion fragment has provided access to a previously undefined gene proximal to d. Initial characterization of this new gene suggests that it may represent the genetically defined pl-3 functional unit

  7. An Isotopic Dilution Experiment Using Liquid Scintillation: A Simple Two-System, Two-Phase Analysis.

    Science.gov (United States)

    Moehs, Peter J.; Levine, Samuel

    1982-01-01

    A simple isotonic, dilution analysis whose principles apply to methods of more complex radioanalyses is described. Suitable for clinical and instrumental analysis chemistry students, experimental manipulations are kept to a minimum involving only aqueous extraction before counting. Background information, procedures, and results are discussed.…

  8. Research on extraction of lithium from dilute solution

    International Nuclear Information System (INIS)

    Takeuchi, Takeji

    1983-01-01

    Lithium has been used as the refrigerant for air conditioning, the additive for aluminum refining and catalyzer and for high performance grease and small batteries so far. The demand in these existing uses has grown on the average 8.8 % yearly, accordingly the cumulative consumption is estimated to be 0.8 x 10 9 kg by 2000. It is expected that the lithium resources of 1 x 10 9 kg available by 2000 will be used up before the practical use of fusion reactors. Lithium is indispensable for generating tritium in fusion reactors. The lithium concentration in sea water is as thin as 0.2 g/m 3 , therefore it is necessary to develop the method of effectively extracting lithium from a large quantity of sea water. As one of the methods, it was found that the corrosion product of metallic aluminum was able to be utilized. Namely, when metallic aluminum such as foils is immersed in sea water, the corrosion product adheres on the surface, and this corrosion product extracts lithium by cation exchange process preferentially. In this method, the process of making an extracting agent is not necessary, and it is also unnecessary to control the condition of sea water. (Kako, I.)

  9. Determination of traces of iridium with thiodibenzoylmethane by substoichiometric isotope dilution analysis

    International Nuclear Information System (INIS)

    Roebisch, G.; Bansse, W.; Ludwig, E.

    1980-01-01

    Iridium(III or IV) reacts with thiodibenzoylmethane on heating at pH 6 to form a 1:3 complex, which can be concentrated by extraction into chloroform. Based on this reaction, a reproducible, selective determination of iridium is achieved by means of substoichiometric isotope dilution analysis, based on 192 Ir. The linear range is 1-11 nmol of iridium. (Auth.)

  10. A probabilistic analysis of rapid boron dilution scenarios

    International Nuclear Information System (INIS)

    Kohut, P.; Diamond, D.J.

    1993-01-01

    A probabilistic and deterministic analysis of a rapid boron dilution scenario related to reactor restart was performed. The event is initiated by a loss of off-site power during the startup dilution process. The automatic restart of the charging pump in such cases may lead to the accumulation of a diluted slug of water in the lower plenum. The restart of the reactor coolant pumps may send the diluted slug through the core, adding sufficient reactivity to overcome the shutdown margin and cause a power excursion. The concern is that the power excursion is sufficient in certain circumstances to cause fuel damage. The estimated core damage frequency based on the scoping analysis is 1.0--3.0E-05/yr for the plants analyzed. These are relatively significant values when compared to desirable goals. The analysis contained assumptions related to plant specific design characteristics which may lead to non-conservative estimates. The most important conservative assumptions were that mixing of the injected diluted water is insignificant and that fuel damage occurs when the slug passes through the core

  11. Evaluation of method for phthalate extraction from milk related to milk dilution ratio

    Directory of Open Access Journals (Sweden)

    Milojković Danica S.

    2015-01-01

    Full Text Available Liquid-liquid extraction techniques were compared coupled with gas chromatography-mass spectrometry (GC-MS, for the extraction and the determination of four phthalates: dimethyl phthalate (DMP, di-n-butyl phthalate (DBP, benzyl butyl phthalate (BBP and di-(2-ethylhexyl phthalate (DEHP in six different kinds of milk-based samples. Extraction factors: sample preparation, organic solvent type and volume, salt effect, agitation and the extraction time were optimized. The ion of base peaks (m/z 149 for DBP, BBP and DEHP and m/z 163 for DMP for investigated phthalates were selected for the screening studies. The acquisition was performed at the selected ion monitoring mode. The MSD response for GC-MS phthalate calibration standards was linear between 0.25 and 2.50 μg mL-1 with calculated LODs between 0.01 μg mL-1 to 0.04 μg mL-1 and LOQs of 0.05 μg mL-1 to 0.12 μg mL-1, while repeatability was between 1.7 % to 4.9 % RSD. The study demonstrated an increase of the recovery of less polar phthalates in matrix milk standards by matrix dilution. Recovery for hydrophilic phthalates, like DMP, was not changed by matrix dilution and it was continuously low for the investigated method. Two spiking levels were tested for influence of matrix dilution on phthalate recovery, showed the same trend. [Projekat Ministarstva nauke Republike Srbije, br. 31060

  12. 1H NMR quantification in very dilute toxin solutions: application to anatoxin-a analysis.

    Science.gov (United States)

    Dagnino, Denise; Schripsema, Jan

    2005-08-01

    A complete procedure is described for the extraction, detection and quantification of anatoxin-a in biological samples. Anatoxin-a is extracted from biomass by a routine acid base extraction. The extract is analysed by GC-MS, without the need of derivatization, with a detection limit of 0.5 ng. A method was developed for the accurate quantification of anatoxin-a in the standard solution to be used for the calibration of the GC analysis. 1H NMR allowed the accurate quantification of microgram quantities of anatoxin-a. The accurate quantification of compounds in standard solutions is rarely discussed, but for compounds like anatoxin-a (toxins with prices in the range of a million dollar a gram), of which generally only milligram quantities or less are available, this factor in the quantitative analysis is certainly not trivial. The method that was developed can easily be adapted for the accurate quantification of other toxins in very dilute solutions.

  13. Direct quantification of creatinine in human urine by using isotope dilution extractive electrospray ionization tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li Xue [Institute of Environmental Pollution and Health, School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, Applied Chemistry Department, East China Institute of Technology, Nanchang 330013 (China); Fang Xiaowei [Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, Applied Chemistry Department, East China Institute of Technology, Nanchang 330013 (China); Yu Zhiqiang; Sheng Guoying [Guangdong Key Laboratory of Environmental Protection and Resource Utilization, State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Wu Minghong [Shanghai Applied Radiation Institute, School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Fu Jiamo [Institute of Environmental Pollution and Health, School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Guangdong Key Laboratory of Environmental Protection and Resource Utilization, State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou 510640 (China); Chen Huanwen, E-mail: chw8868@gmail.com [Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, Applied Chemistry Department, East China Institute of Technology, Nanchang 330013 (China)

    2012-10-20

    Highlights: Black-Right-Pointing-Pointer High throughput analysis of urinary creatinine is achieved by using ID-EESI-MS/MS. Black-Right-Pointing-Pointer Urine sample is directly analyzed and no sample pre-treatment is required. Black-Right-Pointing-Pointer Accurate quantification is accomplished with isotope dilution technique. - Abstract: Urinary creatinine (CRE) is an important biomarker of renal function. Fast and accurate quantification of CRE in human urine is required by clinical research. By using isotope dilution extractive electrospray ionization tandem mass spectrometry (EESI-MS/MS) a high throughput method for direct and accurate quantification of urinary CRE was developed in this study. Under optimized conditions, the method detection limit was lower than 50 {mu}g L{sup -1}. Over the concentration range investigated (0.05-10 mg L{sup -1}), the calibration curve was obtained with satisfactory linearity (R{sup 2} = 0.9861), and the relative standard deviation (RSD) values for CRE and isotope-labeled CRE (CRE-d3) were 7.1-11.8% (n = 6) and 4.1-11.3% (n = 6), respectively. The isotope dilution EESI-MS/MS method was validated by analyzing six human urine samples, and the results were comparable with the conventional spectrophotometric method (based on the Jaffe reaction). Recoveries for individual urine samples were 85-111% and less than 0.3 min was taken for each measurement, indicating that the present isotope dilution EESI-MS/MS method is a promising strategy for the fast and accurate quantification of urinary CRE in clinical laboratories.

  14. Direct quantification of creatinine in human urine by using isotope dilution extractive electrospray ionization tandem mass spectrometry

    International Nuclear Information System (INIS)

    Li Xue; Fang Xiaowei; Yu Zhiqiang; Sheng Guoying; Wu Minghong; Fu Jiamo; Chen Huanwen

    2012-01-01

    Highlights: ► High throughput analysis of urinary creatinine is achieved by using ID-EESI–MS/MS. ► Urine sample is directly analyzed and no sample pre-treatment is required. ► Accurate quantification is accomplished with isotope dilution technique. - Abstract: Urinary creatinine (CRE) is an important biomarker of renal function. Fast and accurate quantification of CRE in human urine is required by clinical research. By using isotope dilution extractive electrospray ionization tandem mass spectrometry (EESI–MS/MS) a high throughput method for direct and accurate quantification of urinary CRE was developed in this study. Under optimized conditions, the method detection limit was lower than 50 μg L −1 . Over the concentration range investigated (0.05–10 mg L −1 ), the calibration curve was obtained with satisfactory linearity (R 2 = 0.9861), and the relative standard deviation (RSD) values for CRE and isotope-labeled CRE (CRE-d3) were 7.1–11.8% (n = 6) and 4.1–11.3% (n = 6), respectively. The isotope dilution EESI–MS/MS method was validated by analyzing six human urine samples, and the results were comparable with the conventional spectrophotometric method (based on the Jaffe reaction). Recoveries for individual urine samples were 85–111% and less than 0.3 min was taken for each measurement, indicating that the present isotope dilution EESI–MS/MS method is a promising strategy for the fast and accurate quantification of urinary CRE in clinical laboratories.

  15. Hot vacuum extraction-isotopic dilution mass spectrometry for determination of hydrogen isotopes in zircaloys

    International Nuclear Information System (INIS)

    Shi, Y.; Leeson, P.K.; Wilkin, D.; Britton, A.; Macleod, R.

    2016-01-01

    A hot vacuum extraction-isotope dilution mass spectrometry (HVE-IDMS) was studied for determination of hydrogen isotopes in zirconium metal and alloys as nuclear reactor materials. A theoretical assessment of the completeness of the extraction of hydrogen isotopes under the chosen condition was carried out based on the hydrogen and deuterium solubility data for zirconium. The optimal isotopic spiking condition for conventional IDMS was further explored for the special case IDMS where the isotope abundance of the samples is varied and non-natural. Applying the optimal conditions, the accurate IDMS determination was realized. The agreement between the measured values and the certified or prepared values of standard reference materials and homemade standard materials validate the method developed. (author)

  16. Towards integrated biorefinery from dried distillers grains: Selective extraction of pentoses using dilute acid hydrolysis

    International Nuclear Information System (INIS)

    Fonseca, Dania A.; Lupitskyy, Robert; Timmons, David; Gupta, Mayank; Satyavolu, Jagannadh

    2014-01-01

    The abundant availability and high level of hemicellulose content make dried distillers grains (DDG) an attractive feedstock for production of pentoses (C5) and conversion of C5 to bioproducts. One target of this work was to produce a C5 extract (hydrolyzate) with high yield and purity with a low concentration of C5 degradation products. A high selectivity towards pentoses was achieved using dilute acid hydrolysis of DDG in a percolation reactor with liquid recirculation. Pretreatment of starting material using screening and ultrasonication resulted in fractional increase of the pentose yield by 42%. A 94% yield of pentoses on the DDG (280.9 g kg −1 ) was obtained. Selective extraction of individual pentoses has been achieved by using a 2-stage hydrolysis process, resulting in arabinose-rich (arabinose 81.5%) and xylose-rich (xylose 85.2%) streams. A broader impact of this work is towards an Integrated Bio-Refinery based on DDG – for production of biofuels, biochemical intermediates, and other bioproducts. - Highlights: • A process for selective extraction of pentoses from DDG was presented as a part of integrated biorefinery approach. • The selectivity for pentoses was high using dilute acid hydrolysis in a percolation reactor with liquid recirculation. • Pretreatment of DDG using screening and ultrasonication resulted in fractional increase of the pentose yield by 42 %. • A 94% yield in pentoses (280.9 g kg −1 of DDG) was obtained. • A 2-stage hydrolysis process, developed to extract individual pentoses, resulted in arabinose and xylose rich streams

  17. Redox substoichiometry in isotope dilution analysis Pt. 4

    International Nuclear Information System (INIS)

    Kambara, T.; Yoshioka, H.; Ugai, Y.

    1980-01-01

    The oxidation reaction of antimony(III) with potassium dichromate has been investigated radiometrically. The quantitative oxidation of antimony(III) was found to be not disturbed even in large amounts of tin(IV). On the basis of these results the redox substoichiometric isotope dilution analysis using potassium dichromate as the oxidizing agent was proposed for the determination of antimony in metallic tin. An antimony content of 1.22+-0.05 μg in metallic tin (10 mg) was determined without separation of the matrix element. (author)

  18. Transient Thermo-Mechanical Analysis of the TPSG4 Beam Diluter

    CERN Document Server

    Goddard, B; Herrera-Martínez, A; Kadi, Y; Marque, S

    2002-01-01

    A new extraction channel is being built in the Super Proton Synchrotron (SPS) Long Straight Section 4 (LSS4) to transfer proton beams to the Large Hadron Collider (LHC) and also to the CERN Neutrino to Gran Sasso (CNGS) target. The beam is extracted in a fast mode during a single turn. For this purpose a protection of the MSE copper septum coil, in the form of a beam diluting element placed upstream, will be required to cope with the new failure modes associated with the fast extraction operation. The present analysis focuses on the thermo-mechanical behavior of the proposed TPSG4 diluter element irradiated by a fast extracted beam (up to 4.9 x 10^13 protons per 7.2 mus pulse) from the SPS. The deposited energy densities, estimated from primary and secondary particle simulations using the high-energy particle transport code FLUKA, were converted to internal heat generation rates taken as a thermal load input for the finite-element engineering analyses code ANSYS. According to the time dependence of the extrac...

  19. Dilute alkali and hydrogen peroxide treatment of microwave liquefied rape straw residue for the extraction of cellulose nanocrystals

    Science.gov (United States)

    Xingyan Huang; Cornelis F. De Hoop; Feng Li; Jiulong Xie; Chung-Yun Hse; Jinqiu Qi; Yongze Jiang; Yuzhu Chen

    2017-01-01

    Microwave-assisted liquefaction of rape straw in methanol was conducted to collect the liquefied residues for the extraction of cellulose nanocrystals (CNCs).The liquefied residue with content of 23.44% from 180∘C/7.5 min was used to fibrillate CNCs with dilute alkali (2% NaOH) and hydrogen peroxide (5% H2O2...

  20. Paradigms in isotope dilution mass spectrometry for elemental speciation analysis

    International Nuclear Information System (INIS)

    Meija, Juris; Mester, Zoltan

    2008-01-01

    Isotope dilution mass spectrometry currently stands out as the method providing results with unchallenged precision and accuracy in elemental speciation. However, recent history of isotope dilution mass spectrometry has shown that the extent to which this primary ratio measurement method can deliver accurate results is still subject of active research. In this review, we will summarize the fundamental prerequisites behind isotope dilution mass spectrometry and discuss their practical limits of validity and effects on the accuracy of the obtained results. This review is not to be viewed as a critique of isotope dilution; rather its purpose is to highlight the lesser studied aspects that will ensure and elevate current supremacy of the results obtained from this method

  1. Dilution and Mixing in transient velocity fields: a first-order analysis

    Science.gov (United States)

    Di Dato, Mariaines; de Barros, Felipe, P. J.; Fiori, Aldo; Bellin, Alberto

    2017-04-01

    An appealing remediation technique is in situ oxidation, which effectiveness is hampered by difficulties in obtaining good mixing of the injected oxidant with the contaminant, particularly when the contaminant plume is contained and therefore its deformation is physically constrained. Under such conditions (i.e. containment), mixing may be augmented by inducing temporal fluctuations of the velocity field. The temporal variability of the flow field may increase the deformation of the plume such that diffusive mass flux becomes more effective. A transient periodic velocity field can be obtained by an engineered sequence of injections and extractions from wells, which may serve also as a hydraulic barrier to confine the plume. Assessing the effectiveness of periodic flows to maximize solute mixing is a difficult task given the need to use a 3D setup and the large number of possible flow configurations that should be analyzed in order to identify the optimal one. This is the typical situation in which analytical solutions, though approximated, may assist modelers in screening possible alternative flow configurations such that solute dilution is maximized. To quantify dilution (i.e. a precondition that enables reactive mixing) we utilize the concept of the dilution index [1]. In this presentation, the periodic flow takes place in an aquifer with spatially variable hydraulic conductivity field which is modeled as a Stationary Spatial Random Function. We developed a novel first-order analytical solution of the dilution index under the hypothesis that the flow can be approximated as a sequence of steady state configurations with the mean velocity changing with time in intensity and direction. This is equivalent to assume that the characteristic time of the transient behavior is small compared to the period characterizing the change in time of the mean velocity. A few closed paths have been analyzed quantifying their effectiveness in enhancing dilution and thereby mixing

  2. Recovery of Cu(II from diluted aqueous solutions by non-dispersive solvent extraction

    Directory of Open Access Journals (Sweden)

    Alguacil, E. J.

    2002-08-01

    Full Text Available The removal of copper from diluted aqueous solutions with ACORGA M5640 extractant using non-dispersive solvent extraction technology was studied. It was possible to remove Cu(II below the international standars from solutions having initially as low concentration as 0,01 g/l under various experimental conditions, i.e aqueous pH 4.0, 10 % v/v ACORGA M5640 in Exxol D100, an organic flow of 100 ml/min, and an aqueous flow 50ml/min. Since the removal occurs by chelating ion exchange between copper from solution and protons from the extractant, the former was stripped by using a 180 g/l sulphuric acid solution which flowed (50 ml/min through the tube side organic was passed (400 ml/min through the shell side of the fibers of the module

    Se estudia la eliminación del cobre presente en disoluciones acuosas diluidas empleando el agente de extracción ACORGA M5640 y la tecnología de extracción con disolventes no dispersiva. Bajo las condiciones experimentales estudiadas, pH de la fase acuosa 4,0 ±0,1, 10 % v/v ACORGA M5640 en Exxsol D100, flujo de la fase orgánica 100 ml/min, flujo de la fase acuosa 50 ml/min, es posible eliminar el Cu(II, por debajo de los límites marcados internacionalmente, en disoluciones con un contenido tan bajo como 0,01 g/1 del metal. Debido a que la extracción transcurre mediante un intercambio catiónico (y formación de un compuesto tipo quelato entre el cobre presente en el medio acuoso y los protones del agente de extracción, el metal se puede reextraer mediante la utilización de una disolución de 180 g/1 de ácido sulfúrico que fluye (50 ml/min a través de la parte interior de las fibras del módulo, mientras que la fase orgánica fluye (400 ml/min por la parte exterior de las mismas fibras.

  3. Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material

    International Nuclear Information System (INIS)

    Hernandez, C.; Fernandez, M.; Quejido, A. L.

    2006-01-01

    Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound esposure time. Due to the complex matrix of this fly ash material, a two-steps purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs

  4. Study of the extraction of the traces of Cadmium through the method of subestequiometric isotope dilution

    International Nuclear Information System (INIS)

    Garate V, Z.

    1990-01-01

    In this work, it has been used the method of subestequiometric isotope dilution for the determination of traces of cadmium and it has been compared with other conventional's methods for study its performance. The conditions of the experiment had been studied carefully in order to optimize the parameters such as pH, (8,0 - 10,1) it used the buffer NH 3 :NH 4 Cl, the time of agitation (>120 s) and the concentration of the organic reactive (dithizone). Besides, it obtains the respective curve of calibration. In this study, we can watch a line relation in all the range studied (5-40 μg of Cd). This method applied to the analysis of Cadmium in a certified sample of H-8 of the IAEA, it gives us the next value: 195 ± 5,4 ppm (LOD= 1,5 ppm, LOQ= 4,8 ppm), it is enough satisfactory in comparison with the certified middle value of 188,9±19 ppm. It demonstrates the utility of the method in the Cadmium traces analysis if it disposes of the radioisotope of this element and the appropriate detection equipment. (DEM). 34 refs., 15 tabs., 7 figs

  5. Analysis of boron dilution in a four-loop PWR

    International Nuclear Information System (INIS)

    Sun, J.G.; Sha, W.T.

    1995-03-01

    Thermal mixing and boron dilution in a pressurized water reactor were analyzed with COMMIX codes. The reactor system was the four-loop Zion reactor. Two boron dilution scenarios were analyzed. In the first scenario, the plant is in cold shutdown and the reactor coolant system has just been filled after maintenance on the steam generators. To flush the air out of the steam generator tubes, a reactor coolant pump (RCP) is started, with the water in the pump suction line devoid of boron and at the same temperature as the coolant in the system. In the second scenario, the plant is at hot standby and the reactor coolant system has been heated to operating temperature after a long outage. It is assumed that an RCP is started, with the pump suction line filled with cold unborated water, forcing a slug of diluted coolant down the downcomer and subsequently through the reactor core. The subsequent transient thermal mixing and boron dilution that would occur in the reactor system is simulated for these two scenarios. The reactivity insertion rate and the total reactivity are evaluated and a sensitivity study is performed to assess the accuracy of the numerical modeling of the geometry of the reactor coolant system

  6. Analysis of ochratoxin A in grapes, musts and wines by LC–MS/MS: First comparison of stable isotope dilution assay and diastereomeric dilution assay methods

    Energy Technology Data Exchange (ETDEWEB)

    Roland, Aurélie, E-mail: aurelie@nyseos.fr [Nyseos, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Bros, Pauline, E-mail: pauline.bros@gmail.com [Institut Français de la Vigne et du Vin, UMT Qualinnov, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Bouisseau, Anaïs, E-mail: anais.bouisseau@gmail.com [Nyseos, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Institut des Biomolécules Max Mousseron, UMR-CNRS-5247, Universités Montpellier I and II, Place Eugène Bataillon, 34095 Montpellier (France); Cavelier, Florine, E-mail: florine@univ-montp2.fr [Institut des Biomolécules Max Mousseron, UMR-CNRS-5247, Universités Montpellier I and II, Place Eugène Bataillon, 34095 Montpellier (France); Schneider, Rémi, E-mail: remi.schneider@vignevin.com [Institut Français de la Vigne et du Vin, UMT Qualinnov, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France)

    2014-03-01

    Highlights: • OTA extraction on immunoaffinity columns is not adapted for DIDA quantification. • The use of a labeled internal standard is compulsory to obtain reliable results. • SIDA and DIDA quantification approaches have been compared for the first time. Abstract: Ochratoxin A (OTA) exhibits potent nephrotoxic, carcinogenic and teratogenic effects and its maximum level in wines has been set to 2 μg L⁻¹ by regulation. Consequently, the analytical procedures for OTA determination in wines have to be both very sensitive and reliable. In this paper, we compared two quantification methods: the stable isotope dilution assay (SIDA) and the diastereomeric dilution assay (DIDA). For this purpose, non-natural analogues of OTA were synthesized: the labeled OTA (OTA-d₄) as a diastereomeric mixture for the SIDA and one non-natural OTA’s diastereomer (OTA-dia) for the DIDA. To quantify OTA in red grapes, musts or wines, the sample preparation was optimized using immunoaffinity column extraction and the analysis was performed by LC–MS/MS in Multiple Reaction Monitoring mode. A validation procedure in agreement with the International Organization of Vine and Wine recommendations was conducted. It appeared that SIDA quantification exhibited excellent sensitivity (LOD < 1 ng L⁻¹), accuracy (recovery = 98%), repeatability (RSD < 3%) and intermediate reproducibility (RSD < 4%) compared to quantification by DIDA. Indeed, DIDA method did not provide satisfactory results demonstrating that immunoaffinity extraction is exclusively selective for the natural OTA and not for its diastereomer, which therefore cannot be considered as a good internal standard for this particular method.

  7. Analysis of ochratoxin A in grapes, musts and wines by LC–MS/MS: First comparison of stable isotope dilution assay and diastereomeric dilution assay methods

    International Nuclear Information System (INIS)

    Roland, Aurélie; Bros, Pauline; Bouisseau, Anaïs; Cavelier, Florine; Schneider, Rémi

    2014-01-01

    Highlights: • OTA extraction on immunoaffinity columns is not adapted for DIDA quantification. • The use of a labeled internal standard is compulsory to obtain reliable results. • SIDA and DIDA quantification approaches have been compared for the first time. - Abstract: Ochratoxin A (OTA) exhibits potent nephrotoxic, carcinogenic and teratogenic effects and its maximum level in wines has been set to 2 μg L −1 by regulation. Consequently, the analytical procedures for OTA determination in wines have to be both very sensitive and reliable. In this paper, we compared two quantification methods: the stable isotope dilution assay (SIDA) and the diastereomeric dilution assay (DIDA). For this purpose, non-natural analogues of OTA were synthesized: the labeled OTA (OTA-d 4 ) as a diastereomeric mixture for the SIDA and one non-natural OTA’s diastereomer (OTA-dia) for the DIDA. To quantify OTA in red grapes, musts or wines, the sample preparation was optimized using immunoaffinity column extraction and the analysis was performed by LC–MS/MS in Multiple Reaction Monitoring mode. A validation procedure in agreement with the International Organization of Vine and Wine recommendations was conducted. It appeared that SIDA quantification exhibited excellent sensitivity (LOD −1 ), accuracy (recovery = 98%), repeatability (RSD < 3%) and intermediate reproducibility (RSD < 4%) compared to quantification by DIDA. Indeed, DIDA method did not provide satisfactory results demonstrating that immunoaffinity extraction is exclusively selective for the natural OTA and not for its diastereomer, which therefore cannot be considered as a good internal standard for this particular method

  8. Effects of diluting medium and holding time on sperm motility analysis by CASA in ram

    Directory of Open Access Journals (Sweden)

    Somayeh Mostafapor

    2014-06-01

    Full Text Available The aim of this study was to evaluate the effects of dilution rate and holding time on various motility parameters using computer-assisted sperm analysis (CASA. The semen samples were collected from three Ghezel rams. Samples were diluted in seminal plasma (SP, phosphate-buffered saline (PBS containing 1% bovine serum albumin (BSA and Bioexcell. The motility parameters that computed and recorded by CASA include curvilinear velocity (VCL, straight line velocity (VSL, average path velocity (VAP, straightness (STR, linearity (LIN, amplitude of lateral head displacement (ALH, and beat cross frequency (BCF. In all diluters, there was a decrease in the average of all three parameters of sperms movement velocity as the time passed, but density of this decrease was more intensive in SP. The average of ALH between diluters indicated a significant difference, as it was more in Bioexcell in comparison with the similar amount in SP and PBS. The average of LIN in the diluted sperms in Bioexcell was less than two other diluters in all three times. The motility parameters of the diluted sperms in Bioexcell and PBS indicated an important and considerable difference with the diluted sperms in SP. According to the gained results, the Bioexcell has greater ability in preserving motility of sperm in comparison with the other diluters but as SP is considered as physiological environment for sperm. It seems that the evaluation of the motility parameters in Bioexcell and PBS cannot be an accurate and comparable evaluation with SP.

  9. Effects of diluting medium and holding time on sperm motility analysis by CASA in ram.

    Science.gov (United States)

    Mostafapor, Somayeh; Farrokhi Ardebili, Farhad

    2014-01-01

    The aim of this study was to evaluate the effects of dilution rate and holding time on various motility parameters using computer-assisted sperm analysis (CASA). The semen samples were collected from three Ghezel rams. Samples were diluted in seminal plasma (SP), phosphate-buffered saline (PBS) containing 1% bovine serum albumin (BSA) and Bioexcell. The motility parameters that computed and recorded by CASA include curvilinear velocity (VCL), straight line velocity (VSL), average path velocity (VAP), straightness (STR), linearity (LIN), amplitude of lateral head displacement (ALH), and beat cross frequency (BCF). In all diluters, there was a decrease in the average of all three parameters of sperms movement velocity as the time passed, but density of this decrease was more intensive in SP. The average of ALH between diluters indicated a significant difference, as it was more in Bioexcell in comparison with the similar amount in SP and PBS. The average of LIN in the diluted sperms in Bioexcell was less than two other diluters in all three times. The motility parameters of the diluted sperms in Bioexcell and PBS indicated an important and considerable difference with the diluted sperms in SP. According to the gained results, the Bioexcell has greater ability in preserving motility of sperm in comparison with the other diluters but as SP is considered as physiological environment for sperm. It seems that the evaluation of the motility parameters in Bioexcell and PBS cannot be an accurate and comparable evaluation with SP.

  10. A comparative study on the skin penetration of pure tryptanthrin and tryptanthrin in Isatis tinctoria extract by dermal microdialysis coupled with isotope dilution ESI-LC-MS.

    Science.gov (United States)

    Oberthür, Christine; Heinemann, Christian; Elsner, Peter; Benfeldt, Eva; Hamburger, Matthias

    2003-05-01

    The indolo[2,1- b]quinazoline alkaloid tryptanthrin has recently been identified as a pharmacologically active compound in Isatis tinctoria, with potent dual inhibitory activity on prostaglandin and leukotriene synthesis. To investigate the skin penetration of tryptanthrin from solutions of pure compound and Isatis extracts, we developed and validated a cutaneous microdialysis model using ex vivo pig foreleg. Microdialysis was performed by placing linear probes in the dermis of the skin in situ, and tryptanthrin concentrations in the dialysates were determined by isotope dilution electrospray ionization LC-MS in the selected ion mode. Measurable concentrations of tryptanthrin were detected 30 min after application. A dose-dependent increase in tryptanthrin concentrations in the dialysate was observed for the Isatis extracts, but not for pure tryptanthrin. Microscopic analysis showed that the pure compound crystallized from the solution but remained in an amorphous state in the extracts.

  11. Double spike isotope dilution GC-ICP-MS for evaluation of mercury species transformation in real fish samples using ultrasound-assisted extraction.

    Science.gov (United States)

    Esteban-Fernández, Diego; Mirat, Manuela; de la Hinojosa, M Ignacia Martín; Alonso, J Ignacio García

    2012-08-29

    Sample preparation continues being a key factor to obtain fast and reliable quantification of Hg species. Assisted procedures enhance the efficiency and reduce the extraction time; however, collateral species transformations have been observed. Moreover, differential interconversions have been observed even between similar matrixes, which introduce an important uncertainty for real sample analysis. Trying to minimize Hg species transformations, we have tested a soft ultrasound-assisted extraction procedure. Species quantification and transformations have been evaluated using double spike isotope dilution analysis (IDA) together with gas chromatography inductively coupled plasma mass spectrometry (GC-ICP-MS) for a CRM material (Tort-2) and shark and swordfish muscle samples. Optimum extraction solution and sonication time led to quantitative extraction and accurate determination of MeHg and IHg in a short time, although different behaviors regarding species preservation were observed depending on the sample. Negligible species transformations were observed in the analysis of the CRM, while a small but significant demethylation factor was observed in the case of real samples. In comparison with other extraction procedures, species transformations became smaller, and fewer differences between fish species were found. Similar results were obtained for fresh and lyophilized samples of both fish samples, which permit one to analyze the fresh sample directly and save time in the sample preparation step. The high grade of species preservation and the affordability of the extraction procedure allow one to obtain accurate determinations even for routine laboratories using quantification techniques, which do not estimate species transformations.

  12. Just add water: Accuracy of analysis of diluted human milk samples using mid-infrared spectroscopy.

    Science.gov (United States)

    Smith, R W; Adamkin, D H; Farris, A; Radmacher, P G

    2017-01-01

    To determine the maximum dilution of human milk (HM) that yields reliable results for protein, fat and lactose when analyzed by mid-infrared spectroscopy. De-identified samples of frozen HM were obtained. Milk was thawed and warmed (40°C) prior to analysis. Undiluted (native) HM was analyzed by mid-infrared spectroscopy for macronutrient composition: total protein (P), fat (F), carbohydrate (C); Energy (E) was calculated from the macronutrient results. Subsequent analyses were done with 1 : 2, 1 : 3, 1 : 5 and 1 : 10 dilutions of each sample with distilled water. Additional samples were sent to a certified lab for external validation. Quantitatively, F and P showed statistically significant but clinically non-critical differences in 1 : 2 and 1 : 3 dilutions. Differences at higher dilutions were statistically significant and deviated from native values enough to render those dilutions unreliable. External validation studies also showed statistically significant but clinically unimportant differences at 1 : 2 and 1 : 3 dilutions. The Calais Human Milk Analyzer can be used with HM samples diluted 1 : 2 and 1 : 3 and return results within 5% of values from undiluted HM. At a 1 : 5 or 1 : 10 dilution, however, results vary as much as 10%, especially with P and F. At the 1 : 2 and 1 : 3 dilutions these differences appear to be insignificant in the context of nutritional management. However, the accuracy and reliability of the 1 : 5 and 1 : 10 dilutions are questionable.

  13. Nutritional assessment by isotope dilution analysis of body composition

    International Nuclear Information System (INIS)

    Szeluga, D.J.; Stuart, R.K.; Utermohlen, V.; Santos, G.W.

    1984-01-01

    The three components of body mass, body cell mass (BCM), extracellular fluid (ECF), and fat + extracellular solids (ECS: bone, tendon, etc) can be quantified using established isotope dilution techniques. With these techniques, total body water (TBW) and ECF are measured using 3H 2 O and 82 Bromine, respectively, as tracers. BCM is calculated from intracellular fluid (ICF) where ICF . TBW - ECF. Fat + ECS is estimated as: body weight - (BCM + ECF). TBW and ECF can be determined by either of two calculation methods, one requiring several timed plasma samples (extrapolation method) and one requiring a single plasma sample and a 4-h urine collection (urine-corrected method). The comparability of the two calculation methods was evaluated in 20 studies in 12 bone marrow transplant recipients. We found that for determination of TBW and ECF there was a very strong linear relationship (r2 greater than 0.98) between the calculation methods. Further comparisons (by t test, 2-sided) indicated that for the determination of ECF, the methods were not significantly (p greater than 0.90) different; however, TBW determined by the urine-corrected method was slightly (0.1 to 6%), but significantly (p less than 0.01) greater than that determined by the extrapolation method. Therefore, relative to the extrapolation method, the urine-corrected method ''over-estimates'' BCM and ''under-estimates'' fat + ECS since determination of these compartment sizes depends on measurement of TBW. We currently use serial isotope dilution studies to monitor the body composition changes of patients receiving therapeutic nutritional support

  14. Isotope dilution analysis for the determination of zinc in blood samples of diabetic patients

    International Nuclear Information System (INIS)

    Garg, A.N.; Kumar, A.; Maheshwari, G.; Sharma, S.

    2005-01-01

    Isotope dilution analysis (IDA) based on solvent extraction has been developed for the determination of zinc in the blood of diabetic patients and healthy adults as controls. The method using 65 Zn as a tracer is based on the formation of a red colored complex with dithizone in chloroform which is measured by counting of the 1115 keV γ-rays by gamma-ray spectrometry. Various extraction parameters such as pH, nature of solvent and amount of reagent were optimized. Zinc concentration in diabetic patients (n = 10) was found in a much wider range (1.5-157 μg/ml) compared to those in healthy adults (3.1-95.9 μg/ml for n = 5). t-Test of data shows 80-90% confidence limits. A comparison of mean values, 28.5 ± 48.5 μg/ml for diabetics and 33.1 ± 34.5 μg/ml for controls shows 13.9% lower zinc concentration in diabetics. No correlation was found with eating (vegetarian/nonvegetarian)/drinking or smoking habits, but in general, females showed somewhat lower concentration compared to those in males though population size in each case was very small. (author)

  15. Dynamic structural analysis of the TPSG4 & TPSG6 beam diluters

    CERN Document Server

    Massidda, L; Kadi, Y; Balhan, B

    2005-01-01

    In this report we present the technical specification for the numerical model and the study of the dynamic structural behaviour of the beam diluter elements (TPSG4 & 6) protecting the extraction septum magnets (MSE & MST) in the event of an asynchronous firing of the extraction kickers (MKE). The deposited energy densities, estimated by the high-energy particle transport code FLUKA, were converted to internal heat generation rates according to the time dependence of the extracted beam. The transient response to this thermal load was obtained by solving the power deposition and structural deformation problem by the spectral-element code ELSE.

  16. Solvent extraction of silver(I) from dilute cyanide solutions with 2,4-dihydroxyacetophenone thiosemicarbazone

    International Nuclear Information System (INIS)

    Reddy, A.V.; Reddy, Y.K.; Reddy, G.S.

    1986-01-01

    The solvent extraction of silver(I) was carried out in 0.5M nitric acid in the presence of cyanide by 2,4-dihydroxyacetophenone thiosemicarbazone (DATS). Ethyl acetate was used as a solvent and quantitative recovery was possible with 12.5-fold excess of the reagent in a single extraction. In this medium silver(I) forms a 2:2 complex (metal:ligand) with DATS. The effect of diverse ions on the extraction of silver(I) was investigated. (author)

  17. Extraction of indium from extremely diluted solutions; Gewinnung von Indium aus extrem verduennten Loesungen

    Energy Technology Data Exchange (ETDEWEB)

    Vostal, Radek; Singliar, Ute; Froehlich, Peter [TU Bergakademie Freiberg (Germany). Inst. fuer Technische Chemie

    2017-02-15

    The demand for indium is rising with the growth of the electronics industry, where it is mainly used. Therefore, a multistage extraction process was developed to separate indium from a model solution whose composition was adequate to sphalerite ore. The initially very low concentration of indium in the solution was significantly increased by several successive extraction and reextraction steps. The process described is characterized by a low requirement for chemicals and a high purity of the obtained indium oxide.

  18. Evaluation of xylitol production using corncob hemicellulosic hydrolysate by combining tetrabutylammonium hydroxide extraction with dilute acid hydrolysis.

    Science.gov (United States)

    Jia, Honghua; Shao, Tingting; Zhong, Chao; Li, Hengxiang; Jiang, Min; Zhou, Hua; Wei, Ping

    2016-10-20

    In this paper, we produced hemicellulosic hydrolysate from corncob by tetrabutylammonium hydroxide (TBAH) extraction and dilute acid hydrolysis combined, further evaluating the feasibility of the resultant corncob hemicellulosic hydrolysate used in xylitol production by Candida tropicalis. Optimized conditions for corncob hemicellulose extraction by TBAH was obtained via response surface methodology: time of 90min, temperature of 60°C, liquid/solid ratio of 12 (v/w), and TBAH concentration of 55%, resulting in a hemicellulose extraction of 80.07% under these conditions. The FT-IR spectrum of the extracted corncob hemicellulose is consistent with that of birchwood hemicellulose and exhibits specific absorbance of hemicelluloses at 1380, 1168, 1050, and 900cm(-1). In addition, we found that C. tropicalis can ferment the resulting corncob hemicellulosic hydrolysate with pH adjustment and activated charcoal treatment leading to a high xylitol yield and productivity of 0.77g/g and 2.45g/(Lh), respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Antioxidant activity of aqueous extract of noni in dilutent for ram semen cryopreservation

    Directory of Open Access Journals (Sweden)

    Ana Lauren Costa Nascimento

    2016-03-01

    Full Text Available Noni (Morinda citrifolia L. is a fruit consumed worldwide because of its nutritional and therapeutic properties resulting from the large amount of phenolic compounds, which has aroused interest of the scientific community. In order to identify new natural sources of antioxidants, the objective of this study was to evaluate the performance of noni in diluent for ram semen cryopreservation. A completely randomized design consisting of four treatments and three repetitions per treatment was used. The treatments differed in terms of the concentration of the aqueous extract of noni added to the diluent: control, no addition of the extract, and three concentrations (24, 72, and 120 µg/mL. The physical and chemical variables of the mature fruit were evaluated: total acidity (8.78, pH (4.12, and soluble solids (8.18%. The vitamin C content was 309.42 mg per 100 g fresh matter. The aqueous extract of noni was also evaluated regarding the quantity of total phenolic compounds, antioxidant activity, and lipid peroxidation inhibition capacity. The aqueous extract contained a moderate amount of phenolic compounds (47.96 ± 1.95 mg gallic acid equivalent/100 g extract. The concentrations of the aqueous extract of 72 and 120 µg/mL in diluent used for semen cryopreservation inhibited lipid peroxidation by 21.75% and 51.32%, respectively. There was no positive effect of the lowest concentration (24 µg/mL. The antioxidant activity index of noni was 33.33, corresponding to very strong antioxidant activity. The aqueous extract of noni exhibits very strong antioxidant activity and its addition to the diluent for semen cryopreservation at a concentration of 72 µg/mL is able to inhibit lipid peroxidation.

  20. Bias due to Preanalytical Dilution of Rodent Serum for Biochemical Analysis on the Siemens Dimension Xpand Plus

    Directory of Open Access Journals (Sweden)

    Jennifer L. Johns

    2018-02-01

    Full Text Available Clinical pathology testing of rodents is often challenging due to insufficient sample volume. One solution in clinical veterinary and exploratory research environments is dilution of samples prior to analysis. However, published information on the impact of preanalytical sample dilution on rodent biochemical data is incomplete. The objective of this study was to evaluate the effects of preanalytical sample dilution on biochemical analysis of mouse and rat serum samples utilizing the Siemens Dimension Xpand Plus. Rats were obtained from end of study research projects. Mice were obtained from sentinel testing programs. For both, whole blood was collected via terminal cardiocentesis into empty tubes and serum was harvested. Biochemical parameters were measured on fresh and thawed frozen samples run straight and at dilution factors 2–10. Dilutions were performed manually, utilizing either ultrapure water or enzyme diluent per manufacturer recommendations. All diluted samples were generated directly from the undiluted sample. Preanalytical dilution caused clinically unacceptable bias in most analytes at dilution factors four and above. Dilution-induced bias in total calcium, creatinine, total bilirubin, and uric acid was considered unacceptable with any degree of dilution, based on the more conservative of two definitions of acceptability. Dilution often caused electrolyte values to fall below assay range precluding evaluation of bias. Dilution-induced bias occurred in most biochemical parameters to varying degrees and may render dilution unacceptable in the exploratory research and clinical veterinary environments. Additionally, differences between results obtained at different dilution factors may confound statistical comparisons in research settings. Comparison of data obtained at a single dilution factor is highly recommended.

  1. Mercury speciation analysis in seafood by species-specific isotope dilution: method validation and occurrence data

    Energy Technology Data Exchange (ETDEWEB)

    Clemens, Stephanie; Guerin, Thierry [Agence Nationale de Securite Sanitaire de l' Alimentation, Laboratoire de Securite des Aliments de Maisons-Alfort, Unite des Contaminants Inorganiques et Mineraux de l' Environnement, ANSES, Maisons-Alfort (France); Monperrus, Mathilde; Donard, Olivier F.X.; Amouroux, David [IPREM UMR 5254 CNRS - Universite de Pau et des Pays de l' Adour, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Institut des Sciences Analytiques et de Physico-chimie pour l' Environnement et les Materiaux, Pau Cedex (France)

    2011-11-15

    Methylmercury (MeHg) and total mercury (THg) in seafood were determined using species-specific isotope dilution analysis and gas chromatography combined with inductively coupled plasma mass spectrometry. Sample preparation methods (extraction and derivation step) were evaluated on certified reference materials using isotopically enriched Hg species. Solid-liquid extraction, derivation by propylation and automated agitation gave excellent accuracy and precision results. Satisfactory figures of merit for the selected method were obtained in terms of limit of quantification (1.2 {mu}g Hg kg{sup -1} for MeHg and 1.4 {mu}g Hg kg{sup -1} for THg), repeatability (1.3-1.7%), intermediate precision reproducibility (1.5% for MeHg and 2.2% for THg) and trueness (bias error less than 7%). By means of a recent strategy based on accuracy profiles ({beta}-expectation tolerance intervals), the selected method was successfully validated in the range of approximately 0.15-5.1 mg kg{sup -1} for MeHg and 0.27-5.2 mg kg{sup -1} for THg. Probability {beta} was set to 95% and the acceptability limits to {+-}15%. The method was then applied to 62 seafood samples representative of consumption in the French population. The MeHg concentrations were generally low (1.9-588 {mu}g kg{sup -1}), and the percentage of MeHg varied from 28% to 98% in shellfish and from 84% to 97% in fish. For all real samples tested, methylation and demethylation reactions were not significant, except in one oyster sample. The method presented here could be used for monitoring food contamination by MeHg and inorganic Hg in the future to more accurately assess human exposure. (orig.)

  2. Calculations for BDAS Setpoint with Non-conservative Boron Dilution Analysis

    International Nuclear Information System (INIS)

    Lee, Hwan Soo; Shin, Ho Cheol; Kim, Yong Bae

    2014-01-01

    BDAS (Boron Dilution Alarm System) utilizes the ex-core detector instrumentation signals to detect a possible inadvertent boron dilution event during operation mode 3, 4, 5, 6. For boron dilution analysis, discrepancies in the active coolant volume and the assumed linearity of the ex-core instrumentation response were identified for CE type PWR and they were reported by NASL-04-02 These discrepancies have potential to impact to determine BDAS setpoint in a non-conservative manner Therefore, in this study, the calculation of BDAS setpoint with those discrepancies condition about OPR1000 was performed and analyzed for checking the safety of BDAS. The new BDAS setpoint is calculated with conservative condition which recommended from Westinghouse Electric Company. The setpoint of BDAS using non-linear ICRR curve decrease to about 5% compared to the setpoint of that using linear ICRR curve. And this effect of the non-linearity is to slightly delay the boron dilution alarm during the inadvertence boron dilution at mode 3, 4, and 5

  3. Effect of wine dilution on the reliability of tannin analysis by protein precipitation

    DEFF Research Database (Denmark)

    Jensen, Jacob Skibsted; Werge, Hans Henrik Malmborg; Egebo, Max

    2008-01-01

    A reported analytical method for tannin quantification relies on selective precipitation of tannins with bovine serum albumin. The reliability of tannin analysis by protein precipitation on wines having variable tannin levels was evaluated by measuring the tannin concentration of various dilutions...... of five commercial red wines. Tannin concentrations of both very diluted and concentrated samples were systematically underestimated, which could be explained by a precipitation threshold and insufficient protein for precipitation, respectively. Based on these findings, we have defined a valid range...... of the tannin response in the protein precipitation-tannin assay, which suffers minimally from these problems....

  4. Use of image analysis for monitoring the dilution of Physalis peruviana pulp

    Directory of Open Access Journals (Sweden)

    Silvana Licodiedoff

    2013-06-01

    Full Text Available The aim of this work was to develop linear models using the image analysis coupled with density measurements to monitor the dilution of the Physalis juice in the concentrations ranging from 0 to 100% in mass of juice pulp. A sample corresponding to 20% in the mass of juice pulp was for validating purposes and a prediction of 19.9±0.3%. The models with three parameters showed the best predictions, providing this technique with a promising future for the monitoring the dilution of fruit juices.

  5. Sub-stoichiometric isotope dilution analysis method for the determination of iodine in common salts using iodine-131 tracer

    International Nuclear Information System (INIS)

    Singh, Vivek; Garg, A.N.

    1994-01-01

    A sub-stoichiometric isotope dilution analysis (SIDA) method was developed for the determination of iodine in different brands of common salts. An aqueous salt solution containing 131 I tracer and NaI as carrier is oxidized by tartaric acid and KIO 3 and the liberated iodine is extracted with CCl 4 . To the extract an aqueous solution of AgNO 3 is added in substoichiometric amount to obtain a colloidal solution of AgI. On adding sodium thiosulfate solution, the NaI so formed passes into aqueous solution, which is then counted. Several different brands of salt were analysed. The method is especially suitable for the determination of microgram amounts of iodide in the presence of excess of chloride. (Author)

  6. Mortality reduction by post-dilution online-haemodiafiltration : A cause-specific analysis

    NARCIS (Netherlands)

    Nubé, Menso J.; Peters, Sanne A E; Blankestijn, Peter J.; Canaud, Bernard; Davenport, Andrew; Grooteman, Muriel P C; Asci, Gulay; Locatelli, Francesco; Maduell, Francisco; Morena, Marion; Ok, Ercan; Torres, Ferran; Bots, Michiel L.; Moreso, Francesc; Pons, Mercedes; Ramos, Rosa; Mora-Macià, Josep; Carreras, Jordi; Soler, Jordi; Campistol, Josep M.; Martinez-Castelao, Alberto; Insensé, B.; Perez, C.; Feliz, T.; Barbetta, M.; Soto, C.; Mora, J.; Juan, A.; Ibrik, O.; Foraster, A.; Nin, J.; Fernández, A.; Arruche, M.; Sánchez, C.; Vidiella, J.; Barbosa, F.; Chiné, M.; Hurtado, S.; Llibre, J.; Ruiz, A.; Serra, M.; Salvó, M.; Poyuelo, T.; Maduell, F.; Carrera, M.; Fontseré, N.; Arias, M.; Merín, A.; Ribera, L.; Galceran, J. M.; Mòdol, J.; Moliner, E.; Ramirez, A.; Aguilera, J.; Alvarez, M.; De La Torre, B.; Molera, M.; Casellas, J.; Martín, G.; Andres, E.; Coll, E.; Valles, M.; Martínez, C.; Castellote, E.; Casals, J. M.; Gabàs, J.; Romero, M.; Martinez-Castelao, A.; Fulladosa, X.; Ramirez-Arellano, M.; Fulquet, M.; Pelegrí, A.; El Manouari, M.; Ramos, N.; Bartolomé, J.; Sans, R.; Fernández, E.; Sarró, F.; Compte, T.; Marco, F.; Mauri, R.; Bronsoms, J.; Arnaiz, J. A.; Beleta, H.; Pejenaute, A.; Ríos, J.; Lara, J.; Ter Wee, P. M.; Van Den Dorpel, M. A.; Dorval, M.; Lévesque, R.; Koopman, M. G.; Konings, C. J A M; Haanstra, W. P.; Kooistra, M.; Van Jaarsveld, B.; Noordzij, T.; Feith, G. W.; Peltenburg, H. G.; Van Buren, M.; Offerman, J. J G; Hoogeveen, E. K.; De Heer, F.; Van De Ven, P. J.; Kremer Hovinga, T. K.; Bax, W. A.; Groeneveld, J. O.; Lavrijssen, A. T J; Schrander-Van Der Meer, A. M.; Reichert, L. J M; Huussen, J.; Rensma, P. L.; Schrama, Y.; Van Hamersvelt, H. W.; Boer, W. H.; Van Kuijk, W. H.; Vervloet, M. G.; Wauters, I. M P M J; Sekse, I.; Toz, Huseyin; Ok, Ebru Sevinc; Kircelli, Fatih; Yilmaz, Mumtaz; Hur, Ender; Demirci, Meltem Sezis; Demirci, Cenk; Duman, Soner; Basci, Ali; Adam, Siddig Momin; Isik, Ismet Onder; Zengin, Murat; Suleymanlar, Gultekin; Yilmaz, Mehmet Emin; Ergin, Mehmet Ozkahya Pinar; Sagdic, Alfert; Kayali, Erkan; Boydak, Can; Colak, Taskin; Caliskan, Sihli; Kaplan, Hakan; Ulas, Hasibe; Kirbiyik, Sait; Berktas, Hakan; Dilbaz, Necati; Cristol, Jean Paul; Leray-Moragues, Hélène; Chenine, Leïla; Picot, Marie Christine; Jaussent, Audrey; Belloc, Claire; Lagarrigue, Mélodie; Chalabi, Lotfi; Debure, Alain; Ouziala, Messaoud; Lefevre, Jean Jacques; Thibaudin, Damien; Mohey, Hesham; Broyet, Christian; Afiani, Aida; Serveaux, Marie Odile; Patrier, Laure; Maurice, François; Rivory, Jean Pierre; Nicoud, Philippe; Durand, Claude; Normand, Michel; Seigneuric, Bruno; Magnant, Eric; Azzouz, Lynda; Islam, Mohamed Shariful; Vido, Sandor; Nzeyimana, Hilaire; Simonin, Danièle; Azymah, Yamina; Farah, Ibrahim; Coindre, Jean Philippe; Puyoo, Olivier; Chabannier, Marie Hélène; Ibos, Richard; Rouleau, Fabienne; Vela, Carlos; Joule, Josiane; Combarnous, François; Turc-Baron, Cécile; Ducret, Francis; Pointet, Philippe; Rey, Isabelle; Potier, Jacky; Bendini, Jean Christophe; Perrin, Franck; Kunz, Kristian; Lefrancois, Gaëlle; Colin, Angélique; Parahy, Sophie; Dancea, Irima; Coupel, Stéphanie; Testa, Angelo; Brunet, Philippe; Lebrun, Gaétan; Jaubert, Dominique; Delcroix, Catherine; Lavainne, Frédéric; Lefebvre, Anne; Guillodo, Marie Paule; Le Grignou, Dominique; Djema, Assia; Maaz, Mehadji; Chiron, Sylvie; Hoffmann, Maxime; Depraetre, Pascale; Haddj-Elmrabet, Atman; Joyeux, Véronique; Fleury, Dominique; Vrigneaud, Laurence; Lemaitre, Vincent; Aguilera, Didier; Guerraoui, Abdallah; Cremault, Alain; Laradi, Achour; Babinet, Francois

    Background. From an individual participant data (IPD) meta-analysis from four randomized controlled trials comparing haemodialysis (HD) with post-dilution online-haemodiafiltration (ol-HDF), previously it appeared that HDF decreases all-cause mortality by 14% (95% confidence interval 25; 1) and

  7. Brewing Bokashi: Strengthening Student Skills in Dilution Theory through Fermentation Analysis

    Directory of Open Access Journals (Sweden)

    Robert E. Zdor

    2016-05-01

    Full Text Available One of the basic microbiological techniques that students should master is that of using dilution theory to calculate the levels of bacteria in a fluid. This tip reports on using a rice water-milk fermentation mixture termed Bokashi as an easily implemented exercise in the basic microbiological lab to give students multiple opportunities to use dilution theory. Due to the shifts in bacterial community composition over time, a variety of microbes can be cultured using selective and nonselective media. Microscopic observation and the use of GEN III microplates to determine the collective phenotypic pattern of the mixture both give additional opportunities for students to hone their skills in bacterial analysis. Due to the decrease in the pH of the mixture over time, the notion of acid tolerance in bacteria can be explored and assessed using the microplate. By performing multiple rounds of serial dilutions and spread plating, students can practice their skill at using dilution theory several times over the course of the exercise.

  8. Development of multi-residue method for the determination of pesticides in cereal matrices by isotopic dilution associated to liquid chromatography coupled to tandem mass spectrometry after pressurized liquid extraction

    International Nuclear Information System (INIS)

    El Mrabet, Khadija

    2008-01-01

    Pesticides are nowadays considered as toxic for human health. The maximal residues levels authorized in water and foodstuff are more and more strict. Therefore, selective analytical techniques are necessary for their identification and their quantification. The aim of this thesis was to develop a multi-residue method for the determination of pesticides by isotopic dilution associated to liquid chromatography (LC) coupled with tandem mass spectrometry (MS"2) after pressurized liquid extraction. In a first step, an analysis method of phenyl-ureas and triazines in groundwater by isotopic dilution associated to LC/MS"2 after solid phase extraction has been developed. The method has been validated and evaluated by participating to an inter-laboratory study. Concerning cereals, an extraction method of pesticides associated to an analysis by LC/MS"2 has been developed for thirty-eight pesticides representative of twenty-six chemicals families and fourteen labeled compounds in wheat. The analysis has been carried out in reversed phase chromatography. Separation and detection conditions have been optimized. A global analytical protocol consisting of a pressurized liquid extraction step using acetonitrile at 100 deg. C and at 100 bars and followed by purification step of the resulting extract on a polymeric sorbent was developed. The developed method enables to extract thirty-eight pesticides and fourteen labeled compounds from wheat with recovery yield about 85% (RSD =4%, n=3). Moreover, the results show that the application of isotopic dilution can be complex. Although some improvements need to be added regarding experimentation of aged matrices or contaminated samples, the potential of the method has been demonstrated. (author) [fr

  9. The analysis of uranium in environmental sample by mass spectrometer combined with isotopic dilution

    International Nuclear Information System (INIS)

    Fu Zhonghua; Jia Baoting; Han Jun

    2003-01-01

    Uranium in the environmental sample was analyzed by mass spectrometer combined with isotopic dilution. Before mass spectrometer analysis, samples were dissolved in a concentrated acidic solution containing HNO 3 , HF and HClO 4 and chemically processed to suit the analysis requirement. Analysis results indicated that the uranium content was 0.08 μg/g in river water, 0.1 μg/g in evergreen foliage, and 5-11 μg/g in surface soil respectively. (authors)

  10. Determination of nanogram amounts of iodide by electrochemical isotope dilution analysis

    International Nuclear Information System (INIS)

    Gabrielsson, A.-B.; Beronius, P.

    1976-01-01

    A known quantity of iodide in ethanol as solvent was labelled with 131 I-and subsequently diluted with a predetermined amount of inactive iodide. Specific activities before and after the isotope dilution were established by anodically depositing small fractions of the halide in each sample on rotating silver micro electrodes and determining the activities of the electrodeposits. The lowest concentration of iodide used in any analysis was 1.10 -5 M. Further deposition studies revealed that iodide can be deposited with 1 100% current efficiency on the rotating silver micro electrode for concentration down to 2.4.10 -6 M. Electrodeposition studies for still lower concentrations have not yet been undertaken. These results suggest that amounts of iodide ion down to about 10 ng, and possibly still smaller quantitites, might be determined with the method developed. Amounts from 42 ng to 1 μg can be determined with an error of 2.5%. (T.G.)

  11. The interlaboratory experiment IDA-72 on mass spectrometric isotope dilution analysis. Vol. 1

    International Nuclear Information System (INIS)

    Beyrich, W.; Drosselmeyer, E.

    1975-07-01

    Within the framework of the Safeguards Project of the Federal Republic of Germany at the Nuclear Research Center Karlsruhe an analytical intercomparison program was carried out in cooperation with 22 laboratories of 13 countries or international organizations. The main objective was the acquisition of basic data on the errors involved in the mass spectrometric isotope dilution analysis if it is applied to the determination of uranium and plutonium in diluted active feed solutions of reprocessing plants in routine operation. The results were evaluated by statistical methods mainly in regard to the calculation of the estimates of the variances for the different error components contributing to the total error of this analytical technique. Furthermore, the performance of two new methods for sample conditioning suggested by the International Atomic Energy Agency, Vienna, and the European Institute for Transuranium Elements (EURATOM), Karlsruhe, was successfully tested. The results of some investigations on the stability of diluted high active feed solutions and on comparison analysis by X-ray fluorescence spectrometry are also included. Data on the analytical efforts (manhours) invested in this study are reported as well as general experiences made in the organization and performance of an experiment on such an extended international level. (orig.) [de

  12. Chromatographic analysis of wheatgrass extracts

    Directory of Open Access Journals (Sweden)

    Masood Shah Khan

    2015-01-01

    Full Text Available Aim: Wheatgrass (WG is the shoot of Triticum aestivum Linn. belongs to the family Gramineae, and possess high chlorophyll content and essential vitamins, minerals, vital enzymes, amino acids, dietary fibers etc., It has been shown to possess anti-cancer, anti-ulcer, antioxidant, and anti-arthritic activity due to the presence of biologically active compounds, and minerals. Therefore, in the present study, high-performance thin layer chromatography (HPTLC, and high-performance liquid chromatography (HPLC methods for qualitative and quantitative analysis have been proposed, which will help in quality evaluation of wheat grass extract. Materials and Methods: Samples for analysis were prepared in methanol and water simply by sonication. These were applied on pre-coated silica plate and chromatograms were developed using toluene: Ethyl acetate: Formic acid. HPLC analysis was done on Waters HPLC system using water, methanol, and acetonitrile as mobile phase. Merck C18 column has been used. Results: HPTLC finger printing of alcoholic extracts of WG was carried out and found 10–11 spots at different wavelengths 254, 366, and 435 nm. HPLC fingerprinting produced 22 peaks at 256 nm. Quantitative HPTLC analysis was done to determine the gallic acid content, and was found to be 0.077% w/w in aqueous extract. By HPLC, the content of gallic acid and rutin was found to be 0.07%, and 0.04% w/w in aqueous extract of WG. Conclusion: The developed HPLC and HPTLC fingerprinting method can be used for the quality control, and standardization of WG and its extracts used as nutritional supplement.

  13. The Aperture and Layout of the LHC Extraction Septa and TCDS Diluter with an Enlarged MSDC Vacuum Chamber

    CERN Document Server

    Goddard, B

    2003-01-01

    The LHC beam dumping system must safely abort the LHC beams over the whole energy range, under all realistically possible fault conditions. These include normal operation, failure of machine elements and also abnormal performance of subsystems of the beam dumping system itself. To avoid unnecessary irradiation and even equipment damage, the MSD extraction septa must provide sufficient aperture both for the circulating and extracted beams. In order to satisfy this requirement, a modified (enlarged) vacuum chamber design will be used for the limiting MSDC septa. The analysis of the available apertures is presented, with emphasis on the dependence on the local orbit and beam emittance.

  14. Field ionization mass spectrometry (FIMS) applied to tracer studies and isotope dilution analysis

    International Nuclear Information System (INIS)

    Anbar, M.; Heck, H.d'A.; McReynolds, J.H.; St John, G.A.

    1975-01-01

    The nonfragmenting nature of field ionization mass spectrometry makes it a preferred technique for the isotopic analysis of multilabeled organic compounds. The possibility of field ionization of nonvolatile thermolabile materials significantly extends the potential uses of this technique beyond those of conventional ionization methods. Multilabeled tracers may be studied in biological systems with a sensitivity comparable to that of radioactive tracers. Isotope dilution analysis may be performed reliably by this technique down to picogram levels. These techniques will be illustrated by a number of current studies using multilabeled metabolites and drugs. The scope and limitations of the methodology are discussed

  15. Application of 1- (3,4-dimenthylphenyl)-dodecanedione-1,2-dioxime (MFDDO) to substoichiometris extraction and determination of nickel(II) by the isotope dilution method

    Energy Technology Data Exchange (ETDEWEB)

    Gorski, Z.; Goraczko, W. [Technical University Poznan, Poznan (Poland). Radio and Photo Chemistry Department

    1997-10-01

    The conditions for use of 1-3,4-dimenthylphenyl-dodecanedione-1,2-dioxime (MFDDO) in toluene solution for substoichiometric extraction of Ni(II) from aqueous phases are described. This procedure allows the determination of 0.006-0.06 g/ml of nickel(II) in human urine and blood`s serum samples by the isotope dilution method using {sup 63}Ni(II) 9 refs., 5 figs.

  16. Stable isotope dilution analysis by thermal ionization mass spectrometry. Pt. 2

    International Nuclear Information System (INIS)

    Broekman, A.; Raaphorst, J.G. van

    1984-01-01

    The combination of stable isotope dilution analysis (SIDA) and thermal ionization mass spectrometry (TIMS) is in use for lead and uranium determination at milligram per kilogram levels for over 20 years. However, several other elements can also be determined accurately by SIDA/TIMS. In this study the determinations of cadmium and copper are described. Details of the digestion, electrochemical and ion-exchange separations and the loading of the elements on a filament are given. The advantages of the SIDA/TIMS technique are shown and illustrated with results for several certified reference materials. (orig.) [de

  17. Error analysis of isotope dilution mass spectrometry method with internal standard

    International Nuclear Information System (INIS)

    Rizhinskii, M.W.; Vitinskii, M.Y.

    1989-02-01

    The computation algorithms of the normalized isotopic ratios and element concentration by isotope dilution mass spectrometry with internal standard are presented. A procedure based on the Monte-Carlo calculation is proposed for predicting the magnitude of the errors to be expected. The estimation of systematic and random errors is carried out in the case of the certification of uranium and plutonium reference materials as well as for the use of those reference materials in the analysis of irradiated nuclear fuels. 4 refs, 11 figs, 2 tabs

  18. Determination of Cd, Pb, Zn and Cu in Sediment Compartments by Sequential Extraction and Isotope Dilution Inductively Coupled Plasma Mass Spectrometry (ID-ICP-MS

    Directory of Open Access Journals (Sweden)

    Gardolinski Paulo C. F. C.

    2002-01-01

    Full Text Available Trace concentrations of Cd, Cu, Pb and Zn in four different sediment fractions extracted in sequence were determined by isotope dilution inductively coupled mass spectrometry (IDICPMS. The metals from each fraction were extracted following the sequential extraction procedure recommended by the Bureau Commun de Référence (BCR of the Commission of the European Communities. As an alternative to external calibration, the elements were quantified by spiking the extracted solutions with 112Cd, 63Cu, 208Pb and 66Zn and application of isotope dilution. The proposed approach was applied to a sample collected from a lake and two standard reference materials, NIST2704 river sediment from the National Institute of Standards & Technology and the BCR-277 estuarine sediment. Detection limits, for each extracted solution, varied from 0.31 to 0.53 mug L¹ for Cd, 0.92 to 2.9 mug L¹ for Cu, 0.22 to 1.1 mug L¹ for Pb and 1.3 to 7.6 mug L¹ for Zn. The sum of the metals concentration in the different fractions was compatible with 95% confidence level found amounts obtained with complete digestion of the samples and with the certified values of the standard reference materials.

  19. Certification of methylmercury in cod fish tissue certified reference material by species-specific isotope dilution mass spectrometric analysis

    Energy Technology Data Exchange (ETDEWEB)

    Inagaki, Kazumi; Kuroiwa, Takayoshi; Narukawa, Tomohiro; Yarita, Takashi; Takatsu, Akiko; Okamoto, Kensaku; Chiba, Koichi [National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, Tsukuba, Ibaraki (Japan)

    2008-07-15

    A new cod fish tissue certified reference material, NMIJ CRM 7402-a, for methylmercury analysis was certified by the National Metrological Institute of Japan in the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Cod fish was collected from the sea close to Japan. The cod muscle was powdered by freeze-pulverization and was placed into 600 glass bottles (10 g each), which were sterilized with {gamma}-ray irradiation. The certification was carried out using species-specific isotope dilution gas chromatography inductively coupled plasma mass spectrometry (SSID-GC-ICPMS), where {sup 202}Hg-enriched methylmercury (MeHg) was used as the spike compound. In order to avoid any possible analytical biases caused by nonquantitative extraction, degradation and/or formation of MeHg in sample preparations, two different extraction methods (KOH/methanol and HCl/methanol extractions) were performed, and one of these extraction methods utilized two different derivatization methods (ethylation and phenylation). A double ID method was adopted to minimize the uncertainty arising from the analyses. In order to ensure not only the reliability of the analytical results but also traceability to SI units, the standard solution of MeHg used for the reverse-ID was prepared from high-purity MeHg chloride and was carefully assayed as follows: the total mercury was determined by ID-ICPMS following aqua regia digestion, and the ratio of Hg as MeHg to the total Hg content was estimated by GC-ICPMS. The certified value given for MeHg is 0.58 {+-} 0.02 mg kg{sup -1} as Hg. (orig.)

