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Sample records for gas chromatographic separation

  1. Fast gas chromatographic separation of biodiesel.

    SciTech Connect

    Pauls, R. E.

    2011-05-01

    A high-speed gas chromatographic method has been developed to determine the FAME distribution of B100 biodiesel. The capillary column used in this work has dimensions of 20 m x 0.100 mm and is coated with a polyethylene glycol film. Analysis times are typically on the order of 4-5 min depending upon the composition of the B100. The application of this method to a variety of vegetable and animal derived B100 is demonstrated. Quantitative results obtained with this method were in close agreement with those obtained by a more conventional approach on a 100 m column. The method, coupled with solid-phase extraction, was also found suitable to determine the B100 content of biodiesel-diesel blends.

  2. Gas chromatographic separation of hydrogen isotopes using metal hydrides

    SciTech Connect

    Aldridge, F.T.

    1984-05-09

    A study was made of the properties of metal hydrides which may be suitable for use in chromatographic separation of hydrogen isotopes. Sixty-five alloys were measured, with the best having a hydrogen-deuterium separation factor of 1.35 at 60/sup 0/C. Chromatographic columns using these alloys produced deuterium enrichments of up to 3.6 in a single pass, using natural abundance hydrogen as starting material. 25 references, 16 figures, 4 tables.

  3. Chiral porous organic frameworks for asymmetric heterogeneous catalysis and gas chromatographic separation.

    PubMed

    Dong, Jinqiao; Liu, Yan; Cui, Yong

    2014-12-11

    Three chiral robust diene-based porous organic frameworks (POFs) are prepared. POF- is shown to be an efficient heterogeneous catalyst after metallation for asymmetric conjugation addition with up to 93% ee, and it can also function as a new chiral stationary phase for gas chromatographic separation of racemates.

  4. Gas Chromatograph.

    DTIC Science & Technology

    Patents, * Gas chromotography , *Hydrocarbons, *Carbon monoxide, *Carbon dioxide, *Water, Field equipment, Portable equipment, Sensitivity, Halogenated hydrocarbons, Test methods, Gases, Liquids, Purity

  5. Microminiature gas chromatograph

    DOEpatents

    Yu, C.M.

    1996-12-10

    A microminiature gas chromatograph ({mu}GC) comprising a least one silicon wafer, a gas injector, a column, and a detector. The gas injector has a normally closed valve for introducing a mobile phase including a sample gas in a carrier gas. The valve is fully disposed in the silicon wafer(s). The column is a microcapillary in silicon crystal with a stationary phase and is mechanically connected to receive the mobile phase from the gas injector for the molecular separation of compounds in the sample gas. The detector is mechanically connected to the column for the analysis of the separated compounds of sample gas with electronic means, e.g., ion cell, field emitter and PIN diode. 7 figs.

  6. Microminiature gas chromatograph

    DOEpatents

    Yu, Conrad M.

    1996-01-01

    A microminiature gas chromatograph (.mu.GC) comprising a least one silicon wafer, a gas injector, a column, and a detector. The gas injector has a normally closed valve for introducing a mobile phase including a sample gas in a carrier gas. The valve is fully disposed in the silicon wafer(s). The column is a microcapillary in silicon crystal with a stationary phase and is mechanically connected to receive the mobile phase from the gas injector for the molecular separation of compounds in the sample gas. The detector is mechanically connected to the column for the analysis of the separated compounds of sample gas with electronic means, e.g., ion cell, field emitter and PIN diode.

  7. Chromatographic hydrogen isotope separation

    DOEpatents

    Aldridge, Frederick T.

    1981-01-01

    Intermetallic compounds with the CaCu.sub.5 type of crystal structure, particularly LaNiCo.sub.4 and CaNi.sub.5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors.

  8. Chromatographic hydrogen isotope separation

    DOEpatents

    Aldridge, F.T.

    Intermetallic compounds with the CaCu/sub 5/ type of crystal structure, particularly LaNiCo/sub 4/ and CaNi/sub 5/, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen cn produce large quantities of heavy water at an effective cost for use in heavy water reactors.

  9. Gas Chromatographic Separation of an Acetylene Vinyl Fluoride-Difluoroethane Mixture on Triethylene Glycol and Silicone Oil,

    DTIC Science & Technology

    The purpose of the research was to study gas-chromatographic separation of impurities of acetylene and difluoroethane in vinyl fluoride obtained by...and difluoroethane . All the components are separated, and the criteria of separation of acetylene-vinyl fluoride and vinyl fluoride- difluoroethane

  10. Development of micromachined preconcentrators and gas chromatographic separation columns by an electroless gold plating technology

    NASA Astrophysics Data System (ADS)

    Kuo, C.-Y.; Chen, P.-S.; Chen, H.-T.; Lu, C.-J.; Tian, W.-C.

    2017-03-01

    In this study, a simple process for fabricating a novel micromachined preconcentrator (μPCT) and a gas chromatographic separation column (μSC) for use in a micro gas chromatograph (μGC) using one photomask is described. By electroless gold plating, a high-surface-area gold layer was deposited on the surface of channels inside the μPCT and μSC. For this process, (3-aminopropyl) trimethoxysilane (APTMS) was used as a promoter for attaching gold nanoparticles on a silicon substrate to create a seed layer. For this purpose, a gold sodium sulfite solution was used as reagent for depositing gold to form heating structures. The microchannels of the μPCT and μSC were coated with the adsorbent and stationary phase, Tenax-TA and polydimethylsiloxane (DB-1), respectively. μPCTs were heated at temperatures greater than 280 °C under an applied electrical power of 24 W and a heating rate of 75 °C s‑1. Repeatable thermal heating responses for μPCTs were achieved; good linearity (R 2  >  0.9997) was attained at three heating rates for the temperature programme for the μSC (0.2, 0.5 and 1 °C s‑1). The volatile organic compounds (VOCs) toluene and m-xylene were concentrated over the μPCT by rapid thermal desorption (peak width of half height (PWHH)  <1.5 s) preconcentration factors for both VOCs are  >7900. The VOCs acetone, benzene, toluene, m-xylene and 1,3,5-trimethylbenzene were also separated on the μSC as evidenced by their different retention times (47–184 s).

  11. Graphitic carbon nitride as high-resolution stationary phase for gas chromatographic separations.

    PubMed

    Zheng, Yunzhong; Qi, Meiling; Fu, Ruonong

    2016-07-08

    This work presents the first example of utilization of graphitic carbon nitride (g-C3N4) as stationary phase for capillary gas chromatographic (GC) separations. The statically coated g-C3N4 column showed the column efficiencies of 3760 plates/m and weak polarity. Its resolving capability and retention behaviours were investigated by using the Grob test mixture, and mixtures of diverse types of analytes, and structural and positional isomers. The results showed superior separation performance of the g-C3N4 stationary phase for some critical analytes and preferential retention for aromatic analytes. Specifically, it exhibited high-resolution capability for aromatic and aliphatic isomers such as methylnaphthalenes and dimethylnaphthalenes, phenanthrene and anthracene and alkane isomers. In addition, g-C3N4 column showed excellent thermal stability up to 280°C and good repeatability with relative standard deviation (RSD) values less than 0.09% for intra-day, below 0.23% for inter-day and in the range of 1.9-8.4% for between-column, respectively. The advantageous separation performance shows the potential of g-C3N4 and related materials as stationary phase in GC and other separation technologies.

  12. Anion exchange chromatographic separation of inositol phosphates and their quantification by gas chromatography.

    PubMed

    Heathers, G P; Juehne, T; Rubin, L J; Corr, P B; Evers, A S

    1989-01-01

    The direct measurement of mass of inositol trisphosphate from biologic samples is described. Separation of inositol monophosphate, bisphosphate, trisphosphate, and inositol tetrakisphosphate was achieved using anion exchange chromatography with a sodium sulfate gradient. In addition, separation of the isomers of each inositol phosphate was performed using HPLC procedures. The individual inositol phosphate fractions were subsequently dephosphorylated and desalted. The myo-inositol from each fraction was then derivatized to the hexatrimethylsilyl derivative and the myo-inositol derivatives were quantified by a novel gas chromatographic analysis using the hexatrimethylsilyl derivative of chiro-inositol as an internal concentration reference. This method is a reproducible and relatively rapid procedure for the direct quantification of inositol phosphate mass which overcomes many of the problems associated with the use of radiolabeled precursors. The method is a significant improvement over existing procedures for the quantitative determination of the mass of inositol phosphate by virtue of improved recovery, sensitivity, and technical simplicity. The applicability of this method is illustrated by the quantitative determination of inositol trisphosphate in response to norepinephrine stimulation of adult canine myocytes and cerebral cortical brain slices and by measurement of the isomers of inositol trisphosphate in isolated myocytes.

  13. Comprehensive two-dimensional gas chromatographic separations with a microfabricated thermal modulator.

    PubMed

    Serrano, Gustavo; Paul, Dibyadeep; Kim, Sung-Jin; Kurabayashi, Katsuo; Zellers, Edward T

    2012-08-21

    Rapid, comprehensive two-dimensional gas chromatographic (GC × GC) separations by use of a microfabricated midpoint thermal modulator (μTM) are demonstrated, and the effects of various μTM design and operating parameters on performance are characterized. The two-stage μTM chip consists of two interconnected spiral etched-Si microchannels (4.2 and 2.8 cm long) with a cross section of 250 × 140 μm(2), an anodically bonded Pyrex cap, and a cross-linked wall coating of poly(dimethylsiloxane) (PDMS). Integrated heaters provide rapid, sequential heating of each μTM stage, while a proximate, underlying thermoelectric cooler provides continual cooling. The first-dimension column used for GC × GC separations was a 6 m long, 250 μm i.d. capillary with a PDMS stationary phase, and the second-dimension column was a 0.5 m long, 100 μm i.d. capillary with a poly(ethylene glycol) phase. Using sets of five to seven volatile test compounds (boiling point ≤174 °C), the effects of the minimum (T(min)) and maximum (T(max)) modulation temperature, stage heating lag/offset (O(s)), modulation period (P(M)), and volumetric flow rate (F) on the quality of the separations were evaluated with respect to several performance metrics. Best results were obtained with a T(min) = -20 °C, T(max) = 210 °C, O(s) = 600 ms, P(M) = 6 s, and F = 0.9 mL/min. Replicate modulated peak areas and retention times were reproducible to <5%. A structured nine-component GC × GC chromatogram was produced, and a 21 component separation was achieved in <3 min. The potential for creating portable μGC × μGC systems is discussed.

  14. Optimisation of temperature-programmed gas chromatographic separation of organochloride pesticides by response surface methodology.

    PubMed

    D'Archivio, Angelo Antonio; Maggi, Maria Anna; Marinelli, Cristina; Ruggieri, Fabrizio; Stecca, Fabrizio

    2015-12-04

    A response surface methodology (RSM) approach is applied to optimise the temperature-programme gas-chromatographic separation of 16 organochloride pesticides, including 12 compounds identified as highly toxic chemicals by the Stockholm Convention on Persistent Organic Pollutants. A three-parameter relationship describing both linear and curve temperature programmes is derived adapting a model previously used in literature to describe concentration gradients in liquid chromatography with binary eluents. To investigate the influence of the three temperature profile descriptors (the starting temperature, the gradient duration and a shape parameter), a three-level full-factorial design of experiments is used to identify suitable combinations of the above variables spanning over a useful domain. Resolutions of adjacent peaks are the responses modelled by RSM using two alternative methods: a multi-layer artificial network (ANN) and usual polynomial regression. The proposed ANN-based approach permits to model simultaneously the resolutions of all the consecutive analyte pairs as a function of the temperature profile descriptors. Four critical pairs giving partially overlapped peaks are identified and multiresponse optimisation is carried out by analysing the surface plot of a global resolution defined as the average of the resolutions of the critical pairs. Descriptive/predictive performance and applicability of the ANN and polynomial RSM methods are compared and discussed.

  15. Deconvolution of gas chromatographic data

    NASA Technical Reports Server (NTRS)

    Howard, S.; Rayborn, G. H.

    1980-01-01

    The use of deconvolution methods on gas chromatographic data to obtain an accurate determination of the relative amounts of each material present by mathematically separating the merged peaks is discussed. Data were obtained on a gas chromatograph with a flame ionization detector. Chromatograms of five xylenes with differing degrees of separation were generated by varying the column temperature at selected rates. The merged peaks were then successfully separated by deconvolution. The concept of function continuation in the frequency domain was introduced in striving to reach the theoretical limit of accuracy, but proved to be only partially successful.

  16. Stable hydrogen isotopic analysis of nanomolar molecular hydrogen by automatic multi-step gas chromatographic separation.

    PubMed

    Komatsu, Daisuke D; Tsunogai, Urumu; Kamimura, Kanae; Konno, Uta; Ishimura, Toyoho; Nakagawa, Fumiko

    2011-11-15

    We have developed a new automated analytical system that employs a continuous flow isotope ratio mass spectrometer to determine the stable hydrogen isotopic composition (δD) of nanomolar quantities of molecular hydrogen (H(2)) in an air sample. This method improves previous methods to attain simpler and lower-cost analyses, especially by avoiding the use of expensive or special devices, such as a Toepler pump, a cryogenic refrigerator, and a special evacuation system to keep the temperature of a coolant under reduced pressure. Instead, the system allows H(2) purification from the air matrix via automatic multi-step gas chromatographic separation using the coolants of both liquid nitrogen (77 K) and liquid nitrogen + ethanol (158 K) under 1 atm pressure. The analytical precision of the δD determination using the developed method was better than 4‰ for >5 nmol injections (250 mL STP for 500 ppbv air sample) and better than 15‰ for 1 nmol injections, regardless of the δD value, within 1 h for one sample analysis. Using the developed system, the δD values of H(2) can be quantified for atmospheric samples as well as samples of representative sources and sinks including those containing small quantities of H(2) , such as H(2) in soil pores or aqueous environments, for which there is currently little δD data available. As an example of such trace H(2) analyses, we report here the isotope fractionations during H(2) uptake by soils in a static chamber. The δD values of H(2) in these H(2)-depleted environments can be useful in constraining the budgets of atmospheric H(2) by applying an isotope mass balance model.

  17. Gas chromatographic separation of diastereomeric isoprenoids as molecular markers of oil pollution.

    PubMed

    Berthou, F; Friovourt, M P

    1981-12-18

    By means of high-performance glass capillary gas chromatography (GC), diastereomeric isoprenoids were resolved into double peaks. The retention indices on three liquid phases and the mass spectra of the diastereoisomers were almost similar. The leading GC peaks represent the isoprenoids of fossil origin, while the rear peaks correspond to those of recent origin. Computerized gas chromatography-mass spectrometry was used for fingerprinting isoprenoids in different samples. The mass fragmentation patterns were characteristic of the branched alkanes. Hydrocarbon mixtures from four crude oil spills in the sea and from polluted and oil-free oyster tissues were investigated. The relative ratios of n-alkanes/pristane or phytane were shown to be strongly dependent on the chromatographic resolution of the isoprenoid peaks. It is suggested that the double GC peaks in the isoprenoid series are an unmistakable sign of oil pollution.

  18. Gas chromatograph injection system

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.; Henderson, M. E.; Donaldson, R. W., Jr. (Inventor)

    1975-01-01

    An injection system for a gas chromatograph is described which uses a small injector chamber (available in various configurations). The sample is placed in the chamber while the chamber is not under pressure and is not heated, and there is no chance of leakage caused by either pressure or heat. It is injected into the apparatus by changing the position of a valve and heating the chamber, and is volatilized and swept by a carrier gas into the analysis apparatus.

  19. Cyclotriveratrylene as a new-type stationary phase for gas chromatographic separations of halogenated compounds and isomers.

    PubMed

    Lv, Qing; Zhang, Qing; Qi, Meiling; Bai, Hua; Ma, Qiang; Meng, Xianshuang; Fu, Ruonong

    2015-07-24

    Cyclotriveratrylene (CTV) is reported here for the first time as stationary phase for capillary gas chromatographic (GC) separations. CTV stationary phase showed weak polarity comparable to the conventional 5% phenyl polysiloxane stationary phase but exhibited different retention behaviours and higher resolution for some of the indicated analytes. Most importantly, CTV stationary phase exhibited preferential selectivity for halogenated compounds, positional and geometrical isomers. Effect of column temperature on retention and thermal stability of CTV column were also investigated. Moreover, CTV capillary column showed good repeatability in terms of run-to-run, day-to-day and column-to-column. The unique physicochemical features and efficient separation ability for analytes of close properties show the potential of CTV as a new-type stationary phase in GC as well as separation science.

  20. Single-walled carbon nanotubes as stationary phase in gas chromatographic separation and determination of argon, carbon dioxide and hydrogen.

    PubMed

    Safavi, Afsaneh; Maleki, Norooz; Doroodmand, Mohammad Mahdi

    2010-08-24

    A chromatographic technique is introduced based on single-walled carbon nanotubes (SWCNTs) as stationary phase for separation of Ar, CO(2) and H(2) at parts per million (ppm) levels. The efficiency of SWCNTs was compared with solid materials such as molecular sieve, charcoal, multi-walled carbon nanotubes and carbon nanofibers. The morphology of SWCNTs was optimized for maximum adsorption of H(2), CO(2) and Ar and minimum adsorption of gases such as N(2), O(2), CO and H(2)O vapour. To control temperature of the gas chromatography column, peltier cooler was used. Mixtures of Ar, CO(2) and H(2) were separated according to column temperature program. Relative standard deviation for nine replicate analyses of 0.2 mL H(2) containing 10 microL of each Ar or CO(2) was 2.5% for Ar, 2.8% for CO(2) and 3.6% for H(2). The interfering effects of CO, and O(2) were investigated. Working ranges were evaluated as 40-600 ppm for Ar, 30-850 ppm for CO(2) and 10-1200 ppm for H(2). Significant sensitivity, small relative standard deviation (RSD) and acceptable limit of detection (LOD) were obtained for each analyte, showing capability of SWCNTs for gas separation and determination processes. Finally, the method was used to evaluate the contents of CO(2) in air sample.

  1. Comprehensive two-dimensional gas chromatographic separations with a temperature programmed microfabricated thermal modulator.

    PubMed

    Collin, William R; Nuñovero, Nicolas; Paul, Dibyadeep; Kurabayashi, Katsuo; Zellers, Edward T

    2016-04-29

    Comprehensive two-dimensional gas chromatography (GC×GC) with a temperature-programmed microfabricated thermal modulator (μTM) is demonstrated. The 0.78 cm(2), 2-stage μTM chip with integrated heaters and a PDMS coated microchannel was placed in thermal contact with a solid-state thermoelectric cooler and mounted on top of a bench scale GC. It was fluidically coupled through heated interconnects to an upstream first-dimension ((1)D) PDMS-coated capillary column and a downstream uncoated capillary or second-dimension ((2)D) PEG-coated capillary. A mixture of n-alkanes C6-C10 was separated isothermally and the full-width-at-half-maximum (fwhm) values of the modulated peaks were assessed as a function of the computer-controlled minimum and maximum stage temperatures of μTM, Tmin and Tmax, respectively. With Tmin and Tmax fixed at -25 and 100°C, respectively, modulated peaks of C6 and C7 had fwhm values<53 ms while the modulated peaks of C10 had a fwhm value of 1.3s, due to inefficient re-mobilization. With Tmin and Tmax fixed at 0 and 210°C, respectively, the fwhm value for the modulated C10 peaks decreased to 67 ms, but C6 and C7 exhibited massive breakthrough. By programming Tmin from -25 to 0°C and Tmax from 100 to 220°C, the C6 and C7 peaks had fwhm values≤50 ms, and the fwhm for C10 peaks remained<95 ms. Using the latter conditions for the GC×GC separation of a sample of unleaded gasoline yielded resolution similar to that reported with a commercial thermal modulator. Replacing the PDMS phase in the μTM with a trigonal-tricationic room temperature ionic liquid eliminated the bleed observed with the PDMS, but also reduced the capacity for several test compounds. Regardless, the demonstrated capability to independently temperature program this low resource μTM enhances its versatility and its promise for use in bench-scale GC×GC systems.

  2. A low-power pressure-and temperature-programmed separation system for a micro gas chromatograph.

    SciTech Connect

    Sacks, Richard D. (University of Michigan, Ann Arbor, MI); Robinson, Alex Lockwood (Advanced Sensor Technologies, Albuquerque, NM); Lambertus, Gordon R. (University of Michigan, Ann Arbor, MI); Potkay, Joseph A. (University of Michigan, Ann Arbor, MI); Wise, Kensall D. (University of Michigan, Ann Arbor, MI)

    2006-10-01

    This thesis presents the theory, design, fabrication and testing of the microvalves and columns necessary in a pressure- and temperature-programmed micro gas chromatograph ({micro}GC). Two microcolumn designs are investigated: a bonded Si-glass column having a rectangular cross section and a vapor-deposited silicon oxynitride (Sion) column having a roughly circular cross section. Both microcolumns contain integrated heaters and sensors for rapid, controlled heating. The 3.2 cm x 3.2 cm, 3 m-long silicon-glass column, coated with a non-polar polydimethylsiloxane (PDMS) stationary phase, separates 30 volatile organic compounds (VOCs) in less than 6 min. This is the most efficient micromachined column reported to date, producing greater than 4000 plates/m. The 2.7 mm x 1.4 mm Sion column eliminates the glass sealing plate and silicon substrate using deposited dielectrics and is the lowest power and fastest GC column reported to date; it requires only 11 mW to raise the column temperature by 100 C and has a response time of 11s and natural temperature ramp rate of 580 C/min. A 1 m-long PDMS-coated Sion microcolumn separates 10 VOCs in 52s. A system-based design approach was used for both columns.

  3. A Small-Scale Low-Cost Gas Chromatograph

    ERIC Educational Resources Information Center

    Gros, Natasa; Vrtacnik, Margareta

    2005-01-01

    The design and application of a small-scale portable gas chromatograph for learning of the basic concepts of chromatography is described. The apparatus consists of two basic separable units, which includes a chromatographic unit and an electronic unit.

  4. Gas chromatographic separation of fatty acid esters of cholesterol and phytosterols on an ionic liquid capillary column.

    PubMed

    Hammann, Simon; Vetter, Walter

    2015-12-15

    Steryl esters are high molecular weight compounds (600-700g/mol) regularly present as a minor lipid class in animal and plant lipids. Different sterol backbones (e.g., cholesterol, β-sitosterol and brassicasterol) which can be esterified with various fatty acids can result in highly complex steryl ester patterns in food samples. The gas chromatographic (GC) analysis of intact steryl esters is challenging, since high elution temperatures are required for their elution. On nonpolar GC phases, steryl esters with fatty acids with differing degree of unsaturation (e.g., oleate and linoleate) cannot be separated and there are only few polar columns available with sufficient temperature stability. In this study, we used gas chromatography with mass spectrometry (GC/MS) and analyzed intact steryl esters on a commercial room temperature ionic liquid (RTIL) column which was shortened to a length of 12m. The column separated the steryl esters both by total carbon number and by degree of unsaturation of the fatty acid. For instance, cholesteryl esters with stearic acid (18:0), oleic acid (18:1n-9), linoleic acid (18:2n-6) and α-linolenic acid (18:3n-3) could be resolved (R≥1.3) from each other. By analysis of synthesized standard substances, the elution orders for different steryl backbones and different fatty acids on a given sterol backbone could be determined. Analysis of spreads and plant oils allowed to determine retention times for 37 steryl esters, although a few co-elutions were observed. The ionic liquid column proved to be well-suited for the analysis of intact steryl esters.

  5. High performance liquid chromatographic separations of gas oil samples and their hydrotreated products using commercial normal phases.

    PubMed

    Oro, Nicole E; Lucy, Charles A

    2011-10-28

    Three commercially available high performance liquid chromatography columns are used in normal phase or quasi-normal phase mode for the separation of gas oil samples. The columns are tested with 20 analytical standards to determine their suitability for separations of petroleum samples and their ability to separate the nitrogen group-types (pyrrole and pyridine) found in petroleum. The columns studied are polymeric hypercrosslinked polystyrene (HGN), a biphenyl phase, and a Chromegabond "DNAP" column from ES Industries. The HGN column separates gas oils based on both ring structure and heteroatom, while the biphenyl phase has low retention of most compounds studied in quasi-normal phase mode. The "DNAP" column is selective for nitrogen-containing compounds, separating them from PAHs as well as oxygen and sulphur compounds. Retention data of standards on all three columns is shown, along with chromatograms of gas oil samples on the HGN and "DNAP" columns.

  6. Hand-held multiple system gas chromatograph

    DOEpatents

    Yu, Conrad M.

    2001-01-01

    A multiple parallel hand-held gas chromatograph (GC) system which includes several independent GCs. Each independent GC has its own injector, separation column, detector and oven and the GCs are mounted in a light weight hand-held assembly. Each GC operates independently and simultaneously. Because of different coatings in different separation columns, different retention times for the same gas will be measured. Thus, for a GC system with multiple parallel GCs, the system can measure, in a short period, different retention times and provide a cross-reference in the determination of the measured gas and to become a two-dimensional system for direct field use.

  7. Dual liquid and gas chromatograph system

    DOEpatents

    Gay, D.D.

    A chromatographic system is described that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a nontransparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extreme low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

  8. Dual liquid and gas chromatograph system

    DOEpatents

    Gay, Don D.

