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Sample records for gas-liquid chromatography analysis

  1. Gas-liquid chromatography in lunar organic analysis.

    NASA Technical Reports Server (NTRS)

    Gehrke, C. W.

    1972-01-01

    Gas-liquid chromatography (GLC) is a powerful and sensitive method for the separation and detection of organic compounds at nanogram levels. The primary requirement for successful analyses is that the compounds of interest must be volatile under the chromatographic conditions employed. Nonvolatile organic compounds must be converted to volatile derivatives prior to analysis. The derivatives of choice must be both amenable to chromatographic separation and be relatively stable. The condition of volatility necessitates the development of efficient derivatization reactions for important groups of compounds as amino acids, carbohydrates, nucleosides, etc. Trimethylsilylation and trifluoroacetylation represent specific areas of recent prominence. Some relevant practical aspects of GLC are discussed.

  2. Mixed Stationary Liquid Phases for Gas-Liquid Chromatography.

    ERIC Educational Resources Information Center

    Koury, Albert M.; Parcher, Jon F.

    1979-01-01

    Describes a laboratory technique for use in an undergraduate instrumental analysis course that, using the interpretation of window diagrams, prepares a mixed liquid phase column for gas-liquid chromatography. A detailed procedure is provided. (BT)

  3. Quantification of milk fat in chocolate fats by triacylglycerol analysis using gas-liquid chromatography.

    PubMed

    Buchgraber, Manuela; Androni, Simona; Anklam, Elke

    2007-05-02

    The development and in-house testing of a method for the quantification of milk fat in chocolate fats is described. A database consisting of the triacylglycerol profiles of 310 genuine milk fat samples from 21 European countries and 947 mixtures thereof with chocolate fats was created under a strict quality control scheme using 26 triacylglycerol reference standards for calibration purposes. Out of the individual triacylglycerol fractions obtained, 1-palmitoyl-2-stearoyl-3-butyroyl-glycerol (PSB) was selected as suitable marker compound for the determination of the proportion of milk fat in chocolate fats. By using PSB values from the standardized database, a calibration function using simple linear regression analysis was calculated to be used for future estimations of the milk fat content. A comparison with the widely used butyric acid method, which is currently used to determine the milk fat content in nonmilk fat mixtures, showed that both methods were equivalent in terms of accuracy. The advantage of the presented approach is that for further applications, i.e., determination of foreign fats in chocolate fats, just a single analysis is necessary, whereas for the same purpose, the C4 method requires two different analytical methods.

  4. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  5. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  6. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  7. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  8. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from...

  9. Gas-liquid chromatography of fecal neutral steriods.

    PubMed

    Gerhardt, K O; Gehrke, C W; Rogers, I T; Flynn, M A; Hentges, D J

    1977-05-21

    A method is described for the analysis of fecal neutral steriods with a dual-column gas-liquid chromatography (GLC) system. After saponification of the fecal slurry, the neutral steroids were extracted with hexane. The GLC separation of the compounds and quantitation were achieved by simultaneous injection of the derivatized and derivatized aliquots of the extract onto dual colmuns under identical conditions. The neutral steroids of interest were than identified by matching the retention times with those of known standards, and identification was confirmed by use of an interfaced GLC high-resolution mass spectrometry system. The detection limit was 0.003 mg of steroid/g of fecal slurry. The pricision of the method is illustrated by a relative standard diviation of 2-10% and a recovery of neutral steroids from 73-96%. The method was applied to the determination of fecal neutral steroids in a "High protein diet in colon cancer study". A considerably larger level of coprostanone than of coprostanol was observed. Data on neutral steroids in fecal samples from subjects on different diets are the subject of a separate publication.

  10. Identification of polychlorinated styrene compounds in heron tissues by gas-liquid chromatography-mass spectrometry.

    PubMed

    Reichel, W L; Prouty, R M; Gay, M L

    1977-01-01

    Unknown compounds detected in Ardea herodias tissues are identified by gas-liquid chromatography-mass spectrometry as residues of octachlorostyrene. Heptachlorostyrene and hexachlorostyrene were tentatively identified.

  11. Identification of polychlorinated styrene compounds in heron tissues by gas-liquid chromatography-mass spectrometry

    USGS Publications Warehouse

    Reichel, W.L.; Prouty, R.M.; Gay, M.L.

    1977-01-01

    Unknown compounds detected in Ardea herodias tissues are identified by gas-liquid chromatography-mass spectrometry as residues of octachlorostyrene. Heptachlorostyrene and hexachlorostyrene were tentatively identified.

  12. Combining NMR Spectroscopy and Gas-Liquid Chromatography for Analysis of the Fatty Acid Composition of Fenugreek Seed Oil (Trigonella foenum graecum L.)

    NASA Astrophysics Data System (ADS)

    Skakovskii, E. D.; Tychinskaya, L. Yu.; Mauchanava, V. A.; Karankevich, E. G.; Lamotkin, S. A.; Ahabalayeva, A. D.; Reshetnikov, V. N.

    2013-11-01

    1H and 13C NMR spectroscopy established that fenugreek seed oil consists mainly of triacylglycerides. Oleic and linoleic acids are found preferentially in the 2 position and α-linolenic acid is found preferentially in the 1,3 positions of the glycerol backbone. By combining NMR and gas-liquid chromatography, we have shown that fenugreek seeds contain 5.5 %-6.8 % oil, consisting mainly of unsaturated fatty acids (68.2 %-82.1 %): linoleic (31.3 %-46.8 %), α-linolenic (15.1 %-36.6 %), and oleic (11.6 %-21.3 %). The highest unsaturated fatty acid content is found in the cultivars D-19, Ovary Gold, Blidet, Ovary 4 and the lowest fatty acid content is found in the Metha cultivar. The percentage of polyunsaturated fatty acids is higher in oils of fenugreek cultivars from northern regions (Belarus, Hungary, France).

  13. Preparation of pure microbiological samples for pyrolysis gas-liquid chromatography studies

    NASA Technical Reports Server (NTRS)

    Oxborrow, G. S.; Fields, N. D.; Puleo, J. R.

    1976-01-01

    Bacterial samples were prepared for pyrolysis gas-liquid chromatography using cells grown on membrane filters. Pyrochromatograms were reproducible when cells harvested from the filters were pyrolyzed without being washed.

  14. Identification of the botanical origin of pine nuts found in food products by gas-liquid chromatography analysis of fatty acid profile.

    PubMed

    Destaillats, Frédéric; Cruz-Hernandez, Cristina; Giuffrida, Francesca; Dionisi, Fabiola

    2010-02-24

    Pine nuts are traditionally used in various part of the world for the preparation of desserts or sauces or in salads. Local production is not sufficient to cope with the high demand of pine nuts around the world, and countries such as China or Pakistan are exporting much of their production to Western countries. Almost all the nuts that are traditionally consumed belong to the Pinus genus, but over the past years, the number of consumer complaints following consumption of commercial pine nuts increased. Some consumers experienced taste disturbance lasting for up to two weeks after consumption. Food safety agencies raised some concerns regarding pine nuts imported from Asia and their association with taste disturbance. However, even though a formal association has not been found to date, the Pinus genus comprises species that are not classified as edible and could be eventually used to adulterate edible species. Pinus spp. seed lipids are known to contain very specific polyunsaturated fatty acids know as Delta5-olefinic acids. Seed fatty acid profile of conifers had been used in the past as a taxonomic marker, and in the present study to identify the botanical origin of pine nut in nine commercial products. Fast gas-liquid chromatography (GLC) was used to resolve the complete fatty acid profile of Pinus spp. samples in less than 5 min. A diagnostic index based on the relative levels of the main fatty acids including distinctive Delta5-olefinic acids was used to identify botanical origins. Results revealed the occurrence of the following Pinus spp. in commercial products: P. pinea, P. koraiensis, P. gerardiana, P. armandii and P. massoniana. The later two species, known as Chinese white pine and Chinese red pine, are only cultivated in China and are not listed as common source of edible pine nuts by the Food and Agriculture Organization (FAO). The present study shows that the botanical origin of pine nuts can be identified in products based on the fatty acid profile.

  15. Resolution of diacylglycerol moieties of natural glycerophospholipids by gas-liquid chromatography on polar capillary columns.

    PubMed

    Myher, J J; Kuksis, A

    1982-06-01

    A rapid and practical method has been developed for the gas-liquid chromatographic determination of the sn-1,2-diacylglycerol moieties of natural glycerophospholipids using polar wall-coated open tubular columns. The method gives complete resolution and quantitative estimates for all species according to molecular weight and degree of unsaturation, including stearoyl docosahexaenoylglycerol and related polyunsaturates. For this purpose the sn-1,2-diacylglycerols are obtained from the glycerophospholipids by hydrolysis with phospholipase C and are converted into the trimethylsilyl or tertiary-butyldimethylsilyl ethers. The silyl ethers are separated by gas-liquid chromatography on the capillary glass columns coated with a polar cyanopropylsiloxane polymer, in the temperature range 175-250 degrees C, using hydrogen as the carrier gas. Practical applications of the method are illustrated by analyses of the sn-1,2-diacylglycerol moieties of the phosphatidylcholines of soybean phosphatides, egg yolk, and rat liver. The method of analysis is applicable to other classes of glycerophospholipids and the total time requirements for the analysis of any one phospholipid class are comparable to those for a fatty acid analysis.

  16. Application of gas-liquid chromatography and high-performance liquid chromatography to the analysis of trace amounts of salicylic acid, acetylsalicylic anhydride and acetylsalicylsalicylic acid in aspirin samples and aspirin formulations.

    PubMed

    Ali, S L

    1976-11-03

    The gas-liquid chromatographic (GLC) determination of salicylic acid (SA) in 12 commercial acetylsalicylic acid (aspirin, ASA) samples and 12 ASA formulations is reported. The GLC determination of SA as an impurity in ASA, utilising methylation with methyl iodide in the presence of potassium carbonate, requires a column chromatographic separation of SA prior to derivatization. Trace amounts of SA in ASA have also been determined by high-performance liquid chromatography (HPLC) on a Sil-X-I adsorption column using light petroleum-ethyl acetate-acetic acid as the mobile phase. Acetylsalicylic anhydride (ASN) and acetylsalicylsalicylic acid (ASSA) were determined by HPLC on a reversed-phase C18 column with water-methanol mixtures as the mobile phase. GLC was also applied to the determination of ASN as an impurity in ASA formulations.

  17. The Separation and Identification of Straight Chain Hydrocarbons: An Experiment Using Gas-Liquid Chromatography.

    ERIC Educational Resources Information Center

    Benson, G. A.

    1982-01-01

    An experiment using gas-liquid chromatography is discussed, introducing the student to concept of dead volume and its measurement, idea and use of an internal reference compound, and to linear relationship existing between measurements of a separation on two different stationary phases. (Author/SK)

  18. Rapid differentiation of the major causative agents of bacterial meningitis by use of frequency-pulsed electron capture gas-liquid chromatography: analysis of amines.

    PubMed

    Brooks, J B; Kellogg, D S; Shepherd, M E; Alley, C C

    1980-01-01

    The major causative agents of bacterial meningitis (Haemophilus influenzae serogroup B, Neisseria meningitidis serogroups B and C, Klebsiella pneumoniae, Steptococcus pneumoniae, and two types of Escherichia coli) were cultured in a chemically defined medium, and selected strains were further studied in Todd-Hewitt medium. After acidic extraction of the spent media with chloroform, a basic extraction was made with chloroform to obtain amines. A third extraction was performed on re-acidified Todd-Hewitt medium with ethyl ether to obtain hydroxyacids. The extracts were derivatized with heptafluorobutyric anhydride-ethanol to form electron-capturing derivatives, and the derivatives were analyzed on a frequency-pulsed electron capture gas-liquid chromatograph (FPEC-GLC) equipped with a PEP-2 computer. The data obtained from the study showed that amines were produced by these organisms that formed characteristic patterns. Different serotypes of K. pneumoniae and the two serogroups of N. meningitidis produced different types of FPEC-GLC profiles within serotypes. E. coli produced several hydroxy acids on Todd-Hewitt medium that made it unique among the organisms studied. The methods used are practical and the techniques have potential for use in clinical laboratories and hospitals as a valuable aid for the rapid identification of the major causative agents of bacterial meningitis.

  19. Pyrolysis-gas-liquid chromatography of fungi: differentiation of species and strains of several members of the Aspergillus flavus group.

    PubMed

    Vincent, P G; Kulik, M M

    1970-12-01

    Four fungi of the Aspergillus flavus group were differentiated to the species level and strain level by pyrolysis-gas-liquid chromotography. Comparisons of pyrochromatograms revealed more similarities than dissimilarities among both species and strains in the pyrolytic elution patterns. Quantitative analysis was made by comparing the number of peaks in which two strains or reference species agreed or disagreed, the degree of superimposability between the pyrolytic elution patterns of strains and reference species, and the presence or absence of peaks for strain pairs within each species. The accuracy and precision of these techniques suggest that pyrolysis-gas-liquid chromatography may have wide application in the detection, enumeration, and identification of fungi by nonmycologically trained personnel.

  20. Gas-liquid chromatography in routine processing of blood cultures for detecting anaerobic bacteraemia.

    PubMed Central

    Reig, M; Molina, D; Loza, E; Ledesma, M A; Meseguer, M A

    1981-01-01

    Gas-liquid chromatography was performed on 233 positive blood cultures and findings were compared with culture results. Obligate anaerobic bacteria were recovered from 78 out of 79 blood cultures containing butyric or iso-valeric acids, or both; from 28 out of 69 blood cultures containing succinic acid; and from only one out of 41 blood cultures containing succinic but not butyric or iso-valeric acid. Good correlations (88%) were found for the recovery of anaerobic bacteria and the detection of butyric and/or iso-valeric acids. Detecting volatile fatty acids by gas-liquid chromatography performed on blood cultures at the first signs of growth can therefore provide an early and reliable indication of the presence of anaerobic bacteria. PMID:7014645

  1. Pyrolysis gas-liquid chromatography of the genus Bacillus: effect of growth media on pyrochromatogram reproducibility.

    PubMed

    Oxborrow, G S; Fields, N D; Puleo, J R

    1977-04-01

    Pyrolysis gas-liquid chromatography was performed on dried Bacillus microorganisms to evaluate the effects of growth media. Six cultures of Bacillus and six lot numbers of Trypticase soy agar (BBL) were used to test the hypothesis that a microorganism grown on various lot numbers of the same chromatogram. Also tested was the effect of three different media on chromatogram reproduction using the same six cultures. Results show little or no differences observed between the chromatograms of the individual Bacillus spp. grown on the six lot numbers of Trypticase soy agar. When chromatograms of the three different media were compared, several differences were observed, particularly in the areas most characteristic of individual species. Pryolysis gas-liquid chromatography can be a useful tool for the characterization or identification of the genus Bacillus if the chromatographic and cultural conditions are maintained.

  2. The sugar spectrum of human cholesterol gallstones, mixed and pigment gallstones: combined quantitative analysis of neutral sugars, N-acetylhexosamines, hexuronic and N-acetylneuraminic acids by capillary gas-liquid chromatography.

    PubMed

    Sabinski, F; Wosiewitz, U

    1984-07-01

    Glycoproteins were investigated in different types of biliary calculi by a methanolysis procedure of the carbohydrate moiety, the formation of 2,6-dinitro-4-trifluoromethylbenzenesulphonate derivatives of N-acetylhexosamines and N-acetylneuraminic acid, followed by separation, identification and quantification of the liberated monosaccharides using capillary gas-liquid chromatography. This indirect method avoids several analytical problems caused by the presence of bile pigment derivatives; unless these are carefully removed they interfere strongly in the measurement of protein. The carbohydrate contents were much higher in pigment stones than in cholesterol and mixed stones. Rhamnose, a non-mammalian monosaccharide, was identified in most samples, but was significant increased in pigment stones, indicating a bacterial history of this stone type.

  3. Use of Gas-Liquid Chromatography to Determine the End Products of Growth of Lactic Acid Bacteria

    PubMed Central

    Thornhill, Patrick J.; Cogan, Timothy M.

    1984-01-01

    A simple gas-liquid chromatographic procedure for analyzing ethanol, acetic acid, acetoin, and racemic and meso-2,3-butylene glycol in broth media is described. Overnight broth cultures were filtered or centrifuged, and the filtrate or supernatant was treated with formic acid to aid separation of volatile fatty acids. Samples were then directly analyzed by gas-liquid chromatography on a 20% Tween 80-Chromosorb W-AW column and propionic acid as an internal standard. A complete analysis took ca. 8 min. The method can be used to distinguish homofermentative from heterofermentative lactic acid bacteria based on the level of ethanol produced and citrate-utilizing from non-citrate-utilizing lactic acid bacteria based on the levels of acetic acid produced. The method also has potential in distinguishing other bacterial fermentations. Of the 13 species of lactic acid bacteria tested, Streptococcus lactis subsp. diacetylactis was the major producer of 2,3-butylene glycol (total range, 0.3 to 3.5 mM), and, except for strain DRC1, both the racemic and meso isomers were produced in approximately equal amounts. PMID:16346562

  4. Gas-liquid chromatography-mass spectrometry of synthetic ceramides containing phytosphingosine.

    PubMed

    Hammarström, S

    1970-05-01

    Ceramides containing phytosphingosine as base and one of the fatty acids 16:0, 18:0, 20:0, 22:0, 23:0, and 24:0, were prepared by direct coupling in the presence of a mixed carbodiimide. The ceramides were analyzed as the 1,3,4-tri-O-trimethylsilyl ether derivatives by gas-liquid chromatography-mass spectrometry. Gas chromatographic data is presented, and structures of mass spectral ions are suggested. The structures are supported by mass spectra of the homologous ceramides, by deuterium-labeling experiments, and by high resolution mass spectrometry. Some ions, formed by cleavage between C-3 and C-4 in the long-chain base, indicate the phytosphingosine nature of the ceramide.

  5. [Rapid simultaneous assay of the principalamide-type local anesthetics by gas-liquid chromatography].

    PubMed

    Desch, G; Cavadore, D; Jullien, Y; Mercier, L; Descomps, B; de Rodez, M

    1981-01-01

    This method can assay simultaneously, using 300 microliters of plasma, of the three principle local anesthetic agents used by peridural injection for post-operative anesthesia and analgesia: xylocaïne, etidocaïne, bupivacaïne. The assay method consists of three steps: (a) the addition of an internal calibrating agent (mepivacaïne). (b) defecation using trichlorocetic acid. (c) alcalinization of the supernatent (pH 11), extraction with dichloromethane and concentration at room temperature of the organic phase. (d) chromotography using an SE 30 or OV 17 impregnated column. The method is sensitive between 0.37 mumoles per l-1 (0.1 microgram . ml-1) and the coefficient for the mean deviation is 10.9% for concentration between 0.37 mumoles 1-1 and 75 mumole1-1 (0.1 microgram . ml-1 and 20 micrograms . ml-1). The correspondence of the figures recorded in this large concentration range without any change in the technique means that the kinetics of the plasma concentrations before and after peridural injection can be followed. The results obtained by gas liquid chromatography for the assay of lidocaïne were compared in 115 different plasma samples with concentrations obtained by an immuno enzymatic method ("EMIT") fitted to a centrifuge analyser. The correlation coefficient between the two methods was: (r = 0.95 with y = 0.09 x +0.25 microgram . ml-1 implying the absence of any interference and the specificity of the two methods. The columns also separate in 20 minutes the two main metabolites of lidocaïne: monoethylglycinexylidide (M.E.G.X.) and glycinexylidide (G.X.). These results demonstrate that continuous peridural injection of lidocaïne produces a high plasma concentration without any clinical toxic phenomena.

  6. Analysis of Developing Gas/liquid Two-Phase Flows

    SciTech Connect

    Elena A. Tselishcheva; Michael Z. Podowski; Steven P. Antal; Donna Post Guillen; Matthias Beyer; Dirk Lucas

    2010-06-01

    The goal of this work is to develop a mechanistically based CFD model that can be used to simulate process equipment operating in the churn-turbulent regime. The simulations were performed using a state-of-the-art computational multiphase fluid dynamics code, NPHASE–CMFD [Antal et al,2000]. A complete four-field model, including the continuous liquid field and three dispersed gas fields representing bubbles of different sizes, was first carefully tested for numerical convergence and accuracy, and then used to reproduce the experimental results from the TOPFLOW test facility at Forschungszentrum Dresden-Rossendorf e.V. Institute of Safety Research [Prasser et al,2007]. Good progress has been made in simulating the churn-turbulent flows and comparison the NPHASE-CMFD simulations with TOPFLOW experimental data. The main objective of the paper is to demonstrate capability to predict the evolution of adiabatic churn-turbulent gas/liquid flows. The proposed modelling concept uses transport equations for the continuous liquid field and for dispersed bubble fields [Tselishcheva et al, 2009]. Along with closure laws based on interaction between bubbles and continuous liquid, the effect of height on air density has been included in the model. The figure below presents the developing flow results of the study, namely total void fraction at different axial locations along the TOPFLOW facility test section. The complete model description, as well as results of simulations and validation will be presented in the full paper.

  7. Multi-scale symbolic time reverse analysis of gas-liquid two-phase flow structures

    NASA Astrophysics Data System (ADS)

    Wang, Hongmei; Zhai, Lusheng; Jin, Ningde; Wang, Youchen

    Gas-liquid two-phase flows are widely encountered in production processes of petroleum and chemical industry. Understanding the dynamic characteristics of multi-scale gas-liquid two-phase flow structures is of great significance for the optimization of production process and the measurement of flow parameters. In this paper, we propose a method of multi-scale symbolic time reverse (MSTR) analysis for gas-liquid two-phase flows. First, through extracting four time reverse asymmetry measures (TRAMs), i.e. Euclidean distance, difference entropy, percentage of constant words and percentage of reversible words, the time reverse asymmetry (TRA) behaviors of typical nonlinear systems are investigated from the perspective of multi-scale analysis, and the results show that the TRAMs are sensitive to the changing of dynamic characteristics underlying the complex nonlinear systems. Then, the MSTR analysis is used to study the conductance signals from gas-liquid two-phase flows. It is found that the multi-scale TRA analysis can effectively reveal the multi-scale structure characteristics and nonlinear evolution properties of the flow structures.

  8. Determination of hexachloro-1,3-butadiene in spinach, eggs, fish, and milk by electron capture gas-liquid chromatography.

    PubMed

    Yurawecz, M P; Dreifuss, P A; Kamps, L R

    1976-05-01

    Hexachloro-1,3-butadiene (HCBD), a waste product formed in the manufacture of perchloroethylene and trichloroethylene, has been found in fish from the lower Mississippi River basin. The AOAC official method for organochlorine pesticide residues in fatty and nonfatty foods has been modified for the determination of HCBD residues in selected food commodities. Acetonitrile extracts of nonfatty foods, or the combined acetonitrile extracts obtained in acetonitrile-petroleum ether partitioning of fat isolated from fatty foods, are diluted with water and extracted with petroleum ether. The petroleum ether extracts are chromatographed on Florisil and HCBD is eluted with petroleum ether. The elute is analyzed by gas-liquid chromatography with an electron capture detector. Average recoveries of HCBD from fortified samples of fatty and nonfatty foods were greater than 90% in the interlaboratory trials of the method.

  9. Use of gas liquid chromatography as an adjunct to conventional bacteriological methods in the diagnosis of anaerobic cerebral abscess.

    PubMed

    Pit, S; Jamal, F; Cheah, F K; Abbas, M A

    1991-07-01

    Forty cases of cerebral abscesses were studied prospectively to establish the microbial agents implicated in these cases. Chronic otitis media (14 patients, 35%), congenital heart disease (five patients, 12.5%),a and meningitis (five patients, 12.5%) were among the important predisposing factors. Streptococcus (14 patients, 35%) was the most common causative pre-isolated, the predominant species being Streptococcus milleri (11 patients, 27.5%). Other organisms isolated included Proteus mirabilis in six patients (15%) and Staphylococcus aureus in five patients (12.5%). Anaerobes (12 patients, 30%), predominantly Bacteroides sp. (eight patients, 20%), played an important role in these cases, the majority of which were isolated in mixed cultures. Gas-liquid chromatographic analysis of pus detected the presence of anaerobes in another 11 cases of cerebral abscess, in which cultures of anaerobes were negative. Therefore, gas-liquid chromotography is useful as an adjunct to conventional bacteriological methods in providing a rapid and sensitive means of detecting anaerobes in pus obtained especially from patients who had received antibiotic therapy prior to hospitalization.

  10. Capillary gas-liquid chromatography separation of phenethylamines in amphetamine-positive urine samples.

    PubMed

    DePace, A; Verebey, K; elSohly, M

    1990-11-01

    Good gas chromatography (GC) separation of molecules is essential for clean gas chromatography/mass spectrometry (GC/MS) confirmation of compounds. The trifluoro derivatives of ephedrine (E) and methamphetamine (MA) coelute on dimethyl silicone capillary columns, such as DB-1, which are most commonly used by chromatographers. Methods are described to separate E and MA to aid GC/MS confirmations of methamphetamine, ephedrine, or both E and MA together, whichever may be present in Enzyme Immunoassay (EIA)-analyzed amphetamine-positive urine samples. The use of the heptafluoro derivatives of E and MA on a DB-1 column, or the trifluoro derivatives of E and MA on a DB-17 column, is suggested for good gas chromatographic separation.

  11. Simulating Retention in Gas-Liquid Chromatography: Benzene, Toluene, and Xylene Solutes

    SciTech Connect

    WICK,COLLIN D.; MARTIN,MARCUS G.; SIEPMANN, J. ILJA; SCHURE,MARK R.

    2000-07-12

    Accurate predictions of retention times, retention indices, and partition constants are a long sought-after goal for theoretical studies in chromatography. Although advances in computational chemistry have improved the understanding of molecular interactions, little attention has been focused on chromatography, let alone calculations of retention properties. Configurational-bias Monte Carlo simulations in the isobaric-isothermal Gibbs ensemble were used to investigate the partitioning of benzene, toluene, and the three xylene isomers between a squalane liquid phase and a helium vapor phase. The united-atom representation of the TraPPE (Transferable Potentials for Phase Equilibria) force field was used for all solutes and squalane. The Gibbs free energies of transfer and Kovats retention indices of the solutes were calculated directly from the partition constants (which were averaged over several independent simulations). While the calculated Kovats indices of benzene and toluene at T = 403 K are significantly higher than their experimental counterparts, much better agreement is found for the xylene isomers at T = 365 K.

  12. Detection and quantification of cocoa butter equivalents in cocoa butter and plain chocolate by gas liquid chromatography of triacylglycerols.

    PubMed

    Buchgraber, Manuela; Senaldi, Chiara; Ulberth, Franz; Anklam, Elke

    2004-01-01

    The development and in-house testing of a method for the detection and quantification of cocoa butter equivalents in cocoa butter and plain chocolate is described. A database consisting of the triacylglycerol profile of 74 genuine cocoa butter and 75 cocoa butter equivalent samples obtained by high-resolution capillary gas liquid chromatography was created, using a certified cocoa butter reference material (IRMM-801) for calibration purposes. Based on these data, a large number of cocoa butter/cocoa butter equivalent mixtures were arithmetically simulated. By subjecting the data set to various statistical tools, reliable models for both detection (univariate regression model) and quantification (multivariate model) were elaborated. Validation data sets consisting of a large number of samples (n = 4050 for detection, n = 1050 for quantification) were used to test the models. Excluding pure illipé fat samples from the data set, the detection limit was determined between 1 and 3% foreign fat in cocoa butter. Recalculated for a chocolate with a fat content of 30%, these figures are equal to 0.3-0.9% cocoa butter equivalent. For quantification, the average error for prediction was estimated to be 1.1% cocoa butter equivalent in cocoa butter, without prior knowledge of the materials used in the blend corresponding to 0.3% in chocolate (fat content 30%). The advantage of the approach is that by using IRMM-801 for calibration, the established mathematical decision rules can be transferred to every testing laboratory.

  13. Detection of metabolites by frequency-pulsed electron capture gas-liquid chromatography in serum and cerebrospinal fluid of a patient with Nocardia infection.

    PubMed

    Brooks, J B; Kasin, J V; Fast, D M; Daneshvar, M I

    1987-02-01

    Serum (SR) and cerebrospinal fluid (CSF) from a patient suspected of having tuberculous meningitis were submitted to our laboratory for analysis by frequency-pulsed electron capture gas-liquid chromatography (FPEC GLC). The samples were tested for the presence of carboxylic acids, alcohols, hydroxy acids, and amines by methods described previously (C. C. Alley, J. B. Brooks, and D. S. Kellogg, Jr., J. Clin. Microbiol. 9:97-102, 1977; J. B. Brooks, C. C. Alley, and J. A. Liddle, Anal. Chem. 46:1930-1934, 1974; J. B. Brooks, D. S. Kellogg, Jr., M. E. Shepherd, and C. C. Alley, J. Clin. Microbiol. 11:45-51, 1980; J. B. Brooks, D. S. Kellogg, Jr., M. E. Shepherd, and C. C. Alley, J. Clin. Microbiol. 11:52-58, 1980). The results were different from previous FPEC GLC profiles of SR and CSF from patients with known tuberculous meningitis. Both the SR and CSF contained several unidentified compounds that were not previously detected in tuberculous meningitis or any of our other studies of body fluids. Nocardia brasiliensis was later isolated from the patient. Detection of these metabolites by FPEC GLC could prove to be useful for rapid diagnosis of Nocardia disease, and their identification will provide a better understanding of metabolites produced by Nocardia sp. in vivo.

  14. [Identification of components of the milky juice of Lactarius pergamenus (Fr.)Fr fungi by gas-liquid chromatography/mass spectrometry].

    PubMed

    Tsyvins'ka, M V; Panchak, L V; Stoĭka, R S; Antoniuk, V O

    2013-01-01

    The authors have proposed method of separation of methanol extract of Lactarius pergamenus basidiomes and investigation of fractions extracted with hexane which, according to our previous studies, possess the highest antiproliferative and antifungal activity. Main attention was given to fractionation and analysis by gas-liquid chromatography-mass spectrometry (GLC/MS) of the fraction 1.4 extracted with hexane. The key role in separation of this fraction was played by the use of dioxane which mixes well with both polar and nonpolar solvents (hexane, chloroform, methanol, water). Chemical composition of hexanoic fraction of methanol extract of dried basidomes Lactarius pergamenus fungi were completely characterized. It was found that this fraction consisted of 38% of fatty acids and their derivatives, 29%--of the phthalates, 13%--of the sesquiterpene, 2%--of aldehydes and 18%--of other compounds (hydrocarbons, alcohols, hydrazine derivatives and unidentified substances). Such combination of constituents allows forming a stable emulsion of milky juice which protects the mushroom fruit body from the bacterial and fungal infections and from eating by the mammalians and insects.

  15. Multi-Scale Morphological Analysis of Conductance Signals in Vertical Upward Gas-Liquid Two-Phase Flow

    NASA Astrophysics Data System (ADS)

    Lian, Enyang; Ren, Yingyu; Han, Yunfeng; Liu, Weixin; Jin, Ningde; Zhao, Junying

    2016-11-01

    The multi-scale analysis is an important method for detecting nonlinear systems. In this study, we carry out experiments and measure the fluctuation signals from a rotating electric field conductance sensor with eight electrodes. We first use a recurrence plot to recognise flow patterns in vertical upward gas-liquid two-phase pipe flow from measured signals. Then we apply a multi-scale morphological analysis based on the first-order difference scatter plot to investigate the signals captured from the vertical upward gas-liquid two-phase flow loop test. We find that the invariant scaling exponent extracted from the multi-scale first-order difference scatter plot with the bisector of the second-fourth quadrant as the reference line is sensitive to the inhomogeneous distribution characteristics of the flow structure, and the variation trend of the exponent is helpful to understand the process of breakup and coalescence of the gas phase. In addition, we explore the dynamic mechanism influencing the inhomogeneous distribution of the gas phase in terms of adaptive optimal kernel time-frequency representation. The research indicates that the system energy is a factor influencing the distribution of the gas phase and the multi-scale morphological analysis based on the first-order difference scatter plot is an effective method for indicating the inhomogeneous distribution of the gas phase in gas-liquid two-phase flow.

  16. Determination of naloxone and naltrexone as perfluoroalkyl ester derivatives by electron-capture gas-liquid chromatography.

    PubMed

    Sams, R A; Malspeis, L

    1976-10-13

    An electron-capture gas chromatographic method is described for the determination of naloxone and naltrexone as the perfluoroalkyl esters. Each compound serves as internal standard for determination of the other. The method permits quantitation of 2-100 ng of either compound. Conditions for derivatization with heptafluorobutyric anhydride (HFBA), pentafluoropropionic anhydride (PFPA), and trifluoroacetic anhydride (TFAA) have been investigated. When catalyzed with pyridine, derivatization with HFBA and PFPA at 70 degrees gives naloxone and naltrexone triesters. Evidence for triester formation was obtained from gas chromatography-methane chemical ionization mass spectrometry and infrared spectral analysis. It was found that both the HFB and PFP triesters are suitable for quantitation of the narcotic antagonists, the HFB derivatives having greater stability than the PFP derivatives. The TFA derivatives are substantially less stable.

  17. Characterization of Mycobacterium paratuberculosis by gas-liquid and thin-layer chromatography and rapid demonstration of mycobactin dependence using radiometric methods

    SciTech Connect

    Damato, J.J.; Knisley, C.; Collins, M.T.

    1987-12-01

    Thirty-six Mycobacterium paratuberculosis isolates of bovine, caprine, and ovine origins were evaluated by using gas-liquid chromatography (GLC), thin-layer chromatography (TLC), and BACTEC 7H12 Middlebrook TB medium in an effort to more rapidly differentiate this group of organisms from other mycobacteria. Bacterial suspensions (0.1 ml) were inoculated by syringe into 7H12 broth containing 2 micrograms of mycobactin P per ml and control broth without mycobactin P. Cultures were incubated at 37/sup 0/C and read daily with a BACTEC Model 301. After 8 days of incubation, the growth index readings for the test broths containing mycobactin P were twice those of the control broths without mycobactin P. Sixty-five isolates of mycobacteria other than M. paratuberculosis were also examined. No difference was noted between the growth index readings of control and mycobactin-containing broths. Except for Mycobacterium avium-Mycobacterium intracellulare, TLC studies differentiated M. paratuberculosis from the other mycobacterial species tested. The GLC data reveal that all M. paratuberculosis isolates had a distinctive peak (14A) which was not found among M. avium-M. intracellulare complex organisms. These data indicate that 7H12 radiometric broth was able to rapidly demonstrate the mycobactin dependence of M. paratuberculosis and GLC and TLC procedures were capable of rapidly differentiating this organism from the other mycobacteria studied.

  18. Lagrangian coherent structures analysis of gas-liquid flow in a bubble column

    NASA Astrophysics Data System (ADS)

    Wu, Qin; Wang, GuoYu; Huang, Biao; Bai, ZeYu

    2014-06-01

    The objective of this paper is to apply a new identifying method to investigating the gas-liquid two-phase flow behaviors in a bubble column with air injected into water. In the numerical simulations, the standard k- ɛ turbulence model is employed to describe the turbulence phenomenon occurring in the continuous fluid. The Finite-Time Lyapunov Exponent (FTLE) and Lagrangian Coherent Structures (LCS) are applied to analyze the vortex structures in multiphase flow. Reasonable agreements are obtained between the numerical and experimental data. The numerical results show that the evolution of gas-liquid in the column includes initial and periodical developing stages. During the initial stage, the bubble hose is forming and extending along the vertical direction with the vortex structures formed symmetrically. During the periodical developing stage, the bubble hose starts to oscillate periodically, and the vortexes move along the bubble hose to the bottom of column alternately. Compared to the Euler-system-based identification criterion of a vortex, the FTLE field presents the boundary of a vortex without any threshold defined and the LCS represents the divergence extent of infinite neighboring particles. During the initial stage, the interfaces between the forward and backward flows are highlighted by the LCS. As for the periodical developing stage, the LCS curls near the vortex centers, providing a method of analyzing a flow field from a dynamical system perspective.

  19. Quantitation of l-alpha-acetylmethadol and its metabolites in human serum by capillary gas-liquid chromatography and nitrogen detection.

    PubMed

    Verebey, K; DePace, A; Mulé, S J

    1985-10-11

    A procedure is described for the simultaneous measurement of l-alpha-acetylmethadol and its two pharmacologically active metabolites: noracetylmethadol and dinoracetylmethadol. In the method an intramolecular conversion reaction of the two metabolites to their amide configuration is utilized. The reaction is performed while the metabolites are still in the serum. Following solvent extraction the samples are analyzed by capillary gas-liquid chromatography coupled with nitrogen detection. Quantitation is achieved by internal standardization. The lower limit of sensitivity is 5 ng/ml in serum. Absolute sensitivity is 0.1 ng for all three compounds. The advantages over other procedures are: speed due to the single extraction step; increased recovery of noracetylmethadol and dinoracetylmethadol due to decreased polarity of the amides; greater stability of the metabolites in the amide configuration; better chromatographic quantitation and separation because detector response for the amides is greater than it is for the original configuration of the metabolites and the area of the chromatographic tracing is free of interfering substances.

  20. Rapid confirmation of enzyme multiplied immunoassay technique (EMIT) cocaine positive urine samples by capillary gas-liquid chromatography/nitrogen phosphorus detection (GLC/NPD).

    PubMed

    Verebey, K; DePace, A

    1989-01-01

    A rapid gas-liquid chromatographic (GLC) method was developed for the confirmation of benzoylecgonine (BE) positive urine samples screened by the enzyme multiplied immunoassay technique (EMIT) assay. The procedure is performed by solvent extraction of BE from 0.1 or 0.2 mL of urine, followed by an aqueous wash of the solvent and evaporation. The dried residue was derivatized with 50 microL of pentafluoropropionic anhydride and 25 microL of pentafluoropropropanol at 90 degrees C for 15 min. The derivatizing reagents were evaporated to dryness, and the derivatized BE, and cocaine if present, were reconstituted and injected into the gas chromatograph. The column was a 15-m by 0.2-mm fused silica capillary column, coated with 0.25 micron of DB-1, terminating in a nitrogen phosphorus detector (NPD). Cocaine and the pentafluoro BE derivatives retention times were 3.2 and 2.6 min, respectively. Nalorphine was used as reference or internal standard with a retention time of 4.78 min. The complete procedure can be performed in approximately 1.5 h. The EMIT cutoff between positive and negative urine samples is 300 ng/mL of BE. The lower limit of sensitivity of this method is 25 ng of BE extracted from urine. Validation studies resulted in confirmation of 101 out of 121 EMIT cocaine positive urine samples that could not be confirmed by thin-layer chromatography (TLC). This represents 84% confirmation efficiency.

  1. [The study of vapor-liquid equilibria for polymer/solvents by using gas-liquid chromatography].

    PubMed

    Xie, J

    1999-05-01

    The infinite dilution weight fraction activity coefficient, omega 1 infinity, and Flory-Huggins interaction parameter, chi, have been determined for systems of polydimethylsiloxane (PDMS)/solvents and polymethyl-methacrylate (PMMA)/solvents by using gas chromatography from 58 degrees C to 180 degrees C. The solvents include styrene, acetone, ethyl ether, methanol, ethanol, acetic acid, trichloromethane, tetrahydrofuran and ethyl acetate in PDMS/solvent systems and n-hexane, n-heptane, cyclohexane, benzene, toluene, ethyl benzene, styrene, acetone, ethyl ether, methanol, ethanol, methyl methacrylate(MMA), trichloromethane, tetrahydrofuran and ethyl acetate in the PMMA/solvent systems. The results showed that omega 1 infinity and chi were decreased with the increase of temperature in the range from 58 degrees C to 180 degrees C. The study showed that UNIFAC and UNIFAC-FV models could not all be used to estimate omega 1 infinity of the solvents in PMMA/solvent systems. Therefore, UNIFAC and UNIFAC-FV models must be corrected or other models must be used.

  2. Theoretical and experimental analysis of a multiphase screw pump, handling gas-liquid mixtures with very high gas volume fractions

    SciTech Connect

    Raebiger, K.; Maksoud, T.M.A.; Ward, J.; Hausmann, G.

    2008-09-15

    In the investigation of the pumping behaviour of multiphase screw pumps, handling gas-liquid mixtures with very high gas volume fractions, theoretical and experimental analyses were performed. A new theoretical screw pump model was developed, which calculates the time-dependent conditions inside the several chambers of a screw pump as well as the exchange of mass and energy between these chambers. By means of the performed experimental analysis, the screw pump model was verified, especially at very high gas volume fractions from 90% to 99%. The experiments, which were conducted with the reference fluids water and air, can be divided mainly into the determination of the steady state pumping behaviour on the one hand and into the analysis of selected transient operating conditions on the other hand, whereas the visualisation of the leakage flows through the circumferential gaps was rounded off the experimental analysis. (author)

  3. Effect of cavitation on the properties of coal-tar pitch as studied by gas-liquid chromatography

    SciTech Connect

    M.I. Baikenov; T.B. Omarbekov; S.K. Amerkhanova

    2008-02-15

    The applicability of the cavitation-wave effect to coal-tar pitch processing is considered. The results of the GLC analysis of the test material before and after rotor-pulsation cavitation treatment are given. The organic matter of coal-tar pitch was found to degrade upon cavitation; as a result of this, the yields of light and medium fractions considerably increased. 5 refs., 2 figs., 4 tabs.

  4. Exergy destruction analysis of a vortices generator in a gas liquid finned tube heat exchanger: an experimental study

    NASA Astrophysics Data System (ADS)

    Ghazikhani, M.; Khazaee, I.; Monazzam, S. M. S.; Takdehghan, H.

    2016-11-01

    In the present work, the effect of using different shapes of vortices generator (VG) on a gas liquid finned heat exchanger is investigated experimentally with irreversibility analysis. In this project the ambient air with mass flow rates of 0.047-0.072 kg/s is forced across the finned tube heat exchanger. Hot water with constant flow rate of 240 L/h is circulated inside heat exchanger tubes with inlet temperature range of 45-73 °C. The tests are carried out on the flat finned heat exchanger and then repeated on the VG finned heat exchanger. The results show that using the vortex generator can decrease the ratio of air side irreversibility to heat transfer (ASIHR) of the heat exchanger. Also the results show that the IASIHR is >1.05 for all air mass flow rates, which means that ASIHR for the initial heat exchanger is higher than 5 % greater than that of improved heat exchanger.

  5. Development of a gas-liquid chromatographic method for the analysis of fatty acid tryptamides in cocoa products.

    PubMed

    Hug, Bernadette; Golay, Pierre-Alain; Giuffrida, Francesca; Dionisi, Fabiola; Destaillats, Frédéric

    2006-05-03

    The determination of the occurrence and level of cocoa shells in cocoa products and chocolate is an important analytical issue. The recent European Union directive on cocoa and chocolate products (2000/36/EC) has not retained the former limit of a maximum amount of 5% of cocoa shells in cocoa nibs (based on fat-free dry matter), previously authorized for the elaboration of cocoa products such as cocoa mass. In the present study, we report a reliable gas-liquid chromatography procedure suitable for the determination of the occurrence of cocoa shells in cocoa products by detection of fatty acid tryptamides (FATs). The precision of the method was evaluated by analyzing nine different samples (cocoa liquors with different ranges of shells) six times (replicate repeatability). The variations of the robust coefficient of variation of the repeatability demonstrated that FAT(C22), FAT(C24), and total FATs are good markers for the detection of shells in cocoa products. The trueness of the method was evaluated by determining the FAT content in two spiked matrices (cocoa liquors and cocoa shells) at different levels (from 1 to 50 mg/100 g). A good relation was found between the results obtained and the spiking (recovery varied between 90 and 130%), and the linearity range was established between 1 and 50 mg/100 g in cocoa products. For total FAT contents of cocoa liquor containing 5% shells, the measurement uncertainty allows us to conclude that FAT is equal to 4.01 +/- 0.8 mg/100 g. This validated method is perfectly suitable to determine shell contents in cocoa products using FAT(C22), FAT(C24), and total FATs as markers. The results also confirmed that cocoa shells contain FAT(C24) and FAT(C22) in a constant ratio of nearly 2:1.

  6. Comparison of two gas-liquid chromatograph columns for the analysis of fatty acids in ruminant meat.

    PubMed

    Alves, Susana P; Bessa, Rui J B

    2009-06-26

    Two gas-liquid chromatograph capillary columns for the analysis of fatty acids (FA) in ruminant fat are compared. Those columns are the CP-Sil 88 of 100 m long with a highly polar stationary phase and the Omegawax 250 of 30 m long with a stationary phase of intermediate polarity. Fatty acid methyl ester (FAME) patterns of branched-chain, cis and trans octadecenoate isomers, as well as conjugated and non-conjugated 18:2 and 18:3 isomers are fairly different between columns, even though most of the FAME could be separated on either column. However, the CP-Sil 88 showed better resolution of 18:1 isomers than Omegawax 250. The analysis of 96 samples of ruminant meat fat in both chromatographic systems showed that averages obtained for total FA content and for most of the individual FA did not differ between columns. Moreover, regression analysis of Omegawax and CP-Sil 88 data is highly correlated. Quantitative differences between chromatographic systems were detected for samples containing more than 66 mg fatty acids per gram of muscle dry matter.

  7. Thermostability analysis of line-tension-associated nucleation at a gas-liquid interface

    NASA Astrophysics Data System (ADS)

    Singha, Sanat Kumar; Das, Prasanta Kumar; Maiti, Biswajit

    2017-01-01

    The influence of line tension on the thermostability of a droplet nucleated from an oversaturated vapor at the interface of the vapor and another immiscible liquid is investigated. Along with the condition of mechanical equilibrium, the notion of extremization of the reversible work of formation is considered to obtain the critical parameters related to heterogeneous nucleation. From the energetic formulation, the critical reversible work of formation is found to be greater than that of homogeneous nucleation for high value of the positive line tension. On the other hand, for high value of the negative line tension, the critical reversible work of formation becomes negative. Therefore, these thermodynamic instabilities under certain substrate wettability situations necessitate a free-energetics-based stability of the nucleated droplet, because the system energy is not minimized under these conditions. This thermostability is analogous to the transition-based stability proposed by Widom [B. Widom, J. Phys. Chem. 99, 2803 (1995)], 10.1021/j100009a041 in the case of partial wetting phenomena along with the positive line tension. The thermostability analysis limits the domain of the solution space of the present critical-value problem as the thermodynamic transformation in connection with homogeneous and workless nucleation is considered. Within the stability range of the geometry-based wetting parameters, three limiting modes of nucleation, i.e., total-dewetting-related homogeneous nucleation, and total-wetting-associated and total-submergence-associated workless nucleation scenarios, are identified. Either of the two related limiting wetting scenarios of workless nucleation, namely, total wetting and total submergence, is found to be favorable depending on the geometry-based wetting conditions. The line-tension-associated nucleation on a liquid surface can be differentiated from that on a rigid substrate, as in the former, the stability based on mechanical

  8. [Standardization criteria for the study of fetal lung maturity by means of gas-liquid chromatography of the fatty acid content of the amniotic fluid].

    PubMed

    Lantieri, P B; Ciangherotti, S; Diani, F; Pecorari, D

    1979-08-15

    Gas-chromatographic analysis of the fatty acids (P/S ratio) in 10 samples of amniotic fluid and 10 samples of the pellets obtained after centrifugation of amniotic fluid at 3500 X g for 60 minutes were carried out to evaluate the effects of contaminants that might be present in amniotic fluid. The P/S ratio is used as an index of the degree of maturity of the fetal or neonatal lung. We propose a standard procedure of centrifugation for 60 minutes at 3500 X g followed by extraction and gas-chromatography as a rapid, valid way to measure the P/S ratio.

  9. Gas-liquid chromatographic and gas-liquid-mass spectometric determination of fenvalerate and permethrin residues in grasshoppers and duck tissue samples

    USGS Publications Warehouse

    Reichel, W.L.; Kolbe, E.J.; Stafford, C.J.

    1981-01-01

    A procedure is described for determining fenvalerate and permethrin residues in grasshoppers and duck tissues. Samples are Soxhlet-extracted with hexane and cleaned up by gel permeation chromatography with an in-line alumina column. Samples are analyzed by gas-liquid chromatography with electron capture detection, and confirmed by gas-liquid chromatography-mass spectrometry. The average recovery from fortified tissues was 97%.

  10. Refined non-steady-state gas-liquid chromatography for accurate determination of limiting activity coefficients of volatile organic compounds in water: application to C(1)-C(5) alkanols.

    PubMed

    Dohnal, Vladimír; Ondo, Daniel

    2005-12-02

    This work presents a new refined method of non-steady-state gas-liquid chromatography (NSGLC) suitable for determination of limiting activity coefficients of VOCs in water. The modifications done to the original NSGLC theory address its elements (as the solvent elution rate from the column) as well as other new aspects. The experimental procedure is modified accordingly, taking advantage of current technical innovations. The refined method is used systematically to determine limiting activity coefficients (Henry's law constants, limiting relative volatilities) of isomeric C(1)-C(5) alkanols in water at 328.15K. Applied to retention data measured in this work the refined NSGLC theory gives values 15-20% higher than those from the original approach. The values obtained by the refined NSGLC method agree very well (typically within 3%) with the most reliable literature data determined by other experimental techniques, this result verifying thus the correct performance of the refined method and demonstrating an improved accuracy of the new results.

  11. Determination of solute partition behavior with room-temperature ionic liquid based micellar gas-liquid chromatography stationary phases using the pseudophase model.

    PubMed

    Lantz, Andrew W; Pino, Verónica; Anderson, Jared L; Armstrong, Daniel W

    2006-05-19

    The use of micelles in ionic liquid based gas-chromatography stationary phases was evaluated using equations derived for a "three-phase" model. This model allows the determination of all three partition coefficients involved in the system, and elucidates the micellar contribution to retention and selectivity. Four types of micellar-ionic liquid columns were examined in this study: 1-butyl-3-methylimidazolium chloride with sodium dodecylsulfate or dioctyl sulfosuccinate, and 1-butyl-3-methylimidazolium hexafluorophosphate with polyoxyethylene-100-stearyl ether or polyoxyethylene-23-lauryl ether. The partition coefficients were measured for a wide range of probe molecules capable of a variety of types and magnitudes of interactions. In general, most probe molecules preferentially partitioned to the micellar pseudophase over the bulk ionic liquid component of the stationary phase. Therefore, addition of surfactant to the stationary phase usually resulted in greater solute retention. It is also shown that the selectivity of the stationary phase is significantly altered by the presence of micelles, either by enhancing or lessening the separation. The effects of surfactant on the interaction parameters of the stationary phase are determined using the Abraham solvation parameter model. The addition of sodium dodecylsulfate and dioctyl sulfosuccinate to 1-butyl-3-methylimidazolium chloride stationary phases generally increased the phase's hydrogen bond basicity and increased the level of dispersion interaction. Polyoxyethylene-100-stearyl ether and polyoxyethylene-23-lauryl ether surfactants, however, enhanced the pi-pi/n-pi, polarizability/dipolarity, and hydrogen bond basicity interactions of 1-butyl-3-methylimidazolium hexafluorophosphate to a greater degree than the ionic surfactants with 1-butyl-3-methylimidazolium chloride. However, these nonionic surfactants appeared to hinder the ability of the stationary phase to interact with solutes via dispersion forces

  12. Supersonic Gas-Liquid Cleaning System

    NASA Technical Reports Server (NTRS)

    Kinney, Frank

    1996-01-01

    The Supersonic Gas-Liquid Cleaning System Research Project consisted mainly of a feasibility study, including theoretical and engineering analysis, of a proof-of-concept prototype of this particular cleaning system developed by NASA-KSC. The cleaning system utilizes gas-liquid supersonic nozzles to generate high impingement velocities at the surface of the device to be cleaned. The cleaning fluid being accelerated to these high velocities may consist of any solvent or liquid, including water. Compressed air or any inert gas is used to provide the conveying medium for the liquid, as well as substantially reduce the total amount of liquid needed to perform adequate surface cleaning and cleanliness verification. This type of aqueous cleaning system is considered to be an excellent way of conducting cleaning and cleanliness verification operations as replacements for the use of CFC 113 which must be discontinued by 1995. To utilize this particular cleaning system in various cleaning applications for both the Space Program and the commercial market, it is essential that the cleaning system, especially the supersonic nozzle, be characterized for such applications. This characterization consisted of performing theoretical and engineering analysis, identifying desirable modifications/extensions to the basic concept, evaluating effects of variations in operating parameters, and optimizing hardware design for specific applications.

  13. A survey of trace contaminants in natural gas liquids

    SciTech Connect

    Wharry, S.M.; Sung, N.J.

    1995-11-01

    A survey of selected contaminants in natural gas liquids (NGL) has been completed for the purpose of determining whether more stringent NGL specifications should be considered by the industry. The survey involved the analysis of over 45 samples from seven independent processors. The trace contaminants that were analyzed include olefins, oxygenated compounds, fluoride, mercury, and arsenic. Not unsurprisingly, the highest levels of olefins were found in the corresponding hydrocarbon streams, (i.e., propylene in the propane streams). The highest levels of oxygenated compounds were found in the propane and raw make streams. The highest fluoride levels were found in the gasoline samples. And finally, for the most part, the mercury and arsenic levels were to close to the detection limits for these samples ({approximately}10 ppb for mercury and {approximately}50 ppb for arsenic) to be able to accurately determine if these contaminants were present in any of the samples. A more exhaustive study would be needed to analyze for these components below these levels. For the olefins, a gas chromatography procedure was used to determine the levels of pentenes and lighter olefins. For the oxygenated compounds, a water extraction method with a gas chromatography follow up was used. This method measures the levels of all water soluble oxygenated compounds, such as the butanols and lighter alcohols as well as acetone. The fluoride analysis involved the determination of the total fluoride per a modified UOP Method 619-83, the Wickbold method. The mercury and arsenic analyses were obtained by first passing the vapor portion of the samples through appropriate trapping media and then desorbing the traps directly into an inductively coupled plasma-mass spectrometer.

  14. Advances in gas-liquid flows 1990

    SciTech Connect

    Kim, J.M. . Nuclear Reactor Lab.); Rohatgi, U.S. ); Hashemi, A. )

    1990-01-01

    Gas-liquid two-phase flows commonly occur in nature and industrial applications. Rain, clouds, geysers, and waterfalls are examples of natural gas-liquid flow phenomena, whereas industrial applications can be found in nuclear reactors, steam generators, boilers, condensers, evaporators, fuel atomization, heat pipes, electronic equipment cooling, petroleum engineering, chemical process engineering, and many others. The household-variety phenomena such as garden sprinklers, shower, whirlpool bath, dripping faucet, boiling tea pot, and bubbling beer provide daily experience of gas-liquid flows. The papers presented in this volume reflect the variety and richness of gas-liquid two-phase flow and the increasing role it plays in modern technology. This volume contains papers dealing with some recent development in gas-liquid flow science and technology, covering basic gas-liquid flows, measurements and instrumentation, cavitation and flashing flows, countercurrent flow and flooding, flow in various components and geometries liquid metals and thermocapillary effects, heat transfer, nonlinear phenomena, instability, and other special and general topics related to gas-liquid flows.

  15. Effect of gas-liquid flow pattern and microbial diversity analysis of a pilot-scale biotrickling filter for anoxic biogas desulfurization.

    PubMed

    Almenglo, Fernando; Bezerra, Tercia; Lafuente, Javier; Gabriel, David; Ramírez, Martín; Cantero, Domingo

    2016-08-01

    Hydrogen sulfide removal from biogas was studied under anoxic conditions in a pilot-scale biotrickling filter operated under counter- and co-current gas-liquid flow patterns. The best performance was found under counter-current conditions (maximum elimination capacity of 140 gS m(-3) h(-1)). Nevertheless, switching conditions between co- and counter-current flow lead to a favorable redistribution of biomass and elemental sulfur along the bed height. Moreover, elemental sulfur was oxidized to sulfate when the feeding biogas was disconnected and the supply of nitrate (electron acceptor) was maintained. Removal of elemental sulfur was important to prevent clogging in the packed bed and, thereby, to increase the lifespan of the packed bed between maintenance episodes. The larger elemental sulfur removal rate during shutdowns was 59.1 gS m(-3) h(-1). Tag-encoded FLX amplicon pyrosequencing was used to study the diversity of bacteria under co-current flow pattern with liquid recirculation and counter-current mode with a single-pass flow of the liquid phase. The main desulfurizing bacteria were Sedimenticola while significant role of heterotrophic, opportunistic species was envisaged. Remarkable differences between communities were found when a single-pass flow of industrial water was fed to the biotrickling filter.

  16. Simultaneous separation of chlorinated/brominated dioxins, polychlorinated biphenyls, polybrominated diphenyl ethers and their methoxylated derivatives from hydroxylated analogues on molecularly imprinted polymers prior to gas/liquid chromatography and mass spectrometry.

    PubMed

    Roszko, Marek; Szymczyk, Krystyna; Jędrzejczak, Renata

    2015-11-01

    Polychlorinated dibenzo-p-dioxins/furans (PCDD/Fs), polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) are important contaminants in the environment. In recent years also polybrominated dibenzo-p-dioxins/dibenzofurans (PBDD/Fs) have been reported as emerging environmental stressors. It has been suggested that hydroxylated polybrominated biphenyl ethers (OH-BDEs) are important - may be even the most important - precursors of brominated dioxins/furans. The aim of this study was to develop a robust, time-saving analytical procedure to collectively separate in animal tissues such compounds prior to determination of individual substances with a gas/liquid chromatograph coupled to an ion trap/time-of-flight mass spectrometer (GC/IT-MS or UPLC/TOF-MS). Two OH-CB/BDE separation methods including alkaline extraction and molecularly imprinted polymers (MIP) were compared. Performance of both methods was validated: absolute recovery values were in the 47-90% range depending on the compound, while recovery relative standard deviation was below 20% in most cases. Levels of the studied compounds have been assessed in some real life samples.

  17. Paper Chromatography as an Adjunct in the Identification of Anaerobic Bacteria

    PubMed Central

    Slifkin, M.; Hercher, H. J.

    1974-01-01

    Modified paper chromatography procedures for the analysis of fatty acids produced by anaerobic bacteria are described. Both ethylamine and hydroxylamine derivatives of fatty acids were prepared from inoculated anaerobic culture broth. The derivatives were spotted on chromatography paper and developed with appropriate solvents. Paper chromatography is a valuable alternative to gas liquid chromatography as an ancillary procedure in the identification of anaerobic bacteria in the clinical bacteriology laboratory. PMID:4596386

  18. Analysis of Microorganisms by Oxidative and Non-Oxidative Pyrolysis Gas Chromatography Ion Trap Mass Spectrometry.

    DTIC Science & Technology

    1992-04-01

    Bacillus subtilis, Bacillus pumilus , Bacillus lichenformis, and Bacillus amyloliquefaciens by Pyrolysis-gas Liquid Chromatography, Deoxyribonucleic...FIGURES Number Page 1. Curie point pyrolysis GC-ITD data for Bacillus subtilis ................... 16 2. Total Ion Chromatograms for Bacillus subtilis...under oxidative and non-oxidative pyrolysis conditions ................................... 17 3. Total Lipid Mass Spectra for Bacillus subtilis under

  19. Analysis of energetic materials by ion chromatography

    SciTech Connect

    Hershey, M.K.

    1985-01-01

    Ion chromatography is a rapid, sensitive, and selective method for ion analysis in a variety of matrices. Ion chromatography was used to determine levels on chloride and chlorate in potassium perchlorate. Comparisons were made with the specific ion electrons method presently being used for these analyses. Also to be discussed are ion chromatographic methods for determining ammonium in boron potassium nitrate, and chloride and ammonium in CP.

  20. Supersonic gas-liquid cleaning system

    NASA Astrophysics Data System (ADS)

    Caimi, Raoul E. B.; Thaxton, Eric A.

    1994-02-01

    A system to perform cleaning and cleanliness verification is being developed to replace solvent flush methods using CFC 113 for fluid system components. The system is designed for two purposes: internal and external cleaning and verification. External cleaning is performed with the nozzle mounted at the end of a wand similar to a conventional pressure washer. Internal cleaning is performed with a variety of fixtures designed for specific applications. Internal cleaning includes tubes, pipes, flex hoses, and active fluid components such as valves and regulators. The system uses gas-liquid supersonic nozzles to generate high impingement velocities at the surface of the object to be cleaned. Compressed air or any inert gas may be used to provide the conveying medium for the liquid. The converging-diverging nozzles accelerate the gas-liquid mixture to supersonic velocities. The liquid being accelerated may be any solvent including water. This system may be used commercially to replace CFC and other solvent cleaning methods widely used to remove dust, dirt, flux, and lubricants. In addition, cleanliness verification can be performed without the solvents which are typically involved. This paper will present the technical details of the system, the results achieved during testing at KSC, and future applications for this system.

  1. Supersonic gas-liquid cleaning system

    NASA Technical Reports Server (NTRS)

    Caimi, Raoul E. B.; Thaxton, Eric A.

    1994-01-01

    A system to perform cleaning and cleanliness verification is being developed to replace solvent flush methods using CFC 113 for fluid system components. The system is designed for two purposes: internal and external cleaning and verification. External cleaning is performed with the nozzle mounted at the end of a wand similar to a conventional pressure washer. Internal cleaning is performed with a variety of fixtures designed for specific applications. Internal cleaning includes tubes, pipes, flex hoses, and active fluid components such as valves and regulators. The system uses gas-liquid supersonic nozzles to generate high impingement velocities at the surface of the object to be cleaned. Compressed air or any inert gas may be used to provide the conveying medium for the liquid. The converging-diverging nozzles accelerate the gas-liquid mixture to supersonic velocities. The liquid being accelerated may be any solvent including water. This system may be used commercially to replace CFC and other solvent cleaning methods widely used to remove dust, dirt, flux, and lubricants. In addition, cleanliness verification can be performed without the solvents which are typically involved. This paper will present the technical details of the system, the results achieved during testing at KSC, and future applications for this system.

  2. Gas-Liquid Processing in Microchannels

    SciTech Connect

    TeGrotenhuis, Ward E.; Stenkamp, Victoria S.; Twitchell, Alvin

    2005-09-01

    Processing gases and liquids together in microchannels having at least one dimension <1 mm has unique advantages for rapid heat and mass transfer. One approach for managing the two phases is to use porous structures as wicks within microchannels to segregate the liquid phase from the gas phase. Gas-liquid processing is accomplished by providing a gas flow path and inducing flow of the liquid phase through or along the wick under an induced pressure gradient. A variety of unit operations are enabled, including phase separation, partial condensation, absorption, desorption, and distillation. Results are reported of an investigation of microchannel phase separation in a transparent, single-channel device. Next, heat exchange is integrated with the microchannel wick approach to create a partial condenser that also separates the condensate. Finally, the scale-up to a multi-channel phase separator is described.

  3. Short-Term Outlook for Hydrocarbon Gas Liquids

    EIA Publications

    2016-01-01

    U.S. liquid fuels production increased from 7.43 million barrels per day (b/d) in 2008 to 13.75 million b/d in 2015. However, the Short-Term Energy Outlook (STEO) expects liquid fuels production to decline to 12.99 million b/d in 2017, mainly as a result of prolonged low oil prices. The liquid fuels production forecast reflects a 1.24 million b/d decline in crude oil production by 2017 that is partially offset by a 450,000 b/d increase in the production of hydrocarbon gas liquids (HGL)—a group of products including ethane, propane, butane (normal and isobutane), natural gasoline, and refinery olefins. This analysis will discuss the outlook for each of these four HGL streams and related infrastructure projects through 2017.

  4. Combined Gas-Liquid Plasma Source for Nanoparticle Synthesis

    NASA Astrophysics Data System (ADS)

    Burakov, V. S.; Kiris, V. V.; Nevar, A. A.; Nedelko, M. I.; Tarasenko, N. V.

    2016-09-01

    A gas-liquid plasma source for the synthesis of colloidal nanoparticles by spark erosion of the electrode material was developed and allowed the particle synthesis regime to be varied over a wide range. The source parameters were analyzed in detail for the electrical discharge conditions in water. The temperature, particle concentration, and pressure in the discharge plasma were estimated based on spectroscopic analysis of the plasma. It was found that the plasma parameters did not change signifi cantly if the condenser capacitance was increased from 5 to 20 nF. Purging the electrode gap with argon reduced substantially the pressure and particle concentration. Signifi cant amounts of water decomposition products in addition to electrode elements were found in the plasma in all discharge regimes. This favored the synthesis of oxide nanoparticles.

  5. Chromatography.

    ERIC Educational Resources Information Center

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  6. Gas-Liquid Flow in Pipelines

    SciTech Connect

    Thomas J. Hanratty

    2005-02-25

    A research program was carried out at the University of Illinois in which develops a scientific approach to gas-liquid flows that explains their macroscopic behavior in terms of small scale interactions. For simplicity, fully-developed flows in horizontal and near-horizontal pipes. The difficulty in dealing with these flows is that the phases can assume a variety of configurations. The specific goal was to develop a scientific understanding of transitions from one flow regime to another and a quantitative understanding of how the phases distribute for a give regime. These basic understandings are used to predict macroscopic quantities of interest, such as frictional pressure drop, liquid hold-up, entrainment in annular flow and frequency of slugging in slug flows. A number of scientific issues are addressed. Examples are the rate of atomization of a liquid film, the rate of deposition of drops, the behavior of particles in a turbulent field, the generation and growth of interfacial waves. The use of drag-reducing polymers that change macroscopic behavior by changing small scale interactions was explored.

  7. Phytanic acid: measurement of plasma concentrations by gas-liquid chromatography-mass spectrometry analysis and associations with diet and other plasma fatty acids.