  20. Radioimmunoassay and liquid-chromatographic analysis for free cortisol in urine compared with isotope dilution-mass spectrometry

    International Nuclear Information System (INIS)

    Lantto, O.

    1982-01-01

    Three different routine methods for analysis for urinary cortisol with those by a highly specific reference method based on isotope dilution-mass spectrometry (I) were compared. A ''high-performance'' liquid-chromatographic method (II) gave the most comparable results (regression coefficient 0.86, intercept 9 nmol/L). For some urines much lower values were obtained by I than by II. Two radioimmunoassay (III) methods, one involving direct assay and one involving extraction, gave less-accurate results (regression coefficients of 1.87 and 1.52 and intercepts of 86 and 12 nmol/L, respectively), although values obtained by III and by I correlated well (r = 0.95-0.99), indicating a relation between the free cortisol and the compounds interfering in III. The apparent accuracy for the extraction method was improved by using as calibration standards urine samples previously assayed by I (regression coefficient 0.90, intercept 6 nmol/L). All four methods investigated showed a statistically significant sex-related difference in 24-h urinary cortisol excretion; evidently such a finding should be a prerequisite in any such method proposed for routine use

  1. Analysis of cesium extracting solvent using GCMS and HPLC

    International Nuclear Information System (INIS)

    White, T.L.; Herman, C.C.; Crump, S.L.; Marinik, A.R.; Lambert, D.P.; Eibling, R.E.

    2007-01-01

    A high-level waste (HLW) remediation process scheduled to begin in 2007 at the Savannah River Site is the Modular Caustic Side Solvent Extraction (CSSX) Unit (MCU). The MCU will use a hydrocarbon solvent (diluent) containing a cesium extractant, a calix[4]arene compound, to extract radioactive cesium from caustic HLW. The resulting decontaminated HLW waste or raffinate will be processed into grout at the Saltstone Production Facility (SPF). The cesium containing CSSX stream will undergo washing with dilute nitric acid followed by stripping of the cesium nitrate into a very dilute nitric acid or the strip effluent stream and the CSSX solvent will be recycled. The Defense Waste Processing Facility (DWPF) will receive the strip effluent stream and immobilize the cesium into borosilicate glass. Excess CSSX solvent carryover from the MCU creates a potential flammability problem during DWPF processing. Bench-scale DWPF process testing was performed with simulated waste to determine the fate of the CSSX solvent components. A simple high performance liquid chromatography (HPLC) method was developed to identify the modifier (which is used to increase Cs extraction and extractant solubility) and extractant within the DWPF process. The diluent and trioctylamine (which is used to suppress impurity effect and ion-pair disassociation) were determined using gas chromatography mass spectroscopy (GCMS). To close the organic balance, two types of sample preparation methods were needed. One involved extracting aqueous samples with methylene chloride or hexane, and the second was capturing the off gas of the DWPF process using carbon tubes and rinsing the tubes with carbon disulfide for analysis. This paper addresses the development of the analytical methods and the bench-scale simulated waste study results. (author)

  2. Quantitative analysis of 39 polybrominated diphenyl ethers by isotope dilution GC/low-resolution MS.

    Science.gov (United States)

    Ackerman, Luke K; Wilson, Glenn R; Simonich, Staci L

    2005-04-01

    A GC/low-resolution MS method for the quantitative isotope dilution analysis of 39 mono- to heptabrominated diphenyl ethers was developed. The effects of two different ionization sources, electron impact (EI) and electron capture negative ionization (ECNI), and the effects of their parameters on production of high-mass fragment ions [M - xH - yBr](-) specific to PBDEs were investigated. Electron energy, emission current, source temperature, ECNI system pressure, and choice of ECNI reagent gases were optimized. Previously unidentified enhancement of PBDE high-mass fragment ion [M - xH - yBr](-) abundance was achieved. Electron energy had the largest impact on PBDE high-mass fragment ion abundance for both the ECNI and EI sources. By monitoring high-mass fragment ions of PBDEs under optimized ECNI source conditions, quantitative isotope dilution analysis of 39 PBDEs was conducted using nine (13)C(12) labeled PBDEs on a low-resolution MS with low picogram to femtogram instrument detection limits.

  3. Quantification of fentanyl in serum by isotope dilution analysis using capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan); Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

    1998-06-01

    The quantitative determination of fentanyl (FT) in serum was examined by isotope dilution analysis using a capillary gas chromatograph equipped with a surface ionization detector. The separation of FT and its deuterated analogue, FT-{sup 2}H{sub 19}, was achieved within 15 min a column temperature of 260degC by using a 25 m column. Measurement of the samples prepared by the addition of a known amount of FT in the range of 0.2 to 40 ng/ml with 20 ng/ml of FT-{sup 2}H{sub 19} to human control serum allowed observation of a linear relationship between the peak area ratio and the added amount ratio. The correlation coefficient obtained by regression analysis was 0.999. The advantage of the present isotope dilution method was demonstrated by comparison with other FT analogues which substituted a propionyl group with an acetyl group or a phenethyl group with a benzyl group as the internal standard. The present method was used to determine the serum level of FT in surgical patients after i.v. administration. No endogenous compounds and concomitant drugs interfered with the detection of FT or FT-{sup 2}H{sub 19}. This method was considered to be useful for the pharmacokinetic study of FT in patients. (author)

  4. Quantification of fentanyl in serum by isotope dilution analysis using capillary gas chromatography

    International Nuclear Information System (INIS)

    Sera, Shoji; Goromaru, Tsuyoshi; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

    1998-01-01

    The quantitative determination of fentanyl (FT) in serum was examined by isotope dilution analysis using a capillary gas chromatograph equipped with a surface ionization detector. The separation of FT and its deuterated analogue, FT- 2 H 19 , was achieved within 15 min a column temperature of 260degC by using a 25 m column. Measurement of the samples prepared by the addition of a known amount of FT in the range of 0.2 to 40 ng/ml with 20 ng/ml of FT- 2 H 19 to human control serum allowed observation of a linear relationship between the peak area ratio and the added amount ratio. The correlation coefficient obtained by regression analysis was 0.999. The advantage of the present isotope dilution method was demonstrated by comparison with other FT analogues which substituted a propionyl group with an acetyl group or a phenethyl group with a benzyl group as the internal standard. The present method was used to determine the serum level of FT in surgical patients after i.v. administration. No endogenous compounds and concomitant drugs interfered with the detection of FT or FT- 2 H 19 . This method was considered to be useful for the pharmacokinetic study of FT in patients. (author)

  5. Isotope dilution and sampling factors of the quality assurance and TQM of environmental analysis

    International Nuclear Information System (INIS)

    Macasek, F.

    1999-01-01

    Sampling and preparatory treatment of environmental objects is discussed from the view of their information content, functional speciation of the pollutant, statistical distribution treatment and uncertainty assessment. During homogenization of large samples, a substantial information may be lost and validity of environmental information becomes vague. Isotope dilution analysis is discussed as the most valuable tool for both validity of analysis and evaluation of samples variance. Data collection for a non-parametric statistical treatment of series of 'non-representative' sub-samples, and physico-chemical speciation of analyte may actually better fulfill criteria of similarity and representativeness. Large samples are often required due to detection limits of analysis, but the representativeness of environmental samples should by understood not only by the mean analyte concentration, but also by its spatial and time variance. Hence, heuristic analytical scenarios and interpretation of results must be designed by cooperation of environmentalists and analytical chemists. (author)

  6. An analysis on boron dilution events during SBLOCA for the KNGR

    International Nuclear Information System (INIS)

    Kim, Young In; Hwang, Young Dong; Park, Jong Kuen; Chung, Young Jong; Sim, Suk Gu

    1999-02-01

    An analysis on boron dilution events during small break loss of coolant accident (LOCA) for Korea Next Generation Reactor (KNGR) was performed using Computational Fluid Dynamic (CFD) computer program FLUENT code. The maximum size of the water slug was determined based on the source of un borated water slug and the possible flow paths. Axisymmetric computational fluid dynamic analysis model is applied for conservative scoping analysis of un borated water slug mixing with recirculation water of the reactor system following small break LOCA assuming one Reactor Coolant Pump (RCP) restart. The computation grid was determined through the sensitivity study on the grid size, which calculates the most conservative results, and the preliminary calculation for boron mixing was performed using the grid. (Author). 17 refs., 3 tabs., 26 figs

  7. The interlaboratory experiment IDA-72 on mass spectrometric isotope dilution analysis. Vol. 2

    International Nuclear Information System (INIS)

    Beyrich, W.; Drosselmeyer, E.

    1975-07-01

    Volume II of the report on the IDA-72 experiment contains papers written by different authors on a number of special topics connected with the preparation, performance and evaluation of the interlaboratory test. In detail the sampling procedures for active samples of the reprocessing plant and the preparation of inactive reference and spike solution from standard material are described as well as new methods of sample conditioning by evaporation. An extra chapter is devoted to the chemical sample treatment as a preparation for mass spectrometric analysis of the U and Pu content of the solutions. Special topics are also methods for mass discrimination corrections, α-spectrometer measurements as a supplement for the determination of Pu-238 and the comparison of concentration determinations by mass spectrometric isotope dilution analysis with those performed by X-ray fluorescence spectrometry. The last part of this volume contains papers connected with the computerized statistical evaluation of the high number of data. (orig.) [de

  8. Antimicrobial Activity of Ephedra pachyclada Methanol Extract on Some Enteric Gram Negative Bacteria Which Causes Nosocomial Infections by Agar Dilution Method

    Directory of Open Access Journals (Sweden)

    Amin Sadeghi Dosari

    2016-10-01

    Full Text Available Background Past history indicates that plants were served as an important source of medicine. Otherwise, in developing countries people use medicinal plants against infectious disease because they cannot afford expensive drugs. Due to increasing rate of drug-resistant diseases, there is an urgent need to detect novel antimicrobial compounds from medicinal plants. Objectives The aim of the present study was to determine Antimicrobial activity of Ephedra pachyclada methanol extract on some enteric Gram-negative bacteria which causes nosocomial infections by agar dilution method. Methods In this cross-sectional study, in order to examine the antimicrobial effects of Ephedra pachyclada extract on intestinal Gram-negative bacteria, we exposed them to 0/128, 0/25, 0/5, 1, 2, 4 and 8 mg/mL of the extract. Ephedra pachyclada was collected from Jiroft Heights and methanolic extract was prepared with maceration method, during which, 50 gr powder of Ephedra pachyclada was dissolved in 300 mL of 80% methanol. Results In this study, the antibacterial effects of Ephedra pachyclada extract on Gram-negative bacteria such as Pseudomonas aeruginosa, Escherichia coli (PTCC-O157, Escherichia coli (ATCC-25922, Klebsiella pnemoniae, Serratia marcescens was investigated, defining the minimum inhibitory concentration (MIC by agar dilution method. It has been demonstrated that methanolic extract of Ephedra pachyclada affect intestinal Gram-negative bacteria. Conclusions The result showed that, Ephedra pachyclada extract has effective antimicrobial ingredients which are cheap and readily available. It can be used for medicinal purposes in the production of antimicrobial drug.

  9. Quantitative gas chromatography-olfactometry carried out at different dilutions of an extract. Key differences in the odor profiles of four high-quality Spanish aged red wines.

    Science.gov (United States)

    Ferreira, V; Aznar, M; López, R; Cacho, J

    2001-10-01

    Four Spanish aged red wines made in different wine-making areas have been extracted, and the extracts and their 1:5, 1:50, and 1:500 dilutions have been analyzed by a gas chromatography-olfactometry (GC-O) approach in which three judges evaluated odor intensity on a four-point scale. Sixty-nine different odor regions were detected in the GC-O profiles of wines, 63 of which could be identified. GC-O data have been processed to calculate averaged flavor dilution factors (FD). Different ANOVA strategies have been further applied on FD and on intensity data to check for significant differences among wines and to assess the effects of dilution and the judge. Data show that FD and the average intensity of the odorants are strongly correlated (r(2) = 0.892). However, the measurement of intensity represents a quantitative advantage in terms of detecting differences. For some odorants, dilution exerts a critical role in the detection of differences. Significant differences among wines have been found in 30 of the 69 odorants detected in the experiment. Most of these differences are introduced by grape compounds such as methyl benzoate and terpenols, by compounds released by the wood, such as furfural, (Z)-whiskey lactone, Furaneol, 4-propylguaiacol, eugenol, 4-ethylphenol, 2,6-dimethoxyphenol, isoeugenol, and ethyl vanillate, by compounds formed by lactic acid bacteria, such as 2,3-butanedione and acetoine, or by compounds formed during the oxidative storage of wines, such as methional, sotolon, o-aminoacetophenone, and phenylacetic acid. The most important differences from a quantitative point of view are due to 2-methyl-3-mercaptofuran, 4-propylguaiacol, 2,6-dimethoxyphenol, and isoeugenol.

  10. Simple and accurate measurement of carbamazepine in surface water by use of porous membrane-protected micro-solid-phase extraction coupled with isotope dilution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Teo, Hui Ling [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore); Wong, Lingkai [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Liu, Qinde, E-mail: liu_qinde@hsa.gov.sg [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Teo, Tang Lin; Lee, Tong Kooi [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Lee, Hian Kee, E-mail: chmleehk@nus.edu.sg [Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore)

    2016-03-17

    To achieve fast and accurate analysis of carbamazepine in surface water, we developed a novel porous membrane-protected micro-solid-phase extraction (μ-SPE) method, followed by liquid chromatography-isotope dilution tandem mass spectrometry (LC-IDMS/MS) analysis. The μ-SPE device (∼0.8 × 1 cm) was fabricated by heat-sealing edges of a polypropylene membrane sheet to devise a bag enclosing the sorbent. The analytes (both carbamazepine and isotope-labelled carbamazepine) were first extracted by μ-SPE device in the sample (10 mL) via agitation, then desorbed in an organic solvent (1 mL) via ultrasonication. Several parameters such as organic solvent for pre-conditioning of μ-SPE device, amount of sorbent, adsorption time, and desorption solvent and time were investigated to optimize the μ-SPE efficiency. The optimized method has limits of detection and quantitation estimated to be 0.5 ng L{sup −1} and 1.6 ng L{sup −1}, respectively. Surface water samples spiked with different amounts of carbamazepine (close to 20, 500, and 1600 ng L{sup −1}, respectively) were analysed for the validation of method precision and accuracy. Good precision was obtained as demonstrated by relative standard deviations of 0.7% for the samples with concentrations of 500 and 1600 ng kg{sup −1}, and 5.8% for the sample with concentration of 20 ng kg{sup −1}. Good accuracy was also demonstrated by the relative recoveries in the range of 96.7%–103.5% for all samples with uncertainties of 1.1%–5.4%. Owing to the same chemical properties of carbamazepine and isotope-labelled carbamazepine, the isotope ratio in the μ-SPE procedure was accurately controlled. The use of μ-SPE coupled with IDMS analysis significantly facilitated the fast and accurate measurement of carbamazepine in surface water. - Highlights: • μ-SPE coupled with IDMS for the measurement of carbamazepine. • The method is the first report of coupling μ-SPE with IDMS. • μ-SPE is fast, time

  11. New Data on Joint Extraction of Nitric Acid, Uranium(VI) and Tetravalent Elements by Diluted TBP and New Approach to Modeling of their Distribution

    International Nuclear Information System (INIS)

    Zilberman, B.Ya.; Fedorov, Yu.S.; Puzikov, E.A.; Blazheva, I.V.

    2008-01-01

    HNO 3 and U(IV) extraction by diluted TBP (tributyl phosphate) appeared significantly higher than believed earlier, requiring correction of mathematical model for extraction of all the species. The proposed model of HNO 3 extraction includes its dissolving in the extracted water, as well as its abduction to UO 2 (NO 3 ) 2 (TBP) 2 . Extraction of U(VI) and tetravalent elements is considered as reaction of their hydrated or partially hydrolyzed forms, the latter could be extracted themselves or as neutral forms with water liberation. The equation of element chemical reaction for modeling is determined by the slope of the linear part of the S-shaped curve representing D/S 2 function as a plot of HNO 3 concentration, where D is a distribution coefficient of the micro-component and S is a TBP concentration free of HNO 3 . The description of tetravalent element extraction in U(VI) presence needs the assumption of cation-cation interaction of element hydrolyzed forms with U(VI) in aqueous phase. Zr distribution is affected by micellar effects. (authors)

  12. Mass spectrometic isotope dilution analysis of Am and Cm in spent fuels

    International Nuclear Information System (INIS)

    Wantschik, M.; Koch, L.; Commission of the European Communities, Karlsruhe; Ganser, B.

    1983-01-01

    Spent nuclear fuels contain Am and Cm in the 10 ppb to 100 ppm range. Because of this low abundance and the necessity of handling small samples of the highly toxic fuel material only a mass-spectrometric isotope dilution analysis can give sufficiently accurate results. Since suitable spikes and/or standards have been lacking, this method has not been applied. Using known masses (+- 0.1%) of Am-241 and Cm-244 metal, Am-243 and Cm-248 spikes were calibrated to an accuracy of better than 0.2%. The standards were reanalysed by chemical titration and several radiometric techniques. The chemical conditioning is based on ionexchange chromatography with alpha-hydroxyisobutyric acid. A sample size of 10 -7 g is sufficient. For the mass-spectrometric measurement 10 -9 g of the elements are required. The accuracy for the determination of the main isotope is 0.5%. (orig./BRB)

  13. Development of isotope dilution gamma-ray spectrometry for plutonium analysis

    Energy Technology Data Exchange (ETDEWEB)

    Li, T.K.; Parker, J.L. (Los Alamos National Lab., NM (United States)); Kuno, Y.; Sato, S.; Kurosawa, A.; Akiyama, T. (Power Reactor and Nuclear Fuel Development Corp., Tokai, Ibaraki (Japan))

    1991-01-01

    We are studying the feasibility of determining the plutonium concentration and isotopic distribution of highly radioactive, spent-fuel dissolver solutions by employing high-resolution gamma-ray spectrometry. The study involves gamma-ray plutonium isotopic analysis for both dissolver and spiked dissolver solution samples, after plutonium is eluted through an ion-exchange column and absorbed in a small resin bead bag. The spike is well characterized, dry plutonium containing {approximately}98% of {sup 239}Pu. By using measured isotopic information, the concentration of elemental plutonium in the dissolver solution can be determined. Both the plutonium concentration and the isotopic composition of the dissolver solution obtained from this study agree well with values obtained by traditional isotope dilution mass spectrometry (IDMS). Because it is rapid, easy to operate and maintain, and costs less, this new technique could be an alternative method to IDMS for input accountability and verification measurements in reprocessing plants. 7 refs., 4 figs., 4 tabs.

  14. Evaluation of matrix effect in isotope dilution mass spectrometry based on quantitative analysis of chloramphenicol residues in milk powder

    International Nuclear Information System (INIS)

    Li, Xiu Qin; Yang, Zong; Zhang, Qing He; Li, Hong Mei

    2014-01-01

    Graphical abstract: -- Highlights: •We develop a strategy to evaluate matrix effect and its impact on the IDMS results. •Matrix effect and IDMS correction factor from different conditions are evaluated. •Ion suppression effect is observed in LLE and HLB pre-treated sample solutions. •Ion enhancement effect is found in MCX pre-treated sample solution. •IDMS correction factor in HLB and MCX solutions in three instruments is close to 1 -- Abstract: In the present study, we developed a comprehensive strategy to evaluate matrix effect (ME) and its impact on the results of isotope dilution mass spectrometry (IDMS) in analysis of chloramphenicol (CAP) residues in milk powder. Stable isotope-labeled internal standards do not always compensate ME, which brings the variation of the ratio (the peak area of analyte/the peak area of isotope). In our investigation, impact factors of this variation were studied in the extraction solution of milk powder using three mass spectrometers coupled with different ion source designs, and deuterium-labeled chloramphenicol (D5-CAP) was used as the internal standard. ME from mobile phases, sample solvents, pre-treatment methods, sample origins and instruments was evaluated, and its impact on the results of IDMS was assessed using the IDMS correction factor (θ). Our data showed that the impact of ME of mobile phase on the correction factor was significantly greater than that of sample solvent. Significant ion suppression and enhancement effects were observed in different pre-treated sample solutions. The IDMS correction factor in liquid–liquid extraction (LLE) and molecular imprinted polymer (MIP) extract with different instruments was greater or less 1.0, and the IDMS correction factor in hydrophilic lipophilic balance (HLB) and mix-mode cation exchange (MCX) extract with different instruments was all close to 1.0. To the instrument coupled with different ion source design, the impact of ME on IDMS quantitative results was

  15. Accurate quantification of polycyclic aromatic hydrocarbons in dust samples using microwave-assisted solvent extraction combined with isotope-dilution mass spectrometry

    International Nuclear Information System (INIS)

    Itoh, Nobuyasu; Fushimi, Akihiro; Yarita, Takashi; Aoyagi, Yoshie; Numata, Masahiko

    2011-01-01

    Highlights: → We applied MAE-IDMS for accurate quantification of PAHs in dust samples. → Both partitioning and isotopic equilibria can be achieved using this technique. → MAE-IDMS can provide accurate concentrations even if extraction efficiencies were low. → Characteristics of samples strongly affected for low extraction efficiencies of PAHs. - Abstract: For accurate quantification of polycyclic aromatic hydrocarbons (PAHs) in dust samples, we investigated the use of microwave-assisted solvent extraction (MAE) combined with isotope-dilution mass spectrometry (IDMS) using deuterium-labelled PAHs (D-PAHs). Although MAE with a methanol/toluene mixture (1:3 by volume) at 160 deg. C for 40 min was best for extracting PAHs from tunnel dust among examined, the recovery yields of D-PAHs decreased with increasing molecular weight (<40% for MW ≥ 264; that of deuterium-labelled indeno[123-cd]pyrene (D-IcdP) was only 7.1%). Although the residues were extracted a second time, the observed concentrations did not change dramatically (<5%), and the recovery yields of heavier D-PAHs (i.e., MW ≥ 264) were approximately half of those of the first extract, including D-IcdP (3.4%). These results suggest that both partitioning and isotopic equilibria of PAHs and D-PAHs between sample and solvent were achieved for extractable heavier PAHs under the condition. Thus, the observed concentrations of PAHs obtained by MAE-IDMS were reasonable, even though recovery yields of D-PAHs were <50%. From the results of carbon analyses and extractable contents, lower recovery yields of D-PAHs from the tunnel dust were due to a large content of char with low extractable contents.

  16. Validation of multi-element isotope dilution ICPMS for the analysis of basalts

    Energy Technology Data Exchange (ETDEWEB)

    Willbold, M.; Jochum, K.P.; Raczek, I.; Amini, M.A.; Stoll, B.; Hofmann, A.W. [Max-Planck-Institut fuer Chemie, Mainz (Germany)

    2003-09-01

    In this study we have validated a newly developed multi-element isotope dilution (ID) ICPMS method for the simultaneous analysis of up to 12 trace elements in geological samples. By evaluating the analytical uncertainty of individual components using certified reference materials we have quantified the overall analytical uncertainty of the multi-element ID ICPMS method at 1-2%. Individual components include sampling/weighing, purity of reagents, purity of spike solutions, calibration of spikes, determination of isotopic ratios, instrumental sources of error, correction of mass discrimination effect, values of constants, and operator bias. We have used the ID-determined trace elements for internal standardization to improve indirectly the analysis of 14 other (mainly mono-isotopic trace elements) by external calibration. The overall analytical uncertainty for those data is about 2-3%. In addition, we have analyzed USGS and MPI-DING geological reference materials (BHVO-1, BHVO-2, KL2-G, ML3B-G) to quantify the overall bias of the measurement procedure. Trace element analysis of geological reference materials yielded results that agree mostly within about 2-3% relative to the reference values. Since these results match the conclusions obtained by the investigation of the overall analytical uncertainty, we take this as a measure for the validity of multi-element ID ICPMS. (orig.)

  17. Doping control analysis of 46 polar drugs in horse plasma and urine using a 'dilute-and-shoot' ultra high performance liquid chromatography-high resolution mass spectrometry approach.

    Science.gov (United States)

    Kwok, Wai Him; Choi, Timmy L S; Kwok, Karen Y; Chan, George H M; Wong, Jenny K Y; Wan, Terence S M

    2016-06-17

    The high sensitivity of ultra high performance liquid chromatography coupled with high resolution mass spectrometry (UHPLC-HRMS) allows the identification of many prohibited substances without pre-concentration, leading to the development of simple and fast 'dilute-and-shoot' methods for doping control for human and equine sports. While the detection of polar drugs in plasma and urine is difficult using liquid-liquid or solid-phase extraction as these substances are poorly extracted, the 'dilute-and-shoot' approach is plausible. This paper describes a 'dilute-and-shoot' UHPLC-HRMS screening method to detect 46 polar drugs in equine urine and plasma, including some angiotensin-converting enzyme (ACE) inhibitors, sympathomimetics, anti-epileptics, hemostatics, the new doping agent 5-aminoimidazole-4-carboxamide-1-β-d-ribofuranoside (AICAR), as well as two threshold substances, namely dimethyl sulfoxide and theobromine. For plasma, the sample (200μL) was protein precipitated using trichloroacetic acid, and the resulting supernatant was diluted using Buffer A with an overall dilution factor of 3. For urine, the sample (20μL) was simply diluted 50-fold with Buffer A. The diluted plasma or urine sample was then analysed using a UHPLC-HRMS system in full-scan ESI mode. The assay was validated for qualitative identification purpose. This straightforward and reliable approach carried out in combination with other screening procedures has increased the efficiency of doping control analysis in the laboratory. Moreover, since the UHPLC-HRMS data were acquired in full-scan mode, the method could theoretically accommodate an unlimited number of existing and new doping agents, and would allow a retrospectively search for drugs that have not been targeted at the time of analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Soluble/insoluble (dilute-HCl-extractable fractionation of Cd, Pb and Cu in Antarctic snow and its relationship with metal fractionations in the aerosol

    Directory of Open Access Journals (Sweden)

    Annibaldi A.

    2013-04-01

    Full Text Available A chemical fractionation methodology for determination of the (water soluble and the insoluble (dilute-HCl-extractable fractions of Cd, Pb and Cu in Antarctic snow was set-up and verified for the additivity of the two fractions detected. Molten samples were filtrated and the water-insoluble fraction was extracted by dilute ultrapure HCl (pH ~1.5. Metal determinations were carried out in the two fractions by square wave anodic stripping voltammetry. The total metal concentrations in samples collected in the 2000–2001 austral summer in a clean area (Faraglione Camp in the neighbourhood of the Mario Zucchelli Italian Station were of the order of Cd 10-20 pg g−1, Pb 20–40 pg g−1, Cu 60–120 pg g−1 with an approximate equidistribution between soluble and insoluble fractions. These fractionations compare well (and show a quite consistent temporal trend with those observed in the aerosol samples collected in the same area/period and confirm the close relationship between metal distributions in snow/ice and in the aerosol. At the station metal concentrations increase due to anthropic contribution and the distribution changes with Cd predominantly present in the soluble fraction (~80%, while Pb and Cu are more concentrated in the insoluble fraction, 70–80% and ~70%, respectively.

  19. Evaluation of accelerated solvent extraction for butyltin speciation in PACS-2 CRM using double-spike isotope dilution-GC/ICPMS.

    Science.gov (United States)

    Encinar, Jorge Ruiz; Rodriguez-González, Pablo; Fernandez, Julio Rodriguez; Alonso, J Ignacio Garcia; Díez, Sergi; Bayona, Josep M; Sanz-Medelt, Alfredo

    2002-10-15

    Pressurized liquid extraction using the accelerated solvent extractor (Dionex ASE 200) has been evaluated for the determination of mono-, di- and tributyltin (MBT, DBT, and TBT, respectively) in PACS-2 certified reference material. A double-enriched spike containing 119Sn-enriched MBT and TBT and 118Sn-enriched DBT allowed for the simultaneous determination of the three butyltin species and the factors governing species interconversion. The stability of the spike was evaluated by reverse isotope dilution experiments covering more than one year with satisfactory results. Quantitative recoveries using ASE for TBT and DBT were obtained at temperatures above 110 degrees C. The effect of the extraction time and number of static cycles was evaluated. Results suggest that extraction efficiency was quantitative with extraction times as low as 10 min for all butyltin species at 110 degrees C. Decomposition reactions were only detected at the higher temperatures assayed (140 and 175 degrees C) and that was only for the degradation of DBT to MBT (approximately 4%). The results found for MBT were approximately 25% higher than the certified value for the PACS-2 sediment reference material in agreement with previous results obtained by ultrasonic and microwave assisted extraction.

  20. The analysis study of plutonium in the environmental sample by mass spectrum combined with isotopic dilution

    International Nuclear Information System (INIS)

    Han Jun; Fu Zhonghua; Mao Xingen; Meng Fanben

    2004-01-01

    The technology of the rhenium filament carbonization was used to increase the ionization efficiency in this paper. The plutonium in the environmental sample was analyzed by Mass Spectrum combined with isotope dilution. Analysis of the 239 Pu blank in the process: The analysis of 239 Pu from the chemical process was carried out in order to establish the influence of the 239 Pu introduced from the process. The analysis results were shown in Table 1 sample 1 was not gone through the process, sample 2 and sample 3 were gone through the process. It was clear that there was no influence of the 239 Pu from the process within the deviation. Results and Discussions: The environmental samples which were dealed with the chemical method were prepared the sample of mass spectrum, The atomic ratio of the 239 Pu and 242 Pu in the environmental samples was measured by Mass Spectrum. The atomic ratio in the tracer 242 Pu was 0.01476±0.00007.The results for nuclide content in environment were given in Table 2. The content of 239 Pu in the tracer was high, so the existing of 239 Pu in the environmental samples can be determined by the changing of the atomic ratio of 242 Pu to 239 Pu. It was clear that there was 239 Pu in the environmental samples except the cypress leaves-2 and the pine leaves-3 within the deviation, and the content of 239 Pu were given in Table 2. Conclusion: a. Plutonium was separated and purified from the impurity by the anion-exchange and the electrodeposition, it was possible to provide the eligible mass spectrum sample. b. The measurement of plutonium in the environmental samples was not influenced by the flow of the background in the experiment. c. As the technology of the rhenium carbonization was used to increase the ionization efficiency, the content of plutonium which was about 10 -13 g in the environmental sample could be quantitatively analyzed by Mass Spectrum combined with isotope dilution. (authors)

  1. Analysis of structure and defects in thin silicon films deposited from hydrogen diluted silane

    International Nuclear Information System (INIS)

    Elzakker, G. van; Nadazdy, V.; Tichelaar, F.D.; Metselaar, J.W.; Zeman, M.

    2006-01-01

    Thin silicon layers have been deposited from silane diluted with hydrogen. The dilution ratio R (R = [H 2 ]/[SiH 4 ]) has been varied between R = 0 and R = 40. The structural properties of Si:H films have been studied using transmission electron microscopy imaging and Raman spectroscopy. The phase evolution from the amorphous phase into the mixed and eventually microcrystalline phase strongly depends on the hydrogen dilution. The initiation of the microcrystalline growth occurs between R = 20 and R = 25. The phase transition becomes more abrupt with increasing hydrogen dilution. Optoelectronic properties of the layers have been determined. Increasing hydrogen dilution results in films with increasing effective defect density and Urbach energy, which is related to inhomogeneous growth. The charge deep-level transient spectroscopy technique (Q-DLTS) was applied for the first time on hydrogen diluted thin silicon films in order to investigate the energy distribution of the defect states in these layers as a function of the dilution ratio R. The Q-DLTS spectra indicate a difference in defect-state distribution when the films evolve from the amorphous phase into the microcrystalline phase

  2. Measurement of isotope abundance variations in nature by gravimetric spiking isotope dilution analysis (GS-IDA).

    Science.gov (United States)

    Chew, Gina; Walczyk, Thomas

    2013-04-02

    Subtle variations in the isotopic composition of elements carry unique information about physical and chemical processes in nature and are now exploited widely in diverse areas of research. Reliable measurement of natural isotope abundance variations is among the biggest challenges in inorganic mass spectrometry as they are highly sensitive to methodological bias. For decades, double spiking of the sample with a mix of two stable isotopes has been considered the reference technique for measuring such variations both by multicollector-inductively coupled plasma mass spectrometry (MC-ICPMS) and multicollector-thermal ionization mass spectrometry (MC-TIMS). However, this technique can only be applied to elements having at least four stable isotopes. Here we present a novel approach that requires measurement of three isotope signals only and which is more robust than the conventional double spiking technique. This became possible by gravimetric mixing of the sample with an isotopic spike in different proportions and by applying principles of isotope dilution for data analysis (GS-IDA). The potential and principle use of the technique is demonstrated for Mg in human urine using MC-TIMS for isotopic analysis. Mg is an element inaccessible to double spiking methods as it consists of three stable isotopes only and shows great potential for metabolically induced isotope effects waiting to be explored.

  3. Simultaneous analysis of urinary phthalate metabolites of residents in Korea using isotope dilution gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kim, Miok; Song, Na Rae; Choi, Jong-Ho; Lee, Jeongae; Pyo, Heesoo

    2014-02-01

    Phthalates are used in industry products, household items, and medical tools as plasticizers. Human exposure to phthalates has raised concern about its toxicity. In the present study, optimization was conducted for the simultaneous analysis of eight kinds of phthalate metabolites using gas chromatography-mass spectrometry (GC-MS): MEP, MiBP, MnBP, MBzP, MiNP, MEHP, MEOHP, and MEHHP. In order to minimize the matrix effect and to do quantitative analysis, isotope dilution and LLE-GC-MS methods were performed. Urine samples were enzymatically hydrolyzed, extracted with a mixture of n-hexane and ethyl ether (8:2; v:v), and subsequently derivatized with trimethylsilylation. All eight kinds of analytes showed clear resolution and high reproducibility in GC-MS results. The method detection limit ranged from 0.05 ng/mL to 0.2 ng/mL. Calibration curves were found to be linear from 0.2 to 100 ng/mL with -(2)>0.992. The relative standard deviation of the intraday precision using water and urine ranged from 2.1% to 16.3%. The analysis was performed with urine samples that were collected from adults residing in the Republic of Korea. The analyzed concentration results were compared according to gender and region. As a result, DEHP metabolites showed the highest detected concentration (75.92 μg/g creatinine, 100%), and MiNP, a metabolite of DiNP, showed the lowest detected concentration (0.42 μg/g creatinine, 22.5%). On average, female urine (200.76 μg/g creatinine) had a higher detected concentration of ∑8 phthalate metabolites than male urine. Samples from rural regions (211.96 μg/g creatinine) had higher levels than samples from urban regions. © 2013.

  4. Separation of uranium(VI) by liquid-solid extraction with tri-n-octylphosphine oxide diluted with naphthalene

    International Nuclear Information System (INIS)

    Shigetomi, Y.; Kojima, T.; Kamba, H.; Yamamoto, Y.

    1980-01-01

    Liquid-liquid distribution with tri-n-octylphosphine oxide (TOPO) and molten naphthalene has been investigated for the extraction of 20 metals from nitric acid and hydrochloric acid solutions. Uranium is quantitatively extracted from 1 M nitric acid or hydrochloric acid by using 100 mg of TOPO and 200 mg of naphthalene and shaking for 5 min at 80 0 C, and separated from transition metals, alkaline earth metals and rare earth metals (except scandium). Addition of naphthalene increases the extraction efficiency. (Auth.)

  5. The measurement of the chemically mobile fraction of lead in soil using isotopic dilution analysis

    International Nuclear Information System (INIS)

    Kirchhoff, J.; Brand, J.; Schuettelkopf, H.

    1992-12-01

    The chemically available fraction of lead in eight soils measured by isotopic dilution analysis using 212 Pb ranged from 7 to 16% of the total content of lead in soil. The soluble fractions achieved values up to 63% of the total content in 1 M NH 4 NO 3 , 1 M MgCl 2 and 0.05 M DTPA solutions. Increasing the contact time between water and soil, the water-soil ratio from 1:1 to 5:1 and increasing the temperature of the soil-water suspension raised the chemically available fraction in soil. Comparing various soil parameters and the mobile fraction of lead, only pH shows a significant correlation. The amphoteric character of lead causes a minimum of mobility about pH 6; pH-values below are responsible for the higher mobility of lead as Pb 2+ , at pH-values above 6 soluble hydroxy and humic acid complexes are formed. (orig.) [de

  6. Multiresidue analysis of persistent organic pollutants in contaminated soil using GC-LRMS, GC-HRMS and isotope dilution analysis

    International Nuclear Information System (INIS)

    Badea, Silviu-Laurentiu; Lundstedt, Staffan; Liljelind, Per; Tysklind, Mats

    2009-01-01

    In this study we evaluated a multiresidue analytical protocol for selected Persistent Organic Pollutants (POPs) in soil, that later can be used in adsorption and leaching studies. The method used was based on Soxhlet extraction and open column chromatographic fractionation and clean-up, as well as liquid-liquid extraction and acetylation for phenolic compounds. Target analytes, i.e. polychlorinated phenols (PCPhs), hexachlorobenzene (HCB), polychlorinated dibenzodioxins and furans (PCDDs/Fs), polychlorinated biphenyl (PCBs) PAHs, were detected and quantified using Gas Chromatography-Low Resolution Mass Spectrometry (GC-LRMS) and Gas Chromatography-High Resolution Mass Spectrometry (GC-HRMS) and isotope dilution methodology. Generally, the results show a good recovery and a low standard deviation for those isomers that have also a 13 C labeled compound present in the sample: 4-mono, 2,4 di, 2,4,5 tri, 2,3,4,5 and penta chlorinated phenols. Our results clearly demonstrate that it is possible to analyse a wide range of compounds in complex soil matrixes. (authors(

  7. Analysis of polonium-210 in food products and bioassay samples by isotope-dilution alpha spectrometry

    International Nuclear Information System (INIS)

    Lin Zhichao; Wu Zhongyu

    2009-01-01

    A rapid and reliable radiochemical method coupled with a simple and compact plating apparatus was developed, validated, and applied for the analysis of 210 Po in variety of food products and bioassay samples. The method performance characteristics, including accuracy, precision, robustness, and specificity, were evaluated along with a detailed measurement uncertainty analysis. With high Po recovery, improved energy resolution, and effective removal of interfering elements by chromatographic extraction, the overall method accuracy was determined to be better than 5% with measurement precision of 10%, at 95% confidence level.

  8. Analysis of polonium-210 in food products and bioassay samples by isotope-dilution alpha spectrometry.

    Science.gov (United States)

    Lin, Zhichao; Wu, Zhongyu

    2009-05-01

    A rapid and reliable radiochemical method coupled with a simple and compact plating apparatus was developed, validated, and applied for the analysis of (210)Po in variety of food products and bioassay samples. The method performance characteristics, including accuracy, precision, robustness, and specificity, were evaluated along with a detailed measurement uncertainty analysis. With high Po recovery, improved energy resolution, and effective removal of interfering elements by chromatographic extraction, the overall method accuracy was determined to be better than 5% with measurement precision of 10%, at 95% confidence level.

  9. Diglycolic acid modified zirconium phosphate and studies on the extraction of Am(III) and Eu(III) from dilute nitric acid medium

    Energy Technology Data Exchange (ETDEWEB)

    Selvan, B. Robert; Suneesh, A.S.; Venkatesan, K.A.; Antony, M.P. [Indira Gandhi Centre for Atomic Research, Kalpakkam (India). Fuel Chemistry Division; Dasthaiah, K.; Gardas, R.L. [Indian Institute of Technology - Madras, Chennai (India). Dept. of Chemistry

    2017-06-01

    Diglycolic acid modified zirconium phosphate (ZrP-DGA) was prepared and studied for the extraction of Am(III) and Eu(III) from dilute nitric acid medium. The distribution coefficient (K{sub d}, mL.g{sup -1}) of Am(III) and Eu(III) was measured as a function of time, pH and concentration of Eu(III) ion etc. The K{sub d} of Am(III) and Eu(III) increased with increase of pH, reached a maximum value of distribution coefficient at pH 1.5 - 2, followed by decrease in K{sub d} values. Rapid extraction of Am(III) and Eu(III) in ZrP-DGA was observed followed by the establishment of equilibrium occurred in 100 min. Kinetics of extraction was fitted in to pseudo second order rate equation. The amount of Eu(III) loaded in ZrP-DGA increased with increase in the concentration of Eu(III) ion in aqueous phase and the isotherm was fitted in to Langmuir and Freundlich adsorption models. The extraction of Am(III) in ZrP-DGA was higher as compared to Eu(III) and the interference of Eu(III) on the extraction of Am(III) was studied. The distribution coefficient of some lanthanides in ZrP-DGA was measured and the K{sub d} of lanthanides increased across the lanthanide series. The extracted trivalent metal ions were recovered in three contacts of loaded ZrP-DGA with 0.5 M nitric acid.

  10. Third phase formation in organic solutions in the extraction of mono-acids by tertiary trialcoyl-amines diluted in very slightly polar organic solvents

    International Nuclear Information System (INIS)

    Robaglia, Michele

    1973-01-01

    The phenomena of third phase formation which can occur during the extraction of an acid with a tertiary amine diluted in a low polarity diluent are studied. In the first part a system including water (TnOA - C 6 H 12 - HCl - H 2 O) is compared with an anhydrous system (TnOA - C 6 H 12 - HCl - N 2 ). There are two kinds of gaps. One during amine salification, another one during the extraction of excess acid. The important part of the water content of the organic phase is demonstrated. The presence of water enhances the gaps. The polar water molecules are dissolved inside the tri-octylamine salt micelles. The heavy phase is formed by aggregates, the light phase represents the solubility of the non soluble species in the medium. In the second part are studied the influence of some parameters (like nature of diluent, acid, amine and temperature) on the gaps formation and on the extraction of excess acid and water. In every cases the part played by water remains the same. Finally some comparisons are made between tertiary systems and binary systems which formed them. The binary systems were studied by the mean of crystallization curves. (author) [fr

  11. Determination of Glyphosate, its Degradation Product Aminomethylphosphonic Acid, and Glufosinate, in Water by Isotope Dilution and Online Solid-Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry

    Science.gov (United States)

    Meyer, Michael T.; Loftin, Keith A.; Lee, Edward A.; Hinshaw, Gary H.; Dietze, Julie E.; Scribner, Elisabeth A.

    2009-01-01

    The U.S. Geological Survey method (0-2141-09) presented is approved for the determination of glyphosate, its degradation product aminomethylphosphonic acid (AMPA), and glufosinate in water. It was was validated to demonstrate the method detection levels (MDL), compare isotope dilution to standard addition, and evaluate method and compound stability. The original method USGS analytical method 0-2136-01 was developed using liquid chromatography/mass spectrometry and quantitation by standard addition. Lower method detection levels and increased specificity were achieved in the modified method, 0-2141-09, by using liquid chromatography/tandem mass spectrometry (LC/MS/MS). The use of isotope dilution for glyphosate and AMPA and pseudo isotope dilution of glufosinate in place of standard addition was evaluated. Stable-isotope labeled AMPA and glyphosate were used as the isotope dilution standards. In addition, the stability of glyphosate and AMPA was studied in raw filtered and derivatized water samples. The stable-isotope labeled glyphosate and AMPA standards were added to each water sample and the samples then derivatized with 9-fluorenylmethylchloroformate. After derivatization, samples were concentrated using automated online solid-phase extraction (SPE) followed by elution in-line with the LC mobile phase; the compounds separated and then were analyzed by LC/MS/MS using electrospray ionization in negative-ion mode with multiple-reaction monitoring. The deprotonated derivatized parent molecule and two daughter-ion transition pairs were identified and optimized for glyphosate, AMPA, glufosinate, and the glyphosate and AMPA stable-isotope labeled internal standards. Quantitative comparison between standard addition and isotope dilution was conducted using 473 samples analyzed between April 2004 and June 2006. The mean percent difference and relative standard deviation between the two quantitation methods was 7.6 plus or minus 6.30 (n = 179), AMPA 9.6 plus or minus 8

  12. Gas chromatography/ion trap mass spectrometry applied for the analysis of triazine herbicides in environmental waters by an isotope dilution technique

    International Nuclear Information System (INIS)

    Cai Zongwei; Wang Dongli; Ma, W.T.

    2004-01-01

    A gas chromatography/ion trap mass spectrometry method was developed for the analysis of simazine, atrazine, cyanazine, as well as the degradation products of atrazine, such as deethylatrazine and deisopropylatrazine in environmental water samples. Isotope dilution technique was applied for the quantitative analysis of atrazine in water at low ng/l levels. One liter of water sample spiked with stable isotope internal standard atrazine-d 5 was extracted with a C 18 solid-phase extraction cartridge. The analysis was performed on an ion trap mass spectrometer operated in MS/MS method. The extraction recoveries were in the range of 83-94% for the triazine herbicides in water at the concentrations of 24, 200, and 1000 ng/l, while poor recoveries were obtained for the degradation products of atrazine. The relative standard deviation (R.S.D.) were within the range of 3.2-16.1%. The detection limits of the method were between 0.75 and 12 ng/l when 1 l of water was analyzed. The method was successfully applied to analyze environmental water samples collected from a reservoir and a river in Hong Kong for atrazine detected at concentrations between 3.4 and 26 ng/l

  13. Pre-column dilution large volume injection ultra-high performance liquid chromatography-tandem mass spectrometry for the analysis of multi-class pesticides in cabbages.

    Science.gov (United States)

    Zhong, Qisheng; Shen, Lingling; Liu, Jiaqi; Yu, Dianbao; Li, Siming; Yao, Jinting; Zhan, Song; Huang, Taohong; Hashi, Yuki; Kawano, Shin-ichi; Liu, Zhaofeng; Zhou, Ting

    2016-04-15

    Pre-column dilution large volume injection (PD-LVI), a novel sample injection technique for reverse phase ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), was developed in this study. The PD-LVI UHPLC-MS/MS system was designed by slightly modifying the commercial UHPLC-MS/MS equipment with a mixer chamber. During the procedure of PD-LVI, sample solution of 200μL was directly carried by the organic mobile phase to the mixer and diluted with the aqueous mobile phase. After the mixture was introduced to the UHPLC column in a mobile phase of acetonitrile-water (15/85, v/v), the target analytes were stacked on the head of the column until following separation. Using QuEChERS extraction, no additional steps such as solvent evaporation or residue redissolution were needed before injection. The features of PD-LVI UHPLC-MS/MS system were systematically investigated, including the injection volume, the mixer volume, the precondition time and the gradient elution. The efficiency of this approach was demonstrated by direct analysis of 24 pesticides in cabbages. Under the optimized conditions, low limits of detection (0.00074-0.8 ng/kg) were obtained. The recoveries were in the range of 63.3-109% with relative standard deviations less than 8.1%. Compared with common UHPLC-MS/MS technique, PD-LVI UHPLC-MS/MS showed significant advantages such as excellent sensitivity and reliability. The mechanism of PD-LVI was demonstrated to be based on the column-head stacking effect with pre-column dilution. Based on the results, PD-LVI as a simple and effective sample injection technique of reverse phase UHPLC-MS/MS for the analysis of trace analytes in complex samples showed a great promising prospect. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Comparison between isotope dilution and activation analysis as a method for determining the macro content of mercury

    International Nuclear Information System (INIS)

    Soedyartomo; Sunoko, S.R.

    1975-01-01

    It is true that the mercury content in the environment should be measured accurately because of its toxicity even at levels of microgram order. The assessment of hazards due to environmental contamination with mercury is based on the results of the metal analysis in a number of different samples. Consequently, the study of the character of analytical methods used, i.e. their accuracy, precision, sensitivity, etc. is essential. A brief description on the microanalysis methods of mercury as given. The discussion of the results obtained from analysing some sludge and water by means of isotope dilution and destructive thermal neutron activation analysis is also presented. It is found that both methods are suitable for routine work. It can be concluded that the isotope dilution method has some advantages. It is more simple, more sensitive, more rapid, and has lower radiation hazard. (author)

  15. Enumeration of haemopoietic progenitors (CFU-C and BFU-E) in liquid microculture using a limiting dilution analysis.

    Science.gov (United States)

    Marchal, G; Milon, G

    1980-01-01

    In order to overcome the difficulty of scoring multicentric colonies of haemopoietic progenitor cells, cultures in 10 microliter of liquid medium were grown. Plated at three different cell concentrations, progenitor cells (CFU-C or BFU-E) are not present in all wells. Their presence is easily scored in each well of microculture 7 days after incubation. A limiting dilution analysis allows one to obtain accurate quantification.

  16. Simultaneous determination of platinum group elements and rhenium in rock samples using isotope dilution inductively coupled plasma mass spectrometry after cation exchange separation followed by solvent extraction

    International Nuclear Information System (INIS)

    Shinotsuka, Kazunori; Suzuki, Katsuhiko

    2007-01-01

    A simple and precise determination method for platinum group elements (PGEs) and Re in rock samples was developed using isotope dilution coupled with inductively coupled plasma mass spectrometry (ID-ICP-MS). Cation exchange separation was employed for simplicity, because it is applicable to group separation and simultaneous isotopic measurement in contrast with the widely used anion exchange separation which entails separate elution. However, its application to ID-ICP-MS has been limited due to spectral interferences from impurities retained in the PGE fraction even after ion chromatography. To overcome this limitation, solvent extraction using N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform was successfully applied for further purification. After the examination of optimum experimental parameters in cation exchange separation and solvent extraction using synthetic PGE solution, the established procedure was applied to the determination of PGEs and Re in some geochemical reference materials. The obtained results agreed well with the literature data determined using the different digestion methods (NiS fire assay and the use of a high-pressure asher) within the analytical uncertainties of each other. Significant difference in reproducibility between Ru, Ir, Pt and Os group, and Pd and Re group was observed in the results for BHVO-2 and JA-2. By considering the error factors affecting analytical reproducibility, we concluded that the difference is ascribed to the sample heterogeneity of minor minerals enriched in Ru, Ir, Pt and Os

  17. Data Extraction Based on Page Structure Analysis

    Directory of Open Access Journals (Sweden)

    Ren Yichao

    2017-01-01

    Full Text Available The information we need has some confusing problems such as dispersion and different organizational structure. In addition, because of the existence of unstructured data like natural language and images, extracting local content pages is extremely difficult. In the light of of the problems above, this article will apply a method combined with page structure analysis algorithm and page data extraction algorithm to accomplish the gathering of network data. In this way, the problem that traditional complex extraction model behave poorly when dealing with large-scale data is perfectly solved and the page data extraction efficiency is also boosted to a new level. In the meantime, the article will also make a comparison about pages and content of different types between the methods of DOM structure based on the page and HTML regularities of distribution. After all of those, we may find a more efficient extract method.

  18. Dilution Confusion: Conventions for Defining a Dilution

    Science.gov (United States)

    Fishel, Laurence A.

    2010-01-01

    Two conventions for preparing dilutions are used in clinical laboratories. The first convention defines an "a:b" dilution as "a" volumes of solution A plus "b" volumes of solution B. The second convention defines an "a:b" dilution as "a" volumes of solution A diluted into a final volume of "b". Use of the incorrect dilution convention could affect…

  19. State of the art regarding the safety analysis of boron dilution events in Germany

    International Nuclear Information System (INIS)

    Kliem, S.; Rohde, U.

    2006-01-01

    In the German practice of considering boron dilution transients (BDT) in safety analysis reports (SAR), a strongly conservative approach is applied, although it is not explicitly requested in German rules and guidelines for SAR. The approach is based on recommendations of the German Gesellschaft fuer Anlagen- und Reaktorsicherheit (GRS) and the technical expert organizations (TUV) and accepted by the Reactor Safety Commission (RSK) and is currently followed by the industries and the facilities . No final recommendation and guidelines exist, because the item is subject of comprehensive discussions and research in Germany currently. This conservative approach is based on a combination of analytical and experimental steps. First of all, in a series of thermal hydraulic system code calculations, the bounding scenarios are determined which lead to maximum realistic (under the conditions assumed for nuclear safety verification calculations) volumes of the lower-borated coolant which can be transported to the reactor core by re-establishing circulation in the primary circuit. These are mainly small break loss of coolant accidents (SBLOCA), during which the decay heat is removed from the core by the reflux-condenser regime. The position and maximum size of lower-borated slugs are identified, and the circulation re-start conditions are determined. The main SBLOCA scenarios are verified on experiments at large scale test facilities (e.g. PKL in Germany). While in the integral tests, the formation and transport of the slugs in the loops is assessed, the mixing is investigated in detail in dedicated mixing test facilities (ROCOM) using the boundary conditions either from the integral tests or from the system code calculations. In this way, the minimum boron concentration at the core inlet, which is reached during the transient, is estimated. Additionally, the minimum boron concentration is calculated by using computational fluid dynamics (CFD) codes. The critical boron

  20. Structural, morphological and magnetic analysis of Cd–Co–S dilute magnetic semiconductor nanofilms

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Suresh [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India); Negi, N.S. [Department of Physics, Himachal Pradesh University, Summer Hill, Shimla, Himachal Pradesh 171005 (India); Katyal, S.C. [Department of Physics, Jaypee Institute of Information Technology, Sec-128, Noida, Uttar Pradesh 201301 (India); Sharma, Pankaj, E-mail: pankaj.sharma@juit.ac.in [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India); Sharma, Vineet [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India)

    2014-10-01

    Cd{sub 1−x}Co{sub x}S dilute magnetic semiconductor nanofilms (0≤x≤0.08 at%) deposited by chemical bath deposition have been investigated using grazing angle x-ray diffraction, atomic force microscopy and vibrating sample magnetometer. The introduction of Co{sup 2+} ions in CdS structure induces structural disorders and hence, results in degradation of crystallinity. The crystallite size, interplanar spacing and lattice parameter ratio decrease with increasing Co{sup 2+} concentration in CdS. The diamagnetic state of CdS disappears with increase in Co concentration and films with x>0.02 exhibit ferromagnetism. This may be explained in terms of the spin–orbit interactions and Co{sup 2+} ion induced the lattice defects and phase separation. - Highlights: • Cd{sub 1−x}Co{sub x}S dilute magnetic semiconductor nanofilms (0≤x≤0.08 at%) deposited by CBD. • The diamagnetic state of CdS vanishes for x=0.02. • For x>0.02, dilute magnetic semiconductor nanofilms shows a ferromagnetic state.

  1. Mixotrophic growth and biochemical analysis of Chlorella vulgaris cultivated with diluted monosodium glutamate wastewater.

    Science.gov (United States)

    Ji, Yan; Hu, Wenrong; Li, Xiuqing; Ma, Guixia; Song, Mingming; Pei, Haiyan

    2014-01-01

    Monosodium glutamate wastewater (MSGW) is a potential medium for microbial cultivation because of containing abundant organic nutrient. This paper seeks to evaluate the feasibility of growing Chlorella vulgaris with MSGW and assess the influence of MSGW concentration on the biomass productivity and biochemical compositions. The MSGW diluted in different concentrations was prepared for microalga cultivation. C. vulgaris growth was greatly promoted with MSGW compared with the inorganic BG11 medium. C. vulgaris obtained the maximum biomass concentration (1.02 g/L) and biomass productivity (61.47 mg/Ld) with 100-time diluted MSGW. The harvested biomass was rich in protein (36.01-50.64%) and low in lipid (13.47-25.4%) and carbohydrate (8.94-20.1%). The protein nutritional quality and unsaturated fatty acids content of algal increased significantly with diluted MSGW. These results indicated that the MSGW is a feasible alternative for mass cultivation of C. vulgaris. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. Neutron activation analysis of medicinal plant extracts

    International Nuclear Information System (INIS)

    Vaz, S.M.; Saiki, M.; Vasconcellos, M.B.A.; Sertie, J.A.A.

    1995-01-01

    Instrumental neutron activation analysis was applied to the determination of the elements Br, Ca, Cl, Cs, Fe, K, La, Mg, Mn, Na, Rb and Zn in medicinal extracts obtained from Centella asiatica, Citrus aurantium L., Achyrolcline satureoides DC, Casearia sylvestris, Solano lycocarpum, Zingiber officinale Roscoe, Solidago microglossa and Stryphnondedron barbatiman plants. The elements Hg and Se were determined using radiochemical separation by means of retention of Se in HMD inorganic exchanger and solvent extraction of Hg by bismuth diethyldithiocarbamate solution. Precision and accuracy of the results were evaluated by analyzing biological reference materials. The therapeutic action of some elements found in plant extracts analyzed is briefly discussed. (author). 15 refs., 5 tabs

  3. Experimental design-based isotope-dilution SPME-GC/MS method development for the analysis of smoke flavouring products.

    Science.gov (United States)

    Giri, Anupam; Zelinkova, Zuzana; Wenzl, Thomas

    2017-12-01

    For the implementation of Regulation (EC) No 2065/2003 related to smoke flavourings used or intended for use in or on foods a method based on solid-phase micro extraction (SPME) GC/MS was developed for the characterisation of liquid smoke products. A statistically based experimental design (DoE) was used for method optimisation. The best general conditions to quantitatively analyse the liquid smoke compounds were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre, 60°C extraction temperature, 30 min extraction time, 250°C desorption temperature, 180 s desorption time, 15 s agitation time, and 250 rpm agitation speed. Under the optimised conditions, 119 wood pyrolysis products including furan/pyran derivatives, phenols, guaiacol, syringol, benzenediol, and their derivatives, cyclic ketones, and several other heterocyclic compounds were identified. The proposed method was repeatable (RSD% <5) and the calibration functions were linear for all compounds under study. Nine isotopically labelled internal standards were used for improving quantification of analytes by compensating matrix effects that might affect headspace equilibrium and extractability of compounds. The optimised isotope dilution SPME-GC/MS based analytical method proved to be fit for purpose, allowing the rapid identification and quantification of volatile compounds in liquid smoke flavourings.

  4. Cadmium determination in natural waters at the limit imposed by European legislation by isotope dilution and TiO2 solid-phase extraction.

    Science.gov (United States)

    García-Ruiz, Silvia; Petrov, Ivan; Vassileva, Emilia; Quétel, Christophe R

    2011-11-01

    The cadmium content in surface water is regulated by the last European Water Framework Directive to a maximum between 0.08 and 0.25 μg L(-1) depending on the water type and hardness. Direct measurement of cadmium at this low level is not straightforward in real samples, and we hereby propose a validated method capable of addressing cadmium content below μg L(-1) level in natural water. It is based on solid-phase extraction using TiO(2) nanoparticles as solid sorbent (0.05 g packed in mini-columns) to allow the separation and preconcentration of cadmium from the sample, combined to direct isotope dilution and detection by inductively coupled plasma mass spectrometry (ID-ICP-MS). The extraction setup is miniaturised and semi-automated to reduce risks of sample contamination and improve reproducibility. Procedural blanks for the whole measurement process were 5.3 ± 2.8 ng kg(-1) (1 s) for 50 g of ultrapure water preconcentrated ten times. Experimental conditions influencing the separation (including loading pH, sample flow rates, and acid concentration in the eluent) were evaluated. With isotope dilution the Cd recovery rate does not have to be evaluated carefully. Moreover, the mathematical model associated to IDMS is known, and provides transparency for the uncertainty propagation. Our validation protocol was in agreement with guidelines of the ISO/IEC 17025 standard (chapter 5.4.5). Firstly, we assessed the experimental factors influencing the final result. Secondly, we compared the isotope ratios measured after our separation procedure to the reference values obtained with a different protocol for the digested test material IMEP-111 (mineral feed). Thirdly, we analysed the certified reference material BCR-609 (groundwater). Finally, combined uncertainties associated to our results were estimated according to ISO-GUM guidelines (typically, 3-4% k = 2 for a cadmium content of around 100 ng kg(-1)). We applied the developed method to the groundwater and wastewater

  5. Cadmium determination in natural waters at the limit imposed by European legislation by isotope dilution and TiO{sub 2} solid-phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Ruiz, Silvia; Quetel, Christophe R. [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); Petrov, Ivan [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); Universite Libre de Bruxelles, Department of Earth and Environmental Sciences, Brussels (Belgium); Vassileva, Emilia [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); IAEA-Marine Environment Laboratories, Monaco (Monaco)

    2011-11-15

    The cadmium content in surface water is regulated by the last European Water Framework Directive to a maximum between 0.08 and 0.25 {mu}g L{sup -1} depending on the water type and hardness. Direct measurement of cadmium at this low level is not straightforward in real samples, and we hereby propose a validated method capable of addressing cadmium content below {mu}g L{sup -1} level in natural water. It is based on solid-phase extraction using TiO{sub 2} nanoparticles as solid sorbent (0.05 g packed in mini-columns) to allow the separation and preconcentration of cadmium from the sample, combined to direct isotope dilution and detection by inductively coupled plasma mass spectrometry (ID-ICP-MS). The extraction setup is miniaturised and semi-automated to reduce risks of sample contamination and improve reproducibility. Procedural blanks for the whole measurement process were 5.3 {+-} 2.8 ng kg{sup -1} (1 s) for 50 g of ultrapure water preconcentrated ten times. Experimental conditions influencing the separation (including loading pH, sample flow rates, and acid concentration in the eluent) were evaluated. With isotope dilution the Cd recovery rate does not have to be evaluated carefully. Moreover, the mathematical model associated to IDMS is known, and provides transparency for the uncertainty propagation. Our validation protocol was in agreement with guidelines of the ISO/IEC 17025 standard (chapter 5.4.5). Firstly, we assessed the experimental factors influencing the final result. Secondly, we compared the isotope ratios measured after our separation procedure to the reference values obtained with a different protocol for the digested test material IMEP-111 (mineral feed). Thirdly, we analysed the certified reference material BCR-609 (groundwater). Finally, combined uncertainties associated to our results were estimated according to ISO-GUM guidelines (typically, 3-4% k = 2 for a cadmium content of around 100 ng kg{sup -1}). We applied the developed method to the

  6. Antimicrobial activity and phytochemical analysis of crude extracts and essential oils from medicinal plants.

    Science.gov (United States)

    Silva, N C C; Barbosa, L; Seito, L N; Fernandes, A

    2012-01-01

    We aimed to establish a phytochemical analysis of the crude extracts and performed GC-MS of the essential oils (EOs) of Eugenia uniflora L. (Myrtaceae) and Asteraceae species Baccharis dracunculifolia DC, Matricaria chamomilla L. and Vernonia polyanthes Less, as well as determining their antimicrobial activity. Establishment of the minimal inhibitory concentrations of the crude extracts and EOs against 16 Staphylococcus aureus and 16 Escherichia coli strains from human specimens was carried out using the dilution method in Mueller-Hinton agar. Some phenolic compounds with antimicrobial properties were established, and all EOs had a higher antimicrobial activity than the extracts. Matricaria chamomilla extract and E. uniflora EO were efficient against S. aureus strains, while E. uniflora and V. polyanthes extracts and V. polyanthes EO showed the best antimicrobial activity against E. coli strains. Staphylococcus aureus strains were more susceptible to the tested plant products than E. coli, but all natural products promoted antimicrobial growth inhibition.

  7. Transition edge sensor-energy-dispersive spectrometer (TES-EDS) using a cryogen-free dilution refrigerator for material analysis

    International Nuclear Information System (INIS)

    Tanaka, Keiichi; Odawara, Akikazu; Nagata, Atsushi; Ikeda, Masanori; Baba, Yukari; Nakayama, Satoshi; Chinone, Kazuo

    2006-01-01

    A cryogen-free energy-dispersive spectrometer (EDS) using a transition edge sensor (TES) was developed for material analysis. This system can maintain a temperature at 130 mK within 30 μK, and has good energy resolution (19 eV for Mn-Kα) for long-time measurement with a drift in the DC level of less than 0.02 eV/min. This system utilizes a dilution refrigerator (φ 272 mmxheight 572 mm) and has a snout (370 mm long and φ25 mm) similar to that in a conventional EDS system. The dilution refrigerator is pre-cooled by a GM refrigerator. A flexible tube between the dilution refrigerator and GM refrigerator damps the mechanical vibration of the GM refrigerator. Two shields (4 and 80 K) thermally protect the Cu rod (φ8 mm) cooled to be 100 mK. Windows composed of polyimide+Al film allow X-ray detection above the C-Kα line. A TES (6 mmx6 mm) and array SQUID amplifier (1.5 mmx3 mm) are mounted on top of the Cu rod. For Mn-Kα, the pulse height is 5.5 μA and decay time (τ eff ) is 90 μs. The maximum count rate (1/20 τ eff ) is estimated at about 500 cps

  8. Isotope-dilution gas chromatography-mass spectrometry method for the analysis of hydroxyurea.

    Science.gov (United States)

    Garg, Uttam; Scott, David; Frazee, Clint; Kearns, Gregory; Neville, Kathleen

    2015-06-01

    Hydroxyurea is used in the treatment of various malignancies and sickle cell disease. There are limited studies on the pharmacokinetics of hydroxyurea, particularly in pediatric patients. An accurate, precise, and sensitive method is needed to support such studies and to monitor therapeutic adherence. We describe a novel gas chromatography-mass spectrometry (GC-MS) method for the determination of hydroxyurea concentration in plasma using stable labeled hydroxyurea C N2 as an internal standard. The method involved an organic extraction followed by the preparation of trimethylsilyl (TMS) derivatives of hydroxyurea for GC-MS selected ion-monitoring analysis. The following mass-to-charge (m/z) ratio ions for silated hydroxyurea and hydroxyurea C N2 were monitored: hydroxyurea-quantitative ion 277, qualifier ions 292 and 249; hydroxyurea C N2-quantitative ion 280, qualifier ion 295. This method was evaluated for reportable range, accuracy, within-run and between-run imprecisions, and limits of quantification. The reportable range for the method was 0.1-100 mcg/mL. All results were accurate within an allowable error of 15%. Within-run and between-run imprecisions were hydroxyurea described here is accurate, sensitive, precise, and robust. Its characteristics make the method suitable for supporting pharmacokinetic studies and/or clinical therapeutic monitoring.

  9. On the nitrogen isotope dilution analysis by means of the automated NA-5A type 15N-analyzer

    International Nuclear Information System (INIS)

    Faust, H.; Mueller, G.; Stoerl, H.J.

    1976-01-01

    The analytical conditions are investigated under which quantitative nitrogen determination through isotope dilution analysis is possible using the NA-5A type 15 N-analyzer. Calculation of the nitrogen quantity, estimation of the maximum error and the evaluation technique are considered in detail. Test analyses performed on ammonia, urea, and amino acid nitrogen model solutions labelled in different ways yielded good correspondence with preset values. This technique was applied to determine the nitrogen content of biomedical materials. A working scheme for direct quantitative determination of ammonia-N, urea-N, and total-N in urine is presented. (author)

  10. Finite-size-scaling analysis of subsystem data in the dilute Ising model

    International Nuclear Information System (INIS)

    Hennecke, M.