    1985-01-01

    A chromatographic system that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a non-transparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extremely low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

  9. Direct quantitative gas chromatographic separation of C2-C6 fatty acids, methanol, and ethyl alcohol in aqueous microbial fermentation media.

    PubMed

    Rogosa, M; Love, L L

    1968-02-01

    A method is described for the direct quantitative gas chromatographic separation of C(2)-C(6) lower fatty acid homologues, methanol, and ethyl alcohol in aqueous microbial fermentation media. A hydrogen flame detector and a single-phase solid column packing, comprising beads of a polyaromatic resin (polystyrene cross-linked with divinyl benzene), were employed. Direct injections of 1 to 10 muliters of aqueous culture supernatant fluids were made. Quantitative recoveries of C(2)-C(6) acids added to culture supernatant fluids were obtained.

  10. Direct Quantitative Gas Chromatographic Separation of C2-C6 Fatty Acids, Methanol, and Ethyl Alcohol in Aqueous Microbial Fermentation Media

    PubMed Central

    Rogosa, M.; Love, L. L.

    1968-01-01

    A method is described for the direct quantitative gas chromatographic separation of C2-C6 lower fatty acid homologues, methanol, and ethyl alcohol in aqueous microbial fermentation media. A hydrogen flame detector and a single-phase solid column packing, comprising beads of a polyaromatic resin (polystyrene cross-linked with divinyl benzene), were employed. Direct injections of 1 to 10 μliters of aqueous culture supernatant fluids were made. Quantitative recoveries of C2-C6 acids added to culture supernatant fluids were obtained. PMID:5645415

  11. Gas chromatographic separation of nitrogen, oxygen, argon, and carbon monoxide using custom-made porous polymers from high purity divinylbenzene

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.; Ohara, D.; Hollis, O. L.

    1984-01-01

    Existing porous polymers were surveyed for their ability to separate the subject gases. Certain products that showed more promise than others were synthesized and the existing synthetic procedures studied and modified to produce new polymers with enhanced ability to separate the subject gases. Evaluation of the porous polymers was carried out practically by gas chromatography at ambient temperature. The modified synthetic procedures were somewhat simpler than the originals. The new porous polymers made with high purity divinylbenzene enabled use of shorter columns to obtain the separations desired.

  12. Gas separating

    DOEpatents

    Gollan, Arye Z.

    1990-12-25

    Feed gas is directed tangentially along the non-skin surface of gas separation membrane modules comprising a cylindrical bundle of parallel contiguous hollow fibers supported to allow feed gas to flow from an inlet at one end of a cylindrical housing through the bores of the bundled fibers to an outlet at the other end while a component of the feed gas permeates through the fibers, each having the skin side on the outside, through a permeate outlet in the cylindrical casing.

  13. Gas separating

    DOEpatents

    Gollan, Arye

    1988-01-01

    Feed gas is directed tangentially along the non-skin surface of gas separation membrane modules comprising a cylindrical bundle of parallel contiguous hollow fibers supported to allow feed gas to flow from an inlet at one end of a cylindrical housing through the bores of the bundled fibers to an outlet at the other end while a component of the feed gas permeates through the fibers, each having the skin side on the outside, through a permeate outlet in the cylindrical casing.

  14. Chromatographic Separation of Glucose and Fructose

    NASA Astrophysics Data System (ADS)

    Kuptsevich, Yu E.; Larionov, Oleg G.; Stal'naya, I. D.; Nakhapetyan, L. A.; Pronin, A. Ya

    1987-03-01

    The structures, mutarotation, and the physicochemical properties of glucose and fructose as well as methods for their separation are examined. Their chromatographic separation on cation exchangers in the calcium-form is discussed in detail. A theory of the formation of complexes of carbohydrates with metal cations is described and the mechanism of the separation of glucose and fructose on cation exchangers in the calcium-form is discussed in detail. Factors influencing the chromatographic separation of glucose and fructose on sulphonic acid cation-exchange resins are also considered. The bibliography includes 138 references.

  15. Fabrication of zeolitic imidazolate framework-8-methacrylate monolith composite capillary columns for fast gas chromatographic separation of small molecules.

    PubMed

    Yusuf, Kareem; Badjah-Hadj-Ahmed, Ahmed Yacine; Aqel, Ahmad; ALOthman, Zeid Abdullah

    2015-08-07

    A composite zeolitic imidazolate framework-8 (ZIF-8) with a butyl methacrylate-co-ethylene dimethacrylate (BuMA-co-EDMA) monolithic capillary column (33.5cm long×250μm i.d.) was fabricated to enhance the separation efficiency of methacrylate monoliths toward small molecules using conventional low-pressure gas chromatography in comparison with a neat butyl methacrylate-co-ethylene dimethacrylate (BuMA-co-EDMA) monolithic capillary column (33.5cm long×250μm i.d.). The addition of 10mgmL(-1) ZIF-8 micro-particles increased the BET surface area of BuMA-co-EDMA by 3.4-fold. A fast separation of five linear alkanes in 36s with high resolution (Rs≥1.3) was performed using temperature program. Isothermal separation of the same sample also showed a high efficiency (3315platesm(-1) for octane) at 0.89min. Moreover, the column was able to separate skeletal isomers, such as iso-octane/octane and 2-methyl octane/nonane. In addition, an iso-butane/iso-butylene gas mixture was separated at ambient temperature. Comparison with an open tubular TR-5MS column (30m long×250μm i.d.) revealed the superiority of the composite column in separating the five-membered linear alkane mixture with 4-5 times increase in efficiency and a total separation time of 0.89min instead of 4.67min. A paint thinner sample was fully separated using the composite column in 2.43min with a good resolution (Rs≥0.89). The perfect combination between the polymeric monolith, with its high permeability, and ZIF-8, with its high surface area and flexible 0.34nm pore openings, led to the fast separation of small molecules with high efficiency and opened a new horizon in GC applications.

  16. Gas chromatographic separation of stereoisomers of non-protein amino acids on modified γ-cyclodextrin stationary phase.

    PubMed

    Fox, Stefan; Strasdeit, Henry; Haasmann, Stephan; Brückner, Hans

    2015-09-11

    Stereoisomers (enantiomers and diastereoisomers) of synthetic, non-protein amino acids comprising α-, β-, and γ-amino acids, including α,α-dialkyl amino acids, were converted into the respective N-trifluoroacetyl-O-methyl esters and analyzed and resolved by gas chromatography (GC) on a commercial fused silica capillary column coated with the chiral stationary phase octakis(3-O-butyryl-2,6-di-O-pentyl)-γ-cyclodextrin. This column is marketed under the trade name Lipodex(®) E. Chromatograms, retention times, and a chart displaying the retention times of approximately 40 stereoisomers of amino acids are presented. With few exceptions, baseline or almost baseline resolution was achieved for enantiomers and diastereoisomers. The chromatographic method presented is considered to be highly suitable for the elucidation of the stereochemistry of non-protein amino acids, for example in natural products, and for evaluating the enantiopurity of genetically non-coded amino acids used for the synthesis and design of conformationally tailored peptides. The method is applicable to extraterrestrial materials or can be used in experimental work related to abiotic syntheses or enantioselective destruction and amplification of amino acids.

  17. Chromatographic Separation of Vitamin E Enantiomers.

    PubMed

    Fu, Ju-Yen; Htar, Thet-Thet; De Silva, Leanne; Tan, Doryn Meam-Yee; Chuah, Lay-Hong

    2017-02-04

    Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

  18. Separation of the fatty acids in menhaden oil as methyl esters with a highly polar ionic liquid gas chromatographic column and identification by time of flight mass spectrometry.

    PubMed

    Fardin-Kia, Ali Reza; Delmonte, Pierluigi; Kramer, John K G; Jahreis, Gerhard; Kuhnt, Katrin; Santercole, Viviana; Rader, Jeanne I

    2013-12-01

    The fatty acids contained in marine oils or products are traditionally analyzed by gas chromatography using capillary columns coated with polyethylene glycol phases. Recent reports indicate that 100 % cyanopropyl siloxane phases should also be used when the analyzed samples contain trans fatty acids. We investigated the separation of the fatty acid methyl esters prepared from menhaden oil using the more polar SLB-IL111 (200 m × 0.25 mm) ionic liquid capillary column and the chromatographic conditions previously optimized for the separation of the complex mixture of fatty acid methyl esters prepared from milk fat. Identifications of fatty acids were achieved by applying Ag(+)-HPLC fractionation and GC-TOF/MS analysis in CI(+) mode with isobutane as the ionization reagent. Calculation of equivalent chain lengths confirmed the assignment of double bond positions. This methodology allowed the identification of 125 fatty acids in menhaden oil, including isoprenoid and furanoid fatty acids, and the novel 7-methyl-6-hexadecenoic and 7-methyl-6-octadecenoic fatty acids. The chromatographic conditions applied in this study showed the potential of separating in a single 90-min analysis, among others, the short chain and trans fatty acids contained in dairy products, and the polyunsaturated fatty acids contained in marine products.

  19. Gas separating

    DOEpatents

    Gollan, A.

    1988-03-29

    Feed gas is directed tangentially along the non-skin surface of gas separation membrane modules comprising a cylindrical bundle of parallel contiguous hollow fibers supported to allow feed gas to flow from an inlet at one end of a cylindrical housing through the bores of the bundled fibers to an outlet at the other end while a component of the feed gas permeates through the fibers, each having the skin side on the outside, through a permeate outlet in the cylindrical casing. 3 figs.

  20. Gas separating

    DOEpatents

    Gollan, A.Z.

    1990-12-25

    Feed gas is directed tangentially along the non-skin surface of gas separation membrane modules comprising a cylindrical bundle of parallel contiguous hollow fibers supported to allow feed gas to flow from an inlet at one end of a cylindrical housing through the bores of the bundled fibers to an outlet at the other end while a component of the feed gas permeates through the fibers, each having the skin side on the outside, through a permeate outlet in the cylindrical casing. 3 figs.

  1. Versatile gas/particle ion chromatograph.

    PubMed

    Ullah, S M Rahmat; Takeuchi, Masaki; Dasgupta, Purnendu K

    2006-02-01

    A new, compact gas/particle ion chromatograph has been developed for measuring ionic constituents in PM2.5 (particulate matter of aerodynamic diameter < or = 2.5 microm) and water-soluble ionogenic gases. The instrument has separate sampling channels for gases and particles. In one, a membrane denuder collects soluble gases for preconcentration and analysis. In the other, a cyclone removes larger particles, a membrane denuder removes soluble gases, and a continuously wetted hydrophilic filter collects particles. A single, multiport, syringe pump handles liquid transport, and one conductivity detector measures anions and ammonium for both channels. Electrodialytically generated gradient hydroxide eluent permits 20 min chromatographic runs. Gas/particle samples are each collected for 40 min, butthe sampling intervals are staggered by 20 min. Liquid samples from the gas denuder and particle collector are aspirated and preconcentrated on sequential cation and anion concentrators and transferred respectively to an ammonia transfer device and an anion separation column. The flow configuration results in an ammonium peak before anion peaks in the chromatogram. The system measures ammonia, organic acids (such as acetic, formic, and oxalic acids), HCl, HONO, SO2, HNO3, and the corresponding ions in the aerosol phase. Low ng/m3 to sub-ng/m3 limits of detection (LODs) are attained for most common gases and particulate constituents, the LODs for gaseous SO2 to NH3 range, for example, from sub parts per trillion by volume (sub-pptv) to approximately 5 pptv.

  2. High performance hand-held gas chromatograph

    SciTech Connect

    Yu, C.M.

    1998-04-28

    The Microtechnology Center of Lawrence Livermore National Laboratory has developed a high performance hand-held, real time detection gas chromatograph (HHGC) by Micro-Electro-Mechanical-System (MEMS) technology. The total weight of this hand-held gas chromatograph is about five lbs., with a physical size of 8{close_quotes} x 5{close_quotes} x 3{close_quotes} including carrier gas and battery. It consumes about 12 watts of electrical power with a response time on the order of one to two minutes. This HHGC has an average effective theoretical plate of about 40k. Presently, its sensitivity is limited by its thermal sensitive detector at PPM. Like a conventional G.C., this HHGC consists mainly of three major components: (1) the sample injector, (2) the column, and (3) the detector with related electronics. The present HHGC injector is a modified version of the conventional injector. Its separation column is fabricated completely on silicon wafers by means of MEMS technology. This separation column has a circular cross section with a diameter of 100 pm. The detector developed for this hand-held GC is a thermal conductivity detector fabricated on a silicon nitride window by MEMS technology. A normal Wheatstone bridge is used. The signal is fed into a PC and displayed through LabView software.

  3. Determination of methyl mercury by aqueous phase Eehylation, followed by gas chromatographic separation with cold vapor atomic fluorescence detection

    USGS Publications Warehouse

    De Wild, John F.; Olsen, Mark L.; Olund, Shane D.

    2002-01-01

    A recent national sampling of streams in the United States revealed low methyl mercury concentrations in surface waters. The resulting median and mean concentrations, calculated from 104 samples, were 0.06 nanograms per liter (ng/L) and 0.15 ng/L, respectively. This level of methyl mercury in surface water in the United States has created a need for analytical techniques capable of detecting sub-nanogram per liter concentrations. In an attempt to create a U.S. Geological Survey approved method, the Wisconsin District Mercury Laboratory has adapted a distillation/ethylation/ gas-phase separation method with cold vapor atomic fluorescence spectroscopy detection for the determination of methyl mercury in filtered and unfiltered waters. This method is described in this report. Based on multiple analyses of surface water and ground-water samples, a method detection limit of 0.04 ng/L was established. Precision and accuracy were evaluated for the method using both spiked and unspiked ground-water and surface-water samples. The percent relative standard deviations ranged from 10.2 to 15.6 for all analyses at all concentrations. Average recoveries obtained for the spiked matrices ranged from 88.8 to 117 percent. The precision and accuracy ranges are within the acceptable method-performance limits. Considering the demonstrated detection limit, precision, and accuracy, the method is an effective means to quantify methyl mercury in waters at or below environmentally relevant concentrations

  4. Capillary gas chromatographic separation of organic bases using a pH-adjusted basic water stationary phase.

    PubMed

    Darko, Ernest; Thurbide, Kevin B

    2016-09-23

    The use of a pH-adjusted water stationary phase for analyzing organic bases in capillary gas chromatography (GC) is demonstrated. Through modifying the phase to typical values near pH 11.5, it is found that various organic bases are readily eluted and separated. Conversely, at the normal pH 7 operating level, they are not. Sodium hydroxide is found to be a much more stable base than ammonium hydroxide for altering the pH due to the higher volatility and evaporation of the latter. In the basic condition, such analytes are not ionized and are observed to produce good peak shapes even for injected masses down to about 20ng. By comparison, analyses on a conventional non-polar capillary GC column yield more peak tailing and only analyte masses of 1μg or higher are normally observed. Through carefully altering the pH, it is also found that the selectivity between analytes can be potentially further enhanced if their respective pKa values differ sufficiently. The analysis of different pharmaceutical and petroleum samples containing organic bases is demonstrated. Results indicate that this approach can potentially offer unique and beneficial selectivity in such analyses.

  5. Separation of short-chain fatty acids on a gas chromatographic column coated with oxidized lubricating oil.

    PubMed

    Moustafa, Nagy Emam

    2007-07-01

    The oxidized lubricating naphthenic base oil was used as a stationary phase for the separation of short-chain free fatty acids (SFFA) either as a pure sample or an aqueous solution containing 0.9-1.2 mg/L of each acid. It is found that the oil oxidation for 20 h improved the separation of SFFA in these two sample forms. This separation improvement represents not only the increase in retention volume intervals and peak symmetries in case of the pure sample but also in acid peak areas in case of the aqueous solution sample.

  6. Gas chromatographic separation of hydrogen isotopes on columns packed with alumina, modified alumina and sol-gel alumina.

    PubMed

    Naik, Y P; Gupta, N K; Pillai, K T; Rao, G A Rama; Venugopal, V

    2012-01-06

    The stationary phase of alumina adsorbents, prepared by different chemical processes, was used to study the separation behaviour of hydrogen isotopes. Three types of alumina, obtained by conventional hydroxide route alumina coated with silicon oxide and alumina prepared by internal gelation process (IGP), were used as packing material to study the separation of HT and T(2) in a mixture at various temperatures. The conventional alumina and silicon oxide coated alumina resolved HT and T(2) at 77K temperature with different retention times. The retention times on SiO(2) coated columns were found to be higher than those of other adsorbents. However, the column filled with IGP alumina was found to be ideal for the separation of HT and T(2) at 240 K. The peaks were well resolved in less than 5 min on this column.

  7. Gas chromatographic analysis of trace gas impurities in tungsten hexafluoride.

    PubMed

    Laurens, J B; de Coning, J P; Swinley, J M

    2001-03-09

    Highly reactive fluorinated gaseous matrices require special equipment and techniques for the gas chromatographic analysis of trace impurities in these gases. The impurities that were analysed at the low-microg/l levels included oxygen, nitrogen, carbon dioxide, carbon monoxide, sulfur hexafluoride and hydrogen. This paper describes the use of a system utilising backflush column switching to protect the columns and detectors in the analysis of trace gas impurities in tungsten hexafluoride. Two separate channels were used for the analysis of H2, O2, N2, CO, CO2 and SF6 impurities with pulsed discharge helium ionisation detection.

  8. A Quantitative Gas Chromatographic Ethanol Determination.

    ERIC Educational Resources Information Center

    Leary, James J.

    1983-01-01

    Describes a gas chromatographic experiment for the quantitative determination of volume percent ethanol in water ethanol solutions. Background information, procedures, and typical results are included. Accuracy and precision of results are both on the order of two percent. (JN)

  9. Packed multi-channels for parallel chromatographic separations in microchips.

    PubMed

    Nagy, Andrea; Gaspar, Attila

    2013-08-23

    Here we report on a simple method to fabricate microfluidic chip incorporating multi-channel systems packed by conventional chromatographic particles without the use of frits. The retaining effectivities of different bottlenecks created in the channels were studied. For the parallel multi-channel chromatographic separations several channel patterns were designed. The obtained multipackings were applied for parallel separations of dyes. The implementation of several chromatographic separation units in microscopic size makes possible faster and high throughput separations.

  10. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    SciTech Connect

    Liu, Ying

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  11. 40 CFR 1065.267 - Gas chromatograph.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas...

  12. 40 CFR 1065.267 - Gas chromatograph.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 33 2011-07-01 2011-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas...

  13. Portable gas chromatograph-mass spectrometer

    DOEpatents

    Andresen, Brian D.; Eckels, Joel D.; Kimmons, James F.; Myers, David W.

    1996-01-01

    A gas chromatograph-mass spectrometer (GC-MS) for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units.

  14. Portable gas chromatograph-mass spectrometer

    DOEpatents

    Andresen, B.D.; Eckels, J.D.; Kimmons, J.F.; Myers, D.W.

    1996-06-11

    A gas chromatograph-mass spectrometer (GC-MS) is described for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units. 4 figs.

  15. Portable gas chromatograph-mass spectrometer

    SciTech Connect

    Andresen, B.D.; Eckels, J.D.; Kimmins, J.F.; Myers, D.W.

    1994-12-31

    A gas chromatograph-mass spectrometer (GC-MS) for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units.

  16. Gas chromatograph-mass spectrometer (GC/MS) system for quantitative analysis of reactive chemical compounds

    DOEpatents

    Grindstaff, Quirinus G.

    1992-01-01

    Described is a new gas chromatograph-mass spectrometer (GC/MS) system and method for quantitative analysis of reactive chemical compounds. All components of such a GC/MS system external to the oven of the gas chromatograph are programmably temperature controlled to operate at a volatilization temperature specific to the compound(s) sought to be separated and measured.

  17. Numerical Simulation of an Optical Chromatographic Separator

    DTIC Science & Technology

    2009-02-02

    its close relative, Bacillus thuringiensis ," Anal. Chem. 78, 3221-3225 (2006). 10. S. J. Hart, A. Terray, K. L. Kuhn, J. Arnold, and T. A. Leski...Terray, T. A. Leski, J. Arnold, and R. Stroud, "Discovery of a significant optical chromatographic difference between spores of Bacillus anthracis and

  18. High-separation efficiency micro-fabricated multi-capillary gas chromatographic columns for simulants of the nerve agents and blister agents

    NASA Astrophysics Data System (ADS)

    Li, Yi; Du, Xiaosong; Wang, Yang; Tai, Huiling; Qiu, Dong; Lin, Qinghao; Jiang, Yadong

    2014-05-01

    To achieve both high speed and separation efficiency in the separation of a mixture of nerve and blister agent simulants, a high-aspect-ratio micro-fabricated multi-capillary column (MCC, a 50-cm-long, 450-μm-deep, and 60-μm-wide four-capillary column) was fabricated by the application of the microelectromechanical system (MEMS) techniques. Mixtures of chemical warfare agent (CWA) simulants - dimethyl methylphosphonate (DMMP), triethyl phosphate (TEP), and methyl salicylate - were used as samples. The fabricated MCC allowed for the separation of all the components of the gaseous mixture within 24 s, even when the difference in boiling point was 4°C, as in the case of TEP and methyl salicylate. Furthermore, interfering agents - dichloromethane, ethanol, and toluene - were also included in the subsequent gaseous mixture samples. The boiling point of these six components ranged from 78°C to 219°C. All six components were clearly separated within 70 s. This study is the first to report the clear separation of gas mixtures of components with close boiling points. The column efficiency was experimentally determined to be 12,810 plates/m.

  19. High-separation efficiency micro-fabricated multi-capillary gas chromatographic columns for simulants of the nerve agents and blister agents

    PubMed Central

    2014-01-01

    To achieve both high speed and separation efficiency in the separation of a mixture of nerve and blister agent simulants, a high-aspect-ratio micro-fabricated multi-capillary column (MCC, a 50-cm-long, 450-μm-deep, and 60-μm-wide four-capillary column) was fabricated by the application of the microelectromechanical system (MEMS) techniques. Mixtures of chemical warfare agent (CWA) simulants - dimethyl methylphosphonate (DMMP), triethyl phosphate (TEP), and methyl salicylate - were used as samples. The fabricated MCC allowed for the separation of all the components of the gaseous mixture within 24 s, even when the difference in boiling point was 4°C, as in the case of TEP and methyl salicylate. Furthermore, interfering agents - dichloromethane, ethanol, and toluene - were also included in the subsequent gaseous mixture samples. The boiling point of these six components ranged from 78°C to 219°C. All six components were clearly separated within 70 s. This study is the first to report the clear separation of gas mixtures of components with close boiling points. The column efficiency was experimentally determined to be 12,810 plates/m. PMID:24899869

  20. Detection system for a gas chromatograph

    DOEpatents

    Hayes, John M.; Small, Gerald J.

    1984-01-01

    A method and apparatus are described for the quantitative analysis of vaporizable compounds, and in particular of polycyclic aromatic hydrocarbons which may be induced to fluoresce. The sample to be analyzed is injected into a gas chromatography column and is eluted through a narrow orifice into a vacuum chamber. The free expansion of the eluted sample into the vacuum chamber creates a supersonic molecular beam in which the sample molecules are cooled to the extent that the excited vibrational and rotational levels are substantially depopulated. The cooled molecules, when induced to fluoresce by laser excitation, give greatly simplified spectra suitable for analytical purposes. The laser induced fluorimetry provides great selectivity, and the gas chromatograph provides quantitative transfer of the sample to the molecular beam.

  1. FTIR gas chromatographic analysis of perfumes

    NASA Astrophysics Data System (ADS)

    Diederich, H.; Stout, Phillip J.; Hill, Stephen L.; Krishnan, K.

    1992-03-01

    Perfumes, natural or synthetic, are complex mixtures consisting of numerous components. Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) techniques have been extensively utilized for the analysis of perfumes and essential oils. A limited number of perfume samples have also been analyzed by FT-IR gas chromatographic (GC-FTIR) techniques. Most of the latter studies have been performed using the conventional light pipe (LP) based GC-FTIR systems. In recent years, cold-trapping (in a matrix or neat) GC-FTIR systems have become available. The cold-trapping systems are capable of sub-nanogram sensitivities. In this paper, comparison data between the LP and the neat cold-trapping GC- FTIR systems is presented. The neat cold-trapping interface is known as Tracer. The results of GC-FTIR analysis of some commercial perfumes is also presented. For comparison of LP and Tracer GC-FTIR systems, a reference (synthetic) mixture containing 16 major and numerous minor constituents was used. The components of the mixture are the compounds commonly encountered in commercial perfumes. The GC-FTIR spectra of the reference mixture was obtained under identical chromatographic conditions from an LP and a Tracer system. A comparison of the two sets of data thus generated do indeed show the enhanced sensitivity level of the Tracer system. The comparison also shows that some of the major components detected by the Tracer system were absent from the LP data. Closer examination reveals that these compounds undergo thermal decomposition on contact with the hot gold surface that is part of the LP system. GC-FTIR data were obtained for three commercial perfume samples. The major components of these samples could easily be identified by spectra search against a digitized spectral library created using the Tracer data from the reference mixture.

  2. Asymmetric gas separation membranes

    SciTech Connect

    Malon, R. F.; Zampini, A.