    PubMed

    Allen, Naomi E; Grace, Philip B; Ginn, Annette; Travis, Ruth C; Roddam, Andrew W; Appleby, Paul N; Key, Timothy

    2008-03-01

    Epidemiological data suggest that a diet rich in animal foods may be associated with an increased risk of several cancers, including cancers of the prostate, colorectum and breast, but the possible mechanism is unclear. It is hypothesised that phytanic acid, a C20 branched-chain fatty acid found predominantly in foods from ruminant animals, may be involved in early cancer development because it has been shown to up regulate activity of alpha-methylacyl-coenzyme A racemase, an enzyme commonly found to be over-expressed in tumour cells compared with normal tissue. However, little is known about the distribution of plasma phytanic acid concentrations or its dietary determinants in the general population. The primary aim of the present cross-sectional study was to determine circulating phytanic acid concentrations among ninety-six meat-eating, lacto-ovo-vegetarian and vegan women, aged 20-69 years, recruited into the Oxford component of the European Prospective Investigation into Cancer and Nutrition (EPIC-Oxford). Meat-eaters had, on average, a 6.7-fold higher geometric mean plasma phytanic acid concentration than the vegans (5.77 v. 0.86 micromol/l; P < 0.0001) and a 47 % higher mean concentration than the vegetarians (5.77 v. 3.93 micromol/l; P = 0.016). The strongest determinant of plasma phytanic acid concentration appeared to be dairy fat intake (r 0.68; P < 0.0001); phytanic acid levels were not associated with age or other lifestyle factors. These data show that a diet high in fat from dairy products is associated with increased plasma phytanic acid concentration, which may play a role in cancer development.

  8. Gas-liquid separator and method of operation

    DOEpatents

    Soloveichik, Grigorii Lev; Whitt, David Brandon

    2009-07-14

    A system for gas-liquid separation in electrolysis processes is provided. The system includes a first compartment having a liquid carrier including a first gas therein and a second compartment having the liquid carrier including a second gas therein. The system also includes a gas-liquid separator fluidically coupled to the first and second compartments for separating the liquid carrier from the first and second gases.

  9. Gas-liquid chromatographic determination of 3-trifluoromethyl-4-nitrophenol residues in fish

    USGS Publications Warehouse

    Allen, J.L.; Sills, J.B.

    1974-01-01

    A procedure for the determination of 3-mftuormethyl-4-nitrophenol (TFM) in fish tissues is described. Homogenized tissues are extracted with hexane-ethyl ether; the extract is cleaned up by partitioning the TFM from the extracting solvent into O.IN NaOB, acidifying the aqueous solution, and partitioning again with hexaneethyl ether. The TFM is methylated with diazomethane and analyzed by gas-liquid chromatography, using electron capture detection. Recoveries ranged from 75 to 1000/., from fish muscles that were spiked with 0.01-2.00 JA#g TFM/g.

  10. Characterization of 22 Vibrio species by gas chromatography analysis of their cellular fatty acids.

    PubMed

    Urdaci, M C; Marchand, M; Grimont, P A

    1990-05-01

    The cellular fatty acid compositions of 51 Vibrio strains belonging to 22 species as well as five Aeromonas strains were determined by using capillary gas-liquid chromatography (GLC). The major fatty acids were most often hexadecenoic, hexadecanoic and octadecenoic acids. Heptadecenoic acid was present in significant amounts in V. alginolyticus, V. natriegens, V. parahaemolyticus and "Vibrio navarrensis". Twenty fatty acids including branched and hydroxy acids were detected in the genus Vibrio. Quantitative results were treated by principal component analysis to display groups of strains. The first three components (accounting for 69% of the variance) showed the type strains of V. fischeri, V. ordalii, V. damsela, V. mediterranei, V. tubiashii, V. campbellii, V. pelagius, V. gazogenes, and V. nereis to be unclustered. V. alginolyticus (4 strains) and V. parahaemolyticus (4 strains) showed some overlap and the type strain of V. natriegens was in their neighborhood. V. harveyi (4 strains) formed a cluster and V. vulnificus was in its vicinity. V. cholerae (5 strains) overlapped with V. diazotrophicus (3 strains) and was close to the type strain of V. mimicus and V. anguillarum. V. metschnikovii (3 strains) clustered with the type strain of V. cincinnatiensis. A decision tree was devised for the identification of Vibrio species based on qualitative characteristics of fatty acid patterns. However, the following three groups, V. alginolyticus-V. parahaemolyticus-V. natriegens, V. metschnikovii-V. cincinnatiensis and V. cholerae-V. mimicus could not be split into such a decision tree.

  11. Acoustic probe for solid-gas-liquid suspensions. 1998 annual progress report

    SciTech Connect

    Tavlarides, L.L.; Sangani, A.S.; Greenwood, M.S.

    1998-06-01

    'The proposed research will develop an acoustic probe for monitoring particle size and volume fraction in slurries in the absence and presence of gas. The goals are to commission and verify the probe components and system operation, develop theory for the forward and inverse problems for acoustic wave propagation through a three phase medium, and experimentally verify the theoretical analysis. The acoustic probe will permit measurement of solid content in gas-liquid-solid waste slurries in tanks across the DOE complex.'

  12. Injector design guidelines for gas/liquid propellant systems

    NASA Technical Reports Server (NTRS)

    Falk, A. Y.; Burick, R. J.

    1973-01-01

    Injector design guidelines are provided for gas/liquid propellant systems. Information was obtained from a 30-month applied research program encompassing an analytical, design, and experimental effort to relate injector design parameters to simultaneous attainment of high performance and component (injector/thrust chamber) compatibility for gas/liquid space storable propellants. The gas/liquid propellant combination studied was FLOX (82.6% F2)/ ambient temperature gaseous methane. Design criteria that provide for simultaneous attainment of high performance and chamber compatibility are presented for both injector types. Parametric data are presented that are applicable for the design of circular coaxial and like-doublet injectors that operate with design parameters similar to those employed. However, caution should be exercised when applying these data to propellant combinations whose elements operate in ranges considerably different from those employed in this study.

  13. Chromatography

    MedlinePlus

    Chromatography is a way of separating two or more chemical compounds. Chemical compounds are chemicals that are ... of chemical compound. There are different kinds of chromatography. These include gas, high pressure liquid, or ion ...

  14. DEVELOPMENT AND VALIDATION OF A MULTIFIELD MODEL OF CHURN-TURBULENT GAS/LIQUID FLOWS

    SciTech Connect

    Elena A. Tselishcheva; Steven P. Antal; Michael Z. Podowski; Donna Post Guillen

    2009-07-01

    The accuracy of numerical predictions for gas/liquid two-phase flows using Computational Multiphase Fluid Dynamics (CMFD) methods strongly depends on the formulation of models governing the interaction between the continuous liquid field and bubbles of different sizes. The purpose of this paper is to develop, test and validate a multifield model of adiabatic gas/liquid flows at intermediate gas concentrations (e.g., churn-turbulent flow regime), in which multiple-size bubbles are divided into a specified number of groups, each representing a prescribed range of sizes. The proposed modeling concept uses transport equations for the continuous liquid field and for each bubble field. The overall model has been implemented in the NPHASE-CMFD computer code. The results of NPHASE-CMFD simulations have been validated against the experimental data from the TOPFLOW test facility. Also, a parametric analysis on the effect of various modeling assumptions has been performed.

  15. Recent applications of hydrophilic interaction liquid chromatography in pharmaceutical analysis.

    PubMed

    Zhang, Qian; Yang, Feng-Qing; Ge, Liya; Hu, Yuan-Jia; Xia, Zhi-Ning

    2017-01-01

    Hydrophilic interaction liquid chromatography, an alternative liquid chromatography mode, is of particular interest in separating hydrophilic and polar ionic compounds. Compared with traditional liquid chromatography techniques, hydrophilic interaction liquid chromatography offers specific advantages mainly including: (1) relatively green and water-soluble mobile phase composition, which enhances the solubility of hydrophilic and polar ionic compounds; (2) no need for ion-pairing reagents and high content of organic solvent, which benefits mass spectrometry detection; (3) high orthogonality to reverse-phase liquid chromatography, well adapted to two-dimensional liquid chromatography for complicated samples. Therefore, hydrophilic interaction liquid chromatography has been rapidly developed in many areas over the past decades. This review summarizes the recent progress (from 2012 to July 2016) of hydrophilic interaction liquid chromatography in pharmaceutical analysis, with the focus on detecting chemical drugs in various matrices, charactering active compounds of natural products and assessing biotherapeutics through typical structure unit. Moreover, the retention mechanism and behavior of analytes in hydrophilic interaction liquid chromatography as well as some novel hydrophilic interaction liquid chromatography columns used for pharmaceutical analysis are also described.

  16. Separation and IR Analysis of a Mixture of Organic Compounds.

    ERIC Educational Resources Information Center

    Thompson, Evan M.; Almy, John

    1982-01-01

    Presents an experiment which includes fractional distillation with gas-liquid chromatography (GLC) and infrared analysis. Objectives are to introduce students to fractional distillation and analysis of each fraction by GLC, to induce them to decide if each fraction is sufficient for infrared analysis, and to identify unknowns. (Author/JN)

  17. Investigation on a gas-liquid ejector using three-dimensional CFD model

    NASA Astrophysics Data System (ADS)

    Kang, S. H.; Song, X. G.; Park, Y. C.

    2012-11-01

    This paper is focusing on the numeral study of a gas-liquid ejector used for ballast water treatment. The gasliquid ejector is investigated through steady three-dimensional multiphase CFD analysis with commercial software ANSYS-CFX 13.0. Water as the primary fluid is driven through the driving nozzle and air is ejected into as the second gas instead of the ozone in real application. Several turbulence models such as Standard k-ɛ model, RNG k-ɛ model, SST model and k-ω model, and different mesh size and compared extensively with the experimental results to eliminate the influence of the auxiliary system, turbulence models and mesh generation. The appropriate numerical model in terms of the best combination of turbulence model and mesh size are used in the subsequent research the study the influence of the operating condition such as the driving pressure/velocity and the back pressure of the ejector on its performance. The results provide deep insight on the influence of various factors on the performance of gas-liquid ejector. And the proposed numerical model will be very helpful in the further design optimization of the gas-liquid ejectors.

  18. A Lab Experiment to Introduce Gas/Liquid Solubility

    ERIC Educational Resources Information Center

    Fonsecaa, I. M. A.; Almeida, J. P. B.; Fachada, H. C.

    2008-01-01

    A simplified version of a volumetric apparatus for gas/liquid solubility measurements is proposed. The procedure familiarizes undergraduate students with the experimental study of the solubility of a gas in a liquid and contributes to the understanding of this important phase equilibrium concept. The experimental results report the determination…

  19. Parallel magnetic resonance imaging of gas-liquid flows

    NASA Astrophysics Data System (ADS)

    Mueller, Christoph; Penn, Alexander; Pruessmann, Klaas P.

    2015-03-01

    Gas-liquids flows are commonly encountered in nature and industry. Experimental measurements of gas-liquid flows are challenging since such systems can be visually opaque and highly dynamic. Here we report the implementation of advanced magnetic resonance imaging (MRI) strategies allowing us to probe the dynamics (voidage and velocity measurements) of gas-liquid flows with ultra-fast acquisition speeds. Specifically, parallel MRI which exploits the spatial encoding capabilities of multiple receiver coils was implemented. To this end a tailored, 16 channels MR receive array was constructed and employed in the MR acquisition. A magnetic susceptibility matched gas-liquid system was set-up and used to probe the motion, splitting and coalescence of bubbles. The temporal and spatial resolution of our acquired data was 5 ms and 3.5 mm x 3.5 mm, respectively. The total field of view was 200 mm x 200 mm. We will conclude with an outlook of further possible advances in MRI that have the potential to reduce substantially the acquisition time, providing flexible gains in temporal and spatial resolution.

  20. Mass spectrometric identification and gas-liquid chromatographic determination of 2-chloroethyl esters of fatty acids in spices and foods.

    PubMed

    Heikes, D L; Griffitt, K R

    1979-07-01

    The 2-chloroethyl esters of 5 fatty acids have been identified in spice and food samples by gas-liquid chromatography-mass spectrometry (GLC/MS). Twenty-four spice samples were analyzed for the 2-chloroethyl esters of fatty acids by AOAC official multiple residues pesticide procedure using GLC with microcoulometric detection. The esters of capric, lauric, myristic, palmitic, and linoleic acids have been identified at levels up to 1400 ppm. 2-Chloroethyl linoleate was the most abundant ester in all samples. Several foods analyzed by the same procedures showed levels of 2-chloroethyl linoleate as high as 35 ppm. Recoveries from fortified samples ranged from 84 to 98% for the various esters. A method using an acid-catalyzed esterification reaction was developed to rapidly determine the fatty acid content of these spices. GLC analysis with microcoulometric detection was used. Recoveries from fortified samples ranged from 92 to 110%. After 2 spice samples found to be free of 2-chloroethyl esters were fumigated with ethylene oxide, the level of 2-chloroethyl linoleate reached 77 ppm. All levels of 2-chloroethyl esters were confirmed by GLC/MS.

  1. Prediction of gas-liquid two-phase flow regime in microgravity

    NASA Technical Reports Server (NTRS)

    Lee, Jinho; Platt, Jonathan A.

    1993-01-01

    An attempt is made to predict gas-liquid two-phase flow regime in a pipe in a microgravity environment through scaling analysis based on dominant physical mechanisms. Simple inlet geometry is adopted in the analysis to see the effect of inlet configuration on flow regime transitions. Comparison of the prediction with the existing experimental data shows good agreement, though more work is required to better define some physical parameters. The analysis clarifies much of the physics involved in this problem and can be applied to other configurations.

  2. Gas-liquid chromatographic determination of kepone in field-collected avian tissues and eggs

    USGS Publications Warehouse

    Stafford, C.J.; Reichel, W.L.; Swineford, D.M.; Prouty, R.M.; Gay, M.L.

    1978-01-01

    A procedure is described for determining Kepone (decachlorooctahydro-1,3,4-metheno-2H-cyclobuta [cd] pentalene-2-one) residues in avian egg, liver, and tissue. Samples were extracted with benzene-isopropanol, and the extract was cleaned up with fuming H2SO4-concentrated H2SO4. Kepone was separated from organochlorine pesticides and polychlorinated biphenyls on a Florisil column and analyzed by electron capture gas-liquid chromatography (GLC). The average recovery from spiked tissues was 86%. The analyses performed on 14 bald eagle carcasses and livers, 3 bald eagle eggs, and 14 osprey eggs show measurable levels which indicate that Kepone accumulates in the tissues of fish-eating birds. Residues were confirmed by GLC-mass spectrometry.

  3. Hydrocarbon Gas Liquids (HGL): Recent Market Trends and Issues

    EIA Publications

    2014-01-01

    Over the past five years, rapid growth in U.S. onshore natural gas and oil production has led to increased volumes of natural gas plant liquids (NGPL) and liquefied refinery gases (LRG). The increasing economic importance of these volumes, as a result of their significant growth in production, has revealed the need for better data accuracy and transparency to improve the quality of historical data and projections for supply, demand, and prices of these liquids, co-products, and competing products. To reduce confusion in terminology and improve its presentation of data, EIA has worked with industry and federal and state governments to clarify gas liquid terminology and has developed the term Hydrocarbon Gas Liquids, or HGL.

  4. Optimum design of space storable gas/liquid coaxial injectors.

    NASA Technical Reports Server (NTRS)

    Burick, R. J.

    1972-01-01

    Review of the results of a program of single-element, cold-flow/hot-fire experiments performed for the purpose of establishing design criteria for a high-performance gas/liquid (FLOX/CH4) coaxial injector. The approach and the techniques employed resulted in the direct design of an injector that met or exceeded the performance and chamber compatibility goals of the program without any need for the traditional 'cut-and-try' development methods.

  5. Acoustic probe for solid-gas-liquid suspensions. 1997 annual progress report

    SciTech Connect

    Tavlarides, L.L.; Sangani, A.S.

    1997-01-01

    'Acoustic probes have shown promise to be quite effective in determining the solid content in solid-liquid suspensions. However, the presence of small amounts of gas in the waste slurries stored in tanks across the DOE complex prevents straightforward application for characterization of these slurries. The proposed research will develop an acoustic probe for monitoring particle size and volume fraction in slurries in the absence and the presence of gas bubbles. Theoretical Analysis Accomplished: Attenuation of sound waves depends on the size distribution of the solids and the volume fraction of solids. These can in principle be calculated from attenuation measured over a range of frequencies. However, small amounts of bubbles distort the measured attenuation. A typical result from theoretical analysis for the attenuation of solid- gas-liquid systems is given in Figure 1. The total attenuation of a sound wave v(o) equals the sum of contributions by a large number of ''bins'' of particle sizes. This notion yields the following equation for the (hitherto) unknown number density of solid particles as a function of particle radius N(a): j k(o,a)N(a)da = v(o), where the kernel k(o,a) is obtained from analysis. If N(a) is given, the above equation is used to calculate the attenuation v(o). This is referred to as solving the ''forward problem''. Solving for N(a) with v(o) given is the ''inverse problem''. A complication that one faces when trying to solve the inverse problem is that the stated problem is mathematically ill-posed, i.e., small fluctuations in v(o) cause large fluctuations in the result for the number density. Therefore the problem needs to be ''regularized'', i.e., the stated problem needs to be changed slightly such as to make it well-posed. This has been done by others for gas-liquid systems in the past. This approach is currently being applied in the present project to solid-liquid systems. As is shown in Figure 2, it successfully recovers the number

  6. DYNAMIC MODELING STRATEGY FOR FLOW REGIME TRANSITION IN GAS-LIQUID TWO-PHASE FLOWS

    SciTech Connect

    X. Wang; X. Sun; H. Zhao

    2011-09-01

    In modeling gas-liquid two-phase flows, the concept of flow regime has been used to characterize the global interfacial structure of the flows. Nearly all constitutive relations that provide closures to the interfacial transfers in two-phase flow models, such as the two-fluid model, are often flow regime dependent. Currently, the determination of the flow regimes is primarily based on flow regime maps or transition criteria, which are developed for steady-state, fully-developed flows and widely applied in nuclear reactor system safety analysis codes, such as RELAP5. As two-phase flows are observed to be dynamic in nature (fully-developed two-phase flows generally do not exist in real applications), it is of importance to model the flow regime transition dynamically for more accurate predictions of two-phase flows. The present work aims to develop a dynamic modeling strategy for determining flow regimes in gas-liquid two-phase flows through the introduction of interfacial area transport equations (IATEs) within the framework of a two-fluid model. The IATE is a transport equation that models the interfacial area concentration by considering the creation and destruction of the interfacial area, such as the fluid particle (bubble or liquid droplet) disintegration, boiling and evaporation; and fluid particle coalescence and condensation, respectively. For the flow regimes beyond bubbly flows, a two-group IATE has been proposed, in which bubbles are divided into two groups based on their size and shape (which are correlated), namely small bubbles and large bubbles. A preliminary approach to dynamically identifying the flow regimes is provided, in which discriminators are based on the predicted information, such as the void fraction and interfacial area concentration of small bubble and large bubble groups. This method is expected to be applied to computer codes to improve their predictive capabilities of gas-liquid two-phase flows, in particular for the applications in

  7. About the statistical description of gas-liquid flows

    SciTech Connect

    Sanz, D.; Guido-Lavalle, G.; Carrica, P.

    1995-09-01

    Elements of the probabilistic geometry are used to derive the bubble coalescence term of the statistical description of gas liquid flows. It is shown that the Boltzmann`s hypothesis, that leads to the kinetic theory of dilute gases, is not appropriate for this kind of flows. The resulting integro-differential transport equation is numerically integrated to study the flow development in slender bubble columns. The solution remarkably predicts the transition from bubbly to slug flow pattern. Moreover, a bubbly bimodal size distribution is predicted, which has already been observed experimentally.

  8. Analysis and quantification of plant membrane lipids by thin-layer chromatography and gas chromatography.

    PubMed

    Wewer, Vera; Dörmann, Peter; Hölzl, Georg

    2013-01-01

    Galactolipids represent the predominant membrane lipid class in plants. In general, galactolipids are restricted to plastids, but during phosphate deficiency, they also accumulate in extraplastidial membranes. Two groups of plants can be distinguished based on the presence of a specific fatty acid, hexadecatrienoic acid (16:3), in chloroplast lipids. Plants that contain galactolipids with 16:3 acids are designated "16:3-plants"; the other group of plants which lack 16:3 contain mostly 18:3 in their galactolipids ("18:3-plants"). The methods in this chapter describe the extraction of membrane lipids from whole leaves, or from subcellular fractions, and their analysis via thin-layer chromatography (TLC) with different staining methods. Furthermore, a protocol for membrane lipid quantification is presented starting with the separation via TLC, transmethylation of the isolated lipids to fatty acid methyl esters, and their quantitative analysis via gas chromatography (GC).

  9. Analysis of protein composition using multidimensional chromatography and mass spectrometry.

    PubMed

    Link, Andrew J; Washburn, Michael P

    2014-11-03

    Multidimensional liquid chromatography of peptides produced by protease digestion of complex protein mixtures followed by tandem mass spectrometry can be coupled with automated database searching to identify large numbers of proteins in complex samples. These methods avoid the limitations of gel electrophoresis and in-gel digestions by directly identifying protein mixtures in solution. One method used extensively is named Multidimensional Protein Identification Technology (MudPIT), where reversed-phase chromatography and strong cation-exchange chromatography are coupled directly in a microcapillary column. This column is then placed in line between an HPLC and a mass spectrometer for complex mixture analysis. MudPIT remains a powerful approach for analyzing complex mixtures like whole proteomes and protein complexes. MudPIT is used for quantitative proteomic analysis of complex mixtures to generate novel biological insights.

  10. Vibration-Induced Gas-Liquid Interface Breakup

    NASA Astrophysics Data System (ADS)

    O'Hern, Timothy; Torczynski, John; Romero, Ed; Shelden, Bion

    2010-11-01

    Gas-liquid interfaces can be forced to break up when subjected to vibrations within critical ranges of frequency and amplitude. This breakup mechanism was examined experimentally using deep layers of silicone oils over a range of viscosity and sinusoidal, primarily axial vibration conditions that can produce dramatic disturbances at the gas-liquid free surface. Although small-amplitude vibrations produce standing Faraday waves, large-amplitude vibrations produce liquid jets into the gas, droplets pinching off from the jets, gas cavities in the liquid from droplet impact, and bubble transport below the interface. Experiments used several different silicone oils over a range of pressures and vibration conditions. Computational simulations exhibiting similar behavior will be included in the presentation. Applications include liquid fuel rockets, inertial sensing devices, moving vehicles, mixing processes, and acoustic excitation. Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

  11. Cellular fatty acid analysis as a potential tool for predicting mosquitocidal activity of Bacillus sphaericus strains.

    PubMed Central

    Frachon, E; Hamon, S; Nicolas, L; de Barjac, H

    1991-01-01

    Gas-liquid chromatography of fatty acid methyl esters and numerical analysis were carried out with 114 Bacillus sphaericus strains. Since only two clusters harbored mosquitocidal strains, this technique could be developed in screening programs to limit bioassays on mosquito larvae. It also allows differentiation of highly homologous strains. PMID:1781697

  12. Spatio-temporal evolution of interfacial instabilities in vertical gas-liquid flows

    NASA Astrophysics Data System (ADS)

    Schmidt, Patrick; Valluri, Prashant; Ó Náraigh, Lennon; Lucquiaud, Mathieu

    2014-11-01

    Vertical gas-liquid flows are characteristic for process engineering and widely employed in various technical applications. However, the dynamic behaviour of the liquid interface in such flows is still not fully understood. We focus in our work on characterising the interfacial instability as well as associated interfacial waves in vertical laminar-laminar gas-liquid flows over a wide range of parameters covering different flow regimes, i.e. counter-current, zero-interface velocity (loading) and partial-to-full liquid flow reversal (flooding). High-resolution direct numerical simulations using the TPLS flow solver (http://sourceforge.net/projects/tpls/) reveal the existence of weakly nonlinear interfacial waves, which are in good agreement with Stuart-Landau theory. These waves travel down- or upstream, depending on the flow regime. Furthermore, spatio-temporal linear stability analysis indicates the occurrence of absolute instability within the investigated parameter range. DNS is used to analyse this feature in more detail whereby agreement with linear theory has been established.

  13. Analysis of beechwood creosote by gas chromatography-mass spectrometry and high-performance liquid chromatography.

    PubMed

    Ogata, N; Baba, T

    1989-12-01

    Compounds in beechwood creosote were analyzed by gas chromatography-mass spectrometry, and 22 major constituents were identified. Of these, 19 were phenolic compounds, i. e., guaiacol, phenol, two cresol isomers, four methylguaiacol (creosol) isomers, six xylenol isomers, two trimethylphenol isomers, 4-ethylguaiacol, 4-ethyl-5-methylguaiacol, and 4-propylguaiacol. The remaining three were hitherto unpredicted five-membered ring compounds, i. e., 3-methyl-2-hydroxy-2-cyclopenten-1-one, 3,5-dimethyl-2-hydroxy-2-cyclopenten-1-one, and 3-ethyl-2-hydroxy-2-cyclopenten-1-one. The relative quantities of these compounds were also compared with those obtained by high-resolution high-performance liquid chromatography. This report probably represents the first extensive analysis of beechwood creosote.

  14. Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

    ERIC Educational Resources Information Center

    Riccio, Daniel; Wood, Derrick C.; Miller, James M.

    2008-01-01

    Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal…

  15. GAS/LIQUID MEMBRANES FOR NATURAL GAS UPGRADING

    SciTech Connect

    Howard S. Meyer

    2003-07-01

    Gas Technology Institute (GTI) is conducting this research program whose objective is to develop gas/liquid membranes for natural gas upgrading to assist DOE in achieving their goal of developing novel methods of upgrading low quality natural gas to meet pipeline specifications. Kvaerner Process Systems (KPS) and W. L. Gore & Associates (GORE) gas/liquid membrane contactors are based on expanded polytetrafluoroethylene (ePTFE) membranes acting as the contacting barrier between the contaminated gas stream and the absorbing liquid. These resilient membranes provide much greater surface area for transfer than other tower internals, with packing densities five to ten times greater, resulting in equipment 50-70% smaller and lower weight for the same treating service. The scope of the research program is to (1) build and install a laboratory- and a field-scale gas/liquid membrane absorber; (2) operate the units with a low quality natural gas feed stream for sufficient time to verify the simulation model of the contactors and to project membrane life in this severe service; and (3) conducted an economic evaluation, based on the data, to quantify the impact of the technology. Chevron, one of the major producers of natural gas, has offered to host the test at a gas treating plant. KPS will use their position as a recognized leader in the construction of commercial amine plants for building the unit along with GORE providing the membranes. GTI will provide operator and data collection support during lab- and field-testing to assure proper analytical procedures are used. Kvaerner and GTI will perform the final economic evaluation. GTI will provide project management and be responsible for reporting and interactions with DOE on this project. Efforts this quarter have concentrated on field site selection. ChevronTexaco has nominated their Headlee Gas Plant in Odessa, TX for a commercial-scale dehydration test. Design and cost estimation for this new site are underway. Potting

  16. Chemical analysis of outgassing contaminants on spacecraft surfaces

    NASA Technical Reports Server (NTRS)

    Mcnutt, R. C.

    1973-01-01

    Methods for analyzing and characterizing outgassing contaminants from such materials as RTV 501 potting compound and S 13 G paint are presented. Fractional distillation of a gross distillate from RTV 501 rubber was carried out and the distilled fractions examined as to their ultraviolet and infrared spectra by gas liquid chromatography. A sensitive technique for structural analysis and molecular identification was found to consist of a gas chromatography-mass spectroscopy system, which was determined to be economically unfeasible at present.

  17. Supercritical fluid chromatography for lipid analysis in foodstuffs.

    PubMed

    Donato, Paola; Inferrera, Veronica; Sciarrone, Danilo; Mondello, Luigi

    2017-01-01

    The task of lipid analysis has always challenged separation scientists, and new techniques in chromatography were often developed for the separation of lipids; however, no single technique or methodology is yet capable of affording a comprehensive screening of all lipid species and classes. This review acquaints the role of supercritical fluid chromatography within the field of lipid analysis, from the early developed capillary separations based on pure CO2 , to the most recent techniques employing packed columns under subcritical conditions, including the niche multidimensional techniques using supercritical fluids in at least one of the separation dimensions. A short history of supercritical fluid chromatography will be introduced first, from its early popularity in the late 1980s, to the sudden fall and oblivion until the last decade, experiencing a regain of interest within the chromatographic community. Afterwards, the subject of lipid nomenclature and classification will be briefly dealt with, before discussing the main applications of supercritical fluid chromatography for food analysis, according to the specific class of lipids.

  18. High-Throughput Gas Chromatography for Volatile Compounds Analysis by Fast Temperature Programming and Adsorption Chromatography.

    PubMed

    Gras, Ronda; Hua, Yujuan; Luong, Jim

    2017-03-20

    The synergy of combining fast temperature programming capability and adsorption chromatography using fused silica based porous layer open tubular columns to achieve high throughput chromatography for the separation of volatile compounds is presented.A gas chromatograph with built-in fast temperature programming capability and having a fast cool down rate was used as a platform. When these performance features were combined with the high degree of selectivity and strong retention characteristic of porous layer open tubular column technology, volatile compounds such as light hydrocarbons of up to C7 , primary alcohols, and mercaptans can be well separated and analyzed in a matter of minutes. This analytical approach substantially improves sample throughput by at least a factor of ten times when compared to published methodologies. In addition, the use of porous layer open tubular columns advantageously eliminates the need for costly and time-consuming cryogenic gas chromatography required for the separation of highly volatile compounds by partition chromatography with wall coated open tubular column technology.Relative standard deviations of retention time for model compounds such as alkanes from methane to hexane were found to be less than 0.3% (n = 10) and less than 0.5% for area counts for the compounds tested at two levels of concentration by manual injection, namely, 10 and 1000 ppm v/v (n = 10). Difficult separations were accomplished in one single analysis in less than 2 min such as the characterization of seventeen components in cracked gas containing alkanes, alkenes, dienes, branched hydrocarbons, and cyclic hydrocarbons. This article is protected by copyright. All rights reserved.

  19. Isothermal gas-liquid flow at reduced gravity

    NASA Technical Reports Server (NTRS)

    Dukler, A. E.

    1990-01-01

    Research on adiabatic gas-liquid flows under reduced gravity condition is presented together with experimental data obtained using a NASA-Lewis RC 100-ft drop tower and in a LeRC Learjet. It is found that flow patterns and characteristics remain unchanged after the first 1.5 s into microgravity conditions and that the calculated time for a continuity wave to traverse the test section is less than 1.2 s. It is also found that the dispersed bubbles move at the same velocity as that of the front of the slug and that the transition between bubbly and slug flow is insensitive to diameter. Both the bubbly and the slug flows are suggested to represent a continuum of the same physical process. The characteristics of annular, slug, and bubbly flows are compared.

  20. The application of a non-thermal plasma generated by gas-liquid gliding arc discharge in sterilization

    NASA Astrophysics Data System (ADS)

    Du, Chang Ming; Wang, Jing; Zhang, Lu; Xia Li, Hong; Liu, Hui; Xiong, Ya

    2012-01-01

    Gliding arc discharge has been investigated in recent years as an innovative physicochemical technique for contaminated water treatment at atmospheric pressure and ambient temperature. In this study we tested a gas-liquid gliding arc discharge reactor, the bacterial suspension of which was treated circularly. When the bacterial suspension was passed through the electrodes and circulated at defined flow rates, almost 100% of the bacteria were killed in less than 3.0 min. Experimental results showed that it is possible to achieve an abatement of 7.0 decimal logarithm units within only 30 s. Circulation flow rates and types of feeding gas caused a certain impact on bacteria inactivation, but the influences are not obvious. So, under the promise of sterilization effect, industrial applications can select their appropriate operating conditions. All inactivation curves presented the same three-phase profile showing an apparent sterilization effect. Analysis of the scanning electron microscope images of bacterial cells supports the speculation that the gas-liquid gliding arc discharge plasma is acting under various mechanisms driven essentially by oxidation and the effect of electric field. These results enhance the possibility of applying gas-liquid gliding arc discharge decontamination systems to disinfect bacterial-contaminated water. Furthermore, correlational research indicates the potential applications of this technology in rapid sterilization of medical devices, spacecraft and food.

  1. Jet Engine Exhaust Analysis by Subtractive Chromatography

    DTIC Science & Technology

    1978-12-01

    and J. J. Brooks. Development of a portable miniature collection system for the exposure as- sessment within the microenvironment for carcinogens ...65 A-2. Recovery of acrylonitrile from standard sample generation system ...... ............. 66 B-I. Jet engine exhaust sampling and analysis...7 n-Butane 0.16 2.6 minutes 8 Propylene oxide 3.14 52 minutes 9 Acrylonitrile 9.35 2.6 hours 10 Phenanthrene 1.9 x 106 61 years 11 4-Bromodiphenyl

  2. Simulating Gas-Liquid-Water Partitioning and Fluid Properties of Petroleum under Pressure: Implications for Deep-Sea Blowouts.

    PubMed

    Gros, Jonas; Reddy, Christopher M; Nelson, Robert K; Socolofsky, Scott A; Arey, J Samuel

    2016-07-19

    With the expansion of offshore petroleum extraction, validated models are needed to simulate the behaviors of petroleum compounds released in deep (>100 m) waters. We present a thermodynamic model of the densities, viscosities, and gas-liquid-water partitioning of petroleum mixtures with varying pressure, temperature, and composition based on the Peng-Robinson equation-of-state and the modified Henry's law (Krychevsky-Kasarnovsky equation). The model is applied to Macondo reservoir fluid released during the Deepwater Horizon disaster, represented with 279-280 pseudocomponents, including 131-132 individual compounds. We define >n-C8 pseudocomponents based on comprehensive two-dimensional gas chromatography (GC × GC) measurements, which enable the modeling of aqueous partitioning for n-C8 to n-C26 fractions not quantified individually. Thermodynamic model predictions are tested against available laboratory data on petroleum liquid densities, gas/liquid volume fractions, and liquid viscosities. We find that the emitted petroleum mixture was ∼29-44% gas and ∼56-71% liquid, after cooling to local conditions near the broken Macondo riser stub (∼153 atm and 4.3 °C). High pressure conditions dramatically favor the aqueous dissolution of C1-C4 hydrocarbons and also influence the buoyancies of bubbles and droplets. Additionally, the simulated densities of emitted petroleum fluids affect previous estimates of the volumetric flow rate of dead oil from the emission source.

  3. Principles of micellar electrokinetic capillary chromatography applied in pharmaceutical analysis.

    PubMed

    Hancu, Gabriel; Simon, Brigitta; Rusu, Aura; Mircia, Eleonora; Gyéresi, Arpád

    2013-01-01

    Since its introduction capillary electrophoresis has shown great potential in areas where electrophoretic techniques have rarely been used before, including here the analysis of pharmaceutical substances. The large majority of pharmaceutical substances are neutral from electrophoretic point of view, consequently separations by the classic capillary zone electrophoresis; where separation is based on the differences between the own electrophoretic mobilities of the analytes; are hard to achieve. Micellar electrokinetic capillary chromatography, a hybrid method that combines chromatographic and electrophoretic separation principles, extends the applicability of capillary electrophoretic methods to neutral analytes. In micellar electrokinetic capillary chromatography, surfactants are added to the buffer solution in concentration above their critical micellar concentrations, consequently micelles are formed; micelles that undergo electrophoretic migration like any other charged particle. The separation is based on the differential partitioning of an analyte between the two-phase system: the mobile aqueous phase and micellar pseudostationary phase. The present paper aims to summarize the basic aspects regarding separation principles and practical applications of micellar electrokinetic capillary chromatography, with particular attention to those relevant in pharmaceutical analysis.

  4. Size-exclusion chromatography system for macromolecular interaction analysis

    DOEpatents

    Stevens, Fred J.

    1988-01-01

    A low pressure, microcomputer controlled system employing high performance liquid chromatography (HPLC) allows for precise analysis of the interaction of two reversibly associating macromolecules such as proteins. Since a macromolecular complex migrates faster than its components during size-exclusion chromatography, the difference between the elution profile of a mixture of two macromolecules and the summation of the elution profiles of the two components provides a quantifiable indication of the degree of molecular interaction. This delta profile is used to qualitatively reveal the presence or absence of significant interaction or to rank the relative degree of interaction in comparing samples and, in combination with a computer simulation, is further used to quantify the magnitude of the interaction in an arrangement wherein a microcomputer is coupled to analytical instrumentation in a novel manner.

  5. Evolution of flow disturbances in cocurrent gas-liquid flows

    SciTech Connect

    McCready, M.J.

    1992-10-01

    Studies of interfacial waves in horizontal gas-liquid flows, close to neutral stability, suggest that the rate of evolution of the interface may be linked to nonlinear interactions between the fundamental mode and the subharmonic -- even if the subharmonic is linearly stable. The rate of evolution increases as the subharmonic becomes more unstable. A comparison of linear stability techniques used to predict the initial behavior of waves reveals similar predictions of growth rates and almost identical speeds between a two layer laminar Orr-Sommerfeld theory and an Orr-Sommerfeld theory when the effect of the (turbulent) gas flow enters as boundary conditions on the liquid layer. However, there is disagreement at small wavenumbers as to the point at which the growth curve crosses 0. This is a significant problem because longwave disturbances, in our case roll waves, form by growth of (initially) small amplitude waves that have frequencies which are 0.5 to 1 Hz, which is in the range where the two theories disagree about the sign of the growth rate. While nonlinear effects are probably involved in the formation of the peak (at least while its amplitude is small), the linear growth rate must play an important role when the amplitude is small.

  6. Study of interfacial behavior in cocurrent gas-liquid flows

    SciTech Connect

    McCready, M.J.

    1990-01-01

    We have examined the mechanism of formation of solitary waves on gas-liquid flows and found, that these form from existing periodic waves which have sufficiently large ({approximately}1.5 to 2 depending upon fluid properties) amplitude to liquid layer-thickness ratios. The exact process for the wave shape change is not understood but it does not seem to be related to the wave steepness (amplitude/wavelength) or to separation of gas flow over the waves. The observed confinement of solitary waves to low liquid Reynolds numbers results because the necessary large precursor waves do not form if the wave speed dispersion is too large or if the wavelength of the dominant waves is too short, as occurs for higher Re{sub L}. Measurements of interface tracings and calculations of power spectra and bispectra as a function of flow distance for conditions close to neutral stability reveal that the initially, linearly unstable mode is stabilized by formation of overtones which are linearly stable and can dissipate energy. As a result, a stable wave field can occur. Mode equations, which include quadratic nonlinearities, can model this process to the extent of producing some degree of quantitative predictions for the amplitudes of the wave modes. However, a complete picture of the wave field must include sidebands as well because these are observed for some flow conditions. 34 refs., 12 figs., 2 tabs.

  7. Gas-liquid interface of room-temperature ionic liquids.

    PubMed

    Santos, Cherry S; Baldelli, Steven

    2010-06-01

    The organization of ions at the interface of ionic liquids and the vacuum is an ideal system to test new ideas and concepts on the interfacial chemistry of electrolyte systems in the limit of no solvent medium. Whilst electrolyte systems have numerous theoretical and experimental methods used to investigate their properties, the ionic liquids are relatively new and our understanding of the interfacial properties is just beginning to be explored. In this critical review, the gas-liquid interface is reviewed, as this interface does not depend on the preparation of another medium and thus produces a natural interface. The interface has been investigated by sum frequency generation vibrational spectroscopy and ultra-high vacuum techniques. The results provide a detailed molecular-level view of the surface composition and structure. These have been complemented by theoretical studies. The combinations of treatments on this interface are starting to provide a somewhat convergent description of how the ions are organized at this neat interface (108 references).

  8. Generation of local concentration gradients by gas-liquid contacting.

    PubMed

    de Jong, Jorrit; Verheijden, Pascal W; Lammertink, Rob G H; Wessling, Matthias

    2008-05-01

    We present a generic concept to create local concentration gradients, based on the absorption of gases or vapors in a liquid. A multilayer microfluidic device with crossing gas and liquid channels is fabricated by micromilling and used to generate multiple gas-liquid contacting regions, separated by a hydrophobic membrane. Each crossing can acts as both a microdosing and microstripping region. Furthermore, the liquid and gas flow rate can be controlled independently of each other. The focus of this conceptual article is on the generation of pH gradients, by locally supplying acidic or basic gases/vapors, such as carbon dioxide, hydrochloric acid, and ammonia, visualized by pH-sensitive dyes. Stationary and moving gradients are presented in devices with 500-microm channel width, depths of 200-400 microm, and lengths of multiple centimeters. It is shown that the method allows for multiple consecutive switching gradients in a single microchannel. Absorption measurements in a microcontactor with the model system CO2/water are presented to indicate the dependence of gas absorption rate on channel depth and residence time. Achievable concentration ranges are ultimately limited by the solubility of used components. The reported devices are easy to fabricate, and their application is not limited to pH gradients. Two proof of principles are demonstrated to indicate new opportunities: (i) local crystallization of NaCl using HCl vapor and (ii) consecutive reactions of ammonia with copper(II) ions in solution.

  9. Gas-Liquid Supersonic Cleaning and Cleaning Verification Spray System

    NASA Technical Reports Server (NTRS)

    Parrish, Lewis M.

    2009-01-01

    NASA Kennedy Space Center (KSC) recently entered into a nonexclusive license agreement with Applied Cryogenic Solutions (ACS), Inc. (Galveston, TX) to commercialize its Gas-Liquid Supersonic Cleaning and Cleaning Verification Spray System technology. This technology, developed by KSC, is a critical component of processes being developed and commercialized by ACS to replace current mechanical and chemical cleaning and descaling methods used by numerous industries. Pilot trials on heat exchanger tubing components have shown that the ACS technology provides for: Superior cleaning in a much shorter period of time. Lower energy and labor requirements for cleaning and de-scaling uper.ninih. Significant reductions in waste volumes by not using water, acidic or basic solutions, organic solvents, or nonvolatile solid abrasives as components in the cleaning process. Improved energy efficiency in post-cleaning heat exchanger operations. The ACS process consists of a spray head containing supersonic converging/diverging nozzles, a source of liquid gas; a novel, proprietary pumping system that permits pumping liquid nitrogen, liquid air, or supercritical carbon dioxide to pressures in the range of 20,000 to 60,000 psi; and various hoses, fittings, valves, and gauges. The size and number of nozzles can be varied so the system can be built in configurations ranging from small hand-held spray heads to large multinozzle cleaners. The system also can be used to verify if a part has been adequately cleaned.

  10. Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

    PubMed

    Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-10-03

    Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system.

  11. Gas-Liquid flow characterization in bubble columns with various gas-liquid using electrical resistance tomography

    NASA Astrophysics Data System (ADS)

    Jin, Haibo; Yuhuan, Han; Suohe, Yang

    2009-02-01

    Electrical resistance tomography (ERT) is an advanced and new detecting technique that can measure and monitor the parameters of two-phase flow on line, such as gas-liquid bubble column. It is fit for the industrial process where the conductible medium serves as the disperse phase to present the key bubble flow characteristics in multi-phase medium. Radial variation of the gas holdup and mean holdups are investigated in a 0.160 m i. d. bubble column using ERT with two axial locations (Plane 1 and Plane 2). In all the experiments, air was used as the gas phase, tap water as liquid phase, and a series of experiments were done by adding KCl, ethanol, oil sodium, and glycerol to change liquid conductivity, liquid surface tension and viscosity. The superficial gas velocity was varied from 0.02 to 0.2 m/s. The effect of conductivity, surface tension, viscosity on the mean holdups and radial gas holdup distribution is discussed. The results showed that the gas holdup decrease with the increase of surface tension and increase with the increase of viscosity. Meanwhile, the settings of initial liquid conductivity slightly influence the gas holdup values, and the experimental data increases with the increase of the initial setting values in the same conditions.

  12. Group type analysis of asphalt by column liquid chromatography

    SciTech Connect

    Zhang, C.; Yang, J.; Xue, Y.; Li, Y.

    2008-07-01

    An improved analysis method for characterization of asphalt was established. The method is based on column chromatography technique. The asphalts were separated into four groups: saturates, aromatics, resins, and asphaltenes, quantitatively. About 0.1 g of sample was required in each analysis. About 20 mL of n-heptanes was used to separate out saturates first. Then about 35 mL of n-heptanes/dichloromethane (.5, v/v) mixture was used to separate out aromatics. About 30 mL of dichloromethane/tetrahydrofuran (1/3, v/v) mixture was used to separate out resin. The quality of the separation was confirmed by infrared spectra (IR) and {sup 1}H NMR analysis. The model compounds, tetracosan for saturates, dibenz(o)anthracen for aromatics, and acetanilide for resins were used for verification. The IR and {sup 1}H NMR analysis of the prepared fractions from the column liquid chromatography were in good agreement that of pure reagents.

  13. Acoustic Probe for Solid-Gas-Liquid Suspension

    SciTech Connect

    Tavlarides, L.L.; Sangani, Ashok

    2003-09-14

    /monitoring two-phase flows in relatively ideal, well-characterized suspensions. Two major factors which we judge has prevented its wide-spread use in the processing industry, particularly for dilute suspensions, is careful selection of the frequency range for interrogation and quantification and removal of the noise introduced by bubbles from the acoustic signal obtained from the suspension. Our research during the first funding period to develop an acoustic probe for solid-gas liquid suspensions has resulted in a theory, supported by our experiments, to describe small amplitude dilute suspensions (Norato, 1999, Spelt et al., 1999, Spelt et al., 2001). The theory agrees well with experimental data of sound attenuation up to 45 {approx}01% suspensions of 0.11 and 77 micron radius polystyrene particles in water and 0.4 to 40 vol %, suspensions of 32 micron soda-lime glass particles in water. Also, analyses of our attenuation experiments for solid-gas liquid experiments suggest the theory can be applied to correct for signal interference due to the presence of bubbles over a selected frequency range to permit determination of the solid-liquid volume fraction. Further, we show experimentally that a reliable linear dependency of weight percent solids with attenuation is obtained for low weight fractions at high frequencies of interrogation where bubble interference is minimal. There was a collaborative effort during the first funding period with the Pacific Northwest National Laboratories in that Dr. Margaret Greenwood was a co-investigator on the project. Dr. Greenwood provided a high level of experimental knowledge and techniques on ultrasound propagation, measurement and data processing. During the second funding period the slurry test loop at Oak Ridge National Laboratories under the direction of Mr. Tom Hylton will be employed to demonstrate the measurement capabilities of the prototype acoustic monitor.

  14. Advances in silver ion chromatography for the analysis of fatty acids and triacylglycerols-2001 to 2011.

    PubMed

    Momchilova, Svetlana M; Nikolova-Damyanova, Boryana M

    2012-01-01

    An effort is made to critically present the achievements in silver ion chromatography during the last decade. Novelties in columns, mobile-phase compositions and detectors are described. Recent applications of silver ion chromatography in the analysis of fatty acids and triacylglycerols are presented while stressing novel analytical strategies or new objects. The tendencies in the application of the method in complementary ways with reversed-phase chromatography, chiral chromatography and, especially, mass detection are outlined.

  15. Reuse of spent natural gas liquid sweetening solutions

    SciTech Connect

    Hahn, W.J.; McKim, M.N.; Smith, L.S.

    1995-12-01

    Partially spent caustic solutions from natural gas liquids (NGL) sweetening processes can be used as reagent for sulfur dioxide (SO{sub 2}) scrubbing facilities, reducing the costs for purchasing scrubber reagent and eliminating the costs and liabilities associated with waste disposal. This paper discusses: (1) the characteristics of typical spent NGL sweetening solutions, (2) State and Federal regulations governing the disposal of these solutions as wastes, (3) the operational variables affecting reuse of these solutions in SO{sub 2} scrubbers, (4) field and laboratory analytical data from a pilot project conducted to evaluate the reuse of a partially spent NGL sweetening solution as SO{sub 2} scrubber reagent, and (5) economic data from the pilot project. For the pilot project, a partially spent caustic NGL sweetening solution was used in place of soda ash solution as reagent in a SO{sub 2} scrubber serving two steam generators burning sour gas. Emissions testing of the scrubber demonstrated that the solution provided effective removal of oxides of sulfur (SO{sub x}) in both gaseous and particulate phases to meet permitted limits. Data from the pilot project is used in the paper to: (1) quantify SO{sub 2} scrubber performance with partially spent caustic solutions in terms of SO{sub x} removal efficiency, (2) identify the necessary modifications in scrubber operation (reagent feed rate, scrubber liquor pH and specific gravity, blowdown rate) to achieve acceptable performance using partially spent caustic solutions, and (3) describe the effect that the use of partially spent caustic solutions has on physical and chemical properties of scrubber liquor.

  16. Hydrophilic interaction chromatography (HILIC) in the analysis of antibiotics.

    PubMed

    Kahsay, Getu; Song, Huiying; Van Schepdael, Ann; Cabooter, Deirdre; Adams, Erwin

    2014-01-01

    This paper presents a general overview of the application of hydrophilic interaction chromatography (HILIC) in the analysis of antibiotics in different sample matrices including pharmaceutical, plasma, serum, fermentation broths, environmental water, animal origin, plant origin, etc. Specific applications of HILIC for analysis of aminoglycosides, β-lactams, tetracyclines and other antibiotics are reviewed. HILIC can be used as a valuable alternative LC mode for separating small polar compounds. Polar samples usually show good solubility in the mobile phase containing some water used in HILIC, which overcomes the drawbacks of the poor solubility often encountered in normal phase LC. HILIC is suitable for analyzing compounds in complex systems that elute near the void in reversed-phase chromatography. Ion-pair reagents are not required in HILIC which makes it convenient to couple with MS hence its increased popularity in recent years. In this review, the retention mechanism in HILIC is briefly discussed and a list of important applications is provided including main experimental conditions and a brief summary of the results. The references provide a comprehensive overview and insight into the application of HILIC in antibiotics analysis.

  17. Short-Term Energy Outlook Model Documentation: Hydrocarbon Gas Liquids Supply and Demand

    EIA Publications

    2015-01-01

    The hydrocarbon gas liquids (ethane, propane, butanes, and natural gasoline) module of the Short-Term Energy Outlook (STEO) model is designed to provide forecasts of U.S. production, consumption, refinery inputs, net imports, and inventories.

  18. Receptivity of a Cryogenic Coaxial Gas-Liquid Jet to Acoustic Disturbances (Briefing Charts)

    DTIC Science & Technology

    2014-03-01

    Gas-Liquid Jet to Acoustic Disturbances 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) 5d. PROJECT NUMBER Wegener , Forliti, Leyva...of a Cryogenic Coaxial Gas-Liquid Jet to Acoustic Disturbances 50th AIAA/ASME/SAE/ASEE Joint Propulsion Conference Jeff Wegener , UCLA David Forliti...DISTRIBUTION STATEMENT A. Approved for public release; distribution unlimited. Previous injectors (Sophonias, 2012) New injector ( Wegener , 2013) 13Place

  19. Field gas chromatography-mass spectrometry for fast analysis.

    PubMed

    Makas, Alexei L; Troshkov, Mikhail L

    2004-02-05

    The objective of this presentation is to demonstrate the original device and procedure for fast gas chromatography-mass spectrometry (GC-MS) analysis of gaseous and liquid samples and to discuss its features and capabilities. The concept was developed in order to expand the range of compounds suitable for GC separation and to reduce the time of analysis. Field GC-MS, consisting of original "concentrator-thermodesorber" (CTD) unit, multiple module GC system and compact magnetic mass spectrometer with powerful two-stage vacuum system and multicollector ion detector, is represented. The whole weight of the device is 90 kg. Power consumption is 250 W. The device and analytical procedures allow high speed screening of toxic substances in air and extracts within 100 s per sample. The examples of applications are described, including fast screening of tributyl phosphate (TBP) in air at low ppt level at the rate 1 sample/min.

  20. Modified electrokinetic sample injection method in chromatography and electrophoresis analysis

    DOEpatents

    Davidson, J. Courtney; Balch, Joseph W.

    2001-01-01

    A sample injection method for horizontal configured multiple chromatography or electrophoresis units, each containing a number of separation/analysis channels, that enables efficient introduction of analyte samples. This method for loading when taken in conjunction with horizontal microchannels allows much reduced sample volumes and a means of sample stacking to greatly reduce the concentration of the sample. This reduction in the amount of sample can lead to great cost savings in sample preparation, particularly in massively parallel applications such as DNA sequencing. The essence of this method is in preparation of the input of the separation channel, the physical sample introduction, and subsequent removal of excess material. By this method, sample volumes of 100 nanoliter to 2 microliters have been used successfully, compared to the typical 5 microliters of sample required by the prior separation/analysis method.

  1. Permanent gas analysis using gas chromatography with vacuum ultraviolet detection.

    PubMed

    Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Fan, Hui; Hildenbrand, Zacariah; Wong, Derek; Wetz, David; Schug, Kevin A

    2015-04-03

    The analysis of complex mixtures of permanent gases consisting of low molecular weight hydrocarbons, inert gases, and toxic species plays an increasingly important role in today's economy. A new gas chromatography detector based on vacuum ultraviolet (VUV) spectroscopy (GC-VUV), which simultaneously collects full scan (115-240 nm) VUV and UV absorption of eluting analytes, was applied to analyze mixtures of permanent gases. Sample mixtures ranged from off-gassing of decomposing Li-ion and Li-metal batteries to natural gas samples and water samples taken from private wells in close proximity to unconventional natural gas extraction. Gas chromatography separations were performed with a porous layer open tubular column. Components such as C1-C5 linear and branched hydrocarbons, water, oxygen, and nitrogen were separated and detected in natural gas and the headspace of natural gas-contaminated water samples. Of interest for the transport of lithium batteries were the detection of flammable and toxic gases, such as methane, ethylene, chloromethane, dimethyl ether, 1,3-butadiene, CS2, and methylproprionate, among others. Featured is the capability for deconvolution of co-eluting signals from different analytes.

  2. Urinary 19-norandrosterone purification by immunoaffinity chromatography: application to gas chromatography/combustion/isotope ratio mass spectrometric analysis.

    PubMed

    Desroches, M C; Mathurin, J C; Richard, Y; Delahaut, P; de Ceaurriz, J

    2002-01-01

    The detection of exogenous 19-norandrosterone (19-NA) in urines was investigated by using gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). 19-NA is, for the first time to our knowledge, isolated from urinary matrix by specific immunoaffinity chromatography (IAC) before analysis. The sample preparation consisted of a preliminary purification of urine by solid-phase extraction after hydrolysis by beta-glucuronidase. Unconjugated 19-NA was thus isolated by IAC and directly analysed by GC/C/IRMS. Optimisation of IAC purification was achieved and the reliability of the technique for anti-doping control is discussed.

  3. A continuous film-recirculable drop gas-liquid equilibration device. Measurement of trace gaseous ammonia

    PubMed

    Genfa; Dasgupta

    2000-07-15

    A miniature gas-liquid equilibrator or a gas collector, intended as a low-volume interface between a soluble gaseous sample and a liquid phase analyzer or between a liquid phase sample and a detector designed for use with gas samples, is described. This paper addresses the application of the device for the measurement of trace atmospheric ammonia. Gas collection occurs solely by diffusive sampling such that aerosol particles are not collected. The device essentially consists of a tube surrounded externally by a jacket. Gas flows through the jacket and contacts a liquid film flowing on the surface of the tube. The flowing film forms a drop at the tube terminus and is aspirated off through the inner bore of the tube. The collected analyte can be (a) directly sent to an analysis system or (b) preconcentrated on a suitable stationary phase; the preconcentrator effluent can be recycled, if desired. With a fluorometric flow injection analysis system harnessed to measure ammonia with such a collector, the limit of detection (LOD, S/N = 3) for a sample drawn for 18 min at 200 mL/min was 4.5 parts per trillion by volume, with the linear range extending up to 30 parts per billion.

  4. Characterizing the correlations between local phase fractions of gas-liquid two-phase flow with wire-mesh sensor.

    PubMed

    Tan, C; Liu, W L; Dong, F

    2016-06-28

    Understanding of flow patterns and their transitions is significant to uncover the flow mechanics of two-phase flow. The local phase distribution and its fluctuations contain rich information regarding the flow structures. A wire-mesh sensor (WMS) was used to study the local phase fluctuations of horizontal gas-liquid two-phase flow, which was verified through comparing the reconstructed three-dimensional flow structure with photographs taken during the experiments. Each crossing point of the WMS is treated as a node, so the measurement on each node is the phase fraction in this local area. An undirected and unweighted flow pattern network was established based on connections that are formed by cross-correlating the time series of each node under different flow patterns. The structure of the flow pattern network reveals the relationship of the phase fluctuations at each node during flow pattern transition, which is then quantified by introducing the topological index of the complex network. The proposed analysis method using the WMS not only provides three-dimensional visualizations of the gas-liquid two-phase flow, but is also a thorough analysis for the structure of flow patterns and the characteristics of flow pattern transition. This article is part of the themed issue 'Supersensing through industrial process tomography'.

  5. Interfacial instability in vertical counter-current gas-liquid film flow: theory, direct numerical simulation and experiment

    NASA Astrophysics Data System (ADS)

    Schmidt, Patrick; Ausner, Ilja; Ó Náraigh, Lennon; Lucquiaud, Mathieu; Valluri, Prashant

    2016-11-01

    The dynamics of vertical counter-current gas-liquid flows are largely determined by interfacial instability, which gives rise to a multitude of complex wave patterns and internal flows. To study the genesis and evolution of the instability in detail, we employ theoretical stability analysis, experiment and a newly developed level set method based in-house solver to carry out direct numerical simulations. Crucial results of these simulations, such as growth rate and phase velocity of interfacial waves, are rigorously compared against linear and weakly nonlinear theory; thereby showing remarkable agreement. The analysis also reveals the spatio-temporal character of the waves, depicting regimes of absolute and convective instability. Complementing the benchmark set by (non-)linear theory, we perform film thickness measurements of a real gas-liquid system (air-silicone oil) by means of a non-intrusive light-induced fluorescence technique to further validate the solver regarding its capability of capturing interfacial dynamics accurately. These measurements are in good agreement with the results of the nonlinear direct numerical simulations with respect to wavelength and wave shape of the most unstable mode.

  6. Identification of Drying Oils in Paints by Gas-Liquid Chromatography.

    DTIC Science & Technology

    1982-06-01

    Stearic 4. Oleic 5. Linoleic 6. Impurity 7. Ricinoleic Figure 2. Chromatogram of castor oil methyl ester. 7 DISTRIBUTION FOR MERADCOM REPORT 2360 No...as methyl esters shown on the chromatogram. D D W 103 ENtTIo* OF 0 NOV 4s IS o06IErTE UNCLASSIFIED SECURITY CLASSIFICATION OF TfIS PAGE tfta Date...ILLUSTRATIONS Figure Title Page I Chromatogram of Soybean Oil Methyl Ester 6 2 Chromatogram of Castor Oil Methyl Ester 7 TABLES Table Title Page I Drying Oils

  7. Simultaneous Determination of Lactulose and Mannitol in Urine of Burn Patients by Gas-Liquid Chromatography

    DTIC Science & Technology

    1992-01-01

    Reprinted from CLINICAL CHEMISTRY , 38, 343 (1992), Copyright 1992 by the American Association of Clinical Chemistry and reprinted by permission of...to 300 °C at 15 °C/min. The Received January 28, 1991; accepted January 9, 1992. program was terminated at 20 min. CLINICAL CHEMISTRY , Vol. 38, No...mannttoklactulose dose 344 CLINICAL CHEMISTRY , Vol. 38, No. 3,1992 MANNII(2 LACTULOSE LACTULOSMAMNITOL Handbook and General Catalog, 1989) eliminates the

  8. Quantitative Aging Pattern in Mouse Urine Vapor as Measured by Gas-Liquid Chromatography

    NASA Technical Reports Server (NTRS)

    Robinson, Arthur B.; Dirren, Henri; Sheets, Alan; Miquel, Jaime; Lundgren, Paul R.

    1975-01-01

    We have discovered a quantitative aging pattern in mouse urine vapor. The diagnostic power of the pattern has been found to be high. We hope that this pattern will eventually allow quantitative estimates of physiological age and some insight into the biochemistry of aging.

  9. An improved method for analysis of biomass sugars and galacturonic acid by anion exchange chromatography

    Technology Transfer Automated Retrieval System (TEKTRAN)

    While the most accurate method for analysis of sugars in biomass is based on gas chromatography of trimethylsilane or alditol acetate derivitives of sugars, the derivation method is time consuming and laborious. In comparison, sample preparation for sugar analysis using liquid chromatography is a si...

  10. [Analysis of the phthalates in cosmetics by capillary gas chromatography].

    PubMed

    Chen, Huiming; Wang, Chao; Wang, Xing

    2004-05-01

    A capillary gas chromatographic method with flame ionization detector (GC-FID) for the detection of the six phthalates (dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), butyl benzyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DOP)) in the cosmetics was developed. The phthalates were extracted from cosmetics with methanol under ultrasonication and then separated with high-speed centrifugation. The supernatant was dehydrated and filtrated through membrane with 0.5 microm pore diameter. The filtrate was injected into the GC system for analysis. Then the positive results observed in the GC-FID chromatogram were confirmed by gas chromatography-electron impact-mass detection (GC-EI-MS) analysis. Retention times of the peaks could be applied for qualitative analysis. External standard method was used for quantitative analysis. The recoveries of the six phthalates were between 82.90% and 109.50%. The relative standard deviations were between 2.1% and 4.6%. The detection limits of the method were: 0.1 ng for DMP, DEP, DBP and BBP, and 0.5 ng for DEHP and DOP, respectively. The method presented the advantages of high precision, high sensitivity, small sample size, and simple pretreatment. The method can be used to test the six phthalates in the cosmetics.

  11. Direct numerical simulation of interfacial wave generation in turbulent gas-liquid flows in horizontal channels

    NASA Astrophysics Data System (ADS)

    Campbell, Bryce; Hendrickson, Kelli; Liu, Yuming; Subramani, Hariprasad

    2014-11-01

    For gas-liquid flows through pipes and channels, a flow regime (referred to as slug flow) may occur when waves form at the interface of a stratified flow and grow until they bridge the pipe diameter trapping large elongated gas bubbles within the liquid. Slug formation is often accompanied by strong nonlinear wave-wave interactions, wave breaking, and gas entrainment. This work numerically investigates the fully nonlinear interfacial evolution of a two-phase density/viscosity stratified flow through a horizontal channel. A Navier-Stokes flow solver coupled with a conservative volume-of-fluid algorithm is use to carry out high resolution three-dimensional simulations of a turbulent gas flowing over laminar (or turbulent) liquid layers. The analysis of such flows over a range of gas and liquid Reynolds numbers permits the characterization of the interfacial stresses and turbulent flow statistics allowing for the development of physics-based models that approximate the coupled interfacial-turbulent interactions and supplement the heuristic models built into existing industrial slug simulators.

  12. Comparison of electrical and optical characteristics in gas-phase and gas-liquid phase discharges

    NASA Astrophysics Data System (ADS)

    Qazi, H. I. A.; Nie, Qiu-Yue; Li, He-Ping; Zhang, Xiao-Fei; Bao, Cheng-Yu

    2015-12-01

    This paper presents an AC-excited argon discharge generated using a gas-liquid (two-phase) hybrid plasma reactor, which mainly consists of a powered needle electrode enclosed in a conical quartz tube and grounded deionized water electrode. The discharges in the gas-phase, as well as in the two-phase, exhibit two discharge modes, i.e., the low current glow-like diffuse mode and the high current streamer-like constrict mode, with a mode transition, which exhibits a negative resistance of the discharges. The optical emission spectral analysis shows that the stronger diffusion of the water vapor into the discharge region in the two-phase discharges boosts up the generation of OH (A-X) radicals, and consequently, leads to a higher rotational temperature in the water-phase plasma plume than that of the gas-phase discharges. Both the increase of the power input and the decrease of the argon flow rate result in the increase of the rotational temperature in the plasma plume of the water-phase discharge. The stable two-phase discharges with a long plasma plume in the water-phase under a low power input and gas flow rate may show a promising prospect for the degradation of organic pollutants, e.g., printing and dyeing wastewater, in the field of environmental protection.

  13. Open, microfluidic flow cell for studies of interfacial processes at gas-liquid interfaces.

    PubMed

    Hoang, Khanh C; Malakhov, Dmitry; Momsen, William E; Brockman, Howard L

    2006-03-01

    Interfacial processes involving peripheral proteins depend on the composition and packing density of the interfacial lipid molecules. As a biological membrane model, lipid monolayers at the gas-liquid interface allow independent control of these parameters. However, measuring protein adsorption to monolayers has been difficult. To aid in this and other studies of the interfacial processes, we have developed an open, microfluidic flow cell with which surface physical properties can be controlled and monitored in well-defined lipid monolayers while varying aqueous-phase composition. Using this apparatus, we implement a recently described fluorescence method (Momsen, W. E.; Mizuno, N. K.; Lowe, M. E.; Brockman, H. L. Anal. Biochem. 2005, 346, 139-49) to characterize the adsorption/desorption of glucagon to 1,2-dioleoyl-sn-glycerol monolayers at 27 mN/m. Analysis of the data gives reasonable and self-consistent results for kinetic and thermodynamic constants. Varying the packing density of 1,2-dioleoyl-sn-glycerol does not alter the extent of glucagon adsorption, but comparable measurements with 1-steaoryl-2-oleoyl-sn-glycero-3-phosphocholine show a critical dependence. Because it allows a high degree of control of both lipid monolayer properties and aqueous-phase composition, this microfluidic flow cell should find wide applicability in many areas of research into interfacial processes.

  14. Comparison of electrical and optical characteristics in gas-phase and gas-liquid phase discharges

    SciTech Connect

    Qazi, H. I. A.; Li, He-Ping Zhang, Xiao-Fei; Bao, Cheng-Yu; Nie, Qiu-Yue

    2015-12-15

    This paper presents an AC-excited argon discharge generated using a gas-liquid (two-phase) hybrid plasma reactor, which mainly consists of a powered needle electrode enclosed in a conical quartz tube and grounded deionized water electrode. The discharges in the gas-phase, as well as in the two-phase, exhibit two discharge modes, i.e., the low current glow-like diffuse mode and the high current streamer-like constrict mode, with a mode transition, which exhibits a negative resistance of the discharges. The optical emission spectral analysis shows that the stronger diffusion of the water vapor into the discharge region in the two-phase discharges boosts up the generation of OH (A–X) radicals, and consequently, leads to a higher rotational temperature in the water-phase plasma plume than that of the gas-phase discharges. Both the increase of the power input and the decrease of the argon flow rate result in the increase of the rotational temperature in the plasma plume of the water-phase discharge. The stable two-phase discharges with a long plasma plume in the water-phase under a low power input and gas flow rate may show a promising prospect for the degradation of organic pollutants, e.g., printing and dyeing wastewater, in the field of environmental protection.