    1993-01-01

    Monte Carlo simulation results for the magnetization of subsystems of finite lattices are used to determine the critical temperature and a critical exponent of the simple-cubic Ising model with quenched site dilution, at a concentration of p=40%. Particular attention is paid to the effect of the finite size of the systems from which the subsystem results are obtained. This finiteness of the lattices involved is shown to be a source of large deviations of critical temperatures and exponents estimated from subsystem data from their values in the thermodynamic limit. By the use of different lattice sizes, the results T c (40%)=1.209±0.002 and ν(40%)=0.78±0.01 could be extrapolated

  11. Isotope dilution analysis for urinary fentanyl and its main metabolite, norfentanyl, in patients by isotopic fractionation using capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan). Faculty of Pharmacy and Pharmaceutical Sciences; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

    1998-07-01

    Isotope dilution analysis was applied to determine urinary excretion of fentanyl (FT) and its main metabolite, norfentanyl (Nor-FT), by isotopic fractionation using a capillary gas chromatograph equipped with a surface ionization detector (SID). Urinary FT was determined quantitatively in the range of 0.4-40 ng/ml using deuterium labeled FT (FT-{sup 2}H{sub 19}), as an internal standard. We also performed isotope dilution analysis of Nor-FT in urine. N-Alkylation was necessary to sensitively detect Nor-FT with SID. Methyl derivative was selected from 3 kinds of N-alkyl derivatives to increase sensitivity and peak resolution, and to prevent interference with urinary compound. Nor-FT concentration was quantitatively determined in the range of 10-400 ng/ml using deuterium labeled Nor-FT (Nor-FT-{sup 2}H{sub 10}). No endogenous compounds or concomitant drugs interfered with the detection of FT and Nor-FT in the urine of patients. The present method will be useful for pharmacokinetic studies and the evaluation of drug interactions in FT metabolism. (author)

  12. The IDA-80 measurement evaluation programme on mass spectrometric isotope dilution analysis of uranium and plutonium. Vol. 1

    International Nuclear Information System (INIS)

    Beyrich, W.; Golly, W.; Spannagel, G.; Kernforschungszentrum Karlsruhe G.m.b.H.; Bievre, P. de; Wolters, W.

    1984-12-01

    The main objective was the acquisition of basic data on the uncertainties involved in the mass spectrometric isotope dilution analysis as applied to the determination of uranium and plutonium in active feed solutions of reprocessing plants. The element concentrations and isotopic compositions of all test materials used were determined by CBNM and NBS with high accuracy. The more than 60000 analytical data reported by the participating laboratories were evaluated by statistical methods applied mainly to the calculation of estimates of the variances for the different uncertainty components contributing to the total uncertainty of this analytical technique. Attention was given to such topics as sample ageing, influence of fission products, spike calibration, ion fractionation, Pu-241 decay correction, minor isotope measurement and errors in data transfer. Furthermore, the performance of the 'dried sample' technique and the 'in-situ' spiking method of undiluted samples of reprocessing fuel solution with U-235/Pu-242 metal alloy spikes, were tested successfully. Considerable improvement of isotope dilution analysis in this safeguards relevant application during the last decade is shown as compared to the results obtained in the IDA-72 interlaboratory experiment, organized by KfK in 1972 on the same subject. (orig./HP) [de

  13. Isotope dilution analysis for urinary fentanyl and its main metabolite, norfentanyl, in patients by isotopic fractionation using capillary gas chromatography

    International Nuclear Information System (INIS)

    Sera, Shoji; Goromaru, Tsuyoshi; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki

    1998-01-01

    Isotope dilution analysis was applied to determine urinary excretion of fentanyl (FT) and its main metabolite, norfentanyl (Nor-FT), by isotopic fractionation using a capillary gas chromatograph equipped with a surface ionization detector (SID). Urinary FT was determined quantitatively in the range of 0.4-40 ng/ml using deuterium labeled FT (FT- 2 H 19 ), as an internal standard. We also performed isotope dilution analysis of Nor-FT in urine. N-Alkylation was necessary to sensitively detect Nor-FT with SID. Methyl derivative was selected from 3 kinds of N-alkyl derivatives to increase sensitivity and peak resolution, and to prevent interference with urinary compound. Nor-FT concentration was quantitatively determined in the range of 10-400 ng/ml using deuterium labeled Nor-FT (Nor-FT- 2 H 10 ). No endogenous compounds or concomitant drugs interfered with the detection of FT and Nor-FT in the urine of patients. The present method will be useful for pharmacokinetic studies and the evaluation of drug interactions in FT metabolism. (author)

  14. Multi-element determination in environmental samples by mass spectrometric isotope dilution analysis using thermal ionization. Pt. 2

    International Nuclear Information System (INIS)

    Hilpert, K.; Waidmann, E.

    1988-01-01

    An analytical procedure for the multi-element analysis of the elements Fe, Ni, Cu, Zn, Ga, Rb, Sr, Cd, Ba, Tl, and Pb in pine needles by mass spectrometric isotope dilution analysis using thermal ionization has been reported in Part I of this paper. This procedure is now transferred to the non-vegetable material 'Oyster Tissue' (Standard Reference Material 1566, National Bureau of Standards, USA). By a modification of the analytical procedure, it was possible to determine Cr in this material in addition to the aforementioned elements. No concentrations are certified for the elements Ga, Ba and Tl analyzed in this work. The concentrations of the remaining elements obtained by the multi-element analysis agree well with those certified. (orig.)

  15. Limiting dilution analysis of the stem cells for T cell lineage

    International Nuclear Information System (INIS)

    Katsura, Y.; Kina, T.; Amagai, T.; Tsubata, T.; Hirayoshi, K.; Takaoki, Y.; Sado, T.; Nishikawa, S.I.

    1986-01-01

    Stem cell activities of bone marrow, spleen, thymus, and fetal liver cells for T cell lineage were studied comparatively by transferring the cells from these organs through i.v. or intrathymus (i.t.) route into right leg- and tail-shielded (L-T-shielded) and 900 R-irradiated recipient mice, which were able to survive without supplying hemopoietic stem cells. Cells from B10.Thy-1.1 (H-2b, Thy-1.1) mice were serially diluted and were transferred into L-T-shielded and irradiated C57BL/6 (H-2b, Thy-1.2) mice, and 21 days later the thymus cells of recipient mice were assayed for Thy-1.1+ cells by flow cytofluorometry. The percentage of recipient mice possessing donor-type T cells was plotted against the number of cells transferred, and the stem cell activity in each cell source was expressed as the 50% positive value, the number of donor cells required for generating donor-type T cells in the thymuses of 50% of recipient mice. In i.v. transfer experiments, the activity of bone marrow cells was similar to that of fetal liver cells, and about 100 times and nearly 1000 times higher than those of spleen cells and thymus cells, respectively. In i.t. transfer experiments, the number of cells required for generating donor-type T cells was much lower than that in i.v. transfer experiments, although the ratio in 50% positive values between i.v. and i.t. transfers differed among cell sources. In i.t. transfers, the 50% positive value of bone marrow cells was five times, 400 times, and 500 times higher than that of fetal liver cells, spleen cells, and thymus cells, respectively. Our previous finding that stem cells are enriched in the spleens of mice which were whole body-irradiated and marrow-reconstituted 7 days earlier was confirmed also by the present limiting dilution assay carried out in i.v. as well as i.t. transfers

  16. Dilute Russel Viper Venom Time analysis in a Haematology Laboratory: An audit.

    Science.gov (United States)

    Kruger, W; Meyer, P W A; Nel, J G

    2018-04-17

    To determine whether the current set of evaluation criteria used for dilute Russel Viper Venom Time (dRVVT) investigations in the routine laboratory meet expectation and identify possible shortcomings. All dRVVT assays requested from January 2015 to December 2015 were appraised in this cross-sectional study. The raw data panels were compared with the new reference interval, established in 2016, to determine the sequence of assays that should have been performed. The interpretive comments were audited, and false-negative reports identified. Interpretive comments according to three interpretation guidelines were compared. The reagent cost per assay was determined, and reagent cost wastage, due to redundant tests, was calculated. Only ~9% of dRVVT results authorized during 2015 had an interpretive comment included in the report. ~15% of these results were false-negative interpretations. There is a significant statistical difference in interpretive comments between the three interpretation methods. Redundant mixing tests resulted in R 7477.91 (~11%) reagent cost wastage in 2015. We managed to demonstrate very evident deficiencies in our own practice and managed to establish a standardized workflow that will potentially render our service more efficient and cost effective, aiding clinicians in making improved treatment decisions and diagnoses. Furthermore, it is essential that standard operating procedures be kept up to date and executed by all staff in the laboratory. © 2018 John Wiley & Sons Ltd.

  17. Analysis of Zero Reynolds Shear Stress Appearing in Dilute Surfactant Drag-Reducing Flow

    Directory of Open Access Journals (Sweden)

    Weiguo Gu

    2011-01-01

    Full Text Available Dilute surfactant solution of 25 ppm in the two-dimensional channel is investigated experimentally compared with water flow. Particle image velocimetry (PIV system is used to take 2D velocity frames in the streamwise and wall-normal plane. Based on the frames of instantaneous vectors and statistical results, the phenomenon of zero Reynolds shear stress appearing in the drag-reducing flow is discussed. It is found that 25 ppm CTAC solution exhibits the highest drag reduction at Re = 25000 and loses drag reduction completely at Re = 40000. When drag reduction lies in the highest, Reynolds shear stress disappears and reaches zero although the RMS of the velocity fluctuations is not zero. By the categorization in four quadrants, the fluctuations of 25 ppm CTAC solution are distributed in all four quadrants equally at Re = 25000, which indicates that turnaround transportation happens in drag-reducing flow besides Reynolds shear stress transportation. Moreover, the contour distribution of streamwise velocity and the fluctuations suggests that turbulence transportation is depressed in drag-reducing flow. The viscoelasticity is possible to decrease the turbulence transportation and cause the turnaround transportation.

  18. The application of three-phase liquid-liquid extraction to the analysis of bismuth and tellurium in sulphide concentrates

    International Nuclear Information System (INIS)

    Nicholas, D.J.

    1976-01-01

    An extraction system consisting of one aqueous and two organic phases is described. Diantipyrylmethane (DAM) is used as the extractant for bismuth and tellurium, which are extracted into the smaller of the two organic phases from nitric acid and perchloric acid respectively. The extraction efficiency is in the range of 90 to 95 per cent, compensation for incomplete extraction being made by the technique of standard addition. Copper, lead, and zinc are not extracted in either procedure. When the solutions contain high concentrations of iron, thioglycolic acid is used as a masking agent for iron in the extraction of bismuth. Atomic-absorption spectrophotometry is used for the analysis of the third phase after it has been diluted with methanol. The precision for bismuth and tellurium is in the range of 3 to 4 per cent. The accuracy, as ascertained from comparative analyses of sulphide concentrates, is good

  19. An application of nitrogen microwave-induced plasma mass spectrometry to isotope dilution analysis of selenium in marine organisms

    Energy Technology Data Exchange (ETDEWEB)

    Shirasaki, Toshihiro [Hitachi Instruments Engineering Co. Ltd., Hitachinaka, Ibaraki (Japan); Yoshinaga, Jun; Morita, Masatoshi; Okumoto, Toyoharu; Oishi, Konosuke

    1996-01-01

    Nitrogen microwave-induced plasma mass spectrometry was studied for its applicability to the isotope dilution analysis of selenium in biological samples. Spectroscopic interference by calcium, which is present in high concentrations in biological samples, was investigated. No detectable background spectrum was observed for the major selenium isotopes of {sup 78}Se and {sup 80}Se. No detectable interferences by sodium, potassium, calcium and phosphorus on the isotope ratio {sup 80}Se/{sup 78}Se were observed up to concentration of 200 mg/ml. The method was applied to the analysis of selenium in biological reference materials of marine organisms. The results showed good agreement between the certified and found values. (author).

  20. LC-HR-MS/MS standard urine screening approach: Pros and cons of automated on-line extraction by turbulent flow chromatography versus dilute-and-shoot and comparison with established urine precipitation.

    Science.gov (United States)

    Helfer, Andreas G; Michely, Julian A; Weber, Armin A; Meyer, Markus R; Maurer, Hans H

    2017-02-01

    Comprehensive urine screening for drugs and metabolites by LC-HR-MS/MS using Orbitrap technology has been described with precipitation as simple workup. In order to fasten, automate, and/or simplify the workup, on-line extraction by turbulent flow chromatography and a dilute-and-shoot approach were developed and compared. After chromatographic separation within 10min, the Q-Exactive mass spectrometer was run in full scan mode with positive/negative switching and subsequent data dependent acquisition mode. The workup approaches were validated concerning selectivity, recovery, matrix effects, process efficiency, and limits of identification and detection for typical drug representatives and metabolites. The total workup time for on-line extraction was 6min, for the dilution approach 3min. For comparison, the established urine precipitation and evaporation lasted 10min. The validation results were acceptable. The limits for on-line extraction were comparable with those described for precipitation, but lower than for dilution. Thanks to the high sensitivity of the LC-HR-MS/MS system, all three workup approaches were sufficient for comprehensive urine screening and allowed fast, reliable, and reproducible detection of cardiovascular drugs, drugs of abuse, and other CNS acting drugs after common doses. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Development of a mass spectrometrical isotope dilution analysis for determination of trace iodine levels and its application for food samples

    International Nuclear Information System (INIS)

    Schindlmeier, W.

    1984-01-01

    A mass spectrometrical isotope dilution procedure for the determination of trace amounts of iodine in various materials was developed using 129 I as indicator isotope, based on the determination of the 129 I/ 127 I isotope relationship. Negative thermionization was used as ionization method. The analysis procedure, which worked with a standard deviation of between 0,1 and 10% (depending on material tested), was used to determine the iodine level of table salt - both iodized and normal salt (3-6 ppm and less than 0,006 ppm respectively), and food samples with an organic matrix. For comparison the iodine levels were also measured with an iodine-selective electrode. Special preparation and separation procedures were done to suit the sample material. A comparison of the levels of iodine concentration in various powdered milks which were measured by international collaborators using varying methods shows the superior reproducibility of the MS-IDA. (RB) [de

  2. Trace analysis of U, Th and other heavy metals in high purity aluminium with isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Beer, B.; Heumann, K.G.

    1992-01-01

    A method for the determination of very low concentrations of U, Th, Fe, Zn, Tl, Cd, Cu and Ag in high purity aluminium with isotope dilution mass spectrometry (IDMS) is developed using a compact and cost-efficient thermal ionization quadrupole mass spectrometer. The detection limits obtained are (in ng/g):U=0.018, Th=0.06, Fe=82, Zn=86, Tl=0.2, Cd=4, Cu=1, Ag=2.6. By this method it is possible to determine the α-emitters U and Th in aluminium down to the sub-ng/g level with good precision of 0.4-10% and 0.5-5%, respectively. The results should also be accurate because IDMS is a reliable analytical method. The dissolution of aluminium is carried out by aqua regia followed by the trace/matrix separation and the isolation of the trace elements by anion exchange chromatography (U, Th, Zn, Tl, Cd), electrodeposition (Cu, Ag) and extraction (Fe). Different aluminium samples are analysed by IDMS and the results are compared with those of other methods. (orig.)

  3. Raman Analysis of Dilute Aqueous Samples by Localized Evaporation of Submicroliter Droplets on the Tips of Superhydrophobic Copper Wires.

    Science.gov (United States)

    Cheung, Melody; Lee, Wendy W Y; McCracken, John N; Larmour, Iain A; Brennan, Steven; Bell, Steven E J

    2016-04-19

    Raman analysis of dilute aqueous solutions is normally prevented by their low signal levels. A very general method to increase the concentration to detectable levels is to evaporate droplets of the sample to dryness, creating solid deposits which are then Raman probed. Here, superhydrophobic (SHP) wires with hydrophilic tips have been used as supports for drying droplets, which have the advantage that the residue is automatically deposited at the tip. The SHP wires were readily prepared in minutes using electroless galvanic deposition of Ag onto copper wires followed by modification with a polyfluorothiol (3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro-1-decanethiol, HDFT). Cutting the coated wires with a scalpel revealed hydrophilic tips which could support droplets whose maximum size was determined by the wire diameter. Typically, 230 μm wires were used to support 0.6 μL droplets. Evaporation of dilute melamine droplets gave solid deposits which could be observed by scanning electron microscopy (SEM) and Raman spectroscopy. The limit of detection for melamine using a two stage evaporation procedure was 1 × 10(-6) mol dm(-3). The physical appearance of dried droplets of sucrose and glucose showed that the samples retained significant amounts of water, even under high vacuum. Nonetheless, the Raman detection limits of sucrose and glucose were 5 × 10(-4) and 2.5 × 10(-3) mol dm(-3), respectively, which is similar to the sensitivity reported for surface-enhanced Raman spectroscopy (SERS) detection of glucose. It was also possible to quantify the two sugars in mixtures at concentrations which were similar to those found in human blood through multivariate analysis.

  4. Supercritical extraction of oleaginous: parametric sensitivity analysis

    Directory of Open Access Journals (Sweden)

    Santos M.M.

    2000-01-01

    Full Text Available The economy has become universal and competitive, thus the industries of vegetable oil extraction must advance in the sense of minimising production costs and, at the same time, generating products that obey more rigorous patterns of quality, including solutions that do not damage the environment. The conventional oilseed processing uses hexane as solvent. However, this solvent is toxic and highly flammable. Thus the search of substitutes for hexane in oleaginous extraction process has increased in the last years. The supercritical carbon dioxide is a potential substitute for hexane, but it is necessary more detailed studies to understand the phenomena taking place in such process. Thus, in this work a diffusive model for semi-continuous (batch for the solids and continuous for the solvent isothermal and isobaric extraction process using supercritical carbon dioxide is presented and submitted to a parametric sensitivity analysis by means of a factorial design in two levels. The model parameters were disturbed and their main effects analysed, so that it is possible to propose strategies for high performance operation.

  5. Analysis of Water Extraction From Lunar Regolith

    Science.gov (United States)

    Hegde, U.; Balasubramaniam, R.; Gokoglu, S.

    2012-01-01

    Distribution of water concentration on the Moon is currently an area of active research. Recent studies suggest the presence of ice particles, and perhaps even ice blocks and ice-cemented regolith on the Moon. Thermal extraction of the in-situ water is an attractive means of sa tisfying water requirements for a lunar mission. In this paper, a model is presented to analyze the processes occurring during the heat-up of icy regolith and extraction of the evolved water vapor. The wet regolith is assumed to be present in an initially evacuated and sealed cell which is subsequently heated. The first step of the analysis invol ves calculating the gradual increase of vapor pressure in the closed cell as the temperature is raised. Then, in the second step, the cell is evacuated to low pressure (e.g., vacuum), allowing the water vapor to leave the cell and be captured. The parameters affecting water vap or pressure build-up and evacuation for the purpose of extracting water from lunar regolith are discussed in the paper. Some comparisons wi th available experimental measurements are also made.

  6. Analysis of Cyanide in Blood by Headspace-Isotope-Dilution-GC-MS

    DEFF Research Database (Denmark)

    Løbger, Lise Lotte; Petersen, Henning Willads; Andersen, Jens Enevold Thaulov

    2008-01-01

    An uncomplicated, rapid, automated procedure for the analysis of low cyanide concentrations in whole blood is reported. The analysis was performed by headspace gas chromatography and mass spectrometry in the (1H12C14N) and m/z 29 (1H13C15N). Carryover from cyanide adsorption onto the surface...

  7. Evaluation and validation of a single-dilution potency assay based upon serology of vaccines containing diphtheria toxoid: statistical analysis

    NARCIS (Netherlands)

    Marsman FR; Akkermans AM; Hendriksen CFM; de Jong WH

    1993-01-01

    This document presents the results of a validation study to the use of a single dilution assay in potency testing of the diphtheria component of DPT-polio vaccines. Based on historical data of multi-dilution assays on 27 consecutive batches a simulation study was performed to test the actual

  8. Analysis of several hazardous conditions for large transfer and back-dilution sequences in Tank 241-SY-101

    International Nuclear Information System (INIS)

    CW Stewart; LA Mahoney; WB Barton

    2000-01-01

    The first transfer of 89 kgal of waste and back-dilution of 61 kgal of water in Hanford Tank 241-SY-101 was accomplished December 18--20, 1999. Limits were placed on the transfer and back-dilution volumes because of concerns about potential gas release, crust sinking, and degradation of mixer pump performance. Additional transfers and back-dilutions are being planned that will bring the total to 500 kgal, which should dissolve a large fraction of the solids in the tank and dilute it well beyond the point where significant gas retention can occur. This report provides the technical bases for removing the limits on transfer and back-dilution volume by evaluating the potential consequences of several postulated hazardous conditions in view of the results of the first campaign and results of additional analyses of waste behavior

  9. Analysis of several hazardous conditions for large transfer and back-dilution sequences in Tank 241-SY-101

    Energy Technology Data Exchange (ETDEWEB)

    CW Stewart; LA Mahoney; WB Barton

    2000-01-28

    The first transfer of 89 kgal of waste and back-dilution of 61 kgal of water in Hanford Tank 241-SY-101 was accomplished December 18--20, 1999. Limits were placed on the transfer and back-dilution volumes because of concerns about potential gas release, crust sinking, and degradation of mixer pump performance. Additional transfers and back-dilutions are being planned that will bring the total to 500 kgal, which should dissolve a large fraction of the solids in the tank and dilute it well beyond the point where significant gas retention can occur. This report provides the technical bases for removing the limits on transfer and back-dilution volume by evaluating the potential consequences of several postulated hazardous conditions in view of the results of the first campaign and results of additional analyses of waste behavior.

  10. On-line double isotope dilution laser ablation inductively coupled plasma mass spectrometry for the quantitative analysis of solid materials.

    Science.gov (United States)

    Fernández, Beatriz; Rodríguez-González, Pablo; García Alonso, J Ignacio; Malherbe, Julien; García-Fonseca, Sergio; Pereiro, Rosario; Sanz-Medel, Alfredo

    2014-12-03

    We report on the determination of trace elements in solid samples by the combination of on-line double isotope dilution and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method requires the sequential analysis of the sample and a certified natural abundance standard by on-line IDMS using the same isotopically-enriched spike solution. In this way, the mass fraction of the analyte in the sample can be directly referred to the certified standard so the previous characterization of the spike solution is not required. To validate the procedure, Sr, Rb and Pb were determined in certified reference materials with different matrices, including silicate glasses (SRM 610, 612 and 614) and powdered samples (PACS-2, SRM 2710a, SRM 1944, SRM 2702 and SRM 2780). The analysis of powdered samples was carried out both by the preparation of pressed pellets and by lithium borate fusion. Experimental results for the analysis of powdered samples were in agreement with the certified values for all materials. Relative standard deviations in the range of 6-21% for pressed pellets and 3-21% for fused solids were obtained from n=3 independent measurements. Minimal sample preparation, data treatment and consumption of the isotopically-enriched isotopes are the main advantages of the method over previously reported approaches. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Automated 99Tc analysis in AW-101 and AN-107 ''diluted feed'' matrixes

    International Nuclear Information System (INIS)

    Egorov, O.B.; DE Kurath, D.E.

    2000-01-01

    A process monitor is needed by British Nuclear Fuels Limited, Inc. (BNFL Inc.) to measure total 99 Tc levels in column effluents during technetium removal from the aqueous fraction of the Hanford high-level tank wastes. The monitor must achieve detection limits of 1 x 10 -8 Ci/mL (0.6 microg/mL). Measurements must be done in near real time, with an analysis frequency of approximately15 min. The monitoring technology must be sufficiently simple and robust for unattended continuous operation in the plant settings

  12. Quantitative analysis and design of a spray aerosol inhaler. Part 1: effects of dilution air inlets and flow paths.

    Science.gov (United States)

    Longest, P Worth; Hindle, Michael

    2009-09-01

    The objective of this study was to evaluate the effects of modifying inhaler design variables on aerosol drug deposition within the mouthpiece for a representative spray system using a quantitative analysis and design approach. Capillary aerosol generation (CAG) was selected as a model spray aerosol system in conjunction with four prototype inhaler body and mouthpiece combinations. In vitro experiments were used to determine drug deposition in the mouthpiece and induction port. Validated computational fluid dynamics (CFD) simulations were implemented to establish relationships between design variables, transport characteristics, and aerosol drug deposition. Results of this study indicated that both the size of the upstream dilution air inlets and the flow pathway configuration near the spray nozzle significantly influenced aerosol transport and deposition. CFD results showed that the primary transport characteristics associated with drug deposition were turbulence intensity and the effective diameter of the mouthpiece. Strong quantitative correlations were developed between the identified transport characteristics and mouthpiece drug deposition. Based on quantitative analysis and design, turbulence intensity and effective mouthpiece diameter were identified as key transport characteristics within the design space that directly influenced aerosol deposition and may be used to predict and optimize drug delivery to the patient.

  13. A new method for the determination of NO2 traces using isotope dilution and mass spectrometry analysis

    International Nuclear Information System (INIS)

    Stevens, C.; Barat, F.; Nguyen Nghi, H.

    1975-01-01

    A new method for the determination of NO 2 traces, in the order of 1ppb (10 -9 ), in atmosphere and stratosphere is described. The method consists in an isotope dilution technique using 15 NO 2 , followed by the reduction of NO 2 to N 2 and a mass spectrometry analysis. A known amount of 15 NO 2 is added to the air samples. Then, NO 2 is separated from H 2 O, HNO 3 , CO 2 and N 2 O and transferred to a SiO 2 reactor by trapping at -196 deg C. In the reactor NO 2 is reduced to N 2 by reaction with electrolytic Cu heated at 580 deg C. The mass 29/mass 30 ratio corresponding to 15 N 14 N and 15 N 15 N is determined by mass spectrometry. The sensitivity of the method depends on the contamination introduced during the analysis of the sample (reagents, separation and measuring devices). The contamination is reproducible and in the order of 4.5+-0.5 10 -2 mm 3 N 2 [fr

  14. An approach for quantification of platinum distribution in tissues by LA-ICP-MS imaging using isotope dilution analysis.

    Science.gov (United States)

    Moraleja, I; Mena, M L; Lázaro, A; Neumann, B; Tejedor, A; Jakubowski, N; Gómez-Gómez, M M; Esteban-Fernández, D

    2018-02-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been revealed as a convenient technique for trace elemental imaging in tissue sections, providing elemental 2D distribution at a quantitative level. For quantification purposes, in the last years several approaches have been proposed in the literature such as the use of CRMs or matrix matched standards. The use of Isotope Dilution (ID) for quantification by LA-ICP-MS has been also described, being mainly useful for bulk analysis but not feasible for spatial measurements so far. In this work, a quantification method based on ID analysis was developed by printing isotope-enriched inks onto kidney slices from rats treated with antitumoral Pt-based drugs using a commercial ink-jet device, in order to perform an elemental quantification in different areas from bio-images. For the ID experiments 194 Pt enriched platinum was used. The methodology was validated by deposition of natural Pt standard droplets with a known amount of Pt onto the surface of a control tissue, where could be quantified even 50pg of Pt, with recoveries higher than 90%. The amount of Pt present in the whole kidney slices was quantified for cisplatin, carboplatin and oxaliplatin-treated rats. The results obtained were in accordance with those previously reported. The amount of Pt distributed between the medullar and cortical areas was also quantified, observing different behavior for the three drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Fuel reprocessing: safety analysis of extraction cycles

    International Nuclear Information System (INIS)

    Dinh, B.; Mauborgne, B.; Baron, P.; Mercier, J.P.

    1991-01-01

    An essential part of the safety analysis related to the extraction cycles of reprocessing plants, is the analysis of their behaviour during steady-state and transient operations, by means of simulation codes. These codes are based on the chemical properties of the main species involved (distribution coefficient and kinetics) and the hydrodynamics inside the contactors (mixer-settlers and pulsed columns). These codes have been consolidated by comparison of calculations with experimental results. The safety analysis is essentially performed in two steps. The first step is a parametric sensitivity analysis of the chemical flowsheet operated: the effect of a misadjustment (flowrate of feed, solvent, etc) is evaluated by successive steady-state calculations. These calculations help the identification of the sensitive parameters for the risk of plutonium accumulation, while indicating the permissible level of misadjustment. These calculations also serve to identify the parameters which should be measured during plant operation. The second step is the study of transient regimes, for the most sensitive parameters related to plutonium accumulation risk. The aim is to confirm the conclusions of the first step and to check that the characteristic process parameters chosen effectively allow, the early and reliable detection of any drift towards a plutonium accumulating regime. The procedures to drive the process backwards to a specified convenient steady-state regime from a drifting-state are also verified. The identification of the sensitive parameters, the process status parameters and the process transient analysis, allow a good control of process operation. This procedure, applied to the first purification cycle of COGEMA's UP3-A La Hague plant has demonstrated the total safety of facility operations

  16. Limiting-dilution analysis for the determination of leukemic cell frequencies after bone marrow decontamination with mafosfamide or merocyanine 540

    International Nuclear Information System (INIS)

    Porcellini, A.; Talevi, N.; Marchetti-Rossi, M.T.; Palazzi, M.; Manna, A.; Sparaventi, G.; Delfini, C.; Valentini, M.

    1987-01-01

    To stimulate a leukemia remission marrow, cell suspensions of normal human bone marrow were mixed with human acute lymphoblastic or myelogenous leukemic cells of the CCRF-SF, Nalm-6, and K-562 lines. The cell mixtures were incubated in vitro with mafosfamide (AZ) or with the photoreactive dye merocyanine 540 (MC-540). A quantity of 10(4) cells of the treated suspensions was dispensed into microculture plates, and graded cell numbers of the line used to contaminate the normal marrow were added. Limiting-dilution analysis was used to estimate the frequency of leukemia cells persisting after treatment with the decontaminating agents. Treatment with AZ or MC-540 produced a total elimination (ie, 6 logs or 5.3 logs respectively) of B cell acute leukemia cells (CCRF-SB), whereas nearly 1.7 logs and 2 logs of K-562 acute myelogenous blasts were still present in the cell mixtures after treatment with MC-540 and AZ, respectively. Treatment of the Nalm-6-contaminated cell mixtures with AZ resulted in 100% elimination of clonogenic cells, whereas nearly 80% decontamination was obtained with MC-540. Our results suggest that treatment with AZ could be an effective method of eliminating clonogenic tumor cells from human bone marrow. MC-540, shown by previous studies to spare sufficient pluripotential stem cells to ensure hemopoietic reconstitution in the murine model and in clinical application, has comparable effects and merits trials for possible clinical use in autologous bone marrow transplantation

  17. Limiting-dilution analysis for the determination of leukemic cell frequencies after bone marrow decontamination with mafosfamide or merocyanine 540

    Energy Technology Data Exchange (ETDEWEB)

    Porcellini, A.; Talevi, N.; Marchetti-Rossi, M.T.; Palazzi, M.; Manna, A.; Sparaventi, G.; Delfini, C.; Valentini, M.

    1987-11-01

    To stimulate a leukemia remission marrow, cell suspensions of normal human bone marrow were mixed with human acute lymphoblastic or myelogenous leukemic cells of the CCRF-SF, Nalm-6, and K-562 lines. The cell mixtures were incubated in vitro with mafosfamide (AZ) or with the photoreactive dye merocyanine 540 (MC-540). A quantity of 10(4) cells of the treated suspensions was dispensed into microculture plates, and graded cell numbers of the line used to contaminate the normal marrow were added. Limiting-dilution analysis was used to estimate the frequency of leukemia cells persisting after treatment with the decontaminating agents. Treatment with AZ or MC-540 produced a total elimination (ie, 6 logs or 5.3 logs respectively) of B cell acute leukemia cells (CCRF-SB), whereas nearly 1.7 logs and 2 logs of K-562 acute myelogenous blasts were still present in the cell mixtures after treatment with MC-540 and AZ, respectively. Treatment of the Nalm-6-contaminated cell mixtures with AZ resulted in 100% elimination of clonogenic cells, whereas nearly 80% decontamination was obtained with MC-540. Our results suggest that treatment with AZ could be an effective method of eliminating clonogenic tumor cells from human bone marrow. MC-540, shown by previous studies to spare sufficient pluripotential stem cells to ensure hemopoietic reconstitution in the murine model and in clinical application, has comparable effects and merits trials for possible clinical use in autologous bone marrow transplantation.

  18. Studies on the analysis of 25-hydroxyvitamin D{sub 3} by isotope-dilution liquid chromatography–tandem mass spectrometry using enzyme-assisted derivatisation

    Energy Technology Data Exchange (ETDEWEB)

    Abdel-Khalik, Jonas, E-mail: J.A.F.A.ABDEL-KHALIK.744116@swansea.ac.uk [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Crick, Peter J. [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Carter, Graham D. [DEQAS, Imperial College Healthcare NHS Trust, Clinical Biochemistry Department, Charing Cross Hospital, Fulham Palace Rd, London W6 8RF (United Kingdom); Makin, Hugh L. [Barts and the Royal London School of Medicine and Dentistry, Queen Mary University of London, London E1 2AD (United Kingdom); Wang, Yuqin [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Griffiths, William J., E-mail: w.j.griffiths@swansea.ac.uk [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom)

    2014-04-11

    Highlights: • New method for the analysis of 25-hydroxyvitamin D{sub 3} exploiting Girard P derivatisation. • Method also applicable to vitamin D{sub 3}, 1α,25- and 24,25-dihydroxyvitamin D{sub 3}. • By modification of the method 3-epi-25-hydroxyvitamin D{sub 3} can also be analysed. - Abstract: The total serum concentration of 25-hydroxyvitamins D (25-hydroxyvitamin D{sub 3} and 25-hydroxyvitamin D{sub 2}) is currently used as an indicator of vitamins D status. Vitamins D insufficiency is claimed to be associated with multiple diseases, thus accurate and precise reference methods for the quantification of 25-hydroxyvitamins D are needed. Here we present a novel enzyme-assisted derivatisation method for the analysis of vitamins D metabolites in adult serum utilising 25-[26,26,26,27,27,27-{sup 2}H{sub 6}]hydroxyvitamin D{sub 3} as the internal standard. Extraction of 25-hydroxyvitamins D from serum is performed with acetonitrile, which is shown to be more efficient than ethanol. Cholesterol oxidase is used to oxidize the 3β-hydroxy group in the vitamins D metabolites followed by derivatisation of the newly formed 3-oxo group with Girard P reagent. 17β-Hydroxysteroid dehydrogenase type 10 is shown to oxidize selectively the 3α-hydroxy group in the 3α-hydroxy epimer of 25-hydroxyvitamin D{sub 3}. Quantification is achieved by isotope-dilution liquid chromatography–tandem mass spectrometry. Recovery experiments for 25-hydroxyvitamin D{sub 3} performed on adult human serum give recovery of 102–106%. Furthermore in addition to 25-hydroxyvitamin D{sub 3}, 24,25-dihydroxyvitamin D{sub 3} and other uncharacterised dihydroxy metabolites, were detected in adult human serum.

  19. Studies on the analysis of 25-hydroxyvitamin D3 by isotope-dilution liquid chromatography–tandem mass spectrometry using enzyme-assisted derivatisation

    International Nuclear Information System (INIS)

    Abdel-Khalik, Jonas; Crick, Peter J.; Carter, Graham D.; Makin, Hugh L.; Wang, Yuqin; Griffiths, William J.

    2014-01-01

    Highlights: • New method for the analysis of 25-hydroxyvitamin D 3 exploiting Girard P derivatisation. • Method also applicable to vitamin D 3 , 1α,25- and 24,25-dihydroxyvitamin D 3 . • By modification of the method 3-epi-25-hydroxyvitamin D 3 can also be analysed. - Abstract: The total serum concentration of 25-hydroxyvitamins D (25-hydroxyvitamin D 3 and 25-hydroxyvitamin D 2 ) is currently used as an indicator of vitamins D status. Vitamins D insufficiency is claimed to be associated with multiple diseases, thus accurate and precise reference methods for the quantification of 25-hydroxyvitamins D are needed. Here we present a novel enzyme-assisted derivatisation method for the analysis of vitamins D metabolites in adult serum utilising 25-[26,26,26,27,27,27- 2 H 6 ]hydroxyvitamin D 3 as the internal standard. Extraction of 25-hydroxyvitamins D from serum is performed with acetonitrile, which is shown to be more efficient than ethanol. Cholesterol oxidase is used to oxidize the 3β-hydroxy group in the vitamins D metabolites followed by derivatisation of the newly formed 3-oxo group with Girard P reagent. 17β-Hydroxysteroid dehydrogenase type 10 is shown to oxidize selectively the 3α-hydroxy group in the 3α-hydroxy epimer of 25-hydroxyvitamin D 3 . Quantification is achieved by isotope-dilution liquid chromatography–tandem mass spectrometry. Recovery experiments for 25-hydroxyvitamin D 3 performed on adult human serum give recovery of 102–106%. Furthermore in addition to 25-hydroxyvitamin D 3 , 24,25-dihydroxyvitamin D 3 and other uncharacterised dihydroxy metabolites, were detected in adult human serum

  20. Chiral-glass transition in a diluted dipolar-interaction Heisenberg system

    International Nuclear Information System (INIS)

    Zhang Kaicheng; Liu Guibin; Zhu Yan

    2011-01-01

    Recently, numerical simulations reveal that a spin-glass transition can occur in the three-dimensional diluted dipolar system. By defining the chirality of triple spins in a diluted dipolar Heisenberg spin glass, we study the chiral ordering in the system using parallel tempering algorithm and heat bath method. The finite-size scaling analysis reveals that the system undergoes a chiral-glass transition at finite temperature. - Highlights: → We define the chirality in a diluted dipolar Heisenberg system. → The system undergoes a chiral-glass transition at finite temperature. → We extract the critical exponents of the chiral-glass transition.

  1. Limiting dilution analysis for precursor frequency of Con A-responsive mouse Thy-1+ dendritic epidermal cells

    International Nuclear Information System (INIS)

    Takashima, A.; Bergstresser, P.R.; Nixon-Fulton, J.L.; Tigelaar, R.E.

    1986-01-01

    The authors have recently demonstrated in vitro proliferation of mouse Thy-1 + dendritic epidermal cells (EC) to Con A and IL-2. The purpose of the present study was to utilize limiting dilution analysis to determine the precursor frequency (PF) of Con A-responsive cells within EC enriched by Isolymph centrifugation for Thy-1 + cells (IEC). AKR IEC were cultured in 96 well U-plates (25-75 cells/well) with 2 μg/ml Con A and 2 x 10 5 irradiated (1600 R) AKR spleen cells/well. Cultures were harvested after 7-21 days following 3 H-thymidine pulsing. Results indicated a PF within IEC of 1.5-4.5%. Inclusion of 10 U/ml IL-2 enhanced significantly the proliferation in positive wells but did not alter this PF. In AKR mice, monoclonal antibody 20-10-5S has been shown to react with Thy-1 + EC, but not with peripheral T cells. FACS purification of IEC using 20-10-5S indicated that Con A responsiveness resides exclusively within the 20-10-5S + population. The PF of Con A-responsive Thy-1 + EC was calculated by dividing the PF of IEC by the fraction of 20-10-5S + cells (13-30%) in the IEC suspension. A significant proportion of Thy-1 + EC (∼12%) were found to possess Con A proliferative capacity. These studies will facilitate analysis at a clonal level of possible functional and phenotypic heterogeneity within the Thy-1 + EC population

  2. Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material; Analisis de Estano en una Ceniza de Combustion mediante Espectrometria de Masas de Ionizacion Termica con Dilucion Isotopica

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez, C; Fernandez, M; Quejido, A L

    2006-07-01

    Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound exposure time. Due to the complex matrix of this fly ash material, a two-step purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs.

  3. Sensitive Quantification of Cannabinoids in Milk by Alkaline Saponification-Solid Phase Extraction Combined with Isotope Dilution UPLC-MS/MS.

    Science.gov (United States)

    Wei, Binnian; McGuffey, James E; Blount, Benjamin C; Wang, Lanqing

    2016-01-01

    Maternal exposure to marijuana during the lactation period-either active or passive-has prompted concerns about transmission of cannabinoids to breastfed infants and possible subsequent adverse health consequences. Assessing these health risks requires a sensitive analytical approach that is able to quantitatively measure trace-level cannabinoids in breast milk. Here, we describe a saponification-solid phase extraction approach combined with ultra-high-pressure liquid chromatography-tandem mass spectrometry for simultaneously quantifying Δ9-tetrahydrocannabinol (THC), cannabidiol (CBD), and cannabinol (CBN) in breast milk. We demonstrate for the first time that constraints on sensitivity can be overcome by utilizing alkaline saponification of the milk samples. After extensively optimizing the saponification procedure, the validated method exhibited limits of detections of 13, 4, and 66 pg/mL for THC, CBN, and CBD, respectively. Notably, the sensitivity achieved was significantly improved, for instance, the limits of detection for THC is at least 100-fold more sensitive compared to that previously reported in the literature. This is essential for monitoring cannabinoids in breast milk resulting from passive or nonrecent active maternal exposure. Furthermore, we simultaneously acquired multiple reaction monitoring transitions for 12 C- and 13 C-analyte isotopes. This combined analysis largely facilitated data acquisition by reducing the repetitive analysis rate for samples exceeding the linear limits of 12 C-analytes. In addition to high sensitivity and broad quantitation range, this method delivers excellent accuracy (relative error within ±10%), precision (relative standard deviation <10%), and efficient analysis. In future studies, we expect this method to play a critical role in assessing infant exposure to cannabinoids through breastfeeding.

  4. Isotope dilution-GC-MS/MS analysis of 16 polycyclic aromatic hydrocarbons in selected medicinal herbs used as health food additives.

    Science.gov (United States)

    Yu, L; Cao, Y; Zhang, J; Cui, Z; Sun, H

    2012-01-01

    Medicinal herbs have a very important role in health protection and disease control, and have been used in health foods. Polycyclic aromatic hydrocarbons (PAHs) have carcinogenic, biological and mutagenic effects. In this paper, the content of 16 PAHs as representative contaminants in nine Chinese medicinal herbs, as additives for health foods, was investigated in order to ensure food safety from this source. A highly sensitive isotope dilution-gas chromatography-tandem mass spectrometry (ID-GC-MS/MS) method combined with gel permeation chromatography (GPC) and solid-phase extraction (SPE) was developed. Calibration curves showed good linearity for all PAHs (R² > 0.999), and the limit of quantification (LOQ) ranged from 0.42 to 2.7 µg kg⁻¹. Average recoveries for these compounds were in the range of 52.5-117%, 52.6-119% and 81.4-108% at the concentrations of 10, 50 and 250 µg kg⁻¹ with RSD of 1.8-15%, 0.9-15% and 1.0-15%, respectively. The proposed method was used for the analysis of nine Chinese medicinal herbs. Total levels of PAHs varied from 98.2 µg kg⁻¹ (cassia seed) to 2245 µg kg⁻¹ (eucommia bark). The highest level was found for phenanthrene (Phe) in liquorice root (631.3 µg kg⁻¹), indigowoad leaf (551.0 µg kg⁻¹), rose flower (435.2 µg kg⁻¹) and eucommia bark (432.3 µg kg⁻¹). The proposed method could provide a useful basis for safety monitoring of herbs and risk management for PAHs in the health food industry.

  5. Quality- and dilution losses in the recycling of ferrous materials from end-of-life passenger cars: input-output analysis under explicit consideration of scrap quality.

    Science.gov (United States)

    Nakamura, Shinichiro; Kondo, Yasushi; Matsubae, Kazuyo; Nakajima, Kenichi; Tasaki, Tomohiro; Nagasaka, Tetsuya

    2012-09-04

    Metals can in theory be infinitely recycled in a closed-loop without any degradation in quality. In reality, however, open-loop recycling is more typical for metal scrap recovered from end-of-life (EoL) products because mixing of different metal species results in scrap quality that no longer matches the originals. Further losses occur when meeting the quality requirement of the target product requires dilution of the secondary material by adding high purity materials. Standard LCA usually does not address these losses. This paper presents a novel approach to quantifying quality- and dilution losses, by means of hybrid input-output analysis. We focus on the losses associated with the recycling of ferrous materials from end-of-life vehicle (ELV) due to the mixing of copper, a typical contaminant in steel recycling. Given the quality of scrap in terms of copper density, the model determines the ratio by which scrap needs to be diluted in an electric arc furnace (EAF), and the amount of demand for EAF steel including those quantities needed for dilution. Application to a high-resolution Japanese IO table supplemented with data on ferrous materials including different grades of scrap indicates that a nationwide avoidance of these losses could result in a significant reduction of CO(2) emissions.

  6. Extracting Minerals from Seawater: An Energy Analysis

    Directory of Open Access Journals (Sweden)

    Ugo Bardi

    2010-04-01

    Full Text Available The concept of recovering minerals from seawater has been proposed as a way of counteracting the gradual depletion of conventional mineral ores. Seawater contains large amounts of dissolved ions and the four most concentrated metal ones (Na, Mg, Ca, K are being commercially extracted today. However, all the other metal ions exist at much lower concentrations. This paper reports an estimate of the feasibility of the extraction of these metal ions on the basis of the energy needed. In most cases, the result is that extraction in amounts comparable to the present production from land mines would be impossible because of the very large amount of energy needed. This conclusion holds also for uranium as fuel for the present generation of nuclear fission plants. Nevertheless, in a few cases, mainly lithium, extraction from seawater could provide amounts of metals sufficient for closing the cycle of metal use in the economy, provided that an increased level of recycling can be attained.

  7. Antioxidants: Characterization, natural sources, extraction and analysis

    OpenAIRE

    OROIAN, MIRCEA; Escriche Roberto, Mª Isabel

    2015-01-01

    [EN] Recently many review papers regarding antioxidants fromdifferent sources and different extraction and quantification procedures have been published. However none of them has all the information regarding antioxidants (chemistry, sources, extraction and quantification). This article tries to take a different perspective on antioxidants for the new researcher involved in this field. Antioxidants from fruit, vegetables and beverages play an important role in human health, fo...

  8. Food Fish Identification from DNA Extraction through Sequence Analysis

    Science.gov (United States)

    Hallen-Adams, Heather E.

    2015-01-01

    This experiment exposed 3rd and 4th y undergraduates and graduate students taking a course in advanced food analysis to DNA extraction, polymerase chain reaction (PCR), and DNA sequence analysis. Students provided their own fish sample, purchased from local grocery stores, and the class as a whole extracted DNA, which was then subjected to PCR,…

  9. The methodology of semantic analysis for extracting physical effects

    Science.gov (United States)

    Fomenkova, M. A.; Kamaev, V. A.; Korobkin, D. M.; Fomenkov, S. A.

    2017-01-01

    The paper represents new methodology of semantic analysis for physical effects extracting. This methodology is based on the Tuzov ontology that formally describes the Russian language. In this paper, semantic patterns were described to extract structural physical information in the form of physical effects. A new algorithm of text analysis was described.

  10. L-edge sum rule analysis on 3d transition metal sites: from d10 to d0 and towards application to extremely dilute metallo-enzymes.

    Science.gov (United States)

    Wang, Hongxin; Friedrich, Stephan; Li, Lei; Mao, Ziliang; Ge, Pinghua; Balasubramanian, Mahalingam; Patil, Daulat S

    2018-03-28

    According to L-edge sum rules, the number of 3d vacancies at a transition metal site is directly proportional to the integrated intensity of the L-edge X-ray absorption spectrum (XAS) for the corresponding metal complex. In this study, the numbers of 3d holes are characterized quantitatively or semi-quantitatively for a series of manganese (Mn) and nickel (Ni) complexes, including the electron configurations 3d 10 → 3d 0 . In addition, extremely dilute (edge jump region; and (2) by adding an inert tracer to the sample that provides a prominent spectral feature to replace the weak edge jump for intensity normalization. In this publication, we present for the first time: (1) L-edge sum rule analysis for a series of Mn and Ni complexes that include electron configurations from an open shell 3d 0 to a closed shell 3d 10 ; (2) a systematic analysis on the uncertainties, especially on that from the edge jump, which was missing in all previous reports; (3) a clearly-resolved edge jump between pre-L 3 and post-L 2 regions from an extremely dilute sample; (4) an evaluation of an alternative normalization standard for L-edge sum rule analysis. XAS from two copper (Cu) proteins measured using a conventional semiconductor X-ray detector are also repeated as bridges between Ni complexes and dilute Ni enzymes. The differences between measuring 1% Cu enzymes and measuring edge sum rule analysis to virtually any 3d metal complex and any dilute biological samples that contain 3d metals.

  11. Antioxidants: Characterization, natural sources, extraction and analysis.

    Science.gov (United States)

    Oroian, Mircea; Escriche, Isabel

    2015-08-01

    Recently many review papers regarding antioxidants from different sources and different extraction and quantification procedures have been published. However none of them has all the information regarding antioxidants (chemistry, sources, extraction and quantification). This article tries to take a different perspective on antioxidants for the new researcher involved in this field. Antioxidants from fruit, vegetables and beverages play an important role in human health, for example preventing cancer and cardiovascular diseases, and lowering the incidence of different diseases. In this paper the main classes of antioxidants are presented: vitamins, carotenoids and polyphenols. Recently, many analytical methodologies involving diverse instrumental techniques have been developed for the extraction, separation, identification and quantification of these compounds. Antioxidants have been quantified by different researchers using one or more of these methods: in vivo, in vitro, electrochemical, chemiluminescent, electron spin resonance, chromatography, capillary electrophoresis, nuclear magnetic resonance, near infrared spectroscopy and mass spectrometry methods. Copyright © 2015. Published by Elsevier Ltd.

  12. Analysis of Intracellular Metabolites from Microorganisms: Quenching and Extraction Protocols.

    Science.gov (United States)

    Pinu, Farhana R; Villas-Boas, Silas G; Aggio, Raphael

    2017-10-23

    Sample preparation is one of the most important steps in metabolome analysis. The challenges of determining microbial metabolome have been well discussed within the research community and many improvements have already been achieved in last decade. The analysis of intracellular metabolites is particularly challenging. Environmental perturbations may considerably affect microbial metabolism, which results in intracellular metabolites being rapidly degraded or metabolized by enzymatic reactions. Therefore, quenching or the complete stop of cell metabolism is a pre-requisite for accurate intracellular metabolite analysis. After quenching, metabolites need to be extracted from the intracellular compartment. The choice of the most suitable metabolite extraction method/s is another crucial step. The literature indicates that specific classes of metabolites are better extracted by different extraction protocols. In this review, we discuss the technical aspects and advancements of quenching and extraction of intracellular metabolite analysis from microbial cells.

  13. Analysis of Intracellular Metabolites from Microorganisms: Quenching and Extraction Protocols

    Directory of Open Access Journals (Sweden)

    Farhana R. Pinu

    2017-10-01

    Full Text Available Sample preparation is one of the most important steps in metabolome analysis. The challenges of determining microbial metabolome have been well discussed within the research community and many improvements have already been achieved in last decade. The analysis of intracellular metabolites is particularly challenging. Environmental perturbations may considerably affect microbial metabolism, which results in intracellular metabolites being rapidly degraded or metabolized by enzymatic reactions. Therefore, quenching or the complete stop of cell metabolism is a pre-requisite for accurate intracellular metabolite analysis. After quenching, metabolites need to be extracted from the intracellular compartment. The choice of the most suitable metabolite extraction method/s is another crucial step. The literature indicates that specific classes of metabolites are better extracted by different extraction protocols. In this review, we discuss the technical aspects and advancements of quenching and extraction of intracellular metabolite analysis from microbial cells.

  14. Analysis of volatiles from irradiated yeast extract

    International Nuclear Information System (INIS)

    Liao Tao; Li Xin; Zu Xiaoyan; Chen Yuxia; Geng Shengrong

    2013-01-01

    The method for determination volatiles from irradiated yeast extract (YE) using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was developed in this paper. The extraction conditions were optimized with reference to the peak area and number of volatiles as aldehyde, ketone, alcohol, acid, ester and sulfur compounds. The optimized conditions of HS-SPME for volatiles in irradiated YE were: divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber, extration time 40 min, extraction temperature 40℃. The volatiles from YE irradiated by 0-19.8 kGy were detected using HS-SPME coupled with GC-MS. The results showed that only 15 volatiles were detected from no irradiated YE and main compounds were acetic acid, 2, 3-butanediol and 1-hexanol, 2-ethyl-. There were 40 volatiles detected from irradiated YE and the main compounds were acetic acid, phenylethyl alcohol, heptanal and nonanal. Compare to no irradiated yeast extract, the aldehyde, ketone, alkene and disulfide, dimethyl were produced by irradiating process. (authors)

  15. Trace uranium analysis in geological sample by isotope dilution-alpha spectrometry and comparison with other techniques

    International Nuclear Information System (INIS)

    Shihomatsu, H.M.; Iyer, S.S.

    1988-12-01

    Establishment of uranium determination in geological samples by alpha spectrometric isotope dilution technique using 233 U tracer is described in the present work. The various steps involved in the method namely, preparation of the sample, electrodeposition, alpha spectrometry, isotope dilution, calculation of the concentration and error statistics are discussed in detail. The experimental parameters for the electrodeposition of uranium, like current density, pH concentration of the electrolyte solution, deposition time, electrode distance were all optimised based on the efficiency of the deposition. The total accuracy and precision of the IDAS using 233 U tracer in the determination of uranium in mineral and granite samples were of the order of 1 to 2% for the concentration range of 50-1500 ppm of U. Our results are compared with those obtained by others workers using similar and different techniques. (author) [pt

  16. Converting Eucalyptus biomass into ethanol: Financial and sensitivity analysis in a co-current dilute acid process. Part II

    International Nuclear Information System (INIS)

    Gonzalez, R.; Treasure, T.; Phillips, R.; Jameel, H.; Saloni, D.; Wright, J.; Abt, R.

    2011-01-01

    The technical and financial performance of high yield Eucalyptus biomass in a co-current dilute acid pretreatment followed by enzymatic hydrolysis process was simulated using WinGEMS registered and Excel registered . Average ethanol yield per dry Mg of Eucalyptus biomass was approximately 347.6 L of ethanol (with average carbohydrate content in the biomass around 66.1%) at a cost of 0.49 L -1 of ethanol, cash cost of ∝0.46 L -1 and CAPEX of 1.03 L -1 of ethanol. The main cost drivers are: biomass, enzyme, tax, fuel (gasoline), depreciation and labor. Profitability of the process is very sensitive to biomass cost, carbohydrate content (%) in biomass and enzyme cost. Biomass delivered cost was simulated and financially evaluated in Part I; here in Part II the conversion of this raw material into cellulosic ethanol using the dilute acid process is evaluated. (author)

  17. Quantitative Analysis of Ingenol in Euphorbia species via Validated Isotope Dilution Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry

    Czech Academy of Sciences Publication Activity Database

    Béres, T.; Dragull, K.; Pospíšil, Jiří; Tarkowská, Danuše; Dančák, M.; Bíba, Ondřej; Tarkowski, P.; Doležal, K.; Strnad, Miroslav

    2018-01-01

    Roč. 29, č. 1 (2018), s. 23-29 ISSN 0958-0344 R&D Projects: GA ČR GA17-14007S; GA MŠk(CZ) LO1204 Institutional support: RVO:61389030 Keywords : Euphorbia genus * ingenol * isotope-dilution method * mass spectrometry * ultra-high performance liquid chromatography Subject RIV: FD - Oncology ; Hematology OBOR OECD: Analytical chemistry Impact factor: 2.292, year: 2016

  18. Neutron activation analysis for the optimal sampling and extraction of extractable organohalogens in human hari

    International Nuclear Information System (INIS)

    Zhang, H.; Chai, Z.F.; Sun, H.B.; Xu, H.F.

    2005-01-01

    Many persistent organohalogen compounds such as DDTs and polychlorinated biphenyls have caused seriously environmental pollution problem that now involves all life. It is know that neutron activation analysis (NAA) is a very convenient method for halogen analysis and is also the only method currently available for simultaneously determining organic chlorine, bromine and iodine in one extract. Human hair is a convenient material to evaluate the burden of such compounds in human body and dan be easily collected from people over wide ranges of age, sex, residential areas, eating habits and working environments. To effectively extract organohalogen compounds from human hair, in present work the optimal Soxhelt-extraction time of extractable organohalogen (EOX) and extractable persistent organohalogen (EPOX) from hair of different lengths were studied by NAA. The results indicated that the optimal Soxhelt-extraction time of EOX and EPOX from human hair was 8-11 h, and the highest EOX and EPOX contents were observed in hair powder extract. The concentrations of both EOX and EPOX in different hair sections were in the order of hair powder ≥ 2 mm > 5 mm, which stated that hair samples milled into hair powder or cut into very short sections were not only for homogeneous. hair sample but for the best hair extraction efficiency.

  19. Analysis, by RELAP5 code, of boron dilution phenomena in a mid-loop operation transient, performed in PKL III F2.1 RUN 1 test

    International Nuclear Information System (INIS)

    Mascari, F.; Vella, G.; Del Nevo, A.; D'Auria, F.

    2007-01-01

    The present paper deals with the post test analysis and accuracy quantification of the test PKL III F2.1 RUN 1 by RELAP5/Mod3.3 code performed in the framework of the international OECD/SETH PKL III Project. The PKL III is a full-height integral test facility (ITF) that models the entire primary system and most of the secondary system (except for turbine and condenser) of pressurized water reactor of KWU design of the 1300-MW (electric) class on a scale of 1:145. Detailed design was based to the largest possible extent on the specific data of Philippsburg nuclear power plant, unit 2. As for the test facilities of this size, the scaling concept aims to simulate overall thermal hydraulic behavior of the full-scale power plant [1]. The main purpose of the project is to investigate PWR safety issues related to boron dilution and in particular this experiment investigates (a) the boron dilution issue during mid-loop operation and shutdown conditions, and (b) assessing primary circuit accident management operations to prevent boron dilution as a consequence of loss of heat removal [2]. In this work the authors deal with a systematic procedure (developed at the university of Pisa) for code assessment and uncertainty qualification and its application to RELAP5 system code. It is used to evaluate the capability of RELAP5 to reproduce the thermal hydraulics of an inadvertent boron dilution event in a PWR. The quantitative analysis has been performed adopting the Fast Fourier Transform Based Method (FFTBM), which has the capability to quantify the errors in code predictions as compared to the measured experimental signal. (author)

  20. Optimisation of beryllium-7 gamma analysis following BCR sequential extraction

    International Nuclear Information System (INIS)

    Taylor, A.; Blake, W.H.; Keith-Roach, M.J.

    2012-01-01

    Graphical abstract: Showing decrease in analytical uncertainty using the optimal (combined preconcentrated sample extract) method. nv (no value) where extract activities were 7 Be geochemical behaviour is required to support tracer studies. ► Sequential extraction with natural 7 Be returns high analytical uncertainties. ► Preconcentrating extracts from a large sample mass improved analytical uncertainty. ► This optimised method can be readily employed in studies using low activity samples. - Abstract: The application of cosmogenic 7 Be as a sediment tracer at the catchment-scale requires an understanding of its geochemical associations in soil to underpin the assumption of irreversible adsorption. Sequential extractions offer a readily accessible means of determining the associations of 7 Be with operationally defined soil phases. However, the subdivision of the low activity concentrations of fallout 7 Be in soils into geochemical fractions can introduce high gamma counting uncertainties. Extending analysis time significantly is not always an option for batches of samples, owing to the on-going decay of 7 Be (t 1/2 = 53.3 days). Here, three different methods of preparing and quantifying 7 Be extracted using the optimised BCR three-step scheme have been evaluated and compared with a focus on reducing analytical uncertainties. The optimal method involved carrying out the BCR extraction in triplicate, sub-sampling each set of triplicates for stable Be analysis before combining each set and coprecipitating the 7 Be with metal oxyhydroxides to produce a thin source for gamma analysis. This method was applied to BCR extractions of natural 7 Be in four agricultural soils. The approach gave good counting statistics from a 24 h analysis period (∼10% (2σ) where extract activity >40% of total activity) and generated statistically useful sequential extraction profiles. Total recoveries of 7 Be fell between 84 and 112%. The stable Be data demonstrated that the

  1. The liquid-liquid extraction of chloro-(trichlorostannato)-rhodium(I/III) and -ruthenium (II) complexes from dilute hydrochloric acid into 4-methylpentan-2-one

    International Nuclear Information System (INIS)

    Wyrley-Birch, J.M.

    1984-10-01

    The effect of stannous chloride on the liquid-liquid extraction of rhodium and ruthenium from hydrochloric acid solutions into 4-methyl-pentan-2-one (MIBK)/hexane mixtures was studied in detail. Stannous chloride concentrations were found to considerably increase the efficiency of the extraction of rhodium and ruthenium into the organic phase. Chloro-(trichlorostannato)-rhodium (I/III) complexes were formed at room temperature. The rate of chloro-(trichlorostannato)-ruthenium (II) complex formation was extremely slow at room temperature, but increased on heating of the aqueous solutions. The amount of rhodium and ruthenium extracted into the organic phase depend on the Sn(II):M molar ratio, the HCl, H sup(+) and Cl sup(-) concentrations, as well as the equilibration time. A 119 Sn NMR study of the MIBK extracts, showed that the stoichiometry of the chloro-(trichlorostannato)-rhodium (I/III) complexes extracted into the organic phase was dependent on the Sn(II):Rh(III) molar ratio as well as the HCl, H sup(+) and Cl sup(-) concentrations in the aqueous phase. The predominant species observed in the organic phase from HCl solutions containing Sn(II):Rh(III) ratios >= 5:1, was shown to be an hydrido complex having the form [RhH(SnCl 3 ) 4 Cl] 3 sup(-) or [RhH(SnCl 3 ) 4 ]2 sup(-). An essentially quantitative separation of rhodium and ruthenium was achieved utilising the variation in the rates of rhodium-tin and ruthenium-tin complex formation

  2. Asymptotic analysis of an ion extraction model

    International Nuclear Information System (INIS)

    Ben Abdallah, N.; Mas-Gallic, S.; Raviart, P.A.

    1993-01-01

    A simple model for ion extraction from a plasma is analyzed. The order of magnitude of the plasma parameters leads to a singular perturbation problem for a semilinear elliptic equation. We first prove existence of solutions for the perturbed problem and uniqueness under certain conditions. Then we prove the convergence of these solutions, when the parameters go to zero, towards the solution of a Child-Langmuir problem

  3. Fuzzy concept analysis for semantic knowledge extraction

    OpenAIRE

    De Maio, Carmen

    2012-01-01

    2010 - 2011 Availability of controlled vocabularies, ontologies, and so on is enabling feature to provide some added values in terms of knowledge management. Nevertheless, the design, maintenance and construction of domain ontologies are a human intensive and time consuming task. The Knowledge Extraction consists of automatic techniques aimed to identify and to define relevant concepts and relations of the domain of interest by analyzing structured (relational databases, XML) and unstructu...

  4. Development of pitanga nectar with different sweeteners by sensory analysis: ideal pulp dilution, ideal sweetness, and sweetness equivalence

    Directory of Open Access Journals (Sweden)

    Mírian Luisa Faria Freitas

    2014-03-01

    Full Text Available The objective of this study was to develop pitanga nectar formulations in which sucrose was replaced with different sweeteners. Consumer tests were conducted with 50 fruit juice consumers, and a just-about-right scale was used to determine the ideal pulp dilution and ideal sweetness with sucrose. Furthermore, the adequate concentrations of six sweeteners were determined to obtain the equivalent sweetness of sucrose using relative to these concentrations the magnitude estimation model with 19 selected assessors. The ideal dilution test resulted in 25% pulp, and the ideal sweetness test, 10% sucrose. Sweetener concentrations to replace sucrose were 0.0160%, 0.0541%, 0.1000%, 0.0999%, 0.0017%, and 0.0360%, respectively, for sucralose, aspartame, stevia 40% rebaudioside A, stevia 95% rebaudioside A, neotame, and a 2:1 cyclamate/saccharin blend. These results can be used to prepare pitanga nectar with different sweeteners and obtain the same sweetness intensity in less caloric products than that of nectar prepared with sucrose.

  5. Optimisation of beryllium-7 gamma analysis following BCR sequential extraction

    Energy Technology Data Exchange (ETDEWEB)

    Taylor, A. [Plymouth University, School of Geography, Earth and Environmental Sciences, 8 Kirkby Place, Plymouth PL4 8AA (United Kingdom); Blake, W.H., E-mail: wblake@plymouth.ac.uk [Plymouth University, School of Geography, Earth and Environmental Sciences, 8 Kirkby Place, Plymouth PL4 8AA (United Kingdom); Keith-Roach, M.J. [Plymouth University, School of Geography, Earth and Environmental Sciences, 8 Kirkby Place, Plymouth PL4 8AA (United Kingdom); Kemakta Konsult, Stockholm (Sweden)

    2012-03-30

    Graphical abstract: Showing decrease in analytical uncertainty using the optimal (combined preconcentrated sample extract) method. nv (no value) where extract activities were extraction with natural {sup 7}Be returns high analytical uncertainties. Black-Right-Pointing-Pointer Preconcentrating extracts from a large sample mass improved analytical uncertainty. Black-Right-Pointing-Pointer This optimised method can be readily employed in studies using low activity samples. - Abstract: The application of cosmogenic {sup 7}Be as a sediment tracer at the catchment-scale requires an understanding of its geochemical associations in soil to underpin the assumption of irreversible adsorption. Sequential extractions offer a readily accessible means of determining the associations of {sup 7}Be with operationally defined soil phases. However, the subdivision of the low activity concentrations of fallout {sup 7}Be in soils into geochemical fractions can introduce high gamma counting uncertainties. Extending analysis time significantly is not always an option for batches of samples, owing to the on-going decay of {sup 7}Be (t{sub 1/2} = 53.3 days). Here, three different methods of preparing and quantifying {sup 7}Be extracted using the optimised BCR three-step scheme have been evaluated and compared with a focus on reducing analytical uncertainties. The optimal method involved carrying out the BCR extraction in triplicate, sub-sampling each set of triplicates for stable Be analysis before combining each set and coprecipitating the {sup 7}Be with metal oxyhydroxides to produce a thin source for gamma analysis. This method was applied to BCR extractions of natural {sup 7}Be in four agricultural soils. The approach gave good counting statistics from a 24 h analysis period ({approx}10% (2

  6. Analysis of nitrosamines in water by automated SPE and isotope dilution GC/HRMS Occurrence in the different steps of a drinking water treatment plant, and in chlorinated samples from a reservoir and a sewage treatment plant effluent.