    1984-12-04

    Asymmetric gas separation membranes of materials having selective permeation of at least one gas of a gaseous mixture over that of one or more remaining gases of the gaseous mixture, exhibit significantly improved permeation selectivities for the at least one gas when the asymmetric membrane is contacted on one or both surfaces with an effective amount of a Lewis acid. The improved asymmetric gas separation membranes, process for producing the improved membrane, and processes utilizing such membranes for selectively separating at least one gas from a gaseous mixture by permeation are disclosed.

  3. Asymmetric gas separation membranes

    SciTech Connect

    Malon, R. F.; Zampini, A.

    1984-09-18

    Asymmetric gas separation membranes of materials having selective permeation of at least one gas of a gaseous mixture over that of one or more remaining gases of the gaseous mixture, exhibit significantly improved permeation selectivities for the at least one gas when the asymmetric membrane is contacted on one or both surfaces with an effective amount of a Br nsted-Lowry acid. The improved asymmetric gas separation membranes, process for producing the improved membrane, and processes utilizing such membranes for selectively separating at least one gas from a gaseous mixture by permeation are disclosed.

  4. Gas Chromatographic Detectors for Exobiology Flight Experiments

    NASA Technical Reports Server (NTRS)

    Kojiro, Daniel R.; Humphry, Donald E.; Takeuchi, Nori; Chang, Sherwood (Technical Monitor)

    1997-01-01

    Exobiology flight experiments require highly sensitive instrumentation for in situ chemical analysis of the volatile chemical species that occur in the atmospheres and surfaces of various bodies within the solar system. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. Future missions to Mars', comets, or planetary moons such as Europa, will perform experiments with complex analyses. In addition, instrumentation for such missions must perform under severely restricted conditions with limited resources. To meet these analytical requirements, improved methods and highly sensitive yet smaller instruments must continually be developed with increasingly greater capabilities. We describe here efforts to achieve this objective, for past and future missions, through the development of new or the improvement of existing sensitive, miniaturized gas chromatographic detectors.

  5. Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

    ERIC Educational Resources Information Center

    Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

    2008-01-01

    Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

  6. Characterization of Gas Chromatographic Liquid Phases Using McReynolds Constants. An Experiment for Instrumental Analysis Laboratory.

    ERIC Educational Resources Information Center

    Erskine, Steven R.; And Others

    1986-01-01

    Describes a laboratory experiment that is designed to aid in the understanding of the fundamental process involved in gas chromatographic separations. Introduces the Kovats retention index system for use by chemistry students to establish criteria for the optimal selection of gas chromatographic stationary phases. (TW)

  7. On-line gas chromatographic analysis of airborne particles

    DOEpatents

    Hering, Susanne V [Berkeley, CA; Goldstein, Allen H [Orinda, CA

    2012-01-03

    A method and apparatus for the in-situ, chemical analysis of an aerosol. The method may include the steps of: collecting an aerosol; thermally desorbing the aerosol into a carrier gas to provide desorbed aerosol material; transporting the desorbed aerosol material onto the head of a gas chromatography column; analyzing the aerosol material using a gas chromatograph, and quantizing the aerosol material as it evolves from the gas chromatography column. The apparatus includes a collection and thermal desorption cell, a gas chromatograph including a gas chromatography column, heated transport lines coupling the cell and the column; and a quantization detector for aerosol material evolving from the gas chromatography column.

  8. Cation exchange chromatographic elution and separation of rubidium

    SciTech Connect

    Mehta, V.P.; Khopkar, S.M.

    1982-01-01

    The systematic cation exchange chromatographic separation of rubidium on Dowex 50W-X8 was carried out with mineral acids and their salts as eluants.A selectivity scale for various eluants in terms of the elution constant was devised. Rubidium was separated from a large number of elements in binary mixtures by the process of gradient or selective elutions or selective sorption. The noteworthy feature of the method is the sequential separation of rubidium from alkali as well as alkaline earth elements.

  9. Rotating annular chromatograph for continuous metal separations and recovery

    SciTech Connect

    Begovich, J.M.; Sisson, W.G.

    1981-01-01

    Multicomponent liquid chromatographic separations have been achieved by using a slowly rotating annular bed of sorbent material. By continuously introducing the feed material to be separated at a stationary point at the top of the bed and eluent everywhere else around the annulus, elution chromatography occurs. The rotation of the sorbent bed causes the separated components to appear as helical bands, each of which has a characteristic, stationary exit point; hence, the separation process is truly continuous. The concept has been developed primarily on a 279-mm-diam by 0.6-m-long device with a 12.7-mm-wide annulus. The effect of annulus width and diameter has recently been studied using the same device with a 50.8-mm-wide annulus and another 0.6-m-long chromatograph with an 89-mm diameter and annulus widths of 6.4, 12.7, and 22.2 mm. These columns have been constructed of Plexiglas and typically operate at a gauge pressure of 175 kPa. To further study the effect of size and pressure, a new 445-mm-diam by 1-m-long column with a 31.8-mm-wide annulus has been fabricated. Its metal construction allows preparative-scale operation with a wide variety of liquids at pressures to 1.3 MPa. Three metal recovery systems have been explored: (1) separation of iron and aluminum in ammonium sulfate-sulfuric acid solutions; (2) separation of hafnium from zirconium in sulfuric acid solutions; and (3) the separation of copper, nickel, and cobalt in ammonium carbonate solutions. This last system simulates the leach liquor of the Caron process for recovering nickel and cobalt from laterite ores. It has been studied, using similar conditions, on each of the chromatographs, and the results demonstrate the effect of column dimensions on the quality and quantity of the separation. 8 figures, 1 table.

  10. Can enantiomers be separated in achiral chromatographic systems?

    NASA Astrophysics Data System (ADS)

    Davankov, V. A.

    2016-10-01

    Consideration of chromatography of a nonracemic mixture on an achiral sorbent from a stereochemical point of view allows the claim that partial separation of the excess enantiomer zone from the racemate zone is possible only with analytes capable of self-associating under the conditions of the chromatographic column. It is from these positions that features of this process can be explained and conditions for its maximal proceeding formulated.

  11. Gas Chromatographic Determination of Enrivonmentally Significant Pesticides.

    ERIC Educational Resources Information Center

    Rudzinski, Walter E.; Beu, Steve

    1982-01-01

    A chromatographic procedure for analyzing organophosphorus pesticides (such as PCB's, nitrosamines, and phthalate esters) in orange juice is described, including a summary of the method, instrumentation, methodology, results/discussion, and calculations. (JN)

  12. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Chromatographic separation material for clinical... Laboratory Instruments § 862.2230 Chromatographic separation material for clinical use. (a) Identification. A chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents,...

  13. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Chromatographic separation material for clinical... Laboratory Instruments § 862.2230 Chromatographic separation material for clinical use. (a) Identification. A chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents,...

  14. Chromatographic enrichment and enantiomer separation of axially chiral polybrominated biphenyls in a technical mixture.

    PubMed

    Berger, Urs; Vetter, Walter; Götsch, Arntraut; Kallenborn, Roland

    2002-10-11

    The separation properties of different chromatographic methods regarding the enantioselective separation of axially chiral (atropisomeric) polybrominated biphenyls (PBB) were studied. For this purpose, the technical hexabromobiphenyl product Firemaster BP-6 was characterised by gas-chromatography coupled to electron capture detection (GC/ECD) and electron-capture negative ion mass spectrometry (GC/ECNI-MS) as well as by liquid chromatographic fractionating on active carbon and celite. Twelve individual PBBs including potential atropisomeric PBBs were isolated from Firemaster BP-6 by reversed-phase high-performance liquid chromatography (HPLC) on three serially coupled octadecylsilane columns. Six of the 12 isolated PBBs (three tri-ortho and di-ortho substituted PBBs, respectively) were separated into atropisomers on a HPLC column containing permethylated beta-cyclodextrin on silica. Moreover, the temperature dependency of the enantiomer separations is discussed. Gas chromatographic enantiomer separation of PBBs is a very demanding task due to high elution temperatures. However, the atropisomers of one tri-ortho substituted PBB congener (PBB 149) could be resolved on a column coated with randomly modified heptakis(6-O-tert.-butyldimethylsilyl-2,3-di-O-methyl)-beta-cyclodextrin in OV 1701.

  15. [The gas chromatographic detection of acetylene in cadaveric material].

    PubMed

    Iablochkin, V D

    1999-01-01

    Acetylene traces were detected by gas chromatography in the cadaveric right crural muscle of a 30-year-old man dead from an explosion of an acetylene reservoir at a plant. Acetylene was identified using the absolute calibration method on 3 standard gas chromatographic columns, reaction gas chromatography, and acetylene "deduction" by silver sulfate on silicagel.

  16. Gas chromatographic determination of sulphur compounds in town gas.

    PubMed

    Hoshika, Y; Iida, Y

    1977-04-11

    The gas chromatographic (GC) determination of the sulphur compounds in town gas (in the Nagoya area) was studied by using a flame-photometric detector (FPD) and the cold-trap method with liquid oxygen. The column packings used were 25% TCEP on Shimalite (AW, DMCS), 25% TCP on Shimalite (AW, DMCS), 10% PPE on Shimalite TPA, Porapak Q and silica gel. The major components identified were carbonyl sulphide, hydrogen sulphide, carbon disulphide, thiophene and tetrahydrothiophene (THT). The identities of thiophene and THT were also confirmed by GC combined with the use of a quadrupole mass spectrometer. The average concentrations and standard deviations of thiophene and THT were 8.8 +/- 1.8and 124 +/- 35 ng per 0.051, respectively. The latter value corresponds to 0.7 ppm, which is relatively high for the concentration of an odorant.

  17. Multi-objective optimization of chromatographic rare earth element separation.

    PubMed

    Knutson, Hans-Kristian; Holmqvist, Anders; Nilsson, Bernt

    2015-10-16

    The importance of rare earth elements in modern technological industry grows, and as a result the interest for developing separation processes increases. This work is a part of developing chromatography as a rare earth element processing method. Process optimization is an important step in process development, and there are several competing objectives that need to be considered in a chromatographic separation process. Most studies are limited to evaluating the two competing objectives productivity and yield, and studies of scenarios with tri-objective optimizations are scarce. Tri-objective optimizations are much needed when evaluating the chromatographic separation of rare earth elements due to the importance of product pool concentration along with productivity and yield as process objectives. In this work, a multi-objective optimization strategy considering productivity, yield and pool concentration is proposed. This was carried out in the frame of a model based optimization study on a batch chromatography separation of the rare earth elements samarium, europium and gadolinium. The findings from the multi-objective optimization were used to provide with a general strategy for achieving desirable operation points, resulting in a productivity ranging between 0.61 and 0.75 kgEu/mcolumn(3), h(-1) and a pool concentration between 0.52 and 0.79 kgEu/m(3), while maintaining a purity above 99% and never falling below an 80% yield for the main target component europium.

  18. Gas separation membranes

    DOEpatents

    Schell, William J.

    1979-01-01

    A dry, fabric supported, polymeric gas separation membrane, such as cellulose acetate, is prepared by casting a solution of the polymer onto a shrinkable fabric preferably formed of synthetic polymers such as polyester or polyamide filaments before washing, stretching or calendering (so called griege goods). The supported membrane is then subjected to gelling, annealing, and drying by solvent exchange. During the processing steps, both the fabric support and the membrane shrink a preselected, controlled amount which prevents curling, wrinkling or cracking of the membrane in flat form or when spirally wound into a gas separation element.

  19. Role of substituents in cyclodextrin derivatives for enantioselective gas chromatographic separation of chiral terpenoids in the essential oils of Mentha spicata.

    PubMed

    Pragadheesh, V S; Yadav, Anju; Chanotiya, Chandan Singh

    2015-10-01

    Enantioselective GC-FID and enantioselective GC-MS have been utilized under temperature gradient mode with differently substituted heptakis- and octakis-cyclodextrins to achieve the resolution of chiral terpenoids in the essential oil of indigenously grown cultivars of Mentha spicata. Modified cyclodextrins were derivatized in GC column for the separation of chiral terpenoids. A 2,3-diethyl-6-tert-butyldimethylsilyl-β-cyclodextrin doped into 14% cyanopropylphenyl/86%dimethylpolysiloxane (TBDE-β-CD) showed good enantioselectivity for all the studied chiral compounds excluding carvone. Carvone enantiomers were well resolved in 2,3-diacetoxy-6-tert-butyldimethylsilyl-β-cyclodextrin column (TBDA-β-CD) with enantioseparation (Es) of 1.006. A TBDE-β-CD provides maximum enantiomeric separation for β-pinene (Es 1.038), sabinene (Es 1.051), limonene (Es 1.045), isomenthone (Es 1.029) and α-terpineol (Es 1.014). Furthermore, enantiomer elution order reversal was observed for sabinene, menthone, terpinen-4-ol and menthol while changing from β- to γ-cyclodextrin phase. Carvone exhibits enantiomer elution order reversal by changing substituents i.e., methyl to acetyl at 2- & 3- position of the cyclodextrin derivative. Chiral constituents such as (+)-isomenthone, (-)-menthone, (1R,2S,5R)-(-)-menthol and (4S)-(+)-piperitone exist as a single enantiomer with >99% excess. Existence of (R)-(+)-limonene and (S)-(+)-carvone enantiomers has been proven first time in M. spicata essential oils and can be used as the marker for Indian origin.

  20. Polymide gas separation membranes

    DOEpatents

    Ding, Yong; Bikson, Benjamin; Nelson, Joyce Katz

    2004-09-14

    Soluble polyamic acid salt (PAAS) precursors comprised of tertiary and quaternary amines, ammonium cations, sulfonium cations, or phosphonium cations, are prepared and fabricated into membranes that are subsequently imidized and converted into rigid-rod polyimide articles, such as membranes with desirable gas separation properties. A method of enhancing solubility of PAAS polymers in alcohols is also disclosed.

  1. Chromatographic separation of neodymium isotopes by using chemical exchange process.

    PubMed

    Ismail, I M; Ibrahim, M; Aly, H F; Nomura, M; Fujii, Y

    2011-05-20

    The neodymium isotope effects were investigated in Nd-malate ligand exchange system using the highly porous cation exchange resin SQS-6. The temperature of the chromatographic columns was kept constant at 50°C by temperature controlled water passed through the columns jackets. The separation coefficient of neodymium isotopes, ɛ's, was calculated from the isotopic ratios precisely measured by means of an ICP mass spectrometer equipped with nine collectors as ion detectors. The separation coefficient, ɛ×10(5), were calculated and found to be 1.4, 4.8, 5.4, 10.6, 16.8 and 20.2 for (143)Nd, (144)Nd, (145)Nd, (146)Nd, (148)Nd and (150)Nd, respectively.

  2. Mathematical model for multicomponent separations on the continuous annular chromatograph

    SciTech Connect

    Bratzler, R.L.; Begovich, J.M.

    1980-12-01

    A model for multicomponent separations on ion exchange columns has been adapted for use in studying the performance of the continuous annular chromatograph. The model accurately predicts solute peak positions in the column effluent and qualitatively predicts trends in solute effluent resolution as a function of increasing bandwidth of the solute feed pulse. The major virtues of the model are its simplicity in terms of the calculations involved and the fact that it incorporates the nonlinear solute-resin binding isotherms common in many ion exchange separations. Because dispersion effects are not accounted for in the model, discrepancies exist between the shapes of the effluent peaks predicted by the model and those determined experimentally.

  3. Gas chromatograph-combustion system for 14C-accelerator mass spectrometry.

    PubMed

    McIntyre, Cameron P; Sylva, Sean P; Roberts, Mark L

    2009-08-01

    A gas chromatograph-combustion (GC-C) system is described for the introduction of samples as CO(2) gas into a (14)C accelerator mass spectrometry (AMS) system with a microwave-plasma gas ion source. Samples are injected into a gas chromatograph fitted with a megabore capillary column that uses H(2) as the carrier gas. The gas stream from the outlet of the column is mixed with O(2) and Ar gas and passed through a combustion furnace where the H(2) carrier gas and separated components are quantitatively oxidized to CO(2) and H(2)O. Water vapor is removed using a heated nafion dryer. The Ar carries the CO(2) to the ion source. The system is able to separate and oxidize up to 10 microg of compound and transfer the products from 7.6 mL/min of H(2) carrier gas into 0.2-1.0 mL/min of Ar carrier gas. Chromatographic performance and isotopic fidelity satisfy the requirements of the (14)C-AMS system for natural abundance measurements. The system is a significant technical advance for GC-AMS and may be capable of providing an increase in sensitivity for other analytical systems such as an isotope-ratio-monitoring GC/MS.

  4. Gas chromatographic analysis of volatiles in fluid and gas inclusions

    USGS Publications Warehouse

    Andrawes, F.; Holzer, G.; Roedder, E.; Gibson, E.K.; Oro, J.

    1984-01-01

    Most geological samples and some synthetic materials contain fluid inclusions. These inclusions preserve for us tiny samples of the liquid and/or the gas phase that was present during formation, although in some cases they may have undergone significant changes from the original material. Studies of the current composition of the inclusions provide data on both the original composition and the change since trapping. These inclusions are seldom larger than 1 millimeter in diameter. The composition varies from a single major compound (e.g., water) in a single phase to a very complex mixture in one or more phases. The concentration of some of the compounds present may be at trace levels. We present here some analyses of inclusions in a variety of geological samples, including diamonds. We used a sample crusher and a gas chromatography-mass spectrometry (GC-MS) system to analyze for organic and inorganic volatiles present as major to trace constituents in inclusions. The crusher is a hardened stainless-steel piston cylinder apparatus with tungsten carbide crusing surfaces, and is operated in a pure helium atmosphere at a controlled temperature. Samples ranging from 1 mg to 1 g were crushed and the released volatiles were analyzed using multi-chromatographic columns and detectors, including the sensitive helium ionization detector. Identification of the GC peaks was carried out by GC-MS. This combination of procedures has been shown to provide geochemically useful information on the process involved in the history of the samples analyzed. ?? 1984.

  5. Comparison of physicochemical and gas chromatographic polarity measures for simple organic compounds.

    PubMed

    Héberger, Károly; Zenkevich, Igor G

    2010-04-23

    The comparison of different polarity measures (parameters, descriptors, variables, scales, etc.) indicates that evaluation of interrelations between these measures is important for better understanding and interpretation of chemical and/or analytical data, especially for chromatographic separation. The best linear correlation between gas chromatographic and non-chromatographic polarity descriptors is revealed for the first time: this pair of variables is the difference of gas chromatographic retention indices on standard polar and non-polar phases as well as the difference between non-dimensional indices of boiling points (known in chromatography since mid-1980s as dispersion indices) and indices of molar refractions. The correlation helps chromatographers to find preferable chemical variables (features) to understand better the separation phenomena and to find better correlations in QSRR models. Principal component analysis (PCA) of ten frequently applied polarity measures shows their similarity and, at the same time, it shows the absence of anomalies within the set of simple organic molecules. A novel ranking method for ten polarity parameters points out that the two most informative polarity measures are (i) the non-dimensional index for boiling point and (ii) the difference in chromatographic retention indices on standard polar and non-polar stationary phases. On the other hand, the hydrophobicity parameter, log P, sometimes considered as polarity parameter in HPLC seems to be the worst one in description of "polarity" in gas chromatography. Surprisingly, such polarity measures like dipole moment and permittivity used often in organic chemistry does not provide the best correlation with gas chromatographic polarity measures.

  6. [Derivative gas chromatographic analysis of fructooligosaccharide in fermented sucrose].

    PubMed

    Cai, W M; Liu, H; Sun, X J

    2000-01-01

    As a new sweetener, fructooligosaccharide is paid more and more attention for its health improvement property. It includes trisaccharide, tetrasaccharide and pentasaccharide, and can be produced from sucrose by the fermentation of microorganism. In order to analyze the content of fructooligosaccharide in fermented sugar by gas chromatography, fructooligosaccharide was transformed into trimethylsilyl derivatives. Based on the modified gas chromatograph SP2308, and under the chosen chromatographic conditions with 0.53 mm capillary column of OV-101, the contents of fructose, glucose, sucrose and fructooligosaccharide were determined by programmed temperature chromatography. The recovery of fructooligosaccharide was satisfactory.

  7. Method for the chromatographic separation of cations from aqueous samples

    DOEpatents

    Horwitz, E.P.; Chiarizia, R.; Dietz, M.L.

    1997-07-29

    An extraction chromatographic material is described for extracting metal cations from a liquid stream. The extraction chromatographic material is prepared by adsorbing a diesterified methanediphosphonic acid on an inert particulate support. 7 figs.

  8. Intact protein separation by chromatographic and/or electrophoretic techniques for top-down proteomics.

    PubMed

    Capriotti, Anna Laura; Cavaliere, Chiara; Foglia, Patrizia; Samperi, Roberto; Laganà, Aldo

    2011-12-09

    Mass spectrometry used in combination with a wide variety of separation methods is the principal methodology for proteomics. In bottom-up approach, proteins are cleaved with a specific proteolytic enzyme, followed by peptide separation and MS identification. In top-down approach intact proteins are introduced into the mass spectrometer. The ions generated by electrospray ionization are then subjected to gas-phase separation, fragmentation, fragment separation, and automated interpretation of mass spectrometric and chromatographic data yielding both the molecular weight of the intact protein and the protein fragmentation pattern. This approach requires high accuracy mass measurement analysers capable of separating the multi-charged isotopic cluster of proteins, such as hybrid ion trap-Fourier transform instruments (LTQ-FTICR, LTQ-Orbitrap). Front-end separation technologies tailored for proteins are of primary importance to implement top-down proteomics. This review intends to provide the state of art of protein chromatographic and electrophoretic separation methods suitable for MS coupling, and to illustrate both monodimensional and multidimensional approaches used for LC-MS top-down proteomics. In addition, some recent progresses in protein chromatography that may provide an alternative to those currently employed are also discussed.

  9. Chromatographic Studies of Protein-Based Chiral Separations.

    PubMed

    Bi, Cong; Zheng, Xiwei; Azaria, Shiden; Beeram, Sandya; Li, Zhao; Hage, David S

    2016-09-01

    The development of separation methods for the analysis and resolution of chiral drugs and solutes has been an area of ongoing interest in pharmaceutical research. The use of proteins as chiral binding agents in high-performance liquid chromatography (HPLC) has been an approach that has received particular attention in such work. This report provides an overview of proteins that have been used as binding agents to create chiral stationary phases (CSPs) and in the use of chromatographic methods to study these materials and protein-based chiral separations. The supports and methods that have been employed to prepare protein-based CSPs will also be discussed and compared. Specific types of CSPs that are considered include those that employ serum transport proteins (e.g., human serum albumin, bovine serum albumin, and alpha1-acid glycoprotein), enzymes (e.g., penicillin G acylase, cellobiohydrolases, and α-chymotrypsin) or other types of proteins (e.g., ovomucoid, antibodies, and avidin or streptavidin). The properties and applications for each type of protein and CSP will also be discussed in terms of their use in chromatography and chiral separations.

  10. Chromatographic Studies of Protein-Based Chiral Separations

    PubMed Central

    Bi, Cong; Zheng, Xiwei; Azaria, Shiden; Beeram, Sandya; Li, Zhao; Hage, David S.

    2016-01-01

    The development of separation methods for the analysis and resolution of chiral drugs and solutes has been an area of ongoing interest in pharmaceutical research. The use of proteins as chiral binding agents in high-performance liquid chromatography (HPLC) has been an approach that has received particular attention in such work. This report provides an overview of proteins that have been used as binding agents to create chiral stationary phases (CSPs) and in the use of chromatographic methods to study these materials and protein-based chiral separations. The supports and methods that have been employed to prepare protein-based CSPs will also be discussed and compared. Specific types of CSPs that are considered include those that employ serum transport proteins (e.g., human serum albumin, bovine serum albumin, and alpha1-acid glycoprotein), enzymes (e.g., penicillin G acylase, cellobiohydrolases, and α-chymotrypsin) or other types of proteins (e.g., ovomucoid, antibodies, and avidin or streptavidin). The properties and applications for each type of protein and CSP will also be discussed in terms of their use in chromatography and chiral separations. PMID:28344977

  11. Gas chromatographic-mass spectrometric analysis of volatile amines produced by several strains of Clostridium.

    PubMed

    Pons, J L; Rimbault, A; Darbord, J C; Leluan, G

    1985-02-08

    A gas chromatographic--mass spectrometric technique is proposed for the analysis of volatile amines which were isolated from Clostridium cultures by vacuum distillation and concentrated as hydrochloride salts. Headspace sampling after alkalinization of the salts under vacuum was the most suitable for subsequent gas chromatographic analysis. With ammonia-loaded helium as carrier gas, methylamines were separated on 4.8% PEG 2OM + 0.3% potassium hydroxide on Carbopack B, and other volatile amines on 28% Pennwalt 223 + 4% potassium hydroxide on Gas-Chrom R. Bacterial volatile amines (dimethylamine, trimethylamine, isobutylamine, 3-methylbutylamine, etc.) were detected with a flame-ionization detector and identified by gas chromatography--mass spectrometry in electron-impact and chemical ionization modes.

  12. Gas separation membrane module assembly

    DOEpatents

    Wynn, Nicholas P; Fulton, Donald A.