  15. A New Void Fraction Measurement Method for Gas-Liquid Two-Phase Flow in Small Channels.

    PubMed

    Li, Huajun; Ji, Haifeng; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing; Wu, Guohua

    2016-01-27

    Based on a laser diode, a 12 × 6 photodiode array sensor, and machine learning techniques, a new void fraction measurement method for gas-liquid two-phase flow in small channels is proposed. To overcome the influence of flow pattern on the void fraction measurement, the flow pattern of the two-phase flow is firstly identified by Fisher Discriminant Analysis (FDA). Then, according to the identification result, a relevant void fraction measurement model which is developed by Support Vector Machine (SVM) is selected to implement the void fraction measurement. A void fraction measurement system for the two-phase flow is developed and experiments are carried out in four different small channels. Four typical flow patterns (including bubble flow, slug flow, stratified flow and annular flow) are investigated. The experimental results show that the development of the measurement system is successful. The proposed void fraction measurement method is effective and the void fraction measurement accuracy is satisfactory. Compared with the conventional laser measurement systems using standard laser sources, the developed measurement system has the advantages of low cost and simple structure. Compared with the conventional void fraction measurement methods, the proposed method overcomes the influence of flow pattern on the void fraction measurement. This work also provides a good example of using low-cost laser diode as a competent replacement of the expensive standard laser source and hence implementing the parameter measurement of gas-liquid two-phase flow. The research results can be a useful reference for other researchers' works.

  16. Gas-liquid phase separation in oppositely charged colloids: stability and interfacial tension.

    PubMed

    Fortini, Andrea; Hynninen, Antti-Pekka; Dijkstra, Marjolein

    2006-09-07

    We study the phase behavior and the interfacial tension of the screened Coulomb (Yukawa) restricted primitive model (YRPM) of oppositely charged hard spheres with diameter sigma using Monte Carlo simulations. We determine the gas-liquid and gas-solid phase transitions using free energy calculations and grand-canonical Monte Carlo simulations for varying inverse Debye screening length kappa. We find that the gas-liquid phase separation is stable for kappasigmagas-liquid interfacial tension using grand-canonical Monte Carlo simulations. The interfacial tension decreases upon increasing the range of the interaction. In particular, we find that simple scaling can be used to relate the interfacial tension of the YRPM to that of the restricted primitive model, where particles interact with bare Coulomb interactions.

  17. Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

    PubMed

    Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

    2016-01-01

    Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed.

  18. Use and practice of achiral and chiral supercritical fluid chromatography in pharmaceutical analysis and purification.

    PubMed

    Lemasson, Elise; Bertin, Sophie; West, Caroline

    2016-01-01

    The interest of pharmaceutical companies for complementary high-performance chromatographic tools to assess a product's purity or enhance this purity is on the rise. The high-throughput capability and economic benefits of supercritical fluid chromatography, but also the "green" aspect of CO2 as the principal solvent, render supercritical fluid chromatography very attractive for a wide range of pharmaceutical applications. The recent reintroduction of new robust instruments dedicated to supercritical fluid chromatography and the progress in stationary phase technology have also greatly benefited supercritical fluid chromatography. Additionally, it was shown several times that supercritical fluid chromatography could be orthogonal to reversed-phase high-performance liquid chromatography and could efficiently compete with it. Supercritical fluid chromatography is an adequate tool for small molecules of pharmaceutical interest: synthetic intermediates, active pharmaceutical ingredients, impurities, or degradation products. In this review, we first discuss about general chromatographic conditions for supercritical fluid chromatography analysis to better suit compounds of pharmaceutical interest. We also discuss about the use of achiral and chiral supercritical fluid chromatography for analytical purposes and the recent applications in these areas. The use of preparative supercritical fluid chromatography by pharmaceutical companies is also covered.

  19. Microemulsion electrokinetic chromatography for analysis of phthalates in soft drinks.

    PubMed

    Hsieh, Sung-Yu; Wang, Chun-Chi; Wu, Shou-Mei

    2013-12-15

    Microemulsion electrokinetic chromatography (MEEKC) is proposed for analysis of di-n-butyl phthalate (DBP) and di-(2-ethylhexyl) phthalate (DEHP) in soft drinks. However, the instability of microemulsion is a critical issue. In this research, a novel material, Pluronic® F-127, which has the properties of polymer and surfactant, was added for stabilizing the microemulsion in the MEEKC system. Our data demonstrate that the presence of Pluronic® F-127 (0.05-0.30%) also helps enhance resolution of highly hydrophobic compounds, DBP and DEHP. The electrokinetic injection of sodium dodecyl sulphate (SDS) including sample (-10 kV, 20 s) was introduced in this MEEKC system and this yielded about 25-fold sensitivity enhancement compared with hydrodynamic injection (1 psi, 10 s). During method validation, calibration curves were linear (r≥0.99), within a range of 75-500 ng/mL for DBP and 150-1000 ng/mL for DEHP. As the precision and accuracy assays, absolute values of relative standard deviation (RSD) and relative error (RE) in intraday (n=3) and interday (n=5) observations were less than 4.93%. This method was further applied for analyzing six commercial soft drinks and one was found containing 453.67 ng/mL of DEHP. This method is considered feasible for serving as a tool for analysis of highly hydrophobic molecules.

  20. The Use of Gas Chromatography for Biogas Analysis

    NASA Astrophysics Data System (ADS)

    Andersen, Amanda; Seeley, John; Aurandt, Jennifer

    2010-04-01

    Energy from natural gas accounts for 24 percent of energy consumed in the US. Natural gas is a robust form of energy which is rich in methane content and is low in impurities. This quality suggests that it is a very clean and safe gas; it can be used in providing heat, a source for cooking, and in powering vehicles. The downside is that it is a non-renewable resource. On the contrary, methane rich gas that is produced by the breakdown of organic material in an anaerobic environment, called biogas, is a renewable energy source. This research focuses on the gas analysis portion of the creation of the anaerobic digestion and verification laboratory where content and forensic analysis of biogas is performed. Gas Chromatography is implemented as the optimal analytical tool for quantifying the components of the biogas including methane, carbon dioxide, hydrogen sulfide and siloxanes. In addition, the problems associated with the undesirable components are discussed. Anaerobic digestion of primary sludge has consistently produced about 55 percent methane; future goals of this research include studying different substrates to increase the methane yield and decrease levels of impurities in the gas.

  1. Analysis of Cordyceps by multi-column liquid chromatography.

    PubMed

    Qian, Zhengming; Li, Shaoping

    2017-03-01

    Cordyceps is a famous traditional Chinese medicine (TCM) that has been used in China for hundreds of years. In the present study a multi-column liquid chromatography (MC-LC) system was developed for the qualitative analysis of macromolecules and micromolecules in Cordyceps. The MC-LC system includes a size exclusion pre-column, a size exclusion column (SEC) and a reversed phase column (RP) which were controlled by column-switching valves. The sample was separated by the size exclusion pre-column into two fractions (macromolecules and micromolecules). These fractions were further separated on SEC and RP columns, respectively. A diode array detector (DAD) and a mass spectrometer (MS) were used to detect the components. This MC-LC method was utilized for analysis of Cordyceps samples. Two macromolecular peaks and 15 micromolecular peaks were found in Cordyceps, and 11 of the micromolecular peaks were identified as adenosine-5'-monophosphate (AMP), phenylalanine, uridine, hypoxanthine, inosine, guanine, guanosine, deoxyadenosine-5'-monophosphate (dAMP), adenosine, adenine and cordycepin (or its isomer). This method is useful for quality control of Cordyceps.

  2. Characterization of annular two-phase gas-liquid flows in microgravity

    NASA Astrophysics Data System (ADS)

    Bousman, W. Scott; McQuillen, John B.

    1994-08-01

    A series of two-phase gas-liquid flow experiments were developed to study annular flows in microgravity using the NASA Lewis Learjet. A test section was built to measure the liquid film thickness around the perimeter of the tube permitting the three dimensional nature of the gas-liquid interface to be observed. A second test section was used to measure the film thickness, pressure drop and wall shear stress in annular microgravity two-phase flows. Three liquids were studied to determine the effects of liquid viscosity and surface tension. The result of this study provide insight into the wave characteristics, pressure drop and droplet entrainment in microgravity annular flows.

  3. A Fixed-Mesh Approach for Gas-Liquid-Rigid Interaction Problems

    NASA Astrophysics Data System (ADS)

    Sugiyama, K.; Okubo, H.; Imahoko, R.; Sakakibara, J.; Takagi, S.

    2016-11-01

    A fixed-mesh approach has been developed to facilitate predicting a certain class of gas-liquid-rigid interaction problems. All the basic equations are discretized on a Cartesian grid in a finite-difference manner. The Volume-Of-Fluid and Boundary Data Immersion methods are employed to treat the gas-liquid and fluid-rigid interfaces, respectively. A hybrid OpenMP- MPI approach is adopted for parallel computing. The developed code is validated through comparisons with experiments of an oil-air flow driven by a rotating disk with holes. The simulated results demonstrate the capability in capturing the velocity distributions.

  4. Characterization of annular two-phase gas-liquid flows in microgravity

    NASA Technical Reports Server (NTRS)

    Bousman, W. Scott; Mcquillen, John B.

    1994-01-01

    A series of two-phase gas-liquid flow experiments were developed to study annular flows in microgravity using the NASA Lewis Learjet. A test section was built to measure the liquid film thickness around the perimeter of the tube permitting the three dimensional nature of the gas-liquid interface to be observed. A second test section was used to measure the film thickness, pressure drop and wall shear stress in annular microgravity two-phase flows. Three liquids were studied to determine the effects of liquid viscosity and surface tension. The result of this study provide insight into the wave characteristics, pressure drop and droplet entrainment in microgravity annular flows.

  5. Analysis of anions in beer using ion chromatography

    PubMed Central

    Bruce, Jonathan

    2002-01-01

    The majority of anions found in beer are a consequence of impurities derived from the water used during the brewing process. The process of beer manufacture consists of malting, brewing and fermentation followed by maturation before filtration and finally storage. Strict quality control is required because the presence of certain anions outside strictly defined tolerance limits can affect the flavour characteristics of the finished product. The anions present were quantified using the technique of ion chromatography with the Metrohm modular system following sample preparation. The analysis produced a result of the order 200 mg l-1 for chloride, phosphate and sulphate and around 20 mg l-1 for nitrate. If the chloride level exceeds 250 mg l-1, then the sweetness of the beer is enhanced, but yeast flocculation can be hindered. An excess of sulphate can give a sharp, dry edge to hopped beers and excessive amounts of nitrate have been found to harm the yeast metabolism after conversion to the nitrite form. As water is a primary ingredient within beer, its quality and type is a fundamental factor in establishing many of the distinctive regional beers that can be found in the United Kingdom and is thus monitored carefully. PMID:18924733

  6. Analysis of anions in beer using ion chromatography.

    PubMed

    Bruce, Jonathan

    2002-01-01

    The majority of anions found in beer are a consequence of impurities derived from the water used during the brewing process. The process of beer manufacture consists of malting, brewing and fermentation followed by maturation before filtration and finally storage. Strict quality control is required because the presence of certain anions outside strictly defined tolerance limits can affect the flavour characteristics of the finished product. The anions present were quantified using the technique of ion chromatography with the Metrohm modular system following sample preparation. The analysis produced a result of the order 200 mg l(-1) for chloride, phosphate and sulphate and around 20 mg l(-1) for nitrate. If the chloride level exceeds 250 mg l(-1), then the sweetness of the beer is enhanced, but yeast flocculation can be hindered. An excess of sulphate can give a sharp, dry edge to hopped beers and excessive amounts of nitrate have been found to harm the yeast metabolism after conversion to the nitrite form. As water is a primary ingredient within beer, its quality and type is a fundamental factor in establishing many of the distinctive regional beers that can be found in the United Kingdom and is thus monitored carefully.

  7. Characterisation of odorants in roasted stem tea using gas chromatography-mass spectrometry and gas chromatography-olfactometry analysis.

    PubMed

    Sasaki, Tetsuya; Koshi, Erina; Take, Harumi; Michihata, Toshihide; Maruya, Masachika; Enomoto, Toshiki

    2017-04-01

    Roasted stem tea has a characteristic flavour, which is obtained by roasting tea stems, by-product of green tea production. This research aims to understand the characteristic odorants in roasted stem tea by comparing it to roasted leaf tea. We revealed potent odorants in commercial roasted stem tea using gas chromatography-mass spectrometry (GC-MS) and gas chromatography-olfactometry with aroma extract dilution analysis (AEDA). The difference between roasted stem and leaf tea derived from the same tea plants were investigated using GC-MS. Pyrazine compounds exhibited a roasted odour and high flavour dilution (FD) factors, as determined via AEDA. Roasted stem tea was richer in these pyrazines than roasted leaf tea. Geraniol and linalool exhibited high FD factors and a floral odour, and roasted stem tea was richer in these compounds than roasted leaf tea. These results may have a positive impact on the development of tea products.

  8. The study of flow characteristic of gas-liquid two-phase flow based on the near-infrared detection device

    NASA Astrophysics Data System (ADS)

    Fang, Lide; Liang, Yujiao; Zhang, Yao; Zhang, Chen; Gao, Jingzhe

    2014-04-01

    With the importance of the two-phase flow, many scholars pay attention on it; and for the so many parameters in the gas-liquid two-phase flow, flow characteristic is the basis. For the four flow patterns in the vertical direction, slug flow, bubbly flow, annular flow, and milk foam-like flow, the paper used the laser diode of 980nm and the silicon photodiode to detect the flow status. The absorption coefficients of the infrared in the gas and the liquid are very different; at the meantime, the infrared is affected by the interface obviously. As a result, it can reflect the fluctuation of the gas-liquid two-phase flow with the detection by the infrared. By analyzing the experiment data, four characteristic parameters are extracted, such as the average value, the variance, the kurtosis, and the frequency center of gravity. They can not only reflect the change of the different flow patterns, but also can reflect the fluctuation in the same flow pattern. The feature vector constituted of the four characteristic parameters can identify the flow pattern correctly in this system. What's more, it can achieve an accurate measurement of the real-time online, providing a basis for the other parameters' analysis in the gas-liquid two-phase flow.

  9. Properties of hydrophobic free energy found by gas-liquid transfer.

    PubMed

    Baldwin, Robert L

    2013-01-29

    The hydrophobic free energy in current use is based on transfer of alkane solutes from liquid alkanes to water, and it has been argued recently that these values are incorrect and should be based instead on gas-liquid transfer data. Hydrophobic free energy is measured here by gas-liquid transfer of hydrocarbon gases from vapor to water. The new definition reduces more than twofold the values of the apparent hydrophobic free energy. Nevertheless, the newly defined hydrophobic free energy is still the dominant factor that drives protein folding as judged by ΔCp, the change in heat capacity, found from the free energy change for heat-induced protein unfolding. The ΔCp for protein unfolding agrees with ΔCp values for solvating hydrocarbon gases and disagrees with ΔCp for breaking peptide hydrogen bonds, which has the opposite sign. The ΔCp values for the enthalpy of liquid-liquid and gas-liquid transfer are similar. The plot of free energy against the apparent solvent-exposed surface area is given for linear alkanes, but only for a single conformation, the extended conformation, of these flexible-chain molecules. The ability of the gas-liquid hydrophobic factor to predict protein stability is tested and reasonable agreement is found, using published data for the dependences on temperature of the unfolding enthalpy of ribonuclease T1 and the solvation enthalpies of the nonpolar and polar groups.

  10. Gas/liquid sensing via chemotaxis of Euglena cells confined in an isolated micro-aquarium.

    PubMed

    Ozasa, Kazunari; Lee, Jeesoo; Song, Simon; Hara, Masahiko; Maeda, Mizuo

    2013-10-21

    We demonstrate on-chip gas/liquid sensing by using the chemotaxis of live bacteria (Euglena gracilis) confined in an isolated micro-aquarium, and gas/liquid permeation through porous polydimethylsiloxane (PDMS). The sensing chip consisted of one closed micro-aquarium and two separated bypass microchannels along the perimeter of the micro-aquarium. Test gas/liquid and reference samples were introduced into the two individual microchannels separately, and the gas/liquid permeated through the PDMS walls and dissolved in the micro-aquarium water, resulting in a chemical concentration gradient in the micro-aquarium. By employing the closed micro-aquarium isolated from sample flows, we succeeded in measuring the chemotaxis of Euglena for a gas substance quantitatively, which cannot be achieved with the conventional flow-type or hydro-gel-type microfluidic devices. We found positive (negative) chemotaxis for CO2 concentrations below (above) 15%, with 64 ppm as the minimum concentration affecting the cells. We also observed chemotaxis for ethanol and H2O2. By supplying culture medium via the microchannels, the Euglena culture remained alive for more than 2 months. The sensing chip is thus useful for culturing cells and using them for environmental toxicity/nutrition studies by monitoring their motion.

  11. Appropriate Formulations for Velocity and Pressure Calculations at Gas-liquid Interface with Collocated Variable Arrangement

    NASA Astrophysics Data System (ADS)

    Ito, Kei; Kunugi, Tomoaki

    A high-precision simulation algorithm for gas-liquid two-phase flows on unstructured meshes has been developed to simulate gas entrainment phenomenon in a sodium-cooled fast reactor. In this study, it became clear that unphysical behaviors near gas-liquid interfaces were caused by conventional algorithms. Then, physics-basis considerations were conducted for mechanical balances at gas-liquid interfaces to derive appropriate formulations. By defining momentum and velocity independently and developing the momentum transport equations for both gas and liquid phases, the physically appropriate formulation of momentum transport was derived, which eliminated the unphysical pressure distribution caused by the conventional formulation. In addition, the physically appropriate formulation was derived for the pressure gradient to satisfy the mechanical balances between pressure and surface tension at gas-liquid interfaces. As the validation test, the rising gas bubble in liquid was simulated by the developed simulation algorithm with the physically appropriate formulations, and the simulated terminal bubble shapes on the structured and highly-distorted unstructured meshes coincided with the experimental data under each simulation condition determined by the Morton and Eötvös numbers.

  12. VACUUM DISTILLATION COUPLED WITH GAS CHROMATOGRAPHY/MASS SPECTROMETRY FOR THE ANALYSIS OF ENVIRONMENTAL SAMPLES

    EPA Science Inventory

    A procedure is presented that uses a vacuum distillation/gas chromatography/mass spectrometry system for analysis of problematic matrices of volatile organic compounds. The procedure compensates for matrix effects and provides both analytical results and confidence intervals from...

  13. Qualitative Analysis of Analgesic Tablets: An Experiment Employing High Pressure Liquid Chromatography.

    ERIC Educational Resources Information Center

    Beaver, Rodney W.; And Others

    1983-01-01

    Describes an experiment on the qualitative analysis of several over-the-counter analgesic tablets. Background information, procedures used (including high pressure liquid chromatography), and typical student results are included. (JN)

  14. Analysis of selected ionic liquid cations by ion exchange chromatography and reversed-phase high performance liquid chromatography.

    PubMed

    Stepnowski, Piotr; Mrozik, Wojciech

    2005-02-01

    The chromatographic behavior of 8 ionic liquids - 7 homologues of 1-alkyl-3-methylimidazolium and 4-methyl-N-butylpyridinium - has been investigated with a strong cation exchange adsorbent. In particular, the dependence of the retention properties of these solutes on mobile phase composition, pH, and buffer concentration was evaluated with the aim of optimizing and improving the selectivity and retention of solute separation. While using the SCX stationary phase, several interactions occurred with varying strengths, depending on the mobile phase composition. Cation exchange, nonspecific hydrophobic interactions, and adsorption chromatography behavior were observed. Reversed phase chromatography occurred at low concentrations of acetonitrile, electrostatic and adsorption interactions at higher organic modifier concentrations. Elevated buffer concentrations lowered the retention factors without affecting the selectivity of ionic liquids. Obtained results were further compared to the chromatographic behaviour of ionic liquids in the reversed phase system. All analyzed ionic liquids follow reversed-phase behavior while being separated. Much lower selectivity in the range of highly hydrophilic compounds is obtained. This suggests preferred use of ion chromatography for separation and analysis of compounds below 4 carbon atoms in the alkyl side chain.

  15. Prediction of acute toxicity of chemicals in mixtures: worms Tubifex tubifex and gas/liquid distribution.

    PubMed

    Tichý, M; Borek-Dohalský, V; Matousová, D; Rucki, M; Feltl, L; Roth, Z

    2002-03-01

    The aim of this contribution is to support our proposal of the procedure for predicting acute toxicity of binary mixtures by QSAR analysis techniques. The changes of a mixture composition are described by molar ratio R and visualized in the R-plot (QCAR--quantitative composition-activity relationships). The approach was inspired by Rault and Dalton's laws, their positive and negative deviations in the behavior of a mixture of real gases, by Loewe and Muischnek isoboles and by the Finney test of additivity. Acute toxicity was determined by the laboratory test with woms Tubifex tubifex. The additivity of the acute toxicity in the binary mixture benzene + nitrobenzene was confirmed and a new interaction is described: "mixed interaction" with the binary mixture aniline + ethanol. The "mixed interaction" means that depending on mixture composition, both potentiation and inhibition can occur. As the first physicochemical descriptor of the changes caused by the changing composition of binary mixtures, the gas/liquid equilibrium was studied and a composition of the gaseous phase was determined by a gas chromatographic method. The method for determination of concentrations in the gaseous phase was described. The gaseous phase composition of benzene + nitrobenzene. benzene + ethanol, benzene + aniline and ethanol + aniline mixtures was analyzed. It was found that if the concentrations of the mixture's components in the gaseous phase behave nonideally (they are not additive), the acute toxicity of the same mixture is not additive as well. Another descriptor to distinguish between potentiation and inhibition will be, however, necessary. The properties, both gaseous phase composition and the acute toxicity, of the benzene + nitrobenzene mixture are additive. In mixtures with the mixed interaction, the R-plot of the composition of the gaseous phase is complex with a large variation of results.

  16. Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography.

    PubMed

    Venkatramani, C J; Al-Sayah, Mohammad; Li, Guannan; Goel, Meenakshi; Girotti, James; Zang, Lisa; Wigman, Larry; Yehl, Peter; Chetwyn, Nik

    2016-02-01

    A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping column/s and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented.

  17. ANALYSIS OF ELECTROLESS NICKEL SOLUTIONS BY ANION CHROMATOGRAPHY

    EPA Science Inventory

    The principal appeal of ion chromatography (IC) as analytical technique lies in the ability to rapidly analyze a mixture of ions of widely varying concentrations and properties in a single elution. It is therefore not surprising that IC has been hampered by the similar ion exchan...

  18. A New Void Fraction Measurement Method for Gas-Liquid Two-Phase Flow in Small Channels

    PubMed Central

    Li, Huajun; Ji, Haifeng; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing; Wu, Guohua

    2016-01-01

    Based on a laser diode, a 12 × 6 photodiode array sensor, and machine learning techniques, a new void fraction measurement method for gas-liquid two-phase flow in small channels is proposed. To overcome the influence of flow pattern on the void fraction measurement, the flow pattern of the two-phase flow is firstly identified by Fisher Discriminant Analysis (FDA). Then, according to the identification result, a relevant void fraction measurement model which is developed by Support Vector Machine (SVM) is selected to implement the void fraction measurement. A void fraction measurement system for the two-phase flow is developed and experiments are carried out in four different small channels. Four typical flow patterns (including bubble flow, slug flow, stratified flow and annular flow) are investigated. The experimental results show that the development of the measurement system is successful. The proposed void fraction measurement method is effective and the void fraction measurement accuracy is satisfactory. Compared with the conventional laser measurement systems using standard laser sources, the developed measurement system has the advantages of low cost and simple structure. Compared with the conventional void fraction measurement methods, the proposed method overcomes the influence of flow pattern on the void fraction measurement. This work also provides a good example of using low-cost laser diode as a competent replacement of the expensive standard laser source and hence implementing the parameter measurement of gas-liquid two-phase flow. The research results can be a useful reference for other researchers’ works. PMID:26828488

  19. Study on measures to improve gas-liquid phase mixing in a multiphase pump impeller under high gas void fraction

    NASA Astrophysics Data System (ADS)

    Zhang, J. Y.; Zhu, H. W.; Ding, K.; Qiang, R.

    2012-11-01

    Rotodynamic multiphase pump can transport crude gas-liquid mixture produced from oil well, and is regarded as the good choice of oil-gas multiphase transportation in offshore product system, for its advantages that compact structure, large flow rate, not sensitive to solid particles in the fluid. However, it is prone to bring about gas-liquid separation within the impeller under high gas void fraction. To solve the problem, this paper presents several measures to break gas packet and inhibit gas-liquid separation, such as, depositing the short blades, opening holes at the blades where gas packets gather, using T-shaped blades, etc. Then, CFD software was used to simulate the flow fields which were added measures to inhibit gas-liquid separation. The results show that streamlines in three new impellers distribute more evenly than in original impeller, the gas-liquid two phases mixed degree was improved, and the gas-liquid separation was inhibited to some extent. However, adding the short blades and using T-blade impeller failed to improve the differential pressure of impellers. So the placement and the geometrical parameters of the measures inhibiting gas-liquid separation should be further optimized.

  20. Strong cation exchange chromatography in analysis of posttranslational modifications: innovations and perspectives.

    PubMed

    Edelmann, Mariola J

    2011-01-01

    Strong cation exchange (SCX) chromatography has been utilized as an excellent separation technique that can be combined with reversed-phase (RP) chromatography, which is frequently used in peptide mass spectrometry. Although SCX is valuable as the second component of such two-dimensional separation methods, its application goes far beyond efficient fractionation of complex peptide mixtures. Here I describe how SCX facilitates mapping of the protein posttranslational modifications (PTMs), specifically phosphorylation and N-terminal acetylation. The SCX chromatography has been mainly used for enrichment of these two PTMs, but it might also be beneficial for high-throughput analysis of other modifications that alter the net charge of a peptide.

  1. Hollow fiber gas-liquid membrane contactors for acid gas capture: a review.

    PubMed

    Mansourizadeh, A; Ismail, A F

    2009-11-15

    Membrane contactors using microporous membranes for acid gas removal have been extensively reviewed and discussed. The microporous membrane acts as a fixed interface between the gas and the liquid phase without dispersing one phase into another that offers a flexible modular and energy efficient device. The gas absorption process can offer a high selectivity and a high driving force for transport even at low concentrations. Using hollow fiber gas-liquid membrane contactors is a promising alternative to conventional gas absorption systems for acid gas capture from gas streams. Important aspects of membrane contactor as an efficient energy devise for acid gas removal including liquid absorbents, membrane characteristics, combination of membrane and absorbent, mass transfer, membrane modules, model development, advantages and disadvantages were critically discussed. In addition, current status and future potential in research and development of gas-liquid membrane contactors for acid gas removal were also briefly discussed.

  2. Measurements of interfacial dynamics of gas-liquid displacement in a capillary

    NASA Astrophysics Data System (ADS)

    Yan, Changfei; Qiu, Huihe

    2016-06-01

    Measurement of liquid film thickness in gas-liquid plug/slug flows is a challenging task. A novel laser interference method for measuring the interfacial film thickness of gas-liquid displacement in a plug flow has been developed. This novel technique utilizes light scattering from different liquid/gas interfaces in forming interference fringes. The interference fringes are used for calculating the film thickness. A set of simultaneous equations is derived based on geometrical optics. The experiment set up is not complex and is easy to install. The fringes are recorded by a charge-coupled device high speed camera and the image data are calculated using fast Fourier transform (FFT) and a non-linear least squares Levenberg-Marquardt algorithm. The uncertainty of this measurement technique is quite small (0.3 μm) and the entire film thickness profile can be measured at the same time.

  3. Investigation Of The High-Voltage Discharge On The Surface Of Gas-Liquid System

    NASA Astrophysics Data System (ADS)

    Nguyen-Kuok, Shi; Morgunov, Aleksandr; Malakhov, Yury; Korotkikh, Ivan

    2016-09-01

    This paper describes an experimental setup for study of physical processes in the high-voltage discharge on the surface of gas-liquid system at atmospheric pressure. Measurements of electrical and optical characteristics of the high-voltage discharge in gas, at the surface of the gas-liquid system and in the electrolyte are obtained. The parameters of the high-voltage discharge and the conditions for its stable operation are presented. Investigations with various electrolytes and cathode assemblies of various materials and sizes were carried out. The installation can be used for the processing and recycling of industrial and chemical liquid waste. Professor of Laboratory of Plasma Physics, National Research University MPEI, Krasnokazarmennya Str.14, 111250, Moscow, Russia.

  4. U.S. crude oil, natural gas, and natural gas liquids reserves 1997 annual report

    SciTech Connect

    Wood, John H.; Grape, Steven G.; Green, Rhonda S.

    1998-12-01

    This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1997, as well as production volumes for the US and selected States and State subdivisions for the year 1997. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), nonassociated gas and associated-dissolved gas (which are the two major types of wet natural gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, reserve estimates for two types of natural gas liquids, lease condensate and natural gas plant liquids, are presented. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. A discussion of notable oil and gas exploration and development activities during 1997 is provided. 21 figs., 16 tabs.

  5. US crude oil, natural gas, and natural gas liquids reserves, 1992 annual report

    SciTech Connect

    Not Available

    1993-10-18

    This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1992, as well as production volumes for the United States, and selected States and State subdivisions for the year 1992. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), its two major components (nonassociated and associated-dissolved gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, two components of natural gas liquids, lease condensate and natural gas plant liquids, have their reserves and production data presented. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. A discussion of notable oil and gas exploration and development activities during 1992 is provided.

  6. Static gas-liquid interfacial direct current discharge plasmas using ionic liquid cathode

    SciTech Connect

    Kaneko, T.

    2009-05-15

    Due to the unique properties of ionic liquids such as their extremely low vapor pressure and high heat capacity, we have succeeded in creating the static and stable gas (plasmas)-liquid (ionic liquids) interfacial field using a direct current discharge under a low gas pressure condition. It is clarified that the ionic liquid works as a nonmetal liquid electrode, and furthermore, a secondary electron emission coefficient of the ionic liquid is larger than that of conventional metal electrodes. The plasma potential structure of the gas-liquid interfacial region, and resultant interactions between the plasma and the ionic liquid are revealed by changing a polarity of the electrode in the ionic liquid. By utilizing the ionic liquid as a cathode electrode, the positive ions in the plasma region are found to be irradiated to the ionic liquid. This ion irradiation causes physical and chemical reactions at the gas-liquid interfacial region without the vaporization of the ionic liquid.

  7. Slug frequency in horizontal gas-liquid flow

    SciTech Connect

    Wallis, G.B. )

    1990-02-01

    This report responds to American Gas Association's(AGA's) objective of initiating and planning means to create a reliable, mechanistic method of slug frequency prediction. Specific objectives were to: update the prior review of existing knowledge; identify one or more alternative modelling approaches; and recommend additional work if required. Examination of empirical correlations for slug frequency shows that they have uncertainties which are large compared with experimental data. A mechanistic approach is sought. Previous mechanistic models have been either incomplete or numerically unstable. Several improvements were made to the Taitel-Dukler model for this process and a new calculation procedure developed using the method of characteristics. It is demonstrated here that this approach alone cannot lead to cyclic slug formation. The processes of wave growth continually wash out downstream without causing new slugs to form upstream. This has led to concentration on the mechanism of slug formation near the inlet to a pipe segment. A new mechanism for cyclic slug formation, dependent on inlet boundary conditions, is proposed and a preliminary analysis developed. It is hypothesized that the formation of each slug transmits pressure fluctuations to the inlet and initiates perturbations there which eventually grow to form a new slug. Given the importance of the inlet conditions in determining slug frequency, lack of detailed knowledge of the boundary conditions for existing slug frequency data precludes meaningful comparisons with those data. It is proposed to develop this theory further and compare it with detailed observations in a small scale air-water test facility where the inlet boundary conditions are well characterized and well controlled in a systematic manner. When the theory is mature, its results will be correlated in a form suitable for practical use. 14 refs., 14 figs.

  8. Column precipitation chromatography: an approach to quantitative analysis of eigencolloids.

    PubMed

    Breynaert, E; Maes, A

    2005-08-01

    A new column precipitation chromatography (CPC) technique, capable of quantitatively measuring technetium eigencolloids in aqueous solutions, is presented. The CPC technique is based on the destabilization and precipitation of eigencolloids by polycations in a confined matrix. Tc(IV) colloids can be quantitatively determined from their precipitation onto the CPC column (separation step) and their subsequent elution upon oxidation to pertechnetate by peroxide (elution step). A clean-bed particle removal model was used to explain the experimental results.

  9. Degradation of Microcystin-LR by Gas-Liquid Interfacial Discharge Plasma

    NASA Astrophysics Data System (ADS)

    Xin, Qing; Zhang, Yi; Wu, Kaibin

    2013-12-01

    In this study, we report on the degradation of microcystin-LR (MC-LR) by gas-liquid interfacial discharge plasma. The influences of operation parameters such as average input voltage, electrode distance and gas flow rate are investigated. Experimental results indicate that the input voltage and gas flow rate have positive influences on MC-LR degradation, while the electrode distance has a negative one. After 6 min discharge with 25 kV average input voltage and 60 L/h air aeration, the degradation rate of MC-LR achieves 75.3%. H2O2 and O3 generated by discharge both in distilled water and MC-LR solution are measured. Moreover, an emission spectroscopy is used as an indicator of the processes that take place on the gas-liquid boundary and inside plasma. Varied types of radicals (O, ·OH, CO, O3, etc.) are proved to be present in the gas phase during gas-liquid interfacial discharge.

  10. U.S. crude oil, natural gas, and natural gas liquids reserves 1995 annual report

    SciTech Connect

    1996-11-01

    The EIA annual reserves report series is the only source of comprehensive domestic proved reserves estimates. This publication is used by the Congress, Federal and State agencies, industry, and other interested parties to obtain accurate estimates of the Nation`s proved reserves of crude oil, natural gas, and natural gas liquids. These data are essential to the development, implementation, and evaluation of energy policy and legislation. This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1995, as well as production volumes for the US and selected States and State subdivisions for the year 1995. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), nonassociated gas and associated-dissolved gas (which are the two major types of wet natural gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, reserve estimates for two types of natural gas liquids, lease condensate and natural gas plant liquids, are presented. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. A discussion of notable oil and gas exploration and development activities during 1995 is provided. 21 figs., 16 tabs.

  11. US crude oil, natural gas, and natural gas liquids reserves 1996 annual report

    SciTech Connect

    1997-12-01

    The EIA annual reserves report series is the only source of comprehensive domestic proved reserves estimates. This publication is used by the Congress, Federal and State agencies, industry, and other interested parties to obtain accurate estimates of the Nation`s proved reserves of crude oil, natural gas, and natural gas liquids. These data are essential to the development, implementation, and evaluation of energy policy and legislation. This report presents estimates of proved reserves of crude oil, natural gas, and natural gas liquids as of December 31, 1996, as well as production volumes for the US and selected States and State subdivisions for the year 1996. Estimates are presented for the following four categories of natural gas: total gas (wet after lease separation), nonassociated gas and associated-dissolved gas (which are the two major types of wet natural gas), and total dry gas (wet gas adjusted for the removal of liquids at natural gas processing plants). In addition, reserve estimates for two types of natural gas liquids, lease condensate and natural gas plant liquids, are presented. Also included is information on indicated additional crude oil reserves and crude oil, natural gas, and lease condensate reserves in nonproducing reservoirs. A discussion of notable oil and gas exploration and development activities during 1996 is provided. 21 figs., 16 tabs.

  12. Ultrasound in gas-liquid systems: effects on solubility and mass transfer.

    PubMed

    Laugier, F; Andriantsiferana, C; Wilhelm, A M; Delmas, H

    2008-09-01

    The effect of ultrasound on the pseudo-solubility of nitrogen in water and on gas-liquid mass transfer kinetics has been investigated in an autoclave reactor equipped with a gas induced impeller. In order to use organic liquids and to investigate the effect of pressure, gas-liquid mass transfer coefficient was calculated from the evolution of autoclave pressure during gas absorption to avoid any side-effects of ultrasound on the concentrations measurements. Ultrasound effect on the apparent solubility is very low (below 12%). Conversely ultrasound greatly improves gas-liquid mass transfer, especially below gas induction speed, this improvement being boosted by pressure. In typical conditions of organic synthesis: 323 K, 1100 rpm, 10 bar, k(L).a is multiplied by 11 with ultrasound (20 kHz/62.6 W). The impact of sonication is much higher on gassing out than on gassing in. In the same conditions, this enhancement is at least five times higher for degassing.

  13. Gas-liquid phase coexistence and crossover behavior of binary ionic fluids with screened Coulomb interactions.

    PubMed

    Patsahan, O

    2014-06-01

    We study the effects of an interaction range on the gas-liquid phase diagram and the crossover behavior of a simple model of ionic fluids: an equimolar binary mixture of equisized hard spheres interacting through screened Coulomb potentials which are repulsive between particles of the same species and attractive between particles of different species. Using the collective variables theory, we find explicit expressions for the relevant coefficients of the effective φ{4} Ginzburg-Landau Hamiltonian in a one-loop approximation. Within the framework of this approximation, we calculate the critical parameters and gas-liquid phase diagrams for varying inverse screening length z. Both the critical temperature scaled by the Yukawa potential contact value and the critical density rapidly decrease with an increase of the interaction range (a decrease of z) and then for z<0.05 they slowly approach the values found for a restricted primitive model (RPM). We find that gas-liquid coexistence region reduces with an increase of z and completely vanishes at z≃2.78. Our results clearly show that an increase in the interaction range leads to a decrease of the crossover temperature. For z≃0.01, the crossover temperature is the same as for the RPM.

  14. Calculations of Gas-liquid Equilibrium in Wellbore with High Carbon dioxide Flow

    NASA Astrophysics Data System (ADS)

    Zhang, Jiaming; Wu, Xiaodong; Wang, Bo; Liu, Kai; Gao, Yue

    2014-05-01

    Carbon dioxide injection not only enhances the oil recovery dramatically, but also it will reduce the greenhouse effect, therefore, Carbon dioxide injection technique is applied extensively. During the process of carbon dioxide displacement, when carbon dioxide breaks though into oil production wells, carbon dioxide content will impacts the phase state and physical properties of the mixed liquor in the wellbore, as a result, it will affect the calculation of temperature and pressure in oil production wells. Applying the conventional black-oil model to calculate the phase state of the miscible fluids is unacceptable. To tackle the problem, this paper uses the gas-liquid flash theory and component model to program software, so that the phase state (gas, liquid or gas-liquid) and physical properties of the mixed liquor (including hydrogen sulfide, carbon dioxide and hydrocarbon) under initial conditions is calculated, moreover, the impact of carbon dioxide content on the physical properties(mainly including density, viscosity, specific heat at const pressure, surface tension, etc) of mixed liquor in oil production wells is analyzed in this paper. The comparison of the results shows that this model can meet the engineering needs with high accuracy.

  15. Broad range analysis of endocrine disruptors and pharmaceuticals using gas chromatography and liquid chromatography tandem mass spectrometry.

    PubMed

    Trenholm, Rebecca A; Vanderford, Brett J; Holady, Janie C; Rexing, David J; Snyder, Shane A

    2006-12-01

    Endocrine disrupting compounds (EDCs) and pharmaceuticals and personal care products (PPCPs) have been globally detected in impacted natural waters. The detection of trace quantities of EDCs and PPCPs in the environment is of great concern since some of these compounds have known physiological responses at low concentrations. EDCs can have a wide range of polarities, acidic and basic moieties, and exist in trace quantities, which often requires numerous complex extractions, large sample collection volumes, and multiple instrumental analyses. A comprehensive method has been developed allowing for the analysis of 58 potential EDCs in various water matrices using a single solid-phase extraction (SPE) of a 1L sample with subsequent analyses using both gas chromatography and liquid chromatography, each coupled with tandem mass spectrometry (GC-MS/MS and LC-MS/MS). Instrument detection limits ranged between 0.12-7.5 pg with corresponding method reporting limits of 1-10 ng l(-1) in water. Recoveries for most compounds were between 50% and 112% with good reproducibility (RSD 6-22%).

  16. Classification of natural resins by liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry using chemometric analysis.

    PubMed

    Rhourrhi-Frih, B; West, C; Pasquier, L; André, P; Chaimbault, P; Lafosse, M

    2012-09-21

    Twenty-six resins from six botanical sources belonging to the class Magnoliopsida were compared based on gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry data. The extracts were analysed by GC after silylation and by reversed phase LC combined with atmospheric pressure photoionisation (APPI) mass spectrometry. The chromatograms were re-organized in data matrices, where each sample was represented by a single column comprising 2755 observations (intensity, time, m/z) in GC-MS and 360 observations in LC-MS. A simple comparison of resin fingerprints was attempted by organizing data according to a three dimensional bubble chart (retention time against m/z where each point was a bubble which size represented the ion intensity) where it is possible to easily superimpose the fingerprints. Thus the common and different species can be easily observed enabling to classify the resins. Hierarchical cluster analysis based on characteristics of GC-MS and LC-MS profiles affords a complete description of the classes of the resins and shows that 26 resins are divided into five main clusters Commiphora mukul, Daniella oliveri, Gardenia gummifera, Canarium madagascariensis, Boswellia dalzielii and Boswellia serrata, respectively. In conclusion, the proposed method has been applied to three other resinous samples from the Burseraceae family to evaluate their alteration state.

  17. Doping control analysis of anabolic steroids in equine urine by gas chromatography-tandem mass spectrometry.

    PubMed

    Wong, April S Y; Leung, Gary N W; Leung, David K K; Wan, Terence S M

    2016-09-08

    Anabolic steroids are banned substances in equine sports. Gas chromatography-mass spectrometry (GC-MS) has been the traditional technique for doping control analysis of anabolic steroids in biological samples. Although liquid chromatography-mass spectrometry (LC/MS) has become an important technique in doping control, the detection of saturated hydroxysteroids by LC-MS remains a problem due to their low ionization efficiency under electrospray. The recent development in fast-scanning gas-chromatography-triple-quadrupole mass spectrometry (GC-MS/MS) has provided a better alternative with a significant reduction in chemical noise by means of selective reaction monitoring. Herein, we present a sensitive and selective method for the screening of over 50 anabolic steroids in equine urine using gas chromatography-tandem mass spectrometry (GC-MS/MS). Copyright © 2016 John Wiley & Sons, Ltd.

  18. [Applications of fast and ultra performance liquid chromatography in the analysis of Chinese herbal medicines].

    PubMed

    Liu, Ying; Zhou, Jianliang; Li, Ping

    2009-09-01

    The analysis of chemical components of Chinese herbal medicines (CHMs) is one of the most critical issues not only for screening and analyzing the bioactive components but also for controlling their quality. However, due to the complexity of the chemical constituents of CHMs, it is difficult to separate them on column within a short time. In the recent, the fast and ultra performance liquid chromatography, including ultra high pressure liquid chromatography, high performance liquid chromatography based on the monolithic columns and high temperature liquid chromatography, are of particular interest because of the high resolution and fast analytical speed provided by these techniques. This overview covers the principle and separation characteristics of these techniques, as well as their applications in Chinese herbal medicines.

  19. Linear and nonlinear instability in vertical counter-current laminar gas-liquid flows

    NASA Astrophysics Data System (ADS)

    Schmidt, Patrick; Ó Náraigh, Lennon; Lucquiaud, Mathieu; Valluri, Prashant

    2016-04-01

    We consider the genesis and dynamics of interfacial instability in vertical gas-liquid flows, using as a model the two-dimensional channel flow of a thin falling film sheared by counter-current gas. The methodology is linear stability theory (Orr-Sommerfeld analysis) together with direct numerical simulation of the two-phase flow in the case of nonlinear disturbances. We investigate the influence of two main flow parameters on the interfacial dynamics, namely the film thickness and pressure drop applied to drive the gas stream. To make contact with existing studies in the literature, the effect of various density contrasts is also examined. Energy budget analyses based on the Orr-Sommerfeld theory reveal various coexisting unstable modes (interfacial, shear, internal) in the case of high density contrasts, which results in mode coalescence and mode competition, but only one dynamically relevant unstable interfacial mode for low density contrast. A study of absolute and convective instability for low density contrast shows that the system is absolutely unstable for all but two narrow regions of the investigated parameter space. Direct numerical simulations of the same system (low density contrast) show that linear theory holds up remarkably well upon the onset of large-amplitude waves as well as the existence of weakly nonlinear waves. For high density contrasts, corresponding more closely to an air-water-type system, linear stability theory is also successful at determining the most-dominant features in the interfacial wave dynamics at early-to-intermediate times. Nevertheless, the short waves selected by the linear theory undergo secondary instability and the wave train is no longer regular but rather exhibits chaotic motion. The same linear stability theory predicts when the direction of travel of the waves changes — from downwards to upwards. We outline the practical implications of this change in terms of loading and flooding. The change in direction of the

  20. Digitally Enhanced Thin-Layer Chromatography: An Inexpensive, New Technique for Qualitative and Quantitative Analysis

    ERIC Educational Resources Information Center

    Hess, Amber Victoria Irish

    2007-01-01

    A study conducted shows that if digital photography is combined with regular thin-layer chromatography (TLC), it could perform highly improved qualitative analysis as well as make accurate quantitative analysis possible for a much lower cost than commercial equipment. The findings suggest that digitally enhanced TLC (DE-TLC) is low-cost and easy…

  1. Effect of Schmidt number on mass transfer across a sheared gas-liquid interface in a wind-driven turbulence

    NASA Astrophysics Data System (ADS)

    Takagaki, Naohisa; Kurose, Ryoichi; Kimura, Atsushi; Komori, Satoru

    2016-11-01

    The mass transfer across a sheared gas-liquid interface strongly depends on the Schmidt number. Here we investigate the relationship between mass transfer coefficient on the liquid side, kL, and Schmidt number, Sc, in the wide range of 0.7 ≤ Sc ≤ 1000. We apply a three-dimensional semi direct numerical simulation (SEMI-DNS), in which the mass transfer is solved based on an approximated deconvolution model (ADM) scheme, to wind-driven turbulence with mass transfer across a sheared wind-driven wavy gas-liquid interface. In order to capture the deforming gas-liquid interface, an arbitrary Lagrangian-Eulerian (ALE) method is employed. Our results show that similar to the case for flat gas-liquid interfaces, kL for the wind-driven wavy gas-liquid interface is generally proportional to Sc‑0.5, and can be roughly estimated by the surface divergence model. This trend is endorsed by the fact that the mass transfer across the gas-liquid interface is controlled mainly by streamwise vortices on the liquid side even for the wind-driven turbulence under the conditions of low wind velocities without wave breaking.

  2. Effect of Schmidt number on mass transfer across a sheared gas-liquid interface in a wind-driven turbulence

    PubMed Central

    Takagaki, Naohisa; Kurose, Ryoichi; Kimura, Atsushi; Komori, Satoru

    2016-01-01

    The mass transfer across a sheared gas-liquid interface strongly depends on the Schmidt number. Here we investigate the relationship between mass transfer coefficient on the liquid side, kL, and Schmidt number, Sc, in the wide range of 0.7 ≤ Sc ≤ 1000. We apply a three-dimensional semi direct numerical simulation (SEMI-DNS), in which the mass transfer is solved based on an approximated deconvolution model (ADM) scheme, to wind-driven turbulence with mass transfer across a sheared wind-driven wavy gas-liquid interface. In order to capture the deforming gas-liquid interface, an arbitrary Lagrangian-Eulerian (ALE) method is employed. Our results show that similar to the case for flat gas-liquid interfaces, kL for the wind-driven wavy gas-liquid interface is generally proportional to Sc−0.5, and can be roughly estimated by the surface divergence model. This trend is endorsed by the fact that the mass transfer across the gas-liquid interface is controlled mainly by streamwise vortices on the liquid side even for the wind-driven turbulence under the conditions of low wind velocities without wave breaking. PMID:27841325

  3. Effect of Schmidt number on mass transfer across a sheared gas-liquid interface in a wind-driven turbulence.

    PubMed

    Takagaki, Naohisa; Kurose, Ryoichi; Kimura, Atsushi; Komori, Satoru

    2016-11-14

    The mass transfer across a sheared gas-liquid interface strongly depends on the Schmidt number. Here we investigate the relationship between mass transfer coefficient on the liquid side, kL, and Schmidt number, Sc, in the wide range of 0.7 ≤ Sc ≤ 1000. We apply a three-dimensional semi direct numerical simulation (SEMI-DNS), in which the mass transfer is solved based on an approximated deconvolution model (ADM) scheme, to wind-driven turbulence with mass transfer across a sheared wind-driven wavy gas-liquid interface. In order to capture the deforming gas-liquid interface, an arbitrary Lagrangian-Eulerian (ALE) method is employed. Our results show that similar to the case for flat gas-liquid interfaces, kL for the wind-driven wavy gas-liquid interface is generally proportional to Sc(-0.5), and can be roughly estimated by the surface divergence model. This trend is endorsed by the fact that the mass transfer across the gas-liquid interface is controlled mainly by streamwise vortices on the liquid side even for the wind-driven turbulence under the conditions of low wind velocities without wave breaking.

  4. On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 1: method of analysis.

    PubMed

    Biedermann, Maurus; Grob, Koni

    2012-09-14

    For the analysis of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH), on-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) offers important advantages: it separates MOSH and MOAH in robust manner, enables direct injection of large aliquots of raw extracts (resulting in a low detection limit), avoids contamination of the sample during preparation and is fully automated. This review starts with an overview of the technology, particularly the fundamentals of introducing large volumes of solvent into GC, and their implementation into various transfer techniques. The main part deals with the concepts of MOSH and MOAH analysis, with a thorough discussion of the choices made. It is followed by a description of the method. Finally auxiliary tools are summarized to remove interfering components, enrich the sample in case of a high fat content and obtain additional information about the MOSH and MOAH composition.

  5. Structural analysis of amorphous phosphates using high performance liquid chromatography

    SciTech Connect

    Sales, B.C.; Boatner, L.A.; Chakoumakos, B.C.; McCallum, J.C.; Ramey, J.O.; Zuhr, R.A.

    1993-12-31

    Determining the atomic-scale structure of amorphous solids has proven to be a formidable scientific and technological problem for the past 100 years. The technique of high-performance liquid chromatography (HPLC) provides unique detailed information regarding the structure of partially disordered or amorphous phosphate solids. Applications of the experimental technique of HPLC to phosphate solids are reviewed, and examples of the type of information that can be obtained with HPLC are presented. Inorganic phosphates encompass a large class of important materials whose applications include: catalysts, ion-exchange media, solid electrolytes for batteries, linear and nonlinear optical components, chelating agents, synthetic replacements for bone and teeth, phosphors, detergents, and fertilizers. Phosphate ions also represent a unique link between living systems and the inorganic world.

  6. Application of gas chromatography to analysis of spirit-based alcoholic beverages.

    PubMed

    Wiśniewska, Paulina; Śliwińska, Magdalena; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek

    2015-01-01

    Spirit-based beverages are alcoholic drinks; their production processes are dependent on the type and origin of raw materials. The composition of this complex matrix is difficult to analyze, and scientists commonly choose gas chromatography techniques for this reason. With a wide selection of extraction methods and detectors it is possible to provide qualitative and quantitative analysis for many chemical compounds with various functional groups. This article describes different types of gas chromatography techniques and their most commonly used associated extraction techniques (e.g., LLE, SPME, SPE, SFE, and SBME) and detectors (MS, TOFMS, FID, ECD, NPD, AED, O or EPD). Additionally, brief characteristics of internationally popular spirit-based beverages and application of gas chromatography to the analysis of selected alcoholic drinks are presented.

  7. Plasma lipid analysis by hydrophilic interaction liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

    PubMed

    Sonomura, Kazuhiro; Kudoh, Shinobu; Sato, Taka-Aki; Matsuda, Fumihiko

    2015-06-01

    A novel method for the analysis of endogenous lipids and related compounds was developed employing hydrophilic interaction liquid chromatography with electrospray ionization tandem mass spectrometry. A hydrophilic interaction liquid chromatography with carbamoyl stationary phase achieved clear separation of phosphatidylcholine, lysophosphatidylcholine, sphingomyelin, ceramide, and mono-hexsosyl ceramide groups with good peak area repeatability (RSD% < 10) and linearity (R(2) > 0.99). The established method was applied to human plasma assays and a total of 117 endogenous lipids were successfully detected and reproducibly identified. In addition, we investigated the simultaneous detection of small polar metabolites such as amino and organic acids co-existing in the same biological samples processed in a single analytical run with lipids. Our results show that hydrophilic interaction liquid chromatography is a useful tool for human plasma lipidome analysis and offers more comprehensive metabolome coverage.

  8. Gas-Liquid Interfacial Non-Equilibrium Plasmas for Structure Controlled Nanoparticles

    NASA Astrophysics Data System (ADS)

    Kaneko, Toshiro

    2013-10-01

    Plasmas generated in liquid or in contact with liquid have attracted much attention as a novel reactive field in the nano-bio material creation because the brand-new chemical and biological reactions are yielded at the gas-liquid interface, which are induced by the physical actions of the non-equilibrium plasmas. In this study, first, size- and structure-controlled gold nanoparticles (AuNPs) covered with DNA are synthesized using a pulse-driven gas-liquid interfacial discharge plasma (GLIDP) for the application to next-generation drug delivery systems. The size and assembly of the AuNPs are found to be easily controlled by changing the plasma parameters and DNA concentration in the liquid. On the other hand, the mono-dispersed, small-sized, and interval-controlled AuNPs are synthesized by using the carbon nanotubes (CNTs) as a template, where the CNTs are functionalized by the ion and radical irradiation in non-equilibrium plasmas. These new materials are now widely applied to the solar cell, optical devices, and so on. Second, highly-ordered periodic structures of the AuNPs are formed by transcribing the periodic plasma structure to the surface of the liquid, where the spatially selective synthesis of the AuNPs is realized. This phenomenon is well explained by the reduction and oxidation effects of the radicals which are generated by the non-equilibrium plasma irradiation to the liquid and resultant dissociation of the liquid. In addition, it is attempted to form nano- or micro-scale periodic structures of the AuNPs based on the self-organizing behavior of turbulent plasmas generated by the nonlinear development of plasma fluctuations at the gas-liquid interface.

  9. Electrical impedance imaging in two-phase, gas-liquid flows: 1. Initial investigation

    NASA Technical Reports Server (NTRS)

    Lin, J. T.; Ovacik, L.; Jones, O. C.

    1991-01-01

    The determination of interfacial area density in two-phase, gas-liquid flows is one of the major elements impeding significant development of predictive tools based on the two-fluid model. Currently, these models require coupling of liquid and vapor at interfaces using constitutive equations which do not exist in any but the most rudimentary form. Work described herein represents the first step towards the development of Electrical Impedance Computed Tomography (EICT) for nonintrusive determination of interfacial structure and evolution in such flows.

  10. Gas liquid flow at microgravity conditions - Flow patterns and their transitions

    NASA Astrophysics Data System (ADS)

    Dukler, A. E.; Fabre, J. A.; McQuillen, J. B.; Vernon, R.

    The prediction of flow patterns during gas-liquid flow in conduits is central to the modern approach for modeling two phase flow and heat transfer. The mechanisms of transition are reasonably well understood for flow in pipes on earth where it has been shown that body forces largely control the behavior observed. This work explores the patterns which exist under conditions of microgravity when these body forces are suppressed. Data are presented which were obtained for air-water flow in tubes during drop tower experiments and Learjet trajectories. Preliminary models to explain the observed flow pattern map are evolved.

  11. On the Motion of an Annular Film in Microgravity Gas-Liquid Flow

    NASA Astrophysics Data System (ADS)

    McQuillen, John B.

    2002-11-01

    Three flow regimes have been identified for gas-liquid flow in a microgravity environment: Bubble, Slug, and Annular. For the slug and annular flow regimes, the behavior observed in vertical upflow in normal gravity is similar to microgravity flow with a thin, symmetrical annular film wetting the tube wall. However, the motion and behavior of this film is significantly different between the normal and low gravity cases. Specifically, the liquid film will slow and come to a stop during low frequency wave motion or slugging. In normal gravity vertical upflow, the film has been observed to slow, stop, and actually reverse direction until it meets the next slug or wave.

  12. Gas liquid flow at microgravity conditions - Flow patterns and their transitions

    NASA Technical Reports Server (NTRS)

    Dukler, A. E.; Fabre, J. A.; Mcquillen, J. B.; Vernon, R.

    1987-01-01

    The prediction of flow patterns during gas-liquid flow in conduits is central to the modern approach for modeling two phase flow and heat transfer. The mechanisms of transition are reasonably well understood for flow in pipes on earth where it has been shown that body forces largely control the behavior observed. This work explores the patterns which exist under conditions of microgravity when these body forces are suppressed. Data are presented which were obtained for air-water flow in tubes during drop tower experiments and Learjet trajectories. Preliminary models to explain the observed flow pattern map are evolved.

  13. Ground Based Studies of Gas-Liquid Flows in Microgravity Using Learjet Trajectories

    NASA Technical Reports Server (NTRS)

    Bousman, W. S.; Dukler, A. E.

    1994-01-01

    A 1.27 cm diameter two phase gas-liquid flow experiment has been developed with the NASA Lewis Research Center to study two-phase flows in microgravity. The experiment allows for the measurement of void fraction, pressure drop, film thickness and bubble and wave velocities as well as for high speed photography. Three liquids were used to study the effects of liquid viscosity and surface tension, and flow pattern maps are presented for each. The experimental results are used to develop mechanistically based models to predict void fraction, bubble velocity, pressure drop and flow pattern transitions in microgravity.

  14. Generalization of low pressure, gas-liquid, metastable sound speed to high pressures

    NASA Technical Reports Server (NTRS)

    Bursik, J. W.; Hall, R. M.

    1981-01-01

    A theory is developed for isentropic metastable sound propagation in high pressure gas-liquid mixtures. Without simplification, it also correctly predicts the minimum speed for low pressure air-water measurements where other authors are forced to postulate isothermal propagation. This is accomplished by a mixture heat capacity ratio which automatically adjusts from its single phase values to approximately the isothermal value of unity needed for the minimum speed. Computations are made for the pure components parahydrogen and nitrogen, with emphasis on the latter. With simplifying assumptions, the theory reduces to a well known approximate formula limited to low pressure.

  15. Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification

    EPA Science Inventory

    Book Chapter 18, titled Application in pesticide analysis: Liquid chromatography - A review of the state of science for biomarker discovery and identification, will be published in the book titled High Performance Liquid Chromatography in Pesticide Residue Analysis (Part of the C...

  16. Hydrophilic interaction chromatography for the analysis of aminoglycosides.

    PubMed

    Kumar, Praveen; Rubies, Antoni; Companyó, Ramon; Centrich, Francesc

    2012-02-01

    The effect of mobile-phase constituents (pH and ionic strength) and chromatographic behaviour of ten aminoglycosides (streptomycin, dihydrostreptomycin, spectinomycin, apramycin, paramomycin, kanamycin A, gentamycin C1, gentamycin C2/C2a, gentamycin C1a and neomycin) in the bare silica, amino, amide and zwitterionic phases of hydrophilic interaction chromatography (HILIC) were studied systematically. Among the stationary phases studied, the zwitterionic phase provided the best separation of aminoglycosides. The effect of pH, ionic concentration and column temperature on retention time, peak shape and sensitivity was studied using a central composite design. pH affected sensitivity of the detection of analytes but not the retention time. High ionic strength in the mobile phase was necessary to control the ionic interactions between ionised aminoglycosides and the hydrophilic phase, thereby influencing peak shape and retention time. Column temperature affected sensitivity of the detection but not the retention time. During method development, crosstalk between the MS/MS channels of the analytes was observed and resolved.

  17. Qualitative analysis of mycotoxins using micellar electrokinetic capillary chromatography

    SciTech Connect

    Holland, R.D.; Sepaniak, M.J. )

    1993-05-01

    Naturally occurring mycotoxins are separated using micellar electrokinetic capillary chromatography. Trends in the retention of these toxins, resulting from changes in mobile-phase composition and pH, are reported and presented as a means of alleviating coelution problems. Two sets of mobile-phase conditions are determined that provide unique separation selectivity. The facile manner by which mobile-phase conditions can be altered, without changes in instrumental configuration, allowed the acquisition of two distinctive, fully resolved chromatograms of 10 mycotoxins in a period of approximately 45 min. By adjusting retention times, using indigenous or added components in mycotoxin samples as normalization standards, it is possible to obtain coefficients of variation in retention time that average less than 1%. The qualitative capabilities of this methodology are evaluated by separating randomly generated mycotoxin-interferent mixtures. In this study, the utilization of normalized retention times applied to separations obtained with two sets of mobile-phase conditions permitted the identification of all the mycotoxins in five unknown samples without any misidentifications. 24 refs., 3 figs., 2 tabs.

  18. Chemical absorption process for degradation of VOC gas using heterogeneous gas-liquid photocatalytic oxidation: toluene degradation by photo-Fenton reaction.

    PubMed

    Tokumura, Masahiro; Nakajima, Rina; Znad, Hussein Tawfeek; Kawase, Yoshinori

    2008-10-01

    A novel process for degradation of toluene in the gas-phase using heterogeneous gas-liquid photocatalytic oxidation has been developed. The degradation of toluene gas by photo-Fenton reaction in the liquid-phase has experimentally examined. The photo-Fenton reaction in the liquid-phase could improve the overall toluene absorption rate by increasing the driving force for mass transfer and as a result enhance the removal of toluene in the exhaust gas. The toluene concentrations in the inlet gas were varied in the range from 0.0968 to 8.69 g m(-3) with initial hydrogen peroxide concentration of 400 mg l(-1) and Fe dose of 5.0 mg l(-1). It was found that toluene in the inlet gas was almost completely dissolved into water and degraded in the liquid-phase for the inlet toluene gas concentration of less than 0.42 g m(-3). The dynamic process of toluene gas degradation by the photo-Fenton reaction providing information for reaction kinetics and mass transfer rate was examined. Toluene removal kinetic analysis indicated that photo-Fenton degradation was significantly affected by H(2)O(2) concentration. The experimental results were satisfactorily described by the predictions simulated using the simplified tanks-in-series model combined with toluene removal kinetic analysis. The present results showed that the proposed chemical absorption process using the photo-Fenton heterogeneous gas-liquid photocatalytic oxidation is very effective for degradation of volatile organic gases.

  19. Analysis and Identification of Acid-Base Indicator Dyes by Thin-Layer Chromatography

    ERIC Educational Resources Information Center

    Clark, Daniel D.

    2007-01-01

    Thin-layer chromatography (TLC) is a very simple and effective technique that is used by chemists by different purposes, including the monitoring of the progress of a reaction. TLC can also be easily used for the analysis and identification of various acid-base indicator dyes.

  20. A multivariate statistical analysis approach to analyze gas chromatography-olfactometry data of tangerine hybrids

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Gas chromatography (GC) hyphenated with olfactometry (O) when a human subject smells the effluent of the GC is a useful technique to identify aroma activity of volatile compounds in a food. Many techniques have been developed, based on olfactory thresholds (CHARM analysis, AEDA), or based on psychop...

  1. ANALYSIS OF FERRIC AND FERROUS IONS IN SOIL EXTRACTS BY ION CHROMATOGRAPHY

    EPA Science Inventory

    A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

  2. High Performance Liquid Chromatography of Some Analgesic Compounds: An Instrumental Analysis Experiment.

    ERIC Educational Resources Information Center

    Haddad, Paul; And Others

    1983-01-01

    Background information, procedures, and results are provided for an experiment demonstrating techniques of solvent selection, gradient elution, pH control, and ion-pairing in the analysis of an analgesic mixture using reversed-phase liquid chromatography on an octadecylsilane column. Although developed using sophisticated/expensive equipment, less…

  3. Flow behaviour and transitions in surfactant-laden gas-liquid vertical flows

    NASA Astrophysics Data System (ADS)

    Zadrazil, Ivan; Chakraborty, Sourojeet; Matar, Omar; Markides, Christos

    2016-11-01

    The aim of this work is to elucidate the effect of surfactant additives on vertical gas-liquid counter-current pipe flows. Two experimental campaigns were undertaken, one with water and one with a light oil (Exxsol D80) as the liquid phase; in both cases air was used as the gaseous phase. Suitable surfactants were added to the liquid phase up to the critical micelle concentration (CMC); measurements in the absence of additives were also taken, for benchmarking. The experiments were performed in a 32-mm bore and 5-m long vertical pipe, over a range of superficial velocities (liquid: 1 to 7 m/s, gas: 1 to 44 m/s). High-speed axial- and side-view imaging was performed at different lengths along the pipe, together with pressure drop measurements. Flow regime maps were then obtained describing the observed flow behaviour and related phenomena, i.e., downwards/upwards annular flow, flooding, bridging, gas/liquid entrainment, oscillatory film flow, standing waves, climbing films, churn flow and dryout. Comparisons of the air-water and oil-water results will be presented and discussed, along with the role of the surfactants in affecting overall and detailed flow behaviour and transitions; in particular, a possible mechanism underlying the phenomenon of flooding will be presented. EPSRC UK Programme Grant EP/K003976/1.

  4. Centrifugal scaling of isothermal gas-liquid flows in horizontal tubes

    NASA Astrophysics Data System (ADS)

    Geraets, Jacques Joseph Marie

    1986-05-01

    To test the similarity criteria of two-phase gas-liquid flows, arising from the governing equations and boundary conditions, the flow of air and a water-glycerine mixture in a 50 mm diameter horizontal tube is compared with a two-phase flow of helium and water in a 5 mm diameter tube rotating around a parallel vertical axis (the effective gravity is 113 g0). Results emphasize that in general only dimensionless correlations provide meaningful predictions. The homogeneous Dukler case 1 (1964b) correlation, which contains no two-phase information, provides the best fit (the standard deviation is 21%) with the measured pressure drops. For predicting flow pattern the most promising approach is that of Taitel and Dukler (1976). Examples of scaling down large diameter, high pressure pipelines are presented. With a scale factor of 1/30 equality of the Froude number, the gas-liquid density ratio, and either the Reynolds number or the Weber number can be realized. Compressibility and gas viscosity are not properly scaled.