    Science.gov (United States)

    Planas, Carles; Palacios, Oscar; Ventura, Francesc; Rivera, Josep; Caixach, Josep

    2008-08-15

    A method based on automated solid-phase extraction (SPE) and isotope dilution gas chromatography/high resolution mass spectrometry (GC/HRMS) has been developed for the analysis of nine nitrosamines in water samples. The combination of automated SPE and GC/HRMS for the analysis of nitrosamines has not been reported previously. The method shows as advantages the selectivity and sensitivity of GC/HRMS analysis and the high efficiency of automated SPE with coconut charcoal EPA 521 cartridges. Low method detection limits (MDLs) were achieved, along with a greater facility of the procedure and less dependence on the operator with regard to the methods based on manual SPE. Quality requirements for isotope dilution-based methods were accomplished for most analysed nitrosamines, regarding to trueness (80-120%), method precision (water samples (16 samples from a drinking water treatment plant {DWTP}, 2 chlorinated samples from a sewage treatment plant {STP} effluent, and 1 chlorinated sample from a reservoir) were analysed. Concentrations of nitrosamines in the STP effluent were 309.4 and 730.2 ng/L, being higher when higher doses of chlorine were applied. N-Nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) were the main compounds identified in the STP effluent, and NDEA was detected above 200 ng/L, regulatory level for NDMA in effluents stated in Ontario (Canada). Lower concentrations of nitrosamines were found in the reservoir (20.3 ng/L) and in the DWTP samples (n.d. -28.6 ng/L). NDMA and NDEA were respectively found in the reservoir and in treated and highly chlorinated DWTP samples at concentrations above 10 ng/L (guide value established in different countries). The highest concentrations of nitrosamines were found after chlorination and ozonation processes (ozonated, treated and highly chlorinated water) in DWTP samples.

  7. Qualitative analysis of hexane flour extract of spelt

    Directory of Open Access Journals (Sweden)

    Vujić Đura N.

    2013-01-01

    Full Text Available Gas chromatography with mass spectrometry (GC-MS was used for performing a qualitative analysis of the hexane flour extract of three samples of spelt. All the three samples were first treated with hexane and the obtained extracts were used for the analysis of the fatty acid lipid components. The transesterification reaction was performed using TMSH (trimethylsulfonium hydroxide, 0.2M in methanol, and the fatty acids were esterified from acylglycerol to methyl-esters. In all analyzed extracts, the predominant component was methyl linoleate, followed by methyl oleate and methyl palmitate. The subsequent tests, performed by cluster analysis, were used to compare the hexane flour extracts of different types of spelt. [Projekat Ministarstva nauke Republike Srbije, br. III46005 i br. TR 31066

  8. Growth and XRD analysis of the diluted magnetic semiconductor Zn{sub 1-x}Ni{sub x}O

    Energy Technology Data Exchange (ETDEWEB)

    Syed Ali, K.S. [Department of Science, Estill High School, Post Office Box 754, Estill, South Carolina - 29918 (United States); Saravanan, R. [Department of Physics, The Madura College, Madurai - 625 011 (India); Acikgoez, M. [Bahcesehir University, Faculty of Arts and Sciences, Besiktas - 34349 (Turkey)

    2011-01-15

    Diluted magnetic semiconductor compound Zn{sub 1-x}Ni{sub x} O(x =0.01, 0.02, 0.03, 0.04 and 0.05) was prepared by sol-gel method and characterized using powder XRD for the distribution of electrons and bonding in the unit cell. The electronic structural studies of this material were carried out by maximum entropy method (MEM) for the quantitative and qualitative measurement on the inclusion and the effect induced on bonding by Ni doping. The spatial arrangement of charge and the bonding behavior of this material were analyzed from 3D, 2D and 1D density distributions. The evidence for the addition of Ni in the host lattice of Zn is realized. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  9. Estimating the extractability of potentially toxic metals in urban soils: A comparison of several extracting solutions

    International Nuclear Information System (INIS)

    Madrid, F.; Reinoso, R.; Florido, M.C.; Diaz Barrientos, E.; Ajmone-Marsan, F.; Davidson, C.M.; Madrid, L.

    2007-01-01

    Metals released by the extraction with aqua regia, EDTA, dilute HCl and sequential extraction (SE) by the BCR protocol were studied in urban soils of Sevilla, Torino, and Glasgow. By multivariate analysis, the amounts of Cu, Pb and Zn liberated by any method were statistically associated with one another, whereas other metals were not. The mean amounts of all metals extracted by HCl and by SE were well correlated, but SE was clearly underestimated by HCl. Individual data for Cu, Pb and Zn by both methods were correlated only if each city was considered separately. Other metals gave poorer relationships. Similar conclusions were reached comparing EDTA and HCl, with much lower values for EDTA. Dilute HCl extraction cannot thus be recommended for general use as alternative to BCR SE in urban soils. - Dilute HCl extraction is tested as an alternative to the BCR sequential extraction in urban soils

  10. Analysis of medicinal plant extracts by neutron activation method

    International Nuclear Information System (INIS)

    Vaz, Sandra Muntz

    1995-01-01

    This dissertation has presented the results from analysis of medicinal plant extracts using neutron activation method. Instrumental neutron activation analysis was applied to the determination of the elements Al, Br, Ca, Ce, Cl, Cr, Cs, Fe, K, La, Mg, Mn, Na, Rb, Sb, Sc and Zn in medicinal extracts obtained from Achyrolcline satureoides DC, Casearia sylvestris, Centella asiatica, Citrus aurantium L., Solano lycocarpum, Solidago microglossa, Stryphnondedron barbatiman and Zingiber officinale R. plants. The elements Hg and Se were determined using radiochemical separation by means of retention of Se in HMD inorganic exchanger and solvent extraction of Hg by bismuth diethyl-dithiocarbamate solution. Precision and accuracy of the results have been evaluated by analysing reference materials. The therapeutic action of some elements found in plant extracts analyzed was briefly discussed

  11. Solid-phase extraction procedures in systematic toxicological analysis

    NARCIS (Netherlands)

    Franke, J.P.; de Zeeuw, R.A

    1998-01-01

    In systematic toxicological analysis (STA) the substance(s) present is (are) not known at the start of the analysis. in such an undirected search the extraction procedure cannot be directed to a given substance but must be a general procedure where a compromise must be reached in that the substances

  12. A comparison of accelerated solvent extraction, Soxhlet extraction, and ultrasonic-assisted extraction for analysis of terpenoids and sterols in tobacco.

    Science.gov (United States)

    Shen, Jinchao; Shao, Xueguang

    2005-11-01

    The performance of accelerated solvent extraction in the analysis of terpenoids and sterols in tobacco samples was investigated and compared with those of Soxhlet extraction and ultrasonically assisted extraction with respect to yield, extraction time, reproducibility and solvent consumption. The results indicate that although the highest yield was achieved by Soxhlet extraction, ASE appears to be a promising alternative to classical methods since it is faster and uses less solvent, especially when applied to the investigation of large batch tobacco samples. However, Soxhlet extraction is still the preferred method for analyzing sterols since it gives a higher extraction efficiency than other methods.

  13. Sensitive analysis of steroid estrogens and bisphenol a in small volumes of water using isotope-dilution ultra-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Chang, Hong; Shen, Xiaoyan; Shao, Bing; Wu, Fengchang

    2018-04-01

    An isotope-dilution ultra-performance liquid chromatography-electrospray tandem mass spectrometry method combined with dansylation was established to sensitively quantify four steroid estrogens (estrone, 17α-estradiol, 17β-estradiol and 17α-ethynylestradiol) and bisphenol A in sewage influent and effluent. A simple hexane extraction was performed from a small volume (10 mL), followed by dansyl chloride derivatization and purification with a silica cartridge. The method effectively reduced the matrix effects in sample extract and permitted the selective and sensitive determination of target compounds from complicated matrices. The detection limits of the method for steroid estrogens were 0.20-0.90 ng L -1 in influent and 0.10-0.20 ng L -1 in effluent samples. For bisphenol A, the limits detection of the method were 20 and 0.80 for influent and effluent samples, respectively. Recoveries of 85%-96% were observed in all matrices. The method was applied to analyze residual estrogens and bisphenol A in sewage influent and effluent samples from Beijing, China. The concentrations of bisphenol A (636-1200 ng L -1 ) were up to 250 times higher than those of steroid estrogens. Estrone was the dominant estrogen in influent and effluent samples, while similar concentrations of 17α-estradiol and 17β-estradiol were detected in all samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

  14. Differential color space analysis for investigating nutrient content in a puréed food dilution-flavor matrix: a step toward objective malnutrition risk assessment

    Science.gov (United States)

    Pfisterer, Kaylen J.; Amelard, Robert; Wong, Alexander

    2018-02-01

    Dysphagia (swallowing difficulty) increases risk for malnutrition and affects at least 15% of American older adults, and 590 million people worldwide. Malnutrition is associated with increased mortality, increased morbidity, decreased quality of life, and accounts for over $15 billion (USD) health-care related costs each year. While modified texture diets (e.g., puréed food) reduce the risk of choking, quality assurance is necessary for monitoring nutrient density to ensure food meets nutritional requirements. However, current methods are subjective and time consuming. The purpose of this study was to investigate the feasibility of optical techniques for an objective assessment of food nutrient density in puréed samples. Motivated by a theoretical optical dilution model, broadband spectral images of commercially prepared purée samples were acquired. Specifically, 13 flavors at five dilutions relative to initial concentration, each with six replicates, were acquired for a total of 390 samples. Purée samples were prepared and loaded onto a white reflectance back plane to maximize photon traversal path length through the purée. The sample was illuminated with a tungsten-halogen illumination source fitted with a front glass fabric diffuser for spatially homogeneous illumination. This broadband illuminant was chosen to observe as many food-light spectral absorbance interactions as possible. Flavor-stratified correlation analysis was performed on this food image dataset to investigate the relationship between nutritional information and color space transformations. A special case of blueberry is presented as the effect of anthocyanins was quantitatively observed through normalized spectral trends in response to pH perturbations across dilutions.

  15. Smart Extraction and Analysis System for Clinical Research.

    Science.gov (United States)

    Afzal, Muhammad; Hussain, Maqbool; Khan, Wajahat Ali; Ali, Taqdir; Jamshed, Arif; Lee, Sungyoung

    2017-05-01

    With the increasing use of electronic health records (EHRs), there is a growing need to expand the utilization of EHR data to support clinical research. The key challenge in achieving this goal is the unavailability of smart systems and methods to overcome the issue of data preparation, structuring, and sharing for smooth clinical research. We developed a robust analysis system called the smart extraction and analysis system (SEAS) that consists of two subsystems: (1) the information extraction system (IES), for extracting information from clinical documents, and (2) the survival analysis system (SAS), for a descriptive and predictive analysis to compile the survival statistics and predict the future chance of survivability. The IES subsystem is based on a novel permutation-based pattern recognition method that extracts information from unstructured clinical documents. Similarly, the SAS subsystem is based on a classification and regression tree (CART)-based prediction model for survival analysis. SEAS is evaluated and validated on a real-world case study of head and neck cancer. The overall information extraction accuracy of the system for semistructured text is recorded at 99%, while that for unstructured text is 97%. Furthermore, the automated, unstructured information extraction has reduced the average time spent on manual data entry by 75%, without compromising the accuracy of the system. Moreover, around 88% of patients are found in a terminal or dead state for the highest clinical stage of disease (level IV). Similarly, there is an ∼36% probability of a patient being alive if at least one of the lifestyle risk factors was positive. We presented our work on the development of SEAS to replace costly and time-consuming manual methods with smart automatic extraction of information and survival prediction methods. SEAS has reduced the time and energy of human resources spent unnecessarily on manual tasks.

  16. Extractables analysis of single-use flexible plastic biocontainers.

    Science.gov (United States)

    Marghitoiu, Liliana; Liu, Jian; Lee, Hans; Perez, Lourdes; Fujimori, Kiyoshi; Ronk, Michael; Hammond, Matthew R; Nunn, Heather; Lower, Asher; Rogers, Gary; Nashed-Samuel, Yasser

    2015-01-01

    Studies of the extractable profiles of bioprocessing components have become an integral part of drug development efforts to minimize possible compromise in process performance, decrease in drug product quality, and potential safety risk to patients due to the possibility of small molecules leaching out from the components. In this study, an effective extraction solvent system was developed to evaluate the organic extractable profiles of single-use bioprocess equipment, which has been gaining increasing popularity in the biopharmaceutical industry because of the many advantages over the traditional stainless steel-based bioreactors and other fluid mixing and storage vessels. The chosen extraction conditions were intended to represent aggressive conditions relative to the application of single-use bags in biopharmaceutical manufacture, in which aqueous based systems are largely utilized. Those extraction conditions, along with a non-targeted analytical strategy, allowed for the generation and identification of an array of extractable compounds; a total of 53 organic compounds were identified from four types of commercially available single-use bags, the majority of which are degradation products of polymer additives. The success of this overall extractables analysis strategy was reflected partially by the effectiveness in the extraction and identification of a compound that was later found to be highly detrimental to mammalian cell growth. The usage of single-use bioreactors has been increasing in biopharmaceutical industry because of the appealing advantages that it promises regarding to the cleaning, sterilization, operational flexibility, and so on, during manufacturing of biologics. However, compared to its conventional counterparts based mainly on stainless steel, single-use bioreactors are more susceptible to potential problems associated with compound leaching into the bioprocessing fluid. As a result, extractable profiling of the single-use system has become

  17. Analysis of PWR auxiliary coolant: determination of chloride in borax/nitrite solution by known addition - known dilution potentiometry

    International Nuclear Information System (INIS)

    Midgley, D.; Gatford, C.

    1989-11-01

    Chloride concentrations of 75-250 μg 1 -1 have been determined in simulated PWR auxiliary coolant containing 1000 mg l -1 each of sodium tetraborate and sodium nitrite. The effects of the two main components of the coolant solution on a variety of chloride-selective electrodes have been studied. Sodium tetraborate posed no problem except through its effect on the pH, which is easily adjusted. Such high concentrations of nitrite, however, caused significant deviations in e.m.f. for all the electrodes and marked tarnishing of the electroactive membrane after only one or two measurements. Sulphamic acid was selected as the best means of removing nitrite and silver chloride electrodes were preferred over mercury(I) chloride electrodes because of their greater robustness in the conditions. At these chloride concentrations, the electrodes are operating in their non-Nernstian response regions and direct potentiometry has poor precision, even if standards could be successfully matched to samples containing such high concentrations of background material. Known addition - known dilution potentiometry was adopted, with internal calibration for both slope factor and standard potential. (author)

  18. CHEMICAL ANALYSIS OF DENSE-GAS EXTRACTS FROM LIME FLOWERS

    Directory of Open Access Journals (Sweden)

    Demyanenko DV

    2015-04-01

    Full Text Available The purpose of this work was to make qualitative and quantitative analysis of phenolic biologically active substances (BAS in the extracts produced from lime flowers with condensed gases, using method of high-performance liquid chromatography (HPLC. Materials and methods: materials for this study were the extracts obtained by consequent processing of the herbal drug and marcs thereof with various condensed gases: difluorochloromethane (Freon R22, difluoromethane (Freon R32, azeotropic mixture of difluoromethane with pentafluoroethane (Freon 410A and freon-ammonium mixture. Extracts obtained with the latter were subjected to further fractionation by liquidliquid separation into hexane, chloroform, ethyl acetate and aqueous-alcohol phases. Besides, the supercritical СО2 extract, obtained from the herbal drug under rather strong conditions (at temperature 60°С and pressure 400 bar, was studied in our previous research. Presence of phenolic BAS and their quantity in the researched samples were determined by method of HPLC with UVspectrometric detection. Results and discussion: It has been found that Freon R22 extracted trace amounts of rutin from lime flowers – its content was only 0.08% of the total extract weight. On the other hand, Freons R32 and R410А showed good selectivity to moderately polar BAS of lime flowers (derivatives of flavonoids and hydroxycinnamic acids: in particular, the extract obtained with freon R32 contained about 1.3% of the total phenolic substances, and it was the only one of the investigated condensed gases used by us which took the basic flavonoid of lime flowers tiliroside – its content was 0.42% of extract weight. Also Freons R32 and R410А were able to withdraw another compound dominating among phenolic substances in the yielded extracts. Its quantity was rather noticeable – up to 0.87% of extract weight. This substance was not identified by existing database, but its UV-spectrum was similar to those of

  19. Determination of water-soluble and insoluble (dilute-HCl-extractable) fractions of Cd, Pb and Cu in Antarctic aerosol by square wave anodic stripping voltammetry: distribution and summer seasonal evolution at Terra Nova Bay (Victoria Land)

    Energy Technology Data Exchange (ETDEWEB)

    Annibaldi, A.; Truzzi, C.; Illuminati, S.; Bassotti, E.; Scarponi, G. [Polytechnic University of Marche - Ancona, Department of Marine Science, Ancona (Italy)

    2007-02-15

    Eight PM10 aerosol samples were collected in the vicinity of the ''Mario Zucchelli'' Italian Antarctic Station (formerly Terra Nova Bay Station) during the 2000-2001 austral summer using a high-volume sampler and precleaned cellulose filters. The aerosol mass was determined by differential weighing of filters carried out in a clean chemistry laboratory under controlled temperature and humidity. A two-step sequential extraction procedure was used to separate the water-soluble and the insoluble (dilute-HCl-extractable) fractions. Cd, Pb and Cu were determined in the two fractions using an ultrasensitive square wave anodic stripping voltammetric (SWASV) procedure set up for and applied to aerosol samples for the first time. Total extractable metals showed maxima at midsummer for Cd and Pb and a less clear trend for Cu. In particular, particulate metal concentrations ranged as follows: Cd 0.84-9.2 {mu}g g{sup -1} (average 4.7 {mu}g g{sup -1}), Pb 13.2-81 {mu}g g{sup -1} (average 33 {mu}g g{sup -1}), Cu 126-628 {mu}g g{sup -1} (average 378 {mu}g g{sup -1}). In terms of atmospheric concentration, the values were: Cd 0.55-6.3 pg m{sup -3} (average 3.4 pg m{sup -3}), Pb 8.7-48 pg m{sup -3} (average 24 pg m{sup -3}), Cu 75-365 pg m{sup -3} (average 266 pg m{sup -3}). At the beginning of the season the three metals appear widely distributed in the insoluble (HCl-extractable) fraction (higher proportions for Cd and Pb, 90-100%, and lower for Cu, 70-90%) with maxima in the second half of December. The soluble fraction then increases, and at the end of the season Cd and Pb are approximately equidistributed between the two fractions, while for Cu the soluble fraction reaches its maximum level of 36%. Practically negligible contributions are estimated for crustal and sea-spray sources. Low but significant volcanic contributions are estimated for Cd and Pb ({proportional_to}10% and {proportional_to}5%, respectively), while there is an evident although not

  20. Analysis preliminary phytochemical raw extract of leaves Nephrolepis pectinata

    Directory of Open Access Journals (Sweden)

    Natally Marreiros Gomes

    2017-06-01

    Full Text Available The Nephrolepis pectinata popularly known as paulista fern, ladder-heaven, cat tail, belongs to the family Davalliaceae. For the beauty of the arrangements of their leaves ferns are quite commercialized in Brazil, however, have not been described in the literature studies on their pharmacological potential. Thus, the objective of this research was to analyze the phytochemical properties of the crude extract of the leaves of Nephrolepis pectinata. To perform the phytochemical analysis were initially made the collection of the vegetable, preparation of voucher specimen, washing, drying and grinding. Then, extraction by percolation method and end the phytochemical analysis. Preliminary results phytochemicals the crude extract of the leaves of Nephrolepis pectinata tested positive for reducing sugars, phenols/tannins (catechins tannins and catechins.

  1. Hybridizing pines with diluted pollen

    Science.gov (United States)

    Robert Z. Callaham

    1967-01-01

    Diluted pollens would have many uses by the tree breeder. Dilutions would be particularly advantageous in making many controlled pollinations with a limited amount of pollen. They also would be useful in artificial mass pollinations of orchards or single trees. Diluted pollens might help overcome troublesome genetic barriers to crossing. Feasibility o,f using diluted...

  2. Criticality experiments: analysis, evaluation, and programs. 8. Prompt Neutron Decay Constants in Uranium Diluted with Matrix Material Systems

    International Nuclear Information System (INIS)

    Sanchez, Rene; Loaiza, David; Brunson, Glenn

    2001-01-01

    Rossi-Alpha measurements were performed on uranium diluted with matrix material systems to determine the prompt neutron decay constants. These constants represent an eigenvalue characteristic of these particular critical assemblies, which can be experimentally measured by the Rossi-Alpha or pulse neutron source techniques and calculated by a deterministic or Monte Carlo method. In the measurements presented in this paper, highly enriched foils diluted in various X/ 235 U ratios with polyethylene and SiO 2 , and polyethylene and aluminum were assembled to a high multiplication, and the prompt neutron decay constants were obtained by the Rossi-Alpha technique. The uranium diluted with matrix material experiments were fueled with highly enriched uranium foils. The average dimensions of the bare foils were 22.86 cm squared and 0.00762 cm thick. The foils were laminated with plastic sheets to reduce the amount of airborne contamination. Each foil weighed ∼70 g. The diluent material consisted of SiO 2 , or 6061 aluminum plates, which were embedded into polyethylene plates. The SiO 2 and aluminum plates were 22.86 cm square and 0.64 cm thick. The polyethylene plates were 39.12 cm square and 1.91 cm thick. Each polyethylene plate had a central recess whose dimensions were 22.86 cm by 22.86 cm by 0.64 cm deep and was used to accommodate the SiO 2 , or aluminum plates as well as the uranium foils. There were eight 39.12-cm-squared by 2.54-cm-thick high density polyethylene plates that form the top and bottom reflectors (four at the top and four at the bottom). Also, one of the polyethylene plates located in the center of the assembly had holes drilled in a radial direction to accommodate neutron detectors. Four 3 He detectors were placed in this plate. The 3 He detectors were 1.27 cm in diameter and ∼15 cm long. Rossi-Alpha measurements were performed at several subcritical separations for both experiments. The data were collected with a type I time analyzer (PATRM

  3. Testing sequential extraction methods for the analysis of multiple stable isotope systems from a bone sample

    Science.gov (United States)

    Sahlstedt, Elina; Arppe, Laura

    2017-04-01

    Stable isotope composition of bones, analysed either from the mineral phase (hydroxyapatite) or from the organic phase (mainly collagen) carry important climatological and ecological information and are therefore widely used in paleontological and archaeological research. For the analysis of the stable isotope compositions, both of the phases, hydroxyapatite and collagen, have their more or less well established separation and analytical techniques. Recent development in IRMS and wet chemical extraction methods have facilitated the analysis of very small bone fractions (500 μg or less starting material) for PO43-O isotope composition. However, the uniqueness and (pre-) historical value of each archaeological and paleontological finding lead to preciously little material available for stable isotope analyses, encouraging further development of microanalytical methods for the use of stable isotope analyses. Here we present the first results in developing extraction methods for combining collagen C- and N-isotope analyses to PO43-O-isotope analyses from a single bone sample fraction. We tested sequential extraction starting with dilute acid demineralization and collection of both collagen and PO43-fractions, followed by further purification step by H2O2 (PO43-fraction). First results show that bone sample separates as small as 2 mg may be analysed for their δ15N, δ13C and δ18OPO4 values. The method may be incorporated in detailed investigation of sequentially developing skeletal material such as teeth, potentially allowing for the investigation of interannual variability in climatological/environmental signals or investigation of the early life history of an individual.

  4. Simultaneous speciation of mercury and butyltin compounds in natural waters and snow by propylation and species-specific isotope dilution mass spectrometry analysis

    Energy Technology Data Exchange (ETDEWEB)

    Monperrus, M.; Tessier, E.; Veschambre, S.; Amouroux, D.; Donard, O. [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique Bio-inorganique et Environnement, CNRS UMR 5034, Helioparc, Pau (France)

    2005-02-01

    A robust method has been developed for simultaneous determination of mercury and butyltin compounds in aqueous samples. This method is capable of providing accurate results for analyte concentrations in the picogram per liter to nanogram per liter range. The simultaneous determination of the mercury and tin compounds is achieved by species-specific isotope dilution, derivatization, and gas chromatography-inductively coupled plasma mass spectrometer (GC-ICP-MS). In derivatization by ethylation and propylation, reaction conditions such as pH and the effect of chloride were carefully studied. Ethylation was found to be more sensitive to matrix effects, especially for mercury compounds. Propylation was thus the preferred derivatization method for simultaneous determination of organomercury and organotin compounds in environmental samples. The analytical method is highly accurate and precise, with RSD values of 1 and 3% for analyte concentrations in the picogram per liter to nanogram per liter range. By use of cleaning procedures and SIDMS blank measurements, detection limits in the range 10-60 pg L{sup -1} were achieved; these are suitable for determination of background levels of these contaminants in environmental samples. This was demonstrated by using the method for analysis of real snow and seawater samples. This work illustrates the great advantage of species-specific isotope dilution for the validation of an analytical speciation method - the possibility of overcoming species transformations and non-quantitative recovery. Analysis time is saved by use of the simultaneous method, because of the use of a single sample-preparation procedure and one analysis. (orig.)

  5. Prediction of fat-free mass by bioelectrical impedance analysis in older adults from developing countries: a cross-validation study using the deuterium dilution method

    International Nuclear Information System (INIS)

    Mateo, H. Aleman; Romero, J. Esparza; Valencia, M.E.

    2010-01-01

    Objective: Several limitations of published bioelectrical impedance analysis (BIA) equations have been reported. The aims were to develop in a multiethnic, elderly population a new prediction equation and cross- validate it along with some published BIA equations for estimating fat-free mass using deuterium oxide dilution as the reference method. Design and setting: Cross-sectional study of elderly from five developing countries. Methods: Total body water (TBW) measured by deuterium dilution was used to determine fat-free mass (FFM) in 383 subjects. Anthropometric and BIA variables were also measured. Only 377 subjects were included for the analysis, randomly divided into development and cross-validation groups after stratified by gender. Stepwise model selection was used to generate the model and Bland Altman analysis was used to test agreement. Results: FFM = 2.95 - 3.89 (Gender) + 0.514 (Ht2/Z) + 0.090 (Waist) + 0.156 (Body weight). The model fit parameters were an R2, total F-Ratio, and the SEE of 0.88, 314.3, and 3.3, respectively. None of the published BIA equations met the criteria for agreement. The new BIA equation underestimated FFM by just 0.3 kg in the cross-validation sample. The mean of the difference between FFM by TBW and the new BIA equation were not significantly different; 95% of the differences were between the limits of agreement of -6.3 to 6.9 kg of FFM. There was no significant association between the mean of the differences and their averages (r= 0.008 and p= 0.2). Conclusions:This new BIA equation offers a valid option compared with some of the current published BIA equations to estimate FFM in elderly subjects from five developing countries. (Authors)

  6. Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction.

    Science.gov (United States)

    Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

    2017-01-01

    The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly ( P essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

  7. Chemical and antimicrobial analysis of husk fiber aqueous extract ...

    African Journals Online (AJOL)

    Chemical and antimicrobial analysis of husk fiber aqueous extract from Cocos nucifera L. Davi Oliveira e Silva, Gabriel Rocha Martins, Antônio Jorge Ribeiro da Silva, Daniela Sales Alviano, Rodrigo Pires Nascimento, Maria Auxiliadora Coelho Kaplan, Celuta Sales Alviano ...

  8. Analysis of the Extracts of Isatis tinctoria by New Analytical ...

    African Journals Online (AJOL)

    The methods of extraction, separation and analysis of alkaloids and indole glucosinolates (GLs) of Isatis tinctoria were reviewed. Different analytical approaches such as High-pressure Liquid Chromatography (HPLC), Liquid Chromatography with Electrospray Ionization Mass Spectrometry (LC/ESI/MS), Electrospray ...

  9. Chromatographic-mass spectrometric analysis of ethanol extract of ...

    African Journals Online (AJOL)

    Methods: The dried root of Maesa perlaria var. formosana was extracted with 95 % ethanol for composition analysis under the following optimum GC-MS conditions: 250 °C inlet temperature, 250 °C MSD detector temperature, and GC oven temperature programmed as follows: initial temperature held at 70 °C for 15 min, ...

  10. Analysis of Coastline Extraction from Landsat-8 OLI Imagery

    Directory of Open Access Journals (Sweden)

    Yaolin Liu

    2017-10-01

    of −4.23 m and optimal MAD of 13.54 m. Further comparisons with single-band thresholding (Band 6, AWEI, and ISODATA also confirmed the superiority of strategy 3. For the various used pansharpening algorithms, five multiresolution analysis MRA-based pansharpening algorithms are more efficient than the component substitution CS-based pansharpening algorithms for coastline extraction from Landsat-8 OLI imagery. Among the five MRA-based fusion methods, the coastlines extracted from the fused images generated by Indusion, additive à trous wavelet transform (ATWT and additive wavelet luminance proportional (AWLP produced the most accurate and visually realistic representation. Therefore, pansharpening approaches can improve the accuracy of coastline extraction from Landsat-8 OLI imagery, and downscaling the PAN band to finer spatial resolution is able to further improve the coastline extraction accuracy, especially in crenulated coasts.

  11. Rapid automatic keyword extraction for information retrieval and analysis

    Science.gov (United States)

    Rose, Stuart J [Richland, WA; Cowley,; E, Wendy [Richland, WA; Crow, Vernon L [Richland, WA; Cramer, Nicholas O [Richland, WA

    2012-03-06

    Methods and systems for rapid automatic keyword extraction for information retrieval and analysis. Embodiments can include parsing words in an individual document by delimiters, stop words, or both in order to identify candidate keywords. Word scores for each word within the candidate keywords are then calculated based on a function of co-occurrence degree, co-occurrence frequency, or both. Based on a function of the word scores for words within the candidate keyword, a keyword score is calculated for each of the candidate keywords. A portion of the candidate keywords are then extracted as keywords based, at least in part, on the candidate keywords having the highest keyword scores.

  12. Gas chromatographic analysis of extractive solvent in reprocessing plants

    International Nuclear Information System (INIS)

    Marlet, B.

    1984-01-01

    Operation of a reprocessing plant using the Purex process is recalled and analytical controls for optimum performance are specified. The aim of this thesis is the development of analytical methods using gas chromatography required to follow the evolution of the extraction solvent during spent fuel reprocessing. The solvent at different concentrations, is analysed along the reprocessing lines in organic or aqueous phases. Solvent degradation interferes with extraction and decomposition products are analysed. The solvent becomes less and less efficient, also it is distilled and quality is checked. Traces of solvent should also be checked in waste water. Analysis are made as simple as possible to facilitate handling of radioactive samples [fr

  13. Helium dilution refrigerator

    International Nuclear Information System (INIS)

    1973-01-01

    A new system of continuous heat exchange for a helium dilution refrigerator is proposed. The 3 He effluent tube is concurrent with the affluent mixed helium tube in a vertical downward direction. Heat exchange efficiency is enhanced by placing in series a number of elements with an enlarged surface area

  14. Fast analysis of quaternary ammonium pesticides in food and beverages using cation-exchange chromatography coupled with isotope-dilution high-resolution mass spectrometry.

    Science.gov (United States)

    Nardin, Tiziana; Barnaba, Chiara; Abballe, Franco; Trenti, Gianmaria; Malacarne, Mario; Larcher, Roberto

    2017-10-01

    A fast separation based on cation-exchange liquid chromatography coupled with high-resolution mass spectrometry is proposed for simultaneous determination of chlormequat, difenzoquat, diquat, mepiquat and paraquat in several food and beverage commodities. Solid samples were extracted using a mixture of water/methanol/formic acid (69.6:30:0.4, v/v/v), while liquid samples were ten times diluted with the same solution. Separation was carried out on an experimental length-modified IonPac CS17 column (2 × 15 mm 2 ) that allowed the use of formic acid and acetonitrile as mobile phase. Detection limits for food and beverage matrices were established at 1.5 μg/L for chlormequat, difenzoquat and mepiquat, and 3 μg/L for diquat and paraquat, while for drinking water a pre-analytical sample concentration allowed detection limits of 9 and 20 ng/L, respectively. Precision, as repeatability (RSD%), ranged from 0.2 to 24%, with a median value of 6%, and trueness, as recovery, ranged from 64 to 118%, with a median value of 96%. The method developed was successfully applied to investigate the presence of herbicide residues in commercial commodities (mineral water, orange juice, beer, tea, green coffee bean, toasted coffee powder, cocoa bean, white corn flour, rice and sugar samples). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Quantitative Isotope-Dilution High-Resolution-Mass-Spectrometry Analysis of Multiple Intracellular Metabolites in Clostridium autoethanogenum with Uniformly 13C-Labeled Standards Derived from Spirulina.

    Science.gov (United States)

    Schatschneider, Sarah; Abdelrazig, Salah; Safo, Laudina; Henstra, Anne M; Millat, Thomas; Kim, Dong-Hyun; Winzer, Klaus; Minton, Nigel P; Barrett, David A

    2018-04-03

    We have investigated the applicability of commercially available lyophilized spirulina ( Arthrospira platensis), a microorganism uniformly labeled with 13 C, as a readily accessible source of multiple 13 C-labeled metabolites suitable as internal standards for the quantitative determination of intracellular bacterial metabolites. Metabolites of interest were analyzed by hydrophilic-interaction liquid chromatography coupled with high-resolution mass spectrometry. Multiple internal standards obtained from uniformly (U)- 13 C-labeled extracts from spirulina were used to enable isotope-dilution mass spectrometry (IDMS) in the identification and quantification of intracellular metabolites. Extraction of the intracellular metabolites of Clostridium autoethanogenum using 2:1:1 chloroform/methanol/water was found to be the optimal method in comparison with freeze-thaw, homogenization, and sonication methods. The limits of quantification were ≤1 μM with excellent linearity for all of the calibration curves ( R 2 ≥ 0.99) for 74 metabolites. The precision and accuracy were found to be within relative standard deviations (RSDs) of 15% for 49 of the metabolites and within RSDs of 20% for all of the metabolites. The method was applied to study the effects of feeding different levels of carbon monoxide (as a carbon source) on the central metabolism and Wood-Ljungdahl pathway of C. autoethanogenum grown in continuous culture over 35 days. Using LC-IDMS with U- 13 C spirulina allowed the successful quantification of 52 metabolites in the samples, including amino acids, carboxylic acids, sugar phosphates, purines, and pyrimidines. The method provided absolute quantitative data on intracellular metabolites that was suitable for computational modeling to understand and optimize the C. autoethanogenum metabolic pathways active in gas fermentation.

  16. Odorant Screening and Quantitation of Thiols in Carmenere Red Wine by Gas Chromatography-Olfactometry and Stable Isotope Dilution Assays.

    Science.gov (United States)

    Pavez, Carolina; Agosin, Eduardo; Steinhaus, Martin

    2016-05-04

    The sensory impact of thiols in Vitis vinifera 'Carmenere' red wines was evaluated. For this purpose, aroma extract dilution analysis was applied to the thiols isolated from a Carmenere red wine by affinity chromatography with a mercurated agarose gel. Results revealed the presence of four odorants, identified as 2-furanylmethanethiol, 3-sulfanylhexyl acetate, 3-sulfanyl-1-hexanol, and 2-methyl-3-sulfanyl-1-butanol, with the latter being described here for the first time in Carmenere red wines. Quantitation of the four thiols in the Carmenere wine screened by aroma extract dilution analysis and in three additional Carmenere wines by stable isotope dilution assays resulted in concentrations above the respective orthonasal odor detection threshold values. Triangle tests applied to wine model solutions with and without the addition of the four thiols showed significant differences, thus suggesting that the compounds do have the potential to influence the overall aroma of red wine.

  17. Analysis of Feature Extraction Methods for Speaker Dependent Speech Recognition

    Directory of Open Access Journals (Sweden)

    Gurpreet Kaur

    2017-02-01

    Full Text Available Speech recognition is about what is being said, irrespective of who is saying. Speech recognition is a growing field. Major progress is taking place on the technology of automatic speech recognition (ASR. Still, there are lots of barriers in this field in terms of recognition rate, background noise, speaker variability, speaking rate, accent etc. Speech recognition rate mainly depends on the selection of features and feature extraction methods. This paper outlines the feature extraction techniques for speaker dependent speech recognition for isolated words. A brief survey of different feature extraction techniques like Mel-Frequency Cepstral Coefficients (MFCC, Linear Predictive Coding Coefficients (LPCC, Perceptual Linear Prediction (PLP, Relative Spectra Perceptual linear Predictive (RASTA-PLP analysis are presented and evaluation is done. Speech recognition has various applications from daily use to commercial use. We have made a speaker dependent system and this system can be useful in many areas like controlling a patient vehicle using simple commands.

  18. Evolution of Analysis of Polyhenols from Grapes, Wines, and Extracts

    Directory of Open Access Journals (Sweden)

    Pierre-Louis Teissedre

    2013-01-01

    Full Text Available Grape and wine phenolics are structurally diverse, from simple molecules to oligomers and polymers usually designated as tannins. They have an important impact on the organoleptic properties of wines, that’s why their analysis and quantification are of primordial importance. The extraction of phenolics from grapes and from wines is the first step involved in the analysis. Then, several analytical methods have been developed for the determination of total content of phenolic, while chromatographic and spectrophotometric analyses are continuously improved in order to achieve adequate separation of phenolic molecules, their subsequent identification and quantification. This review provides a summary of evolution of analysis of polyphenols from grapes, wines and extracts.

  19. Certification of butyltins and phenyltins in marine sediment certified reference material by species-specific isotope-dilution mass spectrometric analysis using synthesized {sup 118}Sn-enriched organotin compounds

    Energy Technology Data Exchange (ETDEWEB)

    Inagaki, Kazumi; Takatsu, Akiko; Watanabe, Takuro; Aoyagi, Yoshie; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi [National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, National Metrology Institute of Japan (NMIJ), Tsukuba, Ibaraki (Japan)

    2007-04-15

    A new marine sediment certified reference material, NMIJ CRM 7306-a, for butyltin and phenyltin analysis has been prepared and certified by the National Metrological Institute of Japan at the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Candidate sediment material was collected at a bay near industrial activity in Japan. After air-drying, sieving, and mixing the material was sterilized with {gamma}-ray irradiation. The material was re-mixed and packaged into 250 glass bottles (15 g each) and these were stored in a freezer at -30 C. Certification was performed by use of three different types of species-specific isotope-dilution mass spectrometry (SSID-MS) - SSID-GC-ICP-MS, SSID-GC-MS, and SSID-LC-ICP-MS, with {sup 118}Sn-enriched organotin compounds synthesized from {sup 118}Sn-enriched metal used as a spike. The {sup 118}Sn-enriched mono-butyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) were synthesized as a mixture whereas the {sup 118}Sn-enriched di-phenyltin (DPhT) and triphenyltin (TPhT) were synthesized individually. Four different extraction methods, mechanical shaking, ultrasonic, microwave-assisted, and pressurized liquid extraction, were adopted to avoid possible analytical bias caused by non-quantitative extraction and degradation or inter-conversion of analytes in sample preparations. Tropolone was used as chelating agent in all the extraction methods. Certified values are given for TBT 44{+-}3 {mu}g kg{sup -1} as Sn, DBT 51 {+-} 2 {mu}g kg{sup -1} as Sn, MBT 67 {+-} 3 {mu}g kg{sup -1} as Sn, TPhT 6.9 {+-} 1.2 {mu}g kg{sup -1} as Sn, and DPhT 3.4 {+-} 1.2 {mu}g kg{sup -1} as Sn. These levels are lower than in other sediment CRMs currently available for analysis of organotin compounds. (orig.)

  20. Fetal source extraction from magnetocardiographic recordings by dependent component analysis

    Energy Technology Data Exchange (ETDEWEB)

    Araujo, Draulio B de [Department of Physics and Mathematics, FFCLRP, University of Sao Paulo, Ribeirao Preto, SP (Brazil); Barros, Allan Kardec [Department of Electrical Engineering, Federal University of Maranhao, Sao Luis, Maranhao (Brazil); Estombelo-Montesco, Carlos [Department of Physics and Mathematics, FFCLRP, University of Sao Paulo, Ribeirao Preto, SP (Brazil); Zhao, Hui [Department of Medical Physics, University of Wisconsin, Madison, WI (United States); Filho, A C Roque da Silva [Department of Physics and Mathematics, FFCLRP, University of Sao Paulo, Ribeirao Preto, SP (Brazil); Baffa, Oswaldo [Department of Physics and Mathematics, FFCLRP, University of Sao Paulo, Ribeirao Preto, SP (Brazil); Wakai, Ronald [Department of Medical Physics, University of Wisconsin, Madison, WI (United States); Ohnishi, Noboru [Department of Information Engineering, Nagoya University (Japan)

    2005-10-07

    Fetal magnetocardiography (fMCG) has been extensively reported in the literature as a non-invasive, prenatal technique that can be used to monitor various functions of the fetal heart. However, fMCG signals often have low signal-to-noise ratio (SNR) and are contaminated by strong interference from the mother's magnetocardiogram signal. A promising, efficient tool for extracting signals, even under low SNR conditions, is blind source separation (BSS), or independent component analysis (ICA). Herein we propose an algorithm based on a variation of ICA, where the signal of interest is extracted using a time delay obtained from an autocorrelation analysis. We model the system using autoregression, and identify the signal component of interest from the poles of the autocorrelation function. We show that the method is effective in removing the maternal signal, and is computationally efficient. We also compare our results to more established ICA methods, such as FastICA.

  1. Defects in dilute nitrides

    International Nuclear Information System (INIS)

    Chen, W.M.; Buyanova, I.A.; Tu, C.W.; Yonezu, H.

    2005-01-01

    We provide a brief review our recent results from optically detected magnetic resonance studies of grown-in non-radiative defects in dilute nitrides, i.e. Ga(In)NAs and Ga(Al,In)NP. Defect complexes involving intrinsic defects such as As Ga antisites and Ga i self interstitials were positively identified.Effects of growth conditions, chemical compositions and post-growth treatments on formation of the defects are closely examined. These grown-in defects are shown to play an important role in non-radiative carrier recombination and thus in degrading optical quality of the alloys, harmful to performance of potential optoelectronic and photonic devices based on these dilute nitrides. (author)

  2. [Automatic Extraction and Analysis of Dosimetry Data in Radiotherapy Plans].

    Science.gov (United States)

    Song, Wei; Zhao, Di; Lu, Hong; Zhang, Biyun; Ma, Jun; Yu, Dahai

    To improve the efficiency and accuracy of extraction and analysis of dosimetry data in radiotherapy plans for a batch of patients. With the interface function provided in Matlab platform, a program was written to extract the dosimetry data exported from treatment planning system in DICOM RT format and exported the dose-volume data to an Excel file with the SPSS compatible format. This method was compared with manual operation for 14 gastric carcinoma patients to validate the efficiency and accuracy. The output Excel data were compatible with SPSS in format, the dosimetry data error for PTV dose interval of 90%-98%, PTV dose interval of 99%-106% and all OARs were -3.48E-5 ± 3.01E-5, -1.11E-3 ± 7.68E-4, -7.85E-5 ± 9.91E-5 respectively. Compared with manual operation, the time required was reduced from 5.3 h to 0.19 h and input error was reduced from 0.002 to 0. The automatic extraction of dosimetry data in DICOM RT format for batch patients, the SPSS compatible data exportation, quick analysis were achieved in this paper. The efficiency of clinical researches based on dosimetry data analysis of large number of patients will be improved with this methods.

  3. Introducing AAA-MS, a rapid and sensitive method for amino acid analysis using isotope dilution and high-resolution mass spectrometry.

    Science.gov (United States)

    Louwagie, Mathilde; Kieffer-Jaquinod, Sylvie; Dupierris, Véronique; Couté, Yohann; Bruley, Christophe; Garin, Jérôme; Dupuis, Alain; Jaquinod, Michel; Brun, Virginie

    2012-07-06

    Accurate quantification of pure peptides and proteins is essential for biotechnology, clinical chemistry, proteomics, and systems biology. The reference method to quantify peptides and proteins is amino acid analysis (AAA). This consists of an acidic hydrolysis followed by chromatographic separation and spectrophotometric detection of amino acids. Although widely used, this method displays some limitations, in particular the need for large amounts of starting material. Driven by the need to quantify isotope-dilution standards used for absolute quantitative proteomics, particularly stable isotope-labeled (SIL) peptides and PSAQ proteins, we developed a new AAA assay (AAA-MS). This method requires neither derivatization nor chromatographic separation of amino acids. It is based on rapid microwave-assisted acidic hydrolysis followed by high-resolution mass spectrometry analysis of amino acids. Quantification is performed by comparing MS signals from labeled amino acids (SIL peptide- and PSAQ-derived) with those of unlabeled amino acids originating from co-hydrolyzed NIST standard reference materials. For both SIL peptides and PSAQ standards, AAA-MS quantification results were consistent with classical AAA measurements. Compared to AAA assay, AAA-MS was much faster and was 100-fold more sensitive for peptide and protein quantification. Finally, thanks to the development of a labeled protein standard, we also extended AAA-MS analysis to the quantification of unlabeled proteins.

  4. Existing and emerging technologies for measuring stable isotope labelled retinol in biological samples: isotope dilution analysis of body retinol stores.

    Science.gov (United States)

    Preston, Tom

    2014-01-01

    This paper discusses some of the recent improvements in instrumentation used for stable isotope tracer measurements in the context of measuring retinol stores, in vivo. Tracer costs, together with concerns that larger tracer doses may perturb the parameter under study, demand that ever more sensitive mass spectrometric techniques are developed. GCMS is the most widely used technique. It has high sensitivity in terms of sample amount and uses high resolution GC, yet its ability to detect low isotope ratios is limited by background noise. LCMSMS may become more accessible for tracer studies. Its ability to measure low level stable isotope tracers may prove superior to GCMS, but it is isotope ratio MS (IRMS) that has been designed specifically for low level stable isotope analysis through accurate analysis of tracer:tracee ratios (the tracee being the unlabelled species). Compound-specific isotope analysis, where GC is interfaced to IRMS, is gaining popularity. Here, individual 13C-labelled compounds are separated by GC, combusted to CO2 and transferred on-line for ratiometric analysis by IRMS at the ppm level. However, commercially-available 13C-labelled retinol tracers are 2 - 4 times more expensive than deuterated tracers. For 2H-labelled compounds, GC-pyrolysis-IRMS has now become more generally available as an operating mode on the same IRMS instrument. Here, individual compounds are separated by GC and pyrolysed to H2 at high temperature for analysis by IRMS. It is predicted that GC-pyrolysis-IRMS will facilitate low level tracer procedures to measure body retinol stores, as has been accomplished in the case of fatty acids and amino acids. Sample size requirements for GC-P-IRMS may exceed those of GCMS, but this paper discusses sample preparation procedures and predicts improvements, particularly in the efficiency of sample introduction.

  5. Mycoestrogen determination in cow milk: Magnetic solid-phase extraction followed by liquid chromatography and tandem mass spectrometry analysis.

    Science.gov (United States)

    Capriotti, Anna Laura; Cavaliere, Chiara; Foglia, Patrizia; La Barbera, Giorgia; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

    2016-12-01

    Recently, magnetic solid-phase extraction has gained interest because it presents various operational advantages over classical solid-phase extraction. Furthermore, magnetic nanoparticles are easy to prepare, and various materials can be used in their synthesis. In the literature, there are only few studies on the determination of mycoestrogens in milk, although their carryover in milk has occurred. In this work, we wanted to develop the first (to the best of our knowledge) magnetic solid-phase extraction protocol for six mycoestrogens from milk, followed by liquid chromatography and tandem mass spectrometry analysis. Magnetic graphitized carbon black was chosen as the adsorbent, as this carbonaceous material, which is very different from the most diffuse graphene and carbon nanotubes, had already shown selectivity towards estrogenic compounds in milk. The graphitized carbon black was decorated with Fe 3 O 4 , which was confirmed by the characterization analyses. A milk deproteinization step was avoided, using only a suitable dilution in phosphate buffer as sample pretreatment. The overall process efficiency ranged between 52 and 102%, whereas the matrix effect considered as signal suppression was below 33% for all the analytes even at the lowest spiking level. The obtained method limits of quantification were below those of other published methods that employ classical solid-phase extraction protocols. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Simultaneous analysis of polychlorinated biphenyls and polychlorinated naphthalenes by isotope dilution comprehensive two-dimensional gas chromatography high-resolution time-of-flight mass spectrometry

    International Nuclear Information System (INIS)

    Xia, Dan; Gao, Lirong; Zheng, Minghui; Wang, Shasha; Liu, Guorui

    2016-01-01

    Polychlorinated biphenyls (PCBs) and polychlorinated naphthalenes (PCNs) are listed as persistent organic pollutants (POPs) under the Stockholm Convention. Because they have similar physical and chemical properties, they are coeluted and are usually analyzed separately by different gas chromatography high-resolution mass spectrometry (GC-HRMS) methods. In this study, a novel method was developed for simultaneous analysis of six indicator PCBs, 12 dioxin-like PCBs, and 16 PCNs using isotope dilution comprehensive two-dimensional gas chromatography with high-resolution time-of-flight mass spectrometry (GC × GC-HRTOF-MS). The method parameters, including the type of GC column, oven temperature program, and modulation period, were systematically optimized. Complete separation of all target analytes and the matrix was achieved with a DB-XLB column in the first dimension and a BPX-70 column in the second dimension. The isotope dilution method was used for quantification of the PCBs and PCNs by GC × GC-HRTOF-MS. The method showed good linearity from 5 to 500 pg μL"−"1 for all the target compounds. The instrumental limit of detection ranged from 0.03 to 0.3 pg μL"−"1 for the 18 PCB congeners and from 0.09 to 0.6 pg μL"−"1 for the 16 PCN congeners. Repeatability for triplicate injections was always lower than 20%. The method was successfully applied to the determination of 18 PCBs present at 0.9–2054 pg g"−"1 and 16 PCNs present at 0.2–15.7 pg g"−"1 in three species of fish. The GC × GC-HRTOF-MS results agreed with those obtained by GC-HRMS. The GC × GC-HRTOF-MS method proved to be a sensitive and accurate technique for simultaneous analysis of the selected PCBs and PCNs. With the excellent chromatographic separation offered by GC × GC and accurate mass measurements offered by HRTOF-MS, this method allowed identification of non-target contaminants in the fish samples, including organochlorine pesticides and polycyclic aromatic

  7. Simultaneous analysis of polychlorinated biphenyls and polychlorinated naphthalenes by isotope dilution comprehensive two-dimensional gas chromatography high-resolution time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Xia, Dan [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China); University of Chinese Academy of Sciences, Beijing 100085 (China); Gao, Lirong, E-mail: gaolr@rcees.ac.cn [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China); Zheng, Minghui; Wang, Shasha; Liu, Guorui [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China)

    2016-09-21

    Polychlorinated biphenyls (PCBs) and polychlorinated naphthalenes (PCNs) are listed as persistent organic pollutants (POPs) under the Stockholm Convention. Because they have similar physical and chemical properties, they are coeluted and are usually analyzed separately by different gas chromatography high-resolution mass spectrometry (GC-HRMS) methods. In this study, a novel method was developed for simultaneous analysis of six indicator PCBs, 12 dioxin-like PCBs, and 16 PCNs using isotope dilution comprehensive two-dimensional gas chromatography with high-resolution time-of-flight mass spectrometry (GC × GC-HRTOF-MS). The method parameters, including the type of GC column, oven temperature program, and modulation period, were systematically optimized. Complete separation of all target analytes and the matrix was achieved with a DB-XLB column in the first dimension and a BPX-70 column in the second dimension. The isotope dilution method was used for quantification of the PCBs and PCNs by GC × GC-HRTOF-MS. The method showed good linearity from 5 to 500 pg μL{sup −1} for all the target compounds. The instrumental limit of detection ranged from 0.03 to 0.3 pg μL{sup −1} for the 18 PCB congeners and from 0.09 to 0.6 pg μL{sup −1} for the 16 PCN congeners. Repeatability for triplicate injections was always lower than 20%. The method was successfully applied to the determination of 18 PCBs present at 0.9–2054 pg g{sup −1} and 16 PCNs present at 0.2–15.7 pg g{sup −1} in three species of fish. The GC × GC-HRTOF-MS results agreed with those obtained by GC-HRMS. The GC × GC-HRTOF-MS method proved to be a sensitive and accurate technique for simultaneous analysis of the selected PCBs and PCNs. With the excellent chromatographic separation offered by GC × GC and accurate mass measurements offered by HRTOF-MS, this method allowed identification of non-target contaminants in the fish samples, including organochlorine pesticides and

  8. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/......., organism, tissue and disease terms. The evaluators in the BioCreative V Interactive Annotation Task found the system to be intuitive, useful, well documented and sufficiently accurate to be helpful in spotting relevant text passages and extracting organism and environment terms. Comparison of fully manual...

  9. Extraction and Quantitative HPLC Analysis of Coumarin in Hydroalcoholic Extracts of Mikania glomerata Spreng: ("guaco" Leaves

    Directory of Open Access Journals (Sweden)

    Celeghini Renata M. S.

    2001-01-01

    Full Text Available Methods for preparation of hydroalcoholic extracts of "guaco" (Mikania glomerata Spreng. leaves were compared: maceration, maceration under sonication, infusion and supercritical fluid extraction. Evaluation of these methods showed that maceration under sonication had the best results, when considering the ratio extraction yield/extraction time. A high performance liquid chromatography (HPLC procedure for the determination of coumarin in these hydroalcoholic extracts of "guaco" leaves is described. The HPLC method is shown to be sensitive and reproducible.

  10. The separation and determination of fatty acids by isotopic dilution and radiogas-liquid chromatography

    International Nuclear Information System (INIS)

    Beardsley, D.A.

    1981-01-01

    A number of static phases have been evaluated for the GLC separation of fatty acids. Of those investigated, only AT 1200 was capable of resolving the isomeric forms of the acids. A radiogas-liquid chromatographic method incorporating isotopic dilution analysis has been developed for the determination of n-butyric acid. The proposed method has been applied to the determination of the acid in hydrolysed butter fat and milk chocolate extracts. (author)

  11. Simultaneous analysis of multiple classes of antimicrobials in environmental water samples using SPE coupled with UHPLC-ESI-MS/MS and isotope dilution.

    Science.gov (United States)

    Tran, Ngoc Han; Chen, Hongjie; Do, Thanh Van; Reinhard, Martin; Ngo, Huu Hao; He, Yiliang; Gin, Karina Yew-Hoong

    2016-10-01

    A robust and sensitive analytical method was developed for the simultaneous analysis of 21 target antimicrobials in different environmental water samples. Both single SPE and tandem SPE cartridge systems were investigated to simultaneously extract multiple classes of antimicrobials. Experimental results showed that good extraction efficiencies (84.5-105.6%) were observed for the vast majority of the target analytes when extraction was performed using the tandem SPE cartridge (SB+HR-X) system under an extraction pH of 3.0. HPLC-MS/MS parameters were optimized for simultaneous analysis of all the target analytes in a single injection. Quantification of target antimicrobials in water samples was accomplished using 15 isotopically labeled internal standards (ILISs), which allowed the efficient compensation of the losses of target analytes during sample preparation and correction of matrix effects during UHPLC-MS/MS as well as instrument fluctuations in MS/MS signal intensity. Method quantification limit (MQL) for most target analytes based on SPE was below 5ng/L for surface waters, 10ng/L for treated wastewater effluents, and 15ng/L for raw wastewater. The method was successfully applied to detect and quantify the occurrence of the target analytes in raw influent, treated effluent and surface water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Selective extraction of actinides by calixarenes: application to bioassay analysis

    International Nuclear Information System (INIS)

    Boulet, B.

    2006-01-01

    In the context of nuclear workers monitoring, the aim of this PhD was to selectively isolate U, Pu, and Am from urine to propose a new analytical procedure to the Medical and Biology Analysis Laboratories. The 1,3,5-OCH 3 -2,4,6-OCH 2 CONHOH-p-tert-butyl-calix[6]arene molecule has been selected as a promising extractant for U, Pu, and Am. Its physico-chemical properties and its affinity for UO 2 2+ have been studied through two approaches, one theoretical (molecular modelling at DFT level), and one experimental. The extractions of the three actinides by the hydroxamic calix[6]arene were quantitative in liquid-liquid and solid-liquid systems. Their separation has also been shown possible and efficient. After optimization, the proposed procedure should allow the laboratories to carry out the chemical treatment of urine, before the measurement, in one day instead of the three days needed nowadays. (author)

  13. Plant Phenolics: Extraction, Analysis and Their Antioxidant and Anticancer Properties

    Directory of Open Access Journals (Sweden)

    Jin Dai

    2010-10-01

    Full Text Available Phenolics are broadly distributed in the plant kingdom and are the most abundant secondary metabolites of plants. Plant polyphenols have drawn increasing attention due to their potent antioxidant properties and their marked effects in the prevention of various oxidative stress associated diseases such as cancer. In the last few years, the identification and development of phenolic compounds or extracts from different plants has become a major area of health- and medical-related research. This review provides an updated and comprehensive overview on phenolic extraction, purification, analysis and quantification as well as their antioxidant properties. Furthermore, the anticancer effects of phenolics in-vitro and in-vivo animal models are viewed, including recent human intervention studies. Finally, possible mechanisms of action involving antioxidant and pro-oxidant activity as well as interference with cellular functions are discussed.

  14. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry

    International Nuclear Information System (INIS)

    2010-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  15. Dehydration of ethanol with salt extractive distillation-a comparative analysis between processes with salt recovery

    Energy Technology Data Exchange (ETDEWEB)

    Ligero, E.L.; Ravagnani, T.M.K. [Departamento de Engenharia de Sistemas Qumicos, Faculdade de Engenharia Qumica, Universidade Estadual de Campinas, Campinas, Sao Paulo (Brazil)

    2003-07-01

    Anhydrous ethanol can be obtained from a dilute aqueous solution of ethanol via extractive distillation with potassium acetate. Two process flowsheets with salt recovery were proposed. In the first, dilute ethanol is directly fed to a salt extractive distillation column and, after that, the salt is recovered in a multiple effect evaporator followed by a spray dryer. In the second, the concentrated ethanol from conventional distillation is fed to a salt extractive distillation column. In this case, salt is recovered in a single spray dryer. In both processes the recovered salt is recycled to be used in the extractive distillation column. Every component of each process was rigorously modeled and its behavior was simulated for a wide range of operating conditions. A global simulation was then carried out. The results show that the second process is more interesting in terms of energy consumption than the first. Furthermore, it would be easier to implement changes on existing benzene extractive anhydrous ethanol plants to convert them to more ecologically attractive concentrated ethanol feed processes. (author)

  16. Chelating agents as stationary phase in extraction chromatography, ch. 11

    International Nuclear Information System (INIS)

    Sebesta, F.

    1975-01-01

    Chelating agents have been used largely in extraction chromatography for separations related to activation analysis, for concentration of metals from dilute solutions, and for preparation of radiochemically pure or carrier-free radionuclides. This review deals with the theory of extraction by chelating agents, the experimental technique, and the chelating agents and systems used (β-diketones, oximes, hydroxamic acid, dithizone and diethyldithiocarbamic acid)

  17. A simplification of the deuterium oxide dilution technique using FT-IR analysis of plasma, for estimating piglet milk intake

    International Nuclear Information System (INIS)

    Glencross, B.D.; Tuckey, R.C.; Hartmann, P.E.; Mullan, B.P.

    1997-01-01

    Previous studies estimating milk intake using deuterium oxide (D 2 O) as a tracer have required sublimation of the sample fluid (usually plasma) to remove solids and retrieve total water. This procedure has been simplified by directly measuring the D 2 O content of plasma with a Fourier transform-infrared (FT-IR) spectrometer, removing the requirement for sample sublimation. Comparisons of samples that were split and then analysed as water of sublimation and as total plasma were performed. It was found that the direct analysis of the plasma could be achieved without a loss in fidelity of the results (sublimated v. plasma, r 2 = 0.976; n = 26). Linearity of assay standards was very high (r 2 > 0.997). The modified technique was used to determine the milk intake by piglets from litters of 7 sows during established lactation (Days 10-15). Water turnover (WTO) was shown to be the primary point by which differences in the piglet milk intakes were influenced. Differences in the milk composition had minimal effect on the milk intake determinations. Milk intake by each piglet was shown to be strongly correlated to piglet growth (r 2 = 0.59, P 2 = 0.84, P < 0.01). Copyright (1997) CSIRO Australia

  18. Introduction to body composition assessment using the deuterium dilution technique with analysis of saliva samples by fourier transform infrared spectrometry

    International Nuclear Information System (INIS)

    2010-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  19. Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction

    Directory of Open Access Journals (Sweden)

    Ghahramanloo KH

    2017-07-01

    Full Text Available Kourosh Hasanzadeh Ghahramanloo,1 Behnam Kamalidehghan,2 Hamid Akbari Javar,3 Riyanto Teguh Widodo,1 Keivan Majidzadeh,4 Mohamed Ibrahim Noordin1 1Department of Pharmacy, Faculty of Medicine, University of Malaya, Kuala Lumpur, Malaysia; 2Medical Genetics Department, National Institute of Genetic Engineering and Biotechnology (NIGEB, 3Department of Pharmaceutics, Faculty of Pharmacy, Tehran University of Medical Sciences (TUMS, 4Breast Cancer Research Center (BCRC Academic Center for Education, Culture and Research, Tehran, Iran Abstract: The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%–61.85% and oleic acid (1.64%–18.97%. Thymoquinone (0.72%–21.03% was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (P<0.05 higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique. Keywords: Nigella sativa L., essential oil extraction, supercritical fluid extraction, solvent extraction, fatty acid composition, thymoquinone, linoleic acid

  20. Independent component analysis for automatic note extraction from musical trills

    Science.gov (United States)

    Brown, Judith C.; Smaragdis, Paris

    2004-05-01

    The method of principal component analysis, which is based on second-order statistics (or linear independence), has long been used for redundancy reduction of audio data. The more recent technique of independent component analysis, enforcing much stricter statistical criteria based on higher-order statistical independence, is introduced and shown to be far superior in separating independent musical sources. This theory has been applied to piano trills and a database of trill rates was assembled from experiments with a computer-driven piano, recordings of a professional pianist, and commercially available compact disks. The method of independent component analysis has thus been shown to be an outstanding, effective means of automatically extracting interesting musical information from a sea of redundant data.

  1. Oxygen isotope analysis of plant water without extraction procedure

    International Nuclear Information System (INIS)

    Gan, K.S.; Wong, S.C.; Farquhar, G.D.; Yong, J.W.H.

    2001-01-01

    Isotopic analyses of plant water (mainly xylem, phloem and leaf water) are gaming importance as the isotopic signals reflect plant-environment interactions, affect the oxygen isotopic composition of atmospheric O 2 and CO 2 and are eventually incorporated into plant organic matter. Conventionally, such isotopic measurements require a time-consuming process of isolating the plant water by azeotropic distillation or vacuum extraction, which would not complement the speed of isotope analysis provided by continuous-flow IRMS (Isotope-Ratio Mass Spectrometry), especially when large data sets are needed for statistical calculations in biological studies. Further, a substantial amount of plant material is needed for water extraction and leaf samples would invariably include unenriched water from the fine veins. To measure sub-microlitre amount of leaf mesophyll water, a new approach is undertaken where a small disc of fresh leaf is cut using a specially designed leaf punch, and pyrolysed directly in an IRMS. By comparing with results from pyrolysis of the dry matter of the same leaf, the 18 O content of leaf water can be determined without extraction from fresh leaves. This method is validated using a range of cellulose-water mixtures to simulate the constituents of fresh leaf. Cotton leaf water δ 18 O obtained from both methods of fresh leaf pyrolysis and azeotropic distillation will be compared. The pyrolysis technique provides a robust approach to measure the isotopic content of water or any volatile present in a homogeneous solution or solid hydrous substance

  2. Prominent feature extraction for review analysis: an empirical study

    Science.gov (United States)

    Agarwal, Basant; Mittal, Namita

    2016-05-01

    Sentiment analysis (SA) research has increased tremendously in recent times. SA aims to determine the sentiment orientation of a given text into positive or negative polarity. Motivation for SA research is the need for the industry to know the opinion of the users about their product from online portals, blogs, discussion boards and reviews and so on. Efficient features need to be extracted for machine-learning algorithm for better sentiment classification. In this paper, initially various features are extracted such as unigrams, bi-grams and dependency features from the text. In addition, new bi-tagged features are also extracted that conform to predefined part-of-speech patterns. Furthermore, various composite features are created using these features. Information gain (IG) and minimum redundancy maximum relevancy (mRMR) feature selection methods are used to eliminate the noisy and irrelevant features from the feature vector. Finally, machine-learning algorithms are used for classifying the review document into positive or negative class. Effects of different categories of features are investigated on four standard data-sets, namely, movie review and product (book, DVD and electronics) review data-sets. Experimental results show that composite features created from prominent features of unigram and bi-tagged features perform better than other features for sentiment classification. mRMR is a better feature selection method as compared with IG for sentiment classification. Boolean Multinomial Naïve Bayes) algorithm performs better than support vector machine classifier for SA in terms of accuracy and execution time.

  3. Quantitative immunoelectrophoretic analysis of extract from cow hair and dander

    Energy Technology Data Exchange (ETDEWEB)

    Prahl, P; Weeke, B; Loewenstein, H [Rigshospitalet, Copenhagen (Denmark)

    1978-01-01

    Quantitative immunoelectrophoresis used for the analysis of a dialysed, centrifuged and freeze-dried extract from cow hair and dander revealed 17 antigens. Five of these were identified as serum proteins. Partial identity to antigens of serum and extract from hair and dander of goat, sheep, swine, horse, dog, cat, and guinea pig, and to antigens of house dust was demonstrated. Sera from 36 patients with manifest allergy to cow hair and dander selected on the basis of case history, RAST, skin and provocation test, were examined in crossed radioimmunoelectrophoresis (CRIE); sera from five persons with high serum IgE, but without allergy to cow hair and dander, and sera from five normal individuals were controls. 31/36 of the sera contained IgE with specific affinity for two of the antigens of the extract. Further, two major and six minor allergens were identified. The control sera showed no specific IgE binding. A significant positive correlation was found between RAST and CRIE for the first group of patients. The approximate molecular weights of the four major allergens obtained by means of gel chromatography were: 2.4 x 10/sup 4/, 2 x 10/sup 4/, 2 x 10/sup 5/ dalton, respectively. Using Con-A and Con-A Sepharose in crossed immunoaffinoelectrophoresis, eight of the antigens were revealed to contain groups with affinity for Con-A.

  4. Quantitative immunoelectrophoretic analysis of extract from cow hair and dander

    International Nuclear Information System (INIS)

    Prahl, P.; Weeke, B.; Loewenstein, H.