    2009-03-31

    A gas-separation membrane module assembly and a gas-separation process using the assembly. The assembly includes a set of tubes, each containing gas-separation membranes, arranged within a housing. The housing contains a tube sheet that divides the space within the housing into two gas-tight spaces. A permeate collection system within the housing gathers permeate gas from the tubes for discharge from the housing.

  13. Chromatographic Separations Using Solid-Phase Extraction Cartridges: Separation of Wine Phenolics

    NASA Astrophysics Data System (ADS)

    Brenneman, Charles A.; Ebeler, Susan E.

    1999-12-01

    We describe a simple laboratory experiment that demonstrates the principles of chromatographic separation using solid-phase extraction columns and red wine. By adjusting pH and mobile phase composition, the wine is separated into three fractions of differing polarity. The content of each fraction can be monitored by UV-vis spectroscopy. When the experiment is combined with experiments involving HPLC or GC separations, students gain a greater appreciation for and understanding of the highly automated instrumental systems currently available. In addition, they learn about the chemistry of polyphenolic compounds, which are present in many foods and beverages and which are receiving much attention for their potentially beneficial health effects.

  14. Characterisation of wax works of art by gas chromatographic procedures.

    PubMed

    Regert, M; Langlois, J; Colinart, S

    2005-10-14

    To identify the various natural and synthetic substances used by sculptors at the end of the 19th century, several contemporary reference samples were investigated by high temperature gas chromatography (HT GC) and HT GC-MS. Using specific chromatographic conditions and minimising sample preparation, we could separate, detect and identify a wide range of biomolecular markers covering a great variety of molecular weights and volatilities, with a minimum amount of sample, in a single run. Beeswax, spermaceti, carnauba, candellila and Japan waxes as well as pine resin derivatives, animal fats, paraffin, ozokerite and stearin, used as additives in wax works of art, were chemically investigated. In the case of low volatile compounds, transbutylation was performed. The structure of long-chain esters of spermaceti was elucidated for the first time by HT GC-MS analysis. Such a method was then carried out on 10 samples collected on a statuette of Junon by Antoine-Louis Barye (Louvre Museum, Paris, France) and on a sculpture by Aimé-Jules Dalou (Musée de la Révolution Française, Vizille, France). The analytical results obtained provide new data on the complex recipes elaborated by sculptors at the end of the 19th century.

  15. Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids.

    PubMed

    Acevska, J; Stefkov, G; Petkovska, R; Kulevanova, S; Dimitrovska, A

    2012-05-01

    The excessive and continuously growing interest in the simultaneous determination of poppy alkaloids imposes the development and optimization of convenient high-throughput methods for the assessment of the qualitative and quantitative profile of alkaloids in poppy straw. Systematic optimization of two chromatographic methods (gas chromatography (GC)/flame ionization detector (FID)/mass spectrometry (MS) and reversed-phase (RP)-high-performance liquid chromatography (HPLC)/diode array detector (DAD)) for the separation of alkaloids from Papaver somniferum L. (Papaveraceae) was carried out. The effects of various conditions on the predefined chromatographic descriptors were investigated using chemometrics. A full factorial linear design of experiments for determining the relationship between chromatographic conditions and the retention behavior of the analytes was used. Central composite circumscribed design was utilized for the final method optimization. By conducting the optimization of the methods in very rational manner, a great deal of excessive and unproductive laboratory research work was avoided. The developed chromatographic methods were validated and compared in line with the resolving power, sensitivity, accuracy, speed, cost, ecological aspects, and compatibility with the poppy straw extraction procedure. The separation of the opium alkaloids using the GC/FID/MS method was achieved within 10 min, avoiding any derivatization step. This method has a stronger resolving power, shorter analysis time, better cost/effectiveness factor than the RP-HPLC/DAD method and is in line with the "green trend" of the analysis. The RP-HPLC/DAD method on the other hand displayed better sensitivity for all tested alkaloids. The proposed methods provide both fast screening and an accurate content assessment of the six alkaloids in the poppy samples obtained from the selection program of Papaver strains.

  16. Gas chromatographic determination of yohimbine in commercial yohimbe products.

    PubMed

    Betz, J M; White, K D; der Marderosian, A H

    1995-01-01

    The bark of Pausinystalia yohimbe [K. Schumann] Pierre (Rubiaceae), long valued as an aphrodisiac in West Africa, recently has been promoted in the United States as a dietary supplement alternative to anabolic steroids for enhancement of athletic performance. As the number of yohimbe products on the retail market increases, concerns about their safety are raised because of the reported toxicity of yohimbine (the major alkaloid of the plant). Although plant materials are usually identified microscopically, we were unable to identify them in many of the products, because as their labels indicated, the products were mixtures of various botanicals or were bark extracts and contained little or no plant material. A method for extraction and capillary gas chromatographic (GC) separation of the alkaloids of P. yohimbe was, therefore, developed and used to analyze a number of commercial yohimbe products. The method involved solvent extraction and partitioning in chloroform-water followed by separation on a methyl silicone capillary GC column (N-P detection). Comparisons of chromatograms of extracts of authentic bark with those of commercial products indicated that, although many products contained measurable quantities of the alkaloid yohimbine, they were largely devoid of the other alkaloids previously reported in this species. Concentrations of yohimbine in the commercial products ranged from < 0.1 to 489 ppm, compared with 7089 ppm in the authentic material. Authentic bark has been reported to contain up to 6% total alkaloids, 10-15% of which are yohimbine. The possible presence of undeclared diluents in the products was indicated by peaks in product chromatograms but not in those of authentic bark.

  17. Chromatographic Separation and NMR An Integrated Approach in Pharmaceutical Development.

    PubMed

    Gonnella, Nina C

    2012-01-01

    Over the past 10 years, major improvements in the performance of LC-NMR have been realized. The addition of postcolumn SPE, advances in probe technology including cryogenic probes and microcoil probes, improved solvent suppression pulse sequences, and shielded magnets with better homogeneity have all contributed to rapid advancements in this technology. Application of LC-NMR to problems in pharmaceutical development has had a major impact on structure elucidation studies. LC-NMR has been successfully applied to determine the structures of degradation products, impurities, mixtures of compounds, and metabolites. Use of stop flow techniques with LC-NMR experiments has been a critical means of identifying unstable compounds and studying conformational kinetics. The integration of SPE as an intermediate step between the LC unit and the NMR spectrometer has vastly improved the power of the hyphenated technique in trace analysis applications. Online postcolumn enrichment of chromatographic peaks by SPE dramatically reduces the NMR acquisition times by allowing repeated injections to be trapped onto the same cartridge or different cartridges. Because protonated solvents can be easily removed with a drying procedure, solvents and buffers may be freely chosen for maximizing chromatographic separation without compromising NMR spectral quality. The compound of interest may then be eluted from an SPE cartridge using deuterated organic solvent, which helps to reduce dynamic range issues. When combined with cryogenically cooled microcapillary probes, the sensitivity of the NMR signal increases about 10-fold over conventional room temperature probes, enabling full structure characterization at the microgram level. Heteronuclear experiments with concentrations previously only possible in a limited number of cases have now become standard experiments. The availability of HSQC and HMBC experiments and microcoil/cryogenic technology opens the possibility of using LC-(SPE) NMR for the

  18. Catalytically-Promoted Analyte Derivatization Inside a Gas Chromatographic Inlet

    PubMed Central

    Fowler, William K.; Gamble, Kelly J.; Wright, Amber R.

    2010-01-01

    Reported here is a preliminary assessment of the feasibility of catalyzing on-line derivatization reactions inside the inlet (i.e., the injection port) of a gas chromatograph (GC) with solid heterogeneous catalysts. The experiments described here entail the installation of candidate catalysts inside the GC inlet liner and the subsequent injection of analyte/reagent mixtures onto the catalyst beds. Two catalysts are identified, each of which clearly catalyzes one of the chosen model derivatization reactions in the inlet of a GC. This result supports our hypothesis that on-line derivatizations can, in principle, be reproducibly catalyzed inside the GC inlet by solid heterogeneous catalysts and that the presence of such catalysts in the inlet do not necessarily cause a serious loss of instrument performance or chromatographic efficiency. PMID:20822662

  19. Evaluation of Gas Chromatographic Methods for Analysis of Gasoline/Oxygenate Blends.

    DTIC Science & Technology

    1981-12-01

    determination of various oxygenated compounds in gasoline by gas chromotography have been developed.(3-6) These include gas chromatographic (GC) analysis of the...ID-Ai33 0i6 EVALUATION OF GAS CHROMATOGRAPHIC METHODS FOR ANALYSIS i/t OF GASOLINE/OXYGEN.. (U) SOUTHWEST RESEARCH INST SAN ANTONIO TX ARMY FUELS...0 EVALUATION OF GAS -CHROMATOGRAPHIC METHODS FOR ANALYSIS OF GASOLINE/OXYGENATE BLENDS INTERIM REPORT

  20. Highly sensitive gas chromatographic determination of ethanol in human urine samples.

    PubMed

    Zilly, Michael; Langmann, Peter; Lenker, Ulrike; Satzinger, Verena; Schirmer, Diana; Klinker, Hartwig

    2003-12-25

    In order to evaluate recent alcohol consumption, a very sensitive and specific gas chromatographic method for ethanol determination in human urine samples was developed. The non-invasive method was performed without any pretreatment and carried out on a Stabilwax capillary column, 30 m x 0.53 mm x 1.0 microm film thickness. Helium was used as carrier gas with a constant inlet pressure of 27.72 kPa (0.277 bar) and a flame ionization detector (FID). Quantification was performed with the use of acetonitrile as an internal standard (IS). The calibration curve was linear throughout the concentration range from 0.5 to 500 mg/l. The calculated intra- and inter-day coefficients of variation were below 8%. A clear chromatographic separation of ethanol from methanol, acetone, 1-propanol and 2-propanol was achieved.

  1. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents, ion exchagne resins, and ion papers) intended for use in ion exchange chromatography, a procedure in which...

  2. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents, ion exchagne resins, and ion papers) intended for use in ion exchange chromatography, a procedure in which...

  3. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents, ion exchagne resins, and ion papers) intended for use in ion exchange chromatography, a procedure in which...

  4. HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF ORGANOPHOSPHORUS PESTICIDES ON POLYSACCHARIDE CHIRAL STATIONARY PHASES

    EPA Science Inventory

    High-performance liquid chromatographic separation of the individual enantiomers of 12 organophosphorus pesticides (OPs) was obtained on polysaccharide enantioselective HPLC columns using alkane-alcohol mobile phase. The OP pesticides were crotoxyphos, dialifor, fonofos, fenamiph...

  5. Gas-chromatographic characterization of physicochemical properties of astatine compounds

    SciTech Connect

    Norseev, Yu.V.

    1995-07-01

    The organoastatine compounds obtained were identified by gas-liquid chromatography on a specially designed gas radiochromatograph with detection of eluted compounds both by their radioactivity and by thermal conductivity. Gas-liquid chromatography is the most efficient method for separation and identification of volatile organoastatine compounds.

  6. Chromatographic separation and concentration of quercetin and (+)-catechin using mesoporous composites based on MCM-41

    NASA Astrophysics Data System (ADS)

    Karpov, S. I.; Belanova, N. A.; Korabel'nikova, E. O.; Nedosekina, I. V.; Roessner, F.; Selemenev, V. F.

    2015-05-01

    Data on chromatographic separation of quercetin and (+)-catechin-flavonoids with similar physicochemical (including sorption) properties—are presented. The highest efficiency of chromatographic process at high sorption capacity of the material with respect to quercetin and slightly lower capacity for (+)-catechin were observed when silylated composites of ordered MCM-41 type materials were used. The application of acetonitrile as a solvent increased the sorption capacity of the material and can be recommended for separation of related polyphenol substances and their determination using ordered MCM-41 modified with trimethylchlorosilane as a stationary phase in a chromatographic column.

  7. Preliminary numerical analysis of improved gas chromatograph model

    NASA Technical Reports Server (NTRS)

    Woodrow, P. T.

    1973-01-01

    A mathematical model for the gas chromatograph was developed which incorporates the heretofore neglected transport mechanisms of intraparticle diffusion and rates of adsorption. Because a closed-form analytical solution to the model does not appear realizable, techniques for the numerical solution of the model equations are being investigated. Criteria were developed for using a finite terminal boundary condition in place of an infinite boundary condition used in analytical solution techniques. The class of weighted residual methods known as orthogonal collocation is presently being investigated and appears promising.

  8. Separation and identification of various vulcanization agents and antioxidants in two types of rubber by chromatographic and spectrometric methods.

    PubMed

    Chauveau, S; Hamon, M; Leleu, E

    1991-11-01

    The aim of this study was to separate and identify by chromatographic and spectrometric methods, the various allergenic vulcanization agents and antioxidants used in the manufacture of industrial rubber. Specimens of elastomers were manufactured specially for this study. The specificity of the gas chromatographic method developed allows separation of all the manufacturing additives in the selected rubber types after one injection only, even though they belong to extremely varied chemical categories. The GLC method was coupled with mass spectrometry, which permitted identification of the peaks obtained and the study of the fragmentation of the 4 reference products under various conditions. Separation by TLC was performed in parallel on the same extracts, allowing rapid identification of the products tested for, and showed new spots after vulcanization.

  9. Techniques of preparing plant material for chromatographic separation and analysis.

    PubMed

    Romanik, G; Gilgenast, E; Przyjazny, A; Kamiński, M

    2007-03-10

    This paper discusses preparation techniques of samples of plant material for chromatographic analysis. Individual steps of the procedures used in sample preparation, including sample collection from the environment or from tissue cultures, drying, comminution, homogenization, leaching, extraction, distillation and condensation, analyte enrichment, and obtaining the final extracts for chromatographic analysis are discussed. The techniques most often used for isolation of analytes from homogenized plant material, i.e., Soxhlet extraction, ultrasonic solvent extraction (sonication), accelerated solvent extraction, microwave-assisted extraction, supercritical-fluid extraction, steam distillation, as well as membrane processes are emphasized. Sorptive methods of sample enrichment and removal of interferences, i.e., solid-phase extraction, and solid-phase micro-extraction are also discussed.

  10. Ionic liquids in chromatographic and electrophoretic techniques: toward additional improvements in the separation of natural compounds

    PubMed Central

    Freire, Carmen S. R.; Coutinho, João A. P.; Silvestre, Armando J. D.; Freire, Mara G.

    2016-01-01

    Due to their unique properties, in recent years, ionic liquids (ILs) have been largely investigated in the field of analytical chemistry. Particularly during the last sixteen years, they have been successfully applied in the chromatographic and electrophoretic analysis of value-added compounds extracted from biomass. Considering the growing interest in the use of ILs in this field, this critical review provides a comprehensive overview on the improvements achieved using ILs as constituents of mobile or stationary phases in analytical techniques, namely in capillary electrophoresis and its different modes, in high performance liquid chromatography, and in gas chromatography, for the separation and analysis of natural compounds. The impact of the IL chemical structure and the influence of secondary parameters, such as the IL concentration, temperature, pH, voltage and analysis time (when applied), are also critically addressed regarding the achieved separation improvements. Major conclusions on the role of ILs in the separation mechanisms and the performance of these techniques in terms of efficiency, resolution and selectivity are provided. Based on a critical analysis of all published results, some target-oriented ILs are suggested. Finally, current drawbacks and future challenges in the field are highlighted. In particular, the design and use of more benign and effective ILs as well as the development of integrated (and thus more sustainable) extraction–separation processes using IL aqueous solutions are suggested within a green chemistry perspective. PMID:27667965

  11. Ionic liquids in chromatographic and electrophoretic techniques: toward additional improvements in the separation of natural compounds.

    PubMed

    Soares, Belinda; Passos, Helena; Freire, Carmen S R; Coutinho, João A P; Silvestre, Armando J D; Freire, Mara G

    2016-09-07

    Due to their unique properties, in recent years, ionic liquids (ILs) have been largely investigated in the field of analytical chemistry. Particularly during the last sixteen years, they have been successfully applied in the chromatographic and electrophoretic analysis of value-added compounds extracted from biomass. Considering the growing interest in the use of ILs in this field, this critical review provides a comprehensive overview on the improvements achieved using ILs as constituents of mobile or stationary phases in analytical techniques, namely in capillary electrophoresis and its different modes, in high performance liquid chromatography, and in gas chromatography, for the separation and analysis of natural compounds. The impact of the IL chemical structure and the influence of secondary parameters, such as the IL concentration, temperature, pH, voltage and analysis time (when applied), are also critically addressed regarding the achieved separation improvements. Major conclusions on the role of ILs in the separation mechanisms and the performance of these techniques in terms of efficiency, resolution and selectivity are provided. Based on a critical analysis of all published results, some target-oriented ILs are suggested. Finally, current drawbacks and future challenges in the field are highlighted. In particular, the design and use of more benign and effective ILs as well as the development of integrated (and thus more sustainable) extraction-separation processes using IL aqueous solutions are suggested within a green chemistry perspective.

  12. Gas Separations using Ceramic Membranes

    SciTech Connect

    Paul KT Liu

    2005-01-13

    This project has been oriented toward the development of a commercially viable ceramic membrane for high temperature gas separations. A technically and commercially viable high temperature gas separation membrane and process has been developed under this project. The lab and field tests have demonstrated the operational stability, both performance and material, of the gas separation thin film, deposited upon the ceramic membrane developed. This performance reliability is built upon the ceramic membrane developed under this project as a substrate for elevated temperature operation. A comprehensive product development approach has been taken to produce an economically viable ceramic substrate, gas selective thin film and the module required to house the innovative membranes for the elevated temperature operation. Field tests have been performed to demonstrate the technical and commercial viability for (i) energy and water recovery from boiler flue gases, and (ii) hydrogen recovery from refinery waste streams using the membrane/module product developed under this project. Active commercializations effort teaming with key industrial OEMs and end users is currently underway for these applications. In addition, the gas separation membrane developed under this project has demonstrated its economical viability for the CO2 removal from subquality natural gas and landfill gas, although performance stability at the elevated temperature remains to be confirmed in the field.

  13. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres.

    PubMed

    Valentin, J R

    1989-03-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan

  14. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.

    1989-01-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan

  15. Reversed-phase liquid chromatographic separation and simultaneous profiling of steroidal glycoalkaloids and their aglycones.

    PubMed

    Kuronen, P; Väänänen, T; Pehu, E

    1999-11-19

    Improved and simplified reversed-phase liquid chromatographic conditions for the separation and simultaneous profiling of both steroidal glycoalkaloids and their aglycones, having solanidane- or spirosolane-type structures, are described. The most reproducible retention behavior for these ionizable compounds on C18 columns was achieved under isocratic and gradient elution conditions using acetonitrile in combination with triethylammonium phosphate buffer at pH 3.0, when basic functional groups of solutes and silanol groups on the silica are fully protonated minimizing ionic interactions. Gradient elution was the only feasible approach for the simultaneous separation of steroidal glycoalkaloids and their aglycones. A Zorbax SB C18 column, specially designed for low-pH separations, showed good performance in critical separations. The impurities of the commercial tomatine and tomatidine standards were studied and confirmed using mass spectrometric, liquid chromatographic and thin-layer chromatographic methods.

  16. Gas chromatographic retention characteristics of phenols with Superox-20M

    SciTech Connect

    White, C.M.; Li, N.C.

    1982-08-01

    The gas chromatographic retention characteristics of a variety of underivatized phenols have been studied by using Superox-20M coated on fused silica. The relative retention times of thes compounds were measured at 160, 150, and 140/sup 0/C in order to determine the effect of operating temperature on relative retention. This information is used to predict relative retention times of phenols for which we had no standards. The linear temperature-programmed retention indexes of the solutes were measured. The retention of phenols on this phase is a function of the compounds vapor pressure, its ability to hydrogen bond with the stationary phase, and the strengths of those hydrogen bonds. These properties are in turn governed by steric, inductive, and resonance effects of the substituents. Linear free-energy relations between the logarithm of the ratio of the activity coefficients of phenol to substituted phenol (calculated from relative retention data) and the chromatographic substituent constant, sigma/sub c/, have been determined for some phenols on Superox-20M. Lastly, it was shown by nuclear magnetic resonance experiments that Superox-20M is apparently a poly(ethylene glycol) (also called a polyoxiran or poly(ethylene oxide)). 5 figures, 3 tables.

  17. Improved Chromatographic Separation of Sitagliptin Phosphate and Metformin Hydrochloride

    PubMed Central

    Hendy, Moataz S.

    2015-01-01

    New UPLC method was developed for determination of sitagliptin and metformin using Symmetry C18 column (100 mm × 2.1 mm, 2.2 μm) and isocratic elution (methanol 20%), pH (3.5) as a mobile phase. The ultraviolet detector was operated at 220 nm and the column temperature was 50°C. Linearity parameters were acceptable over the concentration ranges of 2-12 μgml-1 and 5-35 μgml-1 for sitagliptin and metformin, respectively. The variables were premeditated to adjust the chromatographic conditions using design of experiment. The proposed method was proved to be accurate for the quality control of the mentioned drugs in their pharmaceutical dosage form. PMID:26759536

  18. Solid-phase microextraction-gas chromatographic determination of volatile monoaromatic hydrocarbons in soil.

    PubMed

    Zygmunt, B; Namiesnik, J

    2001-08-01

    Benzene, toluene, ethylbenzene, three isomers of xylene, and cumene have been isolated and enriched from soil samples by a combination of water extraction at room and elevated temperature and headspace-solid-phase microextraction before their gas chromatographic-mass spectrometric (GC-MS) determination. The conditions used for all stages of sample preparation and chromatographic analysis were optimized. Analytes sampled on a polydimethylsiloxane-coated solid-phase microextraction fiber were thermally desorbed in the split/splitless injector of a gas chromatograph (GC) coupled with a mass spectrometer (MS). The desorption temperature was optimized. The GC separation was performed in a capillary column. Detection limits were found to be of the order of ca. 1 ng g(-1). Relative recoveries of the analytes from soils were found to be highly dependent on soil organic-matter content and on compound identity; they ranged from ca 92 to 96% for sandy soil (extraction at room temperature) and from ca 27 to 55% for peaty soil (extraction at elevated temperature). A few real-world soil samples were analyzed; the individual monoaromatic hydrocarbon content ranged from below detection limits to 6.4 ng g(-1) for benzene and 8.1 for the total of p- + m-xylene.

  19. The gas chromatographic resolution of DL-isovaline

    NASA Technical Reports Server (NTRS)

    Flores, J. J.; Bonner, W. A.; Van Dort, M. A.

    1977-01-01

    Isovaline is of cosmological interest because it is one of the 12 non-protein amino acids which have been isolated from the Murchison meteorite, and unlike the other chiral amino acids in this meteorite, it has no alpha-hydrogen at its asymmetric center and hence cannot racemize by the customary alpha-hydrogen-dependent mechanisms which engender racemization in ordinary amino acids. Experiments were conducted in which a .01 M solution of N-TFA-DL-isovalyl-L-leucine isopropyl ester in nitromethane was injected into the capillary column of a gas chromatograph coupled to a digital electronic integrator-recorder. Efflux times and integrated peak area percents are shown next to each diastereometer peak.

  20. Gas chromatographic determination of oxalic acid in foods.

    PubMed

    Ohkawa, H

    1985-01-01

    A new quantitative gas chromatographic (GC) method has been developed for the determination of oxalic acid in foods. Solid sample is extracted with water (soluble oxalic acid) or 2N hydrochloric acid (total oxalic acid) at room temperature. An aliquot of sample extract is evaporated to dryness, and the oxalic acid in the residue is methylated with 7% hydrochloric acid-methanol. The reaction mixture is extracted with chloroform, and dimethyl oxalate is quantitated by GC. Recovery of oxalic acid added to liquid samples averaged 100.6%; recoveries from extracts of solid samples were 96.2-99.5 and 97.2-100.1% for water and hydrochloric acid extractions, respectively. Results are shown for determination of oxalic acid in spinach and beverages. The technique is simple, rapid, and accurate, and small samples may be used. The limit of determination is 20 micrograms.

  1. Fatty acids determination in Bronte pistachios by gas chromatographic method.

    PubMed

    Pantano, Licia; Lo Cascio, Giovanni; Alongi, Angelina; Cammilleri, Gaetano; Vella, Antonio; Macaluso, Andrea; Cicero, Nicola; Migliazzo, Aldo; Ferrantelli, Vincenzo

    2016-10-01

    A gas chromatographic with flame ionization detector (GC-MS FID) method for the identification and quantification of fatty acids based on the extraction of lipids and derivatisation of free acids to form methyl esters was developed and validated. The proposed method was evaluated to a number of standard FAs, and Bronte pistachios samples were used for that purpose and to demonstrate the applicability of the proposed method. In this regard, repeatability, mean and standard deviation of the analytical procedure were calculated. The results obtained have demonstrated oleic acid as the main component of Bronte pistachios (72.2%) followed by linoleic acid (13.4%) and showed some differences in composition with respect to Tunisian, Turkish and Iranian pistachios.

  2. Gas separations using inorganic membranes

    SciTech Connect

    Egan, B.Z.; Singh, S.P.N.; Fain, D.E.; Roettger, G.E.; White, D.E.