  5. Evaluation of high-efficiency gas liquid contactors for natural gas processing

    SciTech Connect

    Palla, N.; Lee, A.L.

    1995-06-01

    The objectives of this program are to develop and evaluate advanced processing technologies that can reduce the cost of upgrading sub quality natural gas to pipeline standards. The successful application of cost-effective, new technologies will facilitate the production of sub quality natural gas that otherwise would be too expensive to produce. The overall program is focused on the following activities: evaluation of the potential of structured packing for the removal of acid gases from natural gases, and expansion of the currently available database of the fluid dynamics of rotating gas liquid contactors. The natural gas sweetening, structured packing field tests are scheduled to be conducted in calendar year 1995. Design, procurement and construction of the field test unit. Expansion of the available data base on the hydraulic characteristics of a rotating gas-liquid contactor is being pursued through a series of laboratory experiments. A 100 GPM, low pressure rotary contactor system has been assembled at IGT`s Energy Development Center to examine the fluid dynamic behavior of this type of contactor. The studies are determining the effects of liquid viscosity, liquid surface tension and operating conditions on liquid residence times and flooding limits.

  6. A compressible two-layer model for transient gas-liquid flows in pipes

    NASA Astrophysics Data System (ADS)

    Demay, Charles; Hérard, Jean-Marc

    2017-03-01

    This work is dedicated to the modeling of gas-liquid flows in pipes. As a first step, a new two-layer model is proposed to deal with the stratified regime. The starting point is the isentropic Euler set of equations for each phase where the classical hydrostatic assumption is made for the liquid. The main difference with the models issued from the classical literature is that the liquid as well as the gas is assumed compressible. In that framework, an averaging process results in a five-equation system where the hydrostatic constraint has been used to define the interfacial pressure. Closure laws for the interfacial velocity and source terms such as mass and momentum transfer are provided following an entropy inequality. The resulting model is hyperbolic with non-conservative terms. Therefore, regarding the homogeneous part of the system, the definition and uniqueness of jump conditions is studied carefully and acquired. The nature of characteristic fields and the corresponding Riemann invariants are also detailed. Thus, one may build analytical solutions for the Riemann problem. In addition, positivity is obtained for heights and densities. The overall derivation deals with gas-liquid flows through rectangular channels, circular pipes with variable cross section and includes vapor-liquid flows.

  7. Observation of Gas-Liquid Flow Near the Exit Orifice of An Effervescent Atomizer

    NASA Astrophysics Data System (ADS)

    Sun, C. H.; Ning, Z.; Lü, M.; Fu, J.; Li, Y. X.

    For deepen the understanding of the mechanism of effervescent atomization: it is necessary to have a better observation on the gas-liquid flow near the exit orifice. Both image and acoustic ways were introduced to observe the gas-fluid flow by a transparent effervescent atomizer. The results show that: It can be clearly seen from images that internal flow regimes make great influence on the spray behavior. Spray acoustic observation is an effective way to grasp the gas-liquid two phases flow behavior when they ejecting from the exit orifice. The acoustic analyzing in time and frequency domain has the ability to obtain the discrete phenomenon existing in effervescent sprays, in thus way, acoustic features could give a new perspective on effervescent spray over time. What's more, the discrete phenomenon in dilute bubbly flow and slug flow can be easily captured from after acoustic analyzing. Uniform two-phase distribution of internal flow shows continues acoustic performance after observing the homogeneous bubbly flow and chum flow.

  8. Decomposition of phenol by hybrid gas/liquid electrical discharge reactors with zeolite catalysts.

    PubMed

    Kusić, Hrvoje; Koprivanac, Natalija; Locke, Bruce R

    2005-10-17

    Application of hybrid gas/liquid electrical discharge reactors and a liquid phase direct electrical discharge reactor for degradation of phenol in the presence and absence of zeolites have been investigated. Hybrid gas/liquid electrical discharges involve simultaneous high voltage electrical discharges in water and in the gas phase above the water surface leading to the additional OH radicals in the liquid phase and ozone formation in the gas phase with subsequent dissolution into the liquid. The role of applied zeolites, namely NH4ZSM5, FeZSM5 and HY, were also studied. Phenol degradation and production of primary phenol by-products, catechol and hydroquinone, during the treatment were monitored by HPLC measurements. The highest phenol removal results, 89.4-93.6%, were achieved by electrical discharge in combination with FeZSM5 in all three configurations of corona reactors. These results indicate that the Fenton reaction has significant influence on overall phenol removal efficiency in the electrical discharge/FeZSM5 system due to the additional OH radical formation from hydrogen peroxide generated by the water phase discharge.

  9. Simulation of drag reduction in superhydrophobic microchannels based on parabolic gas-liquid interfaces

    NASA Astrophysics Data System (ADS)

    Li, Chunxi; Zhang, Shuo; Xue, Quanxi; Ye, Xuemin

    2016-10-01

    Based on the given parabolic gas-liquid interfaces, a two-dimensional fluid flow in superhydrophobic microchannels is numerically simulated with the steady volume of fluid model in the laminar regime. The influence of several crucial parameters on drag reduction effect is discussed. The results indicate that the superhydrophobic microchannel containing rectangular cavities displays significant drag reduction effect. With increasing inlet velocity, the pressure drop reduction decreases slightly. Augments in the pressure drop reduction tend to be large with the increase of the cavity fraction or the decrease of the channel height. The results also reveal that the variation of the normalized slip length with the cavity fraction tends to be more dramatic when the channel height is smaller. As the parabolic height of the gas-liquid interface is enlarged, both the pressure drop reduction and the normalized slip length decrease linearly, while fRe increases linearly. The impact of the cavity depth on the normalized slip length, fRe, and the pressure drop reduction is minimal supposing the depth of the cavity is greater than 40% of its width. The drag reduction effect corresponding to the dovetail cavity model is the best, and the consequence of the rectangular, trapezoidal, and triangular cavity models sequentially worsens.

  10. Shadow imaging in bubbly gas-liquid two-phase flow in porous structures

    NASA Astrophysics Data System (ADS)

    Altheimer, Marco; Häfeli, Richard; Wälchli, Carmen; Rudolf von Rohr, Philipp

    2015-09-01

    Shadow imaging is used for the investigation of bubbly gas-liquid two-phase flow in a porous structure. The porous structure is made of Somos WaterShed XC 11122, a clear epoxy resin used in rapid prototyping. Optical access is provided by using an aqueous solution of sodium iodide and zinc iodide having the same refractive index as the structure material (). Nitrogen is injected into the continuous phase at volumetric transport fractions in the range of resulting in a hold-up of . The obtained images of overlapping bubble shadows are processed to measure the bubble dimensions. Therefore, a new processing sequence is developed to determine bubble dimensions from overlapping bubble shadows by ellipse fitting. The accuracy of the bubble detection and sizing routine is assessed processing synthetic images. It is shown that the developed technique is suitable for volumetric two-phase flow measurements. Important global quantities such as gas hold-up and total interfacial area can be measured with only one camera. Operation parameters for gas-liquid two-phase flows are determined to improve mass and heat transfer between the phases.

  11. A flow reactor setup for photochemistry of biphasic gas/liquid reactions

    PubMed Central

    Schachtner, Josef; Bayer, Patrick

    2016-01-01

    Summary A home-built microreactor system for light-mediated biphasic gas/liquid reactions was assembled from simple commercial components. This paper describes in full detail the nature and function of the required building elements, the assembly of parts, and the tuning and interdependencies of the most important reactor and reaction parameters. Unlike many commercial thin-film and microchannel reactors, the described set-up operates residence times of up to 30 min which cover the typical rates of many organic reactions. The tubular microreactor was successfully applied to the photooxygenation of hydrocarbons (Schenck ene reaction). Major emphasis was laid on the realization of a constant and highly reproducible gas/liquid slug flow and the effective illumination by an appropriate light source. The optimized set of conditions enabled the shortening of reaction times by more than 99% with equal chemoselectivities. The modular home-made flow reactor can serve as a prototype model for the continuous operation of various other reactions at light/liquid/gas interfaces in student, research, and industrial laboratories. PMID:27829887

  12. Two-dimensional thin-layer chromatography in the analysis of secondary plant metabolites.

    PubMed

    Cieśla, Lukasz; Waksmundzka-Hajnos, Monika

    2009-02-13

    Drugs, derived from medicinal plants, have been enjoying a renaissance in the last years. It is due to a great pharmacological potential of herbal drugs, as many natural compounds have been found to exhibit biological activity of wide spectrum. The introduction of whole plants, plant extracts, or isolated natural compounds has led to the need to create the analytical methods suitable for their analysis. The identification of isolated substances is relatively an easy task, but the analysis of plant extracts causes a lot of problems, as they are usually very complex mixtures. Chromatographic methods are one of the most popular techniques applied in the analysis of natural mixtures. Unfortunately the separation power of traditional, one-dimensional techniques, is usually inadequate for separation of more complex samples. In such a case the use of multidimensional chromatography is advised. Planar chromatography gives the possibility of performing two-dimensional separations with the use of one adsorbent with two different eluents or by using bilayer plates or graft thin-layer chromatography (TLC) technique; combinations of different multidimensional techniques are also possible. In this paper, multidimensional planar chromatographic methods, commonly applied in the analysis of natural compounds, were reviewed. A detailed information is given on the methodology of performing two-dimensional separations on one adsorbent, on bilayer plates, with the use of graft TLC and hyphenated methods. General aspects of multidimensionality in liquid chromatography are also described. Finally a reader will find a description of variable two-dimensional methods applied in the analysis of compounds, most commonly encountered in plant extracts. This paper is aimed to draw attention to the potential of two-dimensional planar chromatography in the field of phytochemistry. It may be useful for those who are interested in achieving successful separations of multicomponent mixtures by means

  13. NASA Li/CF(x) cell problem analysis: Anion exchange chromatography analysis

    NASA Astrophysics Data System (ADS)

    Bytella, Joseph

    1991-05-01

    An analysis was made of wiper samples used to wipe down lithium/chlorine fluorine battery components and production equipment. These components and equipment were potentially exposed to thionyl chloride vapors. In the presence of moisture, thionyl chloride decomposes to sulfur dioxide and hydrogen chloride. The wiper samples were analyzed for soluble chlorides and fluorides by anion exchange chromatography. During the examination of the test chromatographs, fluoride contamination was discovered in wiper samples from the test equipment. An analytical method to determine fluoride was developed. The first 3 extracts from the potentially exposed and clean wiper samples were tested, and the total fluoride from both groups determined. A comparison of the results from both groups was made to determine the extent of fluoride contamination.

  14. NASA Li/CF(x) cell problem analysis: Anion exchange chromatography analysis

    NASA Technical Reports Server (NTRS)

    Bytella, Joseph

    1991-01-01

    An analysis was made of wiper samples used to wipe down lithium/chlorine fluorine battery components and production equipment. These components and equipment were potentially exposed to thionyl chloride vapors. In the presence of moisture, thionyl chloride decomposes to sulfur dioxide and hydrogen chloride. The wiper samples were analyzed for soluble chlorides and fluorides by anion exchange chromatography. During the examination of the test chromatographs, fluoride contamination was discovered in wiper samples from the test equipment. An analytical method to determine fluoride was developed. The first 3 extracts from the potentially exposed and clean wiper samples were tested, and the total fluoride from both groups determined. A comparison of the results from both groups was made to determine the extent of fluoride contamination.

  15. Mixed-mode chromatography integrated with high-performance liquid chromatography for protein analysis and separation: Using bovine serum albumin and lysozyme as the model target.

    PubMed

    Xia, Hai-Feng; Don, Bin-Bin; Zheng, Meng-Jie

    2016-05-01

    A type of mixed-mode chromatography was integrated with high-performance liquid chromatography for protein analysis and separation. The chromatographic behavior was tested using bovine serum albumin and lysozyme as model proteins. For the mixed-mode column, the silica beads were activated with γ-(2,3-epoxypropoxy)-propytrimethoxysilane and coupled with 4-mercaptopyridine as the functional ligand. The effects of pH, salt, and the organic solvent conditions of the mobile phase on the retention behavior were studied, which provided valuable clues for separation strategy. When eluted with a suitable pH gradient, salt concentration gradient, and acetonitrile content gradient, the separation behavior of bovine serum albumin and lysozyme could be controlled by altering the conditions of the mobile phase. The results indicated this type of chromatography might be a useful method for protein analysis and separation.

  16. Analysis of phytosterols and phytostanols in enriched dairy products by Fast gas chromatography with mass spectrometry.

    PubMed

    Inchingolo, Raffaella; Cardenia, Vladimiro; Rodriguez-Estrada, Maria Teresa

    2014-10-01

    A Fast gas chromatography and mass spectrometry method for plant sterols/stanols analysis was developed, using a short capillary gas chromatography column (10 m × 0.1 mm internal diameter × 0.1 μm film thickness) coated with 5% diphenyl-polysiloxane. A silylated mixture of the main plant sterols/stanols standards (β-sitosterol, campesterol, stigmasterol, campestanol, sitostanol) was well separated in 1.5 min, with a good peak resolution (>1.4, determined on a critical chromatographic peak pair (β-sitosterol and sitostanol)), repeatability (<13%), and sensitivity (<0.017 ng/mL). The suitability of this Fast chromatography method was tested on plant sterols/stanols-enriched dairy products (yogurt and milk), which were subjected to lipid extraction, cold saponification, and silylation prior to injection. The analytical performance (sensitivity < 0.256 ng/mL and repeatability < 10.36%) and significant reduction of the analysis time and consumables demonstrate that Fast gas chromatography-mass spectrometry method could be also employed for the plant sterols/stanols analysis in functional dairy products.

  17. Recent Advance in Liquid Chromatography/Mass Spectrometry Techniques for Environmental Analysis in Japan

    PubMed Central

    Suzuki, Shigeru

    2014-01-01

    The techniques and measurement methods developed in the Environmental Survey and Monitoring of Chemicals by Japan’s Ministry of the Environment, as well as a large amount of knowledge archived in the survey, have led to the advancement of environmental analysis. Recently, technologies such as non-target liquid chromatography/high resolution mass spectrometry and liquid chromatography with micro bore column have further developed the field. Here, the general strategy of a method developed for the liquid chromatography/mass spectrometry (LC/MS) analysis of environmental chemicals with a brief description is presented. Also, a non-target analysis for the identification of environmental pollutants using a provisional fragment database and “MsMsFilter,” an elemental composition elucidation tool, is presented. This analytical method is shown to be highly effective in the identification of a model chemical, the pesticide Bendiocarb. Our improved micro-liquid chromatography injection system showed substantially enhanced sensitivity to perfluoroalkyl substances, with peak areas 32–71 times larger than those observed in conventional LC/MS. PMID:26819891

  18. Multiresidue analysis of pesticides in soil by gas chromatography with nitrogen-phosphorus detection and gas chromatography mass spectrometry.

    PubMed

    Fenoll, José; Hellín, Pilar; Marín, Cristóbal; Martínez, Carmen M; Flores, Pilar

    2005-10-05

    A rapid multiresidue method for the simultaneous determination of 25 fungicides and insecticides in soil was developed. Soil samples are extracted by sonication with a water-acetonitrile mixture, and the pesticides are partitioned into dichloromethane. Final determination was made by gas chromatography (GC) with nitrogen-phosphorus detection (NPD). Confirmation analysis of pesticides was carried out by GC-MS in the selected ion monitoring (SIM) mode. The identification of compounds was based on retention time and on comparison of the primary and secondary ions. The average recovery by the GC-NPD method obtained for these compounds varied from 68.5% to 112.1% with a relative standard deviation between 1.8% and 6.2%. The GC-NPD method presents good linearity over the range assayed 50-2000 microg/L, and the detection limit for the pesticides studied varied from 0.1 to 10.4 microg/kg. The proposed method was used to determine pesticide levels in soil samples from experimental greenhouse pepper cultivation.

  19. Visualization of gas-liquid mass transfer and wake structure of rising bubbles using pH-sensitive PLIF

    NASA Astrophysics Data System (ADS)

    Stöhr, M.; Schanze, J.; Khalili, A.

    2009-07-01

    A planar laser-induced fluorescence (PLIF) technique for visualizing gas-liquid mass transfer and wake structure of rising gas bubbles is described. The method uses an aqueous solution of the pH-sensitive dye Naphthofluorescein and CO2 as a tracer gas. It features a high spatial resolution and frame rates of up to 500 Hz, providing the ability to capture cinematographic image sequences. By steering the laser beam with a set of two programmable scanning mirrors, sequences of three-dimensional LIF images can be recorded. The technique is applied to freely rising bubbles with diameters between 0.5 and 5 mm, which perform rectilinear, oscillatory or irregular motions. The resulting PLIF image sequences reveal the evolution of characteristic patterns in the near and far wake of the bubbles and prove the potential of the technique to provide new and detailed insights into the spatio-temporal dynamics of mass transfer of rising gas bubbles. The image sequences further allow the estimation of bubble size and rise velocity. The analysis of bubble rise velocities in the Naphthofluorescein solution indicates that surfactant-contaminated conditions are encountered.

  20. TRACE ANALYSIS OF FLUORESCEIN-DERIVATIZED PHENOXY ACID HERBICIDES BY MICELLAR ELECTROKINETIC CHROMATOGRAPHY WITH LASER-INDUCTED FLUORESCENCE DETECTION

    EPA Science Inventory

    Micellar electrokinetic chromatography (MEKC) with laser-induced fluorescence (LIF) detection was used for the trace analysis of phenoxy acid herbicides. Capillary electrophoresis (CE) with LIF detection, which has not previously been used for pesticide analysis, overcomes the po...

  1. High resolution gas chromatography analysis of rice bran oil

    NASA Astrophysics Data System (ADS)

    Yu, Fengxiang; Lin, Qinlu; Chen, Xu; Wei, Xiaojun

    To assess the nutritional value and safety quality of rice bran oil (RBO) ,fatty acids of RBO from 15 species rice come from Hunan Province were analyzed by high resolution gas chromatography (HRGC). Crude RBOs were extracted by hexane 3-times using a solvent-to-rice bran ratio of 3:1 (w/w) at 40°C and composition of RBOs was analyzed by HRGC. The result showed that main fatty acids of 15 kinds of RBO include myristic acid (C14:0), palmitic acid (C16:0), palmitoleic acid (C16:1), stearic acid (C18:0), oleic acid (C18:1), linoleic acid (C18:2), linolenic acid (C18:3), arachidic acid (C20:0), arachidonic acid (C20:1). It is strange that arachidonic acid (C20:1) is not listed in Chinese standard of RBO (GB11192-2003), and it exists in our samples of RBO. The average value of linolenic acid in RBOs is 1.6304% (range from 1.2425% to 2.131%), and it showed higher level comparing with Chinese standard that linolenic acid is less than 1.0%. The average value of USFA and SFA are 76.81% (range 75.96% to 82.06% ) and 20.15% (range 13.72% to 23.06%) respectively, and USFA content is close to olive oil (83.75%), peanut oil (81.75%) and soybean oil (85.86%). USFA in Jingyou 13 RBO is the highest content. The ratio of USFA to SFA content is 4:1 (range from 3.32 to 5.98:1). The ratio of SFA: MUFA: PUFA of 15 RBOs is 1: 2.2: 1.8, and ω6/ω3 ratio is 21.69 (range from16.54 to 27.28) and it is close to the 26:1 which is reported to be helpful to increase SOD activity. The oleic acid /linoleic acid ratio of 15 RBOs is 1.23:1 (rang from 1.04:1 to 1.42:1). Our data analyzed composition of RBOs from 15 species rice of China and will provide new evidence to revise RBO standard. It also helps us to assess nutritional value of RBOs and identify different RBOs from various species rice and places of origin.

  2. Micromachined Gas Chromatography Microsystem For Complex Gas Analysis (BRIEFING CHARTS)

    DTIC Science & Technology

    2007-03-07

    Wireless Integrated Microsystems (WIMS), Applications • Gas Analysis Using µGC • The “Actuator”: Integrated Gas Micropump • Concluding Remarks, Future...mode Analysis mode • No previous gas micropump meets the WIMS µGC requirements. • Size and power...leakage. • Single mode operation Summary of Previous Gas Micropumps NSF ERC for Wireless Integrated MicroSystems (WIMS) 22 • Goal: Develop a miniature

  3. Basic study on an energy conversion system using gas-liquid two-phase flows of magnetic fluid

    SciTech Connect

    Okubo, Masaaki; Ishimoto, Jun; Kamiyama, Schinichi.

    1994-12-31

    The mechanism of the pressure rise in a gas-liquid two-phase pipe flow of magnetic fluid under a nonuniform magnetic field is investigated in detail both theoretically and experimentally. First, governing equations of one-dimensional gas-liquid two-phase magnetic fluid flow are presented and numerically solved. Next, the pressure distribution in a nonuniform magnetic wild region is measured in the cases of two-phase flow, single-phase flow and the stationary state using a new experimental apparatus for the flow system. From the numerical measurement results, the magnitude of the pressure components which contribute to the total driving force is accurately estimated. These results on the pressure distribution will contribute to the development of the new energy conversion system using a gas-liquid two-phase magnetic fluid flow.

  4. A new contactless impedance sensor for void fraction measurement of gas-liquid two-phase flow

    NASA Astrophysics Data System (ADS)

    Ji, Haifeng; Chang, Ya; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing

    2016-12-01

    With impedance elimination principle and phase sensitive demodulation (PSD) technique, this work aims to develop a new contactless impedance sensor, which is suitable for the void fraction measurement of gas-liquid two-phase flow. The impedance elimination principle is used to overcome the unfavorable influences of the coupling capacitances, i.e. the capacitive reactances of the coupling capacitances are eliminated by the inductive reactance of an introduced inductor. PSD technique is used to implement the impedance measurement. Unlike the conventional conductance/impedance sensors which use the equivalent conductance (the real part of the impedance) or the amplitude of the impedance of gas-liquid two-phase flow, the new contactless impedance sensor makes full use of the total impedance information of gas-liquid two-phase flow (including the amplitude, the real part and the imaginary part of the impedance, especially the imaginary part) to implement the void fraction measurement. As a preliminary study, to verify the effectiveness of the new contactless impedance sensor, two prototypes (with different inner diameters of 17.0 mm and 22.0 mm) are developed and experiments are carried out. Two typical flow patterns (bubble flow and stratified flow) of gas-liquid two-phase flow are investigated. The experimental results show that the new contactless impedance sensor is successful and effective. Compared with the conventional conductance/impedance sensors, the new contactless impedance sensor can avoid polarization effect and electrochemical erosion effect. The total impedance information is used and the void fraction measurement performance of the new sensor is satisfactory. The experimental results also indicate that the imaginary part of the impedance of gas-liquid two-phase flow is very useful for the void fraction measurement. Making full use of the total impedance information of gas-liquid two-phase flow can effectively improve the void fraction measurement

  5. Colloidal gas-liquid condensation of polystyrene latex particles with intermediate kappa a values (5 to 160, a > kappa(-1)).

    PubMed

    Ishikawa, Masamichi; Kitano, Ryota

    2010-02-16

    Polystyrene latex particles showed gas-liquid condensation under the conditions of large particle radius (a > kappa(-1)) and intermediate kappa a, where kappa is the Debye-Hückel parameter and a is the particle radius. The particles were dissolved in deionized water containing ethanol from 0 to 77 vol %, settled to the bottom of the glass plate within 1 h, and then laterally moved toward the center of a cell over a 20 h period in reaching a state of equilibrium condensation. All of the suspensions that were 1 and 3 microm in diameter and 0.01-0.20 vol % in concentration realized similar gas-liquid condensation with clear gas-liquid boundaries. In 50 vol % ethanol solvent, additional ethanol was added to enhance the sedimentation force so as to restrict the particles in a monoparticle layer thickness. The coexistence of gas-liquid-solid (crystalline solid) was microscopically recognized from the periphery to the center of the condensates. A phase diagram of the gas-liquid condensation was created as a function of KCl concentration at a particle diameter of 3 microm, 0.10 vol % concentration, and 50:50 water/ethanol solvent at room temperature. The miscibility gap was observed in the concentration range from 1 to 250 microM. There was an upper limit of salt concentration where the phase separation disappeared, showing nearly critical behavior of macroscopic density fluctuation from 250 microM to 1 mM. These results add new experimental evidence to the existence of colloidal gas-liquid condensation and specify conditions of like-charge attraction between particles.

  6. Analysis of nitroguanidine in Aqueous Solutions by HPLC (High Performance Liquid Chromatography) with electrochemical Detection and Voltammetry

    DTIC Science & Technology

    1987-04-01

    The nitroguanidine was analyzed by high performance liquid chromatography (HPLC) with electrochemical detection at a hanging miercury drop electrode...previously reported on the application of solid sorbent collection techniques to the analysis of several explosives in water by high performance liquid chromatography (HPLC

  7. Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

    PubMed

    Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

    2016-04-01

    In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures.

  8. Analysis of radioactive mixed hazardous waste using derivatization gas chromatography/mass spectrometry, liquid chromatography, and liquid chromatography/mass spectrometry

    SciTech Connect

    Campbell, J.A.; Lerner, B.D.; Bean, R.M.; Grant, K.E.; Lucke, R.B.; Mong, G.M.; Clauss, S.A.

    1994-08-01

    Six samples of core segments from Tank 101-SY were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry. The major components detected were ethylenediaminetetraacetic acid, nitroso-iminodiacetic acid, nitrilotriacetic acid, citric acid, succinic acid, and ethylenediaminetriacetic acid. The chelator of highest concentration was ethylenediaminetetraacetic acid in all six samples analyzed. Liquid chromatography was used to quantitate low molecular weight acids including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon in the samples analyzed was accounted for by these acids.

  9. Rapid analysis of phentolamine by high-performance liquid chromatography.

    PubMed

    Webster, Gregory K; Lemmer, Robert R; Greenwald, Steven

    2003-02-01

    A rapid liquid chromatographic method is validated for the quantitative analysis of phentolamine. Phentolamine exists in three forms for this investigation: as a mesylate salt, hydrochloride salt, and free base. In solution, phentolamine dissociates from its salt and is chromatographed as free phentolamine. This validation confirms the analysis of each form, which is simply based upon molar mass differences encountered in weighing. As such, both the United States Pharmacopeia hydrochloride and mesylate standards are used throughout this validation to demonstrate this equivalency. The validation demonstrates that this method may be used to quantitate phentolamine, regardless of its salt form.

  10. The Analysis of Metal Finishing Solutions by Ion Chromatography

    DTIC Science & Technology

    1987-08-01

    traditional chemical methods now in use. This report describes procedures for the analysis of solutions for chromium plating, acid finishing, metal...samples and standards must have similar acid -base characteristics. These methods are an improvement to standard methods now in practice and have been...CITED ............................... 195 iv LIST OF TABLES Page Table 1. Ionization Constants of Acids (12) . 29 Table 2. Common Anion Eluents

  11. Study of Co-Current and Counter-Current Gas-Liquid Two-Phase Flow Through Packed Bed in Microgravity

    NASA Astrophysics Data System (ADS)

    Revankar, Shripad T.

    2002-11-01

    The main goal of the project is to obtain new experimental data and development of models on the co-current and counter-current gas-liquid two-phase flow through a packed bed in microgravity and characterize the flow regime transition, pressure drop, void and interfacial area distribution, and liquid hold up. Experimental data will be obtained for earth gravity and microgravity conditions. Models will be developed for the prediction of flow regime transition, void fraction distribution and interfacial area concentration, which are key parameters to characterize the packed bed performance. Thus the specific objectives of the proposed research are to: (1) Develop experiments for the study of the gas liquid two-phase flow through the packed bed with three different flow combinations: co-current down flow, co-current upflow and counter current flow. (2) Develop pore scale and bed scale two-phase instrumentation for measurement of flow regime transition, void distribution and gas-liquid interfacial area concentration in the packed bed. (3) Obtain database on flow regime transition, pressure drop, void distribution, interfacial area concentration and liquid hold up as a function of bed characteristics such as bed particle size, porosity, and liquid properties such as viscosity and surface tension. (4) Develop mathematical model for flow regime transition, void fraction distribution and interfacial area concentration for co-current gas-liquid flow through the porous bed in gravity and micro gravity conditions.(4) Develop mathematical model for the flooding phenomena in counter-current gas-liquid flow through the porous bed in gravity and micro gravity conditions. The present proposal addresses the most important topic of HEDS-specific microgravity fluid physics research identified by NASA 's one of the strategic enterprises, OBPR Enterprise. The proposed project is well defined and makes efficient use of the ground-based parabolic flight research aircraft facility. The

  12. Critical lines for a generalized three state binary gas-liquid lattice model

    NASA Astrophysics Data System (ADS)

    Meijer, Paul H. E.; Keskin, Mustafa; Pegg, Ian L.

    1988-02-01

    The critical properties of several compressible binary gas-liquid models are described: the three state lattice gas, the Tompa model for polymer solutions, the van der Waals equation for binary mixtures, and an intermediate model. The critical lines are expressed as functions of x1 and x2, the density of type 1 molecules and the density of type 2 molecules, instead of using the pressure and temperature; representative figures are given for each of the models. The general conditions for criticality, stability, and tricriticality are given as functions of x1 and x2 through the intermediary of the spinodal temperature function T(x1,x2). A closed form solution is given for the Berthelot case (geometrical-mean combining rule). All the models exhibit a characteristic intersection of two critical lines, and the behavior near this point is investigated. In the van der Waals case we confirm the coordinates given by van Laar.

  13. Thermal dispersion in vertical gas-liquid flows with foaming and non-foaming liquids

    SciTech Connect

    Pino, L.R.Z.; Saez, A.E.

    1995-05-01

    Heat transfer experiments have been performed in gas-liquid upwards flow in a vertical column with non-foaming (water) and foaming (kerosene) liquids. The main purpose of the experiments has been to characterized the degree of thermal mixing in the system. For the range of conditions employed, the nonfoaming liquid exhibits complete mixing a low liquid superficial velocities. An increased in liquid velocity leads to incomplete mixing. In the latter case, the thermal dispersion coefficient at low gas superficial velocities is larger than what correlations in the literature predict. For the foaming liquid, when foaming and bubbling regions coexist in the bubble column, each region behaves as a completely-mixed subsystem.

  14. An effective device for gas-liquid oxygen removal in enclosed microalgae culture.

    PubMed

    Su, Zhenfeng; Kang, Ruijuan; Shi, Shaoyuan; Cong, Wei; Cai, Zhaoling

    2010-01-01

    A high-performance gas-liquid transmission device (HPTD) was described in this paper. To investigate the HPTD mass transfer characteristics, the overall volumetric mass transfer coefficients, K(A)(La,CO(2)) for the absorption of gaseous CO(2) and K(A)(La,O(2)) for the desorption of dissolved O(2) were determined, respectively, by titration and dissolved oxygen electrode. The mass transfer capability of carbon dioxide was compared with that of dissolved oxygen in the device, and the operating conditions were optimized to suit for the large-scale enclosed micro-algae cultivation. Based on the effectiveness evaluation of the HPTD applied in one enclosed flat plate Spirulina culture system, it was confirmed that the HPTD can satisfy the demand of the enclosed system for carbon supplement and excessive oxygen removal.

  15. Studies of momentum and energy transfer across wavy gas-liquid interfaces. Final report

    SciTech Connect

    Dukler, A.E.

    1993-06-01

    Two phase gas-liquid flow and its associated interfaces exist in a wide variety of situations of importance to the Navy and this has prompted the study of the basic flow mechanics which underlie this complex process. The existence of wind-wave interactions over large bodies of water have long been recognized as a special case of two phase flow where the presence of the deformable interface plays a complex role in the generation of waves due to the action of the wind. Less well recognized, but of great importance, are situations of two phase flow which are found in components of power systems such as condensers, boilers refrigeration loops and cryogen lines. Here the characteristics of two phase flow are critical to the reliable design and safe operation of such systems.

  16. Correlation of the "EMIT" antiepileptic drug assay with a gas liquid chromatographic method.

    PubMed

    Legaz, M; Raisys, V A

    1976-02-01

    Many methodologies have been developed for determining anticonvulsant drug levels in human serum. Unfortunately, most procedures are either time consuming or subject to a variety of interferring substances. The "Enzyme Multiplied Immunoassay Technique" (EMIT) system has been evaluated for its speed, sensitivity, accuracy, and precision. When compared with a gas-liquid chromatographic procedure, the EMIT assay appeared to yield results which were statistically comparable for the drugs diphenylhydantoin, phenobarbital, and primidone. The EMIT assay also demonstrated no significant interference when challenged with extraordinarily high levels of potentially cross reacting drugs. Results obtained with the EMIT assay correlated well with GLC data and rank it as an attractive alternative to many of the existing procedures now being used.

  17. Unit operations for gas-liquid mass transfer in reduced gravity environments

    NASA Technical Reports Server (NTRS)

    Pettit, Donald R.; Allen, David T.

    1992-01-01

    Basic scaling rules are derived for converting Earth-based designs of mass transfer equipment into designs for a reduced gravity environment. Three types of gas-liquid mass transfer operations are considered: bubble columns, spray towers, and packed columns. Application of the scaling rules reveals that the height of a bubble column in lunar- and Mars-based operations would be lower than terrestrial designs by factors of 0.64 and 0.79 respectively. The reduced gravity columns would have greater cross-sectional areas, however, by factors of 2.4 and 1.6 for lunar and Martian settings. Similar results were obtained for spray towers. In contract, packed column height was found to be nearly independent of gravity.

  18. Effect of impeller geometry on gas-liquid mass transfer coefficients in filamentous suspensions.

    PubMed

    Dronawat, S N; Svihla, C K; Hanley, T R

    1997-01-01

    Volumetric gas-liquid mass transfer coefficients were measured in suspensions of cellulose fibers with concentrations ranging from 0 to 20 g/L. The mass transfer coefficients were measured using the dynamic method. Results are presented for three different combinations of impellers at a variety of gassing rates and agitation speeds. Rheological properties of the cellulose fibers were also measured using the impeller viscometer method. Tests were conducted in a 20 L stirred-tank fermentor and in 65 L tank with a height to diameter ratio of 3:1. Power consumption was measured in both vessels. At low agitation rates, two Rushton turbines gave 20% better performance than the Rushton and hydrofoil combination and 40% better performance than the Rushton and propeller combination for oxygen transfer. At higher agitation rates, the Rushton and hydrofoil combination gave 14 and 25% better performance for oxygen transfer than two Rushton turbines and the Rushton and hydrofoil combination, respectively.

  19. Computer code for gas-liquid two-phase vortex motions: GLVM

    NASA Technical Reports Server (NTRS)

    Yeh, T. T.

    1986-01-01

    A computer program aimed at the phase separation between gas and liquid at zero gravity, induced by vortex motion, is developed. It utilizes an explicit solution method for a set of equations describing rotating gas-liquid flows. The vortex motion is established by a tangential fluid injection. A Lax-Wendroff two-step (McCormack's) numerical scheme is used. The program can be used to study the fluid dynamical behavior of the rotational two-phase fluids in a cylindrical tank. It provides a quick/easy sensitivity test on various parameters and thus provides the guidance for the design and use of actual physical systems for handling two-phase fluids.

  20. Dispersed bubble reactor for enhanced gas-liquid-solids contact and mass transfer

    DOEpatents

    Vimalchand, Pannalal; Liu, Guohai; Peng, WanWang; Bonsu, Alexander

    2016-01-26

    An apparatus to promote gas-liquid contact and facilitate enhanced mass transfer. The dispersed bubble reactor (DBR) operates in the dispersed bubble flow regime to selectively absorb gas phase constituents into the liquid phase. The dispersion is achieved by shearing the large inlet gas bubbles into fine bubbles with circulating liquid and additional pumped liquid solvent when necessary. The DBR is capable of handling precipitates that may form during absorption or fine catalysts that may be necessary to promote liquid phase reactions. The DBR can be configured with multistage counter current flow sections by inserting concentric cylindrical sections into the riser to facilitate annular flow. While the DBR can absorb CO.sub.2 in liquid solvents that may lead to precipitates at high loadings, it is equally capable of handling many different types of chemical processes involving solids (precipitates/catalysts) along with gas and liquid phases.

  1. Finite-time thermodynamics and the gas-liquid phase transition

    NASA Astrophysics Data System (ADS)

    Santoro, M.; Schön, J. C.; Jansen, M.

    2007-12-01

    In this paper, we study the application of the concept of finite-time thermodynamics to first-order phase transitions. As an example, we investigate the transition from the gaseous to the liquid state by modeling the liquification of the gas in a finite time. In particular, we introduce, state, and solve an optimal control problem in which we aim at achieving the gas-liquid first-order phase transition through supersaturation within a fixed time in an optimal fashion, in the sense that the work required to supersaturate the gas, called excess work, is minimized by controlling the appropriate thermodynamic parameters. The resulting set of coupled nonlinear differential equations is then solved for three systems, nitrogen N2 , oxygen O2 , and water vapor H2O .

  2. Computer modelling of the surface tension of the gas-liquid and liquid-liquid interface.

    PubMed

    Ghoufi, Aziz; Malfreyt, Patrice; Tildesley, Dominic J

    2016-03-07

    This review presents the state of the art in molecular simulations of interfacial systems and of the calculation of the surface tension from the underlying intermolecular potential. We provide a short account of different methodological factors (size-effects, truncation procedures, long-range corrections and potential models) that can affect the results of the simulations. Accurate calculations are presented for the calculation of the surface tension as a function of the temperature, pressure and composition by considering the planar gas-liquid interface of a range of molecular fluids. In particular, we consider the challenging problems of reproducing the interfacial tension of salt solutions as a function of the salt molality; the simulations of spherical interfaces including the calculation of the sign and size of the Tolman length for a spherical droplet; the use of coarse-grained models in the calculation of the interfacial tension of liquid-liquid surfaces and the mesoscopic simulations of oil-water-surfactant interfacial systems.

  3. Convergence rates to stationary solutions of a gas-liquid model with external forces

    NASA Astrophysics Data System (ADS)

    Fan, Long; Liu, Qingqing; Zhu, Changjiang

    2012-10-01

    In this paper, we study the asymptotic behaviour of solutions to a gas-liquid model with external forces. Under some suitable assumptions on the initial data, if γ > 1 and \\theta\\in(0,\\frac{\\gamma}{2}]\\cap(0,\\gamma-1]\\cap(0,1-\\alpha\\gamma] , we prove the weak solution (cQ (x, t), u(x, t)) behaviour asymptotically to the stationary one by adapting and modifying the technique of weighted estimates. In addition, if \\theta\\in(0,\\frac{\\gamma}{2}]\\cap(0,\\gamma-1)\\cap(0,1-\\alpha\\gamma] , following the same idea used in Zhang and Fang (2006 Arch. Ration. Mech. Anal. 182 223-53), we estimate the stabilization rate of the solution as time tends to infinity in the sense of L∞ norm.

  4. DESIGN AND DEVELOPMENT OF GAS-LIQUID CYLINDRICAL CYCLONE COMPACT SEPARATORS FOR THREE-PHASE FLOW

    SciTech Connect

    Dr. Ram S. Mohan; Dr. Ovadia Shoham

    2003-06-25

    The U.S. Department of Energy (DOE) has awarded a five-year (1997-2002) grant (Mohan and Shoham, DE-FG26-97BC15024, 1997) to The University of Tulsa, to develop compact multiphase separation components for 3-phase flow. The research activities of this project have been conducted through cost sharing by the member companies of the Tulsa University Separation Technology Projects (TUSTP) research consortium and the Oklahoma Center for the Advancement of Science and Technology (OCAST). As part of this project, several individual compact separation components have been developed for onshore and offshore applications. These include gas-liquid cylindrical cyclones (GLCC{copyright}), liquid-liquid cylindrical cyclones (LLCC{copyright}), and the gas-liquid-liquid cylindrical cyclones (GLLCC{copyright}). A detailed study has also been completed for the liquid-liquid hydrocyclones (LLHC). Appropriate control strategies have been developed for proper operation of the GLCC{copyright} and LLCC{copyright}. Testing of GLCC{copyright} at high pressure and real crude conditions for field applications is also completed. Limited studies have been conducted on flow conditioning devices to be used upstream of the compact separators for performance improvement. This report presents a brief overview of the activities and tasks accomplished during the 5-year project period, October 1, 1997-March 31, 2003 (including the no-cost extended period of 6 months). An executive summary is presented initially followed by the tasks of the 5-year budget periods. Then, detailed description of the experimental and modeling investigations are presented. Subsequently, the technical and scientific results of the activities of this project period are presented with some discussions. The findings of this investigation are summarized in the ''Conclusions'' section, followed by relevant references. The publications resulting from this study in the form of MS Theses, Ph.D. Dissertation, Journal Papers and

  5. The inactivation of Chlorella spp. with dielectric barrier discharge in gas-liquid mixture

    NASA Astrophysics Data System (ADS)

    Song, Dan; Sun, Bing; Zhu, Xiaomei; Yan, Zhiyu; Liu, Hui; Liu, Yongjun

    2013-03-01

    The inactivation of Chlorella spp. with high voltage and frequency pulsed dielectric barrier discharge in hybrid gas-liquid reactor with a suspension electrode was studied experimentally. In the hybrid gas-liquid reactor, a steel plate was used as high voltage electrode while a quartz plate as a dielectric layer, another steel plate placing in the aqueous solution worked as a whole ground electrode. A suspension electrode is installed near the surface of solution between high voltage and ground electrode to make the dielectric barrier discharge uniform and stable, the discharge gap was between the quartz plate and the surface of the water. The effect of peak voltage, treatment time, the initial concentration of Chlorella spp. and conductivity of solution on the inactivation rate of Chlorella spp. was investigated, and the inactivation mechanism of Chlorella spp. preliminarily was studied. Utilizing this system inactivation of Chlorella spp., the inactivation rate increased with increasing of peak voltage, treatment time and electric conductivity. It was found that the inactivation rate of Chlorella spp. arrived at 100% when the initial concentration was 4 × 106 cells mL-1, and the optimum operation condition required a peak voltage of 20 kV, a treatment time of 10 min and a frequency of 7 kHz. Though the increasing of initial concentration of the Chlorella spp. contributed to the addition of interaction probability between the Chlorella spp. and O3, H2O2, high-energy electrons, UV radiation and other active substances, the total inactivation number raise, but the inactivation rate of the Chlorella spp. decreased.

  6. Chromatography and its hyphenation to mass spectrometry for extracellular vesicle analysis.

    PubMed

    Pocsfalvi, Gabriella; Stanly, Christopher; Fiume, Immacolata; Vékey, Károly

    2016-03-25

    Extracellular vesicles (EVs), such as exosomes, microvesicles and apoptotic bodies are released by cells, both under physiological and pathological conditions. EVs can participate in a novel type of intercellular communication and deliver cargo of nucleic acids, proteins and lipids near or to distant host cells. EV research is proceeding at a fast pace; now they start to appear as promising therapeutic targets, diagnostic tools and drug delivery systems. Isolation and analysis of EVs are prerequisites for understanding their biological roles and for their clinical exploitation. In this process chromatography and mass spectrometry (MS)-based strategies are rapidly gaining importance; and are reviewed in the present communication. Isolation and purification of EVs is mostly performed by ultracentrifugation at present. Chromatography-based strategies are gaining ground, among which affinity and size exclusion chromatography (SEC) are particularly strong contenders. Their major advantages are the relative simplicity, robustness and throughput. Affinity chromatography has the added advantage of separating EV subtypes based on molecular recognition of EV surface motifs. SEC has the advantage that isolated EVs may retain their biological activity. EVs are typically isolated in small amounts, therefore high sensitivity is required for their analysis. Study of the molecular content of EVs (all compounds beside nucleic acids) is predominantly based on liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis. The chromatographic separation is mostly performed by reverse phase, nanoscale, ultra high performance LC technique. The MS analysis relying typically on nano-electrospray ionization MS/MS provides high sensitivity, selectivity and resolution, so that thousand(s) of proteins can be detected/identified/quantified in a EV sample. Beside protein identification, quantitation and characterization of protein post-translational modifications (PTMs), like glycosylation

  7. Rapid analysis of polyolefin antioxidants and light stabilisers by supercritical fluid chromatography.

    PubMed

    Kithinji, J P; Bartle, K D; Raynor, M W; Clifford, A A

    1990-02-01

    Nineteen commercial antioxidants and light stabilisers, with a wide range of relative molecular masses and boiling-points, present in polyolefins were analysed by packed column supercritical fluid chromatography on four different phases with CO2 or 10% MeOH-CO2 as the mobile phase and with UV detection. The technique is shown to yield short analysis times and sufficient resolution for a number of additives present in a given polyolefin.

  8. RECENT ADVANCES IN ULTRA-HIGH PERFORMANCE LIQUID CHROMATOGRAPHY FOR THE ANALYSIS OF TRADITIONAL CHINESE MEDICINE

    PubMed Central

    Huang, Huilian; Liu, Min; Chen, Pei

    2014-01-01

    Traditional Chinese medicine has been widely used for the prevention and treatment of various diseases for thousands of years in China. Ultra-high performance liquid chromatography (UHPLC) is a relatively new technique offering new possibilities. This paper reviews recent developments in UHPLC in the separation and identification, fingerprinting, quantification, and metabolism of traditional Chinese medicine. Recently, the combination of UHPLC with MS has improved the efficiency of the analysis of these materials. PMID:25045170

  9. Determination of Np-237 by radiochemical neutron activation analysis combined with extraction chromatography.

    PubMed

    Kalmykov, St N; Aliev, R A; Sapozhnikov, D Yu; Sapozhnikov, Yu A; Afinogenov, A M

    2004-01-01

    A procedure for determination of 237Np, 238Pu, 239,240Pu and 241Pu in environmental samples is described. Neptunium-237 is determined using radiochemical neutron activation analysis with pre- and post-irradiation chemistry based on solvent extraction and extraction chromatography. 238Pu, 239,240Pu is determined using alpha spectrometry and 241Pu by liquid scintillation spectrometry. The vertical profiles of 237Np, 238Pu, 239,240Pu in bottom sediments from the Black Sea are presented.

  10. Venus lower atmospheric composition - Analysis by gas chromatography

    NASA Technical Reports Server (NTRS)

    Oyama, V. I.; Carle, G. C.; Woeller, F.; Pollack, J. B.

    1979-01-01

    The first gas chromatographic analysis of the lower atmosphere of Venus is reported. Three atmospheric samples were analyzed. The third of these samples showed carbon dioxide (96.4 percent), molecular nitrogen (3.41 percent), water vapor (0.135 percent), molecular oxygen (69.3 ppm), argon (18.6 ppm), neon (4.31 ppm), and sulfur dioxide (186 ppm). The amounts of water vapor and sulfur dioxide detected are roughly compatible with the requirements of greenhouse models of the high surface temperature of Venus. The large positive gradient of sulfur dioxide, molecular oxygen, and water vapor from the cloud tops to their bottoms, as implied by Earth-based observations and these results, gives added support for the presence of major quantities of aqueous sulfuric acid in the clouds. A comparison of the inventory of inert gases found in the atmospheres of Venus, Earth, and Mars suggests that these components are due to outgassing from the planetary interiors.

  11. [Analysis of psychotropic drug mixtures using high-pressure liquid chromatography in acute poisoning cases].

    PubMed

    Kazlauskiene, Daiva; Vainauskas, Paulius; Kazlauskas, Saulius

    2002-01-01

    The qualitative and quantitative method of determination of amitryptilin, codeine and fluoxetine in the mixture using high-pressure liquid chromatography is described in this paper. Chromatogram is presented which shows, that preparations are fully separated and do not interfere each others analysis. Tables with chromatographical separation characteristics are also presented. Proposed calibration curves of quantitative analysis and calculated medium relative error of quantitative ascertainment for every preparation of the mixture are shown. Final conclusion: method is applicable for qualitative and quantitative analysis of amitryptiline, fluoxetine and codeine in the mixture in hasty poisoning cases.

  12. Analysis of volatile organic compounds in groundwater samples by gas chromatography-mass spectrometry

    SciTech Connect

    Bernhardt, J.

    1995-08-23

    The Savannah River Site contains approximately 1500 monitoring wells from which groundwater samples are collected. Many of these samples are sent off-site for various analyses, including the determination of trace volatile organic compounds (VOCs). This report describes accomplishments that have been made during the past year which will ultimately allow VOC analysis to be performed on-site using gas chromatography-mass spectrometry. Through the use of the on-site approach, it is expected that there will be a substantial cost savings. This approach will also provide split-sample analysis capability which can serve as a quality control measure for off-site analysis.

  13. Quantitative analysis of multiple components based on liquid chromatography with mass spectrometry in full scan mode.

    PubMed

    Xu, Min Li; Li, Bao Qiong; Wang, Xue; Chen, Jing; Zhai, Hong Lin

    2016-08-01

    Although liquid chromatography with mass spectrometry in full scan mode can obtain all the signals simultaneously in a large range and low cost, it is rarely used in quantitative analysis due to several problems such as chromatographic drifts and peak overlap. In this paper, we propose a Tchebichef moment method for the simultaneous quantitative analysis of three active compounds in Qingrejiedu oral liquid based on three-dimensional spectra in full scan mode of liquid chromatography with mass spectrometry. After the Tchebichef moments were calculated directly from the spectra, the quantitative linear models for three active compounds were established by stepwise regression. All the correlation coefficients were more than 0.9978. The limits of detection and limits of quantitation were less than 0.11 and 0.49 μg/mL, respectively. The intra- and interday precisions were less than 6.54 and 9.47%, while the recovery ranged from 102.56 to 112.15%. Owing to the advantages of multi-resolution and inherent invariance properties, Tchebichef moments could provide favorable results even in the situation of peaks shifting and overlapping, unknown interferences and noise signals, so it could be applied to the analysis of three-dimensional spectra in full scan mode of liquid chromatography with mass spectrometry.

  14. Thin layer chromatography coupled to paper spray ionization mass spectrometry for cocaine and its adulterants analysis.

    PubMed

    De Carvalho, Thays C; Tosato, Flavia; Souza, Lindamara M; Santos, Heloa; Merlo, Bianca B; Ortiz, Rafael S; Rodrigues, Rayza R T; Filgueiras, Paulo R; França, Hildegardo S; Augusti, Rodinei; Romão, Wanderson; Vaz, Boniek G

    2016-05-01

    Thin layer chromatography (TLC) is a simple and inexpensive type of chromatography that is extensively used in forensic laboratories for drugs of abuse analysis. In this work, TLC is optimized to analyze cocaine and its adulterants (caffeine, benzocaine, lidocaine and phenacetin) in which the sensitivity (visual determination of LOD from 0.5 to 14mgmL(-1)) and the selectivity (from the study of three different eluents: CHCl3:CH3OH:HCOOHglacial (75:20:5v%), (C2H5)2O:CHCl3 (50:50v%) and CH3OH:NH4OH (100:1.5v%)) were evaluated. Aiming to improve these figures of merit, the TLC spots were identified and quantified (linearity with R(2)>0.98) by the paper spray ionization mass spectrometry (PS-MS), reaching now lower LOD values (>1.0μgmL(-1)). The method developed in this work open up perspective of enhancing the reliability of traditional and routine TLC analysis employed in the criminal expertise units. Higher sensitivity, selectivity and rapidity can be provided in forensic reports, besides the possibility of quantitative analysis. Due to the great simplicity, the PS(+)-MS technique can also be coupled directly to other separation techniques such as the paper chromatography and can still be used in analyses of LSD blotter, documents and synthetic drugs.

  15. Effects of temperature on the location of the gas-liquid interface in a PEM fuel cell

    NASA Astrophysics Data System (ADS)

    Lee, Chun-I.; Chu, Hsin-Sen

    The objective of this study is to investigate the location of the gas-liquid interface at various temperatures in a polymer electrolyte membrane fuel cell under non-isothermal conditions. A mathematical model, coupled with the electrochemical process, two-phase flows, species transfer, and heat transfer is employed. A finite volume-based CFD approach is applied to investigate the species transport behavior in a fuel cell. The effects of two model parameters, namely cell temperature (T cell) and humidification temperature (T h), on the gas-liquid interface and cell performance are presented. Simulation results indicate that variations of these two parameters influence the location of the gas-liquid interface, the cell performance, and the distribution of liquid water saturation. At lower cell temperatures, the gas-liquid interface moves toward the inlet port of the channel when the humidification temperature is greater than the cell temperature. Therefore, the cell performance decreases as the liquid water clogs the passage for the transport of oxygen. Furthermore, these two factors are closely related to the membrane temperature distribution. Obvious variations in magnitude are seen at a cell temperature of 323 K and a humidification temperature of 343 K.

  16. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 21 2011-07-01 2011-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

  17. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 22 2012-07-01 2012-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

  18. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 22 2013-07-01 2013-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

  19. 40 CFR Table Mm-1 to Subpart Mm of... - Default Factors for Petroleum Products and Natural Gas Liquids 1 2

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 21 2014-07-01 2014-07-01 false Default Factors for Petroleum Products... Suppliers of Petroleum Products Pt. 98, Subpt. MM, Table MM-1 Table MM-1 to Subpart MM of Part 98—Default Factors for Petroleum Products and Natural Gas Liquids 1 2 Products Column A: density(metric...

  20. Working process study of a novel scroll type multiphase pump for the transportation of gas-liquid mixtures

    NASA Astrophysics Data System (ADS)

    Wang, J.; Zha, H. B.; Zhang, X. H.; Zhang, D. H.

    2012-11-01

    A novel scroll type multiphase pump was proposed to transport gas-liquid two-phase mixture. There is a pressure unloading gap from compression chambers to the discharge port by constructing scroll wrap profile with variational meshing clearance in this scroll multiphase pump. In the working process when the volume of working chamber decreases, the pressure of gas-liquid mixtures increases gradually, at the same time small amounts of gas-liquid mixture are pushed to the discharge port from compression chambers through the pressure unloading gap. Therefore, this multiphase pump has an advantage of unloading pressure method automatically, and the frequently problem of liquid impacting in volume multiphase pump is solved. The safety and reliability of volumetric multiphase pump are improved, and the scope of multiphase pump of the gas-liquid ratio is expanded. The working process and the performance characteristics of scroll multiphase pump were analyzed too, and the generation method of scroll wrap profile with variational meshing clearance was investigated. The equations of the profile were obtained, and the changing principle of the working volume and the meshing clearance were analyzed. The geometric theory of scroll multiphase pump was formed. All of that lay the theoretical foundation for engineering design of this novel scroll.

  1. GAS-LIQUID CHROMATOGRAPHY OF TERPENES. PART XI. THE VOLATILE OIL OF THE LEAVES OF JUNIPERUS SCOPULORUM SARG

    DTIC Science & Technology

    and smaller amounts of d-limonene (11.4%), d-alpha- pinene (4.2%), gama-terpinene (1.15%), p-cymene (1.4%), l-linalool (1.2%), d-terpinen4-ol (2.9...citronellol (0.2%), l- beta -elemene (0.2-0.3%), three isomeric cadinenes (2.7%), l-elemol (6. 0%), and Safrole (1.85%) were isolated. An unidentified

  2. EXTRACTION AND QUANTITATIVE ANALYSIS OF ELEMENTAL SULFUR FROM SULFIDE MINERAL SURFACES BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY. (R826189)

    EPA Science Inventory

    A simple method for the quantitative determination of elemental sulfur on oxidized sulfide minerals is described. Extraction of elemental sulfur in perchloroethylene and subsequent analysis with high-performance liquid chromatography were used to ascertain the total elemental ...

  3. Multiresidue analysis of pesticides in traditional Chinese medicines using gas chromatography - negative chemical ionization tandem mass spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In this study, a residue analysis method for the simultaneous determination of 107 pesticides in the traditional Chinese medicines (TCMs), Angelica sinensis, Angelica dahurica, Leonurus heterophyllus Sweet, Pogostemon cablin, and Lonicera japonica Thunb, was developed using gas chromatography couple...

  4. Ion Chromatography.

    ERIC Educational Resources Information Center

    Mulik, James D.; Sawicki, Eugene

    1979-01-01

    Accurate for the analysis of ions in solution, this form of analysis enables the analyst to directly assay many compounds that previously were difficult or impossible to analyze. The method is a combination of the methodologies of ion exchange, liquid chromatography, and conductimetric determination with eluant suppression. (Author/RE)

  5. Characterization of the efficiency of microbore liquid chromatography columns by van Deemter and kinetic plot analysis.

    PubMed

    Hetzel, Terence; Loeker, Denise; Teutenberg, Thorsten; Schmidt, Torsten C

    2016-10-01

    The efficiency of miniaturized liquid chromatography columns with inner diameters between 200 and 300 μm has been investigated using a dedicated micro-liquid chromatography system. Fully porous, core-shell and monolithic commercially available stationary phases were compared applying van Deemter and kinetic plot analysis. The sub-2 μm fully porous as well as the 2.7 μm core-shell particle packed columns showed superior efficiency and similar values for the minimum reduced plate heights (2.56-2.69) before correction for extra-column contribution compared to normal-bore columns. Moreover, the influence of extra-column contribution was investigated to demonstrate the difference between apparent and intrinsic efficiency by replacing the column by a zero dead volume union to determine the band spreading caused by the system. It was demonstrated that 72% of the intrinsic efficiency could be reached. The results of the kinetic plot analysis indicate the superior performance of the sub-2 μm fully porous particle packed column for ultra-fast liquid chromatography.

  6. Analysis of antimycin A by reversed-phase liquid chromatography/nuclear magnetic-resonance spectrometry

    USGS Publications Warehouse

    Ha, Steven T.K.; Wilkins, Charles L.; Abidi, Sharon L.

    1989-01-01

    A mixture of closely related streptomyces fermentation products, antimycin A, Is separated, and the components are identified by using reversed-phase high-performance liquid chromatography with directly linked 400-MHz proton nuclear magnetic resonance detection. Analyses of mixtures of three amino acids, alanine, glycine, and valine, are used to determine optimal measurement conditions. Sensitivity increases of as much as a factor of 3 are achieved, at the expense of some loss in chromatographic resolution, by use of an 80-μL NMR cell, Instead of a smaller 14-μL cell. Analysis of the antimycin A mixture, using the optimal analytical high performance liquid chromatography/nuclear magnetic resonance conditions, reveals it to consist of at least 10 closely related components.

  7. Glycosaminoglycans: oligosaccharide analysis by liquid chromatography, capillary electrophoresis, and specific labeling.

    PubMed

    Langeslay, Derek J; Jones, Christopher J; Beni, Szabolcs; Larive, Cynthia K

    2012-01-01

    Glycosaminoglycans (GAGs) are a class of biopolymers that include chondrotin sulfate, dermatan sulfate, keratan sulfate, hyaluronic acid, heparin, and heparan sulfate. The GAGs are linear polysaccharides that are microheterogeneous in composition and polydisperse in size. Because they have the most complex structures, this article is aimed at describing a step-by-step procedure for processing and analyzing heparin and heparan sulfate-derived oligosaccharides, although the basic protocols and procedures apply equally well to other members of the GAG family. The methods described in this manuscript include the preparation of oligosaccharides through enzymatic depolymerization, size fractionation by preparative scale size-exclusion chromatography (SEC), and disaccharide isomer analysis by reverse-phase ion-pair high-performance liquid chromatography (RPIP-HPLC) and capillary electrophoresis (CE).

  8. High pH reversed-phase chromatography with fraction concatenation for 2D proteomic analysis

    SciTech Connect

    Yang, Feng; Shen, Yufeng; Camp, David G.; Smith, Richard D.

    2012-04-01

    Orthogonal high-resolution separations are critical for attaining improved analytical dynamic ranges of proteome measurements. Concatenated high pH reversed phase liquid chromatography affords better separations than the strong cation exchange conventionally applied for two-dimensional shotgun proteomic analysis. For example, concatenated high pH reversed phase liquid chromatography increased identification coverage for peptides (e.g., by 1.8-fold) and proteins (e.g., by 1.6-fold) in shotgun proteomics analyses of a digested human protein sample. Additional advantages of concatenated high pH RPLC include improved protein sequence coverage, simplified sample processing, and reduced sample losses, making this an attractive first dimension separation strategy for two-dimensional proteomics analyses.

  9. Structural analysis of commercial ceramides by gas chromatography-mass spectrometry.

    PubMed

    Bleton, J; Gaudin, K; Chaminade, P; Goursaud, S; Baillet, A; Tchapla, A

    2001-05-11

    A simple method using gas chromatography-mass spectrometry was applied to analyse structures of ceramides. Identification of trimethylsilylated ceramides were obtained in short analysis times (derivatization of ceramides in 30 min at room temperature and 20 min gas chromatography mass spectrometry run) even for complex mixtures. For example in ceramide Type III, 18 peaks were observed which represent 27 various structures. The coeluted compounds were ceramides containing the same functional groups and the same carbon number but with a different distribution on the two alkyl chains of the molecule. They were accurately differentiated by mass spectrometry. Therefore, 83 structures of trimethylsilylated ceramides were identified in 11 different commercial mixtures. For 52 structures of these, mass spectral data were not described in the literature, neither full mass spectra nor characteristic fragments.

  10. A Size-Exclusion Chromatography Method for Analysis of Clostridium difficile Vaccine Toxins.

    PubMed

    Lancaster, Catherine; Rustandi, Richard R; Pannizzo, Paola; Ha, Sha

    2016-01-01

    High-performance size-exclusion chromatography (HPSEC or SEC) is a method that can be applied to measure size distribution of proteins, including aggregates, monomers, and fragments. In the biopharmaceutical industry the quantitation of aggregates contained in biotherapeutics and protein-based vaccines is critical given the potential impact on safety, immunogenicity, and efficacy. Hence, aggregation analysis of therapeutic proteins or protein-based vaccine products is almost always a requirement of regulatory agencies. SEC, also referred to as gel-filtration chromatography, separates molecules by size through a porous resin stationary phase. Under isocratic flow small molecules are retained on the column longer than large molecules. Here we describe the use of this SEC technique to characterize aggregation levels for four different protein antigens for a Clostridium difficile vaccine.

  11. Analysis of antioxidants from orange juice obtained by countercurrent supercritical fluid extraction, using micellar electrokinetic chromatography and reverse-phase liquid chromatography.

    PubMed

    Simó, Carolina; Ibañez, Elena; Señoráns, Francisco J; Barbas, Coral; Reglero, Guillermo; Cifuentes, Alejandro

    2002-11-06

    Antioxidants from orange juice were determined by the combined use of countercurrent supercritical fluid extraction (CC-SFE) prior to reverse-phase liquic chromatography (RP-LC) or micellar electrokinetic chromatography (MEKC). The separation of antioxidants found in the SFE fractions was achieved by using a new MEKC method and a published LC procedure, both using diode array detection. The characterization of the different antioxidants was further done by LC-mass spectrometry. Advantages and drawbacks of LC and MEKC for analyzing the antioxidants found in the different orange extracts are discussed. Although LC yields higher peak area and slightly better reproducibility than MEKC, the latter technique provides information about the CC-SFE extracts in analysis times 7 times faster than by LC. This analysis advantage can be used for the quick adjustment of CC-SFE conditions, thus providing a fast way to obtain orange fractions of specific composition.

  12. Development of gas chromatography analysis of fatty acids in marine organisms.

    PubMed

    Tang, Baokun; Row, Kyung Ho

    2013-08-01

    The gas chromatographic analysis of fatty acids has attracted considerable interest. In this analysis, the common derivatives of fatty acids, such as fatty acid methyl esters, can be detected using a flame ionization detector and the mass spectra can indicate the true structure of fatty acids. This paper reviews gas chromatographic methods for obtaining fatty acids from marine organisms. The stationary phase and detector for applications in gas chromatography are discussed. This article also reviews the components of fatty acids in marine animals, marine plants and marine microorganisms.

  13. [Research on diagnosis of gas-liquid detonation exhaust based on double optical path absortion spectroscopy technique].

    PubMed

    Lü, Xiao-Jing; Li, Ning; Weng, Chun-Sheng

    2014-03-01

    The effect detection of detonation exhaust can provide measurement data for exploring the formation mechanism of detonation, the promotion of detonation efficiency and the reduction of fuel waste. Based on tunable diode laser absorption spectroscopy technique combined with double optical path cross-correlation algorithm, the article raises the diagnosis method to realize the on-line testing of detonation exhaust velocity, temperature and H2O gas concentration. The double optical path testing system is designed and set up for the valveless pulse detonation engine with the diameter of 80 mm. By scanning H2O absorption lines of 1343nm with a high frequency of 50 kHz, the on-line detection of gas-liquid pulse detonation exhaust is realized. The results show that the optical testing system based on tunable diode laser absorption spectroscopy technique can capture the detailed characteristics of pulse detonation exhaust in the transient process of detonation. The duration of single detonation is 85 ms under laboratory conditions, among which supersonic injection time is 5.7 ms and subsonic injection time is 19.3 ms. The valveless pulse detonation engine used can work under frequency of 11 Hz. The velocity of detonation overflowing the detonation tube is 1,172 m x s(-1), the maximum temperature of detonation exhaust near the nozzle is 2 412 K. There is a transitory platform in the velocity curve as well as the temperature curve. H2O gas concentration changes between 0-7% during detonation under experimental conditions. The research can provide measurement data for the detonation process diagnosis and analysis, which is of significance to advance the detonation mechanism research and promote the research of pulse detonation engine control technology.