    1978-01-01

    Quantitative immunoelectrophoresis used for the analysis of a dialysed, centrifuged and freeze-dried extract from cow hair and dander revealed 17 antigens. Five of these were identified as serum proteins. Partial identity to antigens of serum and extract from hair and dander of goat, sheep, swine, horse, dog, cat, and guinea pig, and to antigens of house dust was demonstrated. Sera from 36 patients with manifest allergy to cow hair and dander selected on the basis of case history, RAST, skin and provocation test, were examined in crossed radioimmunoelectrophoresis (CRIE); sera from five persons with high serum IgE, but without allergy to cow hair and dander, and sera from five normal individuals were controls. 31/36 of the sera contained IgE with specific affinity for two of the antigens of the extract. Further, two major and six minor allergens were identified. The control sera showed no specific IgE binding. A significant positive correlation was found between RAST and CRIE for the first group of patients. The approximate molecular weights of the four major allergens obtained by means of gel chromatography were: 2.4 x 10 4 , 2 x 10 4 , 2 x 10 5 dalton, respectively. Using Con-A and Con-A Sepharose in crossed immunoaffinoelectrophoresis, eight of the antigens were revealed to contain groups with affinity for Con-A. (author)

  5. Development of a routine analysis of 4-mercapto-4-methylpentan-2-one in wine by stable isotope dilution assay and mass tandem spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dagan, Laurent; Reillon, Florence; Roland, Aurélie; Schneider, Rémi, E-mail: remi@nyseos.fr

    2014-04-01

    Highlights: • We proposed a routine method to analyze the 4-methyl-4-mercaptopentan-2-one in wine. • We developed the first method with sensitivity below the 4MMP perception threshold. • We obtained an accurate method by using the stable isotope dilution assay approach. Abstract: The 4-mercapto-4-methylpentan-2-one (4MMP) is a key aroma compound in wines, especially in Sauvignon Blanc ones. Its accurate quantification is quite difficult due to its traces levels and its reactivity in wine conferred by the thiol function. In this paper, we proposed a new method for its quantification in wine without any sample preparation, based on automated derivatization procedure by methoximation and SIDA–SPME–GC–MS/MS analysis. The derivatization procedure was adapted from a previously published method in order to decrease the amount of reagents and the volume of wine (only 3 mL are required). The use of SPME and the detection conditions have also been optimized to reach the best sensitivity as possible. The method was then validated according to the International Organization of Vine and Wine recommendations and exhibited excellent performances. Indeed, this method allowed us to quantify the 4MMP in wine at traces levels (LOD = 0.19 ng L₅⁻¹) with reproducible results (RSD < 15%) and a very good accuracy (recovery = 102%)

  6. Analysis, by Relap5 code, of boron dilution phenomena in a Small Break Loca Transient, performed in PKL III E 2.2 test

    International Nuclear Information System (INIS)

    Rizzo, G.; Vella, G.

    2007-01-01

    The present work is finalized to investigate the E2.2 thermal-hydraulics transient of the PKL III facility, which is a scaled reproduction of a typical German PWR, operated by FRAMATOME-ANP in Erlangen, Germany, within the framework of an international cooperation (OECD/SETH project). The main purpose of the project is to study boron dilution events in Pressurized Water Reactors and to contribute to the assessment of thermal-hydraulic system codes like Relap5. The experimental test PKL III E2.2 investigates the behavior of a typical PWR after a Small Break Loss Of Coolant Accident (SB-LOCA) in a cold leg and an immediate injection of borated water in two cold legs. The main purpose of this work is to simulate the PKL III test facility and particularly its experimental transient by Relap5 system code. The adopted nodalization, already available at Department of Nuclear Engineering (DIN), has been reviewed and applied with an accurate analysis of the experimental test parameters. The main result relies in a good agreement of calculated data with experimental measures for a number of main important variables. (author)

  7. Development of a routine analysis of 4-mercapto-4-methylpentan-2-one in wine by stable isotope dilution assay and mass tandem spectrometry

    International Nuclear Information System (INIS)

    Dagan, Laurent; Reillon, Florence; Roland, Aurélie; Schneider, Rémi

    2014-01-01

    Highlights: • We proposed a routine method to analyze the 4-methyl-4-mercaptopentan-2-one in wine. • We developed the first method with sensitivity below the 4MMP perception threshold. • We obtained an accurate method by using the stable isotope dilution assay approach. - Abstract: The 4-mercapto-4-methylpentan-2-one (4MMP) is a key aroma compound in wines, especially in Sauvignon Blanc ones. Its accurate quantification is quite difficult due to its traces levels and its reactivity in wine conferred by the thiol function. In this paper, we proposed a new method for its quantification in wine without any sample preparation, based on automated derivatization procedure by methoximation and SIDA–SPME–GC–MS/MS analysis. The derivatization procedure was adapted from a previously published method in order to decrease the amount of reagents and the volume of wine (only 3 mL are required). The use of SPME and the detection conditions have also been optimized to reach the best sensitivity as possible. The method was then validated according to the International Organization of Vine and Wine recommendations and exhibited excellent performances. Indeed, this method allowed us to quantify the 4MMP in wine at traces levels (LOD = 0.19 ng L −1 ) with reproducible results (RSD < 15%) and a very good accuracy (recovery = 102%)

  8. Enhanced spot preparation for liquid extractive sampling and analysis

    Science.gov (United States)

    Van Berkel, Gary J.; King, Richard C.

    2015-09-22

    A method for performing surface sampling of an analyte, includes the step of placing the analyte on a stage with a material in molar excess to the analyte, such that analyte-analyte interactions are prevented and the analyte can be solubilized for further analysis. The material can be a matrix material that is mixed with the analyte. The material can be provided on a sample support. The analyte can then be contacted with a solvent to extract the analyte for further processing, such as by electrospray mass spectrometry.

  9. Fetal ECG extraction using independent component analysis by Jade approach

    Science.gov (United States)

    Giraldo-Guzmán, Jader; Contreras-Ortiz, Sonia H.; Lasprilla, Gloria Isabel Bautista; Kotas, Marian

    2017-11-01

    Fetal ECG monitoring is a useful method to assess the fetus health and detect abnormal conditions. In this paper we propose an approach to extract fetal ECG from abdomen and chest signals using independent component analysis based on the joint approximate diagonalization of eigenmatrices approach. The JADE approach avoids redundancy, what reduces matrix dimension and computational costs. Signals were filtered with a high pass filter to eliminate low frequency noise. Several levels of decomposition were tested until the fetal ECG was recognized in one of the separated sources output. The proposed method shows fast and good performance.

  10. [Analysis of triterpenoids in Ganoderma lucidum by microwave-assisted continuous extraction].

    Science.gov (United States)

    Lu, Yan-fang; An, Jing; Jiang, Ye

    2015-04-01

    For further improving the extraction efficiency of microwave extraction, a microwave-assisted contijuous extraction (MACE) device has been designed and utilized. By contrasting with the traditional methods, the characteristics and extraction efficiency of MACE has also been studied. The method was validated by the analysis of the triterpenoids in Ganoderma lucidum. The extraction conditions of MACE were: using 95% ethanol as solvent, microwave power 200 W and radiation time 14.5 min (5 cycles). The extraction results were subsequently compared with traditional heat reflux extraction ( HRE) , soxhlet extraction (SE), ultrasonic extraction ( UE) as well as the conventional microwave extraction (ME). For triterpenoids, the two methods based on the microwaves (ME and MACE) were in general capable of finishing the extraction in 10, 14.5 min, respectively, while other methods should consume 60 min and even more than 100 min. Additionally, ME can produce comparable extraction results as the classical HRE and higher extraction yield than both SE and UE, however, notably lower extraction yield than MASE. More importantly, the purity of the crud extract by MACE is far better than the other methods. MACE can effectively combine the advantages of microwave extraction and soxhlet extraction, thus enabling a more complete extraction of the analytes of TCMs in comparison with ME. And therefore makes the analytic result more accurate. It provides a novel, high efficient, rapid and reliable pretreatment technique for the analysis of TCMs, and it could potentially be extended to ingredient preparation or extracting techniques of TCMs.

  11. Determination of fission products and actinides by inductively coupled plasma-mass spectrometry using isotope dilution analysis. A study of random and systematic errors

    International Nuclear Information System (INIS)

    Ignacio Garcia Alonso, Jose

    1995-01-01

    The theory of the propagation of errors (random and systematic) for isotope dilution analysis (IDA) has been applied to the analysis of fission products and actinide elements by inductively coupled plasma-mass spectrometry (ICP-MS). Systematic errors in ID-ICP-MS arising from mass-discrimination (mass bias), detector non-linearity and isobaric interferences in the measured isotopes have to be corrected for in order to achieve accurate results. The mass bias factor and the detector dead-time can be determined by using natural elements with well-defined isotope abundances. A combined method for the simultaneous determination of both factors is proposed. On the other hand, isobaric interferences for some fission products and actinides cannot be eliminated using mathematical corrections (due to the unknown isotope abundances in the sample) and a chemical separation is necessary. The theory for random error propagation in IDA has been applied to the determination of non-natural elements by ICP-MS taking into account all possible sources of uncertainty with pulse counting detection. For the analysis of fission products, the selection of the right spike isotope composition and spike to sample ratio can be performed by applying conventional random propagation theory. However, it has been observed that, in the experimental determination of the isotope abundances of the fission product elements to be determined, the correction for mass-discrimination and the correction for detector dead-time losses contribute to the total random uncertainty. For the instrument used in the experimental part of this study, it was found that the random uncertainty on the measured isotope ratios followed Poisson statistics for low counting rates whereas, for high counting rates, source instability was the main source of error

  12. Liquid paraffin as new dilution medium for the analysis of high boiling point residual solvents with static headspace-gas chromatography.

    Science.gov (United States)

    D'Autry, Ward; Zheng, Chao; Bugalama, John; Wolfs, Kris; Hoogmartens, Jos; Adams, Erwin; Wang, Bochu; Van Schepdael, Ann

    2011-07-15

    Residual solvents are volatile organic compounds which can be present in pharmaceutical substances. A generic static headspace-gas chromatography analysis method for the identification and control of residual solvents is described in the European Pharmacopoeia. Although this method is proved to be suitable for the majority of samples and residual solvents, the method may lack sensitivity for high boiling point residual solvents such as N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide and benzyl alcohol. In this study, liquid paraffin was investigated as new dilution medium for the analysis of these residual solvents. The headspace-gas chromatography method was developed and optimized taking the official Pharmacopoeia method as a starting point. The optimized method was validated according to ICH criteria. It was found that the detection limits were below 1μg/vial for each compound, indicating a drastically increased sensitivity compared to the Pharmacopoeia method, which failed to detect the compounds at their respective limit concentrations. Linearity was evaluated based on the R(2) values, which were above 0.997 for all compounds, and inspection of residual plots. Instrument and method precision were examined by calculating the relative standard deviations (RSD) of repeated analyses within the linearity and accuracy experiments, respectively. It was found that all RSD values were below 10%. Accuracy was checked by a recovery experiment at three different levels. Mean recovery values were all in the range 95-105%. Finally, the optimized method was applied to residual DMSO analysis in four different Kollicoat(®) sample batches. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Reverse isotope dilution method for determining benzene and metabolites in tissues

    International Nuclear Information System (INIS)

    Bechtold, W.E.; Sabourin, P.J.; Henderson, R.F.

    1988-01-01

    A method utilizing reverse isotope dilution for the analysis of benzene and its organic soluble metabolites in tissues of rats and mice is presented. Tissues from rats and mice that had been exposed to radiolabeled benzene were extracted with ethyl acetate containing known, excess quantities of unlabeled benzene and metabolites. Butylated hydroxytoluene was added as an antioxidant. The ethyl acetate extracts were analyzed with semipreparative reversed-phase HPLC. Isolated peaks were collected and analyzed for radioactivity (by liquid scintillation spectrometry) and for mass (by UV absorption). The total amount of each compound present was calculated from the mass dilution of the radiolabeled isotope. This method has the advantages of high sensitivity, because of the high specific activity of benzene, and relative stability of the analyses, because of the addition of large amounts of unlabeled carrier analogue

  14. A Comparative Analysis of Extract, Transformation and Loading (ETL) Process

    Science.gov (United States)

    Runtuwene, J. P. A.; Tangkawarow, I. R. H. T.; Manoppo, C. T. M.; Salaki, R. J.

    2018-02-01

    The current growth of data and information occurs rapidly in varying amount and media. These types of development will eventually produce large number of data better known as the Big Data. Business Intelligence (BI) utilizes large number of data and information for analysis so that one can obtain important information. This type of information can be used to support decision-making process. In practice a process integrating existing data and information into data warehouse is needed. This data integration process is known as Extract, Transformation and Loading (ETL). In practice, many applications have been developed to carry out the ETL process, but selection which applications are more time, cost and power effective and efficient may become a challenge. Therefore, the objective of the study was to provide comparative analysis through comparison between the ETL process using Microsoft SQL Server Integration Service (SSIS) and one using Pentaho Data Integration (PDI).

  15. Influence of extragent dilution upon light rare earths separation

    International Nuclear Information System (INIS)

    Korpusova, R.D.; Smirnova, N.N.

    1978-01-01

    The effect of diluting the extragent on separation of REE in the presence of 6 g-equiv. of LiNO 3 has been studied. For experiments use was made of TBP diluted with kerosene or butylbenzene (40,50,70 vol.%). The separation coefficients have been determined under conditions of saturation. The content of trace amounts of the components has been determined by the weight method; the content of macroimpurities - by the radiometric method. It has been established that the coefficient of Ce-La, Pr-La separation is not affected by the dilution of the extragent. The only exception is the Pr 142 -La pair; in the presence of trace amounts of better extracted element and two-fold dilution the separation coefficient increases almost by 150%. For the Pr-Ce pair the effect of dilution is better noticeable in that case when more extracted element is present in trace amounts. However, a comparison of the effect of dilution on separation coefficients of all REE pairs under study has shown that this effect is the strongest for the samarium-neodymium pair. The data obtained allow an assumption to be made that kerosene, as a diluent, affects the steric factor and coordination. Therefore, upon dilution the coefficient of the samarium-neodymium pair separation is affected most of all

  16. Analysis of 99Tc in the radioactive liquid waste after extraction into suitable solvent

    International Nuclear Information System (INIS)

    Sonar, N.L.; Vaishali De; Pardeshi, V.; Raghvendra, Y.; Valsala, T.P.; Sonavane, M.S.; Kulkarni, Y.; Raj Kanwar

    2012-01-01

    99 Tc is one of the long lived fission product with high fission yield. >From radioactive waste management point of view it is very much essential to evaluate the concentration of technetium in the radioactive liquid waste in order to finalise the treatment process to extract/isolate it from the stream which is discharged to the environment. For the estimation of 99 Tc in the radioactive liquid waste stream, extraction of the stable complex of technetium-tetraphenyl arsonium chloride (TPAC) into chloroform followed by beta counting was studied. Various parameters like pH, time of equilibration, concentration of TPAC in chloroform, use of other solvent for extraction as well as interference of various other radionuclides present in the waste were also studied. The radioactive liquid waste being handled in plant contains high concentrations of salts in the form of sodium nitrate. Hence effect of salt concentration on the percentage extraction was also evaluated. The extraction behavior does not dependent on change in the pH of the solution. Almost 99.5% extraction was observed in the pH range of 1-13.0. High concentration of salt is affecting the extraction. However, this can be taken care by diluting the radioactive waste. It takes almost 90 min time for maximum extraction. Presence of radionuclides like 137 Cs, 90 Sr are not interfering the extraction of 99 Tc. However, 106 Ru is getting slightly extracted along with 99 Tc. The error due to 106 Ru can be eliminated by taking gamma spectrum and deducting the activity from the total beta activity to get 99 Tc activity. Nitrobenzene can be used for extraction of Tc-TPAC complex in place of chloroform. (author)

  17. Extracting Credible Dependencies for Averaged One-Dependence Estimator Analysis

    Directory of Open Access Journals (Sweden)

    LiMin Wang

    2014-01-01

    Full Text Available Of the numerous proposals to improve the accuracy of naive Bayes (NB by weakening the conditional independence assumption, averaged one-dependence estimator (AODE demonstrates remarkable zero-one loss performance. However, indiscriminate superparent attributes will bring both considerable computational cost and negative effect on classification accuracy. In this paper, to extract the most credible dependencies we present a new type of seminaive Bayesian operation, which selects superparent attributes by building maximum weighted spanning tree and removes highly correlated children attributes by functional dependency and canonical cover analysis. Our extensive experimental comparison on UCI data sets shows that this operation efficiently identifies possible superparent attributes at training time and eliminates redundant children attributes at classification time.

  18. THERMODYNAMIC TOPOLOGICAL ANALYSIS OF EXTRACTIVE DISTILLATION OF MAXIMUM BOILING AZEOTROPES

    Directory of Open Access Journals (Sweden)

    W. F. Shen

    2015-12-01

    Full Text Available Abstract This paper provides a feasibility study of azeotropic mixture separation based on a topological analysis combining thermodynamic knowledge of residue curve maps, univolatility and unidistribution curves, and extractive profiles. Thermodynamic topological features related to process operations for typical ternary diagram classes 1.0-2 are, for the first time, discussed. Separating acetone/chloroform is presented as an illustrative example; different entrainers are investigated: several heavy ones, a light one, and water, covering the Serafimov classes 1.0-2, 1.0-1a and 3.1-4, respectively. The general feasibility criterion that was previously established for ternary mixtures including only one azeotrope (1.0-1a or 1.0-2 is now, for the first time, extended to that including three azeotropes (class 3.1–4.

  19. A double isotope dilution method for assaying of polycyclic aromatic hydrocarbons in cigarette smoke condensate

    International Nuclear Information System (INIS)

    Bechtold, W.E.; Chen, B.T.

    1988-01-01

    This report describes a double isotope dilution method for analysis of the polycyclic aromatic hydrocarbons (PAH) phenanthrene, fluor-anthene, pyrene, and benzo[a]pyrene in cigarette smoke particulates. The first isotope dilution used deuterated analogues of the first three PAH as internal standards. The second isotope dilution, for benzo[a]pyrene, used the tritiated analogue as an internal standard. The PAH were isolated from extracts of cigarette smoke particulates using a two-step procedure based on selective extraction from aqueous dimethyl sulfoxide (DMSO) followed by chromatography on silica gel extraction columns. After isolation, aliquots of the samples were analyzed for phenanthrene, pyrene, and fluoranthene by gas chromatography with mass spectrometric detection (GC/MS). Separate aliquots of the samples were analyzed for benzo[a]pyrene by high pressure liquid chromatography with fluorescence detection followed by liquid scintillation spectrometry. PAH levels from cigarette smoke condensates collected from different exposure modes were compared; no exposure-related differences were found. (author)

  20. Extraction and identification of flavonoids from parsley extracts by HPLC analysis

    Science.gov (United States)

    Stan, M.; Soran, M. L.; Varodi, C.; Lung, I.

    2012-02-01

    Flavonoids are phenolic compounds isolated from a wide variety of plants, and are valuable for their multiple properties, including antioxidant and antimicrobial activities. In the present work, parsley (Petroselinum crispum L.) extracts were obtained by three different extraction techniques: maceration, ultrasonic-assisted and microwave-assisted solvent extractions. The extractions were performed with ethanol-water mixtures in various ratios. From these extracts, flavonoids like the flavones apigenin and luteolin, and the flavonols quercetin and kaempferol were identified using an HPLC Shimadzu apparatus equipped with PDA and MS detectors. The separation method involved a gradient step. The mobile phase consisted of two solvents: acetonitrile and distilled water with 0.1% formic acid. The separation was performed on a RP-C18 column.

  1. Quantitation of Rotundone in Grapefruit (Citrus paradisi) Peel and Juice by Stable Isotope Dilution Assay.

    Science.gov (United States)

    Nakanishi, Akira; Fukushima, Yusuke; Miyazawa, Norio; Yoshikawa, Keisuke; Maeda, Tomoko; Kurobayashi, Yoshiko

    2017-06-21

    Aroma extract dilution analyses of the aromas of peels and juices of white and pink grapefruits revealed that rotundone, responsible for peppery, spicy, and woody odors, was detected for the first time at high flavor dilution factors of 256-1024. In both juices, rotundone was detected at the highest flavor dilution factor of 1024. Rotundone in grapefruits was quantitated by a stable isotope dilution assay with a newly synthesized deuterium-labeled internal standard, rotundone-d 2,3 : its levels were 2180 and 1920 ng/kg in white and pink grapefruit peels and 29.6 and 49.8 ng/kg in white and pink grapefruit juices, respectively. On the basis of these results, sensory analysis was performed to assess the effects of rotundone on a white grapefruit juice aroma reconstitute. This sensory analysis revealed that rotundone does not impart a woody odor or affect any of the existing attributes, but increases various attributes, thus confirming that rotundone is indispensable for the aroma of grapefruit juice.

  2. Determination of urea kinetics by isotope dilution with [C-13]urea and gas chromatography isotope ratio mass spectrometry (GC-IRMS) analysis

    NARCIS (Netherlands)

    Kloppenburg, Wybe; Wolthers, BG; Stellaard, F; Elzinga, H; Tepper, T; deJong, PE; Huisman, RM

    1. Stable urea isotopes can be used to study urea kinetics in humans, The use of stable urea isotopes far studying urea kinetic parameters in humans on a large scale is hampered by the high costs of the labelled material, We devised a urea dilution for measurement of the distribution volume,

  3. Extracting neuronal functional network dynamics via adaptive Granger causality analysis.

    Science.gov (United States)

    Sheikhattar, Alireza; Miran, Sina; Liu, Ji; Fritz, Jonathan B; Shamma, Shihab A; Kanold, Patrick O; Babadi, Behtash

    2018-04-24

    Quantifying the functional relations between the nodes in a network based on local observations is a key challenge in studying complex systems. Most existing time series analysis techniques for this purpose provide static estimates of the network properties, pertain to stationary Gaussian data, or do not take into account the ubiquitous sparsity in the underlying functional networks. When applied to spike recordings from neuronal ensembles undergoing rapid task-dependent dynamics, they thus hinder a precise statistical characterization of the dynamic neuronal functional networks underlying adaptive behavior. We develop a dynamic estimation and inference paradigm for extracting functional neuronal network dynamics in the sense of Granger, by integrating techniques from adaptive filtering, compressed sensing, point process theory, and high-dimensional statistics. We demonstrate the utility of our proposed paradigm through theoretical analysis, algorithm development, and application to synthetic and real data. Application of our techniques to two-photon Ca 2+ imaging experiments from the mouse auditory cortex reveals unique features of the functional neuronal network structures underlying spontaneous activity at unprecedented spatiotemporal resolution. Our analysis of simultaneous recordings from the ferret auditory and prefrontal cortical areas suggests evidence for the role of rapid top-down and bottom-up functional dynamics across these areas involved in robust attentive behavior.

  4. Instrument for Solvent Extraction and Analysis (ISEE) of Organics from Regolith Simulant Using Supercritical Fluid Extraction and Chromatography

    Science.gov (United States)

    Franco, Carolina; Hintze, Paul E.

    2017-01-01

    ISEE is an instrument with the potential to perform extractions from regolith found on the surface of asteroids and planets, followed by characterization and quantitation of the extracts using supercritical fluid extraction (SFE) and chromatography (SFC). SFE is a developed technique proven to extract a wide range of organic compounds. SFC is similar to High Performance Liquid Chromatography (HPLC) but has the advantage of performing chiral separations without needing to derivatize the chiral compounds. CO2 will be the solvent for both stages as it is readily available in the Mars atmosphere. ISEE will capture CO2 from the environment, and use it for SFE and SFC. If successful, this would allow ISEE to perform analysis of organic compounds without using consumables. This paper will present results on a preliminary, proof-of-principle effort to use SFE and SFC to extract and analyze lunar regolith simulant spiked with organic compounds representing a range of organics that ISEE would expect to characterize. An optimization of variables for the extraction of the organics from the spiked regolith was successfully developed, using 138 bar pressure and 40 C temperature. The extraction flow rate was optimized at 2% SLPM with 30% methanol modifier. The extractions were successful with a value of 77.3+/- 0.9% of organics extracted. However, the recovery of organics after the extraction was very low with only 48.5+/-14.2%. Moreover, three columns were selected to analyze multiple samples at a time; two of them are Viridis HSS C18 SB and Torus DIOL, and the third column, specific for chiral separations, has not yet been selected yet.

  5. Big data extraction with adaptive wavelet analysis (Presentation Video)

    Science.gov (United States)

    Qu, Hongya; Chen, Genda; Ni, Yiqing

    2015-04-01

    Nondestructive evaluation and sensing technology have been increasingly applied to characterize material properties and detect local damage in structures. More often than not, they generate images or data strings that are difficult to see any physical features without novel data extraction techniques. In the literature, popular data analysis techniques include Short-time Fourier Transform, Wavelet Transform, and Hilbert Transform for time efficiency and adaptive recognition. In this study, a new data analysis technique is proposed and developed by introducing an adaptive central frequency of the continuous Morlet wavelet transform so that both high frequency and time resolution can be maintained in a time-frequency window of interest. The new analysis technique is referred to as Adaptive Wavelet Analysis (AWA). This paper will be organized in several sections. In the first section, finite time-frequency resolution limitations in the traditional wavelet transform are introduced. Such limitations would greatly distort the transformed signals with a significant frequency variation with time. In the second section, Short Time Wavelet Transform (STWT), similar to Short Time Fourier Transform (STFT), is defined and developed to overcome such shortcoming of the traditional wavelet transform. In the third section, by utilizing the STWT and a time-variant central frequency of the Morlet wavelet, AWA can adapt the time-frequency resolution requirement to the signal variation over time. Finally, the advantage of the proposed AWA is demonstrated in Section 4 with a ground penetrating radar (GPR) image from a bridge deck, an analytical chirp signal with a large range sinusoidal frequency change over time, the train-induced acceleration responses of the Tsing-Ma Suspension Bridge in Hong Kong, China. The performance of the proposed AWA will be compared with the STFT and traditional wavelet transform.

  6. Phosphogypsum analysis: total content and extractable element concentrations

    International Nuclear Information System (INIS)

    Gennari, Roseli F.; Medina, Nilberto H.; Garcia, Isabella; Silveira, Marcilei A.G.

    2011-01-01

    Phosphogypsum stand for the chemical origin gypsum generated in fertilizers production, in which phosphate rock is attacked by sulfuric acid resulting in phosphoric acid (H 3 PO 4 ) and phosphate fertilizers. Phosphogypsum is not a commercial product and it is stocked in large open areas or accumulated in lakes inducing to a major environmental problem due to the presence of toxic and radioactive elements. The increasing world agricultural demand is the real responsible for the severity of this environmental problem. Nevertheless, there are some possibilities for the application of this reject material, such as civil construction, waste water treatment, and in cultivated lands, etc. In the agriculture the phosphogypsum is commonly used as a nutrient source due to its large amounts of phosphorus, calcium and sulfur. However, there are still some environmental questions related to the use of this by-product since phosphogypsum is classified as TENORM (Technologically Enhanced Naturally Occurring Radioactive Material), which is a solid waste containing heavy metals and naturally occurring radioactive elements from the rock matrix. In this work, Plasma Mass Spectrometry (ICP-MS) was used to study phosphogypsum samples. Several acid solutions for samples digestion were evaluated in order to be feasible the chemical analysis. BCR sequential extractions were also performed. The results showed analyte concentrations are highly dependent on the acid solution used. The BCR guidelines could not be applied as used for soil, since the phosphogypsum solubility is different. So, it would be necessary to use different mass aliquots in the extractions, to be feasible an environmental evaluation. (author)

  7. Strategies for the extraction and analysis of non-extractable polyphenols from plants.

    Science.gov (United States)

    Domínguez-Rodríguez, Gloria; Marina, María Luisa; Plaza, Merichel

    2017-09-08

    The majority of studies based on phenolic compounds from plants are focused on the extractable fraction derived from an aqueous or aqueous-organic extraction. However, an important fraction of polyphenols is ignored due to the fact that they remain retained in the residue of extraction. They are the so-called non-extractable polyphenols (NEPs) which are high molecular weight polymeric polyphenols or individual low molecular weight phenolics associated to macromolecules. The scarce information available about NEPs shows that these compounds possess interesting biological activities. That is why the interest about the study of these compounds has been increasing in the last years. Furthermore, the extraction and characterization of NEPs are considered a challenge because the developed analytical methodologies present some limitations. Thus, the present literature review summarizes current knowledge of NEPs and the different methodologies for the extraction of these compounds, with a particular focus on hydrolysis treatments. Besides, this review provides information on the most recent developments in the purification, separation, identification and quantification of NEPs from plants. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Comparative chemical and biochemical analysis of extracts of Hibiscus sabdariffa.

    Science.gov (United States)

    Sindi, Heba A; Marshall, Lisa J; Morgan, Michael R A

    2014-12-01

    Hibiscus sabdariffa extracts have attracted attention because of potentially useful bioactivity. However, there have been no systematic studies of extraction efficiencies of H. sabdariffa. The nature of extracts used in different studies has varied considerably, making comparisons difficult. Therefore, a systematic study of extracts of H. sabdariffa made with different solvents was carried out using water, methanol, ethyl acetate and hexane in the presence/absence of formic acid, using different extraction times and temperatures. The extracts were analysed for total polyphenol content, antioxidant capacity using DPPH, FRAP and TEAC assays, and specific anthocyanins were determined using HPLC and LC-MS. The results showed the highest antioxidant capacities were obtained by extracting using water, with or without formic acid, for 10 min at 100°C. These extracts provided the highest concentrations of cyanidin 3-sambubioside and delphinidin 3-sambubioside. It will be important to use extraction conditions giving optimal extraction efficiencies for subsequent bioactivity experiments. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants.

    Science.gov (United States)

    Heub, Sarah; Tscharner, Noe; Kehl, Florian; Dittrich, Petra S; Follonier, Stéphane; Barbe, Laurent

    2016-01-01

    A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17β-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 µl of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

  10. Preliminary thermal analysis of grids for twin source extraction system

    International Nuclear Information System (INIS)

    Pandey, Ravi; Bandyopadhyay, Mainak; Chakraborty, Arun K.

    2017-01-01

    The TWIN (Two driver based Indigenously built Negative ion source) source provides a bridge between the operational single driver based negative ion source test facility, ROBIN in IPR and an ITER-type multi driver based ion source. The source is designed to be operated in CW mode with 180kW, 1MHz, 5s ON/600s OFF duty cycle and also in 5Hz modulation mode with 3s ON/20s OFF duty cycle for 3 such cycle. TWIN source comprises of ion source sub-assembly (consist of driver and plasma box) and extraction system sub-assembly. Extraction system consists of Plasma grid (PG), extraction grid (EG) and Ground grid (GG) sub assembly. Negative ion beams produced at plasma grid seeing the plasma side of ion source will receive moderate heat flux whereas the extraction grid and ground grid would be receiving majority of heat flux from extracted negative ion and co-extracted electron beams. Entire Co-extracted electron beam would be dumped at extraction grid via electron deflection magnetic field making the requirement of thermal and hydraulic design for extraction grid to be critical. All the three grids are made of OFHC Copper and would be actively water cooled keeping the peak temperature rise of grid surface within allowable limit with optimum uniformity. All the grids are to be made by vacuum brazing process where joint strength becomes crucial at elevated temperature. Hydraulic design must maintain the peak temperature at the brazing joint within acceptable limit

  11. Exploring the Potential for Using Inexpensive Natural Reagents Extracted from Plants to Teach Chemical Analysis

    Science.gov (United States)

    Hartwell, Supaporn Kradtap

    2012-01-01

    A number of scientific articles report on the use of natural extracts from plants as chemical reagents, where the main objective is to present the scientific applications of those natural plant extracts. The author suggests that natural reagents extracted from plants can be used as alternative low cost tools in teaching chemical analysis,…

  12. Bayesian analysis of systems with random chemical composition: renormalization-group approach to Dirichlet distributions and the statistical theory of dilution.

    Science.gov (United States)

    Vlad, Marcel Ovidiu; Tsuchiya, Masa; Oefner, Peter; Ross, John

    2002-01-01

    We investigate the statistical properties of systems with random chemical composition and try to obtain a theoretical derivation of the self-similar Dirichlet distribution, which is used empirically in molecular biology, environmental chemistry, and geochemistry. We consider a system made up of many chemical species and assume that the statistical distribution of the abundance of each chemical species in the system is the result of a succession of a variable number of random dilution events, which can be described by using the renormalization-group theory. A Bayesian approach is used for evaluating the probability density of the chemical composition of the system in terms of the probability densities of the abundances of the different chemical species. We show that for large cascades of dilution events, the probability density of the composition vector of the system is given by a self-similar probability density of the Dirichlet type. We also give an alternative formal derivation for the Dirichlet law based on the maximum entropy approach, by assuming that the average values of the chemical potentials of different species, expressed in terms of molar fractions, are constant. Although the maximum entropy approach leads formally to the Dirichlet distribution, it does not clarify the physical origin of the Dirichlet statistics and has serious limitations. The random theory of dilution provides a physical picture for the emergence of Dirichlet statistics and makes it possible to investigate its validity range. We discuss the implications of our theory in molecular biology, geochemistry, and environmental science.

  13. Comparative analysis of protocols for DNA extraction from soybean caterpillars.

    Science.gov (United States)

    Palma, J; Valmorbida, I; da Costa, I F D; Guedes, J V C

    2016-04-07

    Genomic DNA extraction is crucial for molecular research, including diagnostic and genome characterization of different organisms. The aim of this study was to comparatively analyze protocols of DNA extraction based on cell lysis by sarcosyl, cetyltrimethylammonium bromide, and sodium dodecyl sulfate, and to determine the most efficient method applicable to soybean caterpillars. DNA was extracted from specimens of Chrysodeixis includens and Spodoptera eridania using the aforementioned three methods. DNA quantification was performed using spectrophotometry and high molecular weight DNA ladders. The purity of the extracted DNA was determined by calculating the A260/A280 ratio. Cost and time for each DNA extraction method were estimated and analyzed statistically. The amount of DNA extracted by these three methods was sufficient for PCR amplification. The sarcosyl method yielded DNA of higher purity, because it generated a clearer pellet without viscosity, and yielded high quality amplification products of the COI gene I. The sarcosyl method showed lower cost per extraction and did not differ from the other methods with respect to preparation times. Cell lysis by sarcosyl represents the best method for DNA extraction in terms of yield, quality, and cost effectiveness.

  14. Extraction and analysis of Jatropha curcas L. seed oil | Shivani ...

    African Journals Online (AJOL)

    In this study, extraction of Jatropha oil from seeds was optimized using organic solvents. The effects of parameters on the oil extraction namely type of organic solvents and different techniques were also investigated to optimize the processing conditions for achieving maximum oil yield. The acid value and antioxidant ...

  15. Liquid-liquid extraction in flow analysis: A critical review

    Energy Technology Data Exchange (ETDEWEB)

    Silvestre, Cristina I.C.; Santos, Joao L.M. [REQUIMTE, Servico de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, R. Anibal Cunha, 164, 4099-030 Porto (Portugal); Lima, Jose L.F.C., E-mail: limajlfc@ff.up.pt [REQUIMTE, Servico de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, R. Anibal Cunha, 164, 4099-030 Porto (Portugal); Zagatto, Elias A.G. [Centro de Energia Nuclear na Agricultura, Universidade de Sao Paulo, P.O. Box 96, Piracicaba 13400-970 (Brazil)

    2009-10-12

    Liquid-liquid extractions (LLE) are a common sample pre-treatment in many analytical applications. This review aims at providing a critical overview of the distinct automated continuous flow-based approaches that were developed for liquid-liquid extraction with the purpose of pre-concentration and/or separation of multiple analytes, such as ultra-trace metal and metalloid species, phenolic compounds, surfactants, pharmaceuticals, etc., hyphenated with many detection technique such as UV/vis spectrophotometry, atomic spectrometric detection systems and luminescent detectors, including distinct extraction strategies and applications like single and multiple extraction schemes, wetting film extraction, supported liquid membrane extraction, back extraction, closed-loop systems and the utilisation of zone sampling, chromatomembranes and iterative reversal techniques. The analytical performance of the developed flow-based LLE methods and the influence of flow manifold components such as the segmenter, extraction coil and phase separator, is emphasised and object of discussion. An overall presentation of each system components, selectivity, advantages and shortcomings is carried out and exemplified with selected applications.

  16. GC-MS Analysis, Antimicrobial and Antioxidant Activities of Extracts ...

    African Journals Online (AJOL)

    ogundare adebola

    dried and crushed into smaller pieces using mortar and pestle. The plant was weighed and extracted using serial exhaustive extraction method by moving from a non-polar (hexane) solvent to a medium polar solvent (ethyl acetate) and then to a polar solvent. (methanol). Phytochemical screening: Preliminary phytochemical.

  17. Extraction of trapped gases in ice cores for isotope analysis

    International Nuclear Information System (INIS)

    Leuenberger, M.; Bourg, C.; Francey, R.; Wahlen, M.

    2002-01-01

    The use of ice cores for paleoclimatic investigations is discussed in terms of their application for dating, temperature indication, spatial time marker synchronization, trace gas fluxes, solar variability indication and changes in the Dole effect. The different existing techniques for the extraction of gases from ice cores are discussed. These techniques, all to be carried out under vacuum, are melt-extraction, dry-extraction methods and the sublimation technique. Advantages and disadvantages of the individual methods are listed. An extensive list of references is provided for further detailed information. (author)

  18. The decision to extract: part II. Analysis of clinicians' stated reasons for extraction.

    Science.gov (United States)

    Baumrind, S; Korn, E L; Boyd, R L; Maxwell, R

    1996-04-01

    In a recently reported study, the pretreatment records of each subject in a randomized clinical trial of 148 patients with Class I and Class II malocclusions presenting for orthodontic treatment were evaluated independently by five experienced clinicians (drawn from a panel of 14). The clinicians displayed a higher incidence of agreement with each other than had been expected with respect to the decision as to whether extraction was indicated in each specific case. To improve our understanding of how clinicians made their decisions on whether to extract or not, the records of a subset of 72 subjects randomly selected from the full sample of 148, have now been examined in greater detail. In 21 of these cases, all five clinicians decided to treat without extraction. Among the remaining 51 cases, there were 202 decisions to extract (31 unanimous decision cases and 20 split decision cases). The clinicians cited a total of 469 reasons to support these decisions. Crowding was cited as the first reason in 49% of decisions to extract, followed by incisor protrusion (14%), need for profile correction (8%), Class II severity (5%), and achievement of a stable result (5%). When all the reasons for extraction in each clinician's decision were considered as a group, crowding was cited in 73% of decisions, incisor protrusion in 35%, need for profile correction in 27%, Class II severity in 15% and posttreatment stability in 9%. Tooth size anomalies, midline deviations, reduced growth potential, severity of overjet, maintenance of existing profile, desire to close the bite, periodontal problems, and anticipation of poor cooperation accounted collectively for 12% of the first reasons and were mentioned in 54% of the decisions, implying that these considerations play a consequential, if secondary, role in the decision-making process. All other reasons taken together were mentioned in fewer than 20% of cases. In this sample at least, clinicians focused heavily on appearance

  19. Landslide stability analysis on basis of LIDAR data extraction

    Science.gov (United States)

    Hu, Hui; Fernandez-Steeger, Tomas M.; Dong, Mei; Azzam, Rafig

    2010-05-01

    important role during surface construction for further more precise analysis purpose. 3D geological model can be built based on the connection between surface model and geological data like borehole data in GOCAD. Regarding the bench stability analysis, LEM (Limit Equilibrium Method) analysis using Janbu and FEM (Finite Element Method) have been adopted during this analyzing task. A program was developed to convert GOCAD 2D section data directly into the FEM software. The meshed model is then used for stability analysis. In one quarry, 3 cross sections have been extracted on basis of LIDAR original data (original 3 cross sections). To evaluate the advantages of LIDAR data for slope analysis, the results of safety factor (SF) were compared to simplified slope models as they are used normally. The comparison showed that variations of the SF reach up to 9%. Additionally, conservative evaluation demonstrated by SF results based on simplified model is not adaptive for decision making of filling.

  20. Dynamic determination of kinetic parameters for the interaction between polypeptide hormones and cell-surface receptors in the perfused rat liver by the multiple-indicator dilution method

    International Nuclear Information System (INIS)

    Sato, H.; Sugiyama, Y.; Sawada, Y.; Iga, T.; Sakamoto, S.; Fuwa, T.; Hanano, M.

    1988-01-01

    Hepatic elimination of epidermal growth factor (EGF) via receptor-mediated endocytosis was studied by a multiple-indicator dilution method in the isolated perfused rat liver, in which cell polarity and spatial organization are maintained. In this method EGF was given with inulin, an extracellular reference, as a bolus into the portal vein, and dilution curves of both compounds in the hepatic vein effluent were analyzed. Analysis of the dilution curve for EGF, compared with that for somatostatin, which showed no specific binding to isolated liver plasma membranes, resulted as follows: (i) both extraction ratio and distribution volume of 125 I-labeled EGF decreased as the injected amount of unlabeled EGF increased; (ii) the ratio plot of the dilution curve for EGF exhibited an upward straight line initially for a short period of time, whereas the ratio plot of somatostatin gradually decreased. The multiple-indicator dilution method was used for other peptides also. Insulin and glucagon, known to have hepatocyte receptors, behaved similarly to EGF in shape of their ratio plots. The kinetic parameters calculated by this analysis were comparable with reported values obtained by in vitro direct binding measurements at equilibrium using liver homogenates. They conclude that the multiple-indicator dilution method is a good tool for analyzing the dynamics of peptide hormones-cell-surface receptor interaction under a condition in which spatial architecture of the liver is maintained

  1. Anthocyanin extractability assesment of grape skins by texture analysis

    Directory of Open Access Journals (Sweden)

    Luca Rolle

    2008-09-01

    Significance and impact of study: The possibility of having an easy way to determine maturity index able to estimate the extractability of phenol compounds with sufficient reliability, can be a valuable tool for the enological community.

  2. Extraction and analysis of tea (Camellia sinensis) seed oil from ...

    African Journals Online (AJOL)

    OMONDI-GUYA

    2013-02-20

    Feb 20, 2013 ... spectrophotometer (Model JENWAY6705, multi-cell changer) against a blank ... All the tea seed oil extracts were golden yellow in color and liquid at .... respectively, the two being products of oxidative rancidity. (Chindo et al.

  3. A theory of stable-isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Pickup, J.F.; McPherson, C.K.

    1977-01-01

    In order to perform quantitative analysis using stable isotope dilution with mass spectrometry, an equation is derived which describes the relationship between the relative proportions of natural and labelled material and measured isotope ratios

  4. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shan, E-mail: ls_tuzi@163.com; Wang, Mei, E-mail: wmei02@163.com; Zhong, Yizhou, E-mail: yizhz@21cn.com; Zhang, Zehua, E-mail: kazuki.0101@aliyun.com; Yang, Bingyi, E-mail: e_yby@163.com

    2015-09-01

    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea–ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries. - Highlights: • Cloud point extraction was firstly established to determine trace inorganic arsenic(As) species combining with HGAFS. • Separate As(III) and As(V) determinations improve the accuracy. • Ultrasonic release of complexed As(V) enables complete As(V) reduction to As(III). • Direct HGAFS analysis can be performed.

  5. Analysis of human muscle extracts by proton NMR

    International Nuclear Information System (INIS)

    Venkatasubramanian, P.N.; Barany, M.; Arus, C.

    1986-01-01

    Perchloric acid extracts were prepared from pooled human muscle biopsies from patients diagnosed with scoliosis (SCOL) and cerebral palsy (CP). After neutralization with KOH and removal of perchlorate, the extracts were concentrated by freeze drying and dissolved in 2 H 2 O to contain 120 O.D. units at 280 nm per 0.5 ml. 1 H NMR spectroscopy was performed with the 5 mm probe of a Varian XL300 instrument. Creatine, lactate, carnosine, and choline were the major resonances in the one-dimensional spectra of both extracts. With creatine as reference, 2.5-fold more lactate was found in SCOL than in CP, and a much smaller difference was also found in their carnosine content. Two-dimensional COSY comparison revealed several differences between the two extracts. Taurine, N-acetyl glutamate, glycerophosphoryl choline (or phosphoryl choline) and an unidentified spot were present only in the extract from SCOL but not in that from CP. On the other hand, aspartate, hydroxy-proline, carnitine and glycerophosphoryl ethanolamine were only present in CP but absent in SCOL. Alanine, cysteine, lysine and arginine appeared in both extracts without an apparent intensity difference

  6. Dynamical replica analysis of processes on finitely connected random graphs: II. Dynamics in the Griffiths phase of the diluted Ising ferromagnet

    International Nuclear Information System (INIS)

    Mozeika, A; Coolen, A C C

    2009-01-01

    We study the Glauber dynamics of Ising spin models with random bonds, on finitely connected random graphs. We generalize a recent dynamical replica theory with which to predict the evolution of the joint spin-field distribution, to include random graphs with arbitrary degree distributions. The theory is applied to Ising ferromagnets on randomly diluted Bethe lattices, where we study the evolution of the magnetization and the internal energy. It predicts a prominent slowing down of the flow in the Griffiths phase, it suggests a further dynamical transition at lower temperatures within the Griffiths phase, and it is verified quantitatively by the results of Monte Carlo simulations

  7. Analysis of the variation of the activity of a "9"9"mTc sample after dilution with saline solution

    International Nuclear Information System (INIS)

    Kuahara, L.T.; Correa, E.L.; Potiens, M.P.A.

    2016-01-01

    The activity meter is essential equipment in nuclear medicine services.To ensure its good operation and know the factors which may influence its readings is vital for the activity administered to the patient be correct. Many factors may influence the activity meter accuracy, such as the type of container, geometry, and radioactive material volume. The aim of this study was to analyze the measurements variations in 0.5 ml and 1.0 ml of "9"9"mTc pure and diluted in 2.5 ml of saline solution, in containers used in nuclear medicine. Variations of up to 4 % in measured values were found. (author)

  8. Analysis of solvent extracts from coal liquefaction in a flowing solvent reactor

    Energy Technology Data Exchange (ETDEWEB)

    Li, Wen-Ying; Feng, Jie; Xie, Ke-Chang [Key Laboratory of Coal Science and Technology, Taiyuan University of Technology, Ministry of Education and Shanxi Province, No. 79 Yingze West Street, Taiyuan 030024 (China); Kandiyoti, R. [Department of Chemical Engineering and Chemical Technology, Imperial College, University of London, London SW7 2BY (United Kingdom)

    2004-10-15

    Point of Ayr coal has been extracted using three solvents, tetralin, quinoline and 1-methyl-2-pyrrolidinone (NMP) at two temperatures 350 and 450 C, corresponding approximately to before and after the onset of massive covalent bond scission by pyrolysis. The three solvents differ in solvent power and the ability to donate hydrogen atoms to stabilise free radicals produced by pyrolysis of the coal. The extracts were prepared in a flowing solvent reactor to minimise secondary thermal degradation of the primary extracts. Analysis of the pentane-insoluble fractions of the extracts was achieved by size exclusion chromatography, UV-fluorescence spectroscopy in NMP solvent and probe mass. With increasing extraction temperature, the ratio of the amount having big molecular weight to that having small molecular weight in tetralin extracts was increased; the tetralin extract yield increased from 12.8% to 75.9%; in quinoline, increasing extraction temperature did not have an effect on the molecular weight of products but there was a big increase in extract yield. The extracts in NMP showed the enhanced solvent extraction power at both temperatures, with a shift in the ratio of larger molecules to smaller molecules with increasing extraction temperature and with the highest conversion of Point of Ayr coal among these three solvents at both temperatures. Solvent adducts were detected in the tetralin and quinoline extracts by probe mass spectrometry; solvent products were formed from NMP at both temperatures.

  9. EXAFS of dilute systems: fluorescence detection

    International Nuclear Information System (INIS)

    Hastings, J.B.

    1979-01-01

    Since the first observations of the variation of the absorption coefficient for x-rays above the energy thresholds in the thirties until the early seventies, measurements and analysis of these variations were merely intended for the understanding of the underlying physics. Recently, with the understanding of the information available about the local atomic structure in the neighborhood of the absorbing species and the availability of high intensity synchrotron radiation sources, EXAFS has become a powerful structural tool. In these discussions, the details of the measurements for very dilute species are presented. It is shown that for the more dilute systems the measurement of the emission rather than the direct absorption is a more favorable technique

  10. Extraction of intracellular protein from Glaciozyma antarctica for proteomics analysis

    Science.gov (United States)

    Faizura, S. Nor; Farahayu, K.; Faizal, A. B. Mohd; Asmahani, A. A. S.; Amir, R.; Nazalan, N.; Diba, A. B. Farah; Muhammad, M. Nor; Munir, A. M. Abdul

    2013-11-01

    Two preparation methods of crude extracts of psychrophilic yeast Glaciozyma antarctica were compared in order to obtain a good recovery of intracellular proteins. Extraction with mechanical procedures using sonication was found to be more effective for obtaining good yield compare to alkaline treatment method. The procedure is simple, rapid, and produce better yield. A total of 52 proteins were identified by combining both extraction methods. Most of the proteins identified in this study involves in the metabolic process including glycolysis pathway, pentose phosphate pathway, pyruyate decarboxylation and also urea cyle. Several chaperons were identified including probable cpr1-cyclophilin (peptidylprolyl isomerase), macrolide-binding protein fkbp12 and heat shock proteins which were postulate to accelerate proper protein folding. Characteristic of the fundamental cellular processes inferred from the expressed-proteome highlight the evolutionary and functional complexity existing in this domain of life.

  11. Dilute chemical decontamination program review

    International Nuclear Information System (INIS)

    Anstine, L.D.; Blomgren, J.C.; Pettit, P.J.

    1980-01-01

    The objective of the Dilute Chemical Decontamination Program is to develop and evaluate a process which utilizes reagents in dilute concentrations for the decontamination of BWR primary systems and for the maintenance of dose rates on the out-of-core surfaces at acceptable levels. A discussion is presented of the process concept, solvent development, advantages and disadvantages of reagent systems, and VNC loop tests. Based on the work completed to date it is concluded that (1) rapid decontamination of BWRs using dilute reagents is feasible; (2) reasonable reagent conditions for rapid chemical decontamination are: 0.01M oxalic acid + 0.005M citric acid, pH3.0, 90/degree/C, 0.5 to 1.0 ppm dissolved oxygen; (3) control of dissolved oxygen concentration is important, since high levels suppress the rate of decontamination and low levels allow precipitation of ferrous oxalate. 4 refs

  12. Analysis of the Interactions of Botanical Extract Combinations Against the Viability of Prostate Cancer Cell Lines

    Directory of Open Access Journals (Sweden)

    Lynn S. Adams

    2006-01-01

    Full Text Available Herbal medicines are often combinations of botanical extracts that are assumed to have additive or synergistic effects. The purpose of this investigation was to compare the effect of individual botanical extracts with combinations of extracts on prostate cell viability. We then modeled the interactions between botanical extracts in combination isobolographically. Scutellaria baicalensis, Rabdosia rubescens, Panax-pseudo ginseng, Dendranthema morifolium, Glycyrrhiza uralensis and Serenoa repens were collected, taxonomically identified and extracts prepared. Effects of the extracts on cell viability were quantitated in prostate cell lines using a luminescent ATP cell viability assay. Combinations of two botanical extracts of the four most active extracts were tested in the 22Rv1 cell line and their interactions assessed using isobolographic analysis. Each extract significantly inhibited the proliferation of prostate cell lines in a time- and dose-dependent manner except repens. The most active extracts, baicalensis, D. morifolium, G. uralensis and R. rubescens were tested as two-extract combinations. baicalensis and D. morifolium when combined were additive with a trend toward synergy, whereas D. morifolium and R. rubescens together were additive. The remaining two-extract combinations showed antagonism. The four extracts together were significantly more effective than the two-by-two combinations and the individual extracts alone. Combining the four herbal extracts significantly enhanced their activity in the cell lines tested compared with extracts alone. The less predictable nature of the two-way combinations suggests a need for careful characterization of the effects of each individual herb based on their intended use.

  13. Chromatographic-mass spectrometric analysis of ethanol extract of ...

    African Journals Online (AJOL)

    Purpose: This study analyzes the chemical composition of ethanol root extracts of Maesa perlaria var. formosana by .... obtained over a scanning range of 50 to 550 amu at 2 scans/s. .... 142.53 (2,2,6-Trimethyl-bicyclo[4.1.0]hept-1-yl)-methanol.

  14. Quantitative Analysis of Tenofovir by Titrimetric, Extractive Ion-pair ...

    African Journals Online (AJOL)

    Methods: Tenofovir disoproxil forms a complex of 1:1 molar ratio with fumaric acid that was employed in its aqueous titration with sodium hydroxide. Non-aqueous titration was also employed for its determination. Extractive ion-pair spectrophotometric technique using methyl orange was similarly employed to evaluate ...

  15. Physicochemical Analysis of the Aqueous Extracts of Six Nigerian ...

    African Journals Online (AJOL)

    Purpose: Extracts of Picralima nitida seeds, Detarium microcarpum stem bark, Aframomum melagueta seeds, Terminalia catappa leaves, Acacia nilotica pods, and Morinda lucida stem bark, are under consideration for development into suitable dosage forms for treating diabetes mellitus, sickle cell anemia and malaria.

  16. IN SITU SOLID-PHASE EXTRACTION AND ANALYSIS OF ...

    Science.gov (United States)

    Fragrance materials, such as synthetic musks in aqueous samples, are normally analyzed by GC/MS in the selected ion monitoring (SIM) mode to provide maximum sensitivity after liquid-liquid extraction of 1-L samples. A 1-L sample, however, usually provides too little analyte for full-scan data acquisition.We have developed an on-site extraction method for extracting synthetic musks from 60 L of wastewater effluent. Such a large sample volume permits high-quality, full-scan mass spectra to be obtained for various synthetic musk compounds. Quantification of these compounds was conveniently achieved from the full-scan data directly, without preparing SIM descriptors for each compound to acquire SIM data. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-s

  17. Extraction and analysis of Jatropha curcas L. seed oil

    African Journals Online (AJOL)

    use

    2011-12-12

    Dec 12, 2011 ... a mechanical method and defatted in a soxhlet apparatus. The extraction was carried out by using three different solvents such as hexane, isopropanol and petroleum ether. The process continued for 6 h. Solvent was removed by vacuum evaporation and exposure to heat in a drying oven at 50°C. The ...

  18. Analysis of vapor extraction data from applications in Europe

    International Nuclear Information System (INIS)

    Hiller, D.; Gudemann, H.

    1989-01-01

    This paper discusses vapor extraction, an in-situ process to remove volatile organic compounds (VOC) from soils of the vadose zone, applied in Europe since the early 1980s. In a vapor extraction well a negative differential pressure is created by a blower or similar device. The differential pressure generates a steady flow of soil gas towards the extraction well and thus provides a flushing of the soil with air undersaturated in respect to the contaminant concentration. Contaminants will evaporate into the gaseous phase both form the liquid phase and form the soil. Differential pressures applied range from 15 inches - 350 inches of water. The contaminated discharge air can be treated by activated carbon or other suitable methods. The effective radius of vapor extraction systems (VES) ranges typically form 20 feet to 150 feet underneath non-sealed - and up to 300 feet underneath sealed surfaces. Contamination from volatile organic compounds (VOC) have turned out to be widespread due to their almost ubiquitous presence in industrial processes. Specifically, VOC include halogenated hydrocarbons like TCE, PCE or TCA, aromatic hydrocarbons like benzene, toluene, xylene and volatile fuels like gasoline

  19. Comparative analysis of extracted heights from topographic maps ...

    African Journals Online (AJOL)

    Topographic maps represent the three-dimensional landscape by providing relief information in the form of contours in addition to plan information on which natural and man-made landmarks are quite accurately represented. Height information, extractible from topographic maps, comes in handy for most land use planning.

  20. Phytochemical Analysis And Antioxidant Activity of Ethanolic Extract

    African Journals Online (AJOL)

    Aluko B. T.

    MATERIALS AND METHOD. Collection and identification of .... ition o f h yd rogen p eroxid e rad ical. Concentraion µg / ml. EXTRACT. BHT. 0. 0.2. 0.4. 0.6. 0.8. 1. 0 .... activity of commercial soft and hard wheat (Triticum aestivum L.) as affected ...

  1. Process optimization and analysis of microwave assisted extraction of pectin from dragon fruit peel.

    Science.gov (United States)

    Thirugnanasambandham, K; Sivakumar, V; Prakash Maran, J

    2014-11-04

    Microwave assisted extraction (MAE) technique was employed for the extraction of pectin from dragon fruit peel. The extracting parameters were optimized by using four-variable-three-level Box-Behnken design (BBD) coupled with response surface methodology (RSM). RSM analysis indicated good correspondence between experimental and predicted values. 3D response surface plots were used to study the interactive effects of process variables on extraction of pectin. The optimum extraction conditions for the maximum yield of pectin were power of 400 W, temperature of 45 °C, extracting time of 20 min and solid-liquid ratio of 24 g/mL. Under these conditions, 7.5% of pectin was extracted. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Analysis of phosphate esters in plant material. Extraction and purification.

    Science.gov (United States)

    Isherwood, F A; Barrett, F C

    1967-09-01

    1. A critical study was made of the quantitative extraction of nucleotide and sugar phosphates from plant tissue by either boiling aqueous ethanol or cold trichloroacetic acid. The effect of the extraction technique on the inactivation of the enzymes in the plant tissue and the possibility of adsorption of the phosphate esters on the cell wall were especially considered. 2. In the recommended method the plant tissue was frozen in liquid nitrogen, ground to a powder and then blended with cold aqueous trichloroacetic acid containing 8-hydroxyquinoline to prevent adsorption. 3. The extract contained large amounts of trichloroacetic acid, cations, chloride, sugars, amino acids, hydroxy organic acids, phytic acid, orthophosphoric acid and high-molecular-weight material including some phosphorus-containing compounds. All of these were removed as they were liable to interfere with the chromatographic or enzymic assay of the individual nucleotide or sugar phosphates. 4. The procedure was as follows: the last traces of trichloroacetic acid were extracted with ether after the solution had been passed through a column of Dowex AG 50 in the hydrogen form to remove all cations. High-molecular-weight compounds were removed by ultrafiltration and low-molecular-weight solutes by a two-stage chromatography on cellulose columns with organic solvents. In the first stage, sugars, amino acids, chloride and phytic acid were separated by using a basic solvent (propan-1-ol-water-aqueous ammonia) and, in the second stage, the organic acids and orthophosphoric acid were separated by using an acidic solvent (di-isopropyl ether-formic acid-2-methylpropan-2-ol-water). The final solution of nucleotide and sugar phosphates was substantially free from other solutes and was suitable for the detection of individual phosphate esters by either chromatography or enzymic assay. 5. The recovery of d-glucose 6-phosphate or adenosine 5'-triphosphate added to a trichloroacetic acid extract simulating that

  3. EXTRACTION AND ANALYSIS OF CONDENSED TANNINS IN CASTANEA SATIVA MILL.

    OpenAIRE

    J Živković; I Mujić; G Nikolić; S Vidović; A Mujić

    2010-01-01

    Proanthocyanidins, also known as condensed tannins are widespread in woody plants, but are also found in certain forages. Castanea sativa Mill. are exploited for various purposes, but a little is known about potential of this species and possible application in diet and therapy. The parts of chestnut such as: seed, peeled seed, brown seed shell, red internal seed shell, leaves, catkin, spiny bur, as well as the new and old chestnut bark were extracted with 50% ethanol as an extragents. Conten...

  4. Conformational analysis of amide extractants by NMR in organic phase

    International Nuclear Information System (INIS)

    Berthon, C.

    1993-08-01

    This study deals with nuclear fuel reprocessing. We have essentially used NMR spectroscopy. We want to understand which kind of conformational parameters control selectivity and efficiency of amide extractant. The symmetric monoamides used are DOBA (C 3 H 7 CON (CH 2 CH(C 2 H 5 ) C 4 H 9 ) 2 ), DOiBA ((CH 3 ) 2 CCHON (CH 2 CH(C 2 H 5 )C 4 H 9 ) 2 ) and DOTA ((CH 3 ) 3 CCH 2 CON(CH 2 CH(C 2 H 5 )C 4 H 9 ) 2 ). Each gives two quasi equivalent conformers (cis and trans) in organic phases. The selected malonamide DMDBTDMA ((C 4 H 9 (CH 3 )NCO) 2 CHC 14 H 29 ) has four conformers because of its twice disymmetric amide functions. Weak interactions between monoamides which yield to dimer formation. The malonamide also gives dimers but forms aggregates too. Nitric acid extraction is due to the competitive formation of six species L, L 2 , L 2 (HNO 3 ), L(HNO 3 ), L(HNO 3 ) 2 , L(HNO 3 ) 3 (L: monoamide). Complexation between lanthanides (III) and monoamides yields to the stoichiometries L 3 Ln(NO 3 ) 3 and L 2 Ln(NO 3 ) 3 . Their ratio depend of steric hindrance on the carbonyl and the metal ionic radius. The same thing is observed of Pu 4+ and Th 4+ extraction in non acidic media. L 2 An(NO 3 ) 4 is the main stoichiometric except for the Th 4+ - DOBA system where the species (DOBA) 3 Th(NO 3 ) 4 appear. Exchange rates between the ligand and the complex are pointed out. The monoamide conformations obtained with lanthanide and plutonium nitrate can explain the difference in extracting power of this molecule between An 4+ and Ln 3+ . (author). 162 refs., 87 figs., 44 tabs., 7 annexes

  5. Analysis of Extracting Prior BRDF from MODIS BRDF Data

    OpenAIRE

    Hu Zhang; Ziti Jiao; Yadong Dong; Peng Du; Yang Li; Yi Lian; Tiejun Cui

    2016-01-01

    Many previous studies have attempted to extract prior reflectance anisotropy knowledge from the historical MODIS Bidirectional Reflectance Distribution Function (BRDF) product based on land cover or Normalized Difference Vegetation Index (NDVI) data. In this study, the feasibility of the method is discussed based on MODIS data and archetypal BRDFs. The BRDF is simplified into six archetypal BRDFs that represent different reflectance anisotropies. Five-year time series of MODIS BRDF data over ...

  6. Application of Genetic Algorithm (GA) Assisted Partial Least Square (PLS) Analysis on Trilinear and Non-trilinear Fluorescence Data Sets to Quantify the Fluorophores in Multifluorophoric Mixtures: Improving Quantification Accuracy of Fluorimetric Estimations of Dilute Aqueous Mixtures.

    Science.gov (United States)

    Kumar, Keshav

    2018-03-29

    Excitation-emission matrix fluorescence (EEMF) and total synchronous fluorescence spectroscopy (TSFS) are the 2 fluorescence techniques that are commonly used for the analysis of multifluorophoric mixtures. These 2 fluorescence techniques are conceptually different and provide certain advantages over each other. The manual analysis of such highly correlated large volume of EEMF and TSFS towards developing a calibration model is difficult. Partial least square (PLS) analysis can analyze the large volume of EEMF and TSFS data sets by finding important factors that maximize the correlation between the spectral and concentration information for each fluorophore. However, often the application of PLS analysis on entire data sets does not provide a robust calibration model and requires application of suitable pre-processing step. The present work evaluates the application of genetic algorithm (GA) analysis prior to PLS analysis on EEMF and TSFS data sets towards improving the precision and accuracy of the calibration model. The GA algorithm essentially combines the advantages provided by stochastic methods with those provided by deterministic approaches and can find the set of EEMF and TSFS variables that perfectly correlate well with the concentration of each of the fluorophores present in the multifluorophoric mixtures. The utility of the GA assisted PLS analysis is successfully validated using (i) EEMF data sets acquired for dilute aqueous mixture of four biomolecules and (ii) TSFS data sets acquired for dilute aqueous mixtures of four carcinogenic polycyclic aromatic hydrocarbons (PAHs) mixtures. In the present work, it is shown that by using the GA it is possible to significantly improve the accuracy and precision of the PLS calibration model developed for both EEMF and TSFS data set. Hence, GA must be considered as a useful pre-processing technique while developing an EEMF and TSFS calibration model.

  7. Evaluation of sample extraction methods for proteomics analysis of green algae Chlorella vulgaris.

    Science.gov (United States)

    Gao, Yan; Lim, Teck Kwang; Lin, Qingsong; Li, Sam Fong Yau

    2016-05-01

    Many protein extraction methods have been developed for plant proteome analysis but information is limited on the optimal protein extraction method from algae species. This study evaluated four protein extraction methods, i.e. direct lysis buffer method, TCA-acetone method, phenol method, and phenol/TCA-acetone method, using green algae Chlorella vulgaris for proteome analysis. The data presented showed that phenol/TCA-acetone method was superior to the other three tested methods with regards to shotgun proteomics. Proteins identified using shotgun proteomics were validated using sequential window acquisition of all theoretical fragment-ion spectra (SWATH) technique. Additionally, SWATH provides protein quantitation information from different methods and protein abundance using different protein extraction methods was evaluated. These results highlight the importance of green algae protein extraction method for subsequent MS analysis and identification. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Analysis of entropy extraction efficiencies in random number generation systems

    Science.gov (United States)

    Wang, Chao; Wang, Shuang; Chen, Wei; Yin, Zhen-Qiang; Han, Zheng-Fu

    2016-05-01

    Random numbers (RNs) have applications in many areas: lottery games, gambling, computer simulation, and, most importantly, cryptography [N. Gisin et al., Rev. Mod. Phys. 74 (2002) 145]. In cryptography theory, the theoretical security of the system calls for high quality RNs. Therefore, developing methods for producing unpredictable RNs with adequate speed is an attractive topic. Early on, despite the lack of theoretical support, pseudo RNs generated by algorithmic methods performed well and satisfied reasonable statistical requirements. However, as implemented, those pseudorandom sequences were completely determined by mathematical formulas and initial seeds, which cannot introduce extra entropy or information. In these cases, “random” bits are generated that are not at all random. Physical random number generators (RNGs), which, in contrast to algorithmic methods, are based on unpredictable physical random phenomena, have attracted considerable research interest. However, the way that we extract random bits from those physical entropy sources has a large influence on the efficiency and performance of the system. In this manuscript, we will review and discuss several randomness extraction schemes that are based on radiation or photon arrival times. We analyze the robustness, post-processing requirements and, in particular, the extraction efficiency of those methods to aid in the construction of efficient, compact and robust physical RNG systems.

  9. Cluster Analysis of Customer Reviews Extracted from Web Pages

    Directory of Open Access Journals (Sweden)

    S. Shivashankar

    2010-01-01

    Full Text Available As e-commerce is gaining popularity day by day, the web has become an excellent source for gathering customer reviews / opinions by the market researchers. The number of customer reviews that a product receives is growing at very fast rate (It could be in hundreds or thousands. Customer reviews posted on the websites vary greatly in quality. The potential customer has to read necessarily all the reviews irrespective of their quality to make a decision on whether to purchase the product or not. In this paper, we make an attempt to assess are view based on its quality, to help the customer make a proper buying decision. The quality of customer review is assessed as most significant, more significant, significant and insignificant.A novel and effective web mining technique is proposed for assessing a customer review of a particular product based on the feature clustering techniques, namely, k-means method and fuzzy c-means method. This is performed in three steps : (1Identify review regions and extract reviews from it, (2 Extract and cluster the features of reviews by a clustering technique and then assign weights to the features belonging to each of the clusters (groups and (3 Assess the review by considering the feature weights and group belongingness. The k-means and fuzzy c-means clustering techniques are implemented and tested on customer reviews extracted from web pages. Performance of these techniques are analyzed.