    1992-04-01

    This report summarizes the results from a research and development program to develop, fabricate, and evaluate inorganic membranes for separating gases at high temperatures and pressures in hostile process environments encountered in fossil energy conversion processes such as coal gasification. The primary emphasis of the research was on the separation and recovery of hydrogen from synthesis gas. Major aspects of the program included assessment of the worldwide research and development activity related to gas separations using inorganic membranes, identification and selection of candidate membrane materials, fabrication and characterization of membranes using porous membrane technology developed at the Oak Ridge K-25 Site, and evaluation of the separations capability of the fabricated membranes in terms of permeabilities and fluxes of gases.

  3. Asymmetric membranes for gas separations

    SciTech Connect

    Finken, H.

    1985-01-01

    Recent membrane developments for gaseous mixture separations are compared to the development of reverse osmosis membranes for water desalination. The goals of these developments have been the search for ideal permselective polymeric materials, techniques for producing ultrathin membrane layers free of imperfections and transforming gelled reverse osmosis membranes into solid gas permeation membranes. A novel approach to meeting the basic requirements of high permselectivity is attempted by altering the physical polymer structure within the membrane prior to application for gas separation. The influence of these physical interactions on membrane properties is presented. 47 references, 11 figures, 6 tables.

  4. Doxylamine: a cause for false-positive gas chromatographic assay for phencyclidine.

    PubMed

    Schaldenbrand, J D; McClatchey, K D; Patel, J A; Muilenberg, M J

    1981-01-01

    A 25-year-old white woman ingested an unknown quantity of doxylamine succinate and flurazepam. Urine immunoassay screen (EMIT-dau) was positive for benzodiazopine and negative for phencyclidine. Subsequent gas chromatographic assay of the urine revealed a markedly positive assay for phencyclidine. Doxylamine was ultimately found to be the cause for the false-positive gas chromatographic assay for phencyclidine.

  5. High productivity chromatographic separations on monolithic capillary columns

    NASA Astrophysics Data System (ADS)

    Korolev, A. A.; Shiryaeva, V. E.; Popova, T. P.; Kurganov, A. A.

    2013-03-01

    The productivity of monolithic capillary columns based on silica gel and polymers of different polarities (divinylbenzene and ethyleneglycol dimethacrylate) is investigated using a model mixture of light hydrocarbons. It is shown that the productivity of a column is noticeably affected by the type of gas carrier. The highest productivity is observed when using carbon dioxide or dinitrogen monoxide as the gas carrier. The lowest productivity is observed when uisng hydrogen or helium.

  6. High-performance liquid-chromatographic separation of subcomponents of antimycin-A

    USGS Publications Warehouse

    Abidi, S.L.

    1988-01-01

    Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

  7. High-performance liquid chromatographic separation of subcomponents of antimycin A.

    PubMed

    Abidi, S L

    1988-08-05

    Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, A1a, A1b, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins A1, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpreted based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

  8. Phosphazene membranes for gas separations

    DOEpatents

    Stewart, Frederick F.; Harrup, Mason K.; Orme, Christopher J.; Luther, Thomas A.

    2006-07-11

    A polyphosphazene having a glass transition temperature ("T.sub.g") of approximately -20.degree. C. or less. The polyphosphazene has at least one pendant group attached to a backbone of the polyphosphazene, wherein the pendant group has no halogen atoms. In addition, no aromatic groups are attached to an oxygen atom that is bound to a phosphorus atom of the backbone. The polyphosphazene may have a T.sub.g ranging from approximately -100.degree. C. to approximately -20.degree. C. The polyphosphazene may be selected from the group consisting of poly[bis-3-phenyl-1-propoxy)phosphazene], poly[bis-(2-phenyl-1-ethoxy)phosphazene], poly[bis-(dodecanoxypolyethoxy)-phosphazene], and poly[bis-(2-(2-(2-.omega.-undecylenyloxyethoxy)ethoxy)ethoxy)phosphazene]- . The polyphosphazene may be used in a separation membrane to selectively separate individual gases from a gas mixture, such as to separate polar gases from nonpolar gases in the gas mixture.

  9. Chemical characterization of Brickellia cavanillesii (Asteraceae) using gas chromatographic methods.

    PubMed

    Eshiet, Etetor R; Zhu, Jinqiu; Anderson, Todd A; Smith, Ernest E

    2014-03-01

    A methanol extract of lyophilized Brickellia cavanillesii was quantitatively analyzed using gas chromatographic (GC) techniques. The chromatographic methods employed were (i) GC-flame ionization detector (GC-FID), (ii) GC-mass spectrometry (GC-MS), and (iii) purge and trap GC-MS (P&T GC-MS). Thirteen compounds were identified with a quality match of 90% and above using GC-MS. The compounds were (1) Cyclohexene, 6-ethenyl-6-methyl-1-(1-methylethyl)-3-(1-methylethylidene)-, (S)-; (2) Bicylo (2.2.1) heptan-2-one, 1, 7, 7-trimethyl-(1S, 4S)-; (3) Phenol, 2-methoxy-4-(1-propenyl)-; (4) Benzene, 1-(1, 5-dimethyl-4-hexenyl)-4-methyl-; (5) Naphthalene, 1, 2, 3, 5, 6, 8a-hexahydro4, 7-dimethyl-1-1-(1-methylethyl)-, (1S-cis)-; (6) Phenol, 2-methoxy-; (7) Benzaldehyde, 3-hydroxy-4-methoxy-; (8) 11, 13-Eicosadienoic acid, methyl ester; (9) 2-Furancarboxaldehyde, 5-methyl-; (10) Maltol; (11) Phenol; (12) Hydroquinone; (13) 1H-Indene, 1-ethylideneoctahydro-7a-methyl-, (1E, 3a.alpha, 7a.beta.). Other compounds (14) 3-methyl butanal; (15) (D)-Limonene; (16) 1-methyl-4-(1-methyl ethyl) benzene; (17) Butanoic acid methyl ester; (18) 2-methyl propanal; (19) 2-butanone; (20) 2-pentanone; and (21) 2-methyl butane were also identified when P&T GC-MS was performed. Of the 21 compounds identified, 12 were validated using chemical standards. The identified compounds were found to be terpenes, derivatives of terpenes, esters, ketones, aldehydes, and phenol-derived aromatic compounds; these are the primary constituents of the essential oils of many plants and flowers.

  10. Chemical characterization of Brickellia cavanillesii (Asteraceae) using gas chromatographic methods

    PubMed Central

    Eshiet, Etetor R; Zhu, Jinqiu; Anderson, Todd A; Smith, Ernest E

    2014-01-01

    A methanol extract of lyophilized Brickellia cavanillesii was quantitatively analyzed using gas chromatographic (GC) techniques. The chromatographic methods employed were (i) GC-flame ionization detector (GC-FID), (ii) GC-mass spectrometry (GC-MS), and (iii) purge and trap GC-MS (P&T GC-MS). Thirteen compounds were identified with a quality match of 90% and above using GC-MS. The compounds were (1) Cyclohexene, 6-ethenyl-6-methyl-1-(1-methylethyl)-3-(1-methylethylidene)-, (S)-; (2) Bicylo (2.2.1) heptan-2-one, 1, 7, 7-trimethyl-(1S, 4S)-; (3) Phenol, 2-methoxy-4-(1-propenyl)-; (4) Benzene, 1-(1, 5-dimethyl-4-hexenyl)-4-methyl-; (5) Naphthalene, 1, 2, 3, 5, 6, 8a-hexahydro4, 7-dimethyl-1-1-(1-methylethyl)-, (1S-cis)-; (6) Phenol, 2-methoxy-; (7) Benzaldehyde, 3-hydroxy-4-methoxy-; (8) 11, 13-Eicosadienoic acid, methyl ester; (9) 2-Furancarboxaldehyde, 5-methyl-; (10) Maltol; (11) Phenol; (12) Hydroquinone; (13) 1H-Indene, 1-ethylideneoctahydro-7a-methyl-, (1E, 3a.alpha, 7a.beta.). Other compounds (14) 3-methyl butanal; (15) (D)-Limonene; (16) 1-methyl-4-(1-methyl ethyl) benzene; (17) Butanoic acid methyl ester; (18) 2-methyl propanal; (19) 2-butanone; (20) 2-pentanone; and (21) 2-methyl butane were also identified when P&T GC-MS was performed. Of the 21 compounds identified, 12 were validated using chemical standards. The identified compounds were found to be terpenes, derivatives of terpenes, esters, ketones, aldehydes, and phenol-derived aromatic compounds; these are the primary constituents of the essential oils of many plants and flowers. PMID:24804069

  11. The Huygens Gas Chromatograph Mass Spectrometer Investigation Of Titan

    NASA Astrophysics Data System (ADS)

    Atreya, Sushil; Harpold, Dan; Owen, Tobias

    2015-04-01

    A decade ago, on 14 January 2005, the Huygens probe of the Cassini-Huygens mission descended through the smog filled atmosphere of Titan and landed on the surface, revealing for the first time the extraordinary nature of Saturn's largest moon. One of the six payload instruments, the gas chromatograph mass spectrometer (GCMS), was crucial for measuring the composition of the atmosphere and the surface of Titan [1,2]. Most of the GCMS findings were "firsts", including the first direct identification of molecular nitrogen as the bulk constituent of the atmosphere, first vertical profile of Titan's second most abundant volatile, methane, first determination of primordial and radiogenic argon, first quantification of a number of stable gas isotopes, and the first measurements of the make-up of Titan's surface. These data are key to understanding why Titan is so unique amongst planetary moons in possessing a massive atmosphere [3], how Titan maintains a cycle of methane complete with surface reservoirs, evaporation and condensation like the hydrological cycle on earth [3,4,5], and what is responsible for the photochemical smog on Titan that plays a central role in the very existence of an atmosphere on Titan [3]. This presentation will discuss the GCMS investigation and how it helped shape our current view of Titan. [website for downloading pdf's of relevant papers: www.umich.edu/~atreya] [1] Niemann, H. B. et al., The abundances of constituents of Titan's atmosphere from the GCMS instrument on the Huygens probe, Nature 438, 779-784, 2005. [2] Niemann, H. B. et al., The composition of Titan's lower atmosphere and simple surface volatiles as measured by the Cassini-Huygens probe gas chromatograph mass spectrometer experiment, J. Geophys. Res. (Planets) 115, 12006, 2010. [3] Atreya S. K., R. D. Lorenz and J. H. Waite, Volatile origin and cycles: Nitrogen and methane, in Titan from Cassini-Huygens, R. H. Brown, J. P. Lebreton and J. Waite, (eds.), Springer Dordrecht

  12. Liquid chromatographic separation of antidepressant drugs: I. Tricyclics.

    PubMed

    Beierle, F A; Hubbard, R W

    1983-01-01

    A simple normal-phase (silica), high-performance liquid chromatographic (HPLC) assay of amitriptyline (AMI), doxepin (DOX), imipramine (IMI), nortriptyline (NORT), desmethyldoxepin (DESDOX), desipramine (DESIP), and protriptyline (PRO) in serum with no coelution is described here. Trimipramine and promazine were used as internal standards. Extraction of the 1.0-ml serum samples (collected in plastic) was done with Bond-Elut C18 columns. The compounds of interest were eluted with 10 mM methanolic ammonium acetate. The eluates were evaporated at 56-58 degrees C and reconstituted with 200 microliters of the mobile phase. The mobile phase was absolute ethanol-acetonitrile-tert-butylamine (98:2:0.05, vol/vol/vol). Detection of eluted drugs was at 254 nm at 0.01 absorbance units full scale (AUFS), except for PRO, which was detected at 229 nm at 0.02 AUFS. Absolute recoveries were 87-97%. A 5-micron silica (4.6 X 250 mm) HPLC column was used; results with a 10-micron silica column (3.9 X 300 mm) are also presented. Peak height ratios with trimipramine were linear for each analyte between 25 and 1200 ng/ml. Peak height ratios with promazine as the internal standard were linear for each analyte between 25 and 600 ng/ml. Detection limits under the conditions described were 2 ng/ml for AMI, DOX, and IMI, 4 ng/ml for NORT, DESDOX, and DESIP, and 10 ng/ml for PRO. Coefficients of within-day and day-to-day variation at three concentration levels were less than 9.8% and less than 11.2%, respectively. The hydroxylated metabolites of IMI, DES, NORT, and the cis isomer of DOX are discussed. Steady-state daily dosages and corresponding serum levels are presented for 69 patients. The total assay time was less than 10 min for DESIP and 12 min for PRO. This assay can be used in correlating serum levels with clinical effects, compliancy, and pharmacokinetic studies.

  13. Liquid chromatographic separation of the stereoisomers of thiazide diuretics.

    PubMed

    Hyun, M H; Pirkle, W H

    2000-04-21

    A number of racemic thiazide diuretics and analogues were resolved on two diastereomeric chiral stationary phases (CSPs) prepared from (S)- or (R)-alpha-[1-(6,7-dimethyl)naphthyl]-10-dodecenylamine and (S)-2-phenylpropanoic acid. Of the two diastereomeric CSPs, the (S,S) and the (R,S), the former is found to be better than the latter in separating the enantiomers of the racemic thiazide diuretics and their analogues with complete separation being observed on the (S,S)-CSP. Chiral recognition is controlled principally by the (R)- or (S)-alpha-[1-(6,7-dimethyl)naphthyl]-10-dodecenylamine portion of the CSPs. The second stereogenic center of the CSP provides but secondary effects on the chiral recognition presumably involving, in the case of the (S,S)-CSP, face-to-edge pi-pi interaction between the aromatic ring of the analytes and the phenyl on the second stereogenic center.

  14. Thin-Layer Chromatographic Separation of Phenols: An Undergraduate Laboratory Experiment.

    ERIC Educational Resources Information Center

    Kurth, Mark J.

    1986-01-01

    Background information, procedures used, and equipment needed are provided for an experiment in which a series of readily available, inexpensive, and relatively nontoxic phenols are separated using thin-layer chromatographic techniques. The experiment permits a discussion of how relative Rf values may be rationalized by considering a molecule's…

  15. Multidimensional High-Resolution Gas Chromatographic Investigations of Hydrocarbon Fuels and Various Turbine Engine Fuel Precursors.

    DTIC Science & Technology

    1985-08-01

    Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy . 15. B. Welton, Column Switching and Backflush Techniques with Open Tubular and...Packed Columns in Gas Chromatography, Paper presented at 1978 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy . 16. R. Miller... Applied Spectroscopy . 33. J. F. Pankow and L. M. Isabelle, Interface of the Direct Coupling of a Second Gas Chromatograph to a Gas Chromatograph/ Mass

  16. [Chromatographic separation of activated proteases from human plasma].

    PubMed

    Lehmann, B; Taucher, M; Kühne, H; Scheuch, D W

    1988-01-01

    After separation of aceton and dextran sulfate activated human plasma by column chromatography on DEAE-cellulose three esterolytically and amidolytically active fractions, respectively, were obtained, which were assigned to the following species: plasma kallikrein (PK), PK.alpha-macroglobulin.HMW-Kininogen. Their percentage in the whole activity is variable. The proportion of free PK is low (0.11). For characterization of the products we studied inhibition by different polyvalent inhibitors. The Michaelis constant (Km) with p-toluene-sulfonyl-L-arginine methyl ester (TAME) were determined. For simulation of in vivo conditions dextran sulfate activated plasma was inactivated at 37 degrees C. The residual activity and the spontaneous activity in plasma from patients with shock are produced by different active protease inhibitor complexes.

  17. Micro-miniature gas chromatograph column disposed in silicon wafers

    DOEpatents

    Yu, Conrad M.

    2000-01-01

    A micro-miniature gas chromatograph column is fabricated by forming matching halves of a circular cross-section spiral microcapillary in two silicon wafers and then bonding the two wafers together using visual or physical alignment methods. Heating wires are deposited on the outside surfaces of each wafer in a spiral or serpentine pattern large enough in area to cover the whole microcapillary area inside the joined wafers. The visual alignment method includes etching through an alignment window in one wafer and a precision-matching alignment target in the other wafer. The two wafers are then bonded together using the window and target. The physical alignment methods include etching through vertical alignment holes in both wafers and then using pins or posts through corresponding vertical alignment holes to force precision alignment during bonding. The pins or posts may be withdrawn after curing of the bond. Once the wafers are bonded together, a solid phase of very pure silicone is injected in a solution of very pure chloroform into one end of the microcapillary. The chloroform lowers the viscosity of the silicone enough that a high pressure hypodermic needle with a thumbscrew plunger can force the solution into the whole length of the spiral microcapillary. The chloroform is then evaporated out slowly to leave the silicone behind in a deposit.

  18. Capillary gas chromatographic analysis of pans with luminol chemilumnescent detection

    SciTech Connect

    Gaffney, J.; Bornick, R.; Chen, Yu-Harn; Marley, N.

    1996-12-31

    Peroxyacyl nitrates (PANs) are important air pollutants in tropospheric chemistry. PANs are known to be potent phytotoxins at low ppb concentrations and are lachrymators. They can also transport the more reactive nitrogen dioxide long distances, because they are in equilibrium with that NO{sub x} species. Since PANs are trapped peroxyradicals, they are a direct measure of the peroxyradical levels and the of {open_quotes}photochemical age{close_quotes} of an air parcel. The PANs are typically measured in the atmosphere by using electron capture detection methods. These methods suffer from large background signals and detector responses to oxygen and water vapor. This paper describes the combination of a capillary gas chromatographic column with a modified luminol chemiluminescent nitrogen dioxide detector (Scintrex, Luminox) for rapid and sensitive detection of nitrogen dioxide, peroxyacetyl nitrate, peroxypropionyl nitrate, and peroxybutyryl nitrate. Detection limits for this approach in the low tens of parts per trillion have been observed with total analysis times of less than three minutes. We will discuss the potential application of this method to other compounds, particularly, organonitrates, in a pyrolysis system and/or with ozone addition to the sampling streams.

  19. Recent Advances in Water Analysis with Gas Chromatograph Mass Spectrometers

    NASA Technical Reports Server (NTRS)

    MacAskill, John A.; Tsikata, Edem

    2014-01-01

    We report on progress made in developing a water sampling system for detection and analysis of volatile organic compounds in water with a gas chromatograph mass spectrometer (GCMS). Two approaches are described herein. The first approach uses a custom water pre-concentrator for performing trap and purge of VOCs from water. The second approach uses a custom micro-volume, split-splitless injector that is compatible with air and water. These water sampling systems will enable a single GC-based instrument to analyze air and water samples for VOC content. As reduced mass, volume, and power is crucial for long-duration, manned space-exploration, these water sampling systems will demonstrate the ability of a GCMS to monitor both air and water quality of the astronaut environment, thereby reducing the amount of required instrumentation for long duration habitation. Laboratory prototypes of these water sampling systems have been constructed and tested with a quadrupole ion trap mass spectrometer as well as a thermal conductivity detector. Presented herein are details of these water sampling system with preliminary test results.

  20. High-speed counter-current chromatographic separation of phytosterols.

    PubMed

    Schröder, Markus; Vetter, Walter

    2011-07-01

    Phytosterols are bioactive compounds which occur in low concentrations in plant oils. Due to their beneficial effects on human health, phytosterols have already been supplemented to food. Commercial phytosterol standards show insufficient purity and/or are very expensive. In this study, we developed a high-speed counter-current chromatography (HSCCC) method for the fractionation and analysis of a commercial crude β-sitosterol standard (purity ∼60% according to supplier). Different solvent systems were tested in shake-flask experiments, and the system n-hexane/methanol/aqueous silver nitrate solution (34/24/1, v/v/v) was finally used for HSCCC fractionation. About 50 mg phytosterols was injected and distributed into 57 fractions. Selected fractions were condensed and re-injected into the HSCCC system. This measure provided pure sitostanol (>99%) and β-sitosterol (∼99%), as well as a mixture of campesterol and stigmasterol without further phytosterols. An enriched HSCCC fraction facilitated the mass spectrometric analysis of further 11 minor phytosterols (after trimethylsilylation). It was also shown that the commercial product contained about 0.3% carotinoids which eluted without delay into an early HSCCC fraction and which were separated from the phytosterols.

  1. Chromatographic separation as selection process for prebiotic evolution and the origin of the genetic code.

    PubMed

    Lehmann, U

    1985-01-01

    A model for the evolution of a translation apparatus has been suggested where oligonucleotides in a hairpin conformation act as primordial adapters. Specifically activated amino acids are assumed to be attached to these hairpin molecules. For the specific activation, a chromatographic separation of, e.g. ala and CMP from gly and GMP can be accomplished on silica (e.g. of volcanic origin) with aqueous salt solutions. Other adsorbents like clays (kaolin, bentonite, montmorillonite), different silicates (florisil, magnesium trisilicate, calcium silicate, talc), hydroxyapatite, barium sulfate, calcium carbonate, calcium fluoride and titanoxide have been examined as model systems for the separation of nucleotides, nucleosides and amino acids on mineral surfaces. The possible role of chromatographic separation of amino acids for the formation of proteinoids, composed of selected amino acids, is also considered.

  2. Ion chromatographic separation of inorganic ions using a combination of hydrophilic interaction chromatographic column and cation-exchange resin column.

    PubMed

    Arai, Kaori; Mori, Masanobu; Hironaga, Takahiro; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2012-04-01

    A combination of hydrophilic interaction chromatographic (HILIC) column and a weakly acidic cation-exchange resin (WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography (IC). Firstly, the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions. The columns used were SeQuant ZIC-HILIC (ZIC-HILIC) with a sulfobetaine-zwitterion stationary phase (ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase (HILIC-10). When using tartaric acid as the eluent, the HILIC columns indicated strong retentions for anions, based on ion-pair interaction. Especially, HILIC-10 could strongly retain anions compared with ZIC-HILIC. The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I(-) > NO3(-) > Br(-) > Cl(-) > H2PO4(-). However, since HILIC-10 could not separate analyte cations, a WCX column (TSKgel Super IC-A/C) was connected after the HILIC column in series. The combination column system of HILIC and WCX columns could successfully separate ten ions (Na+, NH4+, K+, Mg2+, Ca2+, H2PO4(-), Cl(-), Br(-), NO3(-) and I(-)) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6. The relative standard deviations (RSDs) of analyte ions by the system were in the ranges of 0.02% - 0.05% in retention times and 0.18% - 5.3% in peak areas through three-time successive injections. The limits of detection at signal-to-noise ratio of 3 were 0.24 - 0.30 micromol/L for the cations and 0.31 - 1.2 micromol/L for the anions. This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.

  3. Oxygen carrier for gas chromatographic analysis of inert gases in propellants

    NASA Technical Reports Server (NTRS)

    Cannon, W. A.

    1972-01-01

    Gas chromatographic determination of small quantities of inert gases in reactive propellants is discussed. Operating conditions used for specific analyses of helium in diborane and nitrogen in oxygen difluoride are presented in tabular form.

  4. A Miniature Gas Chromatograph Mass Spectrometer (GCMS) for Planetary Atmospheres Studies

    NASA Astrophysics Data System (ADS)

    Simcic, J.; Madzunkov, S. M.; Bae, B.; Nikolic, D.; Darrach, M.

    2016-10-01

    Presented herein are the latest achievements in developing an instrument with the same analytical performance of commercial Gas Chromatograph Mass Spectrometer systems but approximately an order of magnitude smaller and optimized for space missions.

  5. Gas chromatographic technologies for the analysis of essential oils.

    PubMed

    Marriot, P J; Shellie, R; Cornwell, C

    2001-11-30

    Essential oil analysis has basically had one technical goal: to achieve the best possible separation performance by using the most effective, available technology of the day. The result achieved from this may then be used to answer the research or industrial analysis questions which necessitated the analysis. This may be for comparative purposes, where one oil is contrasted with other(s) for quality control or investigation of adulteration, to discover new components, or to characterise the chemical classes of compounds present. Clearly, today the analyst turns to chromatography as the provider of separation and then may supplement that with mass spectrometry to aid identification. The power of GC-MS means that advances in both the separation technique, and improvements in mass spectrometry detection - along with improved data handling tools - will immediately be relevant to the essential oil area. This present review outlines the developmental nature of instrumental approaches to essential oil analysis using gas chromatography. Mass spectrometry will be included to the extent that it represents the hyphenation of choice for most analysts when analysing essential oils. Thus single-column and multi-dimensional analysis will be covered, as will sample handling or introduction techniques prior to the analysis step, where these techniques provide some measure of separation. The recent demonstration of comprehensive gas chromatography will be discussed as the potentially most powerful separation method for essential oils. This brief review is not intended to be a comprehensive dissertation on the field of essential oil analysis since that would require sufficient space to occupy a book in its own right. Rather, it will outline selected considerations and developments, to help explain where new technology has been applied to advantage in this field.

  6. Sensitive gas chromatographic detection of acetaldehyde and acetone using a reduction gas detector

    NASA Technical Reports Server (NTRS)

    O'Hara, Dean; Singh, Hanwant B.

    1988-01-01

    The response of a newly available mercuric oxide Reduction Gas Detector (RGD-2) to subpicomole and larger quantities of acetaldehyde and acetone is tested. The RGD-2 is found to be capable of subpicomole detection for these carbonyls and is more sensitive than an FID (Flame Ionization Detector) by an order of magnitude. Operating parameters can be further optimized to make the RGD-2 some 20-40 times more sensitive than an FID. The detector is linear over a wide range and is easily adapted to a conventional gas chromatograph (GC). Such a GC-RGD-2 system should be suitable for atmospheric carbonyl measurements in clean as well as polluted environments.