  14. Measurements of liquid-phase turbulence in gas-liquid two-phase flows using particle image velocimetry

    NASA Astrophysics Data System (ADS)

    Zhou, Xinquan; Doup, Benjamin; Sun, Xiaodong

    2013-12-01

    Liquid-phase turbulence measurements were performed in an air-water two-phase flow loop with a circular test section of 50 mm inner diameter using a particle image velocimetry (PIV) system. An optical phase separation method--planar laser-induced fluorescence (PLIF) technique—which uses fluorescent particles and an optical filtration technique, was employed to separate the signals of the fluorescent seeding particles from those due to bubbles and other noises. An image pre-processing scheme was applied to the raw PIV images to remove the noise residuals that are not removed by the PLIF technique. In addition, four-sensor conductivity probes were adopted to measure the radial distribution of the void fraction. Two benchmark tests were performed: the first was a comparison of the PIV measurement results with those of similar flow conditions using thermal anemometry from previous studies; the second quantitatively compared the superficial liquid velocities calculated from the local liquid velocity and void fraction measurements with the global liquid flow rate measurements. The differences of the superficial liquid velocity obtained from the two measurements were bounded within ±7% for single-phase flows and two-phase bubbly flows with the area-average void fraction up to 18%. Furthermore, a preliminary uncertainty analysis was conducted to investigate the accuracy of the two-phase PIV measurements. The systematic uncertainties due to the circular pipe curvature effects, bubble surface reflection effects and other potential uncertainty sources of the PIV measurements were discussed. The purpose of this work is to facilitate the development of a measurement technique (PIV-PLIF) combined with image pre-processing for the liquid-phase turbulence in gas-liquid two-phase flows of relatively high void fractions. The high-resolution data set can be used to more thoroughly understand two-phase flow behavior, develop liquid-phase turbulence models, and assess high

  15. Drop tower experiment for performance evaluation of gas-liquid equilibrium thruster for small spacecraft

    NASA Astrophysics Data System (ADS)

    Motooka, Norizumi; Yamamoto, Takayuki; Mori, Osamu; Okano, Yoshinobu; Kishino, Yoshihiro; Kawaguchi, Junichiro

    JAXA/ISAS is developing the gas-liquid equilibrium thruster for a small spacecraft. In small spacecrafts, the thruster system must be simple and its weight must be light. This thruster system uses HFC-134a (1,1,1,2-tetrafluoroethane) , a kind of liquefied gas, as propellant because of its harmlessness and ease of handling. And this thruster stores propellant as liquid in the tank and ejects propellant as gas using the gas-liquid equilibrium pressure to produce thrust, so the propellant tank only needs to resist the vapor pressure of propellant. In this thruster system, the porous metal is also equipped in the tank for the following performance advantages: (1) liquid fuel retention: The porous metal reduces sloshing problems which cause bad effects on spacecraft attitude by retaining liquid propellant inside the porous metal: (2) vapor-liquid separation: The porous metal also helps propellant separate gas from liquid by advancing propellant vaporization on its large surface area and retaining liquid propellant using its surface tension. In last autumn, we carried out the experiment to evaluate these two advantages of porous metal under micro gravity condition using 50 meters drop tower in Hokkaido, Japan. The system of this experiment divides into two different systems. The first one evaluates liquid propellant retention performance by adding disturbance to liquid propellant absorbed in porous metal. The disturbance is centrifugal force and angular acceleration worked on the liquid propellant by rotating propellant tank controlled by motor. A high speed camera records the behavior of the liquid propellant. The other one evaluates the ability of gas-liquid separation on the case of propellant ejection. In this evaluation, the parameters are full filling porous metal or some ullage in the tank, nozzle diameters and the filling ratio of liquid propellant in the tank. As for (1) liquid fuel retention, in all conducted cases without propellant ejection, liquid propellant

  16. Flow chemistry: intelligent processing of gas-liquid transformations using a tube-in-tube reactor.

    PubMed

    Brzozowski, Martin; O'Brien, Matthew; Ley, Steven V; Polyzos, Anastasios

    2015-02-17

    CONSPECTUS: The previous decade has witnessed the expeditious uptake of flow chemistry techniques in modern synthesis laboratories, and flow-based chemistry is poised to significantly impact our approach to chemical preparation. The advantages of moving from classical batch synthesis to flow mode, in order to address the limitations of traditional approaches, particularly within the context of organic synthesis are now well established. Flow chemistry methodology has led to measurable improvements in safety and reduced energy consumption and has enabled the expansion of available reaction conditions. Contributions from our own laboratories have focused on the establishment of flow chemistry methods to address challenges associated with the assembly of complex targets through the development of multistep methods employing supported reagents and in-line monitoring of reaction intermediates to ensure the delivery of high quality target compounds. Recently, flow chemistry approaches have addressed the challenges associated with reactions utilizing reactive gases in classical batch synthesis. The small volumes of microreactors ameliorate the hazards of high-pressure gas reactions and enable improved mixing with the liquid phase. Established strategies for gas-liquid reactions in flow have relied on plug-flow (or segmented flow) regimes in which the gas plugs are introduced to a liquid stream and dissolution of gas relies on interfacial contact of the gas bubble with the liquid phase. This approach confers limited control over gas concentration within the liquid phase and is unsuitable for multistep methods requiring heterogeneous catalysis or solid supported reagents. We have identified the use of a gas-permeable fluoropolymer, Teflon AF-2400, as a simple method of achieving efficient gas-liquid contact to afford homogeneous solutions of reactive gases in flow. The membrane permits the transport of a wide range of gases with significant control of the stoichiometry of

  17. Evaluation of vermicompost maturity using scanning electron microscopy and paper chromatography analysis.

    PubMed

    Senthil Kumar, D; Satheesh Kumar, P; Rajendran, N M; Uthaya Kumar, V; Anbuganapathi, G

    2014-04-02

    Vermicompost was produced from flower waste inoculated with biofertilizers using the earthworm Eisenia fetida. Principal component analysis (PCA) and cluster analysis (CA) were carried out on the basis of physicochemical parameters of vermicomposted samples. From the results of the PCA and CA, it was possible to classify two different groups of vermicompost samples in the following categories: E2 and E5; and E1, E3, E4, and control. Scanning electron microscopy and biodynamic circular paper chromatography analysis were used to investigate the changes in surface morphology and functional groups in the control and vermicompost products. SEM analysis of E1-E5 shows more fragment and pores than the control. Chromatographic analysis of vermicompost indicated the mature condition of the compost materials.

  18. [Analysis of mouse liver membrane proteins using multidimensional ion exchange chromatography and tandem mass spectrometry].

    PubMed

    Wang, Zhuowei; Peng, Fuli; Wang, Yuan; Tong, Wei; Ren, Yan; Xu, Ningzhi; Liu, Siqi

    2010-02-01

    The analysis of membrane proteins is still a technical obstacle in proteomic investigation. A fundamental question is how to allow the hydrophobic proteins fully solubilizing in a proper solvent environment. We propose that the denatured membrane proteins in high denaturant solution are fully ionized and separated through ion exchange chromatography. The membrane proteins prepared from a mouse liver were dissolved in 4 mol/L urea, 20 mmol/L Tris-HCl buffer (pH 9.0), and loaded onto a tandem chromatography coupled with Q-Sepharose FF and Sephacryl S-200HR. With a linear NaCl gradient elution, the bound proteins were eluted and collected followed by sodium-dodecyl sulphate-polyacrylamide gel electrophoresis (SDS-PAGE) to further separate the eluted proteins. The protein bound on SDS-PAGE were excised and in-gel digested by trypsin, while the digested peptides were delivered to reversed-phase high performance liquid chromatography (HPLC) and ion-trap mass spectrometry for the peptide identifications. Of a total of 392 proteins identified, 306 were membrane proteins or membrane associated proteins reported by literature. Based on the calculation of hydrophobicity, the GRAVY (grand average of hydropathicity) scores of 83 proteins are over or equal to 0.00. Taking all the evidence, we have established an effective approach which is feasible in the investigation towards mouse liver membrane proteomics.

  19. Analysis of trace dicyandiamide in stream water using solid phase extraction and liquid chromatography UV spectrometry.

    PubMed

    Qiu, Huidong; Sun, Dongdi; Gunatilake, Sameera R; She, Jinyan; Mlsna, Todd E

    2015-09-01

    An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction. The extraction procedure (including loading, washing, and eluting) used a flow rate of 1.0mL/min, and dicyandiamide was eluted with 20mL of a methanol/acetonitrile mixture (V/V=2:3), followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography-ultraviolet spectroscopy (HPLC-UV). Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge (with activated carbon). Separation was achieved on a ZIC(®)-Hydrophilic Interaction Liquid Chromatography (ZIC-HILIC) (50mm×2.1mm, 3.5μm) chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions (R(2)>0.999). Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations (RSDs, n=3) were below 6.1% with a detection limit of 5.0ng/mL for stream water samples.

  20. In situ search for organics by gas chromatography analysis: new derivatization / thermochemolysis approach

    NASA Astrophysics Data System (ADS)

    Geffroy, Claude; Buch, Arnaud; David, Marc; Aissat, Lyes; El Mufleh, Amel; Papot, S.; Sternberg, Robert

    Many organic molecules are present in interstellar clouds and might be carried to the early Earth by comets and meteorites during the heavy bombardment phase in the first few hundred million years of the solar system. It has been suggested that extraterrestrial organic material may well represent an important part of the organic material available for the origin of life. Until samples, brought by future space missions, are available on Earth, in situ measurements are one of the way to get unaltered and non-contaminated samples for analysis. The analytical technique has to be robust, sensitive and non-specific due to the large scope of targets molecules. The only currently flight qualified technique of analysis of organic molecules in space is gas chromatography (Viking, Cassini-Huygens, SAM-MSL, COSAC-Rosetta). The main objective of this work is to present a new approach with multi step analysis using derivatisation and thermochemolysis reagents for a one pot in situ analysis of volatile and refractory organics in surface or sub-surface samples (Mars, comets).Indeed, no single technology enables to identify all organic compounds because naturally occurring molecules have different polarities, molecular weights, being extractible or recalcitrant, bonded trapped or adsorbed on minerals. Thus, we propose to wider the scope of chemical reagent already validated for in situ wet chemistry such as MTBSTFA (Rodier et al. 2001, 2002), DMF-DMA (Rodier et al. 2002), or TMAH (Rodier et al, 2005, Geffroy-Rodier et al; 2009) to analyze enantiomers of amino acids, carbohydrates and lipids in a one pot several steps sub system using a multi reagent and multi step approach. Thus using a new derivatizing agent, we successfully identified twenty one amino acids including twelve of the twenty proteinic amino acids without inhibiting following multi step thermochemolysis. *Geffroy-Rodier C, Grasset L, Sternberg R. Buch A. Amblès A. (2009) Thermochemolysis in search for organics in

  1. Comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for analysis of toad skin.

    PubMed

    Li, Jia-Fu; Yan, Xia; Wu, Yun-Long; Fang, Mei-Juan; Wu, Zhen; Qiu, Ying-Kun

    2017-04-15

    An analytical two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was constructed with a newly developed thermal evaporation assisted adsorption (TEAA) interface. This novel TEAA interface with heating temperature above solvent boiling point allowed fast removal of organic NPLC solvent and successfully solved the solvent incompatibility problem between NPLC and RPLC. The system achieved rapid on-line solvent exchange between the two dimensions within a short modulation time of 190 s and was applied in the analysis of an extract from the skin of Bufo bufo gargarizans. This is the first time to realize the on-line comprehensive analysis of a moderate polar natural product by coupling NPLC with reversed phase ultra-high performance liquid chromatography (UHPLC). To be highlighted, with the TEAA interface, the 2D NPLC × RPLC system provided excellent resolution and orthogonality (75.2%), when compared with that of 2D RPLC × RPLC.

  2. Qualitative and quantitative analysis of vetiver essential oils by comprehensive two-dimensional gas chromatography and comprehensive two-dimensional gas chromatography/mass spectrometry.

    PubMed

    Filippi, Jean-Jacques; Belhassen, Emilie; Baldovini, Nicolas; Brevard, Hugues; Meierhenrich, Uwe J

    2013-05-03

    Vetiver essential oils (VEO) are important raw ingredients used in perfume industry, entering the formula of numerous modern fragrances. Vetiver oils are considered to be among the most complex essential oils, resulting most of the time in highly coeluted chromatograms whatever the analytical technique. In this context, conventional gas chromatography has failed to provide a routine tool for the accurate qualitative and quantitative analysis of their constituents. Applying comprehensive two-dimensional gas chromatography techniques (GC×GC-FID/MS) afforded the mean to separate efficiently vetiver oil constituents in order to identify them in a more reliable way. Moreover, this is the first time that a complete true quantitation of each constituent is carried out on such complex oils by means of internal calibration. Finally, we have studied the influence of the injection mode on the determined chemical composition, and showed that several alcohols underwent dehydration under defined chromatographic conditions (splitless mode) usually recommended for quantitation purposes.

  3. Detailed analysis of petroleum hydrocarbon attenuation in biopiles by high-performance liquid chromatography followed by comprehensive two-dimensional gas chromatography.

    PubMed

    Mao, Debin; Lookman, Richard; Van De Weghe, Hendrik; Van Look, Dirk; Vanermen, Guido; De Brucker, Nicole; Diels, Ludo

    2009-02-27

    Enhanced bioremediation of petroleum hydrocarbons in two biopiles was quantified by high-performance liquid chromatography (HPLC) followed by comprehensive two-dimensional gas chromatography (GCXGC). The attenuation of 34 defined hydrocarbon classes was calculated by HPLC-GCXGC analysis of representative biopile samples at start-up and after 18 weeks of biopile operation. In general, a-cyclic alkanes were most efficiently removed from the biopiles, followed by monoaromatic hydrocarbons. Cycloalkanes and polycyclic aromatic hydrocarbons (PAHs) were more resistant to degradation. A-cyclic biomarkers farnesane, trimethyl-C13, norpristane, pristane and phytane dropped to only about 10% of their initial concentrations. On the other hand, C29-C31 hopane concentrations remained almost unaltered after 18 weeks of biopile operation, confirming their resistance to biodegradation. They are thus reliable indicators to estimate attenuation potential of petroleum hydrocarbons in biopile processed soils.

  4. Research and Design of Thermophysical Gas-Liquid Mixture Parameters in Product Pipelines

    NASA Astrophysics Data System (ADS)

    Dudin, S. M.; Zemenkov, Yu D.; Maier, A. V.; Shabarov, A. B.

    2016-10-01

    Operational problems are hard to overcome because of the temperature and pressure conditions of the hydrocarbon flow in the pipe, as well as the composition of the hydrocarbon system and the geometry of the pipeline. It is known that energy costs to pump a unit mass of RH in the form of gas 2-3 times exceed energy costs to pump a unit mass of RH in the form of liquid. As far as energy conservation during RH transportation is concerned, an important task is development and application of a method to calculate the gas-liquid hydrocarbons flow, and heat and mass transfer in process and trunk pipelines during their design and operation. The authors have developed a calculation method which is used to analyze the hydrodynamic state and composition of the hydrocarbon mixture in each ith section of the pipeline when temperature-pressure and hydraulic conditions change. The developed technique was tested on the hydrocarbon mixture of de-ethanized condensate and oil transported from northern oil and gas condensate fields via the main gas condensate line to the refinery.

  5. Gas-Liquid Two-Phase Flows Through Packed Bed Reactors in Microgravity

    NASA Technical Reports Server (NTRS)

    Motil, Brian J.; Balakotaiah, Vemuri

    2001-01-01

    The simultaneous flow of gas and liquid through a fixed bed of particles occurs in many unit operations of interest to the designers of space-based as well as terrestrial equipment. Examples include separation columns, gas-liquid reactors, humidification, drying, extraction, and leaching. These operations are critical to a wide variety of industries such as petroleum, pharmaceutical, mining, biological, and chemical. NASA recognizes that similar operations will need to be performed in space and on planetary bodies such as Mars if we are to achieve our goals of human exploration and the development of space. The goal of this research is to understand how to apply our current understanding of two-phase fluid flow through fixed-bed reactors to zero- or partial-gravity environments. Previous experiments by NASA have shown that reactors designed to work on Earth do not necessarily function in a similar manner in space. Two experiments, the Water Processor Assembly and the Volatile Removal Assembly have encountered difficulties in predicting and controlling the distribution of the phases (a crucial element in the operation of this type of reactor) as well as the overall pressure drop.

  6. Effect of impeller geometry on gas-liquid mass transfer coefficients in filamentous suspensions

    SciTech Connect

    Dronawat, S.N.; Svihla, C.K.; Hanley, T.R.

    1997-12-31

    Volumetric gas-liquid mass transfer coefficients were measured in suspensions of cellulose fibers with concentrations ranging from 0 to 20 g/L. The mass transfer coefficients were measured using the dynamic method. Results are presented for three different combinations of impellers at a variety of gassing rates and agitation speeds. Rheological properties of the cellulose fibers were also measured using the impeller viscometer method. Tests were conducted in a 20 L stirred-tank fermentor and in 65 L tank with a height to diameter ratio of 3:1. Power consumption was measured in both vessels. At low agitation rates, two Rushton turbines gave 20% better performance than the Rushton and hydrofoil combination and 40% better performance than the Rushton and propeller combination for oxygen transfer. At higher agitation rates, the Rushton and hydrofoil combination gave 14 and 25% better performance for oxygen transfer than two Rushton turbines and the Rushton and hydrofoil combination, respectively. 8 refs., 11 figs., 1 tab.

  7. Effects of Gravity on Cocurrent Two-Phase Gas-Liquid Flows Through Packed Columns

    NASA Technical Reports Server (NTRS)

    Motil, Brian J.; Balakotaiah, Vemuri; Kamotani, Yasuhiro

    2001-01-01

    This work presents the experimental results of research on the influence of gravity on flow pattern transitions, pressure drop and flow characteristics for cocurrent gas-liquid two-phase flow through packed columns. The flow pattern transition data indicates that the pulse flow regime exists over a wider range of gas and liquid flow rates under reduced gravity conditions compared to normal gravity cocurrent down-flow. This is illustrated by comparing the flow regime transitions found in reduced gravity with the transitions predicted by Talmor. Next, the effect of gravity on the total pressure drop in a packed column is shown to depend on the flow regime. The difference is roughly equivalent to the liquid static head for bubbly flow but begins to decrease at the onset of pulse flow. As the spray flow regime is approached by increasing the gas to liquid ratio, the effect of gravity on pressure drop becomes negligible. Finally, gravity tends to suppress the amplitude of each pressure pulse. An example of this phenomenon is presented.

  8. Gas-liquid interfacial plasmas producing reactive species for cell membrane permeabilization

    PubMed Central

    Kaneko, Toshiro; Sasaki, Shota; Takashima, Keisuke; Kanzaki, Makoto

    2017-01-01

    Gas-liquid interfacial atmospheric-pressure plasma jets (GLI-APPJ) are used medically for plasma-induced cell-membrane permeabilization. In an attempt to identify the dominant factors induced by GLI-APPJ responsible for enhancing cell-membrane permeability, the concentration and distribution of plasma-produced reactive species in the gas and liquid phase regions are measured. These reactive species are classified in terms of their life-span: long-lived (e.g., H2O2), short-lived (e.g., O2•−), and extremely-short-lived (e.g., •OH). The concentration of plasma-produced •OHaq in the liquid phase region decreases with an increase in solution thickness (<1 mm), and plasma-induced cell-membrane permeabilization is found to decay markedly as the thickness of the solution increases. Furthermore, the horizontally center-localized distribution of •OHaq, resulting from the center-peaked distribution of •OH in the gas phase region, corresponds with the distribution of the permeabilized cells upon APPJ irradiation, whereas the overall plasma-produced oxidizing species such as H2O2aq in solution exhibit a doughnut-shaped horizontal distribution. These results suggest that •OHaq is likely one of the dominant factors responsible for plasma-induced cell-membrane permeabilization. PMID:28163376

  9. Gas-liquid Phase Distribution and Void Fraction Measurements Using the MRI

    NASA Technical Reports Server (NTRS)

    Daidzic, N. E.; Schmidt, E.; Hasan, M. M.; Altobelli, S.

    2004-01-01

    We used a permanent-magnet MRI system to estimate the integral and spatially- and/or temporally-resolved void-fraction distributions and flow patterns in gas-liquid two-phase flows. Air was introduced at the bottom of the stagnant liquid column using an accurate and programmable syringe pump. Air flow rates were varied between 1 and 200 ml/min. The cylindrical non-conducting test tube in which two-phase flow was measured was placed in a 2.67 kGauss MRI with MRT spectrometer/imager. Roughly linear relationship has been obtained for the integral void-fraction, obtained by volume-averaging of the spatially-resolved signals, and the air flow rate in upward direction. The time-averaged spatially-resolved void fraction has also been obtained for the quasi-steady flow of air in a stagnant liquid column. No great accuracy is claimed as this was an exploratory proof-of-concept type of experiment. Preliminary results show that MRI a non-invasive and non-intrusive experimental technique can indeed provide a wealth of different qualitative and quantitative data and is especially well suited for averaged transport processes in adiabatic and diabatic multi-phase and/or multi-component flows.

  10. Rapid nondestructive spectrometric measurement of temperature-dependent gas-liquid solubility equilibria.

    PubMed

    Ma, Jian; Dasgupta, Purnendu K; Yang, Bingcheng

    2011-02-01

    Gas-liquid solubility equilibria (Henry's Law behavior) are of basic interest to many different areas. Temperature-dependent aqueous solubilities of various organic compounds are of fundamental importance in many branches of environmental science. In a number of situations, the gas/dissolved solute of interest has characteristic spectroscopic absorption that is distinct from that of the solvent. For such cases, we report facile nondestructive rapid measurement of the temperature-dependent Henry's law constant (K(H)) in a static sealed spectrometric cell. Combined with a special cell design, multiwavelength measurement permits a large range of K(H) to be spanned. It is possible to derive the K(H) values from the absorbance measured in the gas phase only, the liquid phase only (preferred), and both phases. Underlying principles are developed, and all three approaches are illustrated for a solute like acetone in water. A thermostatic spectrophotometer cell compartment, widely used and available, facilitates rapid temperature changes and allows rapid temperature-dependent equilibrium measurements. Applicability is shown for both acetone and methyl isobutyl ketone. Very little sample is required for the measurement; the K(H) for 4-hydroxynonenal, a marker for oxidative stress, is measured to be 56.9 ± 2.6 M/atm (n = 3) at 37.4 °C with 1 mg of the material available.

  11. Design and Development of Gas-Liquid Cylindrical Cyclone Compact Separators for Three-Phase Flow

    SciTech Connect

    Mohan, Ram S.; Shoham, Ovadia

    1999-10-28

    The objective of this five-year project (October, 1997--September, 2002) is to expand the current research activities of Tulsa University Separation Technology Projects (TUSTP) to multiphase oil/water/gas separation. This project will be executed in two phases. Phase I (1997--2000) will focus on the investigations of the complex multiphase hydrodynamic flow behavior in a three-phase Gas-Liquid Cylindrical Cyclone (GLCC) Separator. The activities of this phase will include the development of a mechanistic model, a computational fluid dynamics (CFD) simulator, and detailed experimentation on the three-phase GLCC. The experimental and CFD simulation results will be suitably integrated with the mechanistic model. In Phase II (2000--2002), the developed GLCC separator will be tested under high pressure and real crudes conditions. This is crucial for validating the GLCC design for field application and facilitating easy and rapid technology deployment. Design criteria for industrial applications will be developed based on these results and will be incorporated into the mechanistic model by TUSTP.

  12. Crystalline Graphdiyne Nanosheets Produced at a Gas/Liquid or Liquid/Liquid Interface.

    PubMed

    Matsuoka, Ryota; Sakamoto, Ryota; Hoshiko, Ken; Sasaki, Sono; Masunaga, Hiroyasu; Nagashio, Kosuke; Nishihara, Hiroshi

    2017-02-15

    Synthetic two-dimensional polymers, or bottom-up nanosheets, are ultrathin polymeric frameworks with in-plane periodicity. They can be synthesized in a direct, bottom-up fashion using atomic, ionic, or molecular components. However, few are based on carbon-carbon bond formation, which means that there is a potential new field of investigation into these fundamentally important chemical bonds. Here, we describe the bottom-up synthesis of all-carbon, π-conjugated graphdiyne nanosheets. A liquid/liquid interfacial protocol involves layering a dichloromethane solution of hexaethynylbenzene on an aqueous layer containing a copper catalyst at room temperature. A multilayer graphdiyne (thickness, 24 nm; domain size, >25 μm) emerges through a successive alkyne-alkyne homocoupling reaction at the interface. A gas/liquid interfacial synthesis is more successful. Sprinkling a very small amount of hexaethynylbenzene in a mixture of dichloromethane and toluene onto the surface of the aqueous phase at room temperature generated single-crystalline graphdiyne nanosheets, which feature regular hexagonal domains, a lower degree of oxygenation, and uniform thickness (3.0 nm) and lateral size (1.5 μm).

  13. Design and Development of Gas-Liquid Cylindrical Cyclone Compact Separators for Three-Phase Flow

    SciTech Connect

    Mohan, R.S.; Shoham, O.

    2001-01-18

    The objective of this five-year project (October 1997 - September 2002) was to expand the current research activities of Tulsa University Separation Technology Projects (TUSTP) to multiphase oil/water/gas separation. This project was executed in two phases. Phase I (1997 - 2000) focused on the investigations of the complex multiphase hydrodynamic flow behavior in a three-phase Gas-Liquid Cylindrical Cyclone (GLCC) Separator. The activities of this phase included the development of a mechanistic model, a computational fluid dynamics (CFD) simulator, and detailed experimentation on the three-phase GLCC. The experimental and CFD simulation results will be suitably integrated with the mechanistic model. In Phase II (2000 - 2002), the developed GLCC separator will be tested under high pressure and real crude conditions. This is crucial for validating the GLCC design for field application and facilitating easy and rapid technology deployment. Design criteria for industrial applications will be developed based on these results and will be incorporated into the mechanistic model by TUSTP.

  14. Design and Development of Gas-Liquid Cylindrical Cyclone Compact Separators for Three-Phase Flow

    SciTech Connect

    Mohan, R.S.; Shoham, O.

    2001-01-10

    The objective of this five-year project (October 1997--September 2002) was to expand the current research activities of Tulsa University Separation Technology Projects (TUSTP) to multiphase oil/water/gas separation. This project was executed in two phases. Phase I (1997--2000) focused on the investigations of the complex multiphase hydrodynamic flow behavior in a three-phase Gas-Liquid Cylindrical Cyclone (GLCC) Separator. The activities of this phase included the development of a mechanistic model, a computational fluid dynamics (CFD) simulator, and detailed experimentation on the three-phase GLCC. The experimental and CFD simulation results will be suitably integrated with the mechanistic model. In Phase II (2000--2002), the developed GLCC separator will be tested under high pressure and real crude conditions. This is crucial for validating the GLCC design for field application and facilitating easy and rapid technology deployment. Design criteria for industrial applications will be developed based on these results and will be incorporated into the mechanistic model by TUSTP.

  15. Two parametric flow measurement in gas-liquid two-phase flow

    NASA Astrophysics Data System (ADS)

    Chen, Z.; Chen, C.; Xu, Y.; Zhao, Z.

    The importance and current development of two parametric measurement during two-phase flow are briefly reviewed in this paper. Gas-liquid two-phase two parametric metering experiments were conducted by using an oval gear meter and a sharp edged orifice mounted in series in a horizontal pipe. Compressed air and water were used as gas and liquid phases respectively. The correlations, which can be used to predict the total flow rate and volumetric quality of two-phase flow or volumetric flow rate of each phase, have also been proposed in this paper. Comparison of the calculated values of flow rate of each phase from the correlations with the test data showed that the root mean square fractional deviation for gas flow rate is 2.9 percent and for liquid flow rate 4.4 percent. The method proposed in this paper can be used to measure the gas and liquid flow rate in two-phase flow region without having to separate the phases.

  16. Acquisition of void fraction of pulsatile gas-liquid two-phase flow in rectangular channel

    NASA Astrophysics Data System (ADS)

    Zhou, Bao; Liu, Jingxing; Tian, Jingda

    2013-07-01

    Experiment on two-phase pulsatile flow in a narrow rectangular visualization channel was carried out and photographed. Every frame was treated and restored as a black-white binary picture with the threshold of both gray-scale and gray-scale gradient. The gas-liquid interface in the binary pictures can be recognized well, including some very obvious interface, which either cannot be distinguished, or introduce big wrong-recognized area with the gray-scale threshold only. Then after such as `dilate', `erode', `fill', `filter' and so on operating, the binary pictures can reflect the twophase distinction situation in the experimental channel well; The instantaneous average void frictions at the length that the camera covered were calculated by counting the black and white pixels from the pictures. The average void fractions in the whole length of the test section were calculated with an iteration method. The average void fractions in the special length covered by camera and the ones in the whole length of the test section are different. The former shows that the void frictions dramatically frequently change, while the later at steady flow almost stay peace, at pulsatile flow change smoothly.

  17. Can we approach the gas-liquid critical point using slab simulations of two coexisting phases?

    PubMed

    Goujon, Florent; Ghoufi, Aziz; Malfreyt, Patrice; Tildesley, Dominic J

    2016-09-28

    In this paper, we demonstrate that it is possible to approach the gas-liquid critical point of the Lennard-Jones fluid by performing simulations in a slab geometry using a cut-off potential. In the slab simulation geometry, it is essential to apply an accurate tail correction to the potential energy, applied during the course of the simulation, to study the properties of states close to the critical point. Using the Janeček slab-based method developed for two-phase Monte Carlo simulations [J. Janec̆ek, J. Chem. Phys. 131, 6264 (2006)], the coexisting densities and surface tension in the critical region are reported as a function of the cutoff distance in the intermolecular potential. The results obtained using slab simulations are compared with those obtained using grand canonical Monte Carlo simulations of isotropic systems and the finite-size scaling techniques. There is a good agreement between these two approaches. The two-phase simulations can be used in approaching the critical point for temperatures up to 0.97 TC(∗) (T(∗) = 1.26). The critical-point exponents describing the dependence of the density, surface tension, and interfacial thickness on the temperature are calculated near the critical point.

  18. New insights into liquid chromatography for more eco-friendly analysis of pharmaceuticals.

    PubMed

    Shaaban, Heba

    2016-10-01

    Greening the analytical methods used for analysis of pharmaceuticals has been receiving great interest aimed at eliminating or minimizing the amount of organic solvents consumed daily worldwide without loss in chromatographic performance. Traditional analytical LC techniques employed in pharmaceutical analysis consume tremendous amounts of hazardous solvents and consequently generate large amounts of waste. The monetary and ecological impact of using large amounts of solvents and waste disposal motivated the analytical community to search for alternatives to replace polluting analytical methodologies with clean ones. In this context, implementing the principles of green analytical chemistry (GAC) in analytical laboratories is highly desired. This review gives a comprehensive overview on different green LC pathways for implementing GAC principles in analytical laboratories and focuses on evaluating the greenness of LC analytical procedures. This review presents green LC approaches for eco-friendly analysis of pharmaceuticals in industrial, biological, and environmental matrices. Graphical Abstract Green pathways of liquid chromatography for more eco-friendly analysis of pharmaceuticals.

  19. Discrimination of honeys using colorimetric sensor arrays, sensory analysis and gas chromatography techniques.

    PubMed

    Tahir, Haroon Elrasheid; Xiaobo, Zou; Xiaowei, Huang; Jiyong, Shi; Mariod, Abdalbasit Adam

    2016-09-01

    Aroma profiles of six honey varieties of different botanical origins were investigated using colorimetric sensor array, gas chromatography-mass spectrometry (GC-MS) and descriptive sensory analysis. Fifty-eight aroma compounds were identified, including 2 norisoprenoids, 5 hydrocarbons, 4 terpenes, 6 phenols, 7 ketones, 9 acids, 12 aldehydes and 13 alcohols. Twenty abundant or active compounds were chosen as key compounds to characterize honey aroma. Discrimination of the honeys was subsequently implemented using multivariate analysis, including hierarchical clustering analysis (HCA) and principal component analysis (PCA). Honeys of the same botanical origin were grouped together in the PCA score plot and HCA dendrogram. SPME-GC/MS and colorimetric sensor array were able to discriminate the honeys effectively with the advantages of being rapid, simple and low-cost. Moreover, partial least squares regression (PLSR) was applied to indicate the relationship between sensory descriptors and aroma compounds.

  20. Supercritical fluid chromatography for GMP analysis in support of pharmaceutical development and manufacturing activities.

    PubMed

    Hicks, Michael B; Regalado, Erik L; Tan, Feng; Gong, Xiaoyi; Welch, Christopher J

    2016-01-05

    Supercritical fluid chromatography (SFC) has long been a preferred method for enantiopurity analysis in support of pharmaceutical discovery and development, but implementation of the technique in regulated GMP laboratories has been somewhat slow, owing to limitations in instrument sensitivity, reproducibility, accuracy and robustness. In recent years, commercialization of next generation analytical SFC instrumentation has addressed previous shortcomings, making the technique better suited for GMP analysis. In this study we investigate the use of modern SFC for enantiopurity analysis of several pharmaceutical intermediates and compare the results with the conventional HPLC approaches historically used for analysis in a GMP setting. The findings clearly illustrate that modern SFC now exhibits improved precision, reproducibility, accuracy and robustness; also providing superior resolution and peak capacity compared to HPLC. Based on these findings, the use of modern chiral SFC is recommended for GMP studies of stereochemistry in pharmaceutical development and manufacturing.

  1. Analysis of the citric acid cycle intermediates using gas chromatography-mass spectrometry.

    PubMed

    Kombu, Rajan S; Brunengraber, Henri; Puchowicz, Michelle A

    2011-01-01

    Researchers view analysis of the citric acid cycle (CAC) intermediates as a metabolomic approach to identifying unexpected correlations between apparently related and unrelated pathways of metabolism. Relationships of the CAC intermediates, as measured by their concentrations and relative ratios, offer useful information to understanding interrelationships between the CAC and metabolic pathways under various physiological and pathological conditions. This chapter presents a relatively simple method that is sensitive for simultaneously measuring concentrations of CAC intermediates (relative and absolute) and other related intermediates of energy metabolism using gas chromatography-mass spectrometry.

  2. Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

    USGS Publications Warehouse

    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.

  3. High-throughput multiclass method for antibiotic residue analysis by liquid chromatography-tandem mass spectrometry.

    PubMed

    Chico, J; Rúbies, A; Centrich, F; Companyó, R; Prat, M D; Granados, M

    2008-12-12

    A simple and rapid method has been developed for the residue analysis of 39 antibiotics (tetracyclines, quinolones, penicillins, sulfonamides and macrolides) in foodstuffs of animal origin. The method combines an effective extraction technique, which uses water-methanol as extracting solvent, with ultra-high-pressure liquid chromatography-tandem mass spectrometry, allowing both confirmation and quantification in a single chromatographic run. The multiresidue method has been validated in chicken muscle matrix according to European Union Decision 2002/657/EC. It has been implemented as a routine method in a Public Health Laboratory, instead of the five plates test and LC methods previously used.

  4. A Laboratory Experiment in Pharmaceutical Analysis: Analysis of Diazepam Tablets by High Pressure Liquid Chromatography

    ERIC Educational Resources Information Center

    Bailey, Leonard

    1978-01-01

    The experiment described was developed for the third-year course in inorganic and analytical pharmaceutical chemistry to provide students with "hands-on" experience with high pressure liquid chromatography. Assay procedures are given along with experimental parameters and student results. (LBH)

  5. Issues pertaining to the analysis of buprenorphine and its metabolites by gas chromatography-mass spectrometry.

    PubMed

    Wang, Yu-Shan; Lin, Dong-Liang; Yang, Shu-Ching; Wu, Meng-Yan; Liu, Ray H; Su, Lien-Wen; Cheng, Pai-Sheng; Liu, Chiareiy; Fuh, Ming-Ren

    2010-03-05

    "Substitution therapy" and the use of buprenorphine (B) as an agent for treating heroin addiction continue to gain acceptance and have recently been implemented in Taiwan. Mature and widely utilized gas chromatography-mass spectrometry (GC-MS) technology can complement the low cost and highly sensitive immunoassay (IA) approach to facilitate the implementation of analytical tasks supporting compliance monitoring and pharmacokinetic/pharmacogenetic studies. Issues critical to GC-MS analysis of B and norbuprenorphine (NB) (free and as glucuronides), including extraction, hydrolysis, derivatization, and quantitation approaches were studied, followed by comparing the resulting data against those derived from IA and two types of liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods. Commercial solid-phase extraction devices, highly effective for recovering all metabolites, may not be suitable for the analysis of free B and NB; acetyl-derivatization products exhibit the most favorable chromatographic, ion intensity, and cross-contribution characteristics for GC-MS analysis. Evaluation of IA, GC-MS, and LC-MS/MS data obtained in three laboratories has proven the 2-aliquot GC-MS protocol effective for the determination of free B and NB and their glucuronides.

  6. Development of Hydrophilic Interaction Liquid Chromatography Method for the Analysis of Moxonidine and Its Impurities

    PubMed Central

    2016-01-01

    Fast and simple hydrophilic interaction liquid chromatography (HILIC) method was developed and validated for the analysis of moxonidine and its four impurities (A, B, C, and D) in pharmaceutical dosage form. All experiments were performed on the Agilent Technologies 1200 high-performance liquid chromatography (HPLC) system using Zorbax RX-SIL, 250 mm × 4.6 mm, 5 μm column as stationary phase (T = 25°C, F = 1 mL/min, and λ = 255 nm), and mixture of acetonitrile and 40 mM ammonium formate buffer (pH 2.8) 80 : 20 (v/v) as mobile phase. Under the optimal chromatographic conditions, selected by central composite design, separation and analysis of moxonidine and its four impurities are enabled within 12 minutes. Validation of the method was conducted in accordance with ICH guidelines. Based on the obtained results selectivity, linearity (r ≥ 0.9976), accuracy (recovery: 93.66%–114.08%), precision (RSD: 0.56%–2.55%), and robustness of the method were confirmed. The obtained values of the limit of detection and quantification revealed that the method can be used for determination of impurities levels below 0.1%. Validated method was applied for determination of moxonidine and its impurities in commercially available tablet formulation. Obtained results confirmed that validated method is fast, simple, and reliable for analysis of moxonidine and its impurities in tablets. PMID:27847672

  7. Stability of Wavy Films in Gas-Liquid Two-Phase Flows at Normal and Microgravity Conditions

    NASA Technical Reports Server (NTRS)

    Balakotaiah, V.; Jayawardena, S. S.

    1996-01-01

    For flow rates of technological interest, most gas-liquid flows in pipes are in the annular flow regime, in which, the liquid moves along the pipe wall in a thin, wavy film and the gas flows in the core region. The waves appearing on the liquid film have a profound influence on the transfer rates, and hence on the design of these systems. We have recently proposed and analyzed two boundary layer models that describe the characteristics of laminar wavy films at high Reynolds numbers (300-1200). Comparison of model predictions to 1-g experimental data showed good agreement. The goal of our present work is to understand through a combined program of experimental and modeling studies the characteristics of wavy films in annular two-phase gas-liquid flows under normal as well as microgravity conditions in the developed and entry regions.

  8. Three-dimensional direct numerical simulations of co/counter-current vertical gas-Liquid annular flows

    NASA Astrophysics Data System (ADS)

    Farhaoui, Asma; Kahouadji, Lyes; Chergui, Jalel; Juric, Damir; Shin, Seungwon; Craster, Richard; Matar, Omar

    2016-11-01

    We carry out three-dimensional numerical simulations of co/counter current Gas-Liquid annular flows using the parallel code, BLUE, based on a projection method for the resolution of the Navier-Stokes equations and a hybrid Front-Tracking/Level-Set method for the interface advection. Gas-Liquid annular flows and falling films in a pipe are present in a broad range of industrial processes. This configuration consists of an important multiphase flow regime where the liquid occupies the area adjacent to the internal circumference of the pipe and the gas flows in the pipe core. Experimentally, four distinctive flow regimes were identified ('dual-wave', 'thick ripple', 'disturbance wave' and 'regular wave' regimes), that we attempt to simulate. In order to visualize these different regimes, various liquid (water) and gas (air) flow-rates are investigated. EPSRC UK Programme Grant EP/K003976/1.

  9. Comprehensive two-dimensional gas chromatography applied to illicit drug analysis.

    PubMed

    Mitrevski, Blagoj; Wynne, Paul; Marriott, Philip J

    2011-11-01

    Multidimensional gas chromatography (MDGC), and especially its latest incarnation--comprehensive two-dimensional gas chromatography (GC × GC)--have proved advantageous over and above classic one-dimensional gas chromatography (1D GC) in many areas of analysis by offering improved peak capacity, often enhanced sensitivity and, especially in the case of GC × GC, the unique feature of 'structured' chromatograms. This article reviews recent advances in MDGC and GC × GC in drug analysis with special focus on ecstasy, heroin and cocaine profiling. Although 1D GC is still the method of choice for drug profiling in most laboratories because of its simplicity and instrument availability, GC × GC is a tempting proposition for this purpose because of its ability to generate a higher net information content. Effluent refocusing due to the modulation (compression) process, combined with the separation on two 'orthogonal' columns, results in more components being well resolved and therefore being analytically and statistically useful to the profile. The spread of the components in the two-dimensional plots is strongly dependent on the extent of retention 'orthogonality' (i.e. the extent to which the two phases possess different or independent retention mechanisms towards sample constituents) between the two columns. The benefits of 'information-driven' drug profiling, where more points of reference are usually required for sample differentiation, are discussed. In addition, several limitations in application of MDGC in drug profiling, including data acquisition rate, column temperature limit, column phase orthogonality and chiral separation, are considered and discussed. Although the review focuses on the articles published in the last decade, a brief chronological preview of the profiling methods used throughout the last three decades is given.

  10. Analysis of macrolide antibiotics, using liquid chromatography-mass spectrometry, in food, biological and environmental matrices.

    PubMed

    Wang, Jian

    2009-01-01

    Macrolides are a group of antibiotics that have been widely used in human medical and veterinary practices. Analysis of macrolides and related compounds in food, biological, and environmental matrices continue to be the focus of scientists for the reasons of food safety, pharmacokinetic studies, and environmental concerns. This article presents an overview on the primary biological properties of macrolides and their associated analytical issues, including extraction, liquid chromatography-mass spectrometry (LC-MS), method validation, and measurement uncertainty. The main techniques that have been used to extract macrolides from various matrices are solid-phase extraction and liquid-liquid extraction. Conventional liquid chromatography (LC) with C18 columns plays a dominant role for the determination of macrolides, whereas ultra-performance liquid chromatography (UPLC) along with sub-2 microm particle C18 columns reduces run time and improves sensitivity. Mass spectrometry (MS), serving as a universal detection technique, has replaced ultraviolet (UV), fluorometric, and electrochemical detection for multi-macrolide analysis. The triple-quadrupole (QqQ), quadrupole ion trap (QIT), triple-quadrupole linear ion trap, time-of-flight (TOF), and quadrupole time-of-flight (QqTOF) mass spectrometers are current choices for the determination of macrolides, including quantification, confirmation, identification of their degradation products or metabolites, and structural elucidation. LC or UPLC coupled to a triple-quadrupole mass spectrometer operated in the multiple-reaction monitoring (MRM) mode (LC/MS/MS) is the first choice for quantification. UPLC-TOF or UPLC-QqTOF has been recognized as an emerging technique for accurate mass measurement and unequivocal identification of macrolides and their related compounds.

  11. Green chromatography.

    PubMed

    Płotka, Justyna; Tobiszewski, Marek; Sulej, Anna Maria; Kupska, Magdalena; Górecki, Tadeusz; Namieśnik, Jacek

    2013-09-13

    Analysis of organic compounds in samples characterized by different composition of the matrix is very important in many areas. A vast majority of organic compound determinations are performed using gas or liquid chromatographic methods. It is thus very important that these methods have negligible environmental impact. Chromatographic techniques have the potential to be greener at all steps of the analysis, from sample collection and preparation to separation and final determination. The paper summarizes the approaches used to accomplish the goals of green chromatography. While complete elimination of sample preparation would be an ideal approach, it is not always practical. Solventless extraction techniques offer a very good alternative. Where solvents must be used, the focus should be on the minimization of their consumption. The approaches used to make chromatographic separations greener differ depending on the type of chromatography. In gas chromatography it is advisable to move away from using helium as the carrier gas because it is a non-renewable resource. GC separations using low thermal mass technology can be greener because of energy savings offered by this technology. In liquid chromatography the focus should be on the reduction of solvent consumption and replacement of toxic and environmentally hazardous solvents with more benign alternatives. Multidimensional separation techniques have the potential to make the analysis greener in both GC and LC. The environmental impact of the method is often determined by the location of the instrument with respect to the sample collection point.

  12. Accelerating analysis for metabolomics, drugs and their metabolites in biological samples using multidimensional gas chromatography.

    PubMed

    Mitrevski, Blagoj S; Kouremenos, Konstantinos A; Marriott, Philip J

    2009-05-01

    Gas chromatography (GC) with mass spectrometry (MS) is one of the great enabling analytical tools available to the chemical and biochemical analyst for the measurement of volatile and semi-volatile compounds. From the analysis result, it is possible to assess progress in chemical reactions, to monitor environmental pollutants in a wide range of soil, water or air samples, to determine if an athlete or horse trainer has contravened doping laws, or if crude oil has migrated through subsurface rock to a reservoir. Each of these scenarios and samples has an associated implementation method for GC-MS. However, few samples and the associated interpretation of data is as complex or important as biochemical sample analysis for trace drugs or metabolites. Improving the analysis in both the GC and MS domains is a continual search for better separation, selectivity and sensitivity. Multidimensional methods are playing important roles in providing quality data to address the needs of analysts.

  13. Application of Pre-Column Labeling Liquid Chromatography for Canine Plasma-Free Amino Acid Analysis

    PubMed Central

    Azuma, Kazuo; Hirao, Yoshiko; Hayakawa, Yoshihiro; Murahata, Yusuke; Osaki, Tomohiro; Tsuka, Takeshi; Imagawa, Tomohiro; Okamoto, Yoshiharu; Ito, Norihiko

    2016-01-01

    Plasma-free amino acid (PFAA) levels are a useful metric for diagnosing cancer and providing a prognosis. However, the use of analysis of PFAA levels has been limited in the veterinary medicine field. We addressed the application of liquid chromatography (LC) using a pre-column labeling technique for analysis of canine PFAA levels. This method significantly shortened the analysis time relative to conventional methods. No diurnal fluctuations were detected at 9:00 AM in most PFAA levels, and food intake increased the levels of some PFAAs, including valine, leucine, tyrosine, phenylalanine, and proline. These results indicate that LC with pre-column labeling is useful for measuring canine PFAA levels, for which time of day and interval after food intake must be taken into consideration. PMID:26771650

  14. Analysis of Total Human Urinary Glycosaminoglycan Disaccharides by Liquid Chromatography-Tandem Mass Spectrometry.

    PubMed

    Sun, Xiaojun; Li, Lingyun; Overdier, Katherine H; Ammons, Lee Anne; Douglas, Ivor S; Burlew, Clay Cothren; Zhang, Fuming; Schmidt, Eric P; Chi, Lianli; Linhardt, Robert J

    2015-06-16

    The determination of complex analytes, present at low concentrations, in biological fluids poses a difficult challenge. This study relies on an optimized method of recovery, enzymatic treatment, and disaccharide analysis by liquid chromatography-tandem mass spectrometry to rapidly determine low concentrations of glycosaminoglycans in human urine. The approach utilizes multiple reaction monitoring (MRM) of glycosaminoglycan disaccharides obtained from treating urine samples with recombinant heparin lyases and chondroitin lyase. This rapid and sensitive method allows the analysis of glycosaminoglycan content and disaccharide composition in urine samples having concentrations 10- to 100-fold lower than those typically analyzed from patients with metabolic diseases, such as mucopolysaccharidosis. The current method facilitates the analysis low (ng/mL) levels of urinary glycosaminoglycans present in healthy individuals and in patients with pathological conditions, such as inflammation and cancers, that can subtly alter glycosaminoglycan content and composition.

  15. Enantiomeric analysis of limonene and carvone by direct introduction of aromatic plants into multidimensional gas chromatography.

    PubMed

    Barba, C; Toledano, R M; Santa-María, G; Herraiz, M; Martínez, R M

    2013-03-15

    Analysis of chiral compounds in complex mixtures is achieved by multidimensional gas chromatography using heptakis-(2,3,6-tri-O-methyl)-β-cyclodextrin stationary phase as the main column of the system to separate specific selected cuts containing components unresolved in the first dimension. The proposed procedure allows rapid analysis of both solid and liquid matrices by direct introduction, into the programmed temperature vaporizer (PTV) of a gas chromatograph, of either the plant material or the essential oil, respectively. A comparison between enantiomeric excesses data obtained, from plant leaves (or plant seeds) and the corresponding essential oils, by direct injection (i.e., without sample pretreatment or concentration step) into the multidimensional system is also included. Reported data demonstrate that no racemization occurs during analysis as identical enantiomeric excesses are obtained in both cases for specific chiral compounds.

  16. High-performance thin-layer chromatography method for inositol phosphate analysis.

    PubMed

    Hatzack, F; Rasmussen, S K

    1999-12-24

    A simple and inexpensive high-performance thin-layer chromatography (HPTLC) method for the analysis of inositol mono- to hexakisphosphates on cellulose precoated plates is described. Plates were developed in 1-propanol-25% ammonia solution-water (5:4:1) and substance quantities as low as 100-200 pmol were detected by molybdate staining. Chromatographic mobilities of nucleotides and phosphorylated carbohydrates were also characterized. Charcoal treatment was employed to separate nucleotides from inositol phosphates with similar R(F) values prior to HPTLC analysis. Practical application of the HPTLC system is demonstrated by analysis of grain extracts from wild type and low-phytate mutant barley as well as phytate degradation products resulting from barley phytase activity.

  17. Multiresidue analysis of 30 organochlorine pesticides in milk and milk powder by gel permeation chromatography-solid phase extraction-gas chromatography-tandem mass spectrometry.

    PubMed

    Zheng, Guocan; Han, Chao; Liu, Yi; Wang, Jing; Zhu, Meiwen; Wang, Chengjun; Shen, Yan

    2014-10-01

    A method for simultaneous determination of the 30 organochlorine pesticides (OCP) in milk and milk powder samples has been developed. Prior to the gas chromatography-tandem mass spectrometric analysis, the residual OCP in samples were extracted with n-hexane and acetone mixture (1/1, vol/vol) and cleaned up by gel permeation chromatography and solid phase extraction. Selected reaction monitoring mode was used for gas chromatography-tandem mass spectrometric data acquisition to identify and quantify the OCP. To avoid the matrix effects, matrix-matched calibration solutions ranging from 2 to 50 ng/mL were used to record the calibration curve. Limits of quantification of all OCP were 0.8 μg/kg. With the exception of endrin, limits of quantification are significantly lower than maximum residue limits set by the European Union and China. The average recoveries were in the range of 70.1 to 114.7% at 3 spiked concentration levels (0.8, 2.0, and 10.0 μg/kg) with residual standard deviation lower than 12.9%. The developed method was successfully applied to analyze the OCP in commercial milk products.

  18. Multivariate analysis of progressive thermal desorption coupled gas chromatography-mass spectrometry.

    SciTech Connect

    Van Benthem, Mark Hilary; Mowry, Curtis Dale; Kotula, Paul Gabriel; Borek, Theodore Thaddeus, III

    2010-09-01

    Thermal decomposition of poly dimethyl siloxane compounds, Sylgard{reg_sign} 184 and 186, were examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a method of producing multiway data using a stepped thermal desorption. The technique involves sequentially heating a sample of the material of interest with subsequent analysis in a commercial GC/MS system. The decomposition chromatograms were analyzed using multivariate analysis tools including principal component analysis (PCA), factor rotation employing the varimax criterion, and multivariate curve resolution. The results of the analysis show seven components related to offgassing of various fractions of siloxanes that vary as a function of temperature. Thermal desorption coupled with gas chromatography-mass spectrometry (TD/GC-MS) is a powerful analytical technique for analyzing chemical mixtures. It has great potential in numerous analytic areas including materials analysis, sports medicine, in the detection of designer drugs; and biological research for metabolomics. Data analysis is complicated, far from automated and can result in high false positive or false negative rates. We have demonstrated a step-wise TD/GC-MS technique that removes more volatile compounds from a sample before extracting the less volatile compounds. This creates an additional dimension of separation before the GC column, while simultaneously generating three-way data. Sandia's proven multivariate analysis methods, when applied to these data, have several advantages over current commercial options. It also has demonstrated potential for success in finding and enabling identification of trace compounds. Several challenges remain, however, including understanding the sources of noise in the data, outlier detection, improving the data pretreatment and analysis methods, developing a software tool for ease of use by the chemist, and demonstrating our belief that

  19. Chirospecific analysis of plant volatiles

    NASA Astrophysics Data System (ADS)

    Tkachev, A. V.

    2007-10-01

    Characteristic features of the analysis of plant volatiles by enantioselective gas (gas-liquid) chromatography and gas chromatography/mass spectrometry are discussed. The most recent advances in the design of enantioselective stationary phases are surveyed. Examples of the preparation of the most efficient phases based on modified cyclodextrins are given. Current knowledge on the successful analytical resolution of different types of plant volatiles (aliphatic and aromatic compounds and mono-, sesqui- and diterpene derivatives) into optical antipodes is systematically described. Chiral stationary phases used for these purposes, temperature conditions and enantiomer separation factors are summarised. Examples of the enantiomeric resolution of fragrance compounds and components of plant extracts, wines and essential oils are given.

  20. High efficiency chlorine removal from polyvinyl chloride (PVC) pyrolysis with a gas-liquid fluidized bed reactor.

    PubMed

    Yuan, G; Chen, D; Yin, L; Wang, Z; Zhao, L; Wang, J Y

    2014-06-01

    In this research a gas-liquid fluidized bed reactor was developed for removing chlorine (Cl) from polyvinyl chloride (PVC) to favor its pyrolysis treatment. In order to efficiently remove Cl within a limited time before extensive generation of hydrocarbon products, the gas-liquid fluidized bed reactor was running at 280-320 °C, where hot N2 was used as fluidizing gas to fluidize the molten polymer, letting the molten polymer contact well with N2 to release Cl in form of HCl. Experimental results showed that dechlorination efficiency is mainly temperature dependent and 300 °C is a proper reaction temperature for efficient dechlorination within a limited time duration and for prevention of extensive pyrolysis; under this temperature 99.5% of Cl removal efficiency can be obtained within reaction time around 1 min after melting is completed as the flow rate of N2 gas was set around 0.47-0.85 Nm(3) kg(-1) for the molten PVC. Larger N2 flow rate and additives in PVC would enhance HCl release but did not change the final dechlorination efficiency; and excessive N2 flow rate should be avoided for prevention of polymer entrainment. HCl is emitted from PVC granules or scraps at the mean time they started to melt and the melting stage should be taken into consideration when design the gas-liquid fluidized bed reactor for dechlorination.

  1. US crude oil, natural gas, and natural gas liquids reserves, 1977-1993 (for microcomputers). Data file

    SciTech Connect

    1994-12-31

    The diskette contains all data published in the reserves and production tables of each annual report of U.S. Crude Oil, Natural Gas and Natural Gas Liquids Reserves from 1977 through 1991 listed in 15 separate ASCII files, one per report year. Within each annual file, the records are separated by hydrocarbon type into the following: Crude Oil, Associated Dissolved Natural Gas, Nonassociated Natural Gas, Total Natural Gas, Lease Condensate, Natural Gas Plant Liquids, and Natural Gas Liquids. During the 15 years collated here, the data items gathered and published have changed, with dry versus wet natural gas being the primary difference and the consequent separation of natural gas liquids. The records are also separated by State or State subregions and a few tabulated combinations of States and State subregions. The EIA requirement to hold confidential the data gathered during the annual surveys has driven changes in the States, subregions and combinations published and therefore included in the diskette over the years. Data given on the records are the following: Proved reserves, beginning-of-year; Net Adjustments; Revision increases; Revision decreases; Extensions; New field Discoveries; New reservoirs in old fields; Production; and Reserves, end-of-year.

  2. Numerical and Experimental Investigation of Stratified Gas-Liquid Two-Phase Flow in Horizontal Circular Pipes

    SciTech Connect

    Faccini, J.L.H.; Sampaio, P.A.B. de

    2006-07-01

    This paper reports numerical and experimental investigation of stratified gas-liquid two-phase flow in horizontal circular pipes. The Reynolds averaged Navier Stokes equations (RANS) with the k-{omega} model for a fully developed stratified gas-liquid two-phase flow are solved by using the finite element method. A smooth and horizontal interface surface is assumed without considering the interfacial waves. The continuity of the shear stress across the interface is enforced with the continuity of the velocity being automatically satisfied by the variational formulation. For each given interface position and longitudinal pressure gradient, an inner iteration loop runs to solve the nonlinear equations. The Newton-Raphson scheme is used to solve the transcendental equations by an outer iteration to determine the interface position and pressure gradient for a given pair of volumetric flow rates. The interface position in a 51.2 mm ID circular pipe was measured experimentally by the ultrasonic pulse-echo technique. The numerical results were also compared with experimental results in a 21 mm ID circular pipe reported by Masala [1]. The good agreement between the numerical and experimental results indicates that the k-{omega} model can be applied for the numerical simulation of stratified gas-liquid two-phase flow. (authors)

  3. Large-Eddy Simulation of Transient Horizontal Gas-Liquid Flow in Continuous Casting Using Dynamic Subgrid-Scale Model

    NASA Astrophysics Data System (ADS)

    Liu, Zhongqiu; Li, Baokuan

    2017-03-01

    Euler-Euler simulations of transient horizontal gas-liquid flow in a continuous-casting mold are presented. The predictions were compared with previous experimental measurements by two-channel laser Doppler velocimeter. Simulations were performed to understand the sensitivity to different turbulence closure models [k-ɛ, shear stress transport (SST), Reynolds stress model (RSM), and large-eddy simulation (LES)] and different interfacial forces (drag, lift, virtual mass, wall lubrication, and turbulent dispersion). It was found that the LES model showed better agreement than the other turbulence models in predicting the velocity components of the liquid phase. Furthermore, an appropriate drag force coefficient model, lift force coefficient model, and virtual mass force coefficient were chosen. Meanwhile, the wall lubrication force and turbulent dispersion force did not have much effect on the current gas-liquid two-phase system. This work highlights the importance of choosing an appropriate bubble size in accordance with experiment. Finally, coupled with the optimized interfacial force models and bubble size, LES with a dynamic subgrid model was used to calculate the transient two-phase turbulent flow inside the mold. More instantaneous details of the two-phase flow characteristics in the mold were captured by LES, including multiscale vortex structures, fluctuation characteristics, and the vorticity distribution. The LES model can also be used to describe the time-averaged gas-liquid flow field, giving reasonably good agreement with mean experimental data. Thus, LES can be used effectively to study transient two-phase flow inside molds.

  4. Quantitative analysis of benzodiazepines in vitreous humor by high-performance liquid chromatography

    PubMed Central

    Bazmi, Elham; Behnoush, Behnam; Akhgari, Maryam; Bahmanabadi, Leila

    2016-01-01

    Objective: Benzodiazepines are frequently screened drugs in emergency toxicology, drugs of abuse testing, and in forensic cases. As the variations of benzodiazepines concentrations in biological samples during bleeding, postmortem changes, and redistribution could be biasing forensic medicine examinations, hence selecting a suitable sample and a validated accurate method is essential for the quantitative analysis of these main drug categories. The aim of this study was to develop a valid method for the determination of four benzodiazepines (flurazepam, lorazepam, alprazolam, and diazepam) in vitreous humor using liquid–liquid extraction and high-performance liquid chromatography. Methods: Sample preparation was carried out using liquid–liquid extraction with n-hexane: ethyl acetate and subsequent detection by high-performance liquid chromatography method coupled to diode array detector. This method was applied to quantify benzodiazepines in 21 authentic vitreous humor samples. Linear curve for each drug was obtained within the range of 30–3000 ng/mL with coefficient of correlation higher than 0.99. Results: The limit of detection and quantitation were 30 and 100 ng/mL respectively for four drugs. The method showed an appropriate intra- and inter-day precision (coefficient of variation < 10%). Benzodiazepines recoveries were estimated to be over 80%. The method showed high selectivity; no additional peak due to interfering substances in samples was observed. Conclusion: The present method was selective, sensitive, accurate, and precise for the quantitative analysis of benzodiazepines in vitreous humor samples in forensic toxicology laboratory. PMID:27635251

  5. Gas chromatography-vacuum ultraviolet spectroscopy for analysis of fatty acid methyl esters.

    PubMed

    Fan, Hui; Smuts, Jonathan; Bai, Ling; Walsh, Phillip; Armstrong, Daniel W; Schug, Kevin A

    2016-03-01

    A new vacuum ultraviolet (VUV) detector for gas chromatography was recently developed and applied to fatty acid methyl ester (FAME) analysis. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 FAMEs, including saturated, monounsaturated, and polyunsaturated types were recorded. Unsaturated FAMEs show significantly different gas phase absorption profiles than saturated ones, and these classes can be easily distinguished with the VUV detector. Another advantage includes differentiating cis/trans-isomeric FAMEs (e.g. oleic acid methyl ester and linoleic acid methyl ester isomers) and the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV also provides high specificity, sensitivity, and a fast data acquisition rate, making it a powerful tool for fatty acid screening when combined with gas chromatography. The fatty acid profile of several food oil samples (olive, canola, vegetable, corn, sunflower and peanut oils) were analyzed in this study to demonstrate applicability to real world samples.

  6. Analysis of amprolium by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

    PubMed

    Martínez-Villalba, Anna; Moyano, Encarnación; Galceran, M Teresa

    2010-09-10

    We present a fast liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the analysis of the coccidiostat amprolium in food samples. Tandem mass spectrometry in a triple quadrupole was used for quantitative purposes, and the information from multiple-stage mass spectrometry in an ion-trap mass analyzer contributed to fragmentation studies. Hydrophilic interaction liquid chromatography (HILIC) in a Fused-Core column using isocratic elution (acetonitrile:formic acid/ammonium formate buffer pH 4, 50 mM (60:40)) successfully analyzed this compound in less than 3 min. The HILIC system was coupled to heated electrospray-MS/MS using highly selective-selected reaction monitoring (H-SRM) to improve sensitivity and selectivity for the analysis of amprolium, after a simple sample treatment based on an "extract and shoot" strategy. Accurate mass measurements were performed to identify the interfering compound responsible for causing matrix ion enhancement in the signal of amprolium. The addition of l-carnitine (the interfering compound) (1 microg L(-1)) to standards and sample extracts allowed the use of the external calibration method for quantitative purposes. The LC-MS/MS (H-SRM) method showed good precision (relative standard deviation, RSD, lower than 13%), accuracy and linearity and allowed the determination of amprolium down to the ppb level (LODs between 0.1 and 0.6 microg kg(-1)).

  7. Capillary ion-exchange chromatography with nanogram sensitivity for the analysis of monoclonal antibodies.

    PubMed

    Rea, Jennifer C; Freistadt, Benny S; McDonald, Daniel; Farnan, Dell; Wang, Yajun Jennifer

    2015-12-11

    Ion-exchange chromatography (IEC) is widely used for profiling the charge heterogeneity of proteins, including monoclonal antibodies (mAbs). Despite good resolving power and robustness, ionic strength-based ion-exchange separations are generally product specific and can be time consuming to develop. In addition, conventional analytical scale ion-exchange separations require tens of micrograms of mAbs for each injection, amounts that are often unavailable in sample-limited applications. We report the development of a capillary IEC (c-IEC) methodology for the analysis of nanogram amounts of mAb charge variants. Several key modifications were made to a commercially available liquid chromatography system to perform c-IEC for charge variant analysis of mAbs with nanogram sensitivity. We demonstrate the method for multiple monoclonal antibodies, including antibody fragments, on different columns from different manufacturers. Relative standard deviations of <10% were achieved for relative peak areas of main peak, acidic and basic regions, which are common regions of interest for quantifying monoclonal antibody charge variants using IEC. The results herein demonstrate the excellent sensitivity of this c-IEC characterization method, which can be used for analyzing charge variants in sample-limited applications, such as early-stage candidate screening and in vivo studies.

  8. Analysis of odour compounds from scented consumer products using gas chromatography-mass spectrometry and gas chromatography-olfactometry.

    PubMed

    Bartsch, Jennifer; Uhde, Erik; Salthammer, Tunga

    2016-01-21

    Scented consumer products are being bought in increasing amounts and gaining more popularity. There is, however, relatively little information available about their ingredients, emissions and allergenic potential. Frequently, a mixture of different fragrance substances and not solely an individual substance contributes to the overall desired smell. The aim of this study was to investigate the odorous volatile organic compounds (OVOCs) in consumer products containing fragrances. Over 44 products were selected: various scented candles, printing products with different scent types and other products types particularly meant to be used indoors. Measurements were carried out in a desiccator. Air samples were collected on thermal desorption tubes to determine the released fragrance substances by means of gas chromatography-mass spectrometry (GC-MS). Moreover, gas chromatography-olfactometry (GC-O) was used to obtain sensory data and to ensure no important odorant was overlooked. Using both methods it was possible to distinguish between odour active and inactive compounds and subsequently to identify almost 300 different odorants across all scented products. Besides the advantage of differentiation, as the human nose is a very sensitive detector, GC-O was found to be a useful tool for detecting traces and chosen target compounds. One focus in this study lay on the 26 EU-regulated fragrance allergens to prove their relevance in scented consumer goods. In total, 18 of them were identified, with at least one substance being present in almost every product. Benzyl alcohol, cinnamaldehyde, citronellol, eugenol, linalool and limonene were the prevalently detected allergens. Particularly linalool and limonene were observed in over 50% of the products. In addition, eugenol appeared to be one of the most frequently detected compounds in trace-level concentrations in the candle emissions.

  9. The Application of High-Performance Liquid Chromatography to the Analysis of Petroleum Materials. Part 2. Quantitative Hydrocarbon-Type Analysis.

    DTIC Science & Technology

    Quantitative hydrocarbon type analysis of middle distillate petroleum products, with emphasis on straight-run (olefin-free) diesel fuels has been accomplished by high performance liquid chromatography using silica gel absorbents.

  10. Relaxation limit of a compressible gas-liquid model with well-reservoir interaction

    NASA Astrophysics Data System (ADS)

    Solem, Susanne; Evje, Steinar

    2017-02-01

    This paper deals with the relaxation limit of a two-phase compressible gas-liquid model which contains a pressure-dependent well-reservoir interaction term of the form q (P_r - P) where q>0 is the rate of the pressure-dependent influx/efflux of gas, P is the (unknown) wellbore pressure, and P_r is the (known) surrounding reservoir pressure. The model can be used to study gas-kick flow scenarios relevant for various wellbore operations. One extreme case is when the wellbore pressure P is largely dictated by the surrounding reservoir pressure P_r. Formally, this model is obtained by deriving the limiting system as the relaxation parameter q in the full model tends to infinity. The main purpose of this work is to understand to what extent this case can be represented by a well-defined mathematical model for a fixed global time T>0. Well-posedness of the full model has been obtained in Evje (SIAM J Math Anal 45(2):518-546, 2013). However, as the estimates for the full model are dependent on the relaxation parameter q, new estimates must be obtained for the equilibrium model to ensure existence of solutions. By means of appropriate a priori assumptions and some restrictions on the model parameters, necessary estimates (low order and higher order) are obtained. These estimates that depend on the global time T together with smallness assumptions on the initial data are then used to obtain existence of solutions in suitable Sobolev spaces.