  10. Dual solid-phase and stir bar sorptive extraction combined with gas chromatography-mass spectrometry analysis provides a suitable tool for assaying limonene-derived mint aroma compounds in red wine.

    Science.gov (United States)

    Picard, Magali; Franc, Céline; de Revel, Gilles; Marchand, Stéphanie

    2018-02-25

    A novel analytical method was developed for quantitative determination of eight limonene-derived monoterpenes responsible for the mint aroma in red wine. As these aromatic compounds are present at trace levels, a new dual extraction approach was proposed, combining solid-phase extraction (SPE) and stir bar sorptive extraction (SBSE), followed by gas chromatography-mass spectrometry analysis. The various parameters affecting the efficiency of extracting the analytes from wine samples in both the SPE and SBSE steps were first investigated, to determine the best compromise for the simultaneous analysis of the compounds studied. Following preliminary optimization of the dilution factor, phase ratio, and methanol content in the SBSE sample, cartridge sorbent mass, type of solvent, elution volume, and wine sample volume in the pre-concentration SPE step were studied. Highest response values were obtained when a 90 mL wine sample was extracted on a 500 mg SPE C18 cartridge and eluted with 1.5 mL methanol. The wine extract was then diluted in 10 mL water to obtain a final methanol content of 15% before the SBSE step. Good linearity, repeatability, reproducibility, accuracy and the required low detection and quantification limits were obtained under the conditions described, making this SPE-SBSE combination a suitable, powerful tool for routine analysis of the selected limonene-derived mint aroma compounds in large series of wine samples. Finally, the validated method was applied to 15 commercial red Bordeaux wines, aged from 3 to 23 years. Most of the compounds studied, present within the ng.L -1 range, were easily quantified for the first time in wine. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Determination of tributyltin (TBT) in marine sediment using pressurised liquid extraction-gas chromatography-isotope dilution mass spectrometry (PLE-GC-IDMS) with a hexane-tropolone mixture.

    Science.gov (United States)

    Konieczka, Piotr; Sejerøe-Olsen, Berit; Linsinger, Thomas P J; Schimmel, Heinz

    2007-06-01

    Extraction conditions for the determination of tributyltin (TBT) in sediment samples have been developed further. The analytical procedure is based on spiking with isotopically labelled analyte, pressurised liquid extraction (PLE) with a hexane/tropolone mixture, Grignard derivatization and quantification by GC-MS. It was applied to two unknown sediment samples as part of an intercomparison exercise of the Comité Consultatif pour la Quantité de Matière (CCQM). The detection limit was approximately 1.5 ng/g TBT as Sn, while the repeatability and intermediate precision (as the coefficient of variation) were 1.9% and 3.2%, respectively. The expanded uncertainty was 6.2% (coverage factor k = 2), and the accuracy was confirmed by measurement of a certified reference material.

  12. Analysis of the servo-spill control for slow beam extraction

    International Nuclear Information System (INIS)

    Sato, Hikaru; Toyama, Takeshi; Marutsuka, Katsumi; Shirakata, Masashi.

    1994-01-01

    This report describes an analysis of servo-spill control system for the slow beam extraction from the KEK PS. Transfer function of extraction process is derived from measurement of the closed-loop characteristic using measured frequency response of each equipment. Result indicates the restriction of the present servo-spill control and give a guide line for the improvement. (author)

  13. Native Liquid Extraction Surface Analysis Mass Spectrometry: Analysis of Noncovalent Protein Complexes Directly from Dried Substrates

    Science.gov (United States)

    Martin, Nicholas J.; Griffiths, Rian L.; Edwards, Rebecca L.; Cooper, Helen J.

    2015-08-01

    Liquid extraction surface analysis (LESA) mass spectrometry is a promising tool for the analysis of intact proteins from biological substrates. Here, we demonstrate native LESA mass spectrometry of noncovalent protein complexes of myoglobin and hemoglobin from a range of surfaces. Holomyoglobin, in which apomyoglobin is noncovalently bound to the prosthetic heme group, was observed following LESA mass spectrometry of myoglobin dried onto glass and polyvinylidene fluoride surfaces. Tetrameric hemoglobin [(αβ)2 4H] was observed following LESA mass spectrometry of hemoglobin dried onto glass and polyvinylidene fluoride (PVDF) surfaces, and from dried blood spots (DBS) on filter paper. Heme-bound dimers and monomers were also observed. The `contact' LESA approach was particularly suitable for the analysis of hemoglobin tetramers from DBS.

  14. MOLECULARLY IMPRINTED SOLID PHASE EXTRACTION FOR TRACE ANALYSIS OF DIAZINON IN DRINKING WATER

    Directory of Open Access Journals (Sweden)

    M. Rahiminejad ، S. J. Shahtaheri ، M. R. Ganjali ، A. Rahimi Forushani ، F. Golbabaei

    2009-04-01

    Full Text Available Amongst organophosphate pesticides, the one most widely used and common environmental contaminant is diazinon; thus methods for its trace analysis in environmental samples must be developed. Use of diazinon imprinted polymers such as sorbents in solid phase extraction, is a prominent and novel application area of molecular imprinted polymers. For diazinon extraction, high performance liquid chromatography analysis was demonstrated in this study. During optimization of the molecular imprinted solid phase extraction procedure for efficient solid phase extraction of diazinon, Plackett-Burman design was conducted. Eight experimental factors with critical influence on molecular imprinted solid phase extraction performance were selected, and 12 different experimental runs based on Plackett-Burman design were carried out. The applicability of diazinon imprinted polymers as the sorbent in solid phase extraction, presented obtained good recoveries of diazinon from LC-grade water. An increase in pH caused an increase in the recovery on molecular imprinted solid phase extraction. From these results, the optimal molecular imprinted solid phase extraction procedure was as follows: solid phase extraction packing with 100 mg diazinon imprinted polymers; conditioning with 5 mL of methanol and 6 mL of LC-grade water; sample loading containing diazinon (pH=10; washing with 1 mL of LC-grade water, 1 mL LC- grade water containing 30% acetonitrile and 0.5 mL of acetonitrile, respectively; eluting with 1 mL of methanol containing 2% acetic acid. The percentage recoveries obtained by the optimized molecular imprinted solid phase extraction were more than 90% with drinking water spiked at different trace levels of diazinon. Generally speaking, the molecular imprinted solid phase extraction procedure and subsequent high performance liquid chromatography analysis can be a relatively fast and proper approach for qualitative and quantitative analysis of diazinon in

  15. Optimization of a flow injection analysis system for multiple solvent extraction

    International Nuclear Information System (INIS)

    Rossi, T.M.; Shelly, D.C.; Warner, I.M.

    1982-01-01

    The performance of a multistage flow injection analysis solvent extraction system has been optimized. The effect of solvent segmentation devices, extraction coils, and phase separators on performance characteristics is discussed. Theoretical consideration is given to the effects and determination of dispersion and the extraction dynamics within both glass and Teflon extraction coils. The optimized system has a sample recovery similar to an identical manual procedure and a 1.5% relative standard deviation between injections. Sample throughput time is under 5 min. These characteristics represent significant improvements over the performance of the same system before optimization. 6 figures, 2 tables

  16. Moderate Dilution of Copper Slag by Natural Gas

    Science.gov (United States)

    Zhang, Bao-jing; Zhang, Ting-an; Niu, Li-ping; Liu, Nan-song; Dou, Zhi-he; Li, Zhi-qiang

    2018-01-01

    To enable use of copper slag and extract the maximum value from the contained copper, an innovative method of reducing moderately diluted slag to smelt copper-containing antibacterial stainless steel is proposed. This work focused on moderate dilution of copper slag using natural gas. The thermodynamics of copper slag dilution and ternary phase diagrams of the slag system were calculated. The effects of blowing time, temperature, matte settling time, and calcium oxide addition were investigated. The optimum reaction conditions were identified to be blowing time of 20 min, reaction temperature of 1250°C, settling time of 60 min, CaO addition of 4% of mass of slag, natural gas flow rate of 80 mL/min, and outlet pressure of 0.1 MPa. Under these conditions, the Fe3O4 and copper contents of the residue were 7.36% and 0.50%, respectively.

  17. The GC/MS Analysis of Volatile Components Extracted by Different Methods from Exocarpium Citri Grandis

    Directory of Open Access Journals (Sweden)

    Zhisheng Xie

    2013-01-01

    Full Text Available Volatile components from Exocarpium Citri Grandis (ECG were, respectively, extracted by three methods, that is, steam distillation (SD, headspace solid-phase microextraction (HS-SPME, and solvent extraction (SE. A total of 81 compounds were identified by gas chromatography-mass spectrometry including 77 (SD, 56 (HS-SPME, and 48 (SE compounds, respectively. Despite of the extraction method, terpenes (39.98~57.81% were the main volatile components of ECG, mainly germacrene-D, limonene, 2,6,8,10,14-hexadecapentaene, 2,6,11,15-tetramethyl-, (E,E,E-, and trans-caryophyllene. Comparison was made among the three methods in terms of extraction profile and property. SD relatively gave an entire profile of volatile in ECG by long-time extraction; SE enabled the analysis of low volatility and high molecular weight compounds but lost some volatiles components; HS-SPME generated satisfactory extraction efficiency and gave similar results to those of SD at analytical level when consuming less sample amount, shorter extraction time, and simpler procedure. Although SD and SE were treated as traditionally preparative extractive techniques for volatiles in both small batches and large scale, HS-SPME coupled with GC/MS could be useful and appropriative for the rapid extraction and qualitative analysis of volatile components from medicinal plants at analytical level.

  18. Passive vapor extraction feasibility study

    International Nuclear Information System (INIS)

    Rohay, V.J.

    1994-01-01

    Demonstration of a passive vapor extraction remediation system is planned for sites in the 200 West Area used in the past for the disposal of waste liquids containing carbon tetrachloride. The passive vapor extraction units will consist of a 4-in.-diameter pipe, a check valve, a canister filled with granular activated carbon, and a wind turbine. The check valve will prevent inflow of air that otherwise would dilute the soil gas and make its subsequent extraction less efficient. The granular activated carbon is used to adsorb the carbon tetrachloride from the air. The wind turbine enhances extraction rates on windy days. Passive vapor extraction units will be designed and operated to meet all applicable or relevant and appropriate requirements. Based on a cost analysis, passive vapor extraction was found to be a cost-effective method for remediation of soils containing lower concentrations of volatile contaminants. Passive vapor extraction used on wells that average 10-stdft 3 /min air flow rates was found to be more cost effective than active vapor extraction for concentrations below 500 parts per million by volume (ppm) of carbon tetrachloride. For wells that average 5-stdft 3 /min air flow rates, passive vapor extraction is more cost effective below 100 ppm

  19. Advances in extraction and analysis of phenolic compounds from plant materials

    Institute of Scientific and Technical Information of China (English)

    XU Cong-Cong; WANG Bing; PU Yi-Qiong; TAO Jian-Sheng; ZHANG Tong

    2017-01-01

    Phenolic compounds,the most abundant secondary metabolites in plants,have received more and more attention in recent years because of their distinct bioactivities.This review summarizes different types of phenolic compounds and their extraction and analytical methods used in the recent reports,involving 59 phenolic compounds from 52 kinds of plants.The extraction methods include solid-liquid extraction,ultrasound-assisted extractions,microwave-assisted extractions,supercritical fluid extraction,and other methods.The analysis methods include spectrophotometry,gas chromatography,liquid chromatography,thin-layer chromatography,capillary electrophoresis,and near-infrared spectroscopy.After illustrating the specific conditions of the analytical methods,the advantages and disadvantages of each method are also summarized,pointing out their respective suitability.This review provides valuable reference for identification and/or quantification of phenolic compounds from natural products.

  20. Phytochemical analysis of Andrographis paniculata and Orthosiphon stamineus leaf extracts for their antibacterial and antioxidant potential.

    Science.gov (United States)

    Malahubban, M; Alimon, A R; Sazili, A Q; Fakurazi, S; Zakry, F A

    2013-09-01

    Leaves of Andrographis paniculata and Orthosiphon stamineus were extracted with water, ethanol, methanol and chloroform to assess their potential as antibacterial and antioxidant agents. High performance liquid chromatography analysis showed that the methanolic extracts of A. paniculata and O. stamineus leaves gave the highest amounts of andrographolide and rosmarinic acid, respectively. These leaf extracts exhibited antimicrobial and antioxidant activities and, at the highest concentration tested (200 mg/mL), showed greater inhibitory effects against the Gram positive bacteria Bacillus cereus and Staphylococcus aureus than 10% acetic acid. Andrographis paniculata and O. stamineus methanolic and ethanolic leaf extracts also showed the strongest antioxidant activity as compared with the other extracts tested. The bioactive compounds present in these leaf extracts have the potential to be developed into natural antibacterial and antioxidant agents that may have applications in animal and human health.

  1. Feature Extraction and Analysis of Breast Cancer Specimen

    Science.gov (United States)

    Bhattacharyya, Debnath; Robles, Rosslin John; Kim, Tai-Hoon; Bandyopadhyay, Samir Kumar

    In this paper, we propose a method to identify abnormal growth of cells in breast tissue and suggest further pathological test, if necessary. We compare normal breast tissue with malignant invasive breast tissue by a series of image processing steps. Normal ductal epithelial cells and ductal / lobular invasive carcinogenic cells also consider for comparison here in this paper. In fact, features of cancerous breast tissue (invasive) are extracted and analyses with normal breast tissue. We also suggest the breast cancer recognition technique through image processing and prevention by controlling p53 gene mutation to some greater extent.

  2. Comparative analysis of in vivo T cell depletion with radiotherapy, combination chemotherapy, and the monoclonal antibody Campath-1G, using limiting dilution methodology

    International Nuclear Information System (INIS)

    Theobald, M.; Hoffmann, T.; Bunjes, D.; Heit, W.

    1990-01-01

    We have investigated the efficacy of standard conditioning regimens for bone marrow transplantation in depleting functional T lymphocytes in vivo and have compared it with the efficacy of the monoclonal antibody Campath-1G. Using limiting dilution techniques the frequencies of proliferating T cell precursors (PTL), cytotoxic T cell precursors (CTL-p), helper T cell precursors (HTL-p), and mature helper T cells (HTL) were determined before and after treatment. Both total body irradiation and combination chemotherapy with busulfan/cyclophosphamide were highly efficient at depleting PTL, CTL-p, and HTL-p (0-4 days) but spared HTL to a variable extent (0-99.5%). In the majority of patients treated with Campath-1G a similar degree of PTL, CTL-p, and HTL-p depletion was achieved, and, in addition, HTL were effectively removed (greater than 95.5%). These results suggest that Campath-1G could be successfully employed in depleting radio- and chemotherapy-resistant host T lymphocytes prior to T-depleted bone marrow transplantation

  3. Estimation by limiting dilution analysis of human IL 2-secreting T cells: detection of IL 2 produced by single lymphokine-secreting T cells

    International Nuclear Information System (INIS)

    Vie, H.; Miller, R.A.

    1986-01-01

    We present here a culture method for the estimation, in human blood, of the number of lymphocytes that can respond to mitogen by producing interleukin 2 (IL 2). T cells are cultured at limiting dilutions with PHA or Con A in the presence of Epstein Barr virus-transformed human lymphoblastoid cells (EB-LCL), and supernatants are tested 3 days later for IL 2 content by a cell proliferation assay. The distribution of negative wells follows the expected Poisson single-hit relationship, suggesting that the assay is sensitive to single cells of a single limiting cell type. On average, 16.3% of peripheral blood mononuclear cells can produce IL 2 in such clonal cultures (mean of 12 determinations; SD = 5.6%). Surprisingly, irradiation (up to 2000 rad) of the titrated responder cell population diminishes the estimated frequencies by less than 50%. The ability to detect IL 2 levels in cultures containing only a single, nonproliferating T lymphocyte allows us to estimate the amount of IL 2 generated by an individual effector cell during a 3-day culture interval after mitogen stimulation. The average responding, irradiated T cell generates 0.92 pg of IL 2 (median) within 3 days. The method presented provides a straightforward way to provide independent estimates of responding cell number and of lymphokine production per cell in a variety of clinical situations

  4. Microscopic Analysis of Pigments Extracted from Spalting Fungi

    Directory of Open Access Journals (Sweden)

    Sarath M. Vega Gutierrez

    2017-03-01

    Full Text Available Pigments that are currently available in the market usually come from synthetic sources, or, if natural, often need mordants to bind to the target substrate. Recent research on the fungal pigment extracts from Scytalidium cuboideum, Scytalidium ganodermophthorum, Chlorociboria aeruginosa, and Chlorociboria aeruginascens have been shown to successfully dye materials, like wood, bamboo, and textiles, however, there is no information about their binding mechanisms. Due to this, a microscopic study was performed to provide information to future manufacturers interested in these pigments. The results of this study show that S. ganodermophthorum and C. aeruginosa form an amorphous layer on substrates, while S. cuboideum forms crystal-like structures. The attachment and morphology indicate that there might be different chemical and physical interactions between the extracted pigments and the materials. This possibility can explain the high resistance of the pigments to UV light and color fastness that makes them competitive against synthetic pigments. These properties make these pigments a viable option for an industry that demands natural pigments with the properties of the synthetic ones.

  5. Alkaline Extraction of DNA from Pathogenic Fungi for PCR-RFLP Analysis

    OpenAIRE

    Matsumoto, Masaru; Mishima, Shinobu; Matsuyama, Nobuaki; 松元, 賢; 松山, 宣明

    1997-01-01

    For the preparation of DNA samples from fungal mycelia alkaline extraction method was applied and assessed its usefulness for PCR-RFLP analysis. Using alkaline treatment protocols, 18S ribosomal DNAs (rDNA) derived from fungal genomic DNA of Pyricularia oryzae, P. zingiberi, Rhizoctonia solani and R. oryzae were PCR-amplified and digested with Hha I, Msp I and Hae ill. RFLP analysis with HhaI showed the divergent polymorphism between genus Pyricularia and Rhizoctonia. The alkaline DNA extract...

  6. Laminar Flame Velocity and Temperature Exponent of Diluted DME-Air Mixture

    Science.gov (United States)

    Naseer Mohammed, Abdul; Anwar, Muzammil; Juhany, Khalid A.; Mohammad, Akram

    2017-03-01

    In this paper, the laminar flame velocity and temperature exponent diluted dimethyl ether (DME) air mixtures are reported. Laminar premixed mixture of DME-air with volumetric dilutions of carbon dioxides (CO2) and nitrogen (N2) are considered. Experiments were conducted using a preheated mesoscale high aspect-ratio diverging channel with inlet dimensions of 25 mm × 2 mm. In this method, flame velocities are extracted from planar flames that were stabilized near adiabatic conditions inside the channel. The flame velocities are then plotted against the ratio of mixture temperature and the initial reference temperature. A non-linear power law regression is observed suitable. This regression analysis gives the laminar flame velocity at the initial reference temperature and temperature exponent. Decrease in the laminar flame velocity and increase in temperature exponent is observed for CO2 and N2 diluted mixtures. The addition of CO2 has profound influence when compared to N2 addition on both flame velocity and temperature exponent. Numerical prediction of the similar mixture using a detailed reaction mechanism is obtained. The computational mechanism predicts higher magnitudes for laminar flame velocity and smaller magnitudes of temperature exponent compared to experimental data.

  7. Model analysis of mechanisms controlling pneumatic soil vapor extraction

    DEFF Research Database (Denmark)

    Høier, Camilla Kruse; Sonnenborg, Torben Obel; Jensen, Karsten Høgh

    2009-01-01

    of heterogeneous soils by enforcing large fluctuating pressure fronts through the contaminated area. Laboratory experiments have suggested that pneumatic SVE considerably improves the recovery rate from low-permeable units. We have analyzed the experimental results using a numerical code and quantified......The efficiency of traditional soil venting or soil vapor extraction (SVE) highly depends on the architecture of the subsurface because imposed advective air flow tends to bypass low-permeable contaminated areas. Pneumatic SVE is a technique developed to enhance remediation efficiency...... level the pneumatic venting technology is superior to the traditional technique, and that the method is particularly efficient in cases where large permeability contrasts exist between soil units in the subsurface....

  8. A method to extract soil water for stable isotope analysis

    Science.gov (United States)

    Revesz, Kinga; Woods, Peter H.

    1990-07-01

    A method has been developed to extract soil water for determination of deuterium (D) and 18O content. The principle of this method is based on the observation that water and toluene form an azeotropic mixture at 84.1°C, but are completely immiscible at ambient temperature. In a specially designed distillation apparatus, the soil water is distilled at 84.1°C with toluene and is separated quantitatively in the collecting funnel at ambient temperature. Traces of toluene are removed and the sample can be analyzed by mass spectrometry. Kerosene may be substituted for toluene. The accuracy of this technique is ± 2 and ± 0.2‰, respectively, for δD and δ 18O. Reduced accuracy is obtained at low water contents.

  9. Techniques to extract physical modes in model-independent analysis of rings

    International Nuclear Information System (INIS)

    Wang, C.-X.

    2004-01-01

    A basic goal of Model-Independent Analysis is to extract the physical modes underlying the beam histories collected at a large number of beam position monitors so that beam dynamics and machine properties can be deduced independent of specific machine models. Here we discuss techniques to achieve this goal, especially the Principal Component Analysis and the Independent Component Analysis.

  10. Cryogen-free dilution refrigerators

    International Nuclear Information System (INIS)

    Uhlig, K

    2012-01-01

    We review briefly our first cryogen-free dilution refrigerator (CF-DR) which was precooled by a GM cryocooler. We then show how today's dry DRs with pulse tube precooling have developed. A few examples of commercial DRs are explained and noteworthy features pointed out. Thereby we describe the general advantages of cryogen-free DRs, but also show where improvements are still desirable. At present, our dry DR has a base temperature of 10 mK and a cooling capacity of 700 μW at a mixing chamber temperature of 100 mK. In our cryostat, in most recent work, an additional refrigeration loop was added to the dilution circuit. This 4 He circuit has a lowest temperature of about 1 K and a refrigeration capacity of up to 100 mW at temperatures slightly above 1 K; the dilution circuit and the 4 He circuit can be run separately or together. The purpose of this additional loop is to increase the cooling capacity for experiments where the cooling power of the still of the DR is not sufficient to cool cold amplifiers and cables, e.g. in studies on superconducting quantum circuits or astrophysical applications.

  11. Cryogen-free dilution refrigerators

    Science.gov (United States)

    Uhlig, K.

    2012-12-01

    We review briefly our first cryogen-free dilution refrigerator (CF-DR) which was precooled by a GM cryocooler. We then show how today's dry DRs with pulse tube precooling have developed. A few examples of commercial DRs are explained and noteworthy features pointed out. Thereby we describe the general advantages of cryogen-free DRs, but also show where improvements are still desirable. At present, our dry DR has a base temperature of 10 mK and a cooling capacity of 700 μW at a mixing chamber temperature of 100 mK. In our cryostat, in most recent work, an additional refrigeration loop was added to the dilution circuit. This 4He circuit has a lowest temperature of about 1 K and a refrigeration capacity of up to 100 mW at temperatures slightly above 1 K; the dilution circuit and the 4He circuit can be run separately or together. The purpose of this additional loop is to increase the cooling capacity for experiments where the cooling power of the still of the DR is not sufficient to cool cold amplifiers and cables, e.g. in studies on superconducting quantum circuits or astrophysical applications.

  12. Plutonium determination by isotope dilution

    International Nuclear Information System (INIS)

    Lucas, M.

    1980-01-01

    The principle is to add to a known amount of the analysed solution a known amount of a spike solution consisting of plutonium 242. The isotopic composition of the resulting mixture is then determined by surface ionization mass spectrometry, and the plutonium concentration in the solution is deduced, from this measurement. For irradiated fuels neutronic studies or for fissile materials balance measurements, requiring the knowledge of the ratio U/Pu or of concentration both uranium and plutonium, it is better to use the double spike isotope dilution method, with a spike solution of known 233 U- 242 Pu ratio. Using this method, the ratio of uranium to plutonium concentration in the irradiated fuel solution can be determined without any accurate measurement of the mixed amounts of sample and spike solutions. For fissile material balance measurements, the uranium concentration is determined by using single isotope dilution, and the plutonium concentration is deduced from the ratio Pu/U and U concentration. The main advantages of isotope dilution are its selectivity, accuracy and very high sensitivity. The recent improvements made to surface ionization mass spectrometers have considerably increased the precision of the measurements; a relative precision of about 0.2% to 0.3% is obtained currently, but it could be reduced to 0.1%, in the future, with a careful control of the experimental procedures. The detection limite is around 0.1 ppb [fr

  13. Extraction optimization and pixel-based chemometric analysis of semi-volatile organic compounds in groundwater

    DEFF Research Database (Denmark)

    Christensen, Peter; Tomasi, Giorgio; Kristensen, Mette

    2017-01-01

    . In this study, we tested the combination of solid phase extraction (SPE) with dispersive liquid-liquid micro extraction (DLLME), or with stir bar sorptive extraction (SBSE), as an extraction method for semi-VOCs in groundwater. Combining SPE with DLLME or SBSE resulted in better separation of peaks...... in an unresolved complex mixture. SPE-DLLME was chosen as the preferred extraction method. SPE-DLLME covered a larger polarity range (logKo/w 2.0-11.2), had higher extraction efficiency at logKo/w 2.0-3.8 and 5.8-11.2, and was faster compared to SPE-SBSE. SPE-DLLME extraction combined with chemical analysis by gas...... chromatography-mass spectrometry (GC-MS) and pixel-based data analysis of summed extraction ion chromatograms (sEICs) was tested as a new method for chemical fingerprinting of semi-VOCs in 15 groundwater samples. The results demonstrate that SPE-DLLME-GC-MS provides an excellent compromise between compound...

  14. Optimization of the cooling circuit and thermo-mechanical analysis for the extraction grid of ELISE

    International Nuclear Information System (INIS)

    Nocentini, R.; Gutser, R.; Heinemann, B.; Froeschle, M.; Riedl, R.

    2011-01-01

    The NNBI test facility ELISE ('Extraction from a Large Ion Source Experiment'), presently under construction at IPP, will have an extraction area with the same width and half the height of the ITER source, acceleration up to 60 kV, for 10 s, every 180 s, and plasma generation up to 1 h. Electrons are co-extracted from the ion source. Suppression magnets in the extraction grid deflect the electrons onto the extraction grid surface. For 30 mA/cm 2 extracted electron current density and 10 kV extraction voltage, localized power density is in the order of 39 MW/m 2 near the grid apertures and a total heat load of 150 kW is deposited onto each extraction grid segment. Heat removal is provided by a water circuit inside the grid. For ELISE, a new cooling circuit has been developed to provide a more reliable operation. The optimization of the cooling circuit and the thermo-mechanical analysis of the extraction grid of ELISE, considering maximum grid temperature, mechanical stresses and grid deformation, has been performed using the codes KOBRA3, TrajAn, the ANSYS finite element package and the fluid dynamics code CFX.

  15. Preliminary phytochemical screening, Antibacterial potential and GC-MS analysis of two medicinal plant extracts.

    Science.gov (United States)

    Vijayaram, Seerangaraj; Kannan, Suruli; Saravanan, Konda Mani; Vasantharaj, Seerangaraj; Sathiyavimal, Selvam; P, Palanisamy Senthilkumar

    2016-05-01

    The presence study was aimed to catalyze the primary metabolites and their confirmation by using GC-MS analysis and antibacterial potential of leaf extract of two important medicinal plant viz., Eucalyptus and Azadirachta indica. The antibacterial potential of the methanol leaf extract of the studied species was tested against Escherichia coli, Pseudomonas aeruginosa, Klebsiellap neumoniae, Streptococcus pyogens, Staphylococcus aureus using by agar well diffusion method. The higher zone of inhibition (16mm) was observed against the bacterium Pseudomonas aeruginosa at 100μl concentration of methanol leaf extract. Preliminary phytochemical analysis of studied species shows that presence of phytochemical compounds like steroids, phenolic compounds and flavonoids. GC-MS analysis confirms the occurrence of 20 different compounds in the methanol leaf extract of the both studied species.

  16. EKSTRAKSI DAN ANALISIS FITOSTEROL LEMBAGA GANDUM [Extraction and analysis of Phytosterol from wheat germ (Triticum sp.

    Directory of Open Access Journals (Sweden)

    Latifah K Darusman3

    2005-04-01

    Full Text Available Phytosterol may reduce the absorption of cholesterol, and used for preventing atherosclerosis. It is limited in soybean, but potentially abundant in wheat germ. Research on the utilization of wheat germ sterol had not been reported so far. Many aspects of germ sterol extraction from wheat germ and its characteristics were still unknown. In this research, the best extraction method, kinds and content of phytosterol from wheat germ were investigated.This research consisted of two steps: (1 extraction of phytosterol directly form whole germ and ground germ using hexane, and indirect extraction through germ oil using hexane and mixed solvent of hexane and ethanol, and direct extraction from ground germ using ethanol; (2 analysis of the type and content of phytosterol in the crude extract through the following steps: preparation of crude extract, fractionation, and analysis.Results showed that indirect extraction through germ oil was considered as the best method which yielded 1.37% of phytosterol. The highest yield was obtained when extracted using a mixed solvent of hexane – ethanol 82:18. However, the odor of ethanol and hexane (gasoline like odor was still detected. The solvent’s ratio of hexane to ethanol at 1:2 resulted better odor of the extract. Extraction of sterol using ethanol yielded 18.39% of sterol when the ratio of germ to ethanol at 1:10 (w/v was applied.Results of quantitative analysis on the main component of crude extract of wheat germ sterol showed that the total content of sterol extracted with mixed solvent was higher than those extracted with ethanol. The ratio of hexane to ethanol at 1:1 (v/v gave higher content of total sterol, stigmasterol and campesterol, whereas higher content of -sitosterol was produced at the solvent’s ratio of hexane to ethanol at 1:2 (v/v.

  17. Stakeholder acceptance analysis: Passive soil vapor extraction using borehole flux

    International Nuclear Information System (INIS)

    Peterson, T.S.

    1995-12-01

    This report presents evaluations, recommendations, and requirements concerning passive soil vapor extraction (PSVE) derived from a three-year program of stakeholder involvement. PSVE takes advantage of the naturally occurring tendency of soil vapor to leave the subsurface during periods of low barometric pressure. PSVE seeks to expedite the release of volatile contaminants through the use of boreholes and technological enhancements. This report is for technology developers and those responsible for making decisions about the use of technology to remediate contamination by volatile organic compounds. Stakeholders' perspectives help those responsible for technology deployment to make good decisions concerning the acceptability and applicability of PSVE to the remediation problems they face. The report provides: stakeholders' final evaluation of the acceptability of PSVE in light of the technology's field test; stakeholders' principal comments concerning PSVE; requirements that stakeholders have of any remediation technology. Technology decision makers should take these conclusions into account in evaluating the effectiveness and acceptability of any remedial method proposed for their site. In addition, the report presents data requirements for the technology's field demonstration defined by stakeholders associated with the Hanford site in Washington State, as well as detailed comments on PSVE from stakeholders from Sandia National Laboratory, Rocky Flats, Idaho National Engineering Laboratory, and Los Alamos National Laboratory

  18. Analysis of synchronized charge extraction for piezoelectric energy harvesting

    International Nuclear Information System (INIS)

    Tang, Lihua; Yang, Yaowen

    2011-01-01

    In the past few years, various power conditioning circuits have been proposed to improve the efficiency of piezoelectric energy harvesting, among which the synchronized charge extraction (SCE) technique has been enthusiastically pursued. In the literature, the SCE technique is investigated based on the uncoupled or in-phase assumptions. The uncoupled assumption is only valid for weak electromechanical coupling and the in-phase assumption is not applicable for energy harvesting at off-resonance. In this paper, we derive an accurate analytical solution for the piezoelectric energy harvesting systems with the SCE technique. Based on this solution, we investigate the applicability of the SCE technique for different cases, i.e. the piezoelectric energy harvester (PEH) with various degrees of electromechanical coupling and the PEH excited at various frequencies. Circuit simulation is also conducted with an accurate circuit model derived for PEHs and the results validate the analytical outcomes. Both the accurate analytical solution and the circuit simulation show that the SCE technique cannot improve or even reduces the power output at resonance if the coupling of the PEH is not negligible. The SCE technique is found capable of significantly boosting the efficiency of energy harvesting only for the PEH vibrating at off-resonance frequencies or with weak coupling

  19. Phytochemical analysis and gastroprotective activity of an olive leaf extract

    Directory of Open Access Journals (Sweden)

    IVANA ARSIĆ

    2009-04-01

    Full Text Available Some medicinal features of olive leaf have been known for centuries. It has been traditionally used as an antimicrobial and to prevent and treat diabetes mellitus and heart disease. Whether olive leaf, a natural antioxidant, influences the gastric defense mechanism and exhibits gastroprotection against experimentally-induced gastric lesions remains unknown. In this study, the content of total phenols, total flavonoids and tannins in olive leaf extract (OLE were determined. Seven phenolic compounds were identified and quantified (oleuropein, caffeic acid, luteolin, luteolin-7-O-glucoside, apigenin-7-O-glucoside, quercetin, and chryseriol. Furthermore, the protective activity of the OLE in gastric mucosal injury induced by a corrosive concentration of ethanol was investigated. In relation to the control group, pretreatment with OLE (40, 80 and 120 mg kg-1 significantly (p < 0.001 attenuated the gastric lesions induced by absolute ethanol. The protective effect of the OLE was similar to that obtained with a reference drug, ranitidine. The results obtained indicate that OLE possesses significant gastroprotective activity, and that the presence of compounds with antioxidative properties would probably explain this effect.

  20. Removal of iron interferences by solvent extraction for geochemical analysis by atomic-absorption spectrophotometry

    Science.gov (United States)

    Zhou, L.; Chao, T.T.; Sanzolone, R.F.

    1985-01-01

    Iron is a common interferent in the determination of many elements in geochemical samples. Two approaches for its removal have been taken. The first involves removal of iron by extraction with methyl isobutyl ketone (MIBK) from hydrochloric acid medium, leaving the analytes in the aqueous phase. The second consists of reduction of iron(III) to iron(II) by ascorbic acid to minimize its extraction into MIBK, so that the analytes may be isolated by extraction. Elements of interest can then be determined using the aqueous solution or the organic extract, as appropriate. Operating factors such as the concentration of hydrochloric acid, amounts of iron present, number of extractions, the presence or absence of a salting-out agent, and the optimum ratio of ascorbic acid to iron have been determined. These factors have general applications in geochemical analysis by atomic-absorption spectrophotometry. ?? 1985.

  1. Hibiscus sabdariffa L extract drying with different carrier agent: Drying rate evaluation and color analysis

    Science.gov (United States)

    Djaeni, M.; Utari, F. D.; Kumoro, A. C.

    2017-03-01

    The aim of this study was to investigate the effect of different carrier agents on roselle or Hibiscus sabdariffa L.extract drying. Carrier agent was used for reducing stickiness of material and avoiding agglomeration as well as improving stability. The method consisted of two steps involving roselle extraction and drying process. The liquid roselle extract was mixed with carrier agent (maltodextrin-arabic gum) in various composition. The mixture was then dried at different air temperature ranging 40 - 80°C. As a response, moisture content in the extract was observed by gravimetry every 10 minutes during90 minutes. The procedurewas repeated for the drying without carrieragent. The result showed that constant rate of drying with carrier agent was higher up to l.7 times than that of without carrier agent. Based on the color analysis,roselle extract drying with carrier agent also showed reasonable quality.

  2. Molecularly imprinted solid-phase extraction in the analysis of agrochemicals.

    Science.gov (United States)

    Yi, Ling-Xiao; Fang, Rou; Chen, Guan-Hua

    2013-08-01

    The molecular imprinting technique is a highly predeterminative recognition technology. Molecularly imprinted polymers (MIPs) can be applied to the cleanup and preconcentration of analytes as the selective adsorbent of solid-phase extraction (SPE). In recent years, a new type of SPE has formed, molecularly imprinted polymer solid-phase extraction (MISPE), and has been widely applied to the extraction of agrochemicals. In this review, the mechanism of the molecular imprinting technique and the methodology of MIP preparations are explained. The extraction modes of MISPE, including offline and online, are discussed, and the applications of MISPE in the analysis of agrochemicals such as herbicides, fungicides and insecticides are summarized. It is concluded that MISPE is a powerful tool to selectively isolate agrochemicals from real samples with higher extraction and cleanup efficiency than commercial SPE and that it has great potential for broad applications.

  3. A novel murmur-based heart sound feature extraction technique using envelope-morphological analysis

    Science.gov (United States)

    Yao, Hao-Dong; Ma, Jia-Li; Fu, Bin-Bin; Wang, Hai-Yang; Dong, Ming-Chui

    2015-07-01

    Auscultation of heart sound (HS) signals serves as an important primary approach to diagnose cardiovascular diseases (CVDs) for centuries. Confronting the intrinsic drawbacks of traditional HS auscultation, computer-aided automatic HS auscultation based on feature extraction technique has witnessed explosive development. Yet, most existing HS feature extraction methods adopt acoustic or time-frequency features which exhibit poor relationship with diagnostic information, thus restricting the performance of further interpretation and analysis. Tackling such a bottleneck problem, this paper innovatively proposes a novel murmur-based HS feature extraction method since murmurs contain massive pathological information and are regarded as the first indications of pathological occurrences of heart valves. Adapting discrete wavelet transform (DWT) and Shannon envelope, the envelope-morphological characteristics of murmurs are obtained and three features are extracted accordingly. Validated by discriminating normal HS and 5 various abnormal HS signals with extracted features, the proposed method provides an attractive candidate in automatic HS auscultation.

  4. Percent body fat and BMI in indigenous and mestizo children from South, Centre and North Mexico derived from bioimpedance analysis (BIA) and deuterium oxide dilution

    International Nuclear Information System (INIS)

    Valencia, Mauro E; Ramirez-Lopez, Erik; Ramos-Salas, Je; Bourges, Hector; Espinoza, Teresa

    2014-01-01

    Full text: Background. Body mass index (BMI) is an international standard to evaluate nutritional status but has the inability to distinguish fat mass from fat free mass, especially with regards to ethnicity. Mexico is the eight country in ethnic diversity in the world. The changes in fat mass and fat free mass offers the possibility to evaluate the effects of intervention programs in shorter periods. Objective. The purpose of the present study was to investigate the relationship between body composition and anthropometric characteristics of indigenous and mestizo Mexican children. Subject and Methods. A total of 1618 male and female indigenous (n = 498) and mestizo (n = 1120) children 7-9 years, were selected by stratified multiple stage cluster sampling. Indigenous groups and States were: Tarahumaras (Chihuahua), Mayos (Sonora), Nahuas (Puebla), Otomíes (Hidalgo), Tzotziles (Chiapas) and Mayas (Yucatan Peninsula). Mestizos form the same regions were included. Fat free mass and fat mass were obtained from a previously reported BIA cross validated equation using deuterium oxide dilution from 339 children from the same population, groups and regions. Results. The indigenous groups had 18.5 + 5.9 % fat compared to 23.5 + 8.4 in the mestizos (p<0.0001). Nahuas had the lowest % fat (p<0.0001) with 16.5 + 5.7, compared to Mayos, Tarahumaras and Mayas that had 18.6 + 6.2, 19.0 + 6.3 and 18.0 + 6.5 respectively. Mestizos form the Centre, North, and South had the highest levels of % body fat (p<0.001) with 25.4 + 7.7, 21.9 + 8.2, and 20.5 + 7.8, respectively. In indigenous children (n = 498) the 5th percentile (95% CI) corresponded to 9 (8,10) % body fat, while for Mestizos (n = 1120), the 5th percentile was 10 (9,11). Using this percentile, only one third of the children approximately of both groups would be classified as thin by WHO and IOTF classifications. Conclusion. Indigenous children had lower body fat than mestizos, however, the relationship of BMI to % body fat

  5. Optimising the Use of TRIzol-extracted Proteins in Surface Enhanced Laser Desorption/ Ionization (SELDI Analysis

    Directory of Open Access Journals (Sweden)

    Perlaky Laszlo

    2006-03-01

    Full Text Available Abstract Background Research with clinical specimens is always hampered by the limited availability of relevant samples, necessitating the use of a single sample for multiple assays. TRIzol is a common reagent for RNA extraction, but DNA and protein fractions can also be used for other studies. However, little is known about using TRIzol-extracted proteins in proteomic research, partly because proteins extracted from TRIzol are very resistant to solubilization. Results To facilitate the use of TRIzol-extracted proteins, we first compared the ability of four different common solubilizing reagents to solubilize the TRIzol-extracted proteins from an osteosarcoma cell line, U2-OS. Then we analyzed the solubilized proteins by Surface Enhanced Laser Desorption/ Ionization technique (SELDI. The results showed that solubilization of TRIzol-extracted proteins with 9.5 M Urea and 2% CHAPS ([3-[(3-cholamidopropyl-dimethylammonio]propanesulfonate] (UREA-CHAPS was significantly better than the standard 1% SDS in terms of solubilization efficiency and the number of detectable ion peaks. Using three different types of SELDI arrays (CM10, H50, and IMAC-Cu, we demonstrated that peak detection with proteins solubilized by UREA-CHAPS was reproducible (r > 0.9. Further SELDI analysis indicated that the number of ion peaks detected in TRIzol-extracted proteins was comparable to a direct extraction method, suggesting many proteins still remain in the TRIzol protein fraction. Conclusion Our results suggest that UREA-CHAPS performed very well in solubilizing TRIzol-extracted proteins for SELDI applications. Protein fractions left over after TRIzol RNA extraction could be a valuable but neglected source for proteomic or biochemical analysis when additional samples are not available.

  6. Determination of microquantities of silver in platinum by isotope dilution

    International Nuclear Information System (INIS)

    Yedinakova, V.; Sladkovska, Y.

    1980-01-01

    A method is described for determining microquantities of silver in platinum. It is based on isotope dilution by means of substoichiometric extraction of dithizonates with carbon tetrachloride. The determination of silver according to this technique is not interfered by zinc or gold in quantities exceeding the silver content by one order of magnitude nor by a great excess of platinum. In the presence of copper the addition of complexon is necessary. (author)

  7. Phytochemical analysis and standardization of Strychnos nux-vomica extract through HPTLC techniques

    Directory of Open Access Journals (Sweden)

    Dinesh Kumar Patel

    2012-05-01

    Full Text Available Objective: The objective is to develop a noval qualitative and quantitative method by which we can determine different phytoconstituents of Strychnos nux-vomica L. Methods: To profile the phyconstituents of Strychnos nux-vomica, in the present study hydroalcoholic extract of Strychnos nux-vomica was subjected to preliminary phytochemical analysis, antimicrobial activities against certain pathogenic microorganisms, solubility test, loss on drying and pH value. Extract was also subjected to the quantitative analysis including total phenol, flavonoid and heavy metal analysis. Quantitative analysis was performed through HPTLC methods using strychnine and brucine as a standard marker. Results: Phytochemical analysis revealed the presence of alkaloid, carbohydrate, tannin, steroid, triterpenoid and glycoside in the extract. Total flavonoid and phenol content of Strychnos nux-vomica L extract was found to be 0.40 % and 0.43%. Result showed that the level of heavy metal (lead, arsenic, mercury and cadmium complie the standard level. Total bacterial count, yeast and moulds contents were found to be under the limit whereas E. coli and salmonella was found to be absent in the extract. Content of strychnine and brucine were found to be 4.75% and 3.91%. Conclusions: These studies provide valluable information for correct identification and selection of the drug from various adulterations. In future this study will be helpful for the quantitative analysis as well as standardization of the Strychnos nux-vomica L.

  8. Analysis of Volatile Compounds from Solanumbetaceum Cav. Fruits from Panama by Head-Space Micro Extraction

    Directory of Open Access Journals (Sweden)

    Armando A. Durant

    2013-01-01

    Full Text Available The characterization of the volatile compounds of two varieties of Solanum betaceum Cav. by means of headspace solid-phase microextraction (HS-SPME coupled with gas chromatography-mass spectrometry ( GC-MS i s presented. The HS-SPME method for extraction of the volatiles compounds was optimized by using a 2 3 central composite design. Maximum extraction of volatile compounds was achieved by using a divinylbenzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS fiber, extraction temperature 76° C, incubation time 44 min, and extraction time of 46 min. The main types of compounds detected in both varieties are terpenoids, followed by aromatics, esters, and aldehydes. Golden-yellow cultivars contained higher levels of esters and terpenes, while the reddish-purple variety contained a significant amount of aromatic compounds. The data structure of the chemical information obtained as well as the relationship between variables was evaluated by means of principal component analysis and cluster analysis.

  9. Antimicrobial activity and some phytochemical analysis of two extracts Vinca minor L.

    Directory of Open Access Journals (Sweden)

    Grujić Sandra M.

    2014-01-01

    Full Text Available This study investigated the antimicrobial activity as well as some phytochemical analysis of ethanol and diethyl ether extracts from plant species Vinca minor L. In vitro antimicrobial activity of extracts was studied on 20 strains of microorganisms (16 bacteria and four yeasts. Testing was performed by microdilution method and minimum inhibitory concentration (MIC and minimum microbicidal concentration (MMC were determined. The strongest antimicrobial activity was detected on G+ bacteria of the genus Bacillus. Tested G- bacteria and yeasts were not sensitive to the action of the extracts or the sensitivity was insignificant. Phytochemical analysis involved determining the amount of total phenolics, flavonoids and tannins, as well as the determination of antioxidant activity monitoring capability to neutralize free radicals (DPPH and the reductive potential. Phytochemical examination indicates that the total phenolic compounds were more in the ethanolic extract and the content of flavonoids and tannins marginally higher in the diethyl ether extract. The antioxidant activity (DPPH of the ethanolic extract of V. minor was significantly stronger as compared to the diethyl ether extract, and the reduction potential was approximately the same.

  10. Supercritical Fluid Extraction of Quinones from Compost for Microbial Community Analysis

    Directory of Open Access Journals (Sweden)

    Ni Luh Gede Ratna Juliasih

    2015-01-01

    Full Text Available Supercritical fluid extraction (SFE was used to extract quinones from compost to monitor the microbial community dynamics during composting. The 0.3 g of dried compost was extracted using 3 mL min−1 of carbon dioxide (90% and methanol (10% at 45°C and 25 MPa for a 30 min extraction time. The extracted quinones were analysed using ultra performance liquid chromatography (UPLC with 0.3 mL min−1 of methanol mobile phase for a 50 min chromatographic run time. A comparable detected amount of quinones was obtained using the developed method and an organic solvent extraction method, being 36.06 μmol kg−1 and 34.54 μmol kg−1, respectively. Significantly low value of dissimilarity index (D between the two methods (0.05 indicated that the quinone profile obtained by both methods was considered identical. The developed method was then applied to determine the maturity of the compost by monitoring the change of quinone during composting. The UQ-9 and MK-7 were predominant quinones in the initial stage of composting. The diversity of quinone became more complex during the cooling and maturation stages. This study showed that SFE had successfully extracted quinones from a complex matrix with simplification and rapidity of the analysis that is beneficial for routine analysis.

  11. Cleanup and analysis of sugar phosphates in biological extracts by using solid phase extraction and anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Smith, Hans Peter; Cohen, A.; Buttler, T.

    1998-01-01

    of Saccharomyces cerevisiae obtained by using cold methanol as quenching agent and chloroform as extraction solvent. It was shown that pretreatment of the cell extract with SPE markedly improved the quality of the liquid chromatography analysis with recoveries of the sugar phosphates close to 100%. Furthermore...

  12. Music video shot segmentation using independent component analysis and keyframe extraction based on image complexity

    Science.gov (United States)

    Li, Wei; Chen, Ting; Zhang, Wenjun; Shi, Yunyu; Li, Jun

    2012-04-01

    In recent years, Music video data is increasing at an astonishing speed. Shot segmentation and keyframe extraction constitute a fundamental unit in organizing, indexing, retrieving video content. In this paper a unified framework is proposed to detect the shot boundaries and extract the keyframe of a shot. Music video is first segmented to shots by illumination-invariant chromaticity histogram in independent component (IC) analysis feature space .Then we presents a new metric, image complexity, to extract keyframe in a shot which is computed by ICs. Experimental results show the framework is effective and has a good performance.

  13. Streamlined Membrane Proteome Preparation for Shotgun Proteomics Analysis with Triton X-100 Cloud Point Extraction and Nanodiamond Solid Phase Extraction

    Directory of Open Access Journals (Sweden)

    Minh D. Pham

    2016-05-01

    Full Text Available While mass spectrometry (MS plays a key role in proteomics research, characterization of membrane proteins (MP by MS has been a challenging task because of the presence of a host of interfering chemicals in the hydrophobic protein extraction process, and the low protease digestion efficiency. We report a sample preparation protocol, two-phase separation with Triton X-100, induced by NaCl, with coomassie blue added for visualizing the detergent-rich phase, which streamlines MP preparation for SDS-PAGE analysis of intact MP and shot-gun proteomic analyses. MP solubilized in the detergent-rich milieu were then sequentially extracted and fractionated by surface-oxidized nanodiamond (ND at three pHs. The high MP affinity of ND enabled extensive washes for removal of salts, detergents, lipids, and other impurities to ensure uncompromised ensuing purposes, notably enhanced proteolytic digestion and down-stream mass spectrometric (MS analyses. Starting with a typical membranous cellular lysate fraction harvested with centrifugation/ultracentrifugation, MP purities of 70%, based on number (not weight of proteins identified by MS, was achieved; the weight-based purity can be expected to be much higher.

  14. Immunohistochemical Analysis of Platelet Extract Effects on Liver Injury Induced by CCl4 in Male Rats

    OpenAIRE

    Zahra Hesami; Maryam Ayatollahi; Bita Geramizadeh; Akram Jamshidzadeh; Akbar Vahdati

    2016-01-01

    Backgrounds & objectives: Liver damage results in a large accumulation of external cellular matrix that affects the function of this important body organ in a long term and finally stops its function completely. The growth factors existing in platelet extract are more cost-effective, available, and stable than recombinant ones. To determine whether the platelet extract effects on histological changes in liver injury induced by carbon tetrachloride (CCl4), we used immunohistochemical analysis ...

  15. A miniaturized plastic dilution refrigerator

    International Nuclear Information System (INIS)

    Bindilatti, V.; Oliveira, N.F.Jr.; Martin, R.V.; Frossati, G.

    1996-01-01

    We have built and tested a miniaturized dilution refrigerator, completely contained (still, heat exchanger and mixing chamber) inside a plastic (PVC) tube of 10 mm diameter and 170 mm length. With a 25 cm 2 CuNi heat exchanger, it reached temperatures below 50 mK, for circulation rates below 70 μmol/s. The cooling power at 100 mK and 63 μmol/s was 45 μW. The experimental space could accommodate samples up to 6 mm in diameter. (author)

  16. Liquid membrane extraction techniques for trace metal analysis and speciation in environmental and biological matrices

    Energy Technology Data Exchange (ETDEWEB)

    Ndungu, Kuria

    1999-04-01

    In this thesis, liquid-membrane-based methods for the analysis of trace metal species in samples of environmental and biological origin were developed. By incorporating extracting reagents in the membrane liquid, trace metal ions were selectively separated from humic-rich natural waters and urine samples, prior to their determination using various instrumental techniques. The extractions were performed in closed flow systems thus allowing easy automation of both the sample clean-up and enrichment. An acidic organophosphorus reagent (DEHPA) and a basic tetraalkylammonium reagent (Aliquat-336) were used as extractants in the membrane liquid to selectively extract and enrich cationic and anionic metal species respectively. A speciation method for chromium species was developed that allowed the determination of cationic Cr(III) species and anionic CR(VI) species in natural water samples without the need of a chromatographic separation step prior to their detection. SLM was also coupled on-line to potentiometric stripping analysis providing a fast and sensitive method for analysis of Pb in urine samples. A microporous membrane liquid-liquid extraction (MMLLE) method was developed for the determination of organotin compounds in natural waters that reduced the number of manual steps involved in the LLE of organotin compounds prior to their CC separation. Clean extracts obtained after running unfiltered humic-rich river water samples through the MMLLE flow system allowed selective determination of all the organotin compounds in a single run using GC-MS in the selected ion monitoring mode (SIM) 171 refs, 9 figs, 4 tabs

  17. Academic vocabulary in learner writing from extraction to analysis

    CERN Document Server

    Paquot, Magali

    2010-01-01

    Academic vocabulary is in fashion, as witnessed by the increasing number of books published on the topic. In the first part of this book, Magali Paquot scrutinizes the concept of academic vocabulary and proposes a corpus-driven procedure based on the criteria of keyness, range and evenness of distribution to select academic words that could be part of a common-core academic vocabulary syllabus. In the second part, the author offers a thorough analysis of academic vocabulary in the International Corpus of Learner English (ICLE) and describes the factors that account for learners difficulties in

  18. Large datasets: Segmentation, feature extraction, and compression

    Energy Technology Data Exchange (ETDEWEB)

    Downing, D.J.; Fedorov, V.; Lawkins, W.F.; Morris, M.D.; Ostrouchov, G.

    1996-07-01

    Large data sets with more than several mission multivariate observations (tens of megabytes or gigabytes of stored information) are difficult or impossible to analyze with traditional software. The amount of output which must be scanned quickly dilutes the ability of the investigator to confidently identify all the meaningful patterns and trends which may be present. The purpose of this project is to develop both a theoretical foundation and a collection of tools for automated feature extraction that can be easily customized to specific applications. Cluster analysis techniques are applied as a final step in the feature extraction process, which helps make data surveying simple and effective.

  19. Phytochemical analysis and antibacterial activities extracts of mangrove leaf against the growth of some pathogenic bacteria.

    Science.gov (United States)

    Alizadeh Behbahani, Behrooz; Tabatabaei Yazdi, Farideh; Shahidi, Fakhri; Noorbakhsh, Hamid; Vasiee, Alireza; Alghooneh, Ali

    2018-01-01

    In this study, the effects of water, ethanol, methanol and glycerin at five levels (0, 31.25, 83.33, 125 and 250 ml) were investigated on the efficiency of mangrove leaf extraction using mixture optimal design. The antimicrobial effect of the extracts on Streptococcus pneumoniae, Enterococcus faecium and Klebsiella pneumoniae was evaluated using disk diffusion, minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) methods. The mangrove leaf extraction components were identified through gas chromatography/mass spectrometry (GC/MS). Phytochemical analysis (alkaloids, tannins, saponins, flavone and glycosides) were evaluated based on qualitative methods. Antioxidant activity of extracts was measured using 2,2-diphenyl-1-picrylhydrazyl (DPPH), ferric reducing antioxidant potential (FRAP) methods. Maximum antimicrobial effect was observed in Enterococcus faecium and highest resistance against mangrove leaf extract in Enterococcus faecium and Klebsiella pneumoniae, respectively. Increasing concentration of mangrove extracts had a significant effect (p ≤ 0.05) on inhibition zone diameter. The MICs of the mangrove leaf extraction varied from 4 mg/ml to 16 mg/ml. The optimum formulation was found to contain glycerin (0 ml), water (28.22 ml), methanol (59.83 ml) and ethanol (161.95 ml). The results showed that the highest antioxidant activity was related to optimum extract of mangrove leaf and ethanolic extract respectively. The results of phytochemical screening of Avicennia marina leaves extract showed the existence of alkaloids, tannins, saponins, flavone and glycosides. 2-Propenoic acid, 3-phenyl- was the major compound of Avicennia marina. The results of non-significant lack of fit tests, and F value (14.62) indicated that the model was sufficiently accurate. In addition, the coefficient of variations (16.8%) showed an acceptable reproducibility. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. A model for the description of the coolant mixing and its application to the analysis of boron dilution transients in pressurized water reactors; Ein Modell zur Beschreibung der Kuehlmittelvermischung und seine Anwendung auf die Analyse von Borverduennungstransienten in Druckwasserreaktoren

    Energy Technology Data Exchange (ETDEWEB)

    Kliem, Soeren

    2010-08-15

    A model for the realistic description of the coolant mixing inside the pressure vessel of a pressurized water reactors has been developed and validated. This fast running model is based on the linear superposition of response functions on Dirac-pulse-like perturbations of the coolant parameters. It has been implemented into the coupled code system DYN3D/ATHLET nad serves as the interface between the one-dimensional thermal hydraulic system code ATHLETE and the 3D neutron kinetic core model DYN3D. By help of this model, the coolant mixing inside the reactor pressure vessel can e simulated in an efficient manner. A methodology for this analysis of hypothetical boron dilution accidents has been developed, which is based on the newly developed model for the coolant mixing. This methodology consists of a combination of stationary and transient calculations including a realistic treatment of the mixing of deborated slugs on the way towards the reactor core. The degree of conservatism can be adjusted by the variation of the initial size of the deborated slug. This new method was applied to two different boron dilution accidents. Besides the start of the first main coolant pump with a deborated slug of coolant in the cold leg of the primary circuit, a deboration event during the operation of the residual heat removal system was investigated. The results of the parameter study for a reactor core with a generic loading pattern demonstrated in both cases, that although the shut-down reactor becomes re-critical safety relevant cladding temperature limits are not reached, even if maximum possible volumes of the deborated slug are considered. The main reason for these results is the use of realistic time-dependent distributions of the boron concentration at the inlet of each fuel assembly.

  1. Guideline on Isotope Dilution Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gaffney, Amy [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2017-05-19

    Isotope dilution mass spectrometry is used to determine the concentration of an element of interest in a bulk sample. It is a destructive analysis technique that is applicable to a wide range of analytes and bulk sample types. With this method, a known amount of a rare isotope, or ‘spike’, of the element of interest is added to a known amount of sample. The element of interest is chemically purified from the bulk sample, the isotope ratio of the spiked sample is measured by mass spectrometry, and the concentration of the element of interest is calculated from this result. This method is widely used, although a mass spectrometer required for this analysis may be fairly expensive.

  2. Evaluation and validation of a single-dilution potency assay based upon serology of vaccines containing diphtheria toxoid: analysis for consistency in production and testing at the laboratory of the Control of Biological Products of the RIVM

    NARCIS (Netherlands)

    Akkermans AM; Hendriksen CFM; Marsman FR; de Jong WH; van de Donk HJM

    1993-01-01

    A single-dilution assay can be a valid procedure to demonstrate that a product exceeds the minimal requirement given for potency provided that consistency in production and testing has been proven. Information is presented justifying the use of a single dilution assay based upon quantitative

  3. Thermal diffusion in dilute nanofluids investigated by photothermal interferometry

    International Nuclear Information System (INIS)

    Philip, J; Nisha, M R

    2010-01-01

    We have carried out a theoretical analysis of the dependence of the particle mass fraction on the thermal diffusivity of dilute suspensions of nanoparticles in liquids (dilute nanofluids). The analysis takes in to account adsorption of an ordered layer of solvent molecules around the nanoparticles. It is found that thermal diffusivity decreases with mass fraction for sufficiently small particle sizes. Beyond a critical particle size thermal diffusivity begins to increase with mass fraction for the same system. The results have been verified experimentally by measuring the thermal diffusivity of dilute suspensions of TiO 2 nanoparticles dispersed in polyvinyl alcohol (PVA) medium. The effect is attributed to Kapitza resistance of thermal waves in the medium.

  4. Determination of Terpenoid Content in Pine by Organic Solvent Extraction and Fast-GC Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Harman-Ware, Anne E., E-mail: anne.ware@nrel.gov; Sykes, Robert [National Bioenergy Center, National Renewable Energy Laboratory, Golden, CO (United States); Peter, Gary F. [School of Forest Resources and Conservation, University of Florida, Gainesville, FL (United States); Davis, Mark [National Bioenergy Center, National Renewable Energy Laboratory, Golden, CO (United States)

    2016-01-25

    Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts from the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. Diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.

  5. Comparative analysis of different methods of extraction of present hydrocarbons in industrial residual waters

    International Nuclear Information System (INIS)

    Santa, Judith Rocio; Serrano, Martin; Stashenko, Elena

    2002-01-01

    A comparison among four extraction techniques such as: liquid - liquid (LLE) continuous and for lots, solid phase extraction (SPE), solid phase micro extraction (SPME) and static headspace (S-HS) was carried out. The main purpose of this research was to determine the highest recovery efficiencies and how reproducible the tests are while varying parameters such as time, extraction technique, type of solvents and others. Chromatographic parameters were optimized in order to carry out the analyses. Hydrocarbon's quantification of residual waters was achieved by using a high-resolution gas chromatography with a gas flame ionization detector (HRGC-FID). Validation of the method was carried out by analyzing real samples taken in different sampling places of the residual waters treatment plant of Ecopetrol - Barrancabermeja. The use of extraction methods that require big solvent quantities and long time for analysis are losing validity day by day. Techniques such as the HS-SPME and static HS are offered as alternatives for quantifying hydrocarbons. They show total lack of solvents, high sensibility, selectivity and the techniques are reproducible. Solid phase micro extraction (SPME) and static headspace (static HS) techniques were chosen as the extraction techniques to validate the method in real samples. Both techniques showed similar results for the determination of total hydrocarbons (in the gasoline range)

  6. Determination of Terpenoid Content in Pine by Organic Solvent Extraction and Fast-GC Analysis

    International Nuclear Information System (INIS)

    Harman-Ware, Anne E.; Sykes, Robert; Peter, Gary F.; Davis, Mark

    2016-01-01

    Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts from the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. Diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.

  7. SCREENING OF PLANT EXTRACTS FOR ANTIMICROBIAL ACTIVITY AGAINST BACTERIA

    Directory of Open Access Journals (Sweden)

    Alexander Vatľák

    2014-02-01

    Full Text Available The aim of this study was antimicrobial action of the methanolic extracts of Equisetum arvense L. and Urtica dioica L. against gramnegative and grampositive bacteria. The antimicrobial activities of the extracts against gramnegative bacteria: Escherichia coli CCM 3988, Listeria ivanovii CCM 5884, Listeria innocua CCM 4030, Pseudomonas aeruginosa CCM 1960, Serratia rubidaea CCM 4684 and grampositive bacteria: Brochothrix thermosphacta CCM 4769, Enterococcus raffinosus CCM 4216, Lactobacillus rhamnosus CCM 1828, Paenobacillus larvae CCM 4483 and Staphylococcus epidermis CCM 4418 were determined by the disc diffusion method and the microbroth dilution method according to CLSI. Probit analysis was used in this experiment. Of the 2 plant extracts tested, all extracts showed antimicrobial activity against one or more species of microorganisms. The most antimicrobial activity showed methanolic plant extract of E. arvense against S. epidermis with disc diffusion method and with microbroth dilution method against S. rubidaea and plant extract Urtica dioica with disc diffusion method against P. aeruginosa and with microbroth dilution method against S. rubidaea and E. coli.

  8. Double-phase liquid membrane extraction for the analysis of pesticides

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Nurul Auni Zainal Abidin; Heng, See Hong; Wan Aini Wan Ibrahim

    2008-01-01

    A simple and solvent minimized sample preparation technique based on two-phase hollow fiber-protected liquid-phase micro extraction was investigated for HPLC analysis of selected pesticides in water samples. Four pesticides (procymidon, methidathion, quinalphos, and vinclozolin) were considered as target analysts. Parameters such as extraction solvent, salt concentration, stirring speed, extraction time, and pH value were optimized using spiked deionised water samples. The analysts were extracted from 12 mL water samples through organic solvent (n-hexane and isooctane) immobilized in the pores of a porous polypropylene hollow fiber into 50 μL acceptor phase present inside the hollow fiber. Excellent separations of analytes were obtained on C18 column using acetonitrile-water ratio of 55:45 v/v at elevated flow rate of 0.8 mL/ min. (author)

  9. Investigation of actinide extraction by calixarenes. Application to radio-toxicological analysis

    International Nuclear Information System (INIS)

    Dinse, Christelle

    1999-01-01

    As measurement of uranium in urine is one of the controls performed for a dosimetric survey of workers exposed to risk of internal contamination, this research thesis aimed at the selection of a new ligand able to selectively extract uranium (even traces of uranium) from urine. Optimal extraction conditions have been achieved and an analysis protocol has been proposed. A calixarene compound comprising three carboxylic functions has been chosen as selective ligand for the uranyl ion. Extraction properties of this calixarene have been studied in a two phase system. The influence of complexing anions generally present in urines (such as chloride, sulphate or phosphate ions) has been assessed. This protocol allows uranium to be isolated in a more repeatable, while simpler and quicker way. Moreover, after de-extraction, uranium measurement can be quickly performed by ICP-MS (Inductively Coupled Plasma - Mass Spectrometry) [fr

  10. Extraction and Analysis of Gigantol from Dendrobium officinale with Response Surface Methodology

    Directory of Open Access Journals (Sweden)

    Siyan Zheng

    2018-04-01

    Full Text Available In order to optimize the extraction of gigantol from Dendrobium officinale, the influence of methanol concentration, ultrasonic temperature, and liquid ratio on extraction efficiency was analysed by the response surface analysis method. The results show that the extraction rate reached a maximum when the methanol concentration was 92.98%, the solid-liquid ratio was 27.2 mL/g, and the extraction temperature was 41.41 °C. The content of gigantol of Dendrobium officinale in leaves was significantly higher than that in stems, reaching 4.7942 μg/g. The content of gigantol in Dendrobium huoshanensis Fengdou was significantly higher than that of other species of Fengdou. This experiment has practical significance for improving the utilization rate of Dendrobium officinale, and provides a reference for the study of the pharmacological and biological activity of gigantol.

  11. Automatic knowledge extraction in sequencing analysis with multiagent system and grid computing.

    Science.gov (United States)

    González, Roberto; Zato, Carolina; Benito, Rocío; Bajo, Javier; Hernández, Jesús M; De Paz, Juan F; Vera, Vicente; Corchado, Juan M

    2012-12-01

    Advances in bioinformatics have contributed towards a significant increase in available information. Information analysis requires the use of distributed computing systems to best engage the process of data analysis. This study proposes a multiagent system that incorporates grid technology to facilitate distributed data analysis by dynamically incorporating the roles associated to each specific case study. The system was applied to genetic sequencing data to extract relevant information about insertions, deletions or polymorphisms.

  12. Automatic knowledge extraction in sequencing analysis with multiagent system and grid computing

    Directory of Open Access Journals (Sweden)

    González Roberto

    2012-12-01

    Full Text Available Advances in bioinformatics have contributed towards a significant increase in available information. Information analysis requires the use of distributed computing systems to best engage the process of data analysis. This study proposes a multiagent system that incorporates grid technology to facilitate distributed data analysis by dynamically incorporating the roles associated to each specific case study. The system was applied to genetic sequencing data to extract relevant information about insertions, deletions or polymorphisms.

  13. Buffer erosion in dilute groundwater

    International Nuclear Information System (INIS)

    Schatz, T.; Kanerva, N.; Martikainen, J.; Sane, P.; Olin, M.; Seppaelae, A.; Koskinen, K.