  7. Design and Performance of a Gas Chromatograph for Automatic Monitoring of Pollutants in Ambient Air

    NASA Technical Reports Server (NTRS)

    Villalobos, R.; Stevens, D.; LeBlanc, R.; Braun, L.

    1971-01-01

    In recent years, interest in air pollution constituents has focused on carbon monoxide and hydrocarbons as prime components of polluted air. Instrumental methods have been developed, and commercial instruments for continuous monitoring of these components have been available for a number of years. For the measurement of carbon monoxide, non-dispersive infrared spectroscopy has been the accepted tool, in spite of its marginal sensitivity at low parts-per-million levels. For continuously monitoring total hydrocarbons, the hydrogen flame ionization analyzer has been widely accepted as the preferred method. The inadequacy of this latter method became evident when it was concluded that methane is non-reactive and cannot be considered a contaminant even though present at over 1 ppm in the earth's atmosphere. Hence, the need for measuring methane separately became apparent as a means of measuring the reactive and potentially harmful non-methane hydrocarbons fraction. A gas chromatographic method for the measurement of methane and total hydrocarbons which met these requirements has been developed. In this technique, methane was separated on conventional gas chromatographic columns and detected by a hydrogen flame ionization detector (FID) while the total hydrocarbons were obtained by introducing a second sample directly into the FID without separating the various components. The reactive, or non-methane hydrocarbons, were determined by difference. Carbon monoxide was also measured after converting to methane over a heated catalyst to render it detectable by the FID. The development of this method made it possible to perform these measurements with a sensitivity of as much as 1 ppm full scale and a minimum detectability of 20 ppb. Incorporating this technique, criteria were developed by APCO for a second generation continuous automatic instrument for atmospheric monitoring stations.

  8. Improving Hydrocarbon Separation In Gas Chromatography

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.; Woeller, F.; Kojiro, D. R.

    1983-01-01

    Modified solica spheres enhance chromatographic separation. Commercially available silica spheres are modified by reacting them with molecules containing isocyante and isothiocyanate groups. Applications of surface derivatized spheres that result from reaction include analysis of samples prouced by atmospheric or soil probes.

  9. Advances in high-throughput and high-efficiency chiral liquid chromatographic separations.

    PubMed

    Patel, Darshan C; Wahab, M Farooq; Armstrong, Daniel W; Breitbach, Zachary S

    2016-10-07

    The need for improved liquid chromatographic chiral separations has led to the advancement of chiral screening techniques as well as the development of new, high efficiency chiral separation methods and stationary phases. This review covers these advancements, which primarily occurred over the last 15 years. High throughput techniques include multi-column screening units, multiple injection sequences, and fast gradient SFC screening. New separation methods and column technologies that aim at high efficiency chiral separations include the use of achiral UHPLC (i.e. sub-2μm) columns for separating derivatized chiral analytes or using chiral additives in the run buffer, UHPLC chiral stationary phases, and superficially porous particle based chiral stationary phases. Finally, the enhancement of chiral separations through these new technologies requires that certain instrumental considerations be made. Future directions in continuing to improve chiral separations are also discussed.

  10. Integrated vacuum absorption steam cycle gas separation

    DOEpatents

    Chen, Shiaguo [Champaign, IL; Lu, Yonggi [Urbana, IL; Rostam-Abadi, Massoud [Champaign, IL

    2011-11-22

    Methods and systems for separating a targeted gas from a gas stream emitted from a power plant. The gas stream is brought into contact with an absorption solution to preferentially absorb the targeted gas to be separated from the gas stream so that an absorbed gas is present within the absorption solution. This provides a gas-rich solution, which is introduced into a stripper. Low pressure exhaust steam from a low pressure steam turbine of the power plant is injected into the stripper with the gas-rich solution. The absorbed gas from the gas-rich solution is stripped in the stripper using the injected low pressure steam to provide a gas stream containing the targeted gas. The stripper is at or near vacuum. Water vapor in a gas stream from the stripper is condensed in a condenser operating at a pressure lower than the stripper to concentrate the targeted gas. Condensed water is separated from the concentrated targeted gas.

  11. Gas chromatographic method for measuring nitrogen dioxide and peroxyacetyl nitrate in air without compressed gas cylinders

    SciTech Connect

    Burkhardt, M.R.; Maniga, N.I.; Stedman, D.H.; Paur, R.J.

    1988-04-15

    A gas chromatographic technique that measures atmospheric concentrations of peroxyacetyl nitrate (PAN) and NO/sub 2/ has been developed that uses luminol-based chemiluminescence for detection. The carrier gas is air that has been scrubbed by passing it over FeSO/sub 4/, which eliminates the need for any compressed gas cylinders. A novel gas sampling system and time enable variable sample volumes of contaminated air to be injected. Ambient PAN and NO/sub 2/ measurements can be made every 40 s with detection limits of 0.12 ppb for PAN and 0.2 ppb for NO/sub 2/. Seven other atmospheric species, including ozone, gave no interference. Linear response was observed for NO/sub 2/ from 0.2 to 170 ppb and for PAN from 1 to 70 ppb.

  12. Chromatographic separation of three monoclonal antibody variants using multicolumn countercurrent solvent gradient purification (MCSGP).

    PubMed

    Müller-Späth, Thomas; Aumann, Lars; Melter, Lena; Ströhlein, Guido; Morbidelli, Massimo

    2008-08-15

    Multicolumn countercurrent solvent gradient purification (MCSGP) is a continuous chromatographic process developed in recent years (Aumann and Morbidelli, 2007a; Aumann et al., 2007) that is particularly suited for applications in the field of bioseparations. Like batch chromatography, MCSGP is suitable for three-fraction chromatographic separations and able to perform solvent gradients but it is superior in terms of solvent consumption, yield, purity, and productivity due to the countercurrent movement of the liquid and the solid phases. In this work, the MCSGP process is applied to the separation of three monoclonal antibody variants on a conventional preparative cation exchange resin. The experimental process performance was compared to simulations based on a lumped kinetic model. Yield and purity values of the target variant of 93%, respectively were obtained experimentally. The batch reference process was clearly outperformed by the MCSGP process.

  13. Chromatographic separation of germanium and arsenic for the production of high purity (77)As.

    PubMed

    Gott, Matthew D; DeGraffenreid, Anthony J; Feng, Yutian; Phipps, Michael D; Wycoff, Donald E; Embree, Mary F; Cutler, Cathy S; Ketring, Alan R; Jurisson, Silvia S

    2016-04-08

    A simple column chromatographic method was developed to isolate (77)As (94±6% (EtOH/HCl); 74±11 (MeOH)) from germanium for potential use in radioimmunotherapy. The separation of arsenic from germanium was based on their relative affinities for different chromatographic materials in aqueous and organic environments. Using an organic or mixed mobile phase, germanium was selectively retained on a silica gel column as germanate, while arsenic was eluted from the column as arsenate. Subsequently, enriched (76)Ge (98±2) was recovered for reuse by elution with aqueous solution (neutral to basic). Greater than 98% radiolabeling yield of a (77)As-trithiol was observed from methanol separated [(77)As]arsenate [17].

  14. Anisotropic membranes for gas separation

    DOEpatents

    Gollan, Arye Z.

    1987-01-01

    A gas separation membrane has a dense separating layer about 10,000 Angstroms or less thick and a porous support layer 10 to 400 microns thick that is an integral unit with gradually and continuously decreasing pore size from the base of the support layer to the surface of the thin separating layer and is made from a casting solution comprising ethyl cellulose and ethyl cellulose-based blends, typically greater than 47.5 ethoxyl content ethyl cellulose blended with compatible second polymers, such as nitrocellulose. The polymer content of the casting solution is from about 10% to about 35% by weight of the total solution with up to about 50% of this polymer weight a compatible second polymer to the ethyl cellulose in a volatile solvent such as isopropanol, methylacetate, methanol, ethanol, and acetone. Typical nonsolvents for the casting solutions include water and formamide. The casting solution is cast in air from about zero to 10 seconds to allow the volatile solvent to evaporate and then quenched in a coagulation bath, typically water, at a temperature of 7.degree.-25.degree. C. and then air dried at ambient temperature, typically 10.degree.-30.degree. C.

  15. Anisotropic membranes for gas separation

    DOEpatents

    Gollan, A.Z.

    1987-07-21

    A gas separation membrane has a dense separating layer about 10,000 Angstroms or less thick and a porous support layer 10 to 400 microns thick that is an integral unit with gradually and continuously decreasing pore size from the base of the support layer to the surface of the thin separating layer and is made from a casting solution comprising ethyl cellulose and ethyl cellulose-based blends, typically greater than 47.5 ethoxyl content ethyl cellulose blended with compatible second polymers, such as nitrocellulose. The polymer content of the casting solution is from about 10% to about 35% by weight of the total solution with up to about 50% of this polymer weight a compatible second polymer to the ethyl cellulose in a volatile solvent such as isopropanol, methylacetate, methanol, ethanol, and acetone. Typical nonsolvents for the casting solutions include water and formamide. The casting solution is cast in air from about zero to 10 seconds to allow the volatile solvent to evaporate and then quenched in a coagulation bath, typically water, at a temperature of 7--25 C and then air dried at ambient temperature, typically 10--30 C. 2 figs.

  16. Passive gas separator and accumulator device

    DOEpatents

    Choe, H.; Fallas, T.T.

    1994-08-02

    A separation device employing a gas separation filter and swirler vanes for separating gas from a gas-liquid mixture is provided. The cylindrical filter utilizes the principle that surface tension in the pores of the filter prevents gas bubbles from passing through. As a result, the gas collects in the interior region of the filter and coalesces to form larger bubbles in the center of the device. The device is particularly suited for use in microgravity conditions since the swirlers induce a centrifugal force which causes liquid to move from the inner region of the filter, pass the pores, and flow through the outlet of the device while the entrained gas is trapped by the filter. The device includes a cylindrical gas storage screen which is enclosed by the cylindrical gas separation filter. The screen has pores that are larger than those of the filters. The screen prevents larger bubbles that have been formed from reaching and interfering with the pores of the gas separation filter. The device is initially filled with a gas other than that which is to be separated. This technique results in separation of the gas even before gas bubbles are present in the mixture. Initially filling the device with the dissimilar gas and preventing the gas from escaping before operation can be accomplished by sealing the dissimilar gas in the inner region of the separation device with a ruptured disc which can be ruptured when the device is activated for use. 3 figs.

  17. Passive gas separator and accumulator device

    DOEpatents

    Choe, Hwang; Fallas, Thomas T.

    1994-01-01

    A separation device employing a gas separation filter and swirler vanes for separating gas from a gasliquid mixture is provided. The cylindrical filter utilizes the principle that surface tension in the pores of the filter prevents gas bubbles from passing through. As a result, the gas collects in the interior region of the filter and coalesces to form larger bubbles in the center of the device. The device is particularly suited for use in microgravity conditions since the swirlers induce a centrifugal force which causes liquid to move from the inner region of the filter, pass the pores, and flow through the outlet of the device while the entrained gas is trapped by the filter. The device includes a cylindrical gas storage screen which is enclosed by the cylindrical gas separation filter. The screen has pores that are larger than those of the filters. The screen prevents larger bubbles that have been formed from reaching and interfering with the pores of the gas separation filter. The device is initially filled with a gas other than that which is to be separated. This technique results in separation of the gas even before gas bubbles are present in the mixture. Initially filling the device with the dissimilar gas and preventing the gas from escaping before operation can be accomplished by sealing the dissimilar gas in the inner region of the separation device with a ruptured disc which can be ruptured when the device is activated for use.

  18. Application of Sigmoidal Transformation Functions in Optimization of Micellar Liquid Chromatographic Separation of Six Quinolone Antibiotics.

    PubMed

    Hadjmohammadi, Mohammadreza; Salary, Mina

    2016-03-01

    A chemometrics approach has been used to optimize the separation of six quinolone compounds by micellar liquid chromatography (MLC). A Derringer's desirability function, a multicriteria decision-making (MCDM) method, was tested for evaluation of two different measures of chromatographic performance (resolution and analysis time). The effect of three experimental parameters on a chromatographic response function (CRF) expressed as a product of two sigmoidal desirability functions was investigated. The sigmoidal functions were used to transform the optimization criteria, resolution and analysis time into the desirability values. The factors studied were the concentration of sodium dodecyl sulfate, butanol content and pH of the mobile phase. The experiments were done according to the face-centered cube central composite design, and the calculated CRF values were fitted to a polynomial model to correlate the CRF values with the variables and their interactions. The developed regression model showed good descriptive and predictive ability (R(2) = 0.815, F = 6.919, SE = 0.038, [Formula: see text]) and used, by a grid search algorithm, to optimize the chromatographic conditions for the separation of the mixture. The efficiency of prediction of polynomial model was confirmed by performing the experiment under the optimal conditions.

  19. Liquid chromatographic separation in metal-organic framework MIL-101: a molecular simulation study.

    PubMed

    Hu, Zhongqiao; Chen, Yifei; Jiang, Jianwen

    2013-02-05

    A molecular simulation study is reported to investigate liquid chromatographic separation in metal-organic framework MIL-101. Two mixtures are considered: three amino acids (Arg, Phe, and Trp) in aqueous solution and three xylene isomers (p-, m-, and o-xylene) dissolved in hexane. For the first mixture, the elution order is found to be Arg > Phe > Trp. The hydrophilic Arg has the strongest interaction with the polar mobile phase (water) and the weakest interaction with the stationary phase (MIL-101), and thus transports at the fastest velocity. Furthermore, Arg forms the largest number of hydrogen bonds with water and possesses the largest hydrophilic solvent-accessible surface area. For the second mixture, the elution order is p-xylene > m-xylene > o-xylene, consistent with available experimental observation. With the largest polarity as compared to p- and m-xylenes, o-xylene interacts the most strongly with the stationary phase and exhibits the slowest transport velocity. For both mixtures, the underlying separation mechanism is elucidated from detailed energetic and structural analysis. It is revealed that the separation can be attributed to the cooperative solute-solvent and solute-framework interactions. This simulation study, for the first time, provides molecular insight into liquid chromatographic separation in a MOF and suggests that MIL-101 might be an interesting material for the separation of industrially important liquid mixtures.

  20. 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.

  1. Superheated water as chromatographic eluent for parabens separation on octadecyl coated zirconia stationary phase.

    PubMed

    Dugo, Paola; Buonasera, Katia; Crupi, Maria Lucia; Cacciola, Francesco; Dugo, Giovanni; Mondello, Luigi

    2007-05-01

    In this study, the use of pure water at superheated temperatures, between 100 and 200 degrees C, as a mobile phase for RP separation is explored. Instrumental parameters, such as temperature, flow rate, preheating and cooling, have shown significant effects on the quality of the chromatographic peaks. The properties of superheated water as an eluent were investigated by observing the chromatographic behaviour of four parabens on a carbon-clad zirconia (ZR) phase with covalently bonded octadecyl groups. Results were compared with those obtained at 30 degrees C on a silica-based phase with octadecyl groups, using water and ACN as mobile phase. The optimized method was finally applied to analyse parabens in a commercial body cream.

  2. High-resolution gas chromatographic profiles of volatile organic compounds produced by microorganisms at refrigerated temperatures.

    PubMed Central

    Lee, M L; Smith, D L; Freeman, L R

    1979-01-01

    Three different strains of bacteria isolated from spoiled, uncooked chicken were grown in pure culture on Trypticase soy agar supplemented with yeast extract. The volatile organic compounds produced by each culture were concentrated on a porous polymer precolumn and analyzed by high-resolution gas chromatographic mass spectrometry. Twenty different compounds were identified. Both qualitative and quantitative differences in the chromatographic profiles from each culture were found. PMID:104660

  3. Liquid Chromatographic Separation and Thermodynamic Investigation of Mirabegron Enantiomers on a Chiralpak AY-H Column.

    PubMed

    Zhou, Fan; Zhou, Yuxia; Zou, Qiaogen; Sun, Lili; Wei, Ping

    2015-09-01

    Liquid chromatographic separation of mirabegron enantiomers on Chiralpak AY-H, a column coated with amylose tris-(5-chloro-2-methylphenylcarbamate) as a chiral stationary phase, was studied under normal phase conditions. The influence of ethanol content (30-45%) and column temperature (20-40°C) on retention, resolution and separation were evaluated. Apparent thermodynamic parameters deduced from Van't Hoff plots were used to understand chiral separation mechanisms, and the chiral separation was enthalpy driven. The optimized chromatographic conditions were using a mixture solution of n-hexane, ethanol and diethyl amine (55 : 45 : 0.1, v/v/v) as a mobile phase at a flow rate of 1.0 mL/min. The column temperature and UV detector were set at 35°C and 254 nm, respectively. The method was validated to be simple, accuracy, sensitive and robust according to the ICH guidelines, and it was suitable for the routine quality control of mirabegron enantiomers for pharmaceutical industries.

  4. Thermal soil desorption for total petroleum hydrocarbon testing on gas chromatographs

    SciTech Connect

    Mott, J.

    1995-12-31

    Testing for total petroleum hydrocarbons (TPH) is one of the most common analytical tests today. A recent development in chromatography incorporates Thermal Soil Desorption technology to enable analyses of unprepared soil samples for volatiles such as BTEX components and semi-volatiles such as diesel, PCBs, PAHs and pesticides in the same chromatogram, while in the field. A gas chromatograph is the preferred method for determining TPH because the column in a GC separates the individual hydrocarbons compounds such as benzene and toluene from each other and measures each individually. A GC analysis will determine not only the total amount of hydrocarbon, but also whether it is gasoline, diesel or another compound. TPH analysis with a GC is typically conducted with a Flame Ionization Detector (FID). Extensive field and laboratory testing has shown that incorporation of a Thermal Soil Desorber offers many benefits over traditional analytical testing methods such as Headspace, Solvent Extraction, and Purge and Trap. This paper presents the process of implementing Thermal Soil Desorption in gas chromatography, including procedures for, and advantages of faster testing and analysis times, concurrent volatile and semi-volatile analysis, minimized sample manipulation, single gas (H{sub 2}) operation, and detection to the part-per billion levels.

  5. Recirculating gas separator for electric submersible

    SciTech Connect

    Powers, M.L.

    1991-01-01

    This patent describes a gas separator apparatus for a submersible well pump. It comprises: a rotary gas separator means; and recirculating means for recirculating a portion of the liquid discharged from the discharge outlet back to the separating chamber so that a gas-to-liquid ratio in the separator means is substantially lower than a gas-to-liquid ratio of well fluid entering the well fluid inlet wherein the recirculating means. This patent also describes a method of pumping liquid from a well producing well fluids having a relatively high gas-to-liquid ratio. It comprises: centrifugally separating the well fluid into a liquid and a gas with a separator located downhole in the well; directing the separated liquid toward an inlet of a submersible well pump; recycling a portion of the separated liquid to the separator; and providing an effective gas-to-liquid ratio in the separator substantially lower than a gas-to-liquid ratio of the well fluid prior to separation.

  6. LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF TRANS-CHLORDANE, CIS-CHLORDANE, HEPTACHLOR, HEPTACHLOR EPOXIDE AND ALPHA-HEXACHLOROCYCLOHEXANE WITH APPLICATION TO SMALL-SCALE PREPARATIVE SEPARATION

    EPA Science Inventory

    Analytical high-performance liquid chromatographic separations of the individual enantiomers of five polychlorinated compounds were obtained on polysaccharide stereoselective HPLC columns. The enantiomers of the pesticides trans-chlordane, cis-chlordane and heptachlor were separa...

  7. A trade off between separation, detection and sustainability in liquid chromatographic fingerprinting.

    PubMed

    Funari, Cristiano S; Carneiro, Renato L; Cavalheiro, Alberto J; Hilder, Emily F

    2014-08-08

    It is now recognized that analytical chemistry must also be a target for green principles, in particular chromatographic methods which typically use relatively large volumes of hazardous organic solvents. More generally, high performance liquid chromatography (HPLC) is employed routinely for quality control of complex mixtures in various industries. Acetonitrile and methanol are the most commonly used organic solvents in HPLC, but they generate an impact on the environment and can have a negative effect on the health of analysts. Ethanol offers an exciting alternative as a less toxic, biodegradable solvent for HPLC. In this work we demonstrate that replacement of acetonitrile with ethanol as the organic modifier for HPLC can be achieved without significantly compromising analytical performance. This general approach is demonstrated through the specific example analysis of a complex plant extract. A benchmark method employing acetonitrile for the analysis of Bidens pilosa extract was statistically optimized using the Green Chromatographic Fingerprinting Response (GCFR) which includes factors relating to separation performance and environmental parameters. Methods employing ethanol at 30 and 80°C were developed and compared with the reference method regarding their performance of separation (GCFR) as well as by a new metric, Comprehensive Metric to Compare Liquid Chromatography Methods (CM). The fingerprint with ethanol at 80°C was similar to or better than that with MeCN according to GCFR and CM. This demonstrates that temperature may be used to replace harmful solvents with greener ones in HPLC, including for solvents with significantly different physiochemical properties and without loss in separation performance. This work offers a general approach for the chromatographic analysis of complex samples without compromising green analytical chemistry principles.

  8. Gas chromatographic column for the storage of sample profiles

    NASA Technical Reports Server (NTRS)

    Dimandja, J. M.; Valentin, J. R.; Phillips, J. B.

    1994-01-01

    The concept of a sample retention column that preserves the true time profile of an analyte of interest is studied. This storage system allows for the detection to be done at convenient times, as opposed to the nearly continuous monitoring that is required by other systems to preserve a sample time profile. The sample storage column is essentially a gas chromatography column, although its use is not the separation of sample components. The functions of the storage column are the selective isolation of the component of interest from the rest of the components present in the sample and the storage of this component as a function of time. Using octane as a test substance, the sample storage system was optimized with respect to such parameters as storage and readout temperature, flow rate through the storage column, column efficiency and storage time. A 3-h sample profile was collected and stored at 30 degrees C for 20 h. The profile was then retrieved, essentially intact, in 5 min at 130 degrees C.

  9. [Development of online conventional array-based two-dimensional liquid chromatographic system for proteins separation in human plasma].

    PubMed

    Huang, Zhi; Hong, Guangfeng; Gao, Mingxia; Zhang, Xiangmin

    2014-04-01

    Human plasma is one of the proteins-containing samples most difficult to characterize on account of the wide dynamic concentration range of its intact proteins. Herein, we developed a high-throughput conventional array-based two-dimensional liquid chromatographic system for proteins separation in human plasma in online mode. In the system, a conventional strong-anion exchange chromatographic column was used as the first separation dimension and eight parallel conventional reversed-phase liquid chromatographic columns were integrated as the second separation dimension. The fractions from the first dimension were sequentially transferred into the corresponding reversed-phase liquid chromatographic precolumns for retention and enrichment using a 10-port electrically actuated multi-position valve. The second dimensional solvent flow was directly and identically split into 8 channels. The fractions were concurrently back-flushed from the precolumns into the 8 conventional RP columns and were separated simultaneously. An 8-channel fraction collector was refitted to collect the reversed-phase liquid chromatographic fractions for further investigation. Bicinchoninic acid (BCA) dyein solution was conveniently used for high-abundance protein location. Two separation dimensions were relatively independent parts, as well as each channel of the second dimensional array separation. Therefore, the new system could improve the separation throughput and total peak capacity. The system was successfully applied for the separation of human plasma intact proteins. The results indicated the established system is an effective method for removing high abundance proteins in plasma and in-depth research in plasma proteomics.

  10. Clickable Periodic Mesoporous Organosilica Monolith for Highly Efficient Capillary Chromatographic Separation.

    PubMed

    Wu, Ci; Liang, Yu; Yang, Kaiguang; Min, Yi; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

    2016-02-02

    A novel clickable periodic mesoporous organosilica monolith with the surface area up to 1707 m(2) g(-1) was in situ synthesized in the capillary by the one-step condensation of the organobridged-bonded alkoxysilane precursor bis(triethoxysilyl)ethylene. With Si-C bonds in the skeleton, the monolith possesses excellent chemical and mechanical stability. With vinyl groups highly loaded and homogeneously distributed throughout the structure, the monolith can be readily functionalized with functional groups by effective thiol-ene "click" chemistry reaction. Herein, with "click" modification of C18, the obtained monolith was successfully applied for capillary liquid chromatographic separation of small molecules and proteins. The column efficiency could reach 148,000 N/m, higher than most reported hybrid monoliths. Moreover, intact proteins could be separated well with good reproducibility, even after the monolithic column was exposed by basic mobile phase (pH 10.0) overnight, demonstrating the great promising of such monolith for capillary chromatographic separation.

  11. Extraction chromatographic separations of tantalum and tungsten from hafnium and complex matrix constituents.

    PubMed

    Snow, Mathew S; Finck, Martha R; Carney, Kevin P; Morrison, Samuel S

    2017-02-10

    Tantalum (Ta), hafnium (Hf), and tungsten (W) analyses from complex matrices require high purification of these analytes from each other and major/trace matrix constituents, however, current state-of-the-art Ta/Hf/W separations rely on traditional anion exchange approaches that show relatively similar distribution coefficient (Kd) values for each element. This work reports an assessment of three commercially available extraction chromatographic resins (TEVA, TRU, and UTEVA) for Ta/Hf/W separations. Batch contact studies show differences in Ta/Hf and Ta/W Kd values of up to 10(6) and 10(4) (respectively), representing an improvement of a factor of 100 and 300 in Ta/Hf and Ta/W Kd values (respectively) over AG1×4 resin. Variations in the Kd values as a function of HCl concentration for TRU resin show that this resin is well suited for Ta/Hf/W separations, with Ta/Hf, Ta/W, and W/Hf Kd value improvements of 10, 200, and 30 (respectively) over AG1×4 resin. Analyses of digested soil samples (NIST 2710a) using TRU resin and tandem TEVA-TRU columns demonstrate the ability to achieve extremely high purification (>99%) of Ta and W from each other and Hf, as well as enabling very high purification of Ta and W from the major and trace elemental constituents present in soils using a single chromatographic step.