  11. Generating Singlet Oxygen Bubbles: A New Mechanism for Gas-Liquid Oxidations in Water

    PubMed Central

    Bartusik, Dorota; Aebisher, David; Ghafari, BiBi

    2012-01-01

    Laser-coupled microphotoreactors were developed to bubble singlet oxygen [1O2 (1Δg)] into an aqueous solution containing an oxidizable compound. The reactors consisted of custom-modified SMA fiber-optic receptacles loaded with 150-μm silicon phthalocyanine glass sensitizer particles, where the particles were isolated from direct contact with water by a membrane adhesively bonded to the bottom of each device. A tube fed O2 gas to the reactor chambers. In the presence of O2, singlet oxygen was generated by illuminating the sensitizer particles with 669-nm light from an optical fiber coupled to the top of the reactor. The generated 1O2 was transported through the membrane by the O2 stream and formed bubbles in solution. In solution, singlet oxygen reacted with probe compounds (either 9,10-anthracene dipropionate dianion, trans-2-methyl-2-pentanoate anion, N-benzoyl-D,L-methionine, and N-acetyl-D,L-methionine) to give oxidized products in two stages. The early stage was rapid and showed that 1O2 transfer occurred via bubbles mainly in the bulk water solution. The later stage was slow, it arose only from 1O2-probe molecule contact at the gas/liquid interface. A mechanism is proposed that involves 1O2 mass transfer and solvation, where smaller bubbles provide better penetration of 1O2 into the flowing stream due to higher surface-to-volume contact between the probe molecules and 1O2. PMID:22260325

  12. DESIGN AND DEVELOPMENT OF GAS-LIQUID CYLINDRICAL CYCLONE COMPACT SEPARATORS FOR THREE-PHASE FLOW

    SciTech Connect

    Dr. Ram S. Mohan; Dr. Ovadia Shoham

    2000-04-28

    The objective of this five-year project (October, 1997-September, 2002) is to expand the current research activities of Tulsa University Separation Technology Projects (TUSTP) to multiphase oil/water/gas separation. This project will be executed in two phases. Phase I (1997-2000) will focus on the investigations of the complex multiphase hydrodynamic flow behavior in a three-phase Gas-Liquid Cylindrical Cyclone (GLCC{copyright}) Separator. The activities of this phase will include the development of a mechanistic model, a computational fluid dynamics (CFD) simulator, and detailed experimentation on the three-phase GLCC{copyright}. The experimental and CFD simulation results will be suitably integrated with the mechanistic model. In Phase II (2000-2002), the developed GLCC{copyright} separator will be tested under high pressure and real crudes conditions. This is crucial for validating the GLCC{copyright} design for field application and facilitating easy and rapid technology deployment. Design criteria for industrial applications will be developed based on these results and will be incorporated into the mechanistic model by TUSTP. This report presents a brief overview of the activities and tasks accomplished during the first half year (October 1, 1999-March 31, 2000) of the budget period (October 1, 1999-September 30, 2000). The total tasks of the budget period are given initially, followed by the technical and scientific results achieved till date. The report concludes with a detailed description of the plans for the conduct of the project for the second half year (April 1, 2000-September 30, 2000) of the current budget period.

  13. Effects of self-pulsation on the spray characteristics of gas-liquid swirl coaxial injector

    NASA Astrophysics Data System (ADS)

    Kang, Zhongtao; Li, Qinglian; Cheng, Peng; Zhang, Xinqiao; Wang, Zhen-guo

    2016-10-01

    To understand the influence of self-pulsation on the spray characteristics of gas-liquid swirl coaxial injector, a back-lighting photography technique has been employed to capture the instantaneous self-pulsated spray and stable spray images with a high speed camera. The diameter and velocity of the droplets in the spray have been characterized with a Dantec Phase Doppler Anemometry (PDA) system. The effects of self-pulsation on the spray pattern, primary breakup, spray angle, diameter and velocity distribution and mass flow rate distribution are analyzed and discussed. The results show that the spray morphology is greatly influenced by self-pulsation. The stable spray has a cone shape, while the self-pulsated spray looks like a Christmas tree. The main difference of these two sprays is the primary breakup. The liquid film of stable spray keeps stable while that of self-pulsated spray oscillates periodically. The film width of self-pulsated spray varies in a large range with 'neck' and 'shoulder' features existing. The liquid film of self-pulsated spray breaks up at the second neck, and then the second shoulder begins to breakup into ligaments. The self-pulsated spray produces droplet clusters periodically, varies horizontal spray width and mass flux periodically. From the point of spatial distribution, self-pulsation is good for the spray, it uniformizes the mass flux along radius and increases the spray angle. However, when self-pulsation occurs, the SMD distribution varies from an inverted V shape to a hollow cone shape, and SMD increases at all the measuring points. Namely, from the point of atomization performance, self-pulsation has negative effects even when the breakup length is smaller. The effects of self-pulsation on the diameter and velocity distributions of the spray are mainly in the center part of the spray. The periphery of stable and self-pulsated spray has similar diameter and velocity distribution.

  14. Analysis of Free Fatty Acids on the Fingertips by High Performance Liquid Chromatography.

    DTIC Science & Technology

    1978-12-20

    This investigation studied the efficiency of high performance liquid chromatography in the determination of free fatty acids present on the...utilized to eliminate the microbial contamination. The high performance liquid chromatography provided excellent separation of skin fatty acids for

  15. High performance thin layer chromatography (HPTLC) and high performance liquid chromatography (HPLC) for the qualitative and quantitative analysis of Calendula officinalis-advantages and limitations.

    PubMed

    Loescher, Christine M; Morton, David W; Razic, Slavica; Agatonovic-Kustrin, Snezana

    2014-09-01

    Chromatography techniques such as HPTLC and HPLC are commonly used to produce a chemical fingerprint of a plant to allow identification and quantify the main constituents within the plant. The aims of this study were to compare HPTLC and HPLC, for qualitative and quantitative analysis of the major constituents of Calendula officinalis and to investigate the effect of different extraction techniques on the C. officinalis extract composition from different parts of the plant. The results found HPTLC to be effective for qualitative analysis, however, HPLC was found to be more accurate for quantitative analysis. A combination of the two methods may be useful in a quality control setting as it would allow rapid qualitative analysis of herbal material while maintaining accurate quantification of extract composition.

  16. Analysis of estrogens and androgens in postmenopausal serum and plasma by liquid chromatography-mass spectrometry.

    PubMed

    Wang, Qingqing; Bottalico, Lisa; Mesaros, Clementina; Blair, Ian A

    2015-07-01

    Liquid chromatography-selected reaction monitoring/mass spectrometry-based methodology has evolved to the point where accurate analyses of trace levels of estrogens and androgens in postmenopausal serum and plasma can be accomplished with high precision and accuracy. A suite of derivatization procedures has been developed, which together with modern mass spectrometry instrumentation provide investigators with robust and sensitive methodology. Pre-ionized derivatives are proving to be useful as they are not subject to suppression of the electrospray signal. Postmenopausal women with elevated plasma or serum estrogens are thought to be at increased risk for breast and endometrial cancer. Therefore, significant advances in risk assessment should be possible now that reliable methodology is available. It is also possible to conduct analyses of multiple estrogens in plasma or serum. Laboratories that are currently employing liquid chromatography/mass spectrometry methodology can now readily implement this strategy. This will help conserve important plasma and serum samples available in Biobanks, as it will be possible to conduct high sensitivity analyses using low initial sample volumes. Reported levels of both conjugated and non-conjugated estrogen metabolites are close to the limits of sensitivity of many assays to date, urging caution in the interpretation of these low values. The analysis of serum androgen precursors in postmenopausal women has not been conducted routinely in the past using liquid chromatography/mass spectrometry methodology. Integration of serum androgen levels into the panel of metabolites analyzed could provide additional information for assessing cancer risk and should be included in the future.

  17. Basic Principles of Chromatography

    NASA Astrophysics Data System (ADS)

    Ismail, Baraem; Nielsen, S. Suzanne

    Chromatography has a great impact on all areas of analysis and, therefore, on the progress of science in general. Chromatography differs from other methods of separation in that a wide variety of materials, equipment, and techniques can be used. [Readers are referred to references (1-19) for general and specific information on chromatography.]. This chapter will focus on the principles of chromatography, mainly liquid chromatography (LC). Detailed principles and applications of gas chromatography (GC) will be discussed in Chap. 29. In view of its widespread use and applications, high-performance liquid chromatography (HPLC) will be discussed in a separate chapter (Chap. 28). The general principles of extraction are first described as a basis for understanding chromatography.

  18. Saffron authentication based on liquid chromatography high resolution tandem mass spectrometry and multivariate data analysis.

    PubMed

    Rubert, Josep; Lacina, Ondrej; Zachariasova, Milena; Hajslova, Jana

    2016-08-01

    Saffron is one of the oldest and most expensive spices, which is often target of fraudulent activities. In this research, a new strategy of saffron authentication based on metabolic fingerprinting was developed. In the first phase, a solid liquid extraction procedure was optimized, the main aim was to isolate as maximal representation of small molecules contained in saffron as possible. In the second step, a detection method based on liquid chromatography coupled with high-resolution mass spectrometry was developed. Initially, principal component analysis (PCA) revealed clear differences between saffron cultivated and packaged in Spain, protected designation of origin (PDO), and saffron packaged in Spain of unknown origin, labeled Spanish saffron. Afterwards, orthogonal partial least square discriminant analysis (OPLS-DA) was favorably used to discriminate between Spanish saffron. The tentative identification of markers showed glycerophospholipids and their oxidized lipids were significant markers according to their origin.

  19. Verification of chemical composition of commercially available propolis extracts by gas chromatography-mass spectrometry analysis.

    PubMed

    Czyżewska, Urszula; Konończuk, Joanna; Teul, Joanna; Drągowski, Paweł; Pawlak-Morka, Renata; Surażyński, Arkadiusz; Miltyk, Wojciech

    2015-05-01

    Propolis is a resin that is collected by honeybees from various plant sources. Due to its pharmacological properties, it is used in commercial production of nutritional supplements in pharmaceutical industry. In this study, gas chromatography-mass spectrometry was applied for quality control analysis of the three commercial specimens containing aqueous-alcoholic extracts of bee propolis. More than 230 constituents were detected in analyzed products, including flavonoids, chalcones, cinnamic acids and their esters, phenylpropenoid glycerides, and phenylpropenoid sesquiterpenoids. An allergenic benzyl cinnamate ester was also identified in all tested samples. This analytical method allows to evaluate biological activity and potential allergenic components of bee glue simultaneously. Studies on chemical composition of propolis samples may provide new approach to quality and safety control analysis in production of propolis supplementary specimens.

  20. [Analysis of amines in water samples by high performance liquid chromatography-laser induced fluorescence detection].

    PubMed

    Liu, Fan; Gao, Fangyuan; Tang, Tao; Sun, Yuanshe; Li, Tong; Zhang, Weibing

    2013-11-01

    A sensitive high performance liquid chromatography (HPLC)-laser induced fluorescence detection (LIFD) method was developed for the determination of amines. The derivatization and separation conditions were investigated. Under the optimized conditions, spermidine, putrescine and histamine were analyzed. The limits of detection (LODs) of the three biogenic amines (S/N = 3) were as low as 10(-10) mol/L. This method showed excellent stability. The RSDs of retention times and peak areas of the three biogenic amines were lower than 0.3% and 3%, respectively. This method was applied in biogenic amine analysis in water samples, and the average recoveries were in the range of 94.99%-104.7%. Furthermore, the amines in seven tea samples were analyzed by this method, and satisfactory results were achieved. The developed assay is of excellent sensitivity and good reproducibility, which can be used in the analysis of the amines in water samples.

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

    NASA Astrophysics Data System (ADS)

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

    1998-05-01

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

  2. Qualitative analysis of Cu2+, Co2+, and Ni2+ cations using thin-layer chromatography.

    PubMed

    Ergül, Soner

    2004-03-01

    The M(DEDTC)2 (M = Cu, Co, or Ni) and M(PyDTC)2 (M = Cu or Co) complexes prepared by reactions of sodium diethyldithiocarbamate and ammonium pyrollidinedithiocarbamate with metal (II) nitrates are examined for qualitative analysis and separation using thin-layer chromatography systems. These complexes and their mixtures are spotted to the activated thin layers of silica gel 60GF254 (Si-60GF254) with a 250-microm thickness. Pure toluene and a toluene-cyclohexane mixture (3:1, v/v) are used as mobile phases for running of the complexes. These chromatographic systems are successfully used for qualitative analysis of corresponding metal cations and separation of components in both M(DEDTC)2 and M(PyDTC)2 complex mixtures.

  3. Size exclusion chromatography with Corona charged aerosol detector for the analysis of polyethylene glycol polymer.

    PubMed

    Kou, Dawen; Manius, Gerald; Zhan, Shangdong; Chokshi, Hitesh P

    2009-07-10

    A technique of using size exclusion chromatography (SEC) with the Corona charged aerosol detector (CAD) was developed and evaluated in comparison with refractive index (RI) and evaporative light scattering detection (ELSD) for fast screening of polyethylene glycol (PEG), a polymer used in preparing pegylated pharmaceutical compounds. These detection techniques were used in the analysis of multiple lots of PEG reagents. CAD was found to provide more accurate impurity and polydispersity profiles of PEG reagents that better differentiate their quality, while RI was not suitable for this application due to its low sensitivity and ELSD led to underestimation of the impurity and polydispersity. The accuracy of polydispersity determination by SEC-CAD was validated against a commercial reference standard of known polydispersity. The SEC-CAD technique and the observed differences between the three detectors can also be applied to polymer analysis in general.

  4. Pesticide residue analysis of vegetables by gas chromatography with electron-capture detection.

    PubMed

    Fenoll, José; Hellín, Pilar; Martínez, Carmen M; Flores, Pilar

    2007-01-01

    A new and original analytical method was developed for the routine analysis of 28 multiclass pesticide residues in vegetables (green pepper, red pepper, and tomato). The extraction was performed with acetone, and the pesticides were partitioned into ethyl acetate-cyclohexane (1 + 1, v/v). Residue levels in vegetables were determined by gas chromatography (GC) with electron-capture detection. Residue identities were confirmed by GC coupled with mass spectrometry in the selected ion monitoring mode. The average recoveries in pepper and tomato obtained for all analytes studied were 67.3 and 123.1%, respectively, with relative standard deviation between 1.8 and 7.0%. The detection limit for the pesticides studied varied from 0.1 to 2.6 microg/kg. The proposed method was applied to the analysis of these compounds in vegetables grown in experimental greenhouses.

  5. Phytochemical analysis of Hibiscus caesius using high performance liquid chromatography coupled with mass spectrometry.

    PubMed

    Ain, Quratul; Naveed, Muhammad Na; Mumtaz, Abdul Samad; Farman, Muhammad; Ahmed, Iftikhar; Khalid, Nauman

    2015-09-01

    Various species in genus Hibiscus are traditionally known for their therapeutic attributes. The present study focused on the phytochemical analysis of a rather unexplored species Hibiscus caesius (H. caesius), using high-pressure liquid chromatography coupled with mass spectrometry (HPLC-MS). The analysis revealed five major compounds in the aqueous extract, viz. vanillic acid, protocatechoic acid, quercetin, quercetin glucoside and apigenin, being reported for the first time in H. caesius. Literature suggests that these compounds have important pharmacological traits such as anti-cancer, anti-inflammatory, anti-bacterial and hepatoprotective etc. however, this requires further pharmacological investigations at in vitro and in vivo scale. The above study concluded the medicinal potential of H. caesius.

  6. Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

    PubMed Central

    Preti, Raffaella

    2016-01-01

    The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large amount of samples must be analyzed fast using reliable and solvent-saving apparatus. The literature hereby described shows how the outstanding performances provided by core-shell particles column on a traditional HPLC instruments are comparable to those obtained with a costly UHPLC instrumentation, making this novel column a promising key tool in food analysis. PMID:27143972

  7. Development of high performance liquid chromatography method for miconazole analysis in powder sample

    NASA Astrophysics Data System (ADS)

    Hermawan, D.; Suwandri; Sulaeman, U.; Istiqomah, A.; Aboul-Enein, H. Y.

    2017-02-01

    A simple high performance liquid chromatography (HPLC) method has been developed in this study for the analysis of miconazole, an antifungal drug, in powder sample. The optimized HPLC system using C8 column was achieved using mobile phase composition containing methanol:water (85:15, v/v), a flow rate of 0.8 mL/min, and UV detection at 220 nm. The calibration graph was linear in the range from 10 to 50 mg/L with r 2 of 0.9983. The limit of detection (LOD) and limit of quantitation (LOQ) obtained were 2.24 mg/L and 7.47 mg/L, respectively. The present HPLC method is applicable for the determination of miconazole in the powder sample with a recovery of 101.28 % (RSD = 0.96%, n = 3). The developed HPLC method provides short analysis time, high reproducibility and high sensitivity.

  8. Improving sensitivity in chiral supercritical fluid chromatography for analysis of active pharmaceutical ingredients.

    PubMed

    Helmy, Roy; Biba, Mirlinda; Zang, Jia; Mao, Bing; Fogelman, Kimber; Vlachos, Vaso; Hosek, Paul; Welch, Christopher J

    2007-11-01

    Despite its status as the preferred method for routine enantiopurity analysis in pharmaceutical research, supercritical fluid chromatography (SFC) has historically been unsuited for the accurate and precise measurements required for release testing of active pharmaceutical ingredients (APIs) under current good manufacturing processes (cGMPs). Insufficient signal to noise, as compared to HPLC, has heretofore been the major limitation of the chiral SFC approach. We herein describe an investigation into the fundamental limitations and sources of noise in the SFC approach, identifying thermal, electronic, and mechanical sources of noise within the flow cell as key parameters contributing to reduced sensitivity. A variety of instrument modifications are explored, ultimately leading to the development of a new and improved flow cell and other instrument modifications that allow suitable sensitivity and accuracy to carry out GMP release testing for enantiopurity analysis using SFC.

  9. Quantitative analysis of vitamin D3 in a feed using normal phase high pressure liquid chromatography.

    PubMed

    Cohen, H; Lapointe, M

    1979-09-01

    A procedure is described for the separation and quantification of Vitamin D3 from different feeds and premixes. The study was conducted, first using a liquid partition step as a preliminary clean-up after extraction, then chromatography on activated Silica gel 60 before final analysis on a high pressure liquid chromatograph (HPLC) using a LiChrosorb NH2 (10 mu) column and a variable wavelength UV detector set at 264 nm. Total analysis on the HPLC was achieved in fifteen minutes. The detector response curve for an authentic D3 standard was linear using peak areas with a minimum detectable amount being 5 ng. The overall percent recovery of D3 in feeds was 94.4 +/- 2.4%. The minimum detectable amount of D3 in animal feeds was found to be in the region of 2,000 I.U./kg.

  10. Application of turbulent flow chromatography to the metabonomic analysis of human plasma: comparison with protein precipitation.

    PubMed

    Michopoulos, Filippos; Edge, Antony M; Theodoridis, Georgios; Wilson, Ian D

    2010-06-01

    The use of turbulent flow chromatography (TFC) as a method for the rapid metabonomic LC-MS analysis of plasma as an alternative to solvent-based protein precipitation has been investigated. This comparison has shown that TFC can be effectively used in this application with the benefit that off-line sample handling is significantly reduced. However, analysis of the data obtained via TFC for human plasma reveals substantial differences in the overall metabolite profiles compared with methanol-precipitated HPLC-MS. This seems in part at least to be related to greatly reduced amounts of phospholipids (ca. 10 fold reduction) for the turbulent flow methodology compared with protein-precipitated samples. The significance of these differences with respect to metabolite profiles as a result of the sample preparation method used are discussed.

  11. Analysis of small carbohydrates in several bioactive botanicals by gas chromatography with mass spectrometry and liquid chromatography with tandem mass spectrometry.

    PubMed

    Moldoveanu, Serban; Scott, Wayne; Zhu, Jeff

    2015-11-01

    Bioactive botanicals contain natural compounds with specific biological activity, such as antibacterial, antioxidant, immune stimulating, and taste improving. A full characterization of the chemical composition of these botanicals is frequently necessary. A study of small carbohydrates from the plant materials of 18 bioactive botanicals is further described. The study presents the identification of the carbohydrate using a gas chromatographic-mass spectrometric analysis that allows detection of molecules as large as maltotetraose, after changing them into trimethylsilyl derivatives. A number of carbohydrates in the plant (fructose, glucose, mannose, sucrose, maltose, xylose, sorbitol, and myo-, chiro-, and scyllo-inositols) were quantitated using a novel liquid chromatography with tandem mass spectrometric technique. Both techniques involved new method developments. The gas chromatography with mass spectrometric analysis involved derivatization and separation on a Rxi(®)-5Sil MS column with H2 as a carrier gas. The liquid chromatographic separation was obtained using a hydrophilic interaction type column, YMC-PAC Polyamine II. The tandem mass spectrometer used an electrospray ionization source in multiple reaction monitoring positive ion mode with the detection of the adducts of the carbohydrates with Cs(+) ions. The validated quantitative procedure showed excellent precision and accuracy allowing the analysis in a wide range of concentrations of the analytes.

  12. Analysis of starch in food systems by high-performance size exclusion chromatography.

    PubMed

    Ovando-Martínez, Maribel; Whitney, Kristin; Simsek, Senay

    2013-02-01

    Starch has unique physicochemical characteristics among food carbohydrates. Starch contributes to the physicochemical attributes of food products made from roots, legumes, cereals, and fruits. It occurs naturally as distinct particles, called granules. Most starch granules are a mixture of 2 sugar polymers: a highly branched polysaccharide named amylopectin and a basically linear polysaccharide named amylose. The starch contained in food products undergoes changes during processing, which causes changes in the starch molecular weight and amylose to amylopectin ratio. The objective of this study was to develop a new, simple, 1-step, and accurate method for simultaneous determination of amylose and amylopectin ratio as well as weight-averaged molecular weights of starch in food products. Starch from bread flour, canned peas, corn flake cereal, snack crackers, canned kidney beans, pasta, potato chips, and white bread was extracted by dissolving in KOH, urea, and precipitation with ethanol. Starch samples were solubilized and analyzed on a high-performance size exclusion chromatography (HPSEC) system. To verify the identity of the peaks, fractions were collected and soluble starch and beta-glucan assays were performed additional to gas chromatography analysis. We found that all the fractions contain only glucose and soluble starch assay is correlated to the HPSEC fractionation. This new method can be used to determine amylose amylopectin ratio and weight-averaged molecular weight of starch from various food products using as low as 25 mg dry samples.

  13. Complementary fragmentation pattern analysis by gas chromatography-mass spectrometry and liquid chromatography tandem mass spectrometry confirmed the precious lignan content of Cirsium weeds.

    PubMed

    Boldizsár, I; Kraszni, M; Tóth, F; Noszál, B; Molnár-Perl, I

    2010-10-01

    In this paper, as novelties to the field, it is confirmed at first, that the fruits of Cirsium species, regarded as injurious weeds, do contain lignans, two, different butyrolactone-type glycoside/aglycone pairs: the well known arctiin/arctigenin and the particularly rare tracheloside/trachelogenin species. These experiences were supported by gas chromatography-mass spectrometry (GC-MS), by liquid chromatography tandem mass spectrometry (LC-MS/(MS)) and by nuclear magnetic resonance (NMR) spectroscopy. The study reflects the powerful impact of the complementary chromatographic mass fragmentation evidences resulting in the identification and quantification, the extremely rare, with on line technique not yet identified and described, tracheloside/trachelogenin pair lignans, without authentic standard compounds. Fragmentation pattern analysis of the trimethylsilyl (TMS) derivative of trachelogenin, based on GC-MS, via two different fragmentation pathways confirmed the detailed structure of the trachelogenin molecule. The complementary chromatographic evidences have been unambiguously confirmed, by (1)H and (13)C NMR analysis of trachelogenin, isolated by preparative chromatography. Identification and quantification of the fruit extracts of four Cirsium (C.) species (C. arvense, C. canum, C. oleraceum, and C. palustre), revealed that (i) all four species do accumulate the tracheloside/trachelogenin or the arctiin/arctigenin butyrolactone-type glycoside/aglycone pairs, (ii) the overwhelming part of lignans are present as glycosides (tracheloside 9.1-14.5 mg/g, arctiin 28.6-39.3 mg/g, expressed on dry fruit basis), (iii) their acidic and enzymatic hydrolyses to the corresponding aglycones, to trachelogenin and arctigenin are fast and quantitative and (iv) the many-sided beneficial trachelogenin and arctigenin can be prepared separately, without impurities, excellent for medicinal purposes.

  14. Online coupling of hydrophilic interaction/strong cation exchange/reversed-phase liquid chromatography with porous graphitic carbon liquid chromatography for simultaneous proteomics and N-glycomics analysis.

    PubMed

    Zhao, Yun; Law, Henry C H; Zhang, Zaijun; Lam, Herman C; Quan, Quan; Li, Guohui; Chu, Ivan K

    2015-10-09

    In this study we developed a fully automated three-dimensional (3D) liquid chromatography methodology-comprising hydrophilic interaction separation as the first dimension, strong cation exchange fractionation as the second dimension, and low-pH reversed-phase (RP) separation as the third dimension-in conjunction downstream with additional complementary porous graphitic carbon separation, to capture non-retained hydrophilic analytes, for both shotgun proteomics and N-glycomics analyses. The performance of the 3D system alone was benchmarked through the analysis of the total lysate of Saccharomyces cerevisiae, leading to improved hydrophilic peptide coverage, from which we identified 19% and 24% more proteins and peptides, respectively, relative to those identified from a two-dimensional hydrophilic interaction liquid chromatography and low-pH RP chromatography (HILIC-RP) system over the same mass spectrometric acquisition time; consequently, the 3D platform also provided enhanced proteome and protein coverage. When we applied the integrated technology to analyses of the total lysate of primary cerebellar granule neurons, we characterized a total of 2201 proteins and 16,937 unique peptides for this primary cell line, providing one of its most comprehensive datasets. Our new integrated technology also exhibited excellent performance in the first N-glycomics analysis of cynomolgus monkey plasma; we successfully identified 122 proposed N-glycans and 135 N-glycosylation sites from 122 N-glycoproteins, and confirmed the presence of 38 N-glycolylneuraminic acid-containing N-glycans, a rare occurrence in human plasma, through tandem mass spectrometry for the first time.

  15. Analysis of a gas-liquid film plasma reactor for organic compound oxidation.

    PubMed

    Hsieh, Kevin; Wang, Huijuan; Locke, Bruce R

    2016-11-05

    A pulsed electrical discharge plasma formed in a tubular reactor with flowing argon carrier gas and a liquid water film was analyzed using methylene blue as a liquid phase hydroxyl radical scavenger and simultaneous measurements of hydrogen peroxide formation. The effects of liquid flow rate, liquid conductivity, concentration of dye, and the addition of ferrous ion on dye decoloration and degradation were determined. Higher liquid flow rates and concentrations of dye resulted in less decoloration percentages and hydrogen peroxide formation due to initial liquid conductivity effects and lower residence times in the reactor. The highest decoloration energy yield of dye found in these studies was 5.2g/kWh when using the higher liquid flow rate and adding the catalyst. The non-homogeneous nature of the plasma discharge favors the production of hydrogen peroxide in the plasma-liquid interface over the chemical oxidation of the organic in the bulk liquid phase and post-plasma reactions with the Fenton catalyst lead to complete utilization of the plasma-formed hydrogen peroxide.

  16. Structural Analysis of Perfluoropropanoyl Fluoride in the Gas, Liquid, and Solid Phases.

    PubMed

    Berrueta Martínez, Yanina; Reuter, Christian G; Vishnevskiy, Yury V; Bava, Yanina B; Picone, A Lorena; Romano, Rosana M; Stammler, Hans-Georg; Neumann, Beate; Mitzel, Norbert W; Della Védova, Carlos O

    2016-04-21

    The coexistence of two conformers in perfluoropropanoyl fluoride, CF3CF2C(O)F, differing in the CC-CF dihedral angle (gauche 85(10)% and anti 15(10)%), has been determined by means of gas-phase electron diffraction (GED). Quantum-chemical calculations performed at the MP2 and B3LYP approximations and cc-pVTZ basis sets reproduce the experimental values with confidence. By contrast, FTIR spectra give no clear evidence for the anti-conformer in the gas phase. Information on this less abundant but stable rotamer is obtained from matrix-isolation/FTIR spectroscopy and liquid Raman spectroscopy. In situ crystallization and single-crystal X-ray diffraction (XRD) data reveal the presence of solely the gauche-conformation in the solid state. A set of intermolecular interactions including C═O···C═O, C-F···F-C, and F···C═O is detected. The nature of bonding and the relative stabilities of gauche- and anti-conformers are explored using natural bond orbitals.

  17. Advances in liquid chromatography-high-resolution mass spectrometry for quantitative and qualitative environmental analysis.

    PubMed

    Aceña, Jaume; Stampachiacchiere, Serena; Pérez, Sandra; Barceló, Damià

    2015-08-01

    This review summarizes the advances in environmental analysis by liquid chromatography-high-resolution mass spectrometry (LC-HRMS) during the last decade and discusses different aspects of their application. LC-HRMS has become a powerful tool for simultaneous quantitative and qualitative analysis of organic pollutants, enabling their quantitation and the search for metabolites and transformation products or the detection of unknown compounds. LC-HRMS provides more information than low-resolution (LR) MS for each sample because it can accurately determine the mass of the molecular ion and its fragment ions if it can be used for MS-MS. Another advantage is that the data can be processed using either target analysis, suspect screening, retrospective analysis, or non-target screening. With the growing popularity and acceptance of HRMS analysis, current guidelines for compound confirmation need to be revised for quantitative and qualitative purposes. Furthermore, new commercial software and user-built libraries are required to mine data in an efficient and comprehensive way. The scope of this critical review is not to provide a comprehensive overview of the many studies performed with LC-HRMS in the field of environmental analysis, but to reveal its advantages and limitations using different workflows.

  18. Reinforcement of frontal affinity chromatography for effective analysis of lectin-oligosaccharide interactions.

    PubMed

    Hirabayashi, J; Arata, Y; Kasai, K

    2000-08-25

    Frontal affinity chromatography is a method for quantitative analysis of biomolecular interactions. We reinforced it by incorporating various merits of a contemporary liquid chromatography system. As a model study, the interaction between an immobilized Caenorhabditis elegans galectin (LEC-6) and fluorescently labeled oligosaccharides (pyridylaminated sugars) was analyzed. LEC-6 was coupled to N-hydroxysuccinimide-activated Sepharose 4 Fast Flow (100 microm diameter), and packed into a miniature column (e.g., 10 x 4.0 mm, 0.126 ml). Twelve pyridylaminated oligosaccharides were applied to the column through a 2-ml sample loop, and their elution patterns were monitored by fluorescence. The volume of the elution front (V) determined graphically for each sample was compared with that obtained in the presence of an excess amount of hapten saccharide, lactose (V0); and the dissociation constant, Kd, was calculated according to the literature [K. Kasai, Y. Oda, M. Nishikawa, S. Ishii, J. Chromatogr. 376 (1986) 33]. This system also proved to be useful for an inverse confirmation; that is, application of galectins to an immobilized glycan column (in the present case, asialofetuin was immobilized on Sepharose 4 Fast Flow), and the elution profiles were monitored by fluorescence based on tryptophan. The relative affinity of various galectins for asialofetuin could be easily compared in terms of the extent of retardation. The newly constructed system proved to be extremely versatile. It enabled rapid (analysis time 12 min/cycle) and sensitive (20 nM for pyridylaminated derivatives, and 1 microg/ml for protein) analyses of lectin-carbohydrate interactions. It should become a powerful tool for elucidation of biomolecular interactions, in particular for functional analysis of a large number of proteins that should be the essential issues of post-genome projects.

  19. Rapid and Sensitive PCR-Dipstick DNA Chromatography for Multiplex Analysis of the Oral Microbiota

    PubMed Central

    Niwa, Kousuke; Kawase, Mitsuo; Tanner, Anne C. R.; Takahashi, Nobuhiro

    2014-01-01

    A complex of species has been associated with dental caries under the ecological hypothesis. This study aimed to develop a rapid, sensitive PCR-dipstick DNA chromatography assay that could be read by eye for multiplex and semiquantitative analysis of plaque bacteria. Parallel oligonucleotides were immobilized on a dipstick strip for multiplex analysis of target DNA sequences of the caries-associated bacteria, Streptococcus mutans, Streptococcus sobrinus, Scardovia wiggsiae, Actinomyces species, and Veillonella parvula. Streptavidin-coated blue-colored latex microspheres were to generate signal. Target DNA amplicons with an oligonucleotide-tagged terminus and a biotinylated terminus were coupled with latex beads through a streptavidin-biotin interaction and then hybridized with complementary oligonucleotides on the strip. The accumulation of captured latex beads on the test and control lines produced blue bands, enabling visual detection with the naked eye. The PCR-dipstick DNA chromatography detected quantities as low as 100 pg of DNA amplicons and demonstrated 10- to 1000-fold higher sensitivity than PCR-agarose gel electrophoresis, depending on the target bacterial species. Semiquantification of bacteria was performed by obtaining a series of chromatograms using serial 10-fold dilution of PCR-amplified DNA extracted from dental plaque samples. The assay time was less than 3 h. The semiquantification procedure revealed the relative amounts of each test species in dental plaque samples, indicating that this disposable device has great potential in analysis of microbial composition in the oral cavity and intestinal tract, as well as in point-of-care diagnosis of microbiota-associated diseases. PMID:25485279

  20. Analysis of vitamin D and its metabolites using thermospray liquid chromatography/mass spectrometry.

    PubMed

    Watson, D; Setchell, K D; Ross, R

    1991-07-01

    A new method is described for the analysis of vitamin D and its metabolites utilizing thermospray (TSP) mass spectrometry as an on-line detector for high performance liquid chromatography. Ionization conditions were optimized for use with isocratic reversed phase chromatography. TSP mass spectrometry was employed in series with a UV absorbance detector to facilitate comparisons between the two methods of detection. Positive ion TSP mass spectra were recorded for vitamin D2, vitamin D3, 25-hydroxyvitamin D3 (25(OH)D3), 1,25-dihydroxyvitamin D3 (1,25(OH)2D3) and 24,25-dihydroxyvitamin D3 (24,25(OH)2D3). The spectra contained protonated molecular ions, ammonium adduct ions and fragment ions due to the loss of one or more molecules of water. A comparison of quantitative precision was made by determining UV absorbance and TSP standard curves for vitamin D3 using two different methods: (1) External standard method with post-column (post UV detector) addition of ammonium acetate. (2) As (1) but using the method of internal standards with a closely eluting internal standard (vitamin D2). In each case the quantitative precision (correlation coefficient) for UV absorbance detection was superior owing to intrinsic instability of the TSP ion beam. A stable isotopically labelled internal standard was employed in the development of an assay for 1,25(OH)2D3. The assay was used to quantify in vitro enzymic conversion of 25(OH)D3 to 1,25(OH)2D3 in guinea pig and sheep renal mitochondrial incubations. TSP LC/MS was also applied to analysis of an extract of human blood plasma in which D3 and each of its principal metabolites were identified in a single analysis.

  1. Pseudo-absolute quantitative analysis using gas chromatography - Vacuum ultraviolet spectroscopy - A tutorial.

    PubMed

    Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Qiu, Changling; McNair, Harold M; Schug, Kevin A

    2017-02-08

    The vacuum ultraviolet detector (VUV) is a new non-destructive mass sensitive detector for gas chromatography that continuously and rapidly collects full wavelength range absorption between 120 and 240 nm. In addition to conventional methods of quantification (internal and external standard), gas chromatography - vacuum ultraviolet spectroscopy has the potential for pseudo-absolute quantification of analytes based on pre-recorded cross sections (well-defined absorptivity across the 120-240 nm wavelength range recorded by the detector) without the need for traditional calibration. The pseudo-absolute method was used in this research to experimentally evaluate the sources of sample loss and gain associated with sample introduction into a typical gas chromatograph. Standard samples of benzene and natural gas were used to assess precision and accuracy for the analysis of liquid and gaseous samples, respectively, based on the amount of analyte loaded on-column. Results indicate that injection volume, split ratio, and sampling times for splitless analysis can all contribute to inaccurate, yet precise sample introduction. For instance, an autosampler can very reproducibly inject a designated volume, but there are significant systematic errors (here, a consistently larger volume than that designated) in the actual volume introduced. The pseudo-absolute quantification capability of the vacuum ultraviolet detector provides a new means for carrying out system performance checks and potentially for solving challenging quantitative analytical problems. For practical purposes, an internal standardized approach to normalize systematic errors can be used to perform quantitative analysis with the pseudo-absolute method.

  2. Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

    SciTech Connect

    Owens, J; Hok, S; Alcaraz, A; Koester, C

    2008-11-13

    Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.

  3. Electron capture gas-liquid chromatographic study of metabolites produced by some arthritic transudate-associated organisms in vitro and in vivo in rabbit models.

    PubMed

    Brooks, J B; Melton, A R

    1978-10-01

    Computerized, frequency-pulsed, modulated electron capture gas-liquid chromatography was used to study the acid metabolites produced in vitro in fetal calf serum and in vivo in an animal chamber model. Several strains of Diplostreptococcus agalactiae, Propionibacterium acnes, Staphylococcus aureus, and Streptococcus serogroups A, B, and G were studied. All of these organisms have been reported to be associated with arthritic transudates in humans. Metabolites were detected by this method from derivatized extracts of both spent fetal calf serum and chamber fluids. Since there was little host response to the organisms cultured in the chambers, it is highly probable that the products detected represent metabolites produced in an in vivo type of environment. The metabolic patterns were reproducible and exhibited many similarities in vitro and in vivo. Production of the acids detected was reproducible, and these acids were useful identification markers. The data support published reports (J. B. Brooks, C. C. Alley, and J. A. Liddle, Anal. Chem. 46: 1930-1934, 1974; J. B. Brooks, G. Choudhary, R. B. Craven, D. Edman, C. C. Alley, and J. A. Liddle, J. Clin. Microbiol. 5:625-628, 1977; J. B. Brooks, R. B. Craven, A. R. Melton, and C. C. Alley, in H. H. Johnson and W. B. Newson, ed., Second International Symposium on Rapid Methods and Automation on Microbiology, 1976; J. B. Brooks, R. B. Craven, D. Schlossberg, C. C. Alley, and F. M. Pitts, J. Clin. Microbiol. 8:203-208, 1978; J. B. Brooks, D. S. Kellogg, C. C. Alley, H. B. Short, and H. H. Handsfield, J. Infect. Dis. 129:660-668, 1974) that bacterial metabolites might be detectable in diseased body fluids. The growth characteristics of the organisms in the animal model and fetal calf serum are discussed, and a moderately priced computer for performing data manipulations is evaluated.

  4. Acoustic probe for the characterization of solid-gas- liquid slurries

    NASA Astrophysics Data System (ADS)

    Norato, Michael Anthony

    1999-10-01

    The development of nuclear weapons technology during the Cold War Era has left a legacy of large quantities of radioactive waste which are stored throughout the US Department of Energy (US DOE) Nuclear Weapons Complex. During the proposed remediation stages of processing, it will be necessary to characterize and monitor these waste slurries by remote methods. Acoustic probes have shown promise because of their non- intrusive nature and ability to penetrate optically opaque slurries. A forward theory for the acoustic response in both dilute and concentrated solid liquid slurries is developed. It is based on ensemble averaging of the equations of motion in the solid and liquid phases to obtain expressions for the ``effective properties'' of the slurry mixture in terms of coefficients which appear in the equations of motion for the solid particle. The attenuations predicted from the theory are in generally good agreement with the experimental data obtained by Toneburst and Pulse/FFT data acquisition methods for solid-liquid slurries of soda-lime glass particles of 14.9 μm and 65 μm mean radius and polystyrene particles of 79 gm radius at concentrations ranging from 5% to 50% solids by volume. The forward theory is readily extended to systems containing more than one dispersed phase, such as particles and gas bubbles, and the theory predictions are observed to be in good agreement with preliminary attenuation data obtained in solid-gas-liquid slurries of soda-lime glass particles of 14.9 gm mean radius at 5% and 10% by volume and gas bubbles ranging from approximately 25 μm to 150 μm radius at volume fractions on the order of 10-5. An inverse theory is also developed to determine the concentration and solids volume fraction distribution in a solid-liquid slurry given its experimentally obtained acoustic response. A Tikhonov scheme is employed to regularize the ill-posed integro-differential equations and solve them as a linear programming problem. Solution of the

  5. High Throughput Quantitative Analysis of Serum Proteins Using Glycopeptide Capture and Liquid Chromatography Mass Spectrometry

    SciTech Connect

    Zhang, Hui; Yi, Eugene C.; Li, Xiao-jun; Mallick, Parag; Kelly-Spratt, Karen S.; Masselon, Christophe D.; Camp, David G.; Smith, Richard D.; Kemp, Christopher J.; Aebersold, Reudi

    2005-02-01

    It is expected that the composition of the serum proteome can provide valuable information about the state of the human body in health and disease and that this information can be extracted via quantitative proteomic measurements. Suitable proteomic techniques need to be sensitive, reproducible, and robust to detect potential biomarkers below the level of highly expressed proteins, generate data sets that are comparable between experiments and laboratories, and have high throughput to support statistical studies. Here we report a method for high throughput quantitative analysis of serum proteins. It consists of the selective isolation of peptides that are N-linked glycosylated in the intact protein, the analysis of these now deglycosylated peptides by liquid chromatography electrospray ionization mass spectrometry, and the comparative analysis of the resulting patterns. By focusing selectively on a few formerly N-linked glycopeptides per serum protein, the complexity of the analyte sample is significantly reduced and the sensitivity and throughput of serum proteome analysis are increased compared with the analysis of total tryptic peptides from unfractionated samples. We provide data that document the performance of the method and show that sera from untreated normal mice and genetically identical mice with carcinogen-induced skin cancer can be unambiguously discriminated using unsupervised clustering of the resulting peptide patterns. We further identify, by tandem mass spectrometry, some of the peptides that were consistently elevated in cancer mice compared with their control littermates.

  6. Densitometric high performance thin-layer chromatography identification and quantitative analysis of psychotropic drugs.

    PubMed

    Maślanka, Anna; Krzek, Jan

    2005-01-01

    A thin-layer chromatography (TLC)-densitometry method has been developed to identify and quantify haloperidol, amitriptyline, sulpiride, promazine, fluphenazine, doxepin, diazepam, trifluoperazine, clonazepam, and chlorpromazine in selected psychotropic drugs. Separation was performed on precoated silica gel 60 F254 TLC plates. Chromatograms were developed in various mobile phases, and 8 of 30 tested phases were selected based on spot location and developing time. The identification and quantification were carried out based on ultraviolet densitometric measurements at chosen wavelengths. In addition to retention coefficients, the absorption spectra recorded directly from chromatograms were also used in qualitative analysis. Under established experimental conditions, high sensitivity of the method was achieved. The limit of detection ranged from 0.009 to 0.260 microg, depending on the wavelength selected for measuring. A satisfactory recovery, ranging from 92.99 to 104.70%, was achieved for individual constituents.

  7. Analysis for urinary catecholamines by liquid chromatography with amperometric detection: methodology and clinical interpretation of results.

    PubMed

    Moyer, T P; Jiang, N S; Tyce, G M; Sheps, S G

    1979-02-01

    A method is presented for the quantitative analysis of urinary unconjugated norepinephrine, epinephrine, and dopamine as discrete entities. The procedure requires initial purification of the specimen on aluminum oxide and a boric acid-gel. We used "high-performance" reversed-phase paired-ion chromatography, with a flow-through amperometric cell as the detector. The CV was 6% for determination of norepinephrine, 11% for epinephrine, and 6% for dopamine monitored at physiologic concentrations of these compounds in urine. In a population study, urine specimens from 117 normal pediatric and adult subjects, 85 hypertensive patients, and 22 patients with surgically proved pheochromocytoma were analyzed. The specificity of the method for detection of pheochromocytoma was 100%, with a sensitivity of 97%.

  8. Forensic analysis of ignitable liquids in fire debris by comprehensive two-dimensional gas chromatography.

    PubMed

    Frysinger, Glenn S; Gaines, Richard B

    2002-05-01

    The application of comprehensive two-dimensional gas chromatography (GC x GC) for the forensic analysis of ignitable liquids in fire debris is reported. GC x GC is a high resolution, multidimensional gas chromatographic method in which each component of a complex mixture is subjected to two independent chromatographic separations. The high resolving power of GC x GC can separate hundreds of chemical components from a complex fire debris extract. The GC x GC chromatogram is a multicolor plot of two-dimensional retention time and detector signal intensity that is well suited for rapid identification and fingerprinting of ignitable liquids. GC x GC chromatograms were used to identify and classify ignitable liquids, detect minor differences between similar ignitable liquids, track the chemical changes associated with weathering, characterize the chemical composition of fire debris pyrolysates, and detect weathered ignitable liquids against a background of fire debris pyrolysates.

  9. [Quantitative analysis of deacylgymnemic acid by high-performance liquid chromatography].

    PubMed

    Suzuki, K; Ishihara, S; Uchida, M; Komoda, Y

    1993-04-01

    A method of the quantitative analysis was established for the determination of deacylgymnemic acid (DAGA) in the alkaline hydrolysate of the sample containing gymnemic acids which are ingredients of Gymnema sylvestre R. BR. leaves, by means of high-performance liquid chromatography. This method was used for comparing the contents of gymnemic acids in various samples. The amount of gymnemic acids analyzed as DAGA in 70% ethanol extract of dry leaves was about twice that in hot water extract. The commercial health-supplemental foods of five companies were investigated for the contents of gymnemic acids as DAGA and there were large differences from 38 to 251 mg in the dosage per day recommended by each company.

  10. Analysis of the surface energy of pharmaceutical powders by inverse gas chromatography.

    PubMed

    Grimsey, Ian M; Feeley, Jane C; York, Peter

    2002-02-01

    The behavior of pharmaceutical solids, during either processing or use, can be noticeably affected by the surface energetics of the constituent particles. Several techniques exist to measure the surface energy, for example, sessile drop, and dynamic contact angle measurements. Inverse gas chromatography (IGC) is an alternative technique where the powder surface is characterized by the retention behavior of minute quantities of well-characterized vapors that are injected into a column containing the material of interest. Recently published articles using IGC on pharmaceutical powders have ranged from linking surface energetic data with triboelectric charging to studying the effect of surface moisture on surface energetics. Molecular modelling has also recently been used to explore the links between IGC data and the structural and chemical factors that influence surface properties, thereby achieving predictive knowledge regarding powder behavior during processing. In this minireview, the reported applications of IGC in the analysis of pharmaceutical powders are summarized and the major findings highlighted.

  11. High-speed, low-pressure gas chromatography-mass spectrometry for essential oil analysis.

    PubMed

    Poynter, Samuel D H; Shellie, Robert A

    2008-07-18

    Analysis of parsley and fennel essential oils was performed by using low-pressure gas chromatography-mass spectrometry (GC-MS). The low-pressure instrument configuration was achieved by fitting a GC-MS instrument with a 530microm I.D. capillary column and an appropriate capillary restrictor at the inlet of the column. Comparison of the performance of the low-pressure GC-MS setup was made with fast GC-MS using a narrow-bore capillary column. By comparing the two approaches side-by-side the benefits of low-pressure GC-MS for characterisation of moderately complex essential oils comprising less than 50 detectable components can be fully appreciated. Although efficiency is sacrificed, the improved sample capacity of the 530microm I.D. column leads to higher peak intensities and in-turn better mass spectral library matching thus providing highly satisfactory results.

  12. Mycolic Acid Analysis by High-Performance Liquid Chromatography for Identification of Mycobacterium Species

    PubMed Central

    Butler, W. Ray; Guthertz, Linda S.

    2001-01-01

    Mycobacterium tuberculosis is the etiologic agent of tuberculosis and can be accurately detected by laboratories using commercial genetic tests. Nontuberculosis mycobacteria (NTM) causing other mycobacterioses can be difficult to identify. The identification processes are confounded by an increasing diversity of newly characterized NTM species. The ubiquitous nature of NTM, combined with their potential to be opportunistic pathogens in immunocompromised as well as nonimmunodeficient patients, further complicates the problem of their identification. Since clinical case management varies depending on the etiologic agent, laboratories must identify the species in a timely manner. However, only a few identification methods can detect the species diversity within the Mycobacterium genus. Over the last decade, high-performance liquid chromatography analysis of the mycolic acids has become an accepted method for identification of mycobacteria. In this review, we assess its development and usefulness as an identification technique for Mycobacterium species. PMID:11585782

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

    PubMed

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

    2007-01-17

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

  14. Analysis of Iranian rosemary essential oil: application of gas chromatography-mass spectrometry combined with chemometrics.

    PubMed

    Jalali-Heravi, Mehdi; Moazeni, Rudabeh Sadat; Sereshti, Hassan

    2011-05-06

    This paper focuses on characterization of the components of Iranian rosemary essential oil using gas chromatography-mass spectrometry (GC-MS). Multivariate curve resolution (MCR) approach was used to overcome the problem of background, baseline offset and overlapping/embedded peaks in GC-MS. The analysis of GC-MS data revealed that sixty eight components exist in the rosemary essential oil. However, with the help of MCR this number was extended to ninety nine components with concentrations higher than 0.01%, which accounts for 98.23% of the total relative content of the rosemary essential oil. The most important constituents of the Iranian rosemary are 1,8-cineole (23.47%), α-pinene (21.74%), berbonone (7.57%), camphor (7.21%) and eucalyptol (4.49%).

  15. Multiresidue analysis of neonicotinoids by solid-phase extraction technique using high-performance liquid chromatography.

    PubMed

    Mohan, Chander; Kumar, Yogesh; Madan, Jyotsana; Saxena, Navneet

    2010-06-01

    For routine monitoring of pesticides, a multiresidue analysis through solid-phase extraction technique and using high-performance liquid chromatography (HPLC) in cotton seed cake (CSC) has been developed. Extraction of fortified samples was carried out with aqueous acetone under vacuum. The concentrated extract was loaded onto the solid-phase extraction units, preconditioned with acetonitrile. The extraction units were then washed with hexane and finally eluted with acetonitrile. The pesticide residues were determined using a multiresidue method by reversed-phase HPLC. The average percentage recoveries were found to range between 65.47% and 110% at spiking levels of 10 to 40 mg/kg. The method developed shows a healthy rate of recovery and can successfully be utilized for the extraction and screening of neonicotinoid residues in CSC. The detection limits for imidacloprid, acetamiprid, and thiacloprid using this method were found to be 5, 10, and 20 mg/kg, respectively.

  16. Analysis of Monosodium l-Glutamate in Food Products by High-Performance Thin Layer Chromatography.

    PubMed

    Krishna, Veni N; Karthika, D; Surya, Devi M; Rubini, Mf; Vishalini, M; Pradeepa, Yj

    2010-07-01

    A simple, fast, specific, and precise high-performance thin layer chromatography method has been developed for the estimation of monosodium l-glutamate (MSG) in food products. Aluminum plates precoated with silica gel 60 GF(254)were used as stationary phase and a mixture of methanol-chloroform-formic acid in the ratio 5:5:1 (v/v) as mobile phase. Quantification was carried out by postchromatographic derivatization using 1% ninhydrin solution, and the developed spots were scanned by using a densitometer in absorbance mode at 485 nM. The R(f)value of MSG was 0.64. The results of the analysis have been validated statistically and by the recovery studies. Linearity was observed in the concentration range of 400-1000 nG.

  17. Integrating Paper Chromatography with Electrochemical Detection for the Trace Analysis of TNT in Soil.

    PubMed

    Ryan, Patrick; Zabetakis, Daniel; Stenger, David A; Trammell, Scott A

    2015-07-14

    We report on the development of an electrochemical probe for the trace analysis of 2,4,6-trinitrotoluene (TNT) in soil samples. The probe is a combination of graphite electrodes, filter paper, with ethylene glycol and choline chloride as the solvent/electrolyte. Square wave chromatovoltammograms show the probes have a sensitivity for TNT of 0.75 nA/ng and a limit of detection of 100 ng. In addition, by taking advantage of the inherent paper chromatography step, TNT can be separated in both time and cathodic peak potential from 4-amino-dinitrotolene co-spotted on the probe or in soil samples with the presence of methyl parathion as a possible interferent.

  18. [Analysis of phthalates in plastic food-packaging bags by thin layer chromatography].

    PubMed

    Chen, Hui; Wang, Yuan; Zhu, Ruohua

    2006-01-01

    The method for simultaneous determination of four phthalates, namely dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) in plastic food-packaging bags by thin layer chromatography (TLC) was developed. The plastic food-packaging bags were extracted with ethanol by ultrasonication, then the mixture was filtrated through membrane (0.45 microm). The mixture of ethyl acetate-anhydrous ether-isooctane (1 : 4 : 15, v/v) was used as developing agent on the TLC silica gel plate for development. The filtered liquid was spotted on the TLC plate dealt by acetone, and detected with scanning wavelength of 275 nm and reference wavelength of 340 nm. The qualitative analysis of the phthalates was performed using the R(f) values of the chromatogram. The quantitative analysis was performed with external standard method. Good linearities were obtained for DMP, DEP, DBP and DEHP. The detection limits were 2.1 ng for DMP, 2.4 ng for DEP, 3.4 ng for DBP and 4.0 ng for DEHP. The relative standard deviations (RSDs) of the four phthalates were 2.8% - 3.5%. The recoveries of the four phthalate standards in real sample were 78.58% - 111.04%. The method presented has the advantages of high precision, high sensitivity, small sample size, and simple pretreatment . The method was used to detect the four phthalates in the food-packaging bags. The contents in real samples were close to the results by gas chromatography.

  19. Multidimensional analysis of poly(ethylene glycols) by size exclusion chromatography and dynamic surface tension detection

    PubMed

    Miller; Bramanti; Prazen; Prezhdo; Skogerboe; Synovec

    2000-09-15

    Substantial improvements in a multidimensional dynamic surface tension detector (DSTD) are presented. Rapid, online calibration and measurement of the dynamic surface tension for high-performance liquid chromatography separations is achieved. Dynamic surface tension is determined by measuring the differential pressure across the liquid-air interface of repeatedly growing and detaching drops. Continuous surface tension measurement throughout the entire drop growth (50 ms to 2 s) is achieved, for each eluting drop, providing insight into the kinetic behavior of molecular orientation processes at the liquid-air interface. Three-dimensional data are obtained, with surface tension first converted to surface pressure, which is plotted as a function of elution time axis versus drop time axis. Two key innovations will be reported. First, a novel calibration procedure is described and implemented. Differential pressure signals from three drops (mobile phase, standard in mobile phase, and analyte in mobile phase) are utilized to make the dynamic surface tension measurement, thereby eliminating the need for optical imaging, and viscosity and hydrostatic pressure corrections, as required by other methods. Only pressure signals from one mobile-phase drop and one standard drop pressure signal are required, while the analyte drop pressure signal is measured along the chromatographic time axis. Second, corrections for drop elongation are not required, because the drops are precisely detached by an air burst actuation method in a regime were the surface tension forces significantly dominate gravitational forces. Drops that would fall with a volume of approximately 10 microL due to gravity are precisely and repeatedly detached earlier at a volume of 2 microL. The sensitivity and unique selectivity of the DSTD opens up new possibilities in the analysis of small molecular weight polymers of varying degrees of surface activity, as illustrated for the size-exclusion chromatography

  20. Anion exchange SPE and liquid chromatography-tandem mass spectrometry in GHB analysis.

    PubMed

    Elian, Albert A; Hackett, Jeffery

    2011-12-01

    In this study, the extraction of γ-hydroxybutyrate (GHB) from urine using solid-phase extraction (SPE) is described. SPE was performed on anion exchange columns after samples of urine had been diluted with de-ionized water. After application of the diluted samples containing GHB-d(6) as an internal standard, the sorbent was washed with deionized water and methanol and dried. The GHB was eluted from the SPE column with a solvent consisting of methanol containing 6% glacial acetic acid. The eluent was collected, evaporated to dryness, and dissolved in mobile phase (100 μL) for analysis by liquid chromatography-tandem mass spectrometry (LC-MS/MS) in negative multiple reaction monitoring (MRM) mode. Liquid chromatography was performed in gradient mode employing a biphenyl column and a mobile phase consisting of acetontitrile (containing 0.1% formic acid) and 0.1% aqueous formic acid. The total run time for each analysis was less than 5 min. The limits of detection/quantification for this method were determined to be 50 and 100 ng/mL, respectively. The method was found to be linear from 500 ng/mL to 10,000 ng/mL (r(2)>0.995). The recovery of GHB was found to be greater than 75%. In this report, results of authentic urine samples analyzed for GHB by this method are presented. GHB concentrations in these samples were found to be range from less than 500 ng/mL to 5110 ng/mL.

  1. Electrophoretic concentration and sweeping-micellar electrokinetic chromatography analysis of cationic drugs in water samples.

    PubMed

    Wuethrich, Alain; Haddad, Paul R; Quirino, Joselito P

    2015-07-03

    Sample preparation by electrophoretic concentration, followed by analysis using sweeping-micellar electrokinetic chromatography, was studied as a green and simple analytical strategy for the trace analysis of cationic drugs in water samples. Electrophoretic concentration was conducted using 50 mmol/L ammonium acetate at pH 5 as acceptor electrolyte. Electrophoretic concentration was performed at 1.0 kV for 50 min and 0.5 kV and 15 min for purified and 10-fold diluted waste water samples, respectively. Sweeping-micellar electrokinetic chromatography was with 100 mmol/L sodium phosphate at pH 2, 100 mmol/L sodium dodecyl sulfate and 27.5%-v/v acetonitrile as separation electrolyte. The separation voltage was -20 kV, UV-detection was at 200 nm, and the acidified concentrate was injected for 36 s at 1 bar (or 72% of the total capillary length, 60 cm). Both purified water and 10-fold diluted waste water exhibited a linear range of two orders of concentration magnitude. The coefficient of determination, and intra- and interday repeatability were 0.991-0.997, 2.5-6.2, and 4.4-9.7%RSD (n=6), respectively, for purified water. The values were 0.991-0.997, 3.4-7.1, and 8.7-9.8%RSD (n=6), correspondingly, for 10-fold diluted waste water. The method detection limit was in the range from 0.04-0.09 to 1.20-6.97 ng/mL for purified and undiluted waste water, respectively.

  2. Direct analysis of opiates in urine by liquid chromatography-tandem mass spectrometry.

    PubMed

    Edinboro, Leslie E; Backer, Ronald C; Poklis, Alphonse

    2005-10-01

    A method for the direct analysis of 10 opiate compounds in urine was developed using liquid chromatography-mass spectrometry-mass spectrometry (LC-MS-MS) with electrospray ionization interface (ESI). Opiates included were morphine-3-P-glucuronide, morphine-6--glucuronide, morphine, oxymorphone, hydromorphone, norcodeine, codeine, oxycodone, 6-monoacetylmorphine (6MAM), and hydrocodone. Urine samples were prepared by centrifugation to remove large particles and direct injection into the LC-MS-MS. Separation and detection of all compounds was accomplished within 6 min. Linearity was established for all opiates except 6MAM from 50 ng/mL to 10,000 ng/mL; 6MAM from 0.25 ng/mL to 50 ng/mL with all correlation coefficients (r) > 0.99. Interrun precision (%CV) ranged from 1.1% to 16.7%, and intrarun precision ranged from 1.3% to 16.3%. Accuracy (% bias) ranged from -7.3% to 13.6% and -8.5% to 11.8 for inter- and intrarun, respectively. Eighty-nine urine samples previously analyzed by gas chromatography-MS were re-analyzed by the LC-MS-MS method. The qualitative results found an 88% agreement for negative samples between the two methods and 94% for positive samples. The LC-MS-MS method identified 19 samples with additional opiates in the positive samples. Overall, the direct injection LC-MS-MS method performed well and permitted the rapid analysis of urine samples for several opiates simultaneously without extensive sample preparation.

  3. Cluster analysis for the systematic grouping of genuine cocoa butter and cocoa butter equivalent samples based on triglyceride patterns.

    PubMed

    Buchgraber, Manuela; Ulberth, Franz; Anklam, Elke

    2004-06-16

    The triglyceride profile of cocoa butters (CBs) from different geographical origins, varieties, growing seasons, and a number of cocoa butter equivalents (CBEs) was determined by capillary gas liquid chromatography. Hierarchical cluster analysis was applied to the five main triglycerides of the samples for the ability to find natural groupings among (a) CBs of various provenance and (b) CBE samples of different types. The samples were clustered using Ward's method, and the similarity values of the linkages were represented by dendrograms. The five triglycerides contained adequate information to obtain a meaningful sample differentiation. This information can be used to assess the purity and the origin of the CB sample examined.

  4. Trenbolone acetate and trenbolone: trace analysis in animal chow, wastewater and human urine by high pressure liquid chromatography and electron capture gas chromatography.

    PubMed

    Holder, C L; Blakemore, W M; Bowman, M C

    1979-02-01

    Analytical methodology is described for determining residues of the synthetic anabolic steroid trenbolone acetate (TBA) and its hydrolysis product trenbolone (TBOH) in admixture in animal chow, human urine, and wastewater. Benzene extracts of the substrates are subjected to liquid-liquid partitioning, further cleanup on a column of silica gel, and direct analysis by high pressure liquid chromotography or derivatization with pentafluoropropionic anhydride and analysis by electron capture gas chromatography. Satisfactory recoveries were obtained with both compounds from all three substrates. Residue levels of TBA and TBOH as low as 0.32 and 0.04 ppm, respectively, could be detected in chow; about 0.6 ppb of each compound could be detected in urine and wastewater. Thin layer chromatographic behavior of the two compounds in 7 solvent systems and other ancillary analytical data are also presented.

  5. Separation of Caffeine from Beverages and Analysis Using Thin-Layer Chromatography and Gas Chromatography-Mass Spectrometry

    ERIC Educational Resources Information Center

    Torres y Torres, Janelle L.; Hiley, Shauna L.; Lorimor, Steven P.; Rhoad, Jonathan S.; Caldwell, Benjamin D.; Zweerink, Gerald L.; Ducey, Michael

    2015-01-01

    The Characterization and Analysis of a Product (CAP) project is used to introduce first-semester general chemistry students to chemical instrumentation through the analysis of caffeine-containing beverage products. Some examples of these products have included coffee, tea, and energy drinks. Students perform at least three instrumental experiments…

  6. Identification and Quantification of Pesticides in Environmental Waters With Solid Phase Microextraction and Analysis Using Field-Portable Gas Chromatography-Mass Spectrometry

    DTIC Science & Technology

    2004-06-10

    Microextraction and Analysis using Field-Portable Gas Chromatography-Mass Spectrometry Name of Candidate: CPT Michael J. Nack...in the thesis manuscript entitled: Identification and Quantification of Pesticides in Environmental Waters with Solid Phase Microextraction ...Pesticides in Environmental Waters with Solid Phase Microextraction and Analysis using Field-Portable Gas Chromatography-Mass Spectrometry

  7. [Analysis of cis-9, trans-11-conjugated linoleic acid in milk fat by capillary gas chromatography].

    PubMed

    Wang, Xiaojing; Shen, Xiangzhen; Han, Hangru; Zhao, Ruqian; Chen, Jie

    2006-11-01

    Conjugated linoleic acid (CLA) is a term representing a mixture of positional and geometric isomers of octadecadienoic acid with a conjugated double bond system. Conjugated linoleic acid has attracted a great deal of interest among nutritionists because it is a natural fat component that appears to have a number of health improvement properties. The cis-9, trans-11-CLA is the major CLA isomer found in dairy products accounting for 75% to 90% of the total CLA in milk fat. A capillary gas chromatographic method equipped with a flame ionization detector for the analysis of the cis-9, trans-11-CLA in milk fat was developed. The cis-9, trans-11-CLA was extracted with hexane-isopropanol, methylated with methanol-sodium methylate and cis-9, trans-11-CLA was separated and quantified using gas chromatography. Retention time of the peaks was used for qualitative analysis, while external standard method was used for quantitative analysis. The recovery of the cis-9, trans-11-CLA was 100.26%. The relative standard deviation was 1.9% (n = 6). This method presented is advantageous for high precision, high sensitivity analysis with smaller sample size and simpler pretreatment. It would be of significance for analyzing the contents of other fatty acids in the milk and milk products.

  8. Comparison of ultra-high performance supercritical fluid chromatography and ultra-high performance liquid chromatography for the analysis of pharmaceutical compounds.

    PubMed

    Grand-Guillaume Perrenoud, Alexandre; Veuthey, Jean-Luc; Guillarme, Davy

    2012-11-30

    Currently, columns packed with sub-2 μm particles are widely employed in liquid chromatography but are scarcely used in supercritical fluid chromatography. The goal of the present study was to compare the performance, possibilities and limitations of both ultra-high performance liquid chromatography (UHPLC) and ultra-high performance supercritical fluid chromatography (UHPSFC) using columns packed with sub-2 μm particles. For this purpose, a kinetic evaluation was first performed, and van Deemter curves and pressure plots were constructed and compared for columns packed with hybrid silica stationary phases composed of 1.7 and 3.5 μm particles. As expected, the kinetic performance of the UHPSFC method was significantly better than that of the UHPLC. Indeed, the h(min) values were in the same range with both strategies and were between 2.2 and 2.8, but u(opt) was increased by a factor of >4 in UHPSFC conditions. Another obvious advantage of UHPSFC over UHPLC is related to the generated backpressure, which is significantly lower in the presence of a supercritical or subcritical fluid. However, the upper pressure limit of the UHPSFC system was only ∼400 bar vs. ∼1000 bar in the UHPLC system, which prevents the use of highly organic mobile phases at high flow rates in UHPSFC. Second, the impact of reducing the particle size (from 3.5 to 1.7 μm) was evaluated in both UHPLC and UHPSFC conditions. The effect of frictional heating on the selectivity was demonstrated in UHPLC and that of fluid density or decompression cooling was highlighted in UHPSFC. However, in both cases, a change in selectivity was observed for only a limited number of compounds. Third, various types of column chemistries packed with 1.7 μm particles were evaluated in both UHPLC and UHPSFC conditions using a model mixture of acidic, neutral and basic compounds. It has been shown that more drastic changes in selectivity were obtained using UHPSFC columns compared to those obtained by changing

  9. Chemical Speciation Analysis of Sports Drinks by Acid-Base Titrimetry and Ion Chromatography: A Challenging Beverage Formulation Project

    ERIC Educational Resources Information Center

    Drossman, Howard

    2007-01-01

    Students have standardized a sodium hydroxide solution and analyzed commercially available sports drinks by titrimetric analysis of the triprotic citric acid, dihydrogen phosphate, and dihydrogen citrate and by ion chromatography for chloride, total phosphate and citrate. These experiments are interesting examples of analyzing real-world food and…

  10. RAPID ANALYSIS OF CYANURIC ACID IN SWIMMING POOL WATERS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY USING POROUS GRAPHITIC CARBON

    EPA Science Inventory

    An innovative approach is presented for reducing analysis times of cynuric acid in swimming pool waters by high performance liquid chromatography (HPLC). The HPLC method exploits the unique selectivity of porous graphitic carbon (PGC) to fully resolve within 10 minutes cyanuric ...