    2013-08-01

    One scenario of interest for repository safety assessment involves the loss of bentonite buffer material in contact with dilute groundwater flowing through a transmissive fracture interface. In order to examine the extrusion/erosion behavior of bentonite buffer material under such circumstances, a series of experiments were performed in a flow-through, 1 mm aperture, artificial fracture system. These experiments covered a range of solution chemistry (salt concentration and composition), material composition (sodium montmorillonite and admixtures with calcium montmorillonite), and flow velocity conditions. No erosion was observed for sodium montmorillonite against solution compositions from 0.5 g/L to 10 g/L NaCl. No erosion was observed for 50/50 calcium/sodium montmorillonite against 0.5 g/L NaCl. Erosion was observed for both sodium montmorillonite and 50/50 calcium/sodium montmorillonite against solution compositions ≤ 0.25 g/L NaCl. The calculated erosion rates for the tests with the highest levels of measured erosion, i.e., the tests run under the most dilute conditions (ionic strength (IS) < ∼1 mM), were well-correlated to flow velocity, whereas the calculated erosion rates for the tests with lower levels of measured erosion, i.e., the tests run under somewhat less dilute conditions (∼1 mM < IS < ∼4 mM), were not similarly correlated indicating that material and solution composition can significantly affect erosion rates. In every experiment, both erosive and non-erosive, emplaced buffer material extruded into the fracture and was observed to be impermeable to water flowing in the fracture effectively forming an extended diffusive barrier around the intersecting fracture/buffer interface. Additionally, a model which was developed previously to predict the rate of erosion of bentonite buffer material in low ionic strength water in rock fracture environments was applied to three different cases: sodium montmorillonite expansion in a vertical tube, a

  14. Screening for Antibacterial and Antioxidant Activities and Phytochemical Analysis of Oroxylum indicum Fruit Extracts.

    Science.gov (United States)

    Sithisarn, Patchima; Nantateerapong, Petcharat; Rojsanga, Piyanuch; Sithisarn, Pongtip

    2016-04-07

    Oroxylum indicum, which is called Pheka in Thai, is a traditional Thai plant in the Bignoniaceae family with various ethnomedical uses such as as an astringent, an anti-inflammatory agent, an anti-bronchitic agent, an anti-helminthic agent and an anti-microbial agent. The young fruits of this plant have also been consumed as vegetables. However, there has been no report concerning its antibacterial activities, especially activities related to clinically isolated pathogenic bacteria and the in vitro antioxidant effects of this plant. Therefore, the extracts from O. indicum fruits and seeds collected from different provinces in Thailand were prepared by decoction and maceration with ethanol and determined for their in vitro antibacterial effects on two clinically isolated bacteria, Streptococcus suis and Staphylococcus intermedius, using disc diffusion assay. Ethanol extracts from O. indicum fruits collected from Nakorn Pathom province at the concentration of 1000 mg/mL exhibited intermediate antibacterial activity against S. intermedius with an inhibition zone of 15.11 mm. Moreover, it promoted moderate inhibitory effects on S. suis with an inhibition zone of 14.39 mm. The extracts prepared by maceration with ethanol promoted higher antibacterial activities than those prepared with water. The ethanol extract from the seeds of this plant, purchased in Bangkok, showed stronger in vitro antioxidant activities than the other extracts, with an EC50 value of 26.33 µg/mL. Phytochemical analysis suggested that the seed ethanol extract contained the highest total phenolic and flavonoid contents (10.66 g% gallic acid equivalent and 7.16 g% quercetin equivalent, respectively) by a significant amount. Thin layer chromatographic analysis of the extracts showed the chromatographic band that could correspond to a flavonoid baicalein. From the results, extracts from O. indicum fruits have an in vitro antioxidant effect, with antibacterial potential, on clinically pathologic

  15. Use of solvent mixtures for total lipid extraction of Chlorella vulgaris and gas chromatography FAME analysis.

    Science.gov (United States)

    Moradi-Kheibari, Narges; Ahmadzadeh, Hossein; Hosseini, Majid

    2017-09-01

    Lipid extraction is the bottleneck step for algae-based biodiesel production. Herein, 12 solvent mixture systems (mixtures of three non-polar and two polar organic solvents) were examined to evaluate their effects on the total lipid yield from Chlorella vulgaris (C. vulgaris). Moreover, the extraction yields of three solvent systems with maximum extraction efficiency of esterifiable lipids were determined by acidic transesterification and GC-FID analysis. Three solvent systems, which resulted in a higher extraction yield, were further subjected to fatty acid methyl ester (FAME) analysis. The total lipid extraction yields (based on dry biomass) were (38.57 ± 1.51), (25.33 ± 0.58), and (25.17 ± 1.14) %, for chloroform-methanol (1:2) (C1M2), hexane-methanol (1:2) (H1M2), and chloroform-methanol (2:1) (C2M1), respectively. The extraction efficiency of C1M2 was approximately 1.5 times higher than H1M2 and C2M1, whereas the FAME profile of extracted lipids by H1M2 and C1M2 were almost identical. Moreover, the esterifiable lipid extraction yields of (18.14 ± 2.60), (16.66 ± 0.35), and (13.22 ± 0.31) % (based on dry biomass) were obtained for C1M2, H1M2, and C2M1 solvent mixture systems, respectively. The biodiesel fuel properties produced from C. vulgaris were empirically predicted and compared to that of the EN 14214 and ASTM 6751 standard specifications.

  16. Analysis of Benzo[a]pyrene in Vegetable Oils Using Molecularly Imprinted Solid Phase Extraction (MISPE Coupled with Enzyme-Linked Immunosorbent Assay (ELISA

    Directory of Open Access Journals (Sweden)

    Michael Pschenitza

    2014-05-01

    Full Text Available This paper describes the development of a molecularly imprinted polymer-based solid phase extraction (MISPE method coupled with enzyme-linked immunosorbent assay (ELISA for determination of the PAH benzo[a]pyrene (B[a]P in vegetable oils. Different molecularly imprinted polymers (MIPs were prepared using non-covalent 4-vinylpyridine/divinylbenzene co-polymerization at different ratios and dichloromethane as porogen. Imprinting was done with a template mixture of phenanthrene and pyrene yielding a broad-specific polymer for PAHs with a maximum binding capacity (Q of ~32 μg B[a]P per 50 mg of polymer. The vegetable oil/n-hexane mixture (1:1, (v/v was pre-extracted with acetonitrile, the solvent evaporated, the residue reconstituted in n-hexane and subjected to MISPE. The successive washing with n-hexane and isopropanol revealed most suitable to remove lipid matrix constituents. After elution of bound PAHs from MISPE column with dichloromethane, the solvent was evaporated, the residue reconstituted with dimethyl sulfoxide and diluted 100-fold with methanol/water (10:90, (v/v for analysis of B[a]P equivalents with an ELISA. The B[a]P recovery rates in spiked vegetable oil samples of different fatty acid composition were determined between 63% and 114%. The presence of multiple PAHs in the oil sample, because of MIP selectivity and cross-reactivity of the ELISA, could yield overestimated B[a]P values.

  17. Desynchronization in diluted neural networks

    International Nuclear Information System (INIS)

    Zillmer, Ruediger; Livi, Roberto; Politi, Antonio; Torcini, Alessandro

    2006-01-01

    The dynamical behavior of a weakly diluted fully inhibitory network of pulse-coupled spiking neurons is investigated. Upon increasing the coupling strength, a transition from regular to stochasticlike regime is observed. In the weak-coupling phase, a periodic dynamics is rapidly approached, with all neurons firing with the same rate and mutually phase locked. The strong-coupling phase is characterized by an irregular pattern, even though the maximum Lyapunov exponent is negative. The paradox is solved by drawing an analogy with the phenomenon of 'stable chaos', i.e., by observing that the stochasticlike behavior is 'limited' to an exponentially long (with the system size) transient. Remarkably, the transient dynamics turns out to be stationary

  18. A compact rotating dilution refrigerator

    Science.gov (United States)

    Fear, M. J.; Walmsley, P. M.; Chorlton, D. A.; Zmeev, D. E.; Gillott, S. J.; Sellers, M. C.; Richardson, P. P.; Agrawal, H.; Batey, G.; Golov, A. I.

    2013-10-01

    We describe the design and performance of a new rotating dilution refrigerator that will primarily be used for investigating the dynamics of quantized vortices in superfluid 4He. All equipment required to operate the refrigerator and perform experimental measurements is mounted on two synchronously driven, but mechanically decoupled, rotating carousels. The design allows for relative simplicity of operation and maintenance and occupies a minimal amount of space in the laboratory. Only two connections between the laboratory and rotating frames are required for the transmission of electrical power and helium gas recovery. Measurements on the stability of rotation show that rotation is smooth to around 10-3 rad s-1 up to angular velocities in excess of 2.5 rad s-1. The behavior of a high-Q mechanical resonator during rapid changes in rotation has also been investigated.

  19. Quantifying the dilution effect for models in ecological epidemiology.

    Science.gov (United States)

    Roberts, M G; Heesterbeek, J A P

    2018-03-01

    The dilution effect , where an increase in biodiversity results in a reduction in the prevalence of an infectious disease, has been the subject of speculation and controversy. Conversely, an amplification effect occurs when increased biodiversity is related to an increase in prevalence. We explore the conditions under which these effects arise, using multi species compartmental models that integrate ecological and epidemiological interactions. We introduce three potential metrics for quantifying dilution and amplification, one based on infection prevalence in a focal host species, one based on the size of the infected subpopulation of that species and one based on the basic reproduction number. We introduce our approach in the simplest epidemiological setting with two species, and show that the existence and strength of a dilution effect is influenced strongly by the choices made to describe the system and the metric used to gauge the effect. We show that our method can be generalized to any number of species and to more complicated ecological and epidemiological dynamics. Our method allows a rigorous analysis of ecological systems where dilution effects have been postulated, and contributes to future progress in understanding the phenomenon of dilution in the context of infectious disease dynamics and infection risk. © 2018 The Author(s).

  20. Quantitative spatial analysis of the mouse brain lipidome by pressurized liquid extraction surface analysis

    DEFF Research Database (Denmark)

    Almeida, Reinaldo; Berzina, Zane; Christensen, Eva Arnspang

    2015-01-01

    extracted directly from tissue sections. PLESA uses a sealed and pressurized sampling probe that enables the use of chloroform-containing extraction solvents for efficient in situ lipid microextraction with a spatial resolution of 400 μm. Quantification of lipid species is achieved by the inclusion...

  1. FY12 Final Report for PL10-Mod Separations-PD12: Electrochemically Modulated Separation of Plutonium from Dilute and Concentrated Dissolver Solutions for Analysis by Gamma Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Pratt, Sandra H.; Arrigo, Leah M.; Duckworth, Douglas C.; Cloutier, Janet M.; Breshears, Andrew T.; Schwantes, Jon M.

    2013-05-01

    Accurate and timely analysis of plutonium in spent nuclear fuel is critical in nuclear safeguards for detection of both protracted and rapid plutonium diversions. Gamma spectroscopy is a viable method for accurate and timely measurements of plutonium provided that the plutonium is well separated from the interfering fission and activation products present in spent nuclear fuel. Electrochemically modulated separation (EMS) is a method that has been used successfully to isolate picogram amounts of Pu from nitric acid matrices. With EMS, Pu adsorption may be turned “on” and “off” depending on the applied voltage, allowing for collection and stripping of Pu without the addition of chemical reagents. In this work, we have scaled up the EMS process to isolate microgram quantities of Pu from matrices encountered in spent nuclear fuel during reprocessing. Several challenges have been addressed including surface area limitations, radiolysis effects, electrochemical cell performance stability, and chemical interferences. After these challenges were resolved, 6 µg Pu was deposited in the electrochemical cell with approximately an 800-fold reduction of fission and activation product levels from a spent nuclear fuel sample. Modeling showed that these levels of Pu collection and interference reduction may not be sufficient for Pu detection by gamma spectroscopy. The main remaining challenges are to achieve a more complete Pu isolation and to deposit larger quantities of Pu for successful gamma analysis of Pu. If gamma analyses of Pu are successful, EMS will allow for accurate and timely on-site analysis for enhanced Pu safeguards.

  2. Solvent. I. Extraction systems applied to uranium analysis. I. Extraction studies with Tributyl phosphate-Methyl-isobutyl-ketone

    International Nuclear Information System (INIS)

    Vera Palomino, J.; Palomares Delgado, F.; Petrement Eguiluz, J. C.

    1964-01-01

    A factorial study of the selective extraction of uranium with a mixture of TBP-MIC was carried out using 0,8 N nitric acid and different salting agents. We use the most suitable salting agent to develop new factorial experiments in order to get an equation involving the percent of extracted uranium, E, the concentration of the extraction agent in the organic phase, c, and the concentration of the slating agent in the aqueous phase, n. (Author) 3 refs

  3. Application of crown ethers to selective extraction and quantitative analysis of technetium 99, iodine 129 and cesium 135 in effluents

    International Nuclear Information System (INIS)

    Paviet, P.

    1992-01-01

    Properties of crown ethers are first recalled. Then extraction of technetium 99 is studied in actual radioactive effluents. Quantitative analysis is carried out by liquid scintillation and interference of tritium is corrected. Iodine 129 is extracted from radioactive effluents and determined by gamma spectrometry. Finally cesium 135 is extracted and determined by thermo ionization mass spectroscopy

  4. Solvent-extraction methods applied to the chemical analysis of uranium. III. Study of the extraction with inert solvents

    International Nuclear Information System (INIS)

    Vera Palomino, J.; Palomares Delgado, F.; Petrement Eguiluz, J. C.

    1964-01-01

    The extraction of uranium on the trace level is studied by using tributylphosphate as active agent under conditions aiming the attainment of quantitative extraction by means of a single step process using a number of salting-out agents and keeping inside the general lines as reported in two precedent papers. Two inert solvents were investigated, benzene and cyclohexane, which allowed to derive the corresponding empirical equations describing the extraction process and the results obtained were compared with those previously reported for solvents which, like ethyl acetate and methylisobuthylketone, favour to a more or less extend the extraction of uranium. (Author) 4 refs

  5. Mechanisms of urine concentration and dilution (1961)

    International Nuclear Information System (INIS)

    Morel, F.; Guinnebault, M.

    1961-01-01

    This paper is devoted to the analysis of a problem in the field of renal physiology which has shown many new developments during the course of the last few years. The following are treated successively: a) the data obtained from measurements of free water clearance and their interpretation; b) the data provided by nephron morphology and the comparative anatomy of the kidney ; c) the data relative to the existence of an intrarenal osmotic gradient; d) the principle of concentration multiplication by a counter current technique; e) the present day theory of counter current concentration of urine, and f) the physiological check on dilution and concentration mechanisms in urine. Lastly, the advantages of the modern theory and the unknown factors which remain are discussed. (authors) [fr

  6. Headspace Solid Phase Microextraction in Pesticide Residues Analysis:1. Optimisation of Extraction Conditions

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2007-01-01

    Full Text Available The method of headspace solid phase microextraction (HS/SPME was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB, tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurementswere performed using a nonpolar polydimethyl siloxane (PDMS fiber. Detection and quantification were done by gas chromatography/mass spectrometry (GC/MS.Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature.Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB, 0.05-25 ng/ml (tefluthrin, 0.05-40 ng/ml (heptachlor, 0.05-40 ng/ml (aldrin, 0.05-25 ng/ml (chlorpyrifos, 0.05-25 ng/ml (fenthionand 0.05-25 ng/ml (bifenthrin.Relative standard deviation (RSD values for triplicate measurements did not exceed 15%.

  7. Process analysis and modeling of a single-step lutein extraction method for wet microalgae.

    Science.gov (United States)

    Gong, Mengyue; Wang, Yuruihan; Bassi, Amarjeet

    2017-11-01

    Lutein is a commercial carotenoid with potential health benefits. Microalgae are alternative sources for the lutein production in comparison to conventional approaches using marigold flowers. In this study, a process analysis of a single-step simultaneous extraction, saponification, and primary purification process for free lutein production from wet microalgae biomass was carried out. The feasibility of binary solvent mixtures for wet biomass extraction was successfully demonstrated, and the extraction kinetics of lutein from chloroplast in microalgae were first evaluated. The effects of types of organic solvent, solvent polarity, cell disruption method, and alkali and solvent usage on lutein yields were examined. A mathematical model based on Fick's second law of diffusion was applied to model the experimental data. The mass transfer coefficients were used to estimate the extraction rates. The extraction rate was found more significantly related with alkali ratio to solvent than to biomass. The best conditions for extraction efficiency were found to be pre-treatment with ultrasonication at 0.5 s working cycle per second, react 0.5 h in 0.27 L/g solvent to biomass ratio, and 1:3 ether/ethanol (v/v) with 1.25 g KOH/L. The entire process can be controlled within 1 h and yield over 8 mg/g lutein, which is more economical for scale-up.

  8. Analysis of the essential oils of Alpiniae Officinarum Hance in different extraction methods

    Science.gov (United States)

    Yuan, Y.; Lin, L. J.; Huang, X. B.; Li, J. H.

    2017-09-01

    It was developed for the analysis of the essential oils of Alpiniae Officinarum Hance extracted by steam distillation (SD), ultrasonic assisted solvent extraction (UAE) and supercritical fluid extraction (SFE) via gas chromatography mass spectrometry (GC-MS) combined with retention index (RI) method. There were multiple volatile components of the oils extracted by the three above-mention methods respectively identified; meanwhile, each one was quantified by area normalization method. The results indicated that the content of 1,8-Cineole, the index constituent, by SD was similar as SFE, and higher than UAE. Although UAE was less time consuming and consumed less energy, the oil quality was poorer due to the use of organic solvents was hard to degrade. In addition, some constituents could be obtained by SFE but could not by SD. In conclusion, essential oil of different extraction methods from the same batch of materials had been proved broadly similarly, however, there were some differences in composition and component ratio. Therefore, development and utilization of different extraction methods must be selected according to the functional requirements of products.

  9. Determination of photooxygenation products of rotenone with isotope dilution method

    International Nuclear Information System (INIS)

    Chubachi, Mitsuo; Hamada, Masayuki

    1975-01-01

    When rotenone dissolved in certain solvent was photochemically oxidized, rotenolones, dehydrorotenone and rotenonone were obtained as main products. In order to determine the quantitative yields of these compounds in photooxygenation products, four compounds mentioned above were labeled with carbon-14 and the isotope dilution method by these labeled compounds was applied to the product analysis. (auth.)

  10. Inhibition Effect of Deanol on Mild Steel Corrosion in Dilute ...

    African Journals Online (AJOL)

    The influence of deanol on the corrosion behaviour of mild steel in dilute sulphuric acid with sodium chloride addition was studied by means of mass-loss, potentiodynamic polarization, electrode potential monitoring, scanning electron microscopy and statistical analysis. Results show that deanol performed excellently with ...

  11. Phytochemical Analysis, Identification and Quantification of Antibacterial Active Compounds in Betel Leaves, Piper betle Methanolic Extract.

    Science.gov (United States)

    Syahidah, A; Saad, C R; Hassan, M D; Rukayadi, Y; Norazian, M H; Kamarudin, M S

    2017-01-01

    The problems of bacterial diseases in aquaculture are primarily controlled by antibiotics. Medicinal plants and herbs which are seemed to be candidates of replacements for conventional antibiotics have therefore gained increasing interest. Current study was performed to investigate the presence of phytochemical constituents, antibacterial activities and composition of antibacterial active compounds in methanolic extract of local herb, Piper betle . Qualitative phytochemical analysis was firstly carried out to determine the possible active compounds in P. betle leaves methanolic extract. The antibacterial activities of major compounds from this extract against nine fish pathogenic bacteria were then assessed using TLC-bioautography agar overlay assay and their quantity were determined simultaneously by HPLC method. The use of methanol has proved to be successful in extracting numerous bioactive compounds including antibacterial compounds. The TLC-bioautography assay revealed the inhibitory action of two compounds which were identified as hydroxychavicol and eugenol. The $-caryophyllene however was totally inactive against all the tested bacterial species. In this study, the concentration of hydroxychavicol in extract was found to be 374.72±2.79 mg g-1, while eugenol was 49.67±0.16 mg g-1. Based on these findings, it could be concluded that hydroxychavicol and eugenol were the responsible compounds for the promising antibacterial activity of P. betle leaves methanolic extract. This inhibitory action has significantly correlated with the amount of the compounds in extract. Due to its potential, the extract of P. betle leaves or it compounds can be alternative source of potent natural antibacterial agents for aquaculture disease management.

  12. Environmental analysis of raw cork extraction in cork oak forests in southern Europe (Catalonia--Spain).

    Science.gov (United States)

    Rives, Jesús; Fernandez-Rodriguez, Ivan; Rieradevall, Joan; Gabarrell, Xavier

    2012-11-15

    Cork oak grows endemically in a narrow region bordering the western Mediterranean, and especially in the Iberian Peninsula. The importance of cork agro-forestry systems lies in the fact that a natural and renewable raw material - cork - can be extracted sustainably without endangering the tree or affecting biodiversity. This paper describes an environmental analysis of the extraction of raw cork in cork oak forests in Catalonia, using data from five representative local forest exploitations. The evaluation was carried out using life cycle assessment (LCA) methodology, and all the forestry management required to obtain a tonne of raw cork was included. The aim of the study was to evaluate the environmental impacts - in terms of global warming, acidification, eutrophication, human toxicity, and so on - caused by cork extraction and determine the carbon dioxide balance of these forestry systems, with a tree lifespan of about 200 years. During the life cycle extraction of cork in Catalonia, 0.2 kg of CO(2) eq. was emitted per kg of raw cork extracted. Moreover, cork cannot be extracted without the tree, which will be fixing carbon dioxide throughout its technological useful life (200 years), despite the fact that the bark is removed periodically: every 13-14 years. If the emission from extraction and the carbon contained in the material is discounted, the carbon dioxide balance indicates that 18 kg of CO(2) are fixed per kg of raw cork extracted. Therefore, cork is a natural, renewable and local material that can replace other non-renewable materials, at local level, to reduce the environmental impacts of products, and particularly to reduce their carbon footprint. Copyright © 2012 Elsevier Ltd. All rights reserved.

  13. Phytochemical screening and analysis of antioxidant properties of aqueous extract of wheatgrass.

    Science.gov (United States)

    Durairaj, Varalakshmi; Hoda, Muddasarul; Shakya, Garima; Babu, Sankar Pajaniradje Preedia; Rajagopalan, Rukkumani

    2014-09-01

    To screen the phytochemical constituents and study antioxidant properties of the aqueous extract of the wheatgrass. The current study was focused on broad parameters namely, phytochemical analysis, gas chromatography-mass spectrometry analysis and antioxidant properties in order to characterize the aqueous extract of wheatgrass as a potential free radical quencher. The phytochemical screening of the aqueous extract of wheatgrass showed the presence of various secondary metabolites but the absence of sterols and quinone in general. Wheatgrass was proved to be an effective radical scavenger in all antioxidant assays. The gas chromatography-mass spectrometry analysis confirmed the presence of diverse category of bioactive compounds such as squalene, caryophyllene and amyrins in varying percentage. From the results obtained, we conclude that wheatgrass aqueous extract contains various effective compounds. It is a potential source of natural antioxidants. Further analysis of this herb will help in finding new effective compounds which can be of potent use in pharmacological field. Copyright © 2014 Hainan Medical College. Published by Elsevier B.V. All rights reserved.

  14. Extracting topographic structure from digital elevation data for geographic information-system analysis

    Science.gov (United States)

    Jenson, Susan K.; Domingue, Julia O.

    1988-01-01

    Software tools have been developed at the U.S. Geological Survey's EROS Data Center to extract topographic structure and to delineate watersheds and overland flow paths from digital elevation models. The tools are specialpurpose FORTRAN programs interfaced with general-purpose raster and vector spatial analysis and relational data base management packages.

  15. Preliminary analysis of proton magnetic resonance 1D spectra of cerebrospinal fluid and brain cancer extracts

    International Nuclear Information System (INIS)

    Toczylowska, B.; Jozwik, A.; Kierul, K.; Matysiak, Z.; Sidor, M.; Wojcik, J.

    1999-01-01

    In series of cerebrospinal fluid samples from 25 patients proton spectra of magnetic resonance were measured. The spectra were measured also for series of brain tumor tissue extracts received from another 25 patients. This paper presents an attempt to apply statistical methods of image recognition for spectra analysis of the two measured series

  16. Regularized generalized eigen-decomposition with applications to sparse supervised feature extraction and sparse discriminant analysis

    DEFF Research Database (Denmark)

    Han, Xixuan; Clemmensen, Line Katrine Harder

    2015-01-01

    We propose a general technique for obtaining sparse solutions to generalized eigenvalue problems, and call it Regularized Generalized Eigen-Decomposition (RGED). For decades, Fisher's discriminant criterion has been applied in supervised feature extraction and discriminant analysis, and it is for...

  17. Ecological observations and GC-MS analysis of methanolic extract of Sacoglossan Elysia bangtawaensis (Swennen)

    Digital Repository Service at National Institute of Oceanography (India)

    Shenai-Tirodkar, P.S.; Desai, N.M.; Jagtap, T.G.

    H and temperature (air and water). Moreover, GC-MS analysis of methanolic extract of E. bangtawaensis showed major constituents of fatty acids such as myristic acid, oleic acid, stearic acid, arachidic acid, etc. The presence of such bioactive compounds (identified...

  18. Chemical analysis and quality control of Ginkgo biloba leaves, extracts, and phytopharmaceuticals

    NARCIS (Netherlands)

    Beek, van T.A.; Montoro, P.

    2009-01-01

    The chemical analysis and quality control of Ginkgo leaves, extracts, phytopharmaceuticals and some herbal supplements is comprehensively reviewed. The review is an update of a similar, earlier review in this journal [T.A. van Beek, J. Chromatogr. A 967 (2002) 21¿55]. Since 2001 over 3000 papers on

  19. Analysis of Fluorotelomer Alcohols in Soils: Optimization of Extraction and Chromatography

    Science.gov (United States)

    This article describes the development of an analytical method for the determination of fluorotelomer alcohols (FTOHs) in soil. The sensitive and selective determination of the telomer alcohols was performed by extraction with mthyl tert-butyl ether (MTBE) and analysis of the ext...

  20. Extraction and analysis of 14C-carbofuran radioactivity in soil sample

    International Nuclear Information System (INIS)

    Maizatul Akmam Mhd Nasir; Nashriyah Mat

    2005-01-01

    Carbofuran insecticide or nematicide sprayed onto soil in the agroecosystem will be taken up by plant. Carbofuran residue will pollute the environment and organisms in the food chain. Extraction and analysis of 14 C-carbofuran in soil from lysimeter were carried out. The Liquid Scintillation Counter (LSC) was used to measure radioactivity of 14 C-carbofuran in soil sample. (Author)

  1. Preliminary design and analysis of a process for the extraction of lithium from seawater

    International Nuclear Information System (INIS)

    Steinberg, M.; Dang, V.D.

    1975-09-01

    The U.S. demand for lithium by the industrial sector and by a fusion power economy in the future is discussed. For a one million MW(e) CTR (D-T fuel cycle) economy, growing into the beginning of the next century (the years 2000 to 2030), the cumulative demand for lithium is estimated to range from (0.55 to 4.7) x 10 7 to 1.0 x 10 9 kg. Present estimates of the available U.S. supply are 6.9 x 10 8 kg of lithium from mineral resources and 4.0 x 10 9 kg of lithium from concentrated natural brines. There is, however, a vast supply of lithium in seawater: 2.5 x 10 14 kg. A preliminary process design for the extraction of lithium from seawater is presented: seawater is first evaporated by solar energy to increase the concentration of lithium and to decrease the concentration of other cations in the bittern which then passes into a Dowex-50 ion exchange bed for cation adsorption. Lithium ions are then eluted with dilute hydrochloric acid forming an aqueous lithium chloride which is subsequently concentrated and electrolyzed. The energy requirement for lithium extraction varies between 0.08 and 2.46 kWh(e)/gm for a range of production rates varying between 10 4 and 10 8 kg/y; this is small compared to the energy produced from the use of lithium in a CTR having a value of 3400 kWh(e)/g Li. Production cost of the process is estimated to be in the range of 2.2 to 3.2 cents/g Li. As a basis for the process design, it is recommended that a phase equilibria study of the solid--liquid crystallization processes of seawater be conducted. Uncertainties exist in the operation of large solar ponds for concentrating large quantities of seawater. A search for a highly selective adsorbent or extractant for Li from low concentration aqueous solutions should be made. Other physical separation processes such as using membranes should be investigated. 9 tables

  2. Isotope dilution mass spectrometry as the primary method of measurement for the amount of matter. Application to cadmium determination in biological materials and comparison with instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Munoz, Luis; Gras, Nuri; Quejido, Alberto; Ferrada, Carlos

    2001-01-01

    A primary method of measurement as defined by the Consultative Committee on the Quantity of Matter (Comite Consultatif pour la Quantite de Matiere, CCQM) of the International Bureau of Weights and Measurements (Bureau International des Poids et Mesures, BIPM), is one whose measurement process is perfectly known, has valid theoretical foundations and is fully described and answers to an equation that relates what is measured with what is intended to be measured without any significant empirical correction factors. It is also a method that has insignificant systematic errors, where only magnitudes from the International System of Units (SI) are used and where, preferably, the uncertainties are small ones. They are, therefore, procedures that do not need instrumental calibration. The absolute methods of measurement allow a chain of traceability to be formed between the result obtained and the magnitude of the SI assigned to what is measured. So the results are said to be traceable to the SI. One of the methods that meets these requirements and is recognized as the primary method by the CCQM is Isotope Dilution Mass Spectrometry (IDMS). Through a project of Technical Cooperation with the International Atomic Energy Agency in the area of Chemical Metrology, the CCHEN obtained training in CIEMAT, Spain, in IDMS and its applications to the analysis of biological samples. This work describes the first experience carried out entirely in Chilean laboratories, applying IDMS to the determination of cadmium in the biological reference materials Oyster Tissue 15566-A from the NIST, United States, Dogfish Liver, DOLT-2 from the NRC-CNRC, Canada and Poplar Leaves GBW07604 from the NRCC, China. The samples were traced with an isotope enriched spike 111 Cd and then shaken to obtain the isotopic exchange. Once dissolved, the isotopic relationship 111 Cd/ 114 Cd was determined in the samples using mass spectrometry with plasma source. These results were compared with those obtained

  3. Studies on the dilution behaviour of effluent discharged into the CCW channel at KGS

    International Nuclear Information System (INIS)

    Sivasubramanian, K.; Srinivasan, S.; Ponraju, D.; Meenakshisundaram, V.; Munusamy, N.

    2003-01-01

    The dilution behaviour of the liquid effluent discharged into condenser cooling water channel of Kaiga Power Plant has been studied using salt addition and dye addition methods. Dilution factors determined experimentally showed that the discharged liquid effluent gets thoroughly mixed with stream of water at the weir and further diluted in the down stream. This paper describes both salt and dye addition methods for determining the dilution factor. The velocity of the stream at various locations were measured and compared with reported values. The selection of representative sampling point for routine analysis of water was identified from this experiment. (author)

  4. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry (French Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  5. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry (Spanish Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  6. Selective extraction of phospholipids from dairy products by micro-solid phase extraction based on titanium dioxide microcolumns followed by MALDI-TOF-MS analysis

    DEFF Research Database (Denmark)

    Calvano, Cosima; Jensen, Ole; Zambonin, Carlo

    2009-01-01

    A new micro-solid phase extraction (micro-SPE) procedure based on titanium dioxide microcolumns was developed for the selective extraction of phospholipids (PLs) from dairy products before matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) analysis. All...... the extraction steps (loading, washing, and elution) have been optimized using a synthetic mixture of PLs standard and the procedure was subsequently applied to food samples such as milk, chocolate milk and butter. The whole method demonstrated to be simpler than traditional approaches and it appears very...

  7. Study of the Qualitative and Semi-quantitative Analysis of Grape Seed Extract by HPLC

    OpenAIRE

    Sorolla, Sílvia; Flores, Antònia; Canals Parelló, Trini; Cantero Gómez, María Rosa; Font Vallès, Joaquim; Ollé Otero, Lluís; Bacardit Dalmases, Anna

    2018-01-01

    The main aim of this study is to carry out a qualitative and semiquantitative analysis of tannin extracts as an alternative to the official analysis method ISO 14088 – IUC 32, so that a correlation between the two methods is established. From the point of view of the chemical composition, tannins are classified into two major groups: i) condensed tannins, also called flavanols or catechins, and ii) hydrolysable tannins, also called pyrogallic tannins. Today, the most widely used convent...

  8. WikiSent : Weakly Supervised Sentiment Analysis Through Extractive Summarization With Wikipedia

    OpenAIRE

    Mukherjee, Subhabrata; Bhattacharyya, Pushpak

    2012-01-01

    This paper describes a weakly supervised system for sentiment analysis in the movie review domain. The objective is to classify a movie review into a polarity class, positive or negative, based on those sentences bearing opinion on the movie alone. The irrelevant text, not directly related to the reviewer opinion on the movie, is left out of analysis. Wikipedia incorporates the world knowledge of movie-specific features in the system which is used to obtain an extractive summary of the review...

  9. Multi-scale Analysis of High Resolution Topography: Feature Extraction and Identification of Landscape Characteristic Scales

    Science.gov (United States)

    Passalacqua, P.; Sangireddy, H.; Stark, C. P.

    2015-12-01

    With the advent of digital terrain data, detailed information on terrain characteristics and on scale and location of geomorphic features is available over extended areas. Our ability to observe landscapes and quantify topographic patterns has greatly improved, including the estimation of fluxes of mass and energy across landscapes. Challenges still remain in the analysis of high resolution topography data; the presence of features such as roads, for example, challenges classic methods for feature extraction and large data volumes require computationally efficient extraction and analysis methods. Moreover, opportunities exist to define new robust metrics of landscape characterization for landscape comparison and model validation. In this presentation we cover recent research in multi-scale and objective analysis of high resolution topography data. We show how the analysis of the probability density function of topographic attributes such as slope, curvature, and topographic index contains useful information for feature localization and extraction. The analysis of how the distributions change across scales, quantified by the behavior of modal values and interquartile range, allows the identification of landscape characteristic scales, such as terrain roughness. The methods are introduced on synthetic signals in one and two dimensions and then applied to a variety of landscapes of different characteristics. Validation of the methods includes the analysis of modeled landscapes where the noise distribution is known and features of interest easily measured.

  10. Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

    Science.gov (United States)

    Belisle, A.A.; Swineford, D.M.

    1988-01-01

    A simple, specific procedure was developed for the analysis of organophosphorus and carbamate pesticides in sediment. The wet soil was mixed with anhydrous sodium sulfate to bind water and the residues were column extracted in acetone:methylene chloride (1:l,v/v). Coextracted water was removed by additional sodium sulfate packed below the sample mixture. The eluate was concentrated and analyzed directly by capillary gas chromatography using phosphorus and nitrogen specific detectors. Recoveries averaged 93 % for sediments extracted shortly after spiking, but decreased significantly as the samples aged.

  11. Pfaff equation and Fourier analysis to phase extraction from an interferogram with carrier frequency

    International Nuclear Information System (INIS)

    Lara-Cortez, Francisco; Meneses-Fabian, Cruz; Rodriguez-Zurita, Gustavo

    2011-01-01

    In the phase extraction techniques, one of the steps most used is to calculate the phase unwrapping from the wrapped phase, which is generally obtained via the inverse tangent function. With the idea to avoid this process, in the present manuscript a method based in the solution of the Pfaff equations is proposed. It is shown that the Pfaff equation is formed with the phase gradient and an auxiliary vector. The phase gradient is obtained from an interference patron with carrier frequency by applying the Fourier transform method and the partial derivatives. In the present manuscript, mathematical analysis, numerical simulation, and the phase extraction of some experimental interferograms are shown.

  12. PERFORMANCE ANALYSIS OF MULTI-TURN EXTRACTION FROM THE PROTON SYNCHROTRON TO THE SUPER PROTON SYNCHROTRON

    CERN Document Server

    Abernethy, Samuel

    2016-01-01

    Within CERN's accelerator complex, the extraction from the Proton Synchrotron to the Super Proton Synchrotron has been done using the so-called ``Continuous Transfer" (CT) method since the 1970's. A new technique, known as Multi-Turn Extraction (MTE), has now been implemented and is in full operation. This report examines a holistic performance analysis of the novel technique in multiple aspects of the accelerator complex, as well as a direct comparison with its predecessor, CT, from the implementation of MTE in 2010 until the end of 2015.

  13. Information analysis of iris biometrics for the needs of cryptology key extraction

    Directory of Open Access Journals (Sweden)

    Adamović Saša

    2013-01-01

    Full Text Available The paper presents a rigorous analysis of iris biometric information for the synthesis of an optimized system for the extraction of a high quality cryptology key. Estimations of local entropy and mutual information were identified as segments of the iris most suitable for this purpose. In order to optimize parameters, corresponding wavelets were transformed, in order to obtain the highest possible entropy and mutual information lower in the transformation domain, which set frameworks for the synthesis of systems for the extraction of truly random sequences of iris biometrics, without compromising authentication properties. [Projekat Ministarstva nauke Republike Srbije, br. TR32054 i br. III44006

  14. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Saliva Samples by Fourier Transform Infrared Spectrometry (Spanish Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  15. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Saliva Samples by Fourier Transform Infrared Spectrometry (French Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  16. Analysis of Free Amino Acids in Different Extracts of Orthosiphon stamineus Leaves by High-Performance Liquid Chromatography Combined with Solid-Phase Extraction.

    Science.gov (United States)

    Shafaei, Armaghan; Halim, Nor Hidayah Ab; Zakaria, Norhidayah; Ismail, Zhari

    2017-10-01

    Orthosiphon stamineus (OS) Benth is a medicinal plant and native in Southeast Asia. Previous studies have shown that OS leaves possess antioxidant, cytotoxic, diuretic, antihypertensive, and uricosuric effects. These beneficial effects have been attributed to the presence of primary and secondary metabolites such as polyphenols, amino acids, and flavonoids. To develop and validate an high-performance liquid chromatography (HPLC)-diode array detector (DAD) method combined with solid-phase extraction that involves precolumn derivatization with O -phthaladehyde for simultaneous analysis of free amino acids in OS leaves extracts. OS leaves were extracted with water (OS-W), ethanol (OS-E), methanol (OS-M), 50% ethanol (OS-EW), and 50% methanol (OS-MW). The extracts were treated by C18 cartridge before derivatization, resulting in great improvement of separation by Zorbox Eclipse XDB-C 18 column. The HPLC-DAD method was successfully developed and validated for analyzing the contents of free amino acids in OS extracts. The results showed that l-aspartic acid with 0.93 ± 0.01 nmol/mg was the major free amino acid in OS-W extract. However, in OS-E, OS-M, OS-EW, and OS-MW, l-glutamic acid with 3.53 ± 0.16, 2.17 ± 0.10, 4.01 ± 0.12, and 2.49 ± 0.12 nmol/mg, respectively, was the major free amino acid. Subsequently, l-serine, which was detected in OS-W, OS-E, and OS-M, was the minor free amino acid with 0.33 ± 0.02, 0.12 ± 0.01, and 0.06 ± 0.01 nmol/mg, respectively. However, l-threonine with 0.26 ± 0.02 and 0.19 ± 0.08 nmol/mL in OS-EW and OS-MW, respectively, had the lowest concentration compared with other amino acid components. All validation parameters of the developed method indicate that the method is reliable and efficient to simultaneously determine the free amino acids content for routine analysis of OS extracts. The HPLC-DAD method combined with solid phase extraction was successfully developed and validated for simultaneous determination and

  17. A Swellable Microneedle Patch to Rapidly Extract Skin Interstitial Fluid for Timely Metabolic Analysis.

    Science.gov (United States)

    Chang, Hao; Zheng, Mengjia; Yu, Xiaojun; Than, Aung; Seeni, Razina Z; Kang, Rongjie; Tian, Jingqi; Khanh, Duong Phan; Liu, Linbo; Chen, Peng; Xu, Chenjie

    2017-10-01

    Skin interstitial fluid (ISF) is an emerging source of biomarkers for disease diagnosis and prognosis. Microneedle (MN) patch has been identified as an ideal platform to extract ISF from the skin due to its pain-free and easy-to-administrated properties. However, long sampling time is still a serious problem which impedes timely metabolic analysis. In this study, a swellable MN patch that can rapidly extract ISF is developed. The MN patch is made of methacrylated hyaluronic acid (MeHA) and further crosslinked through UV irradiation. Owing to the supreme water affinity of MeHA, this MN patch can extract sufficient ISF in a short time without the assistance of extra devices, which remarkably facilitates timely metabolic analysis. Due to covalent crosslinked network, the MN patch maintains the structure integrity in the swelling hydrated state without leaving residues in skin after usage. More importantly, the extracted ISF metabolites can be efficiently recovered from MN patch by centrifugation for the subsequent offline analysis of metabolites such as glucose and cholesterol. Given the recent trend of easy-to-use point-of-care devices for personal healthcare monitoring, this study opens a new avenue for the development of MN-based microdevices for sampling ISF and minimally invasive metabolic detection. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Analysis of glycosaminoglycans in cerebrospinal fluid from patients with mucopolysaccharidoses by isotope-dilution ultra-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhang, Haoyue; Young, Sarah P; Auray-Blais, Christiane; Orchard, Paul J; Tolar, Jakub; Millington, David S

    2011-07-01

    New therapies for the treatment of mucopolysaccharidoses that target the brain, including intrathecal enzyme replacement, are being explored. Quantitative analysis of the glycosaminoglycans (GAGs) that accumulate in these disorders is required to assess the disease burden and monitor the effect of therapy in affected patients. Because current methods lack the required limit of quantification and specificity to analyze GAGs in small volumes of cerebrospinal fluid (CSF), we developed a method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples of CSF (25 μL) were evaporated to dryness and subjected to methanolysis. The GAGs were degraded to uronic acid-N-acetylhexosamine dimers and mixed with internal standards derived from deuteriomethanolysis of GAG standards. Specific dimers derived from heparan, dermatan and chondroitin sulfates (HS, DS and CS) were separated by UPLC and analyzed by electrospray ionization MS/MS using selected reaction monitoring for each targeted GAG product and its corresponding internal standard. CSF from control pediatric subjects (n = 22) contained <0.38 mg/L HS, 0.26 mg/L DS, and 2.8 mg/L CS, whereas CSF from patients with Hurler syndrome (n = 7) contained concentrations of DS and HS that were at least 6-fold greater than the upper control limits. These concentrations were reduced by 17.5% to 82.5% after allogeneic transplantation and treatment with intrathecal and intravenous enzyme replacement therapy. The method described here has potential value in monitoring patients with mucopolysaccharidoses receiving treatment targeted to the brain.

  19. Dynamics of dilute polymer solutions

    International Nuclear Information System (INIS)

    Nicholson, L.K.; Higgins, J.S.

    1980-01-01

    Neutrons scattered by nuclei undergoing slow motion e.g. the internal motion within polymer chains, lose or gain very small amounts of energy. It is therefore the quasi-elastic region of the neutron scattering spectrum which is of interest and in particular the time correlation function (or intermediate scattering law S(Q,t)) which is ideally required to define the motion. The neutron spin echo spectrometer (IN11) at the ILL facilitates the measurement of very small energy changes (down to 10 neV) on scattering from a sample, by changing and keeping track of neutron beam polarization non-parallel to the magnetic guide-field (1). The resultant neutron beam polarization, when normalized against a standard (totally elastic) scatterer is directly proportional to the cosine Fourier Transform of the scattering law S(Q,ω), which is to say the time correlation function is measured directly. Dilute solutions of deuterated polystyrene (PSD) and deuterated polytetrahydrofuran (PTDF) in carbon disulphide, and of their hydrogeneous counterparts (PSH and PTHF respectively) in deuterated benzene were investigated in the range 0.027 A -1 -1 , at 30 0 C. (orig./FKS)

  20. Storm Sewage Dilution in Smaller Streams

    DEFF Research Database (Denmark)

    Larsen, Torben; Vestergaard, Kristian

    1987-01-01

    A numerical model has been used to show how dilution in smaller streams can be effected by unsteady hydraulic conditions caused by a storm sewage overflow.......A numerical model has been used to show how dilution in smaller streams can be effected by unsteady hydraulic conditions caused by a storm sewage overflow....

  1. Cost effectiveness of dilute chemical decontamination

    International Nuclear Information System (INIS)

    LeSurf, J.E.; Weyman, G.D.

    The basic principles of dilute chemical decontamination are described, as well as the method of application. Methods of computing savings in radiation dose and costs are presented, with results from actual experience and illustrative examples. It is concluded that dilute chemical decontamination is beneficial in many cases. It reduces radiation exposure of workers, saves money, and simplifies maintenance work

  2. Phytochemical analysis of Binahong (Anredera Cordifolia) leaves extract to inhibit In Vitro growth of Aeromonas Hydrophila

    Science.gov (United States)

    Basyuni, Mohammad; Ginting, Prita Yulianti Anasta Br; Lesmana, Indra

    2017-11-01

    Binahong (Anredera cordifolia) is one of the medicinal plants commonly used to treat the disease of living organisms. The secondary metabolite of A. cordifolia leaves has been shown antibacterial activity. This study aimed to investigate the secondary metabolite of A. cordifolia leaves showing antibacterial and analysis the effectiveness of antibacterial to inhibit the growth of bacteria Aeromonas hydrophila. A paper disc soaked in a solution of A. cordifolia leaves extract was used to test in vitro at a concentration of 0% (w/v), 0.2%, 0.4%, 0.6%, 0.8%, and positive control of antibiotic (oxytetracycline), respectively. The extracts then placed on a tryptone soy agar (TSA) medium containing bacteria A. hydrophila and incubated at 37 °C for 24 hours. In vitro test showed that A. cordifolia leaves extract inhibited the growth of bacteria A. hydrophila with an inhibition area around the paper disc. The inhibition growth of A. hydrophila increased with the increasing of extract concentration. Bacterial growth was inhibited in the diameter zone of A. hydrophila under different levels of the extracts were 0 mm (0 % negative control), 8.4 mm (0.2 %), 9.4 mm (0.4 %), 10.5 mm (0.6 %), 11.9 mm (0.8 %), 27.5 mm (positive control), respectively. Phytochemical screening of A. cordifolia leaves extract indicated that the extracts contained flavonoid, phenol, saponin, alkaloid, triterpenoid, and β-sitosterol. Our in vitro study demonstrated the inhibition growth of A. hydrophila that caused the disease of motile Aeromonas septicemia (MAS).

  3. Comparative determination of sucrose content in sugar beet by polarimetric and isotope dilution methods

    Energy Technology Data Exchange (ETDEWEB)

    Malec, K; Szuchnik, A [Institute of Nuclear Research, Warsaw (Poland); Rydel, S; Walerianaczyk, E [Instytut Przemyslu Cukrowniczego, Warsaw (Poland)

    1976-01-01

    The comparative determination of sucrose content in sugar beets has been investigated by following methods: polarimetric, direct isotope dilution and double carrier-isotope dilution analysis. Basing upon the obtained results it has been ascertained, that in the case of worse quality beets the polarimetric determinations differ greatly from isotopic data.

  4. Effect of Melanin Free Ink Extracted From Squid (Loligo sp.) on Proximate and Sensory Characteristics of Soft-Bone Milkfish (Chanos chanos) During Storage

    Science.gov (United States)

    Winarni Agustini, Tri; Hadiyanto; Wijayanti, Ima; Amalia, Ulfah; Benjakul, Soottawat

    2018-02-01

    Antioxidant could be extracted and isolated from squid inks. Squid ink in the form of melanin free ink (MFI) could be act as an electron donor which can stabilize free radicals in lipid oxidation. This study was carried out to assess the antioxidant activity of squid inks converted into MFI in different dilution and to optimize the extraction conditions for the application of MFI as an antioxidative agent on fish product. Three different types of MFI extracts i.e : pure squid ink, squid ink with 5 times dilution and squid ink with 10 times dilutions by using cooled ionized water (4°C). The ink was then centrifuged at 18.000 x g for 30 minutes at cooled centrifuge (4°C) followed by DPPH analysis. The results showed that the IC50 of MFI extracts were 2.84 ppm; 1.11 ppm and 0.34 ppm, respectively (p squid ink with 10 times dilution in extraction of MFI had the highest value in free radical inhibitory. Although the IC50 of three different dilutions are equally low, and are considered as very strong antioxidative agent, however, it showed that the MFI extracted from squid ink had the ability to prevent free radical

  5. [Dan'e-fukang soft extract for dysmenorrhea: a meta-analysis].

    Science.gov (United States)

    Yu, Kun; Zhang, Zhen-dong; Xiao, Zheng; Wei, Wei; Wang, Zheng-long

    2014-07-01

    To assess the efficacy and safety of Dan'e-fukang soft extract for dysmenorrhea by meta-analysis. Cochrane Controlled Trials Register, PubMed, EMBASE, CBM, VIP, Wanfang Data, and CNKI databases were searched. Results of randomized controlled trials were also harvested from pharmaceutical companies by manual search. Meta-analysis was carried out according to the method provided by the Cochrane Collaboration with RevMan5.0 software. Twelve Chinese papers were selected, and 1213 patients were included. Significant difference in recovery rate was found between Dan'e-fukang soft extract group and other drugs group (RR=1.33, 95%CI: 1.02-1.75, P0.05). No statistical difference was noticed in total effective rate between two groups (RR=1.04, 95%CI: 1.00-1.08, P>0.05). A statistical difference in improvement of dysmenorrhea symptoms was found before and after treatment in both Dan'e-fukang soft extract group and other drugs group (MD=5.79, 95%CI: 5.01-6.56, P0.05) and after treatment (MD=-0.94, 95%CI: -2.11-0.23, P>0.05). Oral administration of Dan'e-fukang soft extract caused only mild gastrointestinal discomfort, but other drugs had more adverse effects including serious gastrointestinal reaction, severe liver dysfunction, vaginal bleeding, and female masculinity. The existing evidence shows that Dan'e-fukang soft extract has the same efficacy as other drugs in treatment of dysmenorrheal. Because of the quality of the included studies was limited, the evidence of the efficacy and safety of Dan'e-fukang soft extract was not strong, and high-quality randomized trials with large samples are needed.

  6. Comparison of two commercial DNA extraction kits for the analysis of nasopharyngeal bacterial communities

    Directory of Open Access Journals (Sweden)

    Keith A. Crandall

    2016-04-01

    Full Text Available Characterization of microbial communities via next-generation sequencing (NGS requires an extraction ofmicrobial DNA. Methodological differences in DNA extraction protocols may bias results and complicate inter-study comparisons. Here we compare the effect of two commonly used commercial kits (Norgen and Qiagenfor the extraction of total DNA on estimatingnasopharyngeal microbiome diversity. The nasopharynxis a reservoir for pathogens associated with respiratory illnesses and a key player in understandingairway microbial dynamics. Total DNA from nasal washes corresponding to 30 asthmatic children was extracted using theQiagenQIAamp DNA and NorgenRNA/DNA Purification kits and analyzed via IlluminaMiSeq16S rRNA V4 ampliconsequencing. The Norgen samples included more sequence reads and OTUs per sample than the Qiagen samples, but OTU counts per sample varied proportionallybetween groups (r = 0.732.Microbial profiles varied slightly between sample pairs, but alpha- and beta-diversity indices (PCoAand clustering showed highsimilarity between Norgen and Qiagenmicrobiomes. Moreover, no significant differences in community structure (PERMANOVA and adonis tests and taxa proportions (Kruskal-Wallis test were observed betweenkits. Finally, aProcrustes analysis also showed low dissimilarity (M2 = 0.173; P< 0.001 between the PCoAs of the two DNA extraction kits. Contrary to what has been observed in previous studies comparing DNA extraction methods, our 16S NGS analysis of nasopharyngeal washes did not reveal significant differences in community composition or structure between kits. Our findingssuggest congruence between column-based chromatography kits and supportthe comparison of microbiomeprofilesacross nasopharyngeal metataxonomic studies.

  7. Chemical Analysis of Extracts from Newfoundland Berries and Potential Neuroprotective Effects

    Directory of Open Access Journals (Sweden)

    Mohammad Z. Hossain

    2016-10-01

    Full Text Available Various species of berries have been reported to contain several polyphenolic compounds, such as anthocyanins and flavonols, which are known to possess high antioxidant activity and may be beneficial for human health. To our knowledge, a thorough chemical analysis of polyphenolics in species of these plants native to Newfoundland, Canada has not been conducted. The primary objective of this study was to determine the polyphenolic compounds present in commercial extracts from Newfoundland berries, which included blueberries (V. angustifolium, lingonberries (V. vitis-idaea and black currant (Ribes lacustre. Anthocyanin and flavonol glycosides in powdered extracts from Ribes lacustre and the Vaccinium species were identified using the high performance liquid chromatographic (HPLC separation method with mass spectrometric (MS detection. The identified compounds were extracted from dried berries by various solvents via ultrasonication followed by centrifugation. A reverse-phase analytical column was employed to identify the retention time of each chemical component before submission for LC–MS analysis. A total of 21 phenolic compounds were tentatively identified in the three species. Further, we tested the effects of the lingonberry extract for its ability to protect neurons and glia from trauma utilizing an in vitro model of cell injury. Surprisingly, these extracts provided complete protection from cell death in this model. These findings indicate the presence of a wide variety of anthocyanins and flavonols in berries that grow natively in Newfoundland. These powdered extracts maintain these compounds intact despite being processed from berry fruit, indicating their potential use as dietary supplements. In addition, these recent findings and previous data from our lab demonstrate the ability of compounds in berries to protect the nervous system from traumatic insults.

  8. Analysis of Time n Frequency EEG Feature Extraction Methods for Mental Task Classification

    Directory of Open Access Journals (Sweden)

    Caglar Uyulan

    2017-01-01

    Full Text Available Many endogenous and external components may affect the physiological, mental and behavioral states in humans. Monitoring tools are required to evaluate biomarkers, identify biological events, and predict their outcomes. Being one of the valuable indicators, brain biomarkers derived from temporal or spectral electroencephalography (EEG signals processing, allow for the classification of mental disorders and mental tasks. An EEG signal has a nonstationary nature and individual frequency feature, hence it can be concluded that each subject has peculiar timing and data to extract unique features. In order to classify data, which are collected by performing four mental task (reciting the alphabet backwards, imagination of rotation of a cube, imagination of right hand movements (open/close and performing mathematical operations, discriminative features were extracted using four competitive time-frequency techniques; Wavelet Packet Decomposition (WPD, Morlet Wavelet Transform (MWT, Short Time Fourier Transform (STFT and Wavelet Filter Bank (WFB, respectively. The extracted features using both time and frequency domain information were then reduced using a principal component analysis for subset reduction. Finally, the reduced subsets were fed into a multi-layer perceptron neural network (MP-NN trained with back propagation (BP algorithm to generate a predictive model. This study mainly focuses on comparing the relative performance of time-frequency feature extraction methods that are used to classify mental tasks. The real-time (RT conducted experimental results underlined that the WPD feature extraction method outperforms with 92% classification accuracy compared to three other aforementioned methods for four different mental tasks.

  9. Comparison of Different Protein Extraction Methods for Gel-Based Proteomic Analysis of Ganoderma spp.

    Science.gov (United States)

    Al-Obaidi, Jameel R; Saidi, Noor Baity; Usuldin, Siti Rokhiyah Ahmad; Hussin, Siti Nahdatul Isnaini Said; Yusoff, Noornabeela Md; Idris, Abu Seman

    2016-04-01

    Ganoderma species are a group of fungi that have the ability to degrade lignin polymers and cause severe diseases such as stem and root rot and can infect economically important plants and perennial crops such as oil palm, especially in tropical countries such as Malaysia. Unfortunately, very little is known about the complex interplay between oil palm and Ganoderma in the pathogenesis of the diseases. Proteomic technologies are simple yet powerful tools in comparing protein profile and have been widely used to study plant-fungus interaction. A critical step to perform a good proteome research is to establish a method that gives the best quality and a wide coverage of total proteins. Despite the availability of various protein extraction protocols from pathogenic fungi in the literature, no single extraction method was found suitable for all types of pathogenic fungi. To develop an optimized protein extraction protocol for 2-DE gel analysis of Ganoderma spp., three previously reported protein extraction protocols were compared: trichloroacetic acid, sucrose and phenol/ammonium acetate in methanol. The third method was found to give the most reproducible gels and highest protein concentration. Using the later method, a total of 10 protein spots (5 from each species) were successfully identified. Hence, the results from this study propose phenol/ammonium acetate in methanol as the most effective protein extraction method for 2-DE proteomic studies of Ganoderma spp.

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

    International Nuclear Information System (INIS)

    Vestner, Jochen; Fritsch, Stefanie; Rauhut, Doris

    2010-01-01

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

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

    Science.gov (United States)

    Vestner, Jochen; Fritsch, Stefanie; Rauhut, Doris

    2010-02-15

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

  12. Automated gravimetric sample pretreatment using an industrial robot for the high-precision determination of plutonium by isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Surugaya, Naoki; Hiyama, Toshiaki; Watahiki, Masaru

    2008-01-01

    A robotized sample-preparation method for the determination of Pu, which is recovered by extraction reprocessing of spent nuclear fuel, by isotope dilution mass spectrometry (IDMS) is described. The automated system uses a six-axis industrial robot, whose motility is very fast, accurate, and flexible, installed in a glove box. The automation of the weighing and dilution steps enables operator-unattended sample pretreatment for the high-precision analysis of Pu in aqueous solutions. Using the developed system, the Pu concentration in a HNO 3 medium was successfully determined using a set of subsequent mass spectrometric measurements. The relative uncertainty in determining the Pu concentration by IDMS using this system was estimated to be less than 0.1% (k=2), which is equal to that expected of a talented analysis. The operation time required was the same as that for a skilled operator. (author)

  13. Antimicrobial Activity and Chromatographic Analysis of Extracts from Tropaeolum pentaphyllum Lam. Tubers

    Directory of Open Access Journals (Sweden)

    Ritiel Corrêa da Cruz

    2016-04-01

    Full Text Available Background: Tropaeolum pentaphyllum Lam. tubers (Tropaeolaceae are known and used as a condiment and for the treatment of skin infections in Southern Brazil. However, its activity and composition has not yet been investigated. Thus, different extracts and the essential oil from the tubers were tested against a range of microorganisms. The most active extracts were submitted to chromatographic analysis. Methods: Hydroalcoholic extract (70%, fractions of it, and the essential oil from the tubers were tested against several bacteria, yeasts and molds, furnishing the corresponding inhibitory, bactericidal and fungicidal minimal concentration values. The most active extracts were submitted to GC-MS investigation. Results: The strongest effects against different strains of microorganisms, such as Gram-positive and negative bacteria, Candida spp. and dermatophytes were observed for the essential oil and the chloroform fraction, with minimal inhibitory concentrations (MICs well below 200 µg/mL. GC-MS analysis revealed that the major essential oil constituent is benzyl isothiocyanate (BITC, while the chloroform fraction is constituted of BITC, amides, sulfur, fatty acids and its esters, all compounds that may be related to the demonstrated activity. Conclusions: Overall, the results support the popular use of the plant for the treatment of skin infections, and revealed the main active compounds.

  14. MICELLE-MEDIATED EXTRACTION AS A TOOL FOR SEPARATION AND PRECONCENTRATION IN COPPER ANALYSIS

    Directory of Open Access Journals (Sweden)

    F. Ahmadia

    2010-06-01

    Full Text Available A cloud point extraction method was presented for preconcentration of copper in various samples. After complexation with 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline-5-one (ADPP or N-Benzoyl-N-phenylhydroxylamine (BPA  in water, analyte ions are quantitatively extracted to the phase rich in Triton X-114 after centrifugation. 2.0 mol L-1 HNO3 solution in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS. The adopted concentrations for ADPP, Triton X-114, HNO3 and parameters such as bath temperature, centrifuge rate and time were optimized. Detection limits (3SDb/m of 1.3 and 1.9 ng mL-1 for ADPP and BPA along with enrichment factors of 30 and 38 for ADPP and BPA were achieved. The high efficiency of cloud point extraction to carry out the determination of analyte in complex matrices was demonstrated. The proposed method was applied to the analysis of biological, industrial, natural and wastewater, soil and blood samples.   Keywords: 4-Amino-2,3-dimethyl-1-phenyl-3-pyrazoline-5-one (ADPP, N-Benzoyl-N-phenylhydroxylamine (BPA ,   Cloud Point Extraction, Triton X-114, Flame Atomic Absorption Spectrometry.

  15. Needle trap extraction for GC analysis of formic and acetic acids in aqueous solution.

    Science.gov (United States)

    Lee, Xinqing; Huang, Daikuan; Lou, Dawei; Pawliszyn, Janusz

    2012-07-01

    Formic and acetic acids are ubiquitous in the environment, food, and most of the natural products. Extraction of the acids from aqueous solution is required for their isotope analysis by the gas chromatography-isotope ratio mass spectrometry. To this objective, we have previously developed a purge-and-trap technique using the dynamic solid-phase microextraction technology, the NeedlEX. The extraction efficiency, however, remains unexamined. Here, we address this question using the flame ionization detector and isotope ratio mass spectrometer while comparing it with that of the CAR/PDMS fiber. The results show that the NeedlEX is applicable at a wide range of concentration through coordination of purge volume given the minimum amount 3.7 ng and 1.8 ng of formic and acetic, respectively, is extracted. The efficiency of NeedlEX was 6-7 times lower than the fiber at 1000 μg/mL depending on the analyte. It is, however, superior to the latter at 10 μg/mL or less owing to its lower detection limit. The extraction efficiency of both acids is equivalent in molar amount. This is, however, disguised by the different response of the flame ionization detector. The isotope ratio mass spectrometor overcomes this problem but is compromised by relatively large errors. These results are particularly useful for isotopic analysis of carboxylic acids. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

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

    2012-03-01

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

  17. Two-Phase Extraction for Comprehensive Analysis of the Plant Metabolome by NMR.

    Science.gov (United States)

    Schripsema, Jan; Dagnino, Denise

    2018-01-01

    Metabolomics is the area of research, which strives to obtain complete metabolic fingerprints, to detect differences between them, and to provide hypothesis to explain those differences [1]. But obtaining complete metabolic fingerprints is not an easy task. Metabolite extraction is a key step during this process, and much research has been devoted to finding the best solvent mixture to extract as much metabolites as possible.Here a procedure is described for analysis of both polar and apolar metabolites using a two-phase extraction system. D 2 O and CDCl 3 are the solvents of choice, and their major advantage is that, for the identification of the compounds, standard databases can be used because D 2 O and CDCl 3 are the solvents most commonly used for pure compound NMR spectra. The procedure enables the absolute quantification of components via the addition of suitable internal standards. The extracts are also suitable for further analysis with other systems like LC-MS or GC-MS.

  18. Radioisotope dilution technique for determination of vitamin B12 in foods

    International Nuclear Information System (INIS)

    Casey, P.J.; Speckman, K.R.; Ebert, F.J.; Hobbs, W.E.

    1982-01-01

    A radioisotope dilution (RID) method for the determination of vitamin B 12 is presented. The method combines a standard extraction procedure (AOAC 43.108, 12th ed.) with a commercially available RID assay kit. The method was evaluated on a wide range of fortified and unfortified food products. Recovery studies on both groups yielded average recoveries of 98.1 and 95.8%, respectively. Reproducibility data generated from replicate analysis on both groups gave a relative standard deviation of 6.9% for the fortified group and 9.2% for the unfortified group. For the samples studied, the mean vitamin B 12 content determined by the RID method was 8.01 μ/100 g vs a mean of 7.54 μg/100 g by the AOAC microbiological method; the correlation coefficient was r = 0.983

  19. Titanium leaching from red mud by diluted sulfuric acid at atmospheric pressure

    International Nuclear Information System (INIS)

    Agatzini-Leonardou, S.; Oustadakis, P.; Tsakiridis, P.E.; Markopoulos, Ch.