  12. Electrochemical stabilization of transplutonium-element valence states under chromatographic separation conditions

    SciTech Connect

    Kosyakov, V.N.; Yakovlev, N.G.; Vlasov, M.M.

    1987-03-01

    The example of separating berkelium and trivalent transplutonium elements (TPE) is considered for an extraction-chromatographic system containing 4 mole/liter HNO/sub 3/ with D2EHPA, which demonstrates the scope for electrochemical stabilization of valency states. The carrier for the stationary organic phase was a corrosion-resistant conducting material of large surface area (ground vitrocarbon, graphitized carbon fiber, etc.), which at the same time was the working electrode in an electrochemical cell supplied with the appropriate potential. The method does not require the addition of oxidizing or reducing agents and allows remote control.

  13. Chromatographic separation of phenylpropanol enantiomers on a quinidine carbamate-type chiral stationary phase

    SciTech Connect

    Asnin, Leonid; Guiochon, Georges A

    2005-07-01

    The retention and the separation of the enantiomers of 1-phenylpropanol (1PP), 2-phenylpropanol (2PP), and 3-chloro-1-phenylpropanol (3CPP) on silica-bonded quinidine carbamate under normal phase HPLC conditions were investigated. A relatively high selectivity of the stationary phase for 3CPP and 1PP ({alpha} {approx} 1.07-1.09) was achieved with eluents containing ethyl acetate as the polar modifier. These mobile phases were examined in detail. Based on the set of chromatographic and thermodynamic data collected, conclusions regarding the mechanism of enantioselectivity and the structure of the selector chiral center are made.

  14. New Method for Evaluating Irreversible Adsorption and Stationary Phase Bleed in Gas Chromatographic Capillary Columns

    SciTech Connect

    Wright, Bob W.; Wright, Cherylyn W.

    2012-10-26

    A novel method for the evaluation of gas chromatographic (GC) column inertness has been developed using a tandem GC approach. Typically column inertness is measured by analyte peak shape evaluation. In general, silica, glass, and metal surfaces are chemically reactive and can cause analyte adsorption, which typically is observed as chromatographic peak tailing. Adsorption processes produce broad, short chromatographic peaks that confound peak area determinations because a significant portion can reside in the noise. In addition, chromatographic surfaces and stationary phases can irreversibly adsorb certain analytes without obvious degradation of peak shape. The inertness measurements described in this work specifically determine the degree of irreversible adsorption behavior of specific target compounds at levels ranging from approximately 50 picograms to 1 nanogram on selected gas chromatographic columns. Chromatographic columns with 5% phenylmethylsiloxane, polyethylene glycol (wax), trifluoropropylsiloxane, and 78% cyanopropylsiloxane stationary phases were evaluated with a variety of phosphorus- and sulfur- containing compounds selected as test compounds due to their ease of adsorption and importance in trace analytical detection. In addition, the method was shown effective for characterizing column bleed.

  15. On-line gas chromatographic analysis of higher alcohol synthesis products from syngas.

    PubMed

    Andersson, Robert; Boutonnet, Magali; Järås, Sven

    2012-07-20

    An on-line gas chromatographic (GC) system has been developed for rapid and accurate product analysis in catalytic conversion of syngas (a mixture of H₂ and CO) to alcohols, so called "higher alcohol synthesis (HAS)". Conversion of syngas to higher alcohols is an interesting second step in the route of converting coal, natural gas and possibly biomass to liquid alcohol fuel and chemicals. The presented GC system and method are developed for analysis of the products formed from syngas using alkali promoted MoS₂ catalysts, however it is not limited to these types of catalysts. During higher alcohol synthesis not only the wanted short alcohols (∼C₂-C₅) are produced, but also a great number of other products in smaller or greater amounts, they are mainly short hydrocarbons (olefins, paraffins, branched, non-branched), aldehydes, esters and ketones as well as CO₂, H₂O. Trace amounts of sulfur-containing compounds can also be found in the product effluent when sulfur-containing catalysts are used and/or sulfur-containing syngas is feed. In the presented GC system, most of them can be separated and analyzed within 60 min without the use of cryogenic cooling. Previously, product analysis in "higher alcohol synthesis" has in most cases been carried out partly on-line and partly off-line, where the light gases (gases at room temp) are analyzed on-line and liquid products (liquid at room temp) are collected in a trap for later analysis off-line. This method suffers from many drawbacks compared to a complete on-line GC system. In this paper an on-line system using an Agilent 7890 gas chromatograph equipped with two flame ionization detectors (FID) and a thermal conductivity detector (TCD), together with an Agilent 6890 with sulfur chemiluminescence dual plasma detector (SCD) is presented. A two-dimensional GC system with Deans switch (heart-cut) and two capillary columns (HP-FFAP and HP-Al₂O₃) was used for analysis of the organic products on the FIDs. Light

  16. Development and evaluation of a gas chromatographic method for the determination of triazine herbicides in natural water samples

    USGS Publications Warehouse

    Steinheimer, T.R.; Brooks, M.G.

    1984-01-01

    A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0.1 ??g/L in a 1-litre sample. Three different natural water samples were used for error analysis via evaluation of recovery efficiencies and estimation of overall method precision. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.A multi-residue method is described for the determination of triazine herbicides in natural water samples. The technique uses solvent extraction followed by gas chromatographic separation and detection employing nitrogen-selective devices. Seven compounds can be determined simultaneously at a nominal detection limit of 0. 1 mu g/L in a 1-litre sample. As an alternative to liquid-liquid partition (solvent extraction) for removal of compounds of interest from water, solid-phase extraction (SPE) techniques employing chromatographic grade silicas with chemically modified surfaces have been examined. SPE is found to provide rapid and efficient concentration with quantitative recovery of some triazine herbicides from natural water samples. Concentration factors of 500 to 1000 times are obtained readily by the SPE technique.

  17. Rapid detection of bacteria with miniaturized pyrolysis-gas chromatographic analysis

    NASA Astrophysics Data System (ADS)

    Mowry, Curtis; Morgan, Catherine H.; Baca, Quentin; Manginell, Ronald P.; Kottenstette, Richard J.; Lewis, Patrick; Frye-Mason, Gregory C.

    2002-02-01

    Rapid detection and identification of bacteria and other pathogens is important for many civilian and military applications. The profiles of biological markers such as fatty acids can be used to characterize biological samples or to distinguish bacteria at the gram-type, genera, and even species level. Common methods for whole cell bacterial analysis are neither portable nor rapid, requiring lengthy, labor intensive sample preparation and bench-scale instrumentation. These methods chemically derivatize fatty acids to produce more volatile fatty acid methyl esters (FAMEs) that can be separated and analyzed by a gas chromatograph (GC)/mass spectrometer. More recent publications demonstrate decreased sample preparation time with in situ derivatization of whole bacterial samples using pyrolysis/derivatization. Ongoing development of miniaturized pyrolysis/GC instrumentation by this department capitalizes on Sandia advances in the field of microfabricated chemical analysis systems ((mu) ChemLab). Microdevices include rapidly heated stages capable of pyrolysis or sample concentration, gas chromatography columns, and surface acoustic wave (SAW) sensor arrays. We will present results demonstrating the capabilities of these devices toward fulfilling the goal of portable, rapid detection and early warning of the presence of pathogens in air or water.

  18. Capillary gas chromatographic analysis of nitrogen dioxide and pans with luminol chemiluminescent detection.

    SciTech Connect

    Gaffney, J. S.; Bornick, R. M.; Chen, Y.-H.; Marley, N. A.; Environmental Research

    1998-01-01

    Peroxyacyl nitrates (PANs) and nitrogen dioxide are important atmospheric air pollutants in the troposphere. These atmospheric nitrogen species are strongly coupled chemically by a clearly temperature-dependent equilibrium in the troposphere. A chemical method that can measure both nitrogen dioxide and PANs rapidly and with sub-part-per-billion detection is described that is based upon a modified luminol detection system coupled to a capillary gas chromatographic column by using helium as a carrier. The system can readily separate and detect nitrogen dioxide, peroxyacetyl nitrate, peroxyproprionyl nitrate, and peroxybutyrl nitrate with detection limits in the low tens of parts per trillion with total analysis time of less than 1 min. Calibration of PAN by thermal decomposition to nitrogen dioxide is demonstrated with PAN detection sensitivities approximately 75% of the sensitivities observed for NO2 luminol detection by using helium as a carrier gas. The advantages of this method for simultaneous measurement of nitrogen dioxide and PANs over ozone chemiluminescent detection and electron capture detection are discussed, as well as potential applications of this method for heterogeneous surface chemistry studies of PANs and nitrogen dioxide and for tropospheric measurements.

  19. Extraction chromatographic separation of promethium from high active waste solutions of Purex origin

    SciTech Connect

    Ramanujam, A.; Achuthan, P.V.; Dhami, P.S.; Gopalakrishnan, V.; Kannan, R.; Mathur, J.N.

    1995-03-01

    An extraction chromatographic procedure for the separation of {sup 147}Pm from High Active Waste solutions of Purex process has been developed. Octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide(CMPO) and 2-ethylhexyl-2-ethylhexylphosphonic acid (KSM-17), both sorbed separately on an inert support(chromosorb-102) have been sequentially employed for this purpose. In the CMPO column, the rare earths and the trivalent actinides are sorbed together with uranium, plutonium and traces of few other fission products. The elution of this column with 0.04 M HNO{sub 3} gives an eluate containing trivalent actinides and lanthanides. This solution, after adjusting the pH to 2.0, is used as feed for the second extraction chromatographic column based on KSM-17. All the trivalent metal ions are sorbed on the column leaving the trace impurities in the effluent. Fractional elution of the metal ions from this column is carried out with nitric acid of varying concentrations. At 0.09 M HNO{sub 3}, the pure beta emitting fraction of {sup 147}Pm has been obtained. 16 refs., 3 figs., 2 tabs.

  20. Remotely detected NMR for the characterization of flow and fast chromatographic separations using organic polymer monoliths.

    PubMed

    Teisseyre, Thomas Z; Urban, Jiri; Halpern-Manners, Nicholas W; Chambers, Stuart D; Bajaj, Vikram S; Svec, Frantisek; Pines, Alexander

    2011-08-01

    An application of remotely detected magnetic resonance imaging is demonstrated for the characterization of flow and the detection of fast, small molecule separations within hypercrosslinked polymer monoliths. The hyper-cross-linked monoliths exhibited excellent ruggedness, with a transit time relative standard deviation of less than 2.1%, even after more than 300 column volumes were pumped through at high pressure and flow. Magnetic resonance imaging enabled high-resolution intensity and velocity-encoded images of mobile phase flow through the monolith. The images confirm that the presence of a polymer monolith within the capillary disrupts the parabolic laminar flow profile that is characteristic of mobile phase flow within an open tube. As a result, the mobile phase and analytes are equally distributed in the radial direction throughout the monolith. Also, in-line monitoring of chromatographic separations of small molecules at high flow rates is shown. The coupling of monolithic chromatography columns and NMR provides both real-time peak detection and chemical shift information for small aromatic molecules. These experiments demonstrate the unique power of magnetic resonance, both direct and remote, in studying chromatographic processes.

  1. Dried calcium alginate/magnetite spheres: a new support for chromatographic separations and enzyme immobilization

    SciTech Connect

    Burns, M.A.; Kvesitadze, G.I.; Graves, D.J.

    1985-02-01

    Dried spheres made from an alginate solution containing magnetite particles have excellent potential as a support for enzyme immobilization and chromatographic applications. The beads were found to be much stronger than gels such as polyacrylamide and dextran, indicating that high flow rates and pressures could be used in column separations. The support withstood not only temperatures of up to 120/sup 0/C, but also most pH values and common solvents. While some solutions, such as phosphate buffers, dissolved the spheres, stabilization with Tyzor TE eliminated this problem. The physical properties of the beads include a glasslike density of 2.2 g/mL, excellent sphericity, low porosity, and a narrow size distribution. The magnetite present in the support allows the beads to be used for magnetic separations such as high gradient magnetic filtration. Their high degree of microroughness provides a large exposed surface area for enzyme and ligand binding. Mixed Actinomyces fradiae proteases and Aspergillus niger ..cap alpha..-amylase, two enzymes representative of classes which attack large substrates, were immobilized on the bead's surface with high activity and stability. A cyanuric dye which can be used in chromatographic applications (Cibacron Blue F3GA) was also readily coupled to the surface of this support with good yield.

  2. Gas chromatographic determination of water in organic compounds and of organic compounds in water after steam distillations

    SciTech Connect

    Dix, K.D.

    1990-01-01

    A gas chromatograph (GC) with a flame ionization detector (FID) is shown to be effective in the determination of water in organic compounds. Since the FID gives little response for water, a reaction is needed to convert water into a detectable species. The ketal, 2,2-dimethoxypropane (DMP), reacts quantitatively with water to yield the products methanol and acetone when an acid catalyst is present. Acetone is easily determined with a GC equipped with a capillary column and FID. A solid acid catalyst, Nafion, has been effective and is easily separated before sample introduction into the GC.

  3. Novel behavior of the chromatographic separation of linear and cyclic polymers

    PubMed Central

    Montenegro-Burke, J. Rafael; Bennett, Jackson M.; McLean, John A.; Hercules, David M.

    2016-01-01

    In various polymerization processes, the formation of a wide variety of chains, not only in length but also in chemical composition, broadly complicates comprehensive polymer characterization. In this communication, we compare different stationary and mobile phases for the analysis of complex polymer mixtures via size-exclusion chromatography-mass spectrometry (SEC-MS). To the best of our knowledge, we report novel chromatographic effects for the separation of linear and cyclic oligomers for polyesters (PE) and polyurethanes (PUR). A complete separation for the different structures was achieved for both polymer types with a single solvent system (ACN) and without extensive optimization. Additionally, cyclic species were found to show an inverse elution profile compared to their linear counterparts, suggesting distinct physical properties between species. PMID:26637218

  4. Ion chromatographic separation and determination of phosphate and arsenate in water and hair.

    PubMed

    Antony, P J; Karthikeyan, S; Iyer, C S P

    2002-02-15

    A simple and sensitive method for the sequential determination of phosphate and arsenate was developed based on initial ion chromatographic separation followed by detection as the ion-association complex formed by heteropolymolybdophosphate and arsenate with bismuth. With 200 microl sample injection and separation on a AS4A-SC column using an eluent of 3.5 mM sodium hydrogen carbonate-10.0 mM sodium hydroxide, the detection limits which are calculated as the concentration equivalent to twice the baseline noise, were found to be 0.8 microg/l and 4.2 microg/l for P and As, respectively. Spiked samples were analyzed and recoveries were found to be satisfactory in the range of 95-105% for phosphate and 90-105% for arsenate. Samples of water and hair were analyzed by the proposed method.

  5. Evaluation of the separation performance of polyvinylpyrrolidone as a virtual stationary phase for chromatographic NMR.

    PubMed

    Huang, Shaohua; Wu, Rui; Bai, Zhengwu; Yang, Ying; Li, Suying; Dou, Xiaowei

    2014-09-01

    Polyvinylpyrrolidone (PVP) was used as a virtual stationary phase to separate p-xylene, benzyl alcohol, and p-methylphenol by the chromatographic NMR technique. The effects of concentration and weight-average molecular weight (Mw) of PVP, solvent viscosity, solvent polarity, and sample temperature on the resolution of these components were investigated. It was found that both higher PVP concentration and higher PVP Mw caused the increase of diffusion resolution for the three components. Moreover, the diffusion resolution did not change at viscosity-higher solvents. Moreover, the three components showed different resolution at different solvents. As temperature increased, the diffusion resolution between p-xylene and benzyl alcohol gradually increased, and the one between p-xylene and p-methylphenol slightly increased from 278 to 298 K and then decreased above 298 K. It was also found that the polarity of the analytes played an important role for the separation by affecting the diffusion coefficient.

  6. Chromatographic separation of vanadium, tungsten and molybdenum with a liquid anion-exchanger.

    PubMed

    Fritz, J S; Topping, J J

    1971-09-01

    In acidic solution only molybdenum(VI), tungsten(VI), vanadium(V), niobium(V) and tantalum(V) form stable, anionic complexes with dilute hydrogen peroxide. This fact has been used in developing an analytical method of separating molybdenum(VI), tungsten(VI) and vanadium(V) from other metal ions and from each other. Preliminary investigations using reversed-phase paper chromatography and solvent extraction led to a reversed-phase column Chromatographic separation technique. These metal-peroxy anions are retained by a column containing a liquid anion-exchanger (General Mills Aliquat 336) in a solid support. Then molybdenum(VI), tungsten(VI) and vanadium(V) are selectively eluted with aqueous solutions containing dilute hydrogen peroxide and varying concentrations of sulphuric acid.

  7. Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

    NASA Technical Reports Server (NTRS)

    Huz, Kateryna

    2014-01-01

    RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better

  8. Mars Atmospheric Capture and Gas Separation

    NASA Technical Reports Server (NTRS)

    Muscatello, Anthony; Santiago-Maldonado, Edgardo; Gibson, Tracy; Devor, Robert; Captain, James

    2011-01-01

    The Mars atmospheric capture and gas separation project is selecting, developing, and demonstrating techniques to capture and purify Martian atmospheric gases for their utilization for the production of hydrocarbons, oxygen, and water in ISRU systems. Trace gases will be required to be separated from Martian atmospheric gases to provide pure C02 to processing elements. In addition, other Martian gases, such as nitrogen and argon, occur in concentrations high enough to be useful as buffer gas and should be captured as welL To achieve these goals, highly efficient gas separation processes will be required. These gas separation techniques are also required across various areas within the ISRU project to support various consumable production processes. The development of innovative gas separation techniques will evaluate the current state-of-the-art for the gas separation required, with the objective to demonstrate and develop light-weight, low-power methods for gas separation. Gas separation requirements include, but are not limited to the selective separation of: (1) methane and water from un-reacted carbon oxides (C02- CO) and hydrogen typical of a Sabatier-type process, (2) carbon oxides and water from unreacted hydrogen from a Reverse Water-Gas Shift process, (3) carbon oxides from oxygen from a trash/waste processing reaction, and (4) helium from hydrogen or oxygen from a propellant scavenging process. Potential technologies for the separations include freezers, selective membranes, selective solvents, polymeric sorbents, zeolites, and new technologies. This paper and presentation will summarize the results of an extensive literature review and laboratory evaluations of candidate technologies for the capture and separation of C02 and other relevant gases.

  9. ENVIRONMENTAL TECHNOLOGY VERIFICATION REPORT, EXPLOSIVES DETECTION TECHNOLOGY, SRI INSTRUMENTS, MODEL 8610C, GAS CHROMATOGRAPH/THERMIONIC IONIZATION DETECTION

    EPA Science Inventory

    The SRI Model 86 1 OC gas chromatograph (GC) is a transportable instrument that can provide on-site analysis of soils for explosives. Coupling this transportable gas chromatograph with a thermionic ionization detector (TID) allows for the determination of explosives in soil matri...

  10. Simple gas chromatographic system for analysis of microbial respiratory gases

    NASA Technical Reports Server (NTRS)

    Carle, G. C.

    1972-01-01

    Dual column ambient temperature system, consisting of pair of capillary columns, microbead thermistor detector and micro gas-sampling valve, is used in remote life-detection equipment for space experiments. Performance outweighs advantage gained by utilizing single-column systems to reduce weight, conserve carrier gas and operate at lower power levels.

  11. NEAR-CONTINUOUS MEASUREMENT OF HYDROGEN SULFIDE AND CARBONYL SULFIDE BY AN AUTOMATIC GAS CHROMATOGRAPH

    EPA Science Inventory

    An automatic gas chromatograph with a flame photometric detector that samples and analyzes hydrogen sulfide and carbonyl sulfide at 30-s intervals is described. Temperature programming was used to elute trace amounts of carbon disulfide present in each injection from a Supelpak-S...

  12. 40 CFR 1065.267 - Gas chromatograph with a flame ionization detector.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 33 2014-07-01 2014-07-01 false Gas chromatograph with a flame ionization detector. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon...

  13. 40 CFR 1065.267 - Gas chromatograph with a flame ionization detector.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 34 2013-07-01 2013-07-01 false Gas chromatograph with a flame ionization detector. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon...

  14. 40 CFR 1065.267 - Gas chromatograph with a flame ionization detector.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 34 2012-07-01 2012-07-01 false Gas chromatograph with a flame ionization detector. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon...

  15. Liquid chromatographic method for determination of water in soils and the optimization of anion separations by capillary zone electrophoresis

    SciTech Connect

    Benz, N.

    1994-10-01

    A liquid chromatographic method for the determination of water in soil or clay samples is presented. In a separate study, the optimization of electrophoretic separation of alkylated phenolate ions was optimized by varying the pH and acetonitrile concentration of the buffer solutions.

  16. Performance of the MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission

    NASA Astrophysics Data System (ADS)

    Buch, Arnaud; Pinnick, Veronica; Szopa, Cyril; Grand, Noël; Freissinet, Caroline; Danell, Ryan; van Ameron, Friso; Arevalo, Ricardo; Brinckerhoff, William; Raulin, François; Mahaffy, Paul; Goesmann, Fred

    2015-04-01

    The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquir-ing samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis gas chromatograph (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide in-formation on elemental and molecular makeup, po-larity, chirality and isotopic patterns of analyte spe-cies. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatography-mass spec-trometry (GC-MS) mode of operation. Both instruments have been tested separately first and have been coupled in order to test the efficiency of the future MOMA GC-MS instrument. The main objective of the second step has been to test the quantitative response of both instruments while they are coupled and to characterize the combined instrument detection limit for several compounds. A final experiment has been done in order to test the feasibility of the separation and detection of a mixture contained in a soil sample introduced in the MOMA oven.

  17. Development of and fabrication of high resolution gas chromatographic capillary columns

    NASA Technical Reports Server (NTRS)

    Zlatkis, A.

    1982-01-01

    Gas chromatographic columns which are used in the trace gas analyzer (TGA) for the space shuttle are coated with a polyoxyethylene lauryl ether. This stationary phase is of medium polarity and has a temperature limit of 160 C. A polymer for this application which has an improved thermal stability is investigated. The use of fused silica capillary columns with specially bonded phases as well as an introduction system (on column) was also studied.

  18. Gas separation performance of inorganic polyphosphazene membranes

    SciTech Connect

    Stone, M.L.

    1995-07-01

    The objective of this research program was to develop, characterize, and evaluate the potential of phosphazene polymers for separations performed in harsh environments. The program was divided into two general areas, gas separations and metal ion separations involving aqueous solutions. Each of these two areas is the subject of a topical report; this report deals with the gas separations. Throughout the world, there is rapidly growing interest in membrane separation as an energy efficient way to separate components of a process stream or waste stream, such as in desalination of water or clarification of fruit juices. In some cases membranes perform separations that are otherwise very difficult, such as breaking azeotropes. In the early stages of the work reported here, there was interest in separating acid gases from process flue gases and in natural gas sweetening. As a result, research was undertaken to characterize membrane performance. First, a pure gas test apparatus was developed to determine the permeabilities of a number of gases through various membranes at a variety of temperatures. Second, an automated mixed gas test cell was developed in which membranes could be exposed to mixtures of pairs of gases. Each of these approaches has its advantages and each will be discussed separately.

  19. Derivatization in gas chromatographic determination of phenol and aniline traces in aqueous media

    NASA Astrophysics Data System (ADS)

    Gruzdev, I. V.; Zenkevich, I. G.; Kondratenok, B. M.

    2015-06-01

    Substituted anilines and phenols are the most common hydrophilic organic environmental toxicants. The principles of gas chromatographic determination of trace amounts of these compounds in aqueous media at concentrations <=0.1 μg litre-1 based on synthesis of their derivatives (derivatization) directly in the aqueous phase are considered. Conversion of relatively hydrophilic analytes into more hydrophobic derivatives makes it possible to achieve such low detection limits and optimize the protocols of extractive preconcentration and selective chromatographic detection. Among the known reactions, this condition is best met by electrophilic halogenation of compounds at the aromatic moiety. The bibliography includes 177 references.