  11. RAPID ANALYSIS OF CYNANURIC ACID IN SWIMMING POOL WATERS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY USING POROUS GRAPHITIC CARBON COLUMN

    EPA Science Inventory

    An innovative approach is presented for reducing analysis times of cyanuric acid in swimming pool waters by high performance liquid chromatography (HPLC). The HPLC method exploits the unique selectivity of porous graphitic carbon (PGC) to fully resolve cyanuric acid from other p...

  12. ISOTOPE DILUTION ANALYSIS OF BROMATE IN DRINKING WATER MATRIXES BY ION CHROMATOGRAPHY WITH INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRIC DETECTION

    EPA Science Inventory

    Bromate is a disinfection byproduct in drinking water which is formed during the ozonation of source water containing bromide. This paper described the analysis of bromate via ion chromatography-inductively coupled plasma mass spectrometry. The separation of bromate from interfer...

  13. A Laboratory Experiment in Pharmaceutical Analysis: Determination of Drugs of Abuse in Human Urine by Thin-Layer Chromatography.

    ERIC Educational Resources Information Center

    Bailey, Leonard C.

    1979-01-01

    An experiment is described that was developed for a course in Inorganic and Analytical Pharmaceutical Chemistry at Rutgers University to provide pharmacy students with practical experience in the thin-layer chromatography used for the analysis of urine to monitor patient compliance with drug abuse treatment programs. (JMD)

  14. ANALYSIS OF TRACE-LEVEL ORGANIC COMBUSTION PROCESS EMISSIONS USING NOVEL MULTIDIMENSIONAL GAS CHROMATOGRAPHY-MASS SPECTROMETRY PROCEDURES

    EPA Science Inventory

    The paper discusses the analysis of trace-level organic combustion process emissions using novel multidimensional gas chromatography-mass spectrometry (MDGC-MS) procedures. It outlines the application of the technique through the analyses of various incinerator effluent and produ...

  15. Analysis of naphthenic acid mixtures as pentafluorobenzyl derivatives by gas chromatography-electron impact mass spectrometry.

    PubMed

    Gutierrez-Villagomez, Juan Manuel; Vázquez-Martínez, Juan; Ramírez-Chávez, Enrique; Molina-Torres, Jorge; Trudeau, Vance L

    2017-01-01

    In this study, we report for the first time the efficiency of pentafluorobenzyl bromide (PFBBr) for naphthenic acid (NA) mixtures derivatization, and the comparison in the optimal conditions to the most common NAs derivatization reagents, BF3/MeOH and N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA). Naphthenic acids are carboxylic acid mixtures of petrochemical origin. These compounds are important for the oil industry because of their corrosive properties, which can damage oil distillation infrastructure. Moreover, NAs are commercially used in a wide range of products such as paint and ink driers, wood and fabric preservatives, fuel additives, emulsifiers, and surfactants. Naphthenic acids have also been found in sediments after major oils spills in the United States and South Korea. Furthermore, the toxicity of the oil sands process-affected water (OSPW), product of the oil sands extraction activities in Canada's oil sands, has largely been attributed to NAs. One of the main challenges for the chromatographic analysis of these mixtures is the resolution of the components. The derivatization optimization was achieved using surface response analysis with molar ratio and time as factors for derivatization signal yield. After gas chromatography-electron impact mass spectrometry (GC/EIMS) analysis of a mixture of NA standards, it was found that the signal produced by PFB-derivatives was 2.3 and 1.4 times higher than the signal produced by methylated and MTBS-derivatives, respectively. The pentafluorobenzyl derivatives have a characteristic fragment ion at 181m/z that is diagnostic for the differentiation of carboxylic and non-carboxylic acid components within mixtures. In the analysis of a Sigma and a Merichem derivatized oil extract NA mixtures, it was found that some peaks lack the characteristic fragment ion; therefore they are not carboxylic acids. Open column chromatography was used to obtain a hexane and a methanol fraction of the Sigma and

  16. Free amino acids analysis by liquid chromatography with tandem mass spectrometry in several botanicals with antioxidant character.

    PubMed

    Moldoveanu, Serban C; Zhu, Jeff; Qian, Nancy

    2015-07-01

    A novel method based on liquid chromatography with tandem mass spectrometry for the analysis of 19 amino acids in plant materials is described. For the analysis, the plant material is extracted with 0.1 N hydrochloric acid with internal standards present in the extraction solution. The filtered extracts are injected using no clean-up into the liquid chromatographic system coupled with a triple-quadrupole tandem mass spectrometer with an electrospray ionization source. The analytes are separated using ion pair chromatography on a reversed-phase column. The detection is performed in multiple-reaction monitoring positive-ion mode. Quantitation is obtained using calibrations. The validated procedure has been applied for the analysis of amino acids in 18 samples of plant material including botanicals with antioxidant character. The analysis requires 16 min separation time, has excellent precision and accuracy allowing amino acid analysis in a wide range of concentrations.

  17. Headspace Analysis of Philippine Civet Coffee Beans Using Gas Chromatography-Mass Spectrometry and Electronic Nose

    NASA Astrophysics Data System (ADS)

    Ongo, E.; Sevilla, F.; Antonelli, A.; Sberveglieri, G.; Montevecchi, G.; Sberveglieri, V.; de Paola, E. L.; Concina, I.; Falasconi, M.

    2011-11-01

    Civet coffee, the most expensive and best coffee in the world, is an economically important export product of the Philippines. With a growing threat of food adulteration and counterfeiting, a need for quality authentication is essential to protect the integrity and strong market value of Philippine civet coffee. At present, there is no internationally accepted method of verifying whether a bean is an authentic civet coffee. This study presented a practical and promising approach to identify and establish the headspace qualitative profile of Philippine civet coffee using electronic nose (E-nose) and gas chromatography-mass spectrometry (GC-MS). E-nose analysis revealed that aroma characteristic is one of the most important quality indicators of civet coffee. The findings were supported by GC-MS analysis. Principal component analysis (PCA) exhibited a clearly separated civet coffees from their control beans. The chromatographic fingerprints indicated that civet coffees differed with their control beans in terms of composition and concentration of individual volatile constituents.

  18. Ultra-high performance liquid chromatography tandem mass spectrometry for comprehensive analysis of urinary acylcarnitines.

    PubMed

    Zuniga, Azeret; Li, Liang

    2011-03-09

    We report an enabling mass spectrometric method for the analysis of lipid metabolites in order to define better the lipid metabolome in terms of chemical diversity and generate fragment ion spectra of these metabolites as a potential resource for unknown metabolite identification. This work focuses on the analysis of one important class of lipid metabolites, the acylcarnitines. Current analytical methods have only detected and identified a limited number of these metabolites. The method described herein provides the most comprehensive acylcarnitine profile in urine of healthy individuals up to date. It involves an optimized solid phase extraction technique for selective analyte extraction using cartridges containing both lipophilic and cation-exchange properties. The captured analytes are then subjected to ultra-high performance liquid chromatography (UPLC) separation, followed by tandem mass spectrometry (MS/MS) analysis using information-dependent acquisitions and selected reaction monitoring (SRM). The urine of six healthy individuals was analyzed using this method. A total of 355 acylcarnitines were detected; only 43 of them have been previously reported in the urine of healthy individuals. Detection of this large number of acylcarnitines illustrates the great diversity of the lipid metabolome as well as the usefulness of the method for profiling acylcarnitines. Furthermore, the MS/MS spectra of the 355 acylcarnitines will be uploaded to a public human metabolome database as a mass spectrometric resource for unknown metabolite identification.

  19. Analysis of petroleum-contaminated soils by thin-layer chromatography with flame ionization detection

    SciTech Connect

    Napolitano, G.E.; Richmond, J.E.

    1995-12-31

    Thin-layer chromatography with flame ionization detection (TLC-FID) offers a rapid and accurate method for the analysis of non-volatile organic materials. If the instrument is properly calibrated and the operational parameters are standardized, TLC-FID permits a rapid and accurate quantification of total petroleum hydrocarbons (TPH), and offers the possibility of separation and quantification of the major types of components in petroleum and petroleum products. Petroleum hydrocarbons from contaminated soil were extracted overnight with a mixture of chloroform:methanol. The analysis method consisted of spotting a small volume of the samples on silica-coated quartz rods followed by three chromatographic developments in solvent systems of increasing polarities. This series of chromatographic steps resulted in the complete separation of aliphatic hydrocarbons, aromatic hydrocarbons, resins and asphaltenes, starting from mixtures of the materials. This method also allows the quantification of aromatic and aliphatic hydrocarbons without interference from biogenic lipids present in the soil. A simplified version of this method allowed excellent separation of aliphatics plus aromatics (forming a single peak) from resins and asphaltenes. The instrument provides the complete analysis of 10 samples in about one hour after extraction. This rapid analytical tool is especially suited for synoptic studies or for the screening of a large number of samples prior to the consideration of more detailed and costly analyses.

  20. Identification of Dactylopius cochineal species with high-performance liquid chromatography and multivariate data analysis.

    PubMed

    Serrano, Ana; Sousa, Micaela; Hallett, Jessica; Simmonds, Monique S J; Nesbitt, Mark; Lopes, João A

    2013-10-21

    Identification of American cochineal species (Dactylopius genus) can provide important information for the study of historical works of art, entomology, cosmetics, pharmaceuticals and foods. In this study, validated species of Dactylopius, including the domesticated cochineal D. coccus, were analysed by high-performance liquid chromatography with a diode array detector (HPLC-DAD) and submitted to multivariate data analysis, in order to discriminate the species and hence construct a reference library for a wide range of applications. Principal components analysis (PCA) and partial least squares discriminant analysis (PLSDA) models successfully provided accurate species classifications. This library was then applied to the identification of 72 historical insect specimens of unidentified species, mostly dating from the 19th century, and belonging to the Economic Botany Collection, Royal Botanic Gardens, Kew, England. With this approach it was possible to identify anomalies in how insects were labelled historically, as several of them were revealed not to be cochineal. Nevertheless, more than 85% of the collection was determined to be species of Dactylopius and the majority of the specimens were identified as D. coccus. These results have shown that HPLC-DAD, in combination with suitable chemometric methods, is a powerful approach for discriminating related cochineal species.

  1. Toward Sensitive and Accurate Analysis of Antibody Biotherapeutics by Liquid Chromatography Coupled with Mass Spectrometry

    PubMed Central

    An, Bo; Zhang, Ming

    2014-01-01

    Remarkable methodological advances in the past decade have expanded the application of liquid chromatography coupled with mass spectrometry (LC/MS) analysis of biotherapeutics. Currently, LC/MS represents a promising alternative or supplement to the traditional ligand binding assay (LBA) in the pharmacokinetic, pharmacodynamic, and toxicokinetic studies of protein drugs, owing to the rapid and cost-effective method development, high specificity and reproducibility, low sample consumption, the capacity of analyzing multiple targets in one analysis, and the fact that a validated method can be readily adapted across various matrices and species. While promising, technical challenges associated with sensitivity, sample preparation, method development, and quantitative accuracy need to be addressed to enable full utilization of LC/MS. This article introduces the rationale and technical challenges of LC/MS techniques in biotherapeutics analysis and summarizes recently developed strategies to alleviate these challenges. Applications of LC/MS techniques on quantification and characterization of antibody biotherapeutics are also discussed. We speculate that despite the highly attractive features of LC/MS, it will not fully replace traditional assays such as LBA in the foreseeable future; instead, the forthcoming trend is likely the conjunction of biochemical techniques with versatile LC/MS approaches to achieve accurate, sensitive, and unbiased characterization of biotherapeutics in highly complex pharmaceutical/biologic matrices. Such combinations will constitute powerful tools to tackle the challenges posed by the rapidly growing needs for biotherapeutics development. PMID:25185260

  2. Gas Chromatography

    NASA Astrophysics Data System (ADS)

    Qian, Michael C.

    Gas chromatography (GC) has many applications in the analysis of food products. GC has been used for the determination of fatty acids, triglycerides, cholesterol, gases, water, alcohols, pesticides, flavor compounds, and many more. While GC has been used for other food components such as sugars, oligosaccharides, amino acids, peptides, and vitamins, these substances are more suited to analysis by high performance liquid chromatography. GC is ideally suited to the analysis of volatile substances that are thermally stable. Substances such as pesticides and flavor compounds that meet these criteria can be isolated from a food and directly injected into the GC. For compounds that are thermally unstable, too low in volatility, or yield poor chromatographic separation due to polarity, a derivatization step must be done before GC analysis. The two parts of the experiment described here include the analysis of alcohols that requires no derivatization step, and the analysis of fatty acids which requires derivatization. The experiments specify the use of capillary columns, but the first experiment includes conditions for a packed column.

  3. High resolution Dopplerimetry of correlated angular and quantum state-resolved CO(2) scattering dynamics at the gas-liquid interface.

    PubMed

    Perkins, Bradford G; Nesbitt, David J

    2010-11-14

    Full three dimensional (3D) translational distributions for quantum state-resolved scattering dynamics at the gas-liquid interface are presented for experimental and theoretical studies of CO(2) + perfluorinated surfaces. Experimentally, high resolution absorption profiles are measured as a function of incident (θ(inc)) and scattering (θ(scat)) angles for CO(2) that has been scattered from a 300 K perfluorinated polyether surface (PFPE) with an incident energy of E(inc) = 10.6(8) kcal mol(-1). Line shape analysis of the absorption profiles reveals non-equilibrium dynamics that are characterized by trapping-desorption (TD) and impulsive scattering (IS) components, with each channel simply characterized by an effective "temperature" that compares very well with previous results from rotational state analysis [Perkins and Nesbitt, J. Phys. Chem. A, 2008, 112, 9324]. From a theoretical perspective, molecular dynamics (MD) simulations of CO(2) + fluorinated self-assembled monolayer surface (F-SAMs) yield translational probability distributions that are also compared with experimental results. Trajectories are parsed by θ(scat) and J, with the results rigorously corrected by flux-to-density transformation and providing comparisons in near quantitative agreement with experiment. 3D flux and velocity distributions obtained from MD simulations are also presented to illustrate the role of in- and out-of-plane scattering.

  4. The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

    PubMed

    Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

    2014-03-01

    In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved.

  5. Two-column sequential injection chromatography--new approach for fast and effective analysis and its comparison with gradient elution chromatography.

    PubMed

    Chocholous, Petr; Satínský, Dalibor; Sklenárová, Hana; Solich, Petr

    2010-05-23

    This work presents novel approach in low-pressure chromatography flow systems--two-column Sequential Injection Chromatography (2-C SIC) and its comparison with gradient elution chromatography on the same instrument. The system was equipped with two different chromatographic columns (connected to selection valve in parallel design) for isocratic separation and determination of all components in composed anti-inflammatory pharmaceutical preparation (tablets). The sample was first injected on the first column of length 30 mm where less retained analytes were separated and then the sample was injected on the second column of length 10 mm where more retained analytes were separated. The SIC system was based on a commercial SIChrom manifold (8-port high-pressure selection valve and medium-pressure syringe pump with 4 mL reservoir) (FIAlab, USA) with two commercially available monolithic columns the "first column" Chromolith Flash RP-18e (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.) and the "second column" Chromolith RP-18e (10 mm x 4.6 mm i.d.) and CCD UV-vis detector USB 4000 with micro-volume 1.0 cm Z flow cell. Two mobile phases were used for analysis (one for each column). The mobile phase 1 used for elution of paracetamol, caffeine and salicylic acid (internal standard) was acetonitrile/water (10:90, v/v, the water part of pH 3.5 adjusted with acetic acid), flow rate was 0.9 mL min(-1) (volume 3.0 mL of mobile phase per analysis). The mobile phase 2 used for elution of propyphenazone was acetonitrile/water (30:70, v/v); flow rate was 1.2 mL min(-1) (volume 1.5 mL of mobile phase per analysis). Absorbance was monitored at 210 nm. Samples were prepared by dissolving of one tablet in 30% acetonitrile and 10 microL of filtered supernatant was injected on each column (2 x 10 microL). The chromatographic resolution between all compounds was >1.45 and analysis time was 5.5 min under the optimal conditions. Limits of detection were determined at 0.4 microg m

  6. Formation of iron complexs from trifluoroacetic acid based liquid chromatography mobile phases as interference ions in liquid chromatography/electrospray ionization mass spectrometric analysis

    SciTech Connect

    Shukla, Anil K.; Zhang, Rui; Orton, Daniel J.; Zhao, Rui; Clauss, Therese RW; Moore, Ronald J.; Smith, Richard D.

    2011-05-30

    Two unexpected singly charged ions at m/z 1103 and 944 have been observed in mass spectra obtained from electrospray ionization-mass spectrometric analysis of liquid chromatography effluents with mobile phases containing trifluoroacetic acid. Accurate mass measurement and tandem mass spectrometry studies revealed that these two ions are not due to any contamination from solvents and chemicals used for mobile and stationary phases or from the laboratory atmospheric environment. Instead these ions are clusters of trifluoroacetic acid formed in association with acetonitrile, water and iron from the stainless steel union used to connect the column with the electrospray tip and to apply high voltage; the molecular formulae are Fe+((OH)(H2O)2)9(CF3COOH)5 and Fe+((OH)(H2O)2)6 (CF3COOH)5.

  7. Rapid liquid chromatography for paralytic shellfish toxin analysis using superficially porous chromatography with AOAC Official Method 2005.06.

    PubMed

    Hatfield, Robert G; Turner, Andrew D

    2012-01-01

    The bioaccumulation of paralytic shellfish toxins in mussels, oysters, cockles, hard clams, razors, and king scallops is monitored in England, Scotland, and Wales by AOAC Official Method 2005.06 LC-with fluorescence detection (FLD). One of the commonly perceived disadvantages of using this method is the long turnaround time and low throughput in a busy laboratory environment. The chromatographic analysis of each sample typically utilizes a 15 min cycle time to achieve toxin oxidation product separation and column equilibration prior to subsequent analysis. A standard RP C18 analytical column, used successfully in recent years, achieves good separation with a long column lifetime. The analysis of a 40 sample qualitative screening batch takes approximately 18 h, including blanks, standards, and other QC samples. The availability of superficially porous column technology has offered the potential to reduce analysis time while retaining column performance on existing hardware. In this study, AOAC Official Method 2005.06 with LC-FLD was transferred to two different commercially available superficially porous columns, and the method performance characteristics were evaluated. Both columns separated all toxins adequately with cycle times less than half that of the existing method. Linearity for each toxin was acceptable up to two times the European maximum permitted limit of 800 microg di-HCl saxitoxin equivalent/kg flesh. LOD and LOQ values were substantially improved for the majority of toxins, with gonyautoxin 1&4 and neosaxitoxin showing up to a two- and fourfold improvement, respectively, depending on the column used. Quantification results obtained from parallel analysis of contaminated samples were acceptable on both columns. Comparative screen results gave a slight increase in the occurrence of contaminated samples, which was attributed to the improved detection limit for most toxins. Issues with rapidly increasing back pressure, however, were identified with both

  8. Recent advances in ultra-high performance liquid chromatography for the analysis of traditional chinese medicine

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Traditional Chinese medicines (TCMs) have been widely used for the prevention and treatment of various diseases for thousands of years in China. Ultra Performance Liquid Chromatography (UHPLC) is a relatively new technique offering new possibilities in liquid chromatography. This paper reviews recen...

  9. /Chromatography+RECOVERY=superresolution chromatography

    NASA Astrophysics Data System (ADS)

    Kosarev, E. L.; Muranov, K. O.

    2003-04-01

    A method for improving the resolution of the chromatographic analysis based on deriving the point-spread function of a chromatographic column, i.e., a chromatogram of an individual compound, is described. The system of two data sets, namely, a chromatogram of a substance analyzed and a point-spread function of a chromatographic column in combination with the noise statistics, makes it possible to use the RECOVERY signal-reconstruction software package described in paper by Gelfgat et al. (Comp. Phys. Commun. 74 (1993) 335). The proposed method has been tested by chromatography of bovine serum albumin using gel filtration. The resultant resolution exceeds that reached using high-performance liquid chromatography (with the cost of the instruments being lower by a factor of 15-20).

  10. Gas chromatography mass spectrometry computer analysis of volatile halogenated hydrocarbons in man and his environment--A multimedia environmental study.

    PubMed

    Barkley, J; Bunch, J; Bursey, J T; Castillo, N; Cooper, S D; Davis, J M; Erickson, M D; Harris, B S; Kirkpatrick, M; Michael, L C; Parks, S P; Pellizzari, E D; Ray, M; Smith, D; Tomer, K B; Wagner, R; Zweidinger, R A

    1980-04-01

    As part of a study to make a comparative analysis of selected halogenated compounds in man and the environmental media, a quantitative gas chromatography mass spectrometric analysis of the levels of the halogenated compounds found in the breath, blood and urine of an exposed population (Old Love Canal area, Niagara, New York) and their immediate environment (air and water) was undertaken. In addition, levels of halogenated hydrocarbons in air samples taken in the general Buffalo, Niagara Falls area were determined.

  11. Integrated CO2 capture-fixation chemistry via interfacial ionic liquid catalyst in laminar gas/liquid flow.

    PubMed

    Vishwakarma, Niraj K; Singh, Ajay K; Hwang, Yoon-Ho; Ko, Dong-Hyeon; Kim, Jin-Oh; Babu, A Giridhar; Kim, Dong-Pyo

    2017-03-06

    Simultaneous capture of carbon dioxide (CO2) and its utilization with subsequent work-up would significantly enhance the competitiveness of CO2-based sustainable chemistry over petroleum-based chemistry. Here we report an interfacial catalytic reaction platform for an integrated autonomous process of simultaneously capturing/fixing CO2 in gas-liquid laminar flow with subsequently providing a work-up step. The continuous-flow microreactor has built-in silicon nanowires (SiNWs) with immobilized ionic liquid catalysts on tips of cone-shaped nanowire bundles. Because of the superamphiphobic SiNWs, a stable gas-liquid interface maintains between liquid flow of organoamines in upper part and gas flow of CO2 in bottom part of channel. The intimate and direct contact of the binary reagents leads to enhanced mass transfer and facilitating reactions. The autonomous integrated platform produces and isolates 2-oxazolidinones and quinazolines-2,4(1H,3H)-diones with 81-97% yields under mild conditions. The platform would enable direct CO2 utilization to produce high-valued specialty chemicals from flue gases without pre-separation and work-up steps.

  12. Comprehensive study of the evolution of gas-liquid partitioning of aroma compounds during wine alcoholic fermentation.

    PubMed

    Morakul, Sumallika; Athes, Violaine; Mouret, Jean-Roch; Sablayrolles, Jean-Marie

    2010-09-22

    Calculating the gas-liquid partitioning of aromatic molecules during winemaking fermentation is essential to minimize the loss of aroma and to optimize the fermentation conditions. In this study, the effect of the main fermentation parameters on the partition coefficients (ki) of higher alcohols (2-methylpropan-1-ol and 3-methyl butan-1-ol) and esters (ethyl acetate, 3-methyl-1-butyl acetate, and 2-ethyl hexanoate) was assessed. The values of ki were first determined in synthetic media simulating must and wine. They varied considerably with both the hydrophobicity of the compound and the composition of the medium. Then, the effect of temperature on ki was quantified. The absence of any effect of gas composition was also established by replacing air with CO2. Finally, the impact of CO2 stripping was assessed by running specific fermentations in which the rate of CO2 production was kept constant by perfusion with assimilable nitrogen. These fermentations showed that in contrast to temperature and must composition, CO2 stripping did not change the gas-liquid partitioning of higher alcohols and esters.

  13. Spray formation in a quasiplanar gas-liquid mixing layer at moderate density ratios: A numerical closeup

    NASA Astrophysics Data System (ADS)

    Ling, Yue; Fuster, Daniel; Zaleski, Stéphane; Tryggvason, Grétar

    2017-01-01

    The three-dimensional development of instabilities and the subsequent spray formation in a gas-liquid mixing layer are important fundamental problems in the area of multiphase flows. It is highly desirable to visualize this detailed atomization process and to analyze the instabilities and mechanisms involved, and massive numerical simulations are required, in addition to experiment. Rapid development of numerical methods and computer technology in the past decade now allows large-scale three-dimensional direct numerical simulations of atomization to be performed. Nevertheless, the fundamental question, whether all the physical scales involved in the primary breakup process are faithfully resolved, has eluded researchers until now. In the present study, we conduct direct numerical simulations of spray formation in a gas-liquid mixing layer with state-of-the-art computational resources (using up to 4 ×109 cells and 16 384 cores), in order to obtain a high-fidelity numerical closeup of the detailed mechanisms of spray formation. We also aim to examine whether present computational resources are sufficient for a fully resolved direct numerical simulation of atomization.

  14. A New Method for Ultrasound Detection of Interfacial Position in Gas-Liquid Two-Phase Flow

    PubMed Central

    Coutinho, Fábio Rizental; Ofuchi, César Yutaka; de Arruda, Lúcia Valéria Ramos; Jr., Flávio Neves; Morales, Rigoberto E. M.

    2014-01-01

    Ultrasonic measurement techniques for velocity estimation are currently widely used in fluid flow studies and applications. An accurate determination of interfacial position in gas-liquid two-phase flows is still an open problem. The quality of this information directly reflects on the accuracy of void fraction measurement, and it provides a means of discriminating velocity information of both phases. The algorithm known as Velocity Matched Spectrum (VM Spectrum) is a velocity estimator that stands out from other methods by returning a spectrum of velocities for each interrogated volume sample. Interface detection of free-rising bubbles in quiescent liquid presents some difficulties for interface detection due to abrupt changes in interface inclination. In this work a method based on velocity spectrum curve shape is used to generate a spatial-temporal mapping, which, after spatial filtering, yields an accurate contour of the air-water interface. It is shown that the proposed technique yields a RMS error between 1.71 and 3.39 and a probability of detection failure and false detection between 0.89% and 11.9% in determining the spatial-temporal gas-liquid interface position in the flow of free rising bubbles in stagnant liquid. This result is valid for both free path and with transducer emitting through a metallic plate or a Plexiglas pipe. PMID:24858961

  15. Rapid removal of nitrobenzene in a three-phase ozone loaded system with gas-liquid-liquid

    USGS Publications Warehouse

    Li, Shiyin; Zhu, Jiangpeng; Wang, Guoxiang; Ni, Lixiao; Zhang, Yong; Green, Christopher T.

    2015-01-01

    This study explores the removal rate of nitrobenzene (NB) using a new gas-liquid-liquid (G-L-L) three-phase ozone loaded system consisting of a gaseous ozone, an aqueous solvent phase, and a fluorinated solvent phase (perfluorodecalin, or FDC). The removal rate of NB was quantified in relation to six factors including 1) initial pH, 2) initial NB dosage, 3) gaseous ozone dosage, 4) free radical scavenger, 5) FDC pre-aerated gaseous ozone, and 6) reuse of FDC. The NB removal rate is positively affected by the first three factors. Compared with the conventional gas-liquid (water) (G-L) two-phase ozonation system, the free radical scavenger (tertiary butyl alcohol) has much less influence on the removal rate of NB in the G-L-L system. The FDC loaded ozone acts as an ozone reservoir and serves as the main reactive phase in the G-L-L three-phase system. The reuse of FDC has little influence on the removal rate of NB. These experimental results suggest that the oxidation efficiency of ozonation in the G-L-L three-phase system is better than that in the conventional G-L two-phase system.

  16. Measurement of Gas-Liquid Two-Phase Flow in Micro-Pipes by a Capacitance Sensor

    PubMed Central

    Ji, Haifeng; Li, Huajun; Huang, Zhiyao; Wang, Baoliang; Li, Haiqing

    2014-01-01

    A capacitance measurement system is developed for the measurement of gas-liquid two-phase flow in glass micro-pipes with inner diameters of 3.96, 2.65 and 1.56 mm, respectively. As a typical flow regime in a micro-pipe two-phase flow system, slug flow is chosen for this investigation. A capacitance sensor is designed and a high-resolution and high-speed capacitance measurement circuit is used to measure the small capacitance signals based on the differential sampling method. The performance and feasibility of the capacitance method are investigated and discussed. The capacitance signal is analyzed, which can reflect the voidage variation of two-phase flow. The gas slug velocity is determined through a cross-correlation technique using two identical capacitance sensors. The simulation and experimental results show that the presented capacitance measurement system is successful. Research work also verifies that the capacitance sensor is an effective method for the measurement of gas liquid two-phase flow parameters in micro-pipes. PMID:25587879

  17. The Development of a Gas-Liquid Two-Phase Flow Sensor Applicable to CBM Wellbore Annulus.

    PubMed

    Wu, Chuan; Wen, Guojun; Han, Lei; Wu, Xiaoming

    2016-11-18

    The measurement of wellbore annulus gas-liquid two-phase flow in CBM (coalbed methane) wells is of great significance for reasonably developing gas drainage and extraction processes, estimating CBM output, judging the operating conditions of CBM wells and analyzing stratum conditions. Hence, a specially designed sensor is urgently needed for real-time measurement of gas-liquid two-phase flow in CBM wellbore annulus. Existing flow sensors fail to meet the requirements of the operating conditions of CBM wellbore annulus due to such factors as an inapplicable measurement principle, larger size, poor sealability, high installation accuracy, and higher requirements for fluid media. Therefore, based on the principle of a target flowmeter, this paper designs a new two-phase flow sensor that can identify and automatically calibrate different flow patterns of two-phase flows. Upon the successful development of the new flow sensor, lab and field tests were carried out, and the results show that the newly designed sensor, with a measurement accuracy of ±2.5%, can adapt to the operating conditions of CBM wells and is reliable for long-term work.

  18. Integrated CO2 capture-fixation chemistry via interfacial ionic liquid catalyst in laminar gas/liquid flow

    NASA Astrophysics Data System (ADS)

    Vishwakarma, Niraj K.; Singh, Ajay K.; Hwang, Yoon-Ho; Ko, Dong-Hyeon; Kim, Jin-Oh; Babu, A. Giridhar; Kim, Dong-Pyo

    2017-03-01

    Simultaneous capture of carbon dioxide (CO2) and its utilization with subsequent work-up would significantly enhance the competitiveness of CO2-based sustainable chemistry over petroleum-based chemistry. Here we report an interfacial catalytic reaction platform for an integrated autonomous process of simultaneously capturing/fixing CO2 in gas-liquid laminar flow with subsequently providing a work-up step. The continuous-flow microreactor has built-in silicon nanowires (SiNWs) with immobilized ionic liquid catalysts on tips of cone-shaped nanowire bundles. Because of the superamphiphobic SiNWs, a stable gas-liquid interface maintains between liquid flow of organoamines in upper part and gas flow of CO2 in bottom part of channel. The intimate and direct contact of the binary reagents leads to enhanced mass transfer and facilitating reactions. The autonomous integrated platform produces and isolates 2-oxazolidinones and quinazolines-2,4(1H,3H)-diones with 81-97% yields under mild conditions. The platform would enable direct CO2 utilization to produce high-valued specialty chemicals from flue gases without pre-separation and work-up steps.

  19. [Analysis of nine narcotics in urine by microemulsion electrokinetic chromatography-field samplified sample injection].

    PubMed

    Zhang, Yu; Li, Qin; Lu, Minghua; Zhang, Lan; Chen, Guonan; Cai, Zongwei

    2011-08-01

    A simple, sensitive and reproducible method using microemulsion electrokinetic chromatography (MEEKC)-field amplified sample injection (FASI) was developed for the analysis of nine narcotics (morphine, codeine, naloxone, heroin, thebaine, cocaine, pethidine, fentanyl and methadone) in urine. In the MEEKC method, sodium dodecyl sulfate (SDS), 1-butanol and ethyl acetate were used as surfactant, co-surfactant and organic solvent, respectively. The effects of the acidity and concentration of borate buffer, SDS, 1-butanol and ethyl acetate contents were investigated. The optimum concentrations (by mass fraction) of microemulsion system were 0.6% SDS, 1.2% 1-butanol, 0.6% ethyl acetate and 97.6% 10 mmol/L Na2B4O7 buffer (pH 9.5). The applied voltage was 25 kV. FASI was coupled with the MEEKC method to increase the sensitivity. Under the optimum conditions, the nine narcotics were baseline separated within 15 min and the detection limits (S/N = 3) were in the range of 0.3 - 8.0 microg/L. The spiked recoveries in urine samples were between 79.4% and 119.9% with the intraday relative standard deviations (RSDs) less than 5.5%. The developed method has been successfully applied to the analysis of methadone in the samples from in vitro metabolism study.

  20. Nano-liquid chromatography analysis of dansylated biogenic amines in wines.

    PubMed

    Hernández-Borges, Javier; D'Orazio, Giovanni; Aturki, Zeineb; Fanali, Salvatore

    2007-04-20

    In this work, the simultaneous analysis of 10 biogenic amines (ethanolamine, methylamine, tryptamine, 2-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine and spermine) in wines by nano-liquid chromatography (nano-LC) using UV detection and a capillary bidentate C(18) column of 100 microm I.D. is proposed. The 10 selected amines, which are the most important to be determined in wine samples, were derivatized with dansyl-chloride (Dns-Cl) previous to their nano-LC determination. Excess of the derivatizing agent as well as other components of the samples were eliminated by the use of an on-line cleaning step employing a C(18) trapping column which also provided a pre-concentration effect. The mobile phase composed of acetonitrile, water, acetic acid and triethylamine (TEA) mixture was pumped at a low flow rate (634 nL/min). Limits of detection (LODs) achieved ranged between 18.3 and 48.3 ng/mL; while calibration curves showed good linearity (R(2)>0.9924). The method was applied to the analysis of this group of amines in white and red wine samples after suitable treatment with polyvinylpyrrolidone (PVP) and extraction with C(18) cartridges.

  1. Morphological, spectral and chromatography analysis and forensic comparison of PET fibers.

    PubMed

    Farah, Shady; Tsach, Tsadok; Bentolila, Alfonso; Domb, Abraham J

    2014-06-01

    Poly(ethylene terephthalate) (PET) fiber analysis and comparison by spectral and polymer molecular weight determination was investigated. Plain fibers of PET, a common textile fiber and plastic material was chosen for this study. The fibers were analyzed for morphological (SEM and AFM), spectral (IR and NMR), thermal (DSC) and molecular weight (MS and GPC) differences. Molecular analysis of PET fibers by Gel Permeation Chromatography (GPC) allowed the comparison of fibers that could not be otherwise distinguished with high confidence. Plain PET fibers were dissolved in hexafluoroisopropanol (HFIP) and analyzed by GPC using hexafluoroisopropanol:chloroform 2:98 v/v as eluent. 14 PET fiber samples, collected from various commercial producers, were analyzed for polymer molecular weight by GPC. Distinct differences in the molecular weight of the different fiber samples were found which may have potential use in forensic fiber comparison. PET fibers with average molecular weights between about 20,000 and 70,000 g mol(-1) were determined using fiber concentrations in HFIP as low as 1 μg mL(-1). This GPC analytical method can be applied for exclusively distinguish between PET fibers using 1 μg of fiber. This method can be extended to forensic comparison of other synthetic fibers such as polyamides and acrylics.

  2. Simultaneous analysis of multiple neurotransmitters by hydrophilic interaction liquid chromatography coupled to tandem mass spectrometry.

    PubMed

    Tufi, Sara; Lamoree, Marja; de Boer, Jacob; Leonards, Pim

    2015-05-22

    Neurotransmitters are endogenous metabolites that allow the signal transmission across neuronal synapses. Their biological role is crucial for many physiological functions and their levels can be changed by several diseases. Because of their high polarity, hydrophilic interaction liquid chromatography (HILIC) is a promising tool for neurotransmitter analysis. Due to the large number of HILIC stationary phases available, an evaluation of the column performances and retention behaviors has been performed on five different commercial HILIC packing materials (silica, amino, amide and two zwitterionic stationary phases). Several parameters like the linear correlation between retention and the distribution coefficient (logD), the separation factor k and the column resolution Rs have been investigated and the column performances have been visualized with a heat map and hierarchical clustering analysis. An optimized and validated HILIC-MS/MS method based on the ZIC-cHILIC column is proposed for the simultaneous detection and quantification of twenty compounds consisting of neurotransmitters, precursors and metabolites: 3-methoxytyramine (3-MT), 5-hydroxyindoleacetic acid (5-HIAA), 5-hydroxy-L-tripthophan, acetylcholine, choline, L-3,4-dihydroxyphenylalanine (L-DOPA), dopamine, epinephrine, γ-aminobutyric acid (GABA), glutamate, glutamine, histamine, histidine, L-tryptophan, L-tyrosine, norepinephrine, normetanephrine, phenylalanine, serotonin and tyramine. The method was applied to neuronal metabolite profiling of the central nervous system of the freshwater snail Lymnaea stagnalis. This method is suitable to explore neuronal metabolism and its alteration in different biological matrices.

  3. Global Analysis of the Membrane Subproteome of Pseudomonas aeruginosa using Liquid Chromatography-Tandem Mass Spectrometry

    SciTech Connect

    Blonder, Josip; Goshe, Michael B.; Xiao, Wenzhong; Camp, David G.; Wingerd, Mark A.; Davis, Ronald W.; Smith, Richard D.

    2004-05-30

    Pseudomonas aeruginosa is one of the most significant opportunistic bacterial pathogens in humans causing infections and premature death in patients with cystic fibrosis, AIDS, severe burns, organ transplants or cancer. Liquid chromatography coupled online with tandem mass spectrometry (LC-MS/MS) was used for the large-scale proteomic analysis of the P. aeruginosa membrane subproteome. Concomitantly, an affinity labeling technique, using iodoacetyl-PEO biotin to tag cysteinyl-containing proteins, permitted the enrichment and detection of lower abundance membrane proteins. The application of these approaches resulted in the identification of 786 proteins. A total of 333 proteins (42%) had a minimum of one transmembrane domain (TMD; ranging from 1 to 14) and 195 proteins were classified as hydrophobic based on their positive GRAVY values (ranging from 0.01 to 1.32). Key integral inner and outer membrane proteins involved in adaptation and antibiotic resistance were conclusively identified, including the detection of 53% of all predicted opr-type porins (outer integral membrane proteins) and all the components of the mexA-mexB-oprM transmembrane protein complex. This work represents the most comprehensive qualitative proteomic analysis of the membrane subproteome of P. aeruginosa and for prokaryotes in general to date.

  4. Post-column labeling techniques in amino acid analysis by liquid chromatography.

    PubMed

    Rigas, Pantelis G

    2013-10-01

    Amino acid analysis (AAA) has always presented an analytical challenge in terms of sample preparation, separation, and detection. Because of the vast number of amino acids, various separation methods have been applied taking into consideration the large differences in their chemical structures, which span from nonpolar to highly polar side chains. Numerous separation methods have been developed in the past 60 years, and impressive achievements have been made in the fields of separation, derivatization, and detection of amino acids (AAs). Among the separation methods, liquid chromatography (LC) prevailed in the AAA field using either pre-column or post-column labeling techniques in order to improve either separation of AAs or selectivity and sensitivity of AAA. Of the two approaches, the post-column technique is a more rugged and reproducible method and provides excellent AAs separation relatively free from interferences. This review considers current separations combined with post-column labeling techniques for AAA, comparison with the pre-column methods, and the strategies used to develop effective post-column methodology. The focus of the article is on LC methods coupled with post-column labeling techniques and studying the reactions to achieve optimum post-column derivatization (PCD) conditions in order to increase sensitivity and selectivity using various types of detectors (UV-Vis, fluorescence, electrochemical etc.) and illustrating the versatility of the PCD methods for practical analysis.

  5. Proteomic analysis of Taenia ovis metacestodes by high performance liquid chromatography-coupled tandem mass spectrometry.

    PubMed

    Zheng, Yadong

    2017-03-15

    Taenia ovis metacestodes reside in the muscle of sheep and goats, and may cause great economic loss due to condemnation of carcasses if not effectively controlled. Although advances have been made in the control of T. ovis infection, our knowledge of T. ovis biology is limited. Herein the protein profiling of T. ovis metacestodes was determined by liquid chromatography-linked tandem mass spectrometry. A total of 966 proteins were identified and 25.1% (188/748) were annotated to be associated with metabolic pathways. Consistently, GO analysis returned a metabolic process (16.27%) as one of two main biological process terms. Moreover, it was found that 24 proteins, including very low-density lipoprotein receptor, enolase, paramyosin and endophilin B1, were abundant in T. ovis metacestodes. These proteins may be associated with motility, metabolism, signaling, stress, drug resistance and immune responses. Furthermore, comparative analysis of 5 cestodes revealed the presence of Taenia-specific enolases. These data provide clues for better understanding of T. ovis biology, which is informative for effective control of infection.

  6. Analysis of fifteen estrogen metabolites using packed column supercritical fluid chromatography-mass spectrometry.

    PubMed

    Xu, Xia; Roman, John M; Veenstra, Timothy D; Van Anda, Jennifer; Ziegler, Regina G; Issaq, Haleem J

    2006-03-01

    Packed column supercritical fluid chromatography with tandem mass spectrometry was used for the separation of estrone, estradiol, estriol, 16-epiestriol, 17-epiestriol, 16-ketoestradiol, 16alpha-hydroxyestrone, 2-methoxyestrone, 4-methoxyestrone, 2-hydroxyestrone-3-methyl ether, 2-methoxyestradiol, 4-methoxyestradiol, 2-hydroxyestrone, 4-hydroxyestrone, and 2-hydroxyestradiol. A gradient of methanol in carbon dioxide (0-30% methanol in 15 min, 2% change/min) at a flow rate of 2 mL/min and cyanopropyl silica column connected in series with a diol column, both 2.1 mm i.d. x 150 mm long, packed with 5-mum spherical silica-based particles, resulted in the separation and quantification of all 15 estrogens in less than 10 min. The limit of detection (LOD) and limit of quantitation (LOQ) of this pSFC MS/MS method was determined to be 0.5 (S/N = 3), and 5 pg, respectively. Compared with RP-HPLC MS analysis of the same mixture in terms of speed of analysis and sensitivity, pSFC MS is much faster, 10 versus 70 min, with comparable LOD and LOQ.

  7. Enantiomeric separation in comprehensive two-dimensional gas chromatography with accurate mass analysis.

    PubMed

    Chin, Sung-Tong; Nolvachai, Yada; Marriott, Philip J

    2014-11-01

    Chiral comprehensive two-dimensional gas chromatography (eGC×GC) coupled to quadrupole-accurate mass time-of-flight mass spectrometry (QTOFMS) was evaluated for its capability to report the chiral composition of several monoterpenes, namely, α-pinene, β-pinene, and limonene in cardamom oil. Enantiomers in a standard mixture were fully resolved by direct enantiomeric-GC analysis with a 2,3-di-O-methyl-6-t-butylsilyl derivatized β-cyclodextrin phase; however, the (+)-(R)-limonene enantiomer in cardamom oil was overlapped with other background components including cymene and cineole. Verification of (+)-(R)-limonene components based on characteristic ions at m/z 136, 121, and 107 acquired by chiral single-dimension GC-QTOFMS in the alternate MS/MSMS mode of operation was unsuccessful due to similar parent/daughter ions generated by interfering or co-eluting cymene and cineole. Column phases SUPELCOWAX, SLB-IL111, HP-88, and SLB-IL59, were incorporated as the second dimension column ((2)D) in chiral GC×GC analysis; the SLB-IL59 offered the best resolution for the tested monoterpene enantiomers from the matrix background. Enantiomeric ratios for α-pinene, β-pinene, and limonene were determined to be 1.325, 2.703, and 1.040, respectively, in the cardamom oil sample based on relative peak area data.

  8. Molecular Ionization-Desorption Analysis Source (MIDAS) for Mass Spectrometry: Thin-Layer Chromatography

    NASA Astrophysics Data System (ADS)

    Winter, Gregory T.; Wilhide, Joshua A.; LaCourse, William R.

    2016-02-01

    Molecular ionization-desorption analysis source (MIDAS), which is a desorption atmospheric pressure chemical ionization (DAPCI) type source, for mass spectrometry has been developed as a multi-functional platform for the direct sampling of surfaces. In this article, its utility for the analysis of thin-layer chromatography (TLC) plates is highlighted. Amino acids, which are difficult to visualize without staining reagents or charring, were detected and identified directly from a TLC plate. To demonstrate the full potential of MIDAS, all active ingredients from an analgesic tablet, separated on a TLC plate, were successfully detected using both positive and negative ion modes. The identity of each of the compounds was confirmed from their mass spectra and compared against standards. Post separation, the chemical signal (blue permanent marker) as reference marks placed at the origin and solvent front were used to calculate retention factor (Rf) values from the resulting ion chromatogram. The quantitative capabilities of the device were exhibited by scanning caffeine spots on a TLC plate of increasing sample amount. A linear curve based on peak are, R2 = 0.994, was generated for seven spots ranging from 50 to 1000 ng of caffeine per spot.

  9. In situ Analysis of Organic Compounds on Mars using Chemical Derivatization and Gas Chromatography Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Glavin, D. P.; Buch, A.; Cabane, M.; Coll, P.; Navarro-Gonzalez, R.; Mahaffy, P. R.

    2005-01-01

    One of the core science objectives of NASA's 2009 Mars Science Laboratory (MSL) mission is to determine the past or present habitability of Mars. The search for key organic compounds relevant to terrestrial life will be an important part of that assessment. We have developed a protocol for the analysis of amino acids and carboxylic acids in Mars analogue materials using gas chromatography mass spectrometry (GCMS). As shown, a variety of carboxylic acids were readily identified in soil collected from the Atacama Desert in Chile at part-per-billion levels by GCMS after extraction and chemical derivatization using the reagent N,N-tert.-butyl (dimethylsilyl) trifluoroacetamide (MTBSTFA). Several derivatized amino acids including glycine and alanine were also detected by GCMS in the Atacama soil at lower concentrations (chromatogram not shown). Lacking derivatization capability, the Viking pyrolysis GCMS instruments could not have detected amino acids and carboxylic acids, since these non-volatile compounds require chemical transformation into volatile species that are stable in a GC column. We are currently optimizing the chemical extraction and derivatization technique for in situ GCMS analysis on Mars. Laboratory results of analyses of Atacama Desert samples and other Mars analogue materials using this protocol will be presented.

  10. Multiresidue analysis of environmental pollutants in edible vegetable oils by gas chromatography-tandem mass spectrometry.

    PubMed

    Zhou, Rui-Ze; Jiang, Jie; Mao, Ting; Zhao, Ya-Song; Lu, Yong

    2016-09-15

    A novel multiresidue determination of polycyclic aromatic hydrocarbons (PAHs), phthalate esters (PAEs) and alkylphenols (APs) in edible vegetable oils was developed. The samples were extracted with hexane-saturated acetonitrile, and after concentration, the extract was directly qualitatively and quantitatively analyzed by gas chromatography-tandem mass spectrometry (GC-MS/MS) with multiple reaction monitoring (MRM) in positive ion mode. The calibration curve displayed good linearity in the range of 2-100 μg/L, with correlation coefficients greater than 0.99. The mean recoveries were 70.0-110.8% by analysis of spiked oil, and the relative standard deviations (RSDs) were 2.1-10.2% (n=6), respectively. The limits of detection (LODs) for the 23 PAHs, 17 PAEs and 3 APs were 0.1-1.0 μg/kg, 0.1-4.0 μg/kg and 1.2-3.0 μg/kg, respectively. The established method effectively avoided interference from large amounts of lipids and pigments. It was applied to real sample and shown to be a rapid and reliable alternative for determination and confirmation in routine analysis.

  11. Enhanced analysis of steroids by gas chromatography/mass spectrometry using microwave-accelerated derivatization.

    PubMed

    Bowden, John A; Colosi, Dominic M; Stutts, Whitney L; Mora-Montero, Diana C; Garrett, Timothy J; Yost, Richard A

    2009-08-15

    Derivatization of steroids is typically required before analysis by gas chromatography/mass spectrometry (GC/MS); nevertheless, the derivatization process can often be time-consuming and irreproducible. Although several strategies have been employed to enhance this process, few have the potential of microwave-accelerated derivatization (MAD) to be more efficient than traditional thermal derivatization methods. MAD using a synthesis microwave system was evaluated and compared to traditional thermal derivatization methods in terms of yield, reproducibility, and overall analysis time. Parameters affecting MAD, including reaction temperature, time, and power, were systematically optimized for several silyl reagents (BSTFA with TMCS, MSTFA, and BSA) and other derivatization procedures (MOX reagent and MTBSTFA). MSTFA was found to derivatize best with the microwave, as demonstrated by the enhanced relative response factors (RRFs). BSTFA with TMCS, on the other hand, did not couple as well, but RRF values improved significantly upon addition of polar solvents. The rapid (1 min) derivatization reactions associated with MAD had comparable RRFs for all reagents with those obtained with thermal heating (>30 min). This study highlights the best methods for analyzing a comprehensive variety of steroids and also provides ideal strategies for MAD of steroids on an individual or class level.

  12. [Analysis of aliphatic carboxylic acids in anaerobic digestion process waters by ion-exclusion chromatography].

    PubMed

    Ito, Kazuaki; Sakamoto, Jun; Nagaoka, Kazuya; Takayama, Yohichi; Kanahori, Takashi; Sunahara, Hiroshi; Hayashi, Tsuneo; Sato, Shinji; Hirokawa, Takeshi; Tanaka, Kazuhiko

    2012-04-01

    The analysis of seven aliphatic carboxylic acids (formic, acetic, propionic, iso-butyric, n-butyric, iso-valeric and n-valeric acid) in anaerobic digestion process waters for biogas production was examined by ion-exclusion chromatography with dilute acidic eluents (benzoic acid, perfluorobutyric acid (PFBA) and sulfuric acid) and non-suppressed conductivity/ultraviolet (UV) detection. The columns used were a styrene/divinylbenzene-based strongly acidic cation-exchange resin column (TSKgel SCX) and a polymethacrylate-based weakly acidic cation-exchange resin column (TSKgel Super IC-A/C). Good separation was performed on the TSKgel SCX in shorter retention times. For the TSKgel Super IC-A/C, peak shape of the acids was sharp and symmetrical in spite of longer retention times. In addition, the mutual separation of the acids was good except for iso- and n-butyric acids. The better separation and good detection was achieved by using the two columns (TSKgel SCX and TSKgel Super IC-A/C connected in series), lower concentrations of PFBA and sulfuric acid as eluents, non-suppressed conductivity detection and UV detection at 210 nm. This analysis was applied to anaerobic digestion process waters. The chromatograms with conductivity detection were relatively simpler compared with those of UV detection. The use of two columns with different selectivities for the aliphatic carboxylic acids and the two detection modes was effective for the determination and identification of the analytes in anaerobic digestion process waters containing complex matrices.

  13. Sequential micellar electrokinetic chromatography analysis of racemization reaction of alanine enantiomers.

    PubMed

    Fu, Rao; Liu, Lina; Guo, Yingna; Guo, Liping; Yang, Li

    2014-02-28

    A novel method for online monitoring racemization reaction of alanine (Ala) enantiomers was developed, by combining sequential sample injection and micellar electrokinetic chromatography (MEKC) technique. Various conditions were investigated to optimize the sequential injection, Ala derivatization and MEKC chiral separation of d-/l-Ala. High reproducibility of the sequential MEKC analysis was demonstrated by analyzing the standard Ala samples, with relative standard deviation values (n=20) of 1.35%, 1.98%, and 1.09% for peak height, peak area and migration time, respectively. Ala racemization was automatically monitored every 40s from the beginning to the end of the reaction, by simultaneous detection of the consumption of the substrate enantiomer and the formation of the product enantiomer. The Michaelis constants of the racemization reaction were obtained by the sequential MEKC method, and were in good agreement with those obtained by traditional off-line enzyme assay. Our study indicated that the present sequential MEKC method can perform fast, efficient, accurate and reproducible analysis of racemization reaction of amino acids, which is of great importance for the determination of the activity of racemase and thus understanding its metabolic functions.

  14. Analysis of antithyroid drugs in surface water by using liquid chromatography-tandem mass spectrometry.

    PubMed

    Pérez-Fernández, Virginia; Marchese, Stefano; Gentili, Alessandra; García, María Ángeles; Curini, Roberta; Caretti, Fulvia; Perret, Daniela

    2014-11-07

    This paper describes development and validation of a new method for the simultaneous determination of six antithyroid drugs (ATDs) in surface waters by using liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). Target compounds include two ATD classes: thiouracil derivatives (thiouracil (TU), methyl-thiouracil (MTU), propyl-thiouracil (PTU), phenyl-thiouracil (PhTU)) and imidazole derivatives (tapazole (TAP), and mercaptobenzimidazole (MBI)). Sensitivity and selectivity of the LC-multiple reaction monitoring (MRM) analysis allowed applying a simple pre-concentration procedure and "shooting" the concentrated sample into the LC-MS/MS system without any other treatment. Recoveries were higher than 75% for all analytes. Intra-day precision and inter-day precision, calculated as relative standard deviation (RSD), were below 19 and 22%, respectively. Limits of detection (LODs) ranged from 0.05 to 0.25 μg/L; limits of quantitation (LOQs) varied between 0.15 and 0.75 μg/L. The validated method was successfully applied to the analysis of ATD residues in surface water samples collected from the Tiber River basin and three lakes of Lazio (central Italy). The analytes were quantified based on matrix-matched calibration curves with mercaptobenzimidazole-d4 (MBI-d4) as the internal standard (IS). The most widespread compound was TAP, one of the most common ATDs used in human medicine, but also TU and MBI were often detected in the analysed samples.

  15. Ultra Performance Liquid Chromatography and High Resolution Mass Spectrometry for the Analysis of Plant Lipids

    PubMed Central

    Hummel, Jan; Segu, Shruthi; Li, Yan; Irgang, Susann; Jueppner, Jessica; Giavalisco, Patrick

    2011-01-01

    Holistic analysis of lipids is becoming increasingly popular in the life sciences. Recently, several interesting, mass spectrometry-based studies have been conducted, especially in plant biology. However, while great advancements have been made we are still far from detecting all the lipids species in an organism. In this study we developed an ultra performance liquid chromatography-based method using a high resolution, accurate mass, mass spectrometer for the comprehensive profiling of more than 260 polar and non-polar Arabidopsis thaliana leaf lipids. The method is fully compatible to the commonly used lipid extraction protocols and provides a viable alternative to the commonly used direct infusion-based shotgun lipidomics approaches. The whole process is described in detail and compared to alternative lipidomic approaches. Next to the developed method we also introduce an in-house developed database search software (GoBioSpace), which allows one to perform targeted or un-targeted lipidomic and metabolomic analysis on mass spectrometric data of every kind. PMID:22629264

  16. Applying Chromatography.

    ERIC Educational Resources Information Center

    Klein, Jessie W.; Patev, Paul

    1998-01-01

    Presents three experiments to introduce students to different kinds of chromatography: (1) paper chromatography; (2) gel filtration chromatography; and (3) reverse-phase liquid chromatography. Written in the form of a laboratory manual, explanations of each of the techniques, materials needed, procedures, and a glossary are included. (PVD)

  17. [The gas-liquid cromatography with mass spectrometry for the identification of yeasts].

    PubMed

    Paredes-Salido, F; Mira-Gutiérrez, J; Sasián-Macías, P; García-Martos, P

    2001-03-01

    Methods based on gas chromatography, have been used for identification of the yeasts. In order to know the value of the patterns obtained by this method, we have used this technique and mass spectrometry on 44 strains belonging to 16 genus and 21 species of collection yeasts, identifying the corresponding peaks to 22 fatty acids methyl esters by means of the reaction times of the corresponding standards and the confirmation of molecular weigh by mass spectrometry. The correlation coefficient was of 0.848965. The chromatographic technique seems of great utility for the determination of lipidotypes.

  18. Considerations on the temperature dependence of the gas-liquid chromatographic retention.

    PubMed

    González, Francisco Rex

    2002-01-04

    A discussion on the temperature dependence of the partition coefficient K is developed. This discussion embraces topics such as the limitations of conventional thermodynamic approaches followed in the chromatographic literature, qualitative theoretical notions arising from molecular thermodynamics and the experimental information that is accessible through modern capillary gas chromatography. It is shown that the heat capacity difference of solute transfer for flexible molecules has at least one maximum in the chromatographic range of temperature. As a consequence, a great amount of experimental data is required for a correct thermodynamic interpretation of the chromatographic retention.

  19. Supervised pattern recognition procedures for discrimination of whiskeys from gas chromatography/mass spectrometry congener analysis.

    PubMed

    González-Arjona, Domingo; López-Pérez, Germán; González-Gallero, Víctor; González, A Gustavo

    2006-03-22

    The volatile congener analysis of 52 commercialized whiskeys (24 samples of single malt Scotch whiskey, 18 samples of bourbon whiskey, and 10 samples of Irish whiskey) was carried out by gas chromatography/mass spectrometry after liquid-liquid extraction with dichloromethane. Pattern recognition procedures were applied for discrimination of different whiskey categories. Multivariate data analysis includes linear discriminant analysis (LDA), k nearest neighbors (KNN), soft independent modeling of class analogy (SIMCA), procrustes discriminant analysis (PDA), and artificial neural networks techniques involving multilayer perceptrons (MLP) and probabilistic neural networks (PNN). Classification rules were validated by considering the number of false positives (FPs) and false negatives (FNs) of each class associated to the prediction set. Artificial neural networks led to the best results because of their intrinsic nonlinear features. Both techniques, MLP and PNN, gave zero FPs and zero FNs for all of the categories. KNN is a nonparametric method that also provides zero FPs and FNs for every class but only when selecting K = 3 neighbors. PDA produced good results also (zero FPs and FNs always) but only by selecting nine principal components for class modeling. LDA shows a lesser classification performance, because of the building of linear frontiers between classes that does not apply in many real situations. LDA led to one FP for bourbons and one FN for scotches. The worse results were obtained with SIMCA, which gave a higher number of FPs (five for both scotches and bourbons) and FNs (six for scotchs and two for bourbons). The possible cause of these findings is the strong influence of class inhomogeneities on the SIMCA performance. It is remarkable that in any case, all of the methodologies lead to zero FPs and FNs for the Irish whiskeys.

  20. Identification of atmospheric organic sources using the carbon hollow tube-gas chromatography method and factor analysis

    SciTech Connect

    Cobb, G.P.; Braman, R.S.; Gilbert, R.A. )

    1989-04-15

    Atmospheric organics were sampled and analyzed by using the carbon hollow tube-gas chromatography method. Chromatograms from spice mixtures, cigarettes, and ambient air were analyzed. Principal factor analysis of row order chromatographic data produces factors which are eigenchromatograms of the components in the samples. Component sources are identified from the eigenchromatograms in all experiments and the individual eigenchromatogram corresponding to a particular source is determined in most cases. Organic sources in ambient air and in cigaretts are identified with 87% certainty. Analysis of clove cigarettes allows the determination of the relative amount of clove in different cigarettes. A new nondestructive quality control method using the hollow tube-gas chromatography analysis is discussed.

  1. Comparative analysis of steroidal saponins in four Dioscoreae herbs by high performance liquid chromatography coupled with mass spectrometry.

    PubMed

    Guo, Long; Zeng, Su-Ling; Zhang, Yu; Li, Ping; Liu, E-Hu

    2016-01-05

    Steroidal saponins, which exhibit multiple pharmacological effects, are the major bioactive constituents in herbal medicines from Dioscoreae species. In this study, a sensitive method based on high performance liquid chromatography-mass spectrometry (HPLC-MS) was established and validated for qualitative and quantitative analysis of steroidal saponins in four Dioscoreae herbs including Dioscoreae Nipponica Rhizome (DNR) and Dioscoreae Hypoglaucae Rhizome (DHR), Dioscoreae Spongiosae Rhizome (DSR) and Dioscoreae Rhizome (DR). A total of eleven steroidal saponins were identified by high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF/MS). Furthermore, seven major steroidal saponins was simultaneous quantified using a high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-QQQ/MS). The qualitative and quantitative analysis results indicated that the chemical composition of DNR, DHR and DSR samples exhibited a high level of global similarity, while the ingredients in DR varied greatly from the other three herbs. Moreover, principal component analysis (PCA) and hierarchical clustering analysis (HCA) were performed to compare and discriminate the Dioscoreae herbs based on the quantitative data. The results demonstrated the qualitative and quantitative analysis of steroidal saponins based on HPLC-MS is a feasible method for quality control of Dioscoreae herbs.

  2. A rapid analysis of plasma/serum ethylene and propylene glycol by headspace gas chromatography.

    PubMed

    Ehlers, Alexandra; Morris, Cory; Krasowski, Matthew D

    2013-12-01

    A rapid headspace-gas chromatography (HS-GC) method was developed for the analysis of ethylene glycol and propylene glycol in plasma and serum specimens using 1,3-propanediol as the internal standard. The method employed a single-step derivitization using phenylboronic acid, was linear to 200 mg/dL and had a lower limit of quantitation of 1 mg/dL suitable for clinical analyses. The analytical method described allows for laboratories with HS-GC instrumentation to analyze ethanol, methanol, isopropanol, ethylene glycol, and propylene glycol on a single instrument with rapid switch-over from alcohols to glycols analysis. In addition to the novel HS-GC method, a retrospective analysis of patient specimens containing ethylene glycol and propylene glycol was also described. A total of 36 patients ingested ethylene glycol, including 3 patients who presented with two separate admissions for ethylene glycol toxicity. Laboratory studies on presentation to hospital for these patients showed both osmolal and anion gap in 13 patients, osmolal but not anion gap in 13 patients, anion but not osmolal gap in 8 patients, and 1 patient with neither an osmolal nor anion gap. Acidosis on arterial blood gas was present in 13 cases. Only one fatality was seen; this was a patient with initial serum ethylene glycol concentration of 1282 mg/dL who died on third day of hospitalization. Propylene glycol was common in patients being managed for toxic ingestions, and was often attributed to iatrogenic administration of propylene glycol-containing medications such as activated charcoal and intravenous lorazepam. In six patients, propylene glycol contributed to an abnormally high osmolal gap. The common presence of propylene glycol in hospitalized patients emphasizes the importance of being able to identify both ethylene glycol and propylene glycol by chromatographic methods.

  3. Systematic analysis of glycerol: colourimetric screening and gas chromatography-mass spectrometric confirmation.

    PubMed

    Sardela, Vinícius F; Scalco, Fernanda B; Cavalcante, Karina M; Simoni, Ruth E; Silva, Deyvison R; Pereira, Henrique Marcelo G; de Oliveira, Maria Lúcia L Costa; Aquino Neto, Francisco R

    2015-10-01

    Glycerol is a naturally occurring polyol in the human body, essential for several metabolic processes. It is widely used in the food, pharmaceutical, and medical industries and in clinical practice as a plasma volume expander (PVE). Athletes, however, may use glycerol to mask the presence of forbidden substances or to enhance performance, inclusively through hyperhydration achieved by glycerol ingestion with added fluid. These practices are considered doping, and are prohibited by the World Anti-Doping Agency (WADA). Therefore, glycerol was introduced in the prohibited list. Doping through glycerol ingestion can readily be identified by detection of elevated glycerol concentrations in urine. In this paper, a protocol for the fast detection of glycerol in urine is proposed. It consists of a previous visual colourimetric screening, followed by a quantitative/qualitative confirmation analysis by mass spectrometry. The screening procedure involves a reaction in which polyhydric alcohols are oxidized by periodate to formic acid and formaldehyde, which is detected by the addition of a fuchsin solution. For the subsequent qualitative/quantitative confirmation analysis, a gas chromatography-mass spectrometry based approach with a non-deuterated internal standard and a drying step of only 10 min is proposed. The linear correlation was demonstrated within WADA´s threshold range. The calculated RSD were 2.1% for within-day precision and 2.8% for between-day precision. The uncertainty estimation was calculated, and a value of 2.7% was obtained. The procedure may also be used for the analysis of other polyols in urine, as for example the PVE mannitol.

  4. Enhancing concentration and mass sensitivities for liquid chromatography trace analysis of clopyralid in drinking water.

    PubMed

    Gu, Binghe; Meldrum, Brian; McCabe, Terry; Phillips, Scott

    2012-01-01

    A theoretical treatment was developed and validated that relates analyte concentration and mass sensitivities to injection volume, retention factor, particle diameter, column length, column inner diameter and detection wavelength in liquid chromatography, and sample volume and extracted volume in solid-phase extraction (SPE). The principles were applied to improve sensitivity for trace analysis of clopyralid in drinking water. It was demonstrated that a concentration limit of detection of 0.02 ppb (μg/L) for clopyralid could be achieved with the use of simple UV detection and 100 mL of a spiked drinking water sample. This enabled reliable quantitation of clopyralid at the targeted 0.1 ppb level. Using a buffered solution as the elution solvent (potassium acetate buffer, pH 4.5, containing 10% of methanol) in the SPE procedures was found superior to using 100% methanol, as it provided better extraction recovery (70-90%) and precision (5% for a concentration at 0.1 ppb level). In addition, the eluted sample was in a weaker solvent than the mobile phase, permitting the direct injection of the extracted sample, which enabled a faster cycle time of the overall analysis. Excluding the preparation of calibration standards, the analysis of a single sample, including acidification, extraction, elution and LC run, could be completed in 1 h. The method was used successfully for the determination of clopyralid in over 200 clopyralid monoethanolamine-fortified drinking water samples, which were treated with various water treatment resins.