    2008-01-01

    Laboratory-scale research has focused on the recovery of titanium from red mud, which is obtained from bauxite during the Bayer process for alumina production. The leaching process is based on the extraction of this element with diluted sulfuric acid from red mud under atmospheric conditions and without using any preliminary treatment. Statistical design and analysis of experiments were used, in order to determine the main effects and interactions of the leaching process factors, which were: acid normality, temperature and solid to liquid ratio. The titanium recovery efficiency on the basis of red mud weight reached 64.5%. The characterization of the initial red mud, as well as this of the leached residues was carried out by X-ray diffraction, TG-DTA and scanning electron microscopy

  20. Automated CO2 extraction from air for clumped isotope analysis in the atmo- and biosphere

    Science.gov (United States)

    Hofmann, Magdalena; Ziegler, Martin; Pons, Thijs; Lourens, Lucas; Röckmann, Thomas

    2015-04-01

    The conventional stable isotope ratios 13C/12C and 18O/16O in atmospheric CO2 are a powerful tool for unraveling the global carbon cycle. In recent years, it has been suggested that the abundance of the very rare isotopologue 13C18O16O on m/z 47 might be a promising tracer to complement conventional stable isotope analysis of atmospheric CO2 [Affek and Eiler, 2006; Affek et al. 2007; Eiler and Schauble, 2004; Yeung et al., 2009]. Here we present an automated analytical system that is designed for clumped isotope analysis of atmo- and biospheric CO2. The carbon dioxide gas is quantitatively extracted from about 1.5L of air (ATP). The automated stainless steel extraction and purification line consists of three main components: (i) a drying unit (a magnesium perchlorate unit and a cryogenic water trap), (ii) two CO2 traps cooled with liquid nitrogen [Werner et al., 2001] and (iii) a GC column packed with Porapak Q that can be cooled with liquid nitrogen to -30°C during purification and heated up to 230°C in-between two extraction runs. After CO2 extraction and purification, the CO2 is automatically transferred to the mass spectrometer. Mass spectrometric analysis of the 13C18O16O abundance is carried out in dual inlet mode on a MAT 253 mass spectrometer. Each analysis generally consists of 80 change-over-cycles. Three additional Faraday cups were added to the mass spectrometer for simultaneous analysis of the mass-to-charge ratios 44, 45, 46, 47, 48 and 49. The reproducibility for δ13C, δ18O and Δ47 for repeated CO2 extractions from air is in the range of 0.11o (SD), 0.18o (SD) and 0.02 (SD)o respectively. This automated CO2 extraction and purification system will be used to analyse the clumped isotopic signature in atmospheric CO2 (tall tower, Cabauw, Netherlands) and to study the clumped isotopic fractionation during photosynthesis (leaf chamber experiments) and soil respiration. References Affek, H. P., Xu, X. & Eiler, J. M., Geochim. Cosmochim. Acta 71, 5033

  1. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young

    2005-01-01

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties

  2. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2005-03-15

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

  3. Immunohistochemical Analysis of Platelet Extract Effects on Liver Injury Induced by CCl4 in Male Rats

    Directory of Open Access Journals (Sweden)

    Zahra Hesami

    2016-01-01

    Full Text Available Backgrounds & objectives: Liver damage results in a large accumulation of external cellular matrix that affects the function of this important body organ in a long term and finally stops its function completely. The growth factors existing in platelet extract are more cost-effective, available, and stable than recombinant ones. To determine whether the platelet extract effects on histological changes in liver injury induced by carbon tetrachloride (CCl4, we used immunohistochemical analysis in male rats. Methods: In this project the 28 male Wistar rats (250-300 g were randomly divided into 4 groups, each consisting of 7 animals. The rats were divided into four experimental groups as follows: the first group (sham intraperitoneally received only olive oil as the solvent of carbon tetrachloride; second group (CCl4 intraperitoneally received carbon tetrachloride dissolved in olive oil (ratio of about 1: 1 at a concentration of 1 ml/kg and a twice a week for eight weeks; third group subcutaneously received only platelet extract at a concentration of 0.5 ml/kg twice a week for three weeks; and fourth group received both CCl4 intraperitoneally for eight weeks and platelet extract subcutaneously for last three weeks. After 8 weeks of trial blood and liver sampling were done. Blood samples sent for enzymatic (AST, ALT tests and liver samples tested for histological and immunohistochemical studies. The data were analyzed using  one-way ANOVA followed by Tukey test by Graph pad Prism 5 software and data were considered significant at p≤ 0.05. Results: The results show that platelet extract causes a significant (p≤ 0.001 decrease in liver enzymes and albumin improves the function of liver. The level of alfa smooth muscle actin (α-SMA as an index of hepatic stellate cell activation was decreased by platelet extract administration which eventually reduced the necrosis and fibrosis induced by carbon tetrachloride in studied rats

  4. Extraction and isotopic analysis of medium molecular weight hydrocarbons from Murchison using supercritical carbon dioxide

    Science.gov (United States)

    Gilmour, Iain; Pillinger, Colin

    1993-03-01

    The large variety of organic compounds present in carbonaceous chondrites poses particular problems in their analysis not the least of which is terrestrial contamination. Conventional analytical approaches employ simple chromatographic techniques to fractionate the extractable compounds into broad classes of similar chemical structure. However, the use of organic solvents and their subsequent removal by evaporation results in the depletion or loss of semi-volatile compounds as well as requiring considerable preparative work to assure solvent purity. Supercritical fluids have been shown to provide a powerful alternative to conventional liquid organic solvents used for analytical extractions. A sample of Murchison from the Field Museum was analyzed. Two interior fragments were used; the first (2.85 g) was crushed in an agate pestel and mortar to a grain size of ca. 50-100 micron, the second (1.80 g) was broken into chips 3-8 mm in size. Each sample was loaded into a stainless steel bomb and placed in the extraction chamber of an Isco supercritical fluid extractor maintained at 35 C. High purity (99.9995 percent) carbon dioxide was used and was pressurized using an Isco syringe pump. The samples were extracted dynamically by flowing CO2 under pressure through the bomb and venting via a 50 micron fused filica capillary into 5 mls of hexane used as a collection solvent. The hexane was maintained at a temperature of 0.5 C. A series of extractions were done on each sample using CO2 of increasing density. The principal components extracted in each fraction are summarized.

  5. The application of extraction chromatography for analysis of alkali and alkaline earth uranates

    International Nuclear Information System (INIS)

    Tomazic, B.; Cukovic, M.

    1978-01-01

    A method for rapid analysis of alkali and alkaline earth uranates is proposed. The method is based on the use of an HDEHP extraction chromatographic column, which makes possible quantitative separations of alkaline earth ions from macroamounts of uranium(VI). Composition of alkaline earth uranates, based on regression analysis, are presented. The results, which show that under the given experimental conditions alkaline earth triuranates precipitate, are in good agreement with previous data from same laboratory. In addition the HDEHP extraction chromatographic column can be suggested as a tool for separation of representative fission products from irradiated uranium for the purpose of determination of the burn-up factor of nuclear reactor materials. (T.G.)

  6. Analysis of Influence Factors on Extraction Rate of Lutein from Marigold and Optimization of Saponification Conditions

    OpenAIRE

    Wang Xian-Qing; Li Man; Liu Yan-Yan; Liang Ying

    2015-01-01

    After lutein esters extracted by ultrasonic-assisted organic solvent from marigold powder, saponification conditions such as saponification solution concentration, saponification lipuid dosage, saponification temperature and saponification time were optimized by response surface analysis. The results showed that the optimal saponification conditions are saponification solution concentration 10%, saponification lipuid dosage 200 mL, saponification temperature 50°C, saponification time 2 h. Und...

  7. Zero drift and solid Earth tide extracted from relative gravimetric data with principal component analysis

    OpenAIRE

    Hongjuan Yu; Jinyun Guo; Jiulong Li; Dapeng Mu; Qiaoli Kong

    2015-01-01

    Zero drift and solid Earth tide corrections to static relative gravimetric data cannot be ignored. In this paper, a new principal component analysis (PCA) algorithm is presented to extract the zero drift and the solid Earth tide, as signals, from static relative gravimetric data assuming that the components contained in the relative gravimetric data are uncorrelated. Static relative gravity observations from Aug. 15 to Aug. 23, 2014 are used as statistical variables to separate the signal and...

  8. Feasibility analysis of vacuum sieve tray for tritium extraction in the HCLL test blanket system

    Energy Technology Data Exchange (ETDEWEB)

    Okino, Fumito, E-mail: fumito.okino@iae.kyoto-u.ac.jp [Kyoto University Institute of Advanced Energy, 611-0011 Gokasho, Uji, Kyoto (Japan); Calderoni, Pattrick [Fusion For Energy, 08019 Barcelona (Spain); Kasada, Ryuta; Konishi, Satoshi [Kyoto University Institute of Advanced Energy, 611-0011 Gokasho, Uji, Kyoto (Japan)

    2016-11-01

    Highlights: • The authors discovered faster mass transport on a droplet falling in a vacuum. • Primary cause of the hydrogen release from droplet is by the oscillation of a droplet. • The spherical oscillation induces the internal advection and enhances mass transfer. • This assumption agreed with previous experimental results. - Abstract: This paper describes the quantitative analysis for the design of a tritium extraction system that uses liquid PbLi droplets in vacuum (Vacuum Sieve Tray, VST), for application to the ITER helium-cooled lithium lead (HCLL) test blanket system (TBS). The parametric dependences of tritium extraction efficiency from the main geometrical features such as initial droplet velocity, nozzle head height, nozzle diameter, and flow rate are discussed. With nozzle diameters between 0.4 and 0.6 mm, extraction efficiency is estimated from 0.77 to 0.96 at the falling height of 0.5 m, with flow rate between 0.2 and 1.0 kg/s. The device has a height of 1.6 m, within the external dimensions of the HCLL Test Blanket Module (TBM), and no additional pumping power is required. The attained results are considered attractive not only for ITER, but also in view of the application of the VST concept as a candidate tritium extraction system for the European Union's demonstration fusion reactor (DEMO). The extraction efficiency of a single droplet column, which is the basis of the design analysis presented, has been validated experimentally with hydrogen. However, further experiments are required on an integrated system with size relevant to the proposed HCLL-TBS design to validate system-level effects, particularly regarding the desorption process in an array of multiple droplets.

  9. Theoretical modeling of diluted antiferromagnetic systems

    International Nuclear Information System (INIS)

    Pozo, J; Elgueta, R; Acevedo, R

    2000-01-01

    Some magnetic properties of a Diluted Antiferromagnetic System (DAFS) are studied. The model of the two sub-networks for antiferromagnetism is used and a Heisenberg Hamiltonian type is proposed, where the square operators are expressed in terms of boson operators with the approach of spin waves. The behavior of the diluted system's fundamental state depends basically on the competition effect between the anisotropy field and the Weiss molecular field. The approach used allows the diluted system to be worked for strong anisotropies as well as when these are very weak

  10. Comparison of RNA Extraction Methods for Molecular Analysis of Oral Cytology

    Directory of Open Access Journals (Sweden)

    Mônica Ghislaine Oliveira Alves

    2016-01-01

    Full Text Available Objective of work: The aim of this study was to compare three methods of RNA extraction for molecular analysis of oral cytology to establish the best technique, considering its concentration and purity for molecular tests of oral lesions such as real-time reverse transcriptase reaction. Material and methods: The sample included exfoliative cytology from the oral cavity mucosa of patients with no visible clinical changes, using Orcellex Rovers Brush®. The extraction of total RNA was performed using the following three techniques: 30 samples were extracted by Trizol® technique, 30 by the DirectzolTM RNA Miniprep system and 30 by the RNeasy mini Kit. The absorbance was measured by spectrophotometer to estimate the purity. The estimated RNA concentration was obtained by multiplying the value of A260 (ng/mL by 40. Statistical analysis of the obtained data was performed using GraphPad Prism 5.03 software with Student t, analysis of variance and Bonferroni tests, considering p ≤0.05. Results: Trizol® group revealed higher average concentration, followed by Direct-zolTM and Rneasy group. It was observed that the RNA Direct-zolTM group had the highest purity, followed by RNeasy and Trizol® groups, allowing for the two ratios. Conclusion: Considering all aspects, concentration, purity and time spent in the procedures, the Direct-zolTM group showed the best results.

  11. Enhanced detergent extraction for analysis of membrane proteomes by two-dimensional gel electrophoresis

    Directory of Open Access Journals (Sweden)

    Hsu Kimberly K

    2005-06-01

    Full Text Available Abstract Background The analysis of hydrophobic membrane proteins by two-dimensional gel electrophoresis has long been hampered by the concept of inherent difficulty due to solubility issues. We have optimized extraction protocols by varying the detergent composition of the solubilization buffer with a variety of commercially available non-ionic and zwitterionic detergents and detergent-like phospholipids. Results After initial analyses by one-dimensional SDS-PAGE, quantitative two-dimensional analyses of human erythrocyte membranes, mouse liver membranes, and mouse brain membranes, extracted with buffers that included the zwitterionic detergent MEGA 10 (decanoyl-N-methylglucamide and the zwitterionic lipid LPC (1-lauroyl lysophosphatidylcholine, showed selective improvement over extraction with the common 2-DE detergent CHAPS (3 [(3-cholamidopropyldimethylammonio]-1-propanesulfonate. Mixtures of the three detergents showed additive improvements in spot number, density, and resolution. Substantial improvements in the analysis of a brain membrane proteome were observed. Conclusion This study demonstrates that an optimized detergent mix, coupled with rigorous sample handling and electrophoretic protocols, enables simple and effective analysis of membrane proteomes using two-dimensional electrophoresis.

  12. Feature extraction through parallel Probabilistic Principal Component Analysis for heart disease diagnosis

    Science.gov (United States)

    Shah, Syed Muhammad Saqlain; Batool, Safeera; Khan, Imran; Ashraf, Muhammad Usman; Abbas, Syed Hussnain; Hussain, Syed Adnan

    2017-09-01

    Automatic diagnosis of human diseases are mostly achieved through decision support systems. The performance of these systems is mainly dependent on the selection of the most relevant features. This becomes harder when the dataset contains missing values for the different features. Probabilistic Principal Component Analysis (PPCA) has reputation to deal with the problem of missing values of attributes. This research presents a methodology which uses the results of medical tests as input, extracts a reduced dimensional feature subset and provides diagnosis of heart disease. The proposed methodology extracts high impact features in new projection by using Probabilistic Principal Component Analysis (PPCA). PPCA extracts projection vectors which contribute in highest covariance and these projection vectors are used to reduce feature dimension. The selection of projection vectors is done through Parallel Analysis (PA). The feature subset with the reduced dimension is provided to radial basis function (RBF) kernel based Support Vector Machines (SVM). The RBF based SVM serves the purpose of classification into two categories i.e., Heart Patient (HP) and Normal Subject (NS). The proposed methodology is evaluated through accuracy, specificity and sensitivity over the three datasets of UCI i.e., Cleveland, Switzerland and Hungarian. The statistical results achieved through the proposed technique are presented in comparison to the existing research showing its impact. The proposed technique achieved an accuracy of 82.18%, 85.82% and 91.30% for Cleveland, Hungarian and Switzerland dataset respectively.

  13. Further development of IDGS: Isotope dilution gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Li, T.K.; Parker, J.L.; Kuno, Y.; Sato, S.; Kamata, M.; Akiyama, T.

    1991-01-01

    The isotope dilution gamma-ray spectrometry (IDGS) technique for determining the plutonium concentration and isotopic composition of highly radioactive spent-fuel dissolver solutions has been further developed. Both the sample preparation and the analysis have been improved. The plutonium isotopic analysis is based on high-resolution, low-energy gamma-ray spectrometry. The plutonium concentration in the dissolver solutions then is calculated from the measured isotopic differences among the spike, the dissolver solution, and the spiked dissolver solution. Plutonium concentrations and isotopic compositions of dissolver solutions analyzed from this study agree well with those obtained by traditional isotope dilution mass spectrometry (IDMS) and are consistent with the first IDGS experimental result. With the current detector efficiency, sample size, and a 100-min count time, the estimated precision is ∼0.5% for 239 Pu and 240 Pu isotopic analyses and ∼1% for the plutonium concentration analysis. 5 refs., 2 figs., 7 tabs

  14. Ammonium chloride salting out extraction/cleanup for trace-level quantitative analysis in food and biological matrices by flow injection tandem mass spectrometry.

    Science.gov (United States)

    Nanita, Sergio C; Padivitage, Nilusha L T

    2013-03-20

    A sample extraction and purification procedure that uses ammonium-salt-induced acetonitrile/water phase separation was developed and demonstrated to be compatible with the recently reported method for pesticide residue analysis based on fast extraction and dilution flow injection mass spectrometry (FED-FI-MS). The ammonium salts evaluated were chloride, acetate, formate, carbonate, and sulfate. A mixture of NaCl and MgSO4, salts used in the well-known QuEChERS method, was also tested for comparison. With thermal decomposition/evaporation temperature of salts resulted in negligible ion source residual under typical electrospray conditions, leading to consistent method performance and less instrument cleaning. Although all ammonium salts tested induced acetonitrile/water phase separation, NH4Cl yielded the best performance, thus it was the preferred salting out agent. The NH4Cl salting out method was successfully coupled with FI/MS/MS and tested for fourteen pesticide active ingredients: chlorantraniliprole, cyantraniliprole, chlorimuron ethyl, oxamyl, methomyl, sulfometuron methyl, chlorsulfuron, triflusulfuron methyl, azimsulfuron, flupyrsulfuron methyl, aminocyclopyrachlor, aminocyclopyrachlor methyl, diuron and hexazinone. A validation study was conducted with nine complex matrices: sorghum, rice, grapefruit, canola, milk, eggs, beef, urine and blood plasma. The method is applicable to all analytes, except aminocyclopyrachlor. The method was deemed appropriate for quantitative analysis in 114 out of 126 analyte/matrix cases tested (applicability rate=0.90). The NH4Cl salting out extraction/cleanup allowed expansion of FI/MS/MS for analysis in food of plant and animal origin, and body fluids with increased ruggedness and sensitivity, while maintaining high-throughput (run time=30s/sample). Limits of quantitation (LOQs) of 0.01mgkg(-1) (ppm), the 'well-accepted standard' in pesticide residue analysis, were achieved in >80% of cases tested; while limits of detection

  15. A method for the direct injection and analysis of small volume human blood spots and plasma extracts containing high concentrations of organic solvents using revered-phase 2D UPLC/MS.

    Science.gov (United States)

    Rainville, Paul D; Simeone, Jennifer L; Root, Dan S; Mallet, Claude R; Wilson, Ian D; Plumb, Robert S

    2015-03-21

    The emergence of micro sampling techniques holds great potential to improve pharmacokinetic data quality, reduce animal usage, and save costs in safety assessment studies. The analysis of these samples presents new challenges for bioanalytical scientists, both in terms of sample processing and analytical sensitivity. The use of two dimensional LC/MS with, at-column-dilution for the direct analysis of highly organic extracts prepared from biological fluids such as dried blood spots and plasma is demonstrated. This technique negated the need to dry down and reconstitute, or dilute samples with water/aqueous buffer solutions, prior to injection onto a reversed-phase LC system. A mixture of model drugs, including bromhexine, triprolidine, enrofloxacin, and procaine were used to test the feasibility of the method. Finally an LC/MS assay for the probe pharmaceutical rosuvastatin was developed from dried blood spots and protein-precipitated plasma. The assays showed acceptable recovery, accuracy and precision according to US FDA guidelines. The resulting analytical method showed an increase in assay sensitivity of up to forty fold as compared to conventional methods by maximizing the amount loaded onto the system and the MS response for the probe pharmaceutical rosuvastatin from small volume samples.

  16. Identification of antifungal activity substances on seedborn disease from garlic and taxus extracts

    Energy Technology Data Exchange (ETDEWEB)

    Chung, I.M.; Paik, S.B. [Konkuk University, Seoul (Korea, Republic of)

    1999-02-01

    Antifungal substances were isolated and identified from garlic and taxus extracts to develop safe and broad fungicide. The inhibitory effect of seedborn disease of sesame, pepper, radish, chinese cabbage by formulation of antifungal substances was investigated. The antifungal substance isolated through column chromatography from garlic and taxus extracts was confirmed by GC-MS as allicin (C{sub 6}H{sub 10}OS{sub 2}) and taxol(C{sub 47}H{sub 51}NO{sub 14}) and the quantified content from each extracts by HPLC analysis was 0.62%, 0.29%, respectively. The formulation composed of garlic and taxus extracts controlled effectively the seedborn fungi tested in this study at 10X dilution, but at 100X dilution the inhibitory effect decreased. Phytotoxicity of these formulations did not recognized. 22 refs., 6 figs., 5 tabs.

  17. Analysis of perfluorinated carboxylic acids in soils II: optimization of chromatography and extraction.

    Science.gov (United States)

    Washington, John W; Henderson, W Matthew; Ellington, J Jackson; Jenkins, Thomas M; Evans, John J

    2008-02-15

    With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorooctanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary phases, two different liquid chromatography-tandem mass spectrometry (LC/MS/MS) systems, and eight combinations of sample-extract pretreatments, extractions and cleanups on three test soils. For the columns and systems we tested, we achieved the greatest analytical sensitivity for PFCAs using a column with a C(18) stationary phase in a Waters LC/MS/MS. In this system we achieved an instrument detection limit for PFOA of 270 ag/microL, equating to about 14 fg of PFOA on-column. While an elementary acetonitrile/water extraction of soils recovers PFCAs effectively, natural soil organic matter also dissolved in the extracts commonly imparts significant noise that appears as broad, multi-nodal, asymmetric peaks that coelute with several PFCAs. The intensity and elution profile of this noise is highly variable among soils and it challenges detection of low concentrations of PFCAs by decreasing the signal-to-noise contrast. In an effort to decrease this background noise, we investigated several methods of pretreatment, extraction and cleanup, in a variety of combinations, that used alkaline and unbuffered water, acetonitrile, tetrabutylammonium hydrogen sulfate, methyl-tert-butyl ether, dispersed activated carbon and solid-phase extraction. For the combined objectives of complete recovery and minimization of background noise, we have chosen: (1) alkaline pretreatment; (2) extraction with acetonitrile/water; (3) evaporation to dryness; (4) reconstitution with tetrabutylammonium-hydrogen-sulfate ion-pairing solution; (5) ion-pair extraction to methyl-tert-butyl ether; (6) evaporation to dryness; (7) reconstitution with 60/40 acetonitrile/water (v/v); and (8) analysis by LC/MS/MS. Using this method, we

  18. Antimicrobial potential and phyto chemical analysis of different solvent extracted samples of viola pilosa

    International Nuclear Information System (INIS)

    Bakht, J.; Panni, M. K.; Shafi, M.

    2017-01-01

    Investigation of susceptibility of medicinal plants for bacterial pathogens is significant for suitable choice of treatment. Different solvent extracted samples of Viola pilosa shoots were investigated for their antibacterial and phytochemical activities using 0.5, 1 and 2 mg disc-1 concentrations. The antibacterial bioassay was assayed by disc diffusion method against six microbes. The studies revealed that ethyl acetate extracted fractions resulted in maximum growth inhibition of Pseudomonas aeruginosa and Staphylococcus aureus at 2000 mu g disc-1 concentration. Similarly, Xanthomonas campestris and Klebsiella pneumonia were found more susceptible to n-butanol extract. Maximum reduction in the activity of B. subtilis and E. coli was recorded by n-hexane fractions at two mg per disc. The most susceptible microbe was Pseudomonas aeruginosa. The results further revealed that all the tested microbes were found completely resistant to water extracted fractions at all the tested concentrations measuring 0% ZI. Phytochemical analysis showed the presence of various bioactive compounds including flavonoids, glycosides, proteins, fats, alkaloids, steroids, saponins, carbohydrates and tannins. (author)

  19. Preliminary phytochemical and elemental analysis of aqueous and fractionated pod extracts of Acacia nilotica (Thorn mimosa

    Directory of Open Access Journals (Sweden)

    Mohammed Shaibu Auwal

    2014-06-01

    Full Text Available Acacia nilotica (Thorn mimosa is used locally for various medicinal purposes by traditionalists and herbalists in northeastern Nigeria. Plants products have been used since ancient times in the management of various conditions. The bark of A. nilotica has been reported to be used traditionally to manage diabetes, dysentery, leprosy, ulcers, cancers, tumor of the eye, ear and testicles, induration of liver and spleen and also in treatment of various condylomas. The objective of this study is to determine the phytochemical and elemental constituents of the extracts of A. nilotica pods. Flame emission and atomic absorption spectrometry were also used to determine the presence or absence of micro- and macro-elements in the extracts. Phytochemical analysis of the aqueous, ethyl acetate and N-butanol fractionated portions of the pod extracts of A. nilotica revealed the presence of tannins, saponins, flavonoids, carbohydrate, whereas carbohydrates and tannins were the only constituent in the residue portion. Anthraquinones, alkaloids, terpene and steroids were not present in the extracts. The elemental screening revealed the presence of iron, potassium, manganese, zinc, calcium, phosphorous, magnesium, sodium, cadmium and copper. Lead, arsenic and molybdenum were not detected in the pod.

  20. Direct mass spectrometric screening of antibiotics from bacterial surfaces using liquid extraction surface analysis.

    Science.gov (United States)

    Kai, Marco; González, Ignacio; Genilloud, Olga; Singh, Sheo B; Svatoš, Aleš

    2012-10-30

    There is a need to find new antibiotic agents to fight resistant pathogenic bacteria. To search successfully for novel antibiotics from bacteria cultivated under diverse conditions, we need a fast and cost-effective screening method. A combination of Liquid Extraction Surface Analysis (LESA), automated chip-based nanoelectrospray ionization, and high-resolution mass or tandem mass spectrometry using an Orbitrap XL was tested as the screening platform. Actinobacteria, known to produce well-recognized thiazolyl peptide antibiotics, were cultivated on a plate of solid medium and the antibiotics were extracted by organic solvent mixtures from the surface of colonies grown on the plate and analyzed using mass spectrometry (MS). LESA combined with high-resolution MS is a powerful tool with which to extract and detect thiazolyl peptide antibiotics from different Actinobacteria. Known antibiotics were correctly detected with high mass accuracy (antibiotics in particular and natural products in general. The method described in this paper is suitable for (1) screening the natural products produced by bacterial colonies on cultivation plates within the first 2 min following extraction and (2) detecting antibiotics at high mass accuracy; the cost is around 2 Euro per sample. Copyright © 2012 John Wiley & Sons, Ltd.

  1. A simplified radiometabolite analysis procedure for PET radioligands using a solid phase extraction with micellar medium

    International Nuclear Information System (INIS)

    Nakao, Ryuji; Halldin, Christer

    2013-01-01

    A solid phase extraction method has been developed for simple and high-speed direct determination of PET radioligands in plasma. Methods: This methodology makes use of a micellar medium and a solid-phase extraction cartridge for displacement of plasma protein bound radioligand and separation of PET radioligands from their radiometabolites without significant preparation. The plasma samples taken from monkey or human during PET measurements were mixed with a micellar eluent containing an anionic surfactant sodium dodecyl sulphate and loaded onto SPE cartridges. The amount of radioactivity corresponding to parent radioligand (retained on the cartridge) and its radioactive metabolites (eluted with micellar eluent) was measured. Results: Under the optimized conditions, excellent separation of target PET radioligands from their radiometabolites was achieved with a single elution and short run-time of 1 min. This method was successfully applied to study the metabolism for 11 C-labelled radioligands in human or monkey plasma. The amount of parent PET radioligands estimated by micellar solid phase extraction strongly corresponded with that determined by radio-LC. The improved throughput permitted the analysis of a large number of plasma samples (up to 13 samples per one PET study) for accurate estimation of metabolite-corrected input function during quantitative PET imaging studies. Conclusion: Solid phase extraction together with micellar medium is fast, sensitive and easy to use, and therefore it is an attractive alternative method to determine relative composition of PET radioligands in plasma

  2. A user-friendly robotic sample preparation program for fully automated biological sample pipetting and dilution to benefit the regulated bioanalysis.

    Science.gov (United States)

    Jiang, Hao; Ouyang, Zheng; Zeng, Jianing; Yuan, Long; Zheng, Naiyu; Jemal, Mohammed; Arnold, Mark E

    2012-06-01

    Biological sample dilution is a rate-limiting step in bioanalytical sample preparation when the concentrations of samples are beyond standard curve ranges, especially when multiple dilution factors are needed in an analytical run. We have developed and validated a Microsoft Excel-based robotic sample preparation program (RSPP) that automatically transforms Watson worklist sample information (identification, sequence and dilution factor) to comma-separated value (CSV) files. The Freedom EVO liquid handler software imports and transforms the CSV files to executable worklists (.gwl files), allowing the robot to perform sample dilutions at variable dilution factors. The dynamic dilution range is 1- to 1000-fold and divided into three dilution steps: 1- to 10-, 11- to 100-, and 101- to 1000-fold. The whole process, including pipetting samples, diluting samples, and adding internal standard(s), is accomplished within 1 h for two racks of samples (96 samples/rack). This platform also supports online sample extraction (liquid-liquid extraction, solid-phase extraction, protein precipitation, etc.) using 96 multichannel arms. This fully automated and validated sample dilution and preparation process has been applied to several drug development programs. The results demonstrate that application of the RSPP for fully automated sample processing is efficient and rugged. The RSPP not only saved more than 50% of the time in sample pipetting and dilution but also reduced human errors. The generated bioanalytical data are accurate and precise; therefore, this application can be used in regulated bioanalysis.

  3. Extraction and analysis of left ventricular contours in cardiac radionuclide angiographies

    International Nuclear Information System (INIS)

    Jouan, A.

    1991-01-01

    The analysis of cardiac scintigraphic sequences is commonly realized with the help of functional or parametric images. The decomposition of the original sequence into a linear combination of the main temporal behaviors yields, after orthogonalization, a set of parametric images representing the pure temporal behaviors present in the original data. The properties of these images are used to extract automatically the left ventricular boundary. The Fourier Descriptors method is then used to get a quantified analysis of the shape of the ventricle. Because of their property of invariance by change of scale, the Fourier descriptors method applied on a sequence of left ventricular contours yields a quantified assessment of the cardiac contraction

  4. Towards automatic music transcription: note extraction based on independent subspace analysis

    Science.gov (United States)

    Wellhausen, Jens; Hoynck, Michael

    2005-01-01

    Due to the increasing amount of music available electronically the need of automatic search, retrieval and classification systems for music becomes more and more important. In this paper an algorithm for automatic transcription of polyphonic piano music into MIDI data is presented, which is a very interesting basis for database applications, music analysis and music classification. The first part of the algorithm performs a note accurate temporal audio segmentation. In the second part, the resulting segments are examined using Independent Subspace Analysis to extract sounding notes. Finally, the results are used to build a MIDI file as a new representation of the piece of music which is examined.

  5. Pure endmember extraction using robust kernel archetypoid analysis for hyperspectral imagery

    Science.gov (United States)

    Sun, Weiwei; Yang, Gang; Wu, Ke; Li, Weiyue; Zhang, Dianfa

    2017-09-01

    A robust kernel archetypoid analysis (RKADA) method is proposed to extract pure endmembers from hyperspectral imagery (HSI). The RKADA assumes that each pixel is a sparse linear mixture of all endmembers and each endmember corresponds to a real pixel in the image scene. First, it improves the re8gular archetypal analysis with a new binary sparse constraint, and the adoption of the kernel function constructs the principal convex hull in an infinite Hilbert space and enlarges the divergences between pairwise pixels. Second, the RKADA transfers the pure endmember extraction problem into an optimization problem by minimizing residual errors with the Huber loss function. The Huber loss function reduces the effects from big noises and outliers in the convergence procedure of RKADA and enhances the robustness of the optimization function. Third, the random kernel sinks for fast kernel matrix approximation and the two-stage algorithm for optimizing initial pure endmembers are utilized to improve its computational efficiency in realistic implementations of RKADA, respectively. The optimization equation of RKADA is solved by using the block coordinate descend scheme and the desired pure endmembers are finally obtained. Six state-of-the-art pure endmember extraction methods are employed to make comparisons with the RKADA on both synthetic and real Cuprite HSI datasets, including three geometrical algorithms vertex component analysis (VCA), alternative volume maximization (AVMAX) and orthogonal subspace projection (OSP), and three matrix factorization algorithms the preconditioning for successive projection algorithm (PreSPA), hierarchical clustering based on rank-two nonnegative matrix factorization (H2NMF) and self-dictionary multiple measurement vector (SDMMV). Experimental results show that the RKADA outperforms all the six methods in terms of spectral angle distance (SAD) and root-mean-square-error (RMSE). Moreover, the RKADA has short computational times in offline

  6. Analysis of urinary 8-isoprostane as an oxidative stress biomarker by stable isotope dilution using automated online in-tube solid-phase microextraction coupled with liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Mizuno, Keisuke; Kataoka, Hiroyuki

    2015-08-10

    We have developed a simple and sensitive method for the determination of the oxidative stress biomarker 8-isoprostane (8-IP) in human urine by automated online in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) using a Zorbax Eclipse XDB-8 column and 0.1% formic acid/methanol (25/75, v/v) as a mobile phase. Electrospray MS/MS for 8-IP was performed on an API 4000 triple quadruple mass spectrometer in negative ion mode. The optimum in-tube SPME conditions were 20 draw/eject cycles with a sample size of 40 μL using a Carboxen 1006 PLOT capillary column for the extraction. The extracted compounds were easily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Total analysis time of this method including online extraction and analysis was about 30 min for each sample. The in-tube SPME LC-MS/MS method showed good linearity in the concentration range of 20-1000 pg/mL with a correlation coefficient r = 0.9999 for 8-IP using a stable isotope-labeled internal standard, 8-IP-d4. The detection limit of 8-IP was 3.3 pg/mL and the proposed method showed 42-fold higher sensitivity than the direct injection method. The intra-day and inter-day precisions (relative standard deviations) were below 5.0% and 8.5% (n = 5), respectively. This method was applied successfully to the analysis of urine samples without pretreatment or interference peaks. The recovery rates of 8-IP spiked into urine samples were above 92%. This method is useful for assessing the effects of oxidative stress and antioxidant intake. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Feature extraction with deep neural networks by a generalized discriminant analysis.

    Science.gov (United States)

    Stuhlsatz, André; Lippel, Jens; Zielke, Thomas

    2012-04-01

    We present an approach to feature extraction that is a generalization of the classical linear discriminant analysis (LDA) on the basis of deep neural networks (DNNs). As for LDA, discriminative features generated from independent Gaussian class conditionals are assumed. This modeling has the advantages that the intrinsic dimensionality of the feature space is bounded by the number of classes and that the optimal discriminant function is linear. Unfortunately, linear transformations are insufficient to extract optimal discriminative features from arbitrarily distributed raw measurements. The generalized discriminant analysis (GerDA) proposed in this paper uses nonlinear transformations that are learnt by DNNs in a semisupervised fashion. We show that the feature extraction based on our approach displays excellent performance on real-world recognition and detection tasks, such as handwritten digit recognition and face detection. In a series of experiments, we evaluate GerDA features with respect to dimensionality reduction, visualization, classification, and detection. Moreover, we show that GerDA DNNs can preprocess truly high-dimensional input data to low-dimensional representations that facilitate accurate predictions even if simple linear predictors or measures of similarity are used.

  8. Improved solid-phase extraction method for systematic toxicological analysis in biological fluids.

    Science.gov (United States)

    Soriano, T; Jurado, C; Menéndez, M; Repetto, M

    2001-03-01

    A method for the simultaneous qualitative and quantitative determination of drugs of abuse (opiates, cocaine, or amphetamines) and prescribed drugs (tricyclic antidepressants, phenotiazines, benzodiazepines, etc.) in biological fluids--blood, urine, bile, and gastric contents--was developed. This procedure involves solid-phase extraction with Bond-Elut Certify columns followed by analysis by gas chromatography-nitrogen-phosphorus detection (GC-NPD) and confirmation by gas chromatography-mass spectrometry (GC-MS), after derivatization, when necessary. Pretreatment was performed on all samples: sonication for 15 min plus enzymatic hydrolysis with beta-glucuronidase in urine. With respect to the internal standards, nalorphine and trihexylamine were used for basic substances, allobarbital for acidic drugs, and prazepam for benzodiazepines. Acidic and basic compounds were extracted from different aliquots of samples at different pH levels: 6-6.5 for the acidic and neutral and 8-8.5 for the basic and the benzodiazepines. Several areas of experimental design were considered in the process of method optimization. These included internal standards, pH, sonication, flow rate and washing solvents. It was found that systematic analysis could be reliably performed using optimized extraction conditions. The recovery rates for the compounds tested were always higher than 61.02%.

  9. Proteome Analysis of Human Sebaceous Follicle Infundibula Extracted from Healthy and Acne-Affected Skin

    Science.gov (United States)

    Bek-Thomsen, Malene; Lomholt, Hans B.; Scavenius, Carsten; Enghild, Jan J.; Brüggemann, Holger

    2014-01-01

    Acne vulgaris is a very common disease of the pilosebaceous unit of the human skin. The pathological processes of acne are not fully understood. To gain further insight sebaceous follicular casts were extracted from 18 healthy and 20 acne-affected individuals by cyanoacrylate-gel biopsies and further processed for mass spectrometry analysis, aiming at a proteomic analysis of the sebaceous follicular casts. Human as well as bacterial proteins were identified. Human proteins enriched in acne and normal samples were detected, respectively. Normal follicular casts are enriched in proteins such as prohibitins and peroxiredoxins which are involved in the protection from various stresses, including reactive oxygen species. By contrast, follicular casts extracted from acne-affected skin contained proteins involved in inflammation, wound healing and tissue remodeling. Among the most distinguishing proteins were myeloperoxidase, lactotransferrin, neutrophil elastase inhibitor and surprisingly, vimentin. The most significant biological process among all acne-enriched proteins was ‘response to a bacterium’. Identified bacterial proteins were exclusively from Propionibacterium acnes. The most abundant P. acnes proteins were surface-exposed dermatan sulphate adhesins, CAMP factors, and a so far uncharacterized lipase in follicular casts extracted from normal as well as acne-affected skin. This is a first proteomic study that identified human proteins together with proteins of the skin microbiota in sebaceous follicular casts. PMID:25238151

  10. Vibration Feature Extraction and Analysis for Fault Diagnosis of Rotating Machinery-A Literature Survey

    Directory of Open Access Journals (Sweden)

    Saleem Riaz

    2017-02-01

    Full Text Available Safety, reliability, efficiency and performance of rotating machinery in all industrial applications are the main concerns. Rotating machines are widely used in various industrial applications. Condition monitoring and fault diagnosis of rotating machinery faults are very important and often complex and labor-intensive. Feature extraction techniques play a vital role for a reliable, effective and efficient feature extraction for the diagnosis of rotating machinery. Therefore, developing effective bearing fault diagnostic method using different fault features at different steps becomes more attractive. Bearings are widely used in medical applications, food processing industries, semi-conductor industries, paper making industries and aircraft components. This paper review has demonstrated that the latest reviews applied to rotating machinery on the available a variety of vibration feature extraction. Generally literature is classified into two main groups: frequency domain, time frequency analysis. However, fault detection and diagnosis of rotating machine vibration signal processing methods to present their own limitations. In practice, most healthy ingredients faulty vibration signal from background noise and mechanical vibration signals are buried. This paper also reviews that how the advanced signal processing methods, empirical mode decomposition and interference cancellation algorithm has been investigated and developed. The condition for rotating machines based rehabilitation, prevent failures increase the availability and reduce the cost of maintenance is becoming necessary too. Rotating machine fault detection and diagnostics in developing algorithms signal processing based on a key problem is the fault feature extraction or quantification. Currently, vibration signal, fault detection and diagnosis of rotating machinery based techniques most widely used techniques. Furthermore, the researchers are widely interested to make automatic

  11. Gas Chromatography-Mass Spectrometry Analysis of Ulva fasciata (Green Seaweed) Extract and Evaluation of Its Cytoprotective and Antigenotoxic Effects.

    Science.gov (United States)

    Rodeiro, Idania; Olguín, Sitlali; Santes, Rebeca; Herrera, José A; Pérez, Carlos L; Mangas, Raisa; Hernández, Yasnay; Fernández, Gisselle; Hernández, Ivones; Hernández-Ojeda, Sandra; Camacho-Carranza, Rafael; Valencia-Olvera, Ana; Espinosa-Aguirre, Jesús Javier

    2015-01-01

    The chemical composition and biological properties of Ulva fasciata aqueous-ethanolic extract were examined. Five components were identified in one fraction prepared from the extract by gas chromatography-mass spectrometry, and palmitic acid and its ethyl ester accounted for 76% of the total identified components. Furthermore, we assessed the extract's antioxidant properties by using the DPPH, ABTS, and lipid peroxidation assays and found that the extract had a moderate scavenging effect. In an experiment involving preexposition and coexposition of the extract (1-500 µg/mL) and benzo[a]pyrene (BP), the extract was found to be nontoxic to C9 cells in culture and to inhibit the cytotoxicity induced by BP. As BP is biotransformed by CYP1A and CYP2B subfamilies, we explored the possible interaction of the extract with these enzymes. The extract (25-50 µg/mL) inhibited CYP1A1 activity in rat liver microsomes. Analysis of the inhibition kinetics revealed a mixed-type inhibitory effect on CYP1A1 supersome. The effects of the extract on BP-induced DNA damage and hepatic CYP activity in mice were also investigated. Micronuclei induction by BP and liver CYP1A1/2 activities significantly decreased in animals treated with the extract. The results suggest that Ulva fasciata aqueous-ethanolic extract inhibits BP bioactivation and it may be a potential chemopreventive agent.

  12. Gluconeogenesis from labeled carbon: estimating isotope dilution

    International Nuclear Information System (INIS)

    Kelleher, J.K.

    1986-01-01

    To estimate the rate of gluconeogenesis from steady-state incorporation of labeled 3-carbon precursors into glucose, isotope dilution must be considered so that the rate of labeling of glucose can be quantitatively converted to the rate of gluconeogenesis. An expression for the value of this isotope dilution can be derived using mathematical techniques and a model of the tricarboxylic acid (TCA) cycle. The present investigation employs a more complex model than that used in previous studies. This model includes the following pathways that may affect the correction for isotope dilution: 1) flux of 3-carbon precursor to the oxaloacetate pool via acetyl-CoA and the TCA cycle; 2) flux of 4- or 5-carbon compounds into the TCA cycle; 3) reversible flux between oxaloacetate (OAA) and pyruvate and between OAA and fumarate; 4) incomplete equilibrium between OAA pools; and 5) isotope dilution of 3-carbon tracers between the experimentally measured pool and the precursor for the TCA-cycle OAA pool. Experimental tests are outlined which investigators can use to determine whether these pathways are significant in a specific steady-state system. The study indicated that flux through these five pathways can significantly affect the correction for isotope dilution. To correct for the effects of these pathways an alternative method for calculating isotope dilution is proposed using citrate to relate the specific activities of acetyl-CoA and OAA

  13. Selective Liquid-Liquid Extraction of Lead Ions Using Newly Synthesized Extractant 2-(Dibutylcarbamoylbenzoic Acid

    Directory of Open Access Journals (Sweden)

    Hossein Soltani

    2015-12-01

    Full Text Available A new carboxylic acid extractant, named 2-(dibutylcarbamoylbenzoic acid, is prepared and its potential for selective solvent extraction and recovery of lead ions from industrial samples was investigated. The slope analysis indicated that the lead ions are extracted by formation of 1:2 metal to ligand complexes. The effect of the parameters influencing the extraction efficiency including kind of the organic diluent, extractant concentration, type of the salt used for ionic strength adjustment, contact time and temperature was evaluated and discussed. Under optimized conditions (aqueous phase: 5 ml, initial lead concentration 1 × 10-4 M, pH 4, sodium chloride 0.1 M; organic phase: 5 ml dichloromethane, ligand concentration 0.05 M, a quantitative (75.2 ± 0.8% and highly selective extraction of lead ions in the presence of zinc, nickel, cobalt and cadmium ions (each 1 × 10-4 M was achieved, after 20 min. magnetically stirring of the phases, at      25 °C. The extracted lead ions were stripped from the organic phase by diluted nitric acid (0.1 M solution. The proposed method was successfully applied for separation of lead from industrial samples. The study of the effect of temperature allowed evaluating the thermodynamic parameters of the extraction process of lead ions by the studied extractant into dichloromethane.

  14. Modeling and analysis of power extraction circuits for passive UHF RFID applications

    International Nuclear Information System (INIS)

    Fan Bo; Dai Yujie; Zhang Xiaoxing; Lue Yingjie

    2009-01-01

    Modeling and analysis of far field power extraction circuits for passive UHF RF identification (RFID) applications are presented. A mathematical model is derived to predict the complex nonlinear performance of UHF voltage multiplier using Schottky diodes. To reduce the complexity of the proposed model, a simple linear approximation for Schottky diode is introduced. Measurement results show considerable agreement with the values calculated by the proposed model. With the derived model, optimization on stage number for voltage multiplier to achieve maximum power conversion efficiency is discussed. Furthermore, according to the Bode-Fano criterion and the proposed model, a limitation on maximum power up range for passive UHF RFID power extraction circuits is also studied.

  15. Coacervative extraction as a green technique for sample preparation for the analysis of organic compounds.

    Science.gov (United States)

    Melnyk, A; Wolska, L; Namieśnik, J

    2014-04-25

    One of the present trends in analytical chemistry is miniaturization, which is one of the methods of green analytical chemistry application. A particular emphasis is placed on the elimination of the use of large amounts of organic solvents which are toxic and harmful to the environment, maintaining high efficiency of the extraction process, high recovery values and low values of quantification (LOQ) and detection (LOD) limits. These requirements are fulfilled by coacervative extraction (CAE) technique. In this review, theoretical aspects of the coacervation process are presented along with environmental and bioanalytical applications of this technique, its advantages, limitations and competitiveness with other techniques. Due to its simplicity and rapidity, CAE is an excellent alternative for currently practiced procedures of sample preparation for the analysis of organic compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Blind Extraction of Chaotic Signals by Using the Fast Independent Component Analysis Algorithm

    International Nuclear Information System (INIS)

    Hong-Bin, Chen; Jiu-Chao, Feng; Yong, Fang

    2008-01-01

    We report the results of using the fast independent component analysis (FastICA) algorithm to realize blind extraction of chaotic signals. Two cases are taken into consideration: namely, the mixture is noiseless or contaminated by noise. Pre-whitening is employed to reduce the effect of noise before using the FastICA algorithm. The correlation coefficient criterion is adopted to evaluate the performance, and the success rate is defined as a new criterion to indicate the performance with respect to noise or different mixing matrices. Simulation results show that the FastICA algorithm can extract the chaotic signals effectively. The impact of noise, the length of a signal frame, the number of sources and the number of observed mixtures on the performance is investigated in detail. It is also shown that regarding a noise as an independent source is not always correct

  17. Alcoholic extraction enables EPR analysis to characterize radiation-induced cellulosic signals in spices.

    Science.gov (United States)

    Ahn, Jae-Jun; Sanyal, Bhaskar; Akram, Kashif; Kwon, Joong-Ho

    2014-11-19

    Different spices such as turmeric, oregano, and cinnamon were γ-irradiated at 1 and 10 kGy. The electron paramagnetic resonance (EPR) spectra of the nonirradiated samples were characterized by a single central signal (g = 2.006), the intensity of which was significantly enhanced upon irradiation. The EPR spectra of the irradiated spice samples were characterized by an additional triplet signal at g = 2.006 with a hyperfine coupling constant of 3 mT, associated with the cellulose radical. EPR analysis on various sample pretreatments in the irradiated spice samples demonstrated that the spectral features of the cellulose radical varied on the basis of the pretreatment protocol. Alcoholic extraction pretreatment produced considerable improvements of the EPR signals of the irradiated spice samples relative to the conventional oven and freeze-drying techniques. The alcoholic extraction process is therefore proposed as the most suitable sample pretreatment for unambiguous detection of irradiated spices by EPR spectroscopy.

  18. Equivalent water height extracted from GRACE gravity field model with robust independent component analysis

    Science.gov (United States)

    Guo, Jinyun; Mu, Dapeng; Liu, Xin; Yan, Haoming; Dai, Honglei

    2014-08-01

    The Level-2 monthly GRACE gravity field models issued by Center for Space Research (CSR), GeoForschungs Zentrum (GFZ), and Jet Propulsion Laboratory (JPL) are treated as observations used to extract the equivalent water height (EWH) with the robust independent component analysis (RICA). The smoothing radii of 300, 400, and 500 km are tested, respectively, in the Gaussian smoothing kernel function to reduce the observation Gaussianity. Three independent components are obtained by RICA in the spatial domain; the first component matches the geophysical signal, and the other two match the north-south strip and the other noises. The first mode is used to estimate EWHs of CSR, JPL, and GFZ, and compared with the classical empirical decorrelation method (EDM). The EWH STDs for 12 months in 2010 extracted by RICA and EDM show the obvious fluctuation. The results indicate that the sharp EWH changes in some areas have an important global effect, like in Amazon, Mekong, and Zambezi basins.

  19. Antimicrobial activity of grapefruit seed and pulp ethanolic extract.

    Science.gov (United States)

    Cvetnić, Zdenka; Vladimir-Knezević, Sanda

    2004-09-01

    Antibacterial and antifungal activity of ethanolic extract of grapefruit (Citrus paradisi Macf., Rutaceae) seed and pulp was examined against 20 bacterial and 10 yeast strains. The level of antimicrobial effects was established using an in vitro agar assay and standard broth dilution susceptibility test. The contents of 3.92% of total polyphenols and 0.11% of flavonoids were determined spectrometrically in crude ethanolic extract. The presence of flavanones naringin and hesperidin in the extract was confirmed by TLC analysis. Ethanolic extract exibited the strongest antimicrobial effect against Salmonella enteritidis (MIC 2.06%, m/V). Other tested bacteria and yeasts were sensitive to extract concentrations ranging from 4.13% to 16.50% (m/V).

  20. Microbial diversity in fecal samples depends on DNA extraction method

    DEFF Research Database (Denmark)

    Mirsepasi, Hengameh; Persson, Søren; Struve, Carsten

    2014-01-01

    was to evaluate two different DNA extraction methods in order to choose the most efficient method for studying intestinal bacterial diversity using Denaturing Gradient Gel Electrophoresis (DGGE). FINDINGS: In this study, a semi-automatic DNA extraction system (easyMag®, BioMérieux, Marcy I'Etoile, France......BACKGROUND: There are challenges, when extracting bacterial DNA from specimens for molecular diagnostics, since fecal samples also contain DNA from human cells and many different substances derived from food, cell residues and medication that can inhibit downstream PCR. The purpose of the study...... by easyMag® from the same fecal samples. Furthermore, DNA extracts obtained using easyMag® seemed to contain inhibitory compounds, since in order to perform a successful PCR-analysis, the sample should be diluted at least 10 times. DGGE performed on PCR from DNA extracted by QIAamp DNA Stool Mini Kit DNA...

  1. Development of an extraction method for perchlorate in soils.

    Science.gov (United States)

    Cañas, Jaclyn E; Patel, Rashila; Tian, Kang; Anderson, Todd A

    2006-03-01

    Perchlorate originates as a contaminant in the environment from its use in solid rocket fuels and munitions. The current US EPA methods for perchlorate determination via ion chromatography using conductivity detection do not include recommendations for the extraction of perchlorate from soil. This study evaluated and identified appropriate conditions for the extraction of perchlorate from clay loam, loamy sand, and sandy soils. Based on the results of this evaluation, soils should be extracted in a dry, ground (mortar and pestle) state with Milli-Q water in a 1 ratio 1 soil ratio water ratio and diluted no more than 5-fold before analysis. When sandy soils were extracted in this manner, the calculated method detection limit was 3.5 microg kg(-1). The findings of this study have aided in the establishment of a standardized extraction method for perchlorate in soil.

  2. First Extraction of Transversity from a Global Analysis of Electron-Proton and Proton-Proton Data

    Science.gov (United States)

    Radici, Marco; Bacchetta, Alessandro

    2018-05-01

    We present the first extraction of the transversity distribution in the framework of collinear factorization based on the global analysis of pion-pair production in deep-inelastic scattering and in proton-proton collisions with a transversely polarized proton. The extraction relies on the knowledge of dihadron fragmentation functions, which are taken from the analysis of electron-positron annihilation data. For the first time, the transversity is extracted from a global analysis similar to what is usually done for the spin-averaged and helicity distributions. The knowledge of transversity is important for, among other things, detecting possible signals of new physics in high-precision low-energy experiments.

  3. Automatic extraction of soft tissues from 3D MRI head images using model driven analysis

    International Nuclear Information System (INIS)

    Jiang, Hao; Yamamoto, Shinji; Imao, Masanao.

    1995-01-01

    This paper presents an automatic extraction system (called TOPS-3D : Top Down Parallel Pattern Recognition System for 3D Images) of soft tissues from 3D MRI head images by using model driven analysis algorithm. As the construction of system TOPS we developed, two concepts have been considered in the design of system TOPS-3D. One is the system having a hierarchical structure of reasoning using model information in higher level, and the other is a parallel image processing structure used to extract plural candidate regions for a destination entity. The new points of system TOPS-3D are as follows. (1) The TOPS-3D is a three-dimensional image analysis system including 3D model construction and 3D image processing techniques. (2) A technique is proposed to increase connectivity between knowledge processing in higher level and image processing in lower level. The technique is realized by applying opening operation of mathematical morphology, in which a structural model function defined in higher level by knowledge representation is immediately used to the filter function of opening operation as image processing in lower level. The system TOPS-3D applied to 3D MRI head images consists of three levels. First and second levels are reasoning part, and third level is image processing part. In experiments, we applied 5 samples of 3D MRI head images with size 128 x 128 x 128 pixels to the system TOPS-3D to extract the regions of soft tissues such as cerebrum, cerebellum and brain stem. From the experimental results, the system is robust for variation of input data by using model information, and the position and shape of soft tissues are extracted corresponding to anatomical structure. (author)

  4. Forms of vitamin B12 in radioisotope dilution assays

    International Nuclear Information System (INIS)

    Begley, J.A.; Hall, C.A.

    1981-01-01

    Since the presence of analogues of vitamin B 12 (B 12 , cobalamin, Cbl) has been postulated as the basis for the high values obtained by some radioisotope dilution assays (RIDA) of serum Cbl, serum was examined for analogues. None could be demonstrated in the extracts of serum prepared for RIDA as sought by both direct and indirect techniques. The natural forms of serum Cbl were converted to cyanocobalamin (CN Cbl) by this process of extraction which included cyanide (CN). The correctly performed RIDA for Cbl based on R binder gave higher values than a RIDA based on intrinsic factor or than by bioassay. By exclusion, the difference appeared to be due to unidentified factors rather than the presence of analogues. (author)

  5. Freezing fecal samples prior to DNA extraction affects the Firmicutes to Bacteroidetes ratio determined by downstream quantitative PCR analysis

    DEFF Research Database (Denmark)

    Bahl, Martin Iain; Bergström, Anders; Licht, Tine Rask

    2012-01-01

    Freezing stool samples prior to DNA extraction and downstream analysis is widely used in metagenomic studies of the human microbiota but may affect the inferred community composition. In this study, DNA was extracted either directly or following freeze storage of three homogenized human fecal...

  6. Freezing fecal samples prior to DNA extraction affects the Firmicutes to Bacteroidetes ratio determined by downstream quantitative PCR analysis

    DEFF Research Database (Denmark)

    Bahl, Martin Iain; Bergström, Anders; Licht, Tine Rask

    Freezing stool samples prior to DNA extraction and downstream analysis is widely used in metagenomic studies of the human microbiota but may affect the inferred community composition. In this study DNA was extracted either directly or following freeze storage of three homogenized human fecal...

  7. Spectroscopic analysis of the role of extractives on heat-induced discoloration of black locust (Robinia pseudoacacia)

    Science.gov (United States)

    Yao Chen; Yongming Fan; Jianmin Gao; Mandla A. Tshabalala; Nicole M. Stark

    2012-01-01

    To investigate the role of extractives on heat-induced discoloration of wood, samples of black locust (Robinia pseudoacacia) wood flour were extracted with various solvents prior to heat-treatment. Analysis of their color parameters and chromophoric structures showed that the chroma value of the unextracted sample decreased while that of the...

  8. Multi-resolution analysis for region of interest extraction in thermographic nondestructive evaluation

    Science.gov (United States)

    Ortiz-Jaramillo, B.; Fandiño Toro, H. A.; Benitez-Restrepo, H. D.; Orjuela-Vargas, S. A.; Castellanos-Domínguez, G.; Philips, W.

    2012-03-01

    Infrared Non-Destructive Testing (INDT) is known as an effective and rapid method for nondestructive inspection. It can detect a broad range of near-surface structuring flaws in metallic and composite components. Those flaws are modeled as a smooth contour centered at peaks of stored thermal energy, termed Regions of Interest (ROI). Dedicated methodologies must detect the presence of those ROIs. In this paper, we present a methodology for ROI extraction in INDT tasks. The methodology deals with the difficulties due to the non-uniform heating. The non-uniform heating affects low spatial/frequencies and hinders the detection of relevant points in the image. In this paper, a methodology for ROI extraction in INDT using multi-resolution analysis is proposed, which is robust to ROI low contrast and non-uniform heating. The former methodology includes local correlation, Gaussian scale analysis and local edge detection. In this methodology local correlation between image and Gaussian window provides interest points related to ROIs. We use a Gaussian window because thermal behavior is well modeled by Gaussian smooth contours. Also, the Gaussian scale is used to analyze details in the image using multi-resolution analysis avoiding low contrast, non-uniform heating and selection of the Gaussian window size. Finally, local edge detection is used to provide a good estimation of the boundaries in the ROI. Thus, we provide a methodology for ROI extraction based on multi-resolution analysis that is better or equal compared with the other dedicate algorithms proposed in the state of art.

  9. Comparison of the methods for tissue triiodothyronine T(3) extraction and subsequent radioimmunoassay

    International Nuclear Information System (INIS)

    Takaishi, M.; Miyachi, Y.; Aoki, M.; Shishiba, Y.; Asahi Life Foundation, Tokyo

    1978-01-01

    Although there have been various reports on tissue T 3 concentration, the examination of the quality of radioimmunoassay has not been available. In the present study, we tried to determine whether the available methods for T 3 extraction are adequate for the various methods of T 3 radioimmunoassays used. T 3 was extracted from liver by ethanol extraction or by acid butanol extraction (Flock's method) and the extract was applied to radioimmunoassay either by Seralute T 3 column, ANS-double antibody or the ANS-charcoal method. The values of T 3 were compared with those obtained by isotope-equilibration method. The dilution curve of ethanol extract was not parallel with that of the standard in ANS-charcoal or ANS-double antibody technique. When the extract was tested by Seralate method, the dilution curve was parallel to the standard, whereas the T 3 value obtained with this method was two-fold higher than that with the isotope equilibration technique. The analysis of the ethanol extract suggested that the lipid extracted by ethanol interfered with the assay. The acid butanol extract when tested either by the ANS-double antibody or Seralate method, showed parallelism to the standard curve and gave T 3 values almost identical with those by the isotope-equilibration method. When tested by ANS-charcoal method, the dilution curve of the acid butanol extract was not parallel to the standard. Thus, to obtain reliable results, tissue extraction by Flock's method and subsequent T 3 radioimmunoassay by either ANS-double antibody or Seralate T 3 method are recommended. (author)

  10. Effect temperature of supercritical CO2 fluid extraction on phytochemical analysis and antioxidant activity of Zingiber officinale Roscoe

    Science.gov (United States)

    Sondari, Dewi; Irawadi, Tun Tedja; Setyaningsih, Dwi; Tursiloadi, Silvester

    2017-11-01

    Supercritical fluid extraction of Zingiber officinale Roscoe has been carried out at a pressure of 16 MPa, with temperatures between 20-40 °C, during extraction time of 6 hours and the flow rate of CO2 fluid 5.5 ml/min. The result of supercritical method was compared with the extraction maceration using a mixture of water and ethanol (70% v/v) for 24 hours. The main content in ginger that has a main role as an antioxidant is a gingerol compound that can help neutralize the damaging effects caused by free radicals in the body, as anti-coagulant, and inhibit the occurrence of blood clots. This study aims to determine the effect of temperature on chemical components contained in rough extract of Zingiber officinale Roscoe and its antioxidant activity, total phenol and total flavonoid content. To determine the chemical components contained in the crude extract of Zingiber officinale Roscoe extracted by supercritical fluid and maceration extraction, GC-MS analysis was performed. Meanwhile, the antioxidant activity of the extract was evaluated based on a 2.2-diphenyl-1-picrylhydrazyl (DPPH) free radical damping method. The results of the analysis show that the result of ginger extract by using the supercritical CO2 extraction method has high antioxidant activity than by using maceration method. The highest total phenol content and total flavonoids were obtained on ginger extraction using supercritical CO2 fluid extraction, indicating that phenol and flavonoid compounds contribute to antioxidant activity. Chromatographic analysis showed that the chemical profile of ginger extract containing oxygenated monoterpenes, monoterpene hydrocarbons, sesquiterpene hydrocarbons, oxygenated monoterpene gingerol and esters. In supercritical fluid extraction, the compounds that can be identified at a temperature of 20-40 °C contain 27 compounds, and 11 compounds from the result of maceration extract. The main component of Zingiber officinale Roscoe extracted using supercritical fluid

  11. Computation of dilution discharge and mean concentration of effluents in Beypore Estuary, west coast of India

    Digital Repository Service at National Institute of Oceanography (India)

    DineshKumar, P.K.; Josanto, V.; Sankaranarayanan, V.N.

    Tide dominated Beypore estuary along the west coast of India was studied to estimate the mean flow available for diluting the conservative effluents based on the distribution of ambient salinity as a guide through one dimensional analysis...

  12. Experiments made to separate the trace elements in seawater by extraction and their determination by neutron activation analysis

    International Nuclear Information System (INIS)

    Heuss, E.; Lieser, K.H.

    1979-01-01

    The problems of trace element determination in seawater by neutron activation analysis are discussed. Experiments with tri-n-octylphosphinoxide (TOPO) did not bring satisfactory results because of the strong interference of the bremsstrahlung from 32 P. Experiments with oxin at different pH showed that in each case only few elements are extracted in greater amounts. An extraction apparatus is described making possible the extraction of up to 10 l water by 50 ml of an organic solution. Extraction experiments using different complexing agents were satisfactory but the evaporation of the organic phase to dryness for irradiation was difficult. (author)

  13. Modifications to the SPS LSS6 Septa for LHC and the SPS Septa Diluters

    CERN Document Server

    Borburgh, Y; Goddard, B; Kadi, Y

    2006-01-01

    The Large Hadron Collider required the modification of the existing extraction channel in the long straight section (LSS) 6 of the CERN Super Proton Synchrotron (SPS), including the suppression of the electrostatic wire septa. The newly set up fast extraction will be used to transfer protons at 450 GeV/c as well as ions via the 2.9 km long transfer line TI 2 to Ring 1 of the LHC. The girder of the existing SPS DC septa was modified to accommodate a new septum protection element. Changes were also applied to the septum diluter in the fast extraction channel in LSS4, leading to the other LHC ring and the CNGS facility. The requirements and the layout of the new LSS6 extraction channel will be described including a discussion of the design and performance of the installed septum diluters.

  14. Consistent Feature Extraction From Vector Fields: Combinatorial Representations and Analysis Under Local Reference Frames

    Energy Technology Data Exchange (ETDEWEB)

    Bhatia, Harsh [Univ. of Utah, Salt Lake City, UT (United States)

    2015-05-01

    This dissertation presents research on addressing some of the contemporary challenges in the analysis of vector fields—an important type of scientific data useful for representing a multitude of physical phenomena, such as wind flow and ocean currents. In particular, new theories and computational frameworks to enable consistent feature extraction from vector fields are presented. One of the most fundamental challenges in the analysis of vector fields is that their features are defined with respect to reference frames. Unfortunately, there is no single “correct” reference frame for analysis, and an unsuitable frame may cause features of interest to remain undetected, thus creating serious physical consequences. This work develops new reference frames that enable extraction of localized features that other techniques and frames fail to detect. As a result, these reference frames objectify the notion of “correctness” of features for certain goals by revealing the phenomena of importance from the underlying data. An important consequence of using these local frames is that the analysis of unsteady (time-varying) vector fields can be reduced to the analysis of sequences of steady (timeindependent) vector fields, which can be performed using simpler and scalable techniques that allow better data management by accessing the data on a per-time-step basis. Nevertheless, the state-of-the-art analysis of steady vector fields is not robust, as most techniques are numerical in nature. The residing numerical errors can violate consistency with the underlying theory by breaching important fundamental laws, which may lead to serious physical consequences. This dissertation considers consistency as the most fundamental characteristic of computational analysis that must always be preserved, and presents a new discrete theory that uses combinatorial representations and algorithms to provide consistency guarantees during vector field analysis along with the uncertainty

  15. Gas Chromatography-Mass Spectrometry Analysis of Ulva fasciata (Green Seaweed Extract and Evaluation of Its Cytoprotective and Antigenotoxic Effects

    Directory of Open Access Journals (Sweden)

    Idania Rodeiro

    2015-01-01

    Full Text Available The chemical composition and biological properties of Ulva fasciata aqueous-ethanolic extract were examined. Five components were identified in one fraction prepared from the extract by gas chromatography-mass spectrometry, and palmitic acid and its ethyl ester accounted for 76% of the total identified components. Furthermore, we assessed the extract’s antioxidant properties by using the DPPH, ABTS, and lipid peroxidation assays and found that the extract had a moderate scavenging effect. In an experiment involving preexposition and coexposition of the extract (1–500 µg/mL and benzo[a]pyrene (BP, the extract was found to be nontoxic to C9 cells in culture and to inhibit the cytotoxicity induced by BP. As BP is biotransformed by CYP1A and CYP2B subfamilies, we explored the possible interaction of the extract with these enzymes. The extract (25–50 µg/mL inhibited CYP1A1 activity in rat liver microsomes. Analysis of the inhibition kinetics revealed a mixed-type inhibitory effect on CYP1A1 supersome. The effects of the extract on BP-induced DNA damage and hepatic CYP activity in mice were also investigated. Micronuclei induction by BP and liver CYP1A1/2 activities significantly decreased in animals treated with the extract. The results suggest that Ulva fasciata aqueous-ethanolic extract inhibits BP bioactivation and it may be a potential chemopreventive agent.

  16. Dilute solution, flow behavior, thixotropy and viscoelastic characterization of cress seed (Lepidium sativum) gum fractions

    DEFF Research Database (Denmark)

    Razmkhah, Somayeh; Razavi, Seyed Mohammad Ali; Mohammadifar, Mohammad Amin

    2017-01-01

    In this study, rheological properties of cress seed gum (CSG) and its fractions (F1, F2, F3; fractionated using stepwise extraction with water) were investigated. Cress seed gum and its fractions revealed random coil conformation in dilute regimes; chain flexibility and intrinsic viscosity...... indicated that CSG and the fractions exhibited significantly different rheological properties....

  17. Fifty years of solid-phase extraction in water analysis--historical development and overview.

    Science.gov (United States)

    Liska, I

    2000-07-14

    The use of an appropriate sample handling technique is a must in an analysis of organic micropollutants in water. The efforts to use a solid phase for the recovery of analytes from a water matrix prior to their detection have a long history. Since the first experimental trials using activated carbon filters that were performed 50 years ago, solid-phase extraction (SPE) has become an established sample preparation technique. The initial experimental applications of SPE resulted in widespread use of this technique in current water analysis and also to adoption of SPE into standardized analytical methods. During the decades of its evolution, chromatographers became aware of the advantages of SPE and, despite many innovations that appeared in the last decade, new SPE developments are still expected in the future. A brief overview of 50 years of the history of the use of SPE in organic trace analysis of water is given in presented paper.

  18. Simultaneous column chromatographic extraction and purification of abscisic acid in peanut plants for direct HPLC analysis.

    Science.gov (United States)

    Zhang, Ya-Wen; Fan, Wei-Wei; Li, Hui; Ni, He; Han, Han-Bing; Li, Hai-Hang

    2015-10-01

    Abscisic acid (ABA), a universal signaling molecule, plays important roles in regulating plant growth, development and stress responses. The low contents and complex components in plants make it difficult to be accurately analyzed. A novel one-step sample preparation method for ABA in plants was developed. Fresh peanut (Arachis hypogaea) plant materials were fixed by oven-drying, microwave drying, boiling or Carnoy's fixative, and loaded onto a mini-preparing column. After washed the impurities, ABA was eluted with a small amount of solvent. ABA in plant materials was completely extracted and purified in 2mL solution and directly analyzed by HPLC, with a 99.3% recovery rate. Multiple samples can be simultaneously prepared. Analyses using this method indicated that the endogenous ABA in oven-dried peanut leaves increased 20.2-fold from 1.01 to 20.37μgg(-1) dry weight within 12h and then decreased in 30% polyethylene glycol 6000 treated plants, and increased 3.34-fold from 0.85 to 2.84μgg(-1) dry weight in 5 days and then decreased in soil drought treated plants. The method combined the column chromatographic extraction and solid-phase separation technologies in one step and can completely extracted plant endogenous ABA in a purified and highly concentrated form for direct HPLC analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Extraction of Coal and Gangue Geometric Features with Multifractal Detrending Fluctuation Analysis

    Directory of Open Access Journals (Sweden)

    Kai Liu

    2018-03-01

    Full Text Available The separation of coal and gangue is an important process of the coal preparation technology. The conventional way of manual selection and separation of gangue from the raw coal can be replaced by computer vision technology. In the literature, researc