  5. Analysis of Dyes Extracted from Millimeter-Size Nylon Fibers by Micellar Electrokinetic Chromatography

    SciTech Connect

    Lewis, L.A.

    2001-07-30

    The Learning Objective is to present to the forensic community a potential qualitative/quantitative method for trace-fiber color comparisons using micellar electrokinetic chromatography (MEKC). Developing a means of analyzing extracted dye constituents from millimeter-size nylon fiber samples was the objective of this research initiative. Aside from ascertaining fiber type, color evaluation and source comparison of trace-fiber evidence plays a critical role in forensic-fiber examinations. Literally thousands of dyes exist to date, including both natural and synthetic compounds. Typically a three-color-dye combination is employed to affect a given color on fiber material. The result of this practice leads to a significant number of potential dye combinations capable of producing a similar color and shade. Since a typical forensic fiber sample is 2 mm or less in length, an ideal forensic dye analysis would qualitatively and quantitatively identify the extracted dye constituents from a sample size of 1 mm or smaller. The goal of this research was to develop an analytical method for comparing individual dye constituents from trace-fiber evidence with dyes extracted from a suspected source, while preserving as much of the original evidence as possible.

  6. Analysis of acrylamide in coffee and cocoa by isotope dilution liquid chromatography-tandem mass spectrometry.

    PubMed

    Aguas, Patricia C; Fitzhenry, Matthew J; Giannikopoulos, Georgina; Varelis, Peter

    2006-08-01

    An accurate and precise method for the quantification of acrylamide using stable isotope dilution liquid chromatography-tandem mass spectrometry was developed and used to measure acrylamide in coffee and cocoa samples. The sample preparation involved extraction of the analyte and its internal standard, 13C3-acrylamide, into water and subsequent defatting of the aqueous extract with dichloromethane. An aliquot of the resulting aqueous extract was then azeotropically dried under reduced pressure and subsequently purified using an aminopropyl-bonded silica cartridge. The purified extracts were then chromatographed on a 5-microm 2.1 x 150 mm Hypercarb column, the effluent of which was monitored for the analyte and its internal standard using positive-ion APCI-selected reaction monitoring. The intra-laboratory reproducibility of the method, expressed as a relative coefficient of variation (%, n=5), was determined at four levels of concentration (12.3, 42.3, 139.3 and 464.8 microg kg(-1)) and was found to vary between 0.6-2.5%. The accuracy of the method was assessed using a reference sample of coffee. The average result obtained using our method differed from the assigned value of the reference material by less than 1%. An analysis of a cocoa sample revealed that the method is capable of precisely estimating acrylamide in challenging matrices down to a level of at least 12.3 microg kg(-1).

  7. Analysis of Fluconazole in Human Urine Sample by High Performance Liquid Chromatography Method

    NASA Astrophysics Data System (ADS)

    Hermawan, D.; Ali, N. A. Md; Ibrahim, W. A. Wan; Sanagi, M. M.

    2013-04-01

    A method for determination of fluconazole, antifungal drug in human urine by using reversed-phased high performance liquid chromatography (RP-HPLC) with ultraviolet (UV) detector was developed. Optimization HPLC conditions were carried out by changing the flow rate and composition of mobile phase. The optimum separation conditions at a flow rate 0.85 mL/min with a composition of mobile phase containing methanol:water (70:30, v/v) with UV detection at a wavelength 254 nm was able to analyze fluconazole within 3 min. The excellent linearity was obtained in the range of concentration 1 to 10 μg/mL with r2 = 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.39 μg/mL and 1.28 μg/mL, respectively. Solid phase extraction (SPE) method using octadecylsilane (C18) as a sorbent was used to clean-up and pre-concentrated of the urine sample prior to HPLC analysis. The average recoveries of fluconazole in spiked urine sample was 72.4% with RSD of 3.21% (n=3).

  8. Analysis of lipoprotein profiles of healthy cats by gel-permeation high-performance liquid chromatography

    PubMed Central

    MIZUTANI, Hisashi; SAKO, Toshinori; OKUDA, Hiroko; ARAI, Nobuaki; KURIYAMA, Koji; MORI, Akihiro; YOSHIMURA, Itaru; KOYAMA, Hidekazu

    2016-01-01

    Density gradient ultracentrifugation (DGUC) and gel electrophoresis are conventionally used to obtain lipoprotein profiles of animals. We recently applied high-performance liquid chromatography with a gel permeation column (GP-HPLC) and an on-line dual enzymatic system to dogs for lipoprotein profile analysis. We compared the GP-HPLC with DGUC as a method to obtain a feline lipoprotein profile. The lipoprotein profiles showed large and small peaks, which corresponded to high-density lipoprotein (HDL) and low-density lipoprotein (LDL), respectively, whereas very low-density lipoprotein (VLDL) and chylomicron (CM) were only marginally detected. This profile was very similar to that of dogs reported previously. Healthy cats also had a small amount of cholesterol-rich particles distinct from the normal LDL or HDL profile. There was no difference in lipoprotein profiles between the sexes, but males had a significantly larger LDL particle size (P=0.015). This study shows the feasibility of GP-HPLC for obtaining accurate lipoprotein profiles with small sample volumes and provides valuable reference data for healthy cats that should facilitate diagnoses. PMID:27170431

  9. [Serum metabolomics analysis on benign prostate hyperplasia in mice based on liquid chromatography-mass spectrometry].

    PubMed

    Geng, Yue; Sun, Fengxia; Ma, Yu; Deng, Ligang; Lü, Jianyun; Li, Teng; Wang, Congcong

    2014-12-01

    Benign prostatic hyperplasia (BPH) increasingly becomes a common factor affecting the quality of life of aging men. Its pathogenesis has not yet been fully elucidated. Ultra-high pressure liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) was employed to detect the changes of serum metabolites in normal mice, benign prostatic hyperplasia model mice and BPH model mice with finasteride intervention. The serum metabolite profiles of the three groups of mice were analyzed. Partial least squares-discriminant analysis (PLS-DA) was used for group differentiation and biomarker selection. The results showed good distinction among the three groups of mice serum metabolite spectra. Three potential biomarkers, 1-hexadecanoyl-SN-glycero-3-phosphocholine, 1-O-hexadecyl-2-O-acetyl-sn-glyceryl-3-phosphorylcholine and (Z)-13-docosenamide, were discovered and identified. They all indicated the occurrence of benign prostatic hypertrophy is closely related to the disorders of lipid metabolism. Coinpared with the control group, the contents of the first two substances were significantly increased in the serum of BPH model mice, and significantly decreased after intervened by finasteride. The contents of (Z)-13-docosenamide decreased significantly in the serum of model group, and increased after intervened by finasteride. Compared with the control group, the contents of three biomarkers in finasteride group did not recover completely and had significant differences. This study is conductive to open new avenues of diagnosis and medical treatment for BPH.

  10. Analysis of testosterone and dihydrotestosterone in mouse tissues by liquid chromatography-electrospray tandem mass spectrometry

    PubMed Central

    Weng, Yan; Xie, Fang; Xu, Li; Zagorevski, Dmitri; Spink, David C.; Ding, Xinxin

    2010-01-01

    A novel method was established for simultaneous quantitation of testosterone (T) and dihydrotestosterone (DHT) in murine tissue and serum samples. Endogenous T and DHT, together with the internal standards, 17α-methyl-T and 17α-methyl-DHT, were extracted from tissues, and then derivatized by reaction with 2-hydrazino-4-(trifluoromethyl)-pyrimidine (HTP). Analysis by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) resulted in production spectra of HTP derivatives of both T and DHT that showed analyte-specific fragmentations; the latter fragmentations were characterized by use of high-resolution Orbitrap MS/MS. These specific fragmentations enabled quantitation of T and DHT in the multiple-reaction monitoring (MRM) mode. The method was validated with charcoal-stripped serum as the matrix; the LLOQ was 0.10 ng/ml for T and 0.50 ng/ml for DHT. The method was then used for determination of serum and tissue levels of T and DHT in transgenic mice carrying a hypomorphic NADPH-cytochrome P450 reductase gene (Cpr-low mice). Remarkably, ovarian T levels in Cpr-low mice were found to be 25-fold higher than those in wild-type mice, a finding that at least partly explains the female infertility seen in the Cpr-low mice. In conclusion, our method provides excellent sensitivity and selectivity for determination of endogenous levels of T and DHT in mouse tissues. PMID:20361922

  11. Analysis of siloxanes in hydrocarbon mixtures using comprehensive two-dimensional gas chromatography.

    PubMed

    Ghosh, Abhijit; Seeley, Stacy K; Nartker, Steven R; Seeley, John V

    2014-09-19

    A comprehensive two-dimensional gas chromatography (GC×GC) method for separating siloxanes from hydrocarbons has been developed using a systematic process. First, the retention indices of a set of siloxanes and a set of hydrocarbons were determined on 6 different stationary phases. The retention indices were then used to model GC×GC separation on 15 different stationary phase pairs. The SPB-Octyl×DB-1 pair was predicted to provide the best separation of the siloxanes from the hydrocarbons. The efficacy of this stationary phase pair was experimentally tested by performing a GC×GC analysis of gasoline spiked with siloxanes and by analyzing biogas obtained from a local wastewater treatment facility. The model predictions agreed well with the experimental results. The SPB-Octyl×DB-1 stationary phase pair constrained the hydrocarbons to a narrow range of secondary retention times and fully isolated the siloxanes from the hydrocarbon band. The resulting GC×GC method allows siloxanes to be resolved from complex mixtures of hydrocarbons without requiring the use of a selective detector.

  12. Analysis of nerve agent metabolites from nail clippings by liquid chromatography tandem mass spectrometry.

    PubMed

    Appel, Amanda S; Logue, Brian A

    2016-09-15

    While several methods for the bioanalysis of nerve agents or their metabolites have been developed for the verification of nerve agent exposure, these methods are generally limited in the amount of time after an exposure that markers of exposure can be detected (due to rapid metabolism from biological matrices). In this study, a method for the analysis of nerve agent hydrolysis products from nail clippings was developed to allow evaluation of nails as a long-term repository of these markers. Pinacolyl methylphosphonic acid (PMPA) and isopropyl methylphosphonic acid (IMPA) were extracted from nail samples with N,N-dimethylformamide and subsequently analyzed by liquid chromatography-tandem mass spectrometry. Limits of detection for PMPA and IMPA were 0.3μg/kg and 7.5μg/kg and linear ranges were 0.75-300μg/kg and 30-1500μg/kg, respectively. Precision was within 10% and 8% for PMPA and IMPA, respectively, and accuracy was 100±12% for both analytes. The approach presented here is complementary to current methods for nerve agent exposure verification, and should allow for long-term determination of nerve agent poisoning.

  13. High performance liquid chromatography analysis of canthinone alkaloids from Eurycoma longifolia.

    PubMed

    Choo, Chee-Yan; Chan, Kit-Lam

    2002-04-01

    A reversed phase-high performance liquid chromatography method with a photodiode array detector was developed for the simultaneous determination of three major alkaloids, 9-methoxycanthin-6-one (1), 3-methylcanthin-5,6-dione (2) and its 9-methoxy analogue (3) in Eurycoma longifolia Jack. These alkaloids were easily separated by a gradient elution protocol of 20 - 42 % acetonitrile in 0.1 % acetic acid. Compound 1 showed characteristic absorption at 350 nm only whereas its dione analogues, 2 and 3 displayed strong absorptions at both 350 and 451 nm. The linear calibration ranges were 0.7 - 50 microg x mL(-1) for 1, 1.5-50 microg x mL(-1) for 2 and 3.1 -100 microg x mL(-1) for 3. The recoveries of the three alkaloids were 90.8-101.0% with relative standard deviations from 0.35 to 6.31 % (n = 3). The limits of detection for all the alkaloids were within the range of 0.35 - 0.7 microg x mL(-1). This method was successfully applied to the phytochemical analysis of E. longifolia roots obtained from different sources.

  14. Liquid Chromatography-Tandem Mass Spectrometry for Analysis of Intestinal Permeability of Loperamide in Physiological Buffer

    PubMed Central

    Rubelt, Miriam S.; Amasheh, Salah; Grobosch, Thomas; Stein, Christoph

    2012-01-01

    Analysis of in vitro samples with high salt concentrations represents a major challenge for fast and specific quantification with liquid chromatography-tandem mass spectrometry (LC-MS/MS). To investigate the intestinal permeability of opioids in vitro employing the Ussing chamber technique, we developed and validated a fast, sensitive and selective method based on LC–MS/MS for the determination of loperamide in HEPES-buffered Ringer's solution. Chromatographic separation was achieved with an Atlantis dC18 column, 2.1 mm×20 mm, 3 µm particle size and a gradient consisting of methanol/0.1% formic acid and ammonium acetate. The flow rate was 0.7 ml/min, and the total run time was 3 min. For quantification, two mass transitions for loperamide and a deuterated internal standard (methadone-d3) were used. The lower limit of loperamide quantification was 0.2 ng/ml. This new LC-MS/MS method can be used for the detection of loperamide in any experimental setup using HEPES-buffered Ringer's solution as a matrix compound. PMID:23144895

  15. Holistic analysis of seven active ingredients by micellar electrokinetic chromatography from three medicinal herbs composing Shuanghuanglian.

    PubMed

    Zhou, Xian-Jing; Chen, Juan; Li, Ying-Dong; Jin, Ling; Shi, Yan-Ping

    2015-01-01

    A simple and reliable method has been developed with a new strategy named holistic analysis of multiple constituents to evaluate the quality of the well-known traditional Chinese medicine (TCM) Shuanghuanglian (SHL) oral liquid and soft capsule. Seven main constituents of the medicine, i.e., baicalein, baicalin, chlorogenic acid, wogonin, scutellarin, forsythin and hyperin, were selected as the evaluation markers and analyzed by micellar electrokinetic chromatography. The effects of buffer pH, concentration of electrolyte, organic modifier and applied voltage on migration behavior were studied systematically. The optimum conditions for the separation were achieved in a 12.5 mM borate-10 mM sodium dihydrogen phosphate-10 mM sodium dodecyl sulfate buffer at pH 9.1 containing 10% (v/v) acetonitrile under 15 kV. The analytes were identified by their relative time with regard to para-hydroxybenzoic acid migration time used as an internal standard. The method was validated in terms of linearity, limit of detection and quantification, precision, accuracy and recoveries. The correlation coefficient ranged from 0.9962 to 0.9992. The limits of detection (S/N = 3) were from 0.15 to 3.95 μg mL(-1). Recoveries of seven analytes in the SHL samples ranged from 89.00 to 103.04%. The proposed method was successfully applied for the quality control of complicated TCM SHL.

  16. Analysis of protein-glutathione mixed disulfides by high performance liquid chromatography.

    PubMed

    Meredith, M J

    1983-06-01

    After precipitation of proteins; serum, hepatocytes, or glutathione-derivatized bovine serum albumin, by perchloric acid, dithiothreitol was used to reduce glutathione-protein mixed disulfides in the ether-washed, resuspended pellet. Following neutralization and S-carboxymethylation of free sulfhydral groups in the acid soluble fraction by iodoacetic acid. 2,4-dinitrophenyl derivatives of released compounds were produced by addition of ethanolic fluorodinitrobenzene. The 2,4-dinitrophenyl derivative of S-carboxymethylglutathione was measured by high-performance liquid chromatography. The method was found to be reproducible and limited only by the sensitivity of the glutathione analysis (about 10 pmol/sample). Quantitation of protein-bound glutathione was shown to be independent of the ratio of bound to soluble glutathione as well as the protein concentration in the sample. This method was found to produce glutathione values identical to those measured after borohydride reduction without the problems of foaming, sample loss, and the need of continuous pH adjustment during reduction.

  17. Qualitative and quantitative analysis of four species of Curcuma rhizomes using twice development thin layer chromatography.

    PubMed

    Zhang, J S; Guan, J; Yang, F Q; Liu, H G; Cheng, X J; Li, S P

    2008-11-04

    The rhizomes of Curcuma phaeocaulis, Curcuma kwangsiensis, Curcuma wenyujin and Curcuma longa are used as Ezhu or Jianghuang in traditional Chinese medicine for a long time. Due to their similar morphological characters, it is difficult to distinguish their origins of raw materials used in clinic. In this study, a simple, rapid and reliable twice development TLC method was developed for qualitative and quantitative analysis of the four species of Curcuma rhizomes. The chromatography was performed on silica gel 60F(254) plate with chloroform-methanol-formic acid (80:4:0.8, v/v/v) and petroleum ether-ethyl acetate (90:10, v/v) as mobile phase for twice development. The TLC markers were colorized with 1% vanillin-H(2)SO(4) solution. The four species of Curcuma were easily discriminated based on their characteristic TLC profiles, and simultaneous quantification of eight compounds, including bisdemethoxycurcumin, demethoxycurcumin, curcumine, curcumenol, curcumol, curdione, furanodienone and curzerene, in Curcuma were also performed densitometrically at lambda(scan)=518nm and lambda(reference)=800 nm. The investigated compounds had good linearity (r(2)>0.9905) within test ranges. Therefore, the developed TLC method can be used for quality control of Curcuma rhizomes.

  18. Multiclass analysis of antibiotic residues in honey by ultraperformance liquid chromatography-tandem mass spectrometry.

    PubMed

    Vidal, Jose Luis Martínez; Aguilera-Luiz, María Del Mar; Romero-González, Roberto; Frenich, Antonia Garrido

    2009-03-11

    A method has been developed and validated for the simultaneous analysis of different veterinary drug residues (macrolides, tetracyclines, quinolones, and sulfonamides) in honey. Honey samples were dissolved with Na(2)EDTA, and veterinary residues were extracted from the supernatant by solid-phase extraction (SPE), using OASIS HLB cartridges. The separation and determination was carried out by ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS), using an electrospay ionization source (ESI) in positive mode. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring (MRM) of two ion transitions per compound to provide a high degree of sensitivity and specificity. The method was validated, and mean recoveries were evaluated at three concentration levels (10, 50, and 100 microg/kg), ranging from 70 to 120% except for doxycycline, erythromycin, and tylmicosin with recovery higher than 50% at the three levels assayed. Relative standard deviations (RSDs) of the recoveries were less than 20% within the intraday precision and less than 25% within the interday precision. The limits of quantification (LOQs) were always lower than 4 microg/kg. The developed procedure was applied to 16 honey samples, and erythromycin, sarafloxacin, and tylosin were found in a few samples.

  19. Systematic Optimization of Long Gradient Chromatography Mass Spectrometry for Deep Analysis of Brain Proteome

    SciTech Connect

    Wang, Hong; Yang, Yanling; Li, Yuxin; Bai, Bing; Wang, Xusheng; Tan, Haiyan; Liu, Tao; Beach, Thomas G.; Peng, Junmun; Wu, Zhiping

    2015-02-06

    Development of high resolution liquid chromatography (LC) is essential for improving the sensitivity and throughput of mass spectrometry (MS)-based proteomics. Here we present systematic optimization of a long gradient LC-MS/MS platform to enhance protein identification from a complex mixture. The platform employed an in-house fabricated, reverse phase column (100 μm x 150 cm) coupled with Q Exactive MS. The column was capable of achieving a peak capacity of approximately 700 in a 720 min gradient of 10-45% acetonitrile. The optimal loading level was about 6 micrograms of peptides, although the column allowed loading as many as 20 micrograms. Gas phase fractionation of peptide ions further increased the number of peptide identification by ~10%. Moreover, the combination of basic pH LC pre-fractionation with the long gradient LC-MS/MS platform enabled the identification of 96,127 peptides and 10,544 proteins at 1% protein false discovery rate in a postmortem brain sample of Alzheimer’s disease. As deep RNA sequencing of the same specimen suggested that ~16,000 genes were expressed, current analysis covered more than 60% of the expressed proteome. Further improvement strategies of the LC/LC-MS/MS platform were also discussed.

  20. Sources of Variability in Chlorophyll Analysis by Fluorometry and by High Performance Liquid Chromatography. Chapter 22

    NASA Technical Reports Server (NTRS)

    VanHeukelem, Laurie; Thomas, Crystal S.; Glibert, Patricia M.

    2001-01-01

    The need for accurate determination of chlorophyll a (chl a) is of interest for numerous reasons. From the need for ground-truth data for remote sensing to pigment detection for laboratory experimentation, it is essential to know the accuracy of the analyses and the factors potentially contributing to variability and error. Numerous methods and instrument techniques are currently employed in the analyses of chl a. These methods range from spectrophotometric quantification, to fluorometric analysis and determination by high performance liquid chromatography. Even within the application of HPLC techniques, methods vary. Here we provide the results of a comparison among methods and provide some guidance for improving the accuracy of these analyses. These results are based on a round-robin conducted among numerous investigators, including several in the Sensor Intercomparison and Merger for Biological and Interdisciplinary Oceanic Studies (SIMBIOS) and HyCODE Programs. Our purpose here is not to present the full results of the laboratory intercalibration; those results will be presented elsewhere. Rather, here we highlight some of the major factors that may contribute to the variability observed. Specifically, we aim to assess the comparability of chl a analyses performed by fluorometry and HPLC, and we identify several factors in the analyses which may contribute disproportionately to this variability.

  1. Analysis of EPA and DHA in the viscera of marine fish using gas chromatography.

    PubMed

    Zhang, De-Yong; Xu, Xiao-Lu; Shen, Xiu-Ying; Mei, Yu; Xu, Hui-Ying

    2016-03-01

    The viscera of 10 kinds of marine fishes were collected for fish oil extraction and detection of DHA and EPA, two most important polyunsaturated fatty acids. The fish oil extraction ratio for the evaluated fishes varied from 0.95% to 10.18% (wt%). Pseudosciaena crocea presented the highest fish oil yield, followed by Mustelus manazo, Hippoglossus and Sciaenopsocellatus. A gas chromatography method was then established for analysis of EPA/DHA. The EPA concentration (in methyl ester form) in the fish oil varied from 1.39 to 10.65(mg/g). Epinephelus awoara presented the highest EPA concentration (p<0.05), followed by Epinephelussp, Sciaenopsocellatus and Hippoglossus. The DHA concentration (in methyl ester form) in the fish oil varied from 0.58 to 37.02 (mg/g). Epinephelus awoara presented the highest DHA concentration (p<0.05), followed by Sciaenopsocellatus, Pseudosciaena crocea and Hippoglossus. No strict positive correlation between the EPA/DHA concentration and the sea depth where the fish live was observed. The fishes living in middle depth presented highest EPA/DHA concentration.

  2. Analysis of amphetamines and metabolites in urine with ultra performance liquid chromatography tandem mass spectrometry.

    PubMed

    Ramírez Fernández, María del Mar; Wille, Sarah M R; di Fazio, Vincent; Gosselin, Matthias; Samyn, Nele

    2010-06-01

    A simple, rapid and sensitive ultra performance liquid chromatography tandem mass spectrometry method was developed and fully validated for the quantitative determination of seven amphetamines and metabolites in urine. The method was validated for selectivity, linearity, LOQ, LOD, imprecision, bias, analyte and processed sample stability, matrix effect, recovery, carryover and dilution integrity. A classic liquid-liquid extraction with ethyl acetate was used as sample preparation procedure. The compounds were separated on an Acquity UPLC HSS C18 column in 6.8 min. The linear dynamic range was established from 25 to 500 ng/mL. The limit of quantification was fixed to the lowest calibrator level and the limit of detection ranged from 0.125 to 2.5 ng/mL. The method presented an excellent intra- and inter-assay imprecision and bias (<10.7%) at each measured concentration of two external quality controls (QC) and three "in house" QC. No matrix effects were observed and good recoveries (>70%) were obtained for all the compounds. No carryover was observed after the analysis of high concentrated samples (8000 ng/mL). The method was subsequently applied to authentic samples.

  3. Irreversible and reversible reactive chromatography: analytical solutions and moment analysis for rectangular pulse injections.

    PubMed

    Bibi, Sameena; Qamar, Shamsul; Seidel-Morgenstern, Andreas

    2015-03-13

    This work is concerned with the analysis of models for linear reactive chromatography describing irreversible A→B and reversible A↔B reactions. In contrast to previously published results rectangular reactant pulses are injected into initially empty or pre-equilibrated columns assuming both Dirichlet and Danckwerts boundary conditions. The models consist of two partial differential equations, accounting for convection, longitudinal dispersion and first order chemical reactions. Due to the effect of involved mechanisms on solute transport, analytical and numerical solutions of the models could be helpful to understand, design and optimize chromatographic reactors. The Laplace transformation is applied to solve the model equations analytically for linear adsorption isotherms. Statistical temporal moments are derived from solutions in the Laplace domain. Analytical results are compared with numerical predictions generated using a high-resolution finite volume scheme for two sets of boundary conditions. Several case studies are carried out to analyze reactive liquid chromatographic processes for a wide range of mass transfer and reaction kinetics. Good agreements in the results validate the correctness of the analytical solutions and accuracy of the proposed numerical algorithm.

  4. Comprehensive analysis of lipids in biological systems by liquid chromatography-mass spectrometry

    PubMed Central

    2014-01-01

    Liquid chromatography-mass spectrometry (LC-MS)-based lipidomics has been a subject of dramatic developments over the past decade. This review focuses on state of the art in LC-MS-based lipidomics, covering all the steps of global lipidomic profiling. On the basis of review of 185 original papers and application notes, we can conclude that typical LC-MS-based lipidomics methods involve: (1) extraction using chloroform/MeOH or MTBE/MeOH protocols, both with addition of internal standards covering each lipid class; (2) separation of lipids using short microbore columns with sub-2-μm or 2.6–2.8-μm (fused-core) particle size with C18 or C8 sorbent with analysis time <30 min; (3) electrospray ionization in positive- and negative-ion modes with full spectra acquisition using high-resolution MS with capability to MS/MS. Phospholipids (phosphatidylcholines, phosphatidylethanolamines, phosphatidylinositols, phosphatidylserines, phosphatidylglycerols) followed by sphingomyelins, di- and tri-acylglycerols, and ceramides were the most frequently targeted lipid species. PMID:25309011

  5. [Analysis of 7-aminonitrazepam in urine by trimethylsilyl derivatization-gas chromatography/mass spectrometry].

    PubMed

    Zhu, Yu; Tan, Jia-Yi; Sun, Yu-Qing

    2002-09-01

    A highly sensitive method has been developed for the analysis of 7-aminonitrazepam (7-ANIZ), the major metabolite of nitrazepam, in urine by trimethylsilyl derivatization-gas chromatography/mass spectrometry. Urine samples were extracted with ethyl ether-ethyl acetate (99:1, volume ratio). The extracts were derivatized with N,O-bis (trimethylsilyl) trifluoroacetamide, and the total ion current chromatograms of derivatives were acquired. 7-ANIZ was identified by the relative abundance of major characteristic ions in the mass spectrum of its derivative and the retention time of the mass chromatogram peaks of these characteristic ions. Based on the mass chromatogram of the base peak ion, quantification was performed using 7-aminoclonazepam (7-ACLZ) as the internal standard. The extraction efficiency of 7-ANIZ was 82.8%. The linear range was 10 microg/L - 500 microg/L. The limit of detection was 1.2 microg/L and the limit of quantification was 3.5 microg/L. The recoveries were 94.7% - 103.5%, and the RSDs were 3.9% - 5.4%. 7-ANIZ in the urine sample excreted by the subject over 96 h period after oral administration of 10 mg nitrazepam was measured. It is demonstrated that the method can be applied to the forensic identification.

  6. Method for analysis of polar volatile trace components in aqueous samples by gas chromatography.

    PubMed

    Pettersson, Johan; Roeraade, Johan

    2005-05-15

    A new method has been developed for direct analysis of volatile polar trace compounds in aqueous samples by gas chromatography. Water samples are injected onto a short packed precolumn containing anhydrous lithium chloride. A capillary column is coupled in series with the prefractionation column for final separation of the analytes. The enrichment principle of the salt precolumn is reverse to the principles employed in conventional methods such as SPE or SPME in which a sorbent or adsorbent is utilized to trap or concentrate the analytes. Such methods are not efficient for highly polar compounds. In the LiCl precolumn concept, the water matrix is strongly retained on the hygroscopic salt, whereas polar as well as nonpolar volatile organic compounds show very low retention and are eluted ahead of the water. After transfer of the analytes to the capillary column, the retained bulk water is removed by backflushing the precolumn at elevated temperature. For direct injections of 120 microL of aqueous samples, the combined time for injection and preseparation is only 3.5 min. With this procedure, direct repetitive automated analyses of highly volatile polar compounds such as methanol or tetrahydrofuran can be performed, and a limit of quantification in the low parts-per-billion region utilizing a flame ionization detector is demonstrated.

  7. Liquid chromatography-mass spectrometry analysis of diethylcarbamazine in human plasma for clinical pharmacokinetic studies.

    PubMed

    Schmidt, Mark S; King, Christopher L; Thomsen, Edward K; Siba, Peter M; Sanuku, Nelly; Fleckenstein, Lawrence

    2014-09-01

    A sensitive and selective liquid chromatographic method using mass spectrometric detection was developed for the determination of diethylcarbamazine (DEC) in human plasma. DEC and its stable isotope internal standard d3-DEC were extracted from 0.25mL of human plasma using solid phase extraction. Chromatography was performed using a Phenomenex Synergi 4μ Fusion-RP column (2mm×250mm) with gradient elution. The retention time was approximately 4.8min. The assay was linear from 4 to 2200ng/mL. Analysis of quality control samples at 12, 300, and 1700ng/mL (N=15) had interday coefficients of variation of 8.4%, 5.4%, and 6.2%, respectively (N=15). Interday bias results were -2.2%, 6.0%, and 0.8%, respectively. Recovery of DEC from plasma ranged from 84.2% to 90.1%. The method was successfully applied to clinical samples from patients with lymphatic filariasis from a drug-drug interaction study between DEC and albendazole and/or ivermectin.

  8. Analysis of anthraquinones in rhubarb (Rheum palmatum and Rheum officinale) by supercritical fluid chromatography.

    PubMed

    Aichner, Dorothea; Ganzera, Markus

    2015-11-01

    The first report on the separation of five anthraquinones (chrysophanol, physcion, emodin, aloeemodin, and rhein) from rhubarb by supercritical fluid chromatography indicates that this technique is an interesting analytical alternative not just for non-polar substances. Within less than five minutes the compounds could be baseline resolved, using a mobile phase comprising supercritical carbon dioxide and methanol with 0.05% diethylamine. The optimum stationary phase showed to be an Acquity UPC(2) HSS C18 SB 1.8 µm column, operated at a flow rate of 2 ml/min and a temperature of 30 °C. Method validation confirmed that the developed procedure is selective, linear (R(2)≥0.999), accurate (recovery rates: 95.4% to 103.1%), and precise (intra-day≤6.9%, inter-day≤4.7%); the limit of detection was below 0.5 ng on-column. The analysis of plant extracts was feasible with acceptable repeatability (σrel≤3.8%), and it determined 0.3 to 0.7% of free aglyca in the native samples. After hydrolysis according to the European Pharmacopoeia, a rise in the total content up to 2.1% was observed, with rhein being the most dominant derivative in nearly all specimens.

  9. Analysis of perfluorinated carboxylic acids in soils II: optimization of chromatography and extraction.

    PubMed

    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

  10. Separation techniques: Chromatography

    PubMed Central

    Coskun, Ozlem

    2016-01-01

    Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

  11. ENVIRONMENTAL ANALYSIS BY AB INITIO QUANTUM MECHANICAL COMPUTATION AND GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED SPECTROMETRY.

    EPA Science Inventory

    Computational chemistry, in conjunction with gas chromatography/mass spectrometry/Fourier transform infrared spectrometry (GC/MS/FT-IR), was used to tentatively identify seven tetrachlorobutadiene (TCBD) isomers detected in an environmental sample. Computation of the TCBD infrare...

  12. ANALYSIS OF PERFLUORINATED CARBOXYLIC ACIDS IN SOILS II: OPTIMIZATION OF CHROMATOGRAPHY AND EXTRACTION

    EPA Science Inventory

    With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorinated octanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary p...

  13. [Preparation of flavonoid reference standards from Scutellariae Radix under the guidance of high performance liquid chromatography-mass spectrometry analysis].

    PubMed

    Guo, Henan; Yang, Xuedong; Liu, Jun; Zheng, Wenfeng

    2012-07-01

    Flavonoid reference standards were targeted-prepared from Scutellariae Radix under the guidance of high performance liquid chromatography-mass spectrometry (HPLC-MS) analysis. With HPLC-MS analysis of Scutellariae Radix, 19 flavonoid components were identified by analyzing and comparing their retention times, ultraviolet spectra, and mass spectrometry data with literature. The separation and purification protocols of all targeted flavonoid reference standards were optimally designed according to the results of HPLC-MS analysis and related literature. The ethanol extract of Scutellariae Radix was suspended in water and extracted with petroleum ether, ethyl acetate, and n-butanol successively. The ethyl acetate extract and n-butanol extract were separately subjected to primary separation by low pressure reverse phase preparative chromatography. Then the fractions containing targeted compounds were further purified by low pressure reverse and normal phases preparative chromatography. Finally, baicalin and wogonoside reference standards were obtained from n-butanol extract; baicaelin, wogonin, and oroxylin A reference standards were obtained from ethyl acetate extract. The structures of the 5 reference standards were identified by mass spectrometry (MS) and 1H nuclear magnetic resonance (1H NMR) spectroscopy. The HPLC analytical results showed that the purities of the 5 reference standards were all above 98%. It is demonstrated that the rapid targeted-preparation method under the guidance of the HPLC-MS analysis is applicable for the isolation and preparation of chemical components in traditional Chinese medicines.

  14. Comprehensive analysis of pharmaceutical products using simultaneous mixed-mode (ion-exchange/reversed-phase) and hydrophilic interaction liquid chromatography.

    PubMed

    Kazarian, Artaches A; Nesterenko, Pavel N; Soisungnoen, Phimpha; Burakham, Rodjana; Srijaranai, Supalax; Paull, Brett

    2014-08-01

    Liquid chromatographic assays were developed using a mixed-mode column coupled in sequence with a hydrophilic interaction liquid chromatography column to allow the simultaneous comprehensive analysis of inorganic/organic anions and cations, active pharmaceutical ingredients, and excipients (carbohydrates). The approach utilized dual sample injection and valve-mediated column switching and was based upon a single high-performance liquid chromatography gradient pump. The separation consisted of three distinct sequential separation mechanisms, namely, (i) ion-exchange, (ii) mixed-mode interactions under an applied dual gradient (reversed-phase/ion-exchange), and (iii) hydrophilic interaction chromatography. Upon first injection, the Scherzo SS C18 column (Imtakt) provided resolution of inorganic anions and cations under isocratic conditions, followed by a dual organic/salt gradient to elute active pharmaceutical ingredients and their respective organic counterions and potential degradants. At the top of the mixed-mode gradient (high acetonitrile content), the mobile phase flow was switched to a preconditioned hydrophilic interaction liquid chromatography column, and the standard/sample was reinjected for the separation of hydrophilic carbohydrates, some of which are commonly known excipients in drug formulations. The approach afforded reproducible separation and resolution of up to 23 chemically diverse solutes in a single run. The method was applied to investigate the composition of commercial cough syrups (Robitussin®), allowing resolution and determination of inorganic ions, active pharmaceutical ingredients, excipients, and numerous well-resolved unknown peaks.

  15. Enantioselective simultaneous analysis of selected pharmaceuticals in environmental samples by ultrahigh performance supercritical fluid based chromatography tandem mass spectrometry.

    PubMed

    Camacho-Muñoz, Dolores; Kasprzyk-Hordern, Barbara; Thomas, Kevin V

    2016-08-31

    In order to assess the true impact of each single enantiomer of pharmacologically active compounds (PACs) in the environment, highly efficient, fast and sensitive analytical methods are needed. For the first time this paper focuses on the use of ultrahigh performance supercritical fluid based chromatography coupled to a triple quadrupole mass spectrometer to develop multi-residue enantioselective methods for chiral PACs in environmental matrices. This technique exploits the advantages of supercritical fluid chromatography, ultrahigh performance liquid chromatography and mass spectrometry. Two coated modified 2.5 μm-polysaccharide-based chiral stationary phases were investigated: an amylose tris-3,5-dimethylphenylcarbamate column and a cellulose tris-3-chloro-4-methylphenylcarbamate column. The effect of different chromatographic variables on chiral recognition is highlighted. This novel approach resulted in the baseline resolution of 13 enantiomers PACs (aminorex, carprofen, chloramphenicol, 3-N-dechloroethylifosfamide, flurbiprofen, 2-hydroxyibuprofen, ifosfamide, imazalil, naproxen, ofloxacin, omeprazole, praziquantel and tetramisole) and partial resolution of 2 enantiomers PACs (ibuprofen and indoprofen) under fast-gradient conditions (<10 min analysis time). The overall performance of the methods was satisfactory. The applicability of the methods was tested on influent and effluent wastewater samples. To the best of our knowledge, this is the first feasibility study on the simultaneous separation of chemically diverse chiral PACs in environmental matrices using ultrahigh performance supercritical fluid based chromatography coupled with tandem mass spectrometry.

  16. Gas-liquid chromotography of trimethylsilyl and alkyl oxime-trimethylsilyl derivatives of some prostaglandins.

    PubMed

    Middleditch, B S; Desiderio, D M

    1972-08-01

    TMS (trimethylsilyl), MO-TMS (methyl oxime-TMS), and EO-TMS (ethyl oxime-TMS) derivatives of several prostaglandins (A, B1, B2, E1, 8-iso-E1, E2 and 8-iso-E2) were prepared and their gas chromatographic properties examined on a moderately polar (OV-17) and a relatively non-polar (SE-30) stationary phase. Combined gas chromatography-mass spectrometry (GC-MS) using an LKB 9000 instrument was used to identify the different derivatives. Although the TMS derivatives are more easily prepared, the TMS derivatives of the PgE series are thermally somewhat unstable. Thus, MO-TMS and EO-TMS derivatives which exhibit more regular retention increments are more useful for analytical work. The EO-TMS derivatives may be useful in determining mass spectral fragmentation modes of the prostaglandin derivatives.

  17. Multiphase Transport in Porous Media: Gas-Liquid Separation Using Capillary Pressure Gradients International Space Station (ISS) Flight Experiment Development

    NASA Technical Reports Server (NTRS)

    Wheeler, Richard R., Jr.; Holtsnider, John T.; Dahl, Roger W.; Deeks, Dalton; Javanovic, Goran N.; Parker, James M.; Ehlert, Jim

    2013-01-01

    Advances in the understanding of multiphase flow characteristics under variable gravity conditions will ultimately lead to improved and as of yet unknown process designs for advanced space missions. Such novel processes will be of paramount importance to the success of future manned space exploration as we venture into our solar system and beyond. In addition, because of the ubiquitous nature and vital importance of biological and environmental processes involving airwater mixtures, knowledge gained about fundamental interactions and the governing properties of these mixtures will clearly benefit the quality of life here on our home planet. The techniques addressed in the current research involving multiphase transport in porous media and gas-liquid phase separation using capillary pressure gradients are also a logical candidate for a future International Space Station (ISS) flight experiment. Importantly, the novel and potentially very accurate Lattice-Boltzmann (LB) modeling of multiphase transport in porous media developed in this work offers significantly improved predictions of real world fluid physics phenomena, thereby promoting advanced process designs for both space and terrestrial applications.This 3-year research effort has culminated in the design and testing of a zero-g demonstration prototype. Both the hydrophilic (glass) and hydrophobic (Teflon) media Capillary Pressure Gradient (CPG) cartridges prepared during the second years work were evaluated. Results obtained from ground testing at 1-g were compared to those obtained at reduced gravities spanning Martian (13-g), Lunar (16-g) and zero-g. These comparisons clearly demonstrate the relative strength of the CPG phenomena and the efficacy of its application to meet NASAs unique gas-liquid separation (GLS) requirements in non-terrestrial environments.LB modeling software, developed concurrently with the zero-g test effort, was shown to accurately reproduce observed CPG driven gas-liquid separation

  18. Advanced proteomic liquid chromatography

    SciTech Connect

    Xie, Fang; Smith, Richard D.; Shen, Yufeng

    2012-10-26

    Liquid chromatography coupled with mass spectrometry is the predominant platform used to analyze proteomics samples consisting of large numbers of proteins and their proteolytic products (e.g., truncated polypeptides) and spanning a wide range of relative concentrations. This review provides an overview of advanced capillary liquid chromatography techniques and methodologies that greatly improve separation resolving power and proteomics analysis coverage, sensitivity, and throughput.

  19. The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry

    SciTech Connect

    Johnson, Steven

    1999-02-12

    The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

  20. High-Throughput Analysis of Sucrose Fatty Acid Esters by Supercritical Fluid Chromatography/Tandem Mass Spectrometry

    PubMed Central

    Hori, Katsuhito; Tsumura, Kazunobu; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-01-01

    Supercritical fluid chromatography (SFC) coupled with triple quadrupole mass spectrometry was applied to the profiling of sucrose fatty acid esters (SEs). The SFC conditions (column and modifier gradient) were optimized for the effective separation of SEs. In the column test, a silica gel reversed-phase column was selected. Then, the method was used for the detailed characterization of commercial SEs and the successful analysis of SEs containing different fatty acids. The present method allowed for fast and high-resolution separation of monoesters to tetra-esters within a shorter time (15 min) as compared to the conventional high-performance liquid chromatography. The applicability of our method for the analysis of SEs was thus demonstrated. PMID:26819875

  1. Monosaccharide composition analysis of immunomodulatory polysaccharides by on-line hollow fiber microextraction with high-performance liquid chromatography.

    PubMed

    Wang, Nani; Wang, Xuping; Huang, Xiaowen; Mao, Zhujun; Zhang, Yang; Yu, Yong; Shou, Dan

    2016-03-01

    The monosaccharide compositions of functional polysaccharides are essential for structure elucidation and biological activity determination. A sensitive method based on on-line hollow-fiber liquid-phase microextraction with high-performance liquid chromatography has been established for the analysis of ten monosaccharide compositions (two uronic acids, two amino sugars and six neutral sugars) of the immunomodulatory polysaccharides. After derivatization, the sample was injected into the lumen of a hollow fiber immersed in butyl ether and separated by liquid chromatography. Under optimized conditions, the calibration curves were linear (r ≥ 0.9996) in the range of 10-2000 μmol L(-1) . The limits of detection were in the range of 0.04-1.58 μmol L(-1) , and the recoveries were in the range of 92.1-99.6%, which shows that the method is applicable to the analysis of the monosaccharide composition of various polysaccharides.

  2. The Applications and Features of Liquid Chromatography-Mass Spectrometry in the Analysis of Traditional Chinese Medicine

    PubMed Central

    2016-01-01

    With increasingly improved separation of complex samples and detection of unknown material capabilities, liquid chromatography coupled with mass spectrometry (LC-MS) has been widely used in traditional Chinese medicine (TCM) research. This article describes the principles of liquid chromatography (LC) and mass spectrometry (MS) and their advantages and disadvantages in qualitative and quantitative analysis of TCM. We retrieved research literatures about the application of LC-MS in TCM published during the past five years at home and abroad. To better guide the analysis of TCM, this review mainly focuses on the applications category of LC-MS, how often different kinds of LC-MS are used, and the qualitative and quantitative ability of various LC-MS in the study of TCM. PMID:27956918

  3. Impact of growing environment on chickasaw blackberry (Rubus L.) aroma evaluated by gas chromatography olfactometry dilution analysis.

    PubMed

    Wang, Yuanyuan; Finn, Chad; Qian, Michael C

    2005-05-04

    The aroma extract of Chickasaw blackberry (Rubus L.) was separated with silica gel normal phase chromatography into six fractions. Gas chromatography-olfactometry (GCO) was performed on each fraction to identify aroma active compounds. Aroma extraction dilution analysis (AEDA) was employed to characterize the aroma profile of Chickasaw blackberries from two growing regions of the United States: Oregon and Arkansas. Comparative AEDA analysis showed that the berries grown in the two regions had similar aroma compositions; however, those odorants had various aroma impacts in each region. The compounds with high flavor dilution factors in Oregon's Chickasaw were ethyl butanoate, linalool, methional, trans,cis-2,6-nonadienal, cis-1,5-octadien-3-one, and 2,5-dimethyl-4-hydroxy-3(2H)-furanone, whereas in the Chickasaw grown in Arkansas, they were ethyl butanoate, linalool, methional, ethyl 2-methylbutanoate, beta-damascenone, and geraniol.

  4. Extraction and chromatography-mass spectrometric analysis of the active principles from selected Chinese herbs and other medicinal plants.

    PubMed

    Wang, Xiaosuo; Kapoor, Vimal; Smythe, George A

    2003-01-01

    Medicinal herbs have a long history of use in the practice of traditional Chinese medicine and a substantial body of evidence has, over recent decades, demonstrated a range of important pharmacological properties. Western biomedical researchers are examining not only the efficacy of the traditional herbal products but, through the use of a range of bioassays and analytical techniques, are developing improved methods to isolate and characterize active components. This review briefly describes the different extraction methodologies used in the preparation of herbal extracts and reviews the utility of chromatography-mass spectrometry for the analysis of their active components. In particular, applications of gas or liquid chromatography with mass spectrometry for the isolation and characterization of active components of ginseng are critically assessed. The analysis of toxic substances from herb extracts with mass spectrometric techniques is also discussed along with the potential for mass spectrometric methods to investigate the proteomics of herbal extracts.

  5. Recent advances in hydrophilic interaction chromatography for quantitative analysis of endogenous and pharmaceutical compounds in plasma samples.

    PubMed

    Isokawa, Muneki; Kanamori, Takahiro; Funatsu, Takashi; Tsunoda, Makoto

    2014-09-01

    There is an increasing need for new analytical methods that can handle a large number of analytes in complex matrices. Hydrophilic interaction chromatography (HILIC) has recently been demonstrated as an important supplement to reversed-phase liquid chromatography for polar analytes, particularly endogenous compounds. With the increasing popularity of HILIC, progressively more polar phases with diverse functional groups have been developed. In addition, the coupling of HILIC to mass spectrometry offers the advantages of improved sensitivity by employing an organic-rich mobile phase. This article reviews recent applications of HILIC for the analysis of endogenous and pharmaceutical compounds in plasma samples. Furthermore, based on recent studies, we provide a discussion of column selection, sample pretreatment for HILIC analysis, and detection sensitivity.

  6. Analysis of phospholipids in bio-oils and fats by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

    PubMed

    Viidanoja, Jyrki

    2015-09-15

    A new, sensitive and selective liquid chromatography-electrospray ionization-tandem mass spectrometric (LC-ESI-MS/MS) method was developed for the analysis of Phospholipids (PLs) in bio-oils and fats. This analysis employs hydrophilic interaction liquid chromatography-scheduled multiple reaction monitoring (HILIC-sMRM) with a ZIC-cHILIC column. Eight PL class selective internal standards (homologs) were used for the semi-quantification of 14 PL classes for the first time. More than 400 scheduled MRMs were used for the measurement of PLs with a run time of 34min. The method's performance was evaluated for vegetable oil, animal fat and algae oil. The averaged within-run precision and between-run precision were ≤10% for all of the PL classes that had a direct homologue as an internal standard. The method accuracy was generally within 80-120% for the tested PL analytes in all three sample matrices.

  7. Analysis of 23 polycyclic aromatic hydrocarbons in smokeless tobacco by gas chromatography-mass spectrometry

    PubMed Central

    Stepanov, Irina; Villalta, Peter W.; Knezevich, Aleksandar; Jensen, Joni; Hatsukami, Dorothy; Hecht, Stephen S.

    2009-01-01

    Smokeless tobacco contains 28 known carcinogens and causes precancerous oral lesions and oral and pancreatic cancer. A recent study conducted by our research team identified 8 different polycyclic aromatic hydrocarbons (PAH) in U.S. moist snuff, encouraging further investigations of this group of toxicants and carcinogens in smokeless tobacco products. In this study, we developed a gas chromatography-mass spectrometry method that allows simultaneous analysis of 23 various PAH in smokeless tobacco after a simple two-step extraction and purification procedure. The method produced coefficients of variation under 10% for most PAH. The limits of quantitation for different PAH varied between 0.3 ng/g tobacco and 11 ng/g tobacco, starting with a 300-mg sample. The recovery of the stable isotope-labeled internal standards averaged 87%. The method was applied to analysis of 23 moist snuff samples that include various flavors of the most popular U.S. moist snuff brands, as well as 17 samples representing the currently marketed brands of spit-free tobacco pouches, a relatively new type of smokeless tobacco. The sum of all detected PAH in conventional moist snuff averaged 11.6 (± 3.7) µg/g dry weight, 20% of this amount being comprised by carcinogenic PAH. The levels of PAH in new spit-free tobacco products were much lower than those in moist snuff, the sum of all detected PAH averaging 1.3 (±0.28) µg/g dry weight. Our findings render PAH one of the most prevalent groups of carcinogens in smokeless tobacco, along with tobacco-specific nitrosamines. Urgent measures are required from the U.S. tobacco industry to modify manufacturing processes so that the levels of these toxicants and carcinogens in the U.S. moist snuff are greatly reduced. PMID:19860436

  8. Using computer simulation to assist in the robustness analysis of an ion-exchange chromatography step.

    PubMed

    Jakobsson, Niklas; Karlsson, David; Axelsson, Jan Peter; Zacchi, Guido; Nilsson, Bernt

    2005-01-21

    This paper presents a methodology to gain process knowledge and assist in the robustness analysis of an ion-exchange step in a protein purification process using a model-based approach. Factorial experimental design is common practice in industry today to obtain robustness characterization of unit operations with respect to variations in process parameters. This work aims at providing a better insight into what process variations affect quality and to further reduce the experimental work to the regions of process variation that are of most interest. This methodology also greatly increases the ability to predict process performance and promotes process understanding. The model calibration part of the methodology involves three consecutive steps to calibrate a steric mass action (SMA) ion-exchange chromatography model. Firstly, a number of gradient elution experiments are performed. Secondly, experimental breakthrough curves have to be generated for the proteins if the adsorption capacity of the medium for each component is not known. Thirdly, a multi-component loading experiment is performed to calibrate the multi-component effects that cannot be determined from the single-component experiments. The separation process studied in this work is the separation of polyclonal IgG from a mixture containing IgG, myoglobin and BSA. The calibrated model is used to simulate six process variations in a full factorial experiment. The results of the simulations provide information about the importance of the different process variations and the simulations are also used to determine the crucial points for the process parameter variations. The methodology can be used to assist in the robustness analysis normally performed in the pharmaceutical industry today as it is able to predict the impact on process performance resulting from variations in salt concentration, column load, protein concentration and flow rate.

  9. Analysis of 23 polycyclic aromatic hydrocarbons in smokeless tobacco by gas chromatography-mass spectrometry.

    PubMed

    Stepanov, Irina; Villalta, Peter W; Knezevich, Aleksandar; Jensen, Joni; Hatsukami, Dorothy; Hecht, Stephen S

    2010-01-01

    Smokeless tobacco contains 28 known carcinogens and causes precancerous oral lesions and oral and pancreatic cancer. A recent study conducted by our research team identified eight different polycyclic aromatic hydrocarbons (PAHs) in U.S. moist snuff, encouraging further investigations of this group of toxicants and carcinogens in smokeless tobacco products. In this study, we developed a gas chromatography-mass spectrometry method that allows simultaneous analysis of 23 various PAHs in smokeless tobacco after a simple two-step extraction and purification procedure. The method produced coefficients of variation under 10% for most PAHs. The limits of quantitation for different PAHs varied between 0.3 and 11 ng/g tobacco, starting with a 300 mg sample. The recovery of the stable isotope-labeled internal standards averaged 87%. The method was applied to analysis of 23 moist snuff samples that included various flavors of the most popular U.S. moist snuff brands, as well as 17 samples representing the currently marketed brands of spit-free tobacco pouches, a relatively new type of smokeless tobacco. The sum of all detected PAHs in conventional moist snuff averaged 11.6 (+/-3.7) microg/g dry weight; 20% of this amount was comprised of carcinogenic PAHs. The levels of PAHs in new spit-free tobacco products were much lower than those in moist snuff; the sum of all detected PAHs averaged 1.3 (+/-0.28) microg/g dry weight. Our findings render PAHs one of the most prevalent groups of carcinogens in smokeless tobacco. Urgent measures are required from the U.S. tobacco industry to modify manufacturing processes so that the levels of these toxicants and carcinogens in U.S. moist snuff are greatly reduced.

  10. Analysis of epinephrine, norepinephrine, and dopamine in urine samples of hospital patients by micellar liquid chromatography.

    PubMed

    García Ferrer, Daniel; García García, Aurelio; Peris-Vicente, Juan; Gimeno-Adelantado, José Vicente; Esteve-Romero, Josep

    2015-12-01

    An analytical method based on micellar liquid chromatography was developed to determine the concentration of three catecholamines (epinephrine, norepinephrine, and dopamine) in urine. The detection of these compounds in urine can be useful to diagnose several diseases, related to stress and sympathoadrenal system dysfunction, using a non-invasive collection procedure. The sample pretreatment was a simple dilution in a micellar solution, filtration, and direct injection, thus avoiding time-consuming and tedious extraction steps. Therefore, there is no need to use an internal standard. The three catecholamines were eluted using a C18 column and a mobile phase of 0.055 M sodium dodecyl sulfate-1.5% methanol buffered at pH 3.8 running at 1.5 mL/min under isocratic mode in less than 25 min. The detection was performed by amperometry applying a constant potential of +0.5 V. The procedure was validated following the guidelines of the European Medicines Agency in terms of the following: calibration range (0.09-5 μg/mL), linearity (r(2) > 0.9995), limit of detection (0.02 μg/mL), within- and between-run accuracy (-6.5 to +8.4%) and precision (<10.2%), dilution integrity, matrix effect, robustness (<8.4), and stability. The obtained values were below those required by the guide. The method was rapid, easy-to-handle, eco-friendly, and safe and provides reliable quantitative data, and is thus useful for routine analysis. The procedure was applied to the analysis of epinephrine, norepinephrine, and dopamine in urine samples from patients of a local hospital.

  11. Analysis of polar urinary metabolites for metabolic phenotyping using supercritical fluid chromatography and mass spectrometry.

    PubMed

    Sen, Arundhuti; Knappy, Christopher; Lewis, Matthew R; Plumb, Robert S; Wilson, Ian D; Nicholson, Jeremy K; Smith, Norman W

    2016-06-03

    Supercritical fluid chromatography (SFC) is frequently used for the analysis and separation of non-polar metabolites, but remains relatively underutilised for the study of polar molecules, even those which pose difficulties with established reversed-phase (RP) or hydrophilic interaction liquid chromatographic (HILIC) methodologies. Here, we present a fast SFC-MS method for the analysis of medium and high-polarity (-7≤cLogP≤2) compounds, designed for implementation in a high-throughput metabonomics setting. Sixty polar analytes were first screened to identify those most suitable for inclusion in chromatographic test mixtures; then, a multi-dimensional method development study was conducted to determine the optimal choice of stationary phase, modifier additive and temperature for the separation of such analytes using SFC. The test mixtures were separated on a total of twelve different column chemistries at three different temperatures, using CO2-methanol-based mobile phases containing a variety of polar additives. Chromatographic performance was evaluated with a particular emphasis on peak capacity, overall resolution, peak distribution and repeatability. The results suggest that a new generation of stationary phases, specifically designed for improved robustness in mixed CO2-methanol mobile phases, can improve peak shape, peak capacity and resolution for all classes of polar analytes. A significant enhancement in chromatographic performance was observed for these urinary metabolites on the majority of the stationary phases when polar additives such as ammonium salts (formate, acetate and hydroxide) were included in the organic modifier, and the use of water or alkylamine additives was found to be beneficial for specific subsets of polar analytes. The utility of these findings was confirmed by the separation of a mixture of polar metabolites in human urine using an optimised 7min gradient SFC method, where the use of the recommended column and co

  12. Analysis of free amino acids in natural waters by liquid chromatography-tandem mass spectrometry.

    PubMed

    How, Zuo Tong; Busetti, Francesco; Linge, Kathryn L; Kristiana, Ina; Joll, Cynthia A; Charrois, Jeffrey W A

    2014-11-28

    This paper reports a new analytical method for the analysis of 18 amino acids in natural waters using solid-phase extraction (SPE) followed by liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS) operated in multiple reaction monitoring mode. Two different preconcentration methods, solid-phase extraction and concentration under reduced pressure, were tested in development of this method. Although concentration under reduced pressure provided better recoveries and method limits of detection for amino acids in ultrapure water, SPE was a more suitable extraction method for real samples due to the lower matrix effects for this method. Even though the strong cation exchange resin used in SPE method introduced exogenous matrix interferences into the sample extracts (inorganic salt originating from the acid-base reaction during the elution step), the SPE method still incorporates a broad sample clean-up and minimised endogenous matrix effects by reducing interferences originating from real water samples. The method limits of quantification (MLQ) for the SPE LC-MS/MS method in ultrapure water ranged from 0.1 to 100 μg L(-1) as N for the different amino acids. The MLQs of the early eluting amino acids were limited by the presence of matrix interfering species, such as inorganic salts in natural water samples. The SPE LC-MS/MS method was successfully applied to the analysis of amino acids in 3 different drinking water source waters: the average total free amino acid content in these waters was found to be 19 μg L(-1) as N, while among the 18 amino acids analysed, the most abundant amino acids were found to be tyrosine, leucine and isoleucine.

  13. Trend analysis of performance parameters of pre-packed columns for protein chromatography over a time span of ten years.

    PubMed

    Scharl, Theresa; Jungreuthmayer, Christian; Dürauer, Astrid; Schweiger, Susanne; Schröder, Tim; Jungbauer, Alois

    2016-09-23

    Pre-packed small scale chromatography columns are increasingly used for process development, for determination of design space in bioprocess development, and for post-licence process verifications. The packing quality of 30,000 pre-packed columns delivered to customers over a period 10 years has been analyzed by advanced statistical tools. First, the data were extracted and checked for inconsistencies, and then were tabulated and made ready for statistical processing using the programming language Perl (https://www.perl.org/) and the statistical computing environment R (https://www.r-project.org/). Reduced HETP and asymmetry were plotted over time to obtain a trend of packing quality over 10 years. The obtained data were used as a visualized coefficient of variation analysis (VCVA), a process that has often been applied in other industries such as semiconductor manufacturing. A typical fluctuation of reduced HETP was seen. A Tsunami effect in manufacturing, the effect of propagation of manufacturing deviations leading to out-of-specification products, was not observed with these pre-packed columns. Principal component analysis (PCA) showed that all packing materials cluster. Our data analysis showed that the current commercially available chromatography media used for biopharmaceutical manufacturing can be reproducibly and uniformly packed in polymer-based chromatography columns, which are designed for ready-to-use purposes. Although the number of packed columns has quadrupled over one decade the packing quality has remained stable.

  14. Analysis of therapeutic proteins and peptides using multiangle light scattering coupled to ultra high performance liquid chromatography.

    PubMed

    Espinosa-de la Garza, Carlos E; Miranda-Hernández, Mariana P; Acosta-Flores, Lilia; Pérez, Néstor O; Flores-Ortiz, Luis F; Medina-Rivero, Emilio

    2015-05-01

    Analysis of the physical properties of biotherapeutic proteins is crucial throughout all the stages of their lifecycle. Herein, we used size-exclusion ultra high performance liquid chromatography coupled to multiangle light scattering and refractive index detection systems to determine the molar mass, mass-average molar mass, molar-mass dispersity and hydrodynamic radius of two monoclonal antibodies (rituximab and trastuzumab), a fusion protein (etanercept), and a synthetic copolymer (glatiramer acetate) employed as models. A customized instrument configuration was set to diminish band-broadening effects and enhance sensitivity throughout detectors. The customized configuration showed a performance improvement with respect to the high-performance liquid chromatography standard configuration, as observed by a 3 h column conditioning and a higher resolution analysis in 20 min. Analysis of the two monoclonal antibodies showed averaged values of 148.0 kDa for mass-average molar mass and 5.4 nm for hydrodynamic radius, whereas for etanercept these values were 124.2 kDa and 6.9 nm, respectively. Molar-mass dispersity was 1.000 on average for these proteins. Regarding glatiramer acetate, a molar mass range from 3 to 45 kDa and a molar-mass dispersity of 1.304 were consistent with its intrinsic peptide diversity, and its mass-average molar mass was 10.4 kDa. Overall, this method demonstrated an accurate determination of molar mass, overcoming the difficulties of size-exclusion chromatography.

  15. Mathematical Simulation of Unsteady-State Gas-Liquid Mixture Flow in a Bed-Well System

    NASA Astrophysics Data System (ADS)

    Abbasov, É. M.; Imamaliev, S. A.

    2016-09-01

    Based on theoretical investigations, the influence of various forms of pressure variation at the wellhead with a nonstationary flow of a two-phase fluid in a bed-well system on the character of change in the bottom-hole pressure has been investigated, which makes it possible to determine this pressure from the wellhead operation parameters. The trapezoidal form of the change in pressure is considered as an example. The coupled equations of filtration and the equations describing nonstationary motion of a gas-liquid mixture in a pipeline have been solved jointly. Analytical formulas have been obtained allowing one to determine the bottom-hole pressure from the technological parameters at the wellhead with account for the dynamic connection of the bed-well system at different forms of change in the wellhead pressure. The influence of the wellhead pressure pulsation frequencies on the bottom-hole pressure dynamics has been established.

  16. Optical and application study of gas-liquid discharge excited by bipolar nanosecond pulse in atmospheric air

    NASA Astrophysics Data System (ADS)

    Wang, Sen; Wang, Wen-chun; Yang, De-zheng; Liu, Zhi-jie; Zhang, Shuai

    2014-10-01

    In this study, a bipolar nanosecond pulse with 20 ns rising time is employed to generate air gas-liquid diffuse discharge plasma with room gas temperature in quartz tube at atmospheric pressure. The image of the discharge and optical emission spectra of active species in the plasma are recorded. The plasma gas temperature is determined to be approximately 390 K by compared the experimental spectra with the simulated spectra, which is slightly higher than the room temperature. The result indicated that the gas temperature rises gradually with pulse peak voltage increasing, while decreases slightly with the electrode gap distance increasing. As an important application, bipolar nanosecond pulse discharge is used to sterilize the common microorganisms (Actinomycetes, Candida albicans and Escherichia coli) existing in drinking water, which performs high sterilization efficiency.

  17. Slug front gas entrainment in gas-liquid two-phase horizontal flow using hi-speed slug-tracking

    NASA Astrophysics Data System (ADS)

    Zadrazil, Ivan; Matar, Omar; Markides, Christos

    2013-11-01

    A gas-liquid flow regime where liquid-continuous regions travel at high speeds (i.e. slugs) through a pipe separated by regions of stratified flow (i.e. elongated bubbles) is referred to as a ``slug flow.'' This regime is characterised by the turbulent entrainment of gas into the slug front body. We use a high-speed camera mounted on a moving robotic linear rail to track the formation of naturally occurring slugs over 150 pipe diameters. We show that the dynamics of the slugs become progressively more complex with increasing liquid and gas Reynolds numbers. Based on the slug-tracking visualization we present, over a range of conditions: (i) phenomenological observations of the formation and development of slugs, and (ii) statistical data on the slug velocity and gas entrainment rate into the slug body. EPSRC Programme Grant EP/K003976/1.

  18. Flow Injection Analysis and Liquid Chromatography for Multifunctional Chemical Analysis (MCA) Systems

    ERIC Educational Resources Information Center

    Mayo, Ana V.; Loegel, Thomas N.; Bretz, Stacey Lowery; Danielson, Neil D.

    2013-01-01

    The large class sizes of first-year chemistry labs makes it challenging to provide students with hands-on access to instrumentation because the number of students typically far exceeds the number of research-grade instruments available to collect data. Multifunctional chemical analysis (MCA) systems provide a viable alternative for large-scale…

  19. [CFD numerical simulation onto the gas-liquid two-phase flow behavior during vehicle refueling process].

    PubMed

    Chen, Jia-Qing; Zhang, Nan; Wang, Jin-Hui; Zhu, Ling; Shang, Chao

    2011-12-01

    With the gradual improvement of environmental regulations, more and more attentions are attracted to the vapor emissions during the process of vehicle refueling. Research onto the vehicle refueling process by means of numerical simulation has been executed abroad since 1990s, while as it has never been involved so far domestically. Through reasonable simplification about the physical system of "Nozzle + filler pipe + gasoline storage tank + vent pipe" for vehicle refueling, and by means of volume of fluid (VOF) model for gas-liquid two-phase flow and Re-Normalization Group kappa-epsilon turbulence flow model provided in commercial computational fluid dynamics (CFD) software Fluent, this paper determined the proper mesh discretization scheme and applied the proper boundary conditions based on the Gambit software, then established the reasonable numerical simulation model for the gas-liquid two-phase flow during the refueling process. Through discussing the influence of refueling velocity on the static pressure of vent space in gasoline tank, the back-flowing phenomenon has been revealed in this paper. It has been demonstrated that, the more the flow rate and the refueling velocity of refueling nozzle is, the higher the gross static pressure in the vent space of gasoline tank. In the meanwhile, the variation of static pressure in the vent space of gasoline tank can be categorized into three obvious stages. When the refueling flow rate becomes higher, the back-flowing phenomenon of liquid gasoline can sometimes be induced in the head section of filler pipe, thus making the gasoline nozzle pre-shut-off. Totally speaking, the theoretical work accomplished in this paper laid some solid foundation for self-researching and self-developing the technology and apparatus for the vehicle refueling and refueling emissions control domestically.

  20. EPA CRL MS014: Analysis of Aldicarb, Bromadiolone, Carbofuran, Oxamyl and Methomyl in Water by Multiple Reaction Monitoring Liquid Chromatography / Tandem Mass Spectrometry (LC/MS/MS)

    EPA Pesticide Factsheets

    Method MS014 describes procedures for solvent extraction of aldicarb, bromadiolone, carbofuran, oxamyl and methomyl from water samples, followed by analysis using liquid chromatography tandem mass spectrometry (LC-MS-MS).