  20. Utilization of a diol-stationary phase column in ion chromatographic separation of inorganic anions.

    PubMed

    Arai, Kaori; Mori, Masanobu; Kozaki, Daisuke; Nakatani, Nobutake; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2012-12-28

    We describe the ion chromatographic separation of inorganic anions using a diol-stationary phase column (-CH(OH)CH(2)OH; diol-column) without charged functional groups. Anions were separated using acidic eluent as in typical anion-exchange chromatography. The retention volumes of anions on the diol-column increased with increasing H(+) concentration in the eluent. The anion-exchange capacities of diol-columns in the acidic eluent (pH 2.8) were larger than that of zwitterionic stationary phase column but smaller than that of an anion-exchange column. The separation of anions using the diol-column was strongly affected by the interaction of H(+) ions with the diol-functional groups and by the types of the eluents. In particular, the selection of the eluent was very important for controlling the retention time and resolution. Good separation was obtained using a diol-column (HILIC-10) with 5 mM phthalic acid as eluent. The limits of detection at a signal-to-noise ratio of 3 ranged from 1.2 to 2.7 μM with relative standard deviations (RSD, n=5) of 0.04-0.07% for the retention time and 0.4-2.0% for the peak areas. This method was successfully applied to the determination of H(2)PO(4)(-), Cl(-), and NO(3)(-) in a liquid fertilizer sample.

  1. Thin-layer chromatographic (TLC) separations and bioassays of plant extracts to identify antimicrobial compounds.

    PubMed

    Kagan, Isabelle A; Flythe, Michael D

    2014-03-27

    A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungi or bacteria in broth or agar), allowing time for the microbes to grow in a humid environment, and visualizing zones with no microbial growth. The effectiveness of this screening method, known as bioautography, depends on both the quality of the chromatographic separation and the care taken with microbial culture conditions. This paper describes standard protocols for TLC and contact bioautography with a novel application to amino acid-fermenting bacteria. The extract is separated on flexible (aluminum-backed) silica TLC plates, and bands are visualized under ultraviolet (UV) light. Zones are cut out and incubated face down onto agar inoculated with the test microorganism. Inhibitory bands are visualized by staining the agar plates with tetrazolium red. The method is applied to the separation of red clover (Trifolium pratense cv. Kenland) phenolic compounds and their screening for activity against Clostridium sticklandii, a hyper ammonia-producing bacterium (HAB) that is native to the bovine rumen. The TLC methods apply to many types of plant extracts and other bacterial species (aerobic or anaerobic), as well as fungi, can be used as test organisms if culture conditions are modified to fit the growth requirements of the species.

  2. Kinetics and equilibria of the chromatographic separation of maltose and trehalose.

    PubMed

    He, Dengjun; Zhou, Jiachun; Xia, Quanming; Jiang, Lihua; Qiu, Yongjun; Zhao, Liming

    2015-07-01

    Trehalose, a nonreducing disaccharide, has been extensively applied to food, cosmetics, and pharmaceutical goods. The resultant solution of trehalose prepared by enzymatic methods includes high amounts of maltose. However, it is quite difficult to separate maltose and trehalose on an industrial scale because of their similar properties. In this paper, a high-performance resin was selected as a stationary phase to separate trehalose and maltose, and the resolution of these sugars was 0.59. The potential of a cation exchange resin was investigated as the stationary phase in separating trehalose and maltose using deionized water as the mobile phase. Based on the equilibrium dispersive model, the axial dispersion coefficients and overall mass transfer coefficients of maltose and trehalose were determined by moment analysis at two different temperatures, 50 and 70°C. Other parameters, including the column void and the adsorption isotherms, were also determined and applied to simulate the elution curves of trehalose and maltose. The simulated results matched the experimental data, validating the parameters. The optimized parameters are critical to the chromatographic separation of trehalose and maltose on an industrial scale.

  3. Separative analyses of a chromatographic column packed with a core-shell adsorbent for lithium isotope separation

    SciTech Connect

    Sugiyama, T.; Sugura, K.; Enokida, Y.; Yamamoto, I.

    2015-03-15

    Lithium-6 is used as a blanket material for sufficient tritium production in DT fueled fusion reactors. A core-shell type adsorbent was proposed for lithium isotope separation by chromatography. The mass transfer model in a chromatographic column consisted of 4 steps, such as convection and dispersion in the column, transfer through liquid films, intra-particle diffusion and and adsorption or desorption at the local adsorption sites. A model was developed and concentration profiles and time variation in the column were numerically simulated. It became clear that core-shell type adsorbents with thin porous shell were saturated rapidly relatively to fully porous one and established a sharp edge of adsorption band. This is very important feature because lithium isotope separation requires long-distance development of adsorption band. The values of HETP (Height Equivalent of a Theoretical Plate) for core-shell adsorbent packed column were estimated by statistical moments of the step response curve. The value of HETP decreased with the thickness of the porous shell. A core-shell type adsorbent is, then, useful for lithium isotope separation. (authors)

  4. Evolutionary multi-objective optimization based comparison of multi-column chromatographic separation processes for a ternary separation.

    PubMed

    Heinonen, Jari; Kukkonen, Saku; Sainio, Tuomo

    2014-09-05

    Performance characteristics of two advanced multi-column chromatographic separation processes with discontinuous feed, Multi-Column Recycling Chromatogrphy (MCRC) and Japan Organo (JO), were investigated for a ternary separation using multi-objective optimization with an evolutionary algorithm. Conventional batch process was used as a reference. Fractionation of a concentrated acid hydrolysate of wood biomass into sulfuric acid, monosaccharide, and acetic acid fractions was used as a model system. Comparison of the separation processes was based on selected performance parameters in their optimized states. Flow rates and step durations were taken as decision variables whereas the column configuration and dimensions were fixed. The MCRC process was found to be considerably more efficient than the other processes with respect to eluent consumption. The batch process gave the highest productivity and the JO process the lowest. Both of the multi-column processes gave significantly higher monosaccharide yield than the batch process. When eluent consumption and monosaccharide yield are taken into account together with productivity, the MCRC process was found to be the most efficient in the studied case.

  5. Indirect gas chromatographic measurement of water for process streams

    SciTech Connect

    Barbour, F.A.

    1993-05-01

    This project was conducted to develop a moisture measurement method for process gas streams of fossil fuels. Objective was to from pyrolysis to measure the molar concentration of water in a gas stream without flow measurements. The method developed has been incorporated into the hydrocarbon gas analysis method currently used at Western Research Institute. A literature search of types of direct measuring moisture sensors was conducted, and a list of sensors available is given; most of them could not survive in the environment of the process streams. Indirect methods of measuring water involve changing the water via reaction to a compound that can be more readily measured. These methods react water with various reagents to form hydrogen, acetylene, and acetone. The method chose for this study uses a calcium carbide reaction column to convert the water present in the gas stream to acetylene for analysis. Relative deviation for the daily determination of water varied from 0.5 to 3.4%. The method chosen was tested for linearity over a wide range of gas stream water content. Response over 2 to 15 mole % water appears to be linear with a correlation coefficient of 0.991.

  6. Radioactive-gas separation technique

    NASA Technical Reports Server (NTRS)

    Haney, R.; King, K. J.; Nellis, D. O.; Nisson, R. S.; Robling, P.; Womack, W.

    1977-01-01

    Cryogenic technique recovers gases inexpensively. Method uses differences in vapor pressures, melting points, and boiling points of components in gaseous mixture. Series of temperature and pressure variations converts gases independently to solid and liquid states, thereby simplifying separation. Apparatus uses readily available cryogen and does not require expensive refrigeration equipment.

  7. Modified gas chromatographic/mass spectrometric method for determination of daminozide in high protein food products.

    PubMed

    Faughnan, K T; Woodruff, M A

    1991-01-01

    A modified version of the Conditt and Baumgardner gas chromatographic/mass spectroscopic (GC/MS) method for determination of daminozide in peanut butter and raw peanuts is described. Daminozide in the food product is hydrolyzed to unsymmetrical dimethylhydrazine (UDMH) by sodium hydroxide digestion. The generated UDMH is distilled from the food matrix and captured by reaction with salicylaldehyde in a condensation trap. Resulting high pH distillates generated by peanuts and peanut products are adjusted back to a pH of 5-6 through addition of glacial acetic acid. After thermal incubation and extraction into methylene chloride, salicylaldehyde dimethylhydrazone is separated from interferences by capillary GC and quantitated by MS using the selective ion monitoring (SIM) mode. Quantitation of daminozide is based on the ratio of the salicylaldehyde dimethylhydrazone molecular ion (m/z 164) to the molecular ion (m/z 153) of the internal standard, 4-nitroanisole. Confirmation of daminozide identity is determined by relative intensity of the m/z 164 ion to the m/z 120 (C7H4ON) ion. Improved m/z 164 ion intensity and reduction of neighboring interferences due to acetic acid treatment permitted a daminozide detection limit of 0.005 ppm in a 50 g sample and an associated 0.02 ppm limit of quantitation. This modification is specific for high protein samples that generate high pH distillates such as peanuts and peanut products and is not specifically intended for analysis of low protein samples.

  8. Gas chromatographic/mass spectrometric determination of daminozide in high protein food products.

    PubMed

    Conditt, M K; Baumgardner, J R; Hellmann, L M

    1988-01-01

    A gas chromatographic/mass spectrometric (GC/MS) method for determining daminozide in high protein products has been developed. Daminozide is hydrolyzed in the presence of a strong base to form unsymmetrical dimethylhydrazine (UDMH) which is then distilled from the food matrix. A stable derivative is formed by reacting UDMH with salicyladehyde to form salicyaldehyde dimethylhydrazone. This derivative is separated and quantitated by GC/MS using selected ion monitoring (SIM) of key ions in the fragmentation pattern: m/z 164 (molecular ion of hydrazone) and m/z 120 (C7H6ON). An internal standard, 4-nitroanisole, is monitored at m/z 153 (molecular ion) and m/z 123 (C6H5O2N). The limit of detection is 0.01 ppm daminozide in a 50 g sample; however, because of variation at low levels, the limit of quantitation is 0.1 ppm. Recoveries are 90% or greater from peanuts and peanut butter spiked at the 0.1-2 ppm level. Reproducibility of the method depends on the food matrix and is 26% RSD in the worst case. Data are compared for the GC/MS method and the official EPA colorimetric procedure. Results showed a high bias in the colorimetric method, especially when roasted peanut products were analyzed.

  9. Purge and trap with monolithic sorbent for gas chromatographic analysis of pesticides in honey.

    PubMed

    Chienthavorn, Orapin; Dararuang, Kanittha; Sasook, Anupop; Ramnut, Narumol

    2012-01-01

    Polydivinylbenzene (P-DVB) and silica monolithic materials were synthesised in capillaries and then used to adsorb nine organonitrogen pesticides extracted from honey. After adsorption, each monolith-capillary was connected to a gas chromatograph (GC) with nitrogen-phosphorous detector (NPD). The silica monolith gave better peak shape and intensity than the P-DVB monolith. Formulation of silica monolith with tetramethoxysilane (TMOS) as a sole initiator provided better separation and higher peak intensity, compared to those with methyltrimethoxysilane (MTMS) and (3:1) TMOS/MTMS initiators. The optimum internal diameter and length of silica monolith-capillary were 0.25 mm and 5 cm, respectively. The purge and trap conditions were optimised by purging with nitrogen and heating the honey sample solution at 100 °C for 60 min. Recovery of the method was in a range of 84.95-99.71% and the detection limits of the pesticides determined by using GC-NPD and GC-mass spectrometric detector (MSD) ranged between 0.36-1.75 and 0.13-0.25 ng g(-1), respectively.

  10. Chromatographic cation exchange separation of decigram quantities of californium and other transplutonium elements

    SciTech Connect

    Benker, D.E.; Chattin, F.R.; Collins, E.D.; Knauer, J.B.; Orr, P.B.; Ross, R.G.; Wiggins, J.T.

    1981-01-01

    Decigram quantities of highly radioactive transplutonium elements are routinely partitioned at TRU by chromatographic elution from cation resin using AHIB eluents. Batch runs containing up to 200 mg of /sup 252/Cf can be made in about 5 h (2 h to load the feed and 3 h for the elution), with two high-pressure ion exchange columns, a small one for the initial loading of the feed and a large one for the elution. The separations achieved in the column are preserved by routing the column effluent through an alpha detector and using the response from the detector to select appropriate product fractions. The high-pressure ion exchange process has been reliable and relatively easy to operate; therefore it will continue to be used for partitioning transplutonium elements at TRU. 3 figures, 1 table.

  11. 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.

  12. 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.

  13. Simulation of Ultrasonic-driven Gas Separations

    SciTech Connect

    Rector, David R.; Greenwood, Margaret S.; Ahmed, Salahuddin; Doctor, Steven R.; Posakony, Gerald J.; Stenkamp, Victoria S.

    2007-06-01

    The separation of components in a gas mixture is important for a wide range of applications. One method for achieving this separation is by passing a traveling acoustic wave through the gas mixture, which creates a flux of the lighter components away from the transducer. A series of simulation were performed to assess the effectiveness of this method for separating a binary mixture of argon and helium using the lattice kinetics method. The energy transport equation was modified to account for adiabatic expansion and compression. The species transport equation was modified to include a barodiffusion term. Simulations were performed on two different scales; detailed acoustic wave simulations to determine the net component flux as a function of local concentration, pressure, etc., and device scale simulations to predict the gas composition as a function of time inside a gas separation cylinder. The method is first validated using data from literature and then applied to mixtures of argon and helium. Results are presented and discussed.

  14. Method for improved gas-solids separation

    DOEpatents

    Kusik, Charles L.; He, Bo X.

    1990-01-01

    Methods are disclosed for the removal of particulate solids from a gas stream at high separation efficiency, including the removal of submicron size particles. The apparatus includes a cyclone separator type of device which contains an axially mounted perforated cylindrical hollow rotor. The rotor is rotated at high velocity in the same direction as the flow of an input particle-laden gas stream to thereby cause enhanced separation of particulate matter from the gas stream in the cylindrical annular space between the rotor and the sidewall of the cyclone vessel. Substantially particle-free gas passes through the perforated surface of the spinning rotor and into the hollow rotor, from when it is discharged out of the top of the apparatus. Separated particulates are removed from the bottom of the vessel.

  15. Method for improved gas-solids separation

    DOEpatents

    Kusik, C.L.; He, B.X.

    1990-11-13

    Methods are disclosed for the removal of particulate solids from a gas stream at high separation efficiency, including the removal of submicron size particles. The apparatus includes a cyclone separator type of device which contains an axially mounted perforated cylindrical hollow rotor. The rotor is rotated at high velocity in the same direction as the flow of an input particle-laden gas stream to thereby cause enhanced separation of particulate matter from the gas stream in the cylindrical annular space between the rotor and the sidewall of the cyclone vessel. Substantially particle-free gas passes through the perforated surface of the spinning rotor and into the hollow rotor, from where it is discharged out of the top of the apparatus. Separated particulates are removed from the bottom of the vessel. 4 figs.

  16. The Construction of a Simple Pyrolysis Gas Chromatograph.

    ERIC Educational Resources Information Center

    Hedrick, Jack L.

    1982-01-01

    Describes a simple and inexpensive pyrolysis gas chromatography (PGC) system constructed from items available in undergraduate institutions. The system is limited, accepting only liquid samples and pyrolyzing "on the fly" rather than statically and not allowing for reductive pyrolysis. Applications, experiments, and typical results are included.…

  17. Development of gas chromatographic system for dissolved organic carbon analysis in seawater

    SciTech Connect

    Chipman, D.W.; Takahashi, T.

    1992-12-01

    During the first six months of this two-year grant, we have completed the construction of the analytical portion of a prototype gas chromatograph-based system for the analysis of dissolved organic carbon in seawater. We also have begun testing the procedures to be used to cryogenically concentrate and transfer carbon dioxide from the oxidizing atmosphere of the high-temperature furnace into the reducing hydrogen carrier gas of the gas chromatograph. During the second half of the first year, we will construct the high-temperature catalytic oxidation furnace and test the entire system on laboratory-prepared aqueous solutions of various organic compounds. Also during this period, we will take part in an initial scoping study within the Cape Hatteras field area on board the R/V Gyre. This study will involve both the collection of samples of seawater for organic and inorganic carbon analysis and the measurement of surface-water pCO[sub 2].

  18. Development of gas chromatographic system for dissolved organic carbon analysis in seawater. Annual progress report

    SciTech Connect

    Chipman, D.W.; Takahashi, T.

    1992-12-01

    During the first six months of this two-year grant, we have completed the construction of the analytical portion of a prototype gas chromatograph-based system for the analysis of dissolved organic carbon in seawater. We also have begun testing the procedures to be used to cryogenically concentrate and transfer carbon dioxide from the oxidizing atmosphere of the high-temperature furnace into the reducing hydrogen carrier gas of the gas chromatograph. During the second half of the first year, we will construct the high-temperature catalytic oxidation furnace and test the entire system on laboratory-prepared aqueous solutions of various organic compounds. Also during this period, we will take part in an initial scoping study within the Cape Hatteras field area on board the R/V Gyre. This study will involve both the collection of samples of seawater for organic and inorganic carbon analysis and the measurement of surface-water pCO{sub 2}.

  19. Estimation of the vapor pressure of petroleum distillate fractions from gas chromatographic data

    SciTech Connect

    Eggertsen, F.T.; Nygard, N.R.; Nickoley, L.D.

    1980-11-01

    The vapor pressure of petroleum distillate fractions is estimated conveniently by applying ideal gas and solution laws to gas chromatographic data. The vapor pressure is computed as a summation of the partial pressures for carbon number groups in the chromatogram, each partial pressure being derived as the product of mole fraction, determined from the chromatogram, and saturation pressure, calculated using the Antoine equation. A rapid method of computation with a programmable calculator was used. The method assumes approximate conformance to Raoult's and Dalton's laws relating to partial pressures from a solution. The results generally agree well with values obtained manometrically. Advantages of the method are the general availability of suitable gas chromatographic equipment, convenience and speed of the procedure and calculations, applicability over a wide range of volatility, freedom from temperature equilibration problems, and small sample requirement. 4 figures, 6 tables.

  20. Effect of Coriolis force on counter-current chromatographic separation by centrifugal partition chromatography.

    PubMed

    Ikehata, Jun-Ichi; Shinomiya, Kazufusa; Kobayashi, Koji; Ohshima, Hisashi; Kitanaka, Susumu; Ito, Yoichiro

    2004-02-06

    The effect of Coriolis force on the counter-current chromatographic separation was studied using centrifugal partition chromatography (CPC) with four different two-phase solvent systems including n-hexane-acetonitrile (ACN); tert-butyl methyl ether (MtBE)-aqueous 0.1% trifluoroacetic acid (TFA) (1:1); MtBE-ACN-aqueous 0.1% TFA (2:2:3); and 12.5% (w/w) polyethylene glycol (PEG) 1000-12.5% (w/w) dibasic potassium phosphate. Each separation was performed by eluting either the upper phase in the ascending mode or the lower phase in the descending mode, each in clockwise (CW) and counterclockwise column rotation. Better partition efficiencies were attained by the CW rotation in both mobile phases in all the two-phase solvent systems examined. The mathematical analysis also revealed the Coriolis force works favorably under the CW column rotation for both mobile phases. The overall results demonstrated that the Coriolis force produces substantial effects on CPC separation in both organic-aqueous and aqueous-aqueous two-phase systems.

  1. Miniature radio-frequency mobility analyzer as a gas chromatographic detector for oxygen-containing volatile organic compounds, pheromones and other insect attractants.

    PubMed

    Eiceman, G A; Tadjikov, B; Krylov, E; Nazarov, E G; Miller, R A; Westbrook, J; Funk, P

    2001-05-11

    A high electric field, radio-frequency ion mobility spectrometry (RF-IMS) analyzer was used as a small detector in gas chromatographic separations of mixtures of volatile organic compounds including alcohols, aldehydes, esters, ethers, pheromones, and other chemical attractants for insects. The detector was equipped with a 2 mCi 63Ni ion source and the drift region for ion characterization was 5 mm wide, 15 mm long and 0.5 mm high. The rate of scanning for the compensation voltages was 60 V s(-1) and permitted four to six scans to be obtained across a capillary chromatographic elution profile for each component. The RF-IMS scans were characteristic of a compound and provided a second dimension of chemical identity to chromatographic retention adding specificity in instances of co-elution. Limits of detection were 1.6-55 x 10(-11) g with an average detection limit for all chemicals of 9.4 x 10(-11) g. Response to mass was linear from 2-50 x 10(-10) g with an average sensitivity of 4 pA ng(-1). Separations of pheromones and chemical attractants for insects illustrated the distinct patterns obtained from gas chromatography with RF-IMS scans in real time and suggest an analytical utility of the RF-IMS as a small, advanced detector for on-site gas chromatographs.

  2. HAPSITE(Trademark) Gas Chromatograph/Mass Spectrometer Variability Assessment

    DTIC Science & Technology

    2005-07-27

    in an uncharacterized chemical environment that involves chemical warfare agents (CWA) or toxic industrial chemicals ( TIC ). Gas Chromatography/Mass...Research Institute (MRI) in Kansas City, Missouri conducted a study to optimize the use of a tri-bed concentrator with TIC . The tni-bed concentrator...The remaining 81 TIC were added based on a Navy threat assessment of chemicals that could be used in a terrorist attack or potentially hazardous

  3. An automated multidimensional preparative gas chromatographic system for isolation and enrichment of trace amounts of xenon from ambient air.

    PubMed

    Larson, Tuula; Östman, Conny; Colmsjö, Anders

    2011-04-01

    The monitoring of radioactive xenon isotopes is one of the principal methods for the detection of nuclear explosions in order to identify clandestine nuclear testing. In this work, a miniaturized, multiple-oven, six-column, preparative gas chromatograph was constructed in order to isolate trace quantities of radioactive xenon isotopes from ambient air, utilizing nitrogen as the carrier gas. The multidimensional chromatograph comprised preparative stainless steel columns packed with molecular sieves, activated carbon, and synthetic carbon adsorbents (e.g., Anasorb®-747 and Carbosphere®). A combination of purification techniques--ambient adsorption, thermal desorption, back-flushing, thermal focusing, and heart cutting--was selectively optimized to produce a well-defined xenon peak that facilitated reproducible heart cutting and accurate quantification. The chromatographic purification of a sample requires approximately 4 h and provides complete separation of xenon from potentially interfering components (such as water vapor, methane, carbon dioxide, and radon) with recovery and accuracy close to 100%. The preparative enrichment process isolates and concentrates a highly purified xenon gas fraction that is suitable for subsequent ultra-low-level γ-, ß/γ-spectroscopic or high-resolution mass spectrometric measurement (e.g., to monitor the gaseous fission products of nuclear explosions at remote locations). The Xenon Processing Unit is a free-standing, relatively lightweight, and transportable system that can be interfaced to a variety of sampling and detection systems. It has a relatively inexpensive, rugged, and compact modular (19-inch rack) design that provides easy access to all parts for maintenance and has a low power requirement.

  4. [Optimization of two-dimensional high performance liquid chromatographic columns for highly efficient separation of intact proteins].

    PubMed

    Hong, Guangfeng; Gao, Mingxia; Yan, Guoquan; Guan, Xia; Tao, Qian; Zhang, Xiangmin

    2010-02-01

    In order to optimize two-dimensional liquid chromatographic (2D-LC) columns for highly efficient separation of proteins, several liquid chromatographic columns were investigated and evaluated. Weak anion-exchange (WAX) column was chosen as the first dimension because of its extensive protein separation power. By comparison of different WAX chromatographic columns for human liver protein separation, TSKgel DEAE-5PW column was selected as the first dimension of a 2D-LC system. For the second dimension, ten typical reversed-phase (RP) LC columns (250 mm x 4.6 mm, 5 microm, 30 nm) were investigated and evaluated. Their silica based RP stationary phases were butyl (C4), octyl (C8) or octadecyl (C18). To evaluate the retention behavior and non-specific protein adsorption ability of these ten columns, four neutral compounds (uracil, nitrobenzene, naphthalene and fluorene) and three standard proteins (cytochrome C, myoglobin and albumin from chicken egg white) were adopted and separated by RPLC. Meantime, WAX fractions were used to investigate the separation ability of different alkyl-bonded silica stationary phase columns for complex protein samples. By comparison of column separation efficiency, adsorption of intact proteins and sample analysis, Jupiter 300 C4 column was finally employed for its excellent separation ability. Optimization of WAX and RPLC columns offers reliable foundation for the construction of 2D-LC protein separation systems.

  5. Gas Chromatographic Analysis of Acidic Indole Auxins in Nicotiana1

    PubMed Central

    Bayer, Margret H.

    1969-01-01

    Acidic indole auxins have been extracted from N. glauca, N. langsdorffii and their 2 tumor-prone 4n- and 2n-hybrids. After purification of the extracts and thin-layer chromatography, acidic indoles were subjected to esterification and gas chromatography. The esters of 4 indole acids were detected and determined: indole-3-acetic acid, indole-3-carboxylic acid, indole-3-propionic acid and indole-3-butyric acid. The indolic nature of fractionated samples was confirmed by spectrophotofluorometry and the physiological significance of the indole esters proven in a biotest. A substantial increase in extractable indole-3-butyric acid in the tumor-prone hybrids suggests an additional pathway of auxin synthesis in these tissues. PMID:5774173

  6. A novel and effective chromatographic approach to the separation of isoflavone derivatives from Pueraria lobata.

    PubMed

    Fu, Jiang; Jing, Wenguang; Wang, Weihao; Chen, Sha; Zhang, Jun; Liu, An

    2015-03-05

    A novel and effective chromatographic approach to the separation and purification of isoflavone compounds from Pueraria lobata is described. The method is based on flash chromatography (FC), coupled to preparative high performance liquid chromatography (prep-HPLC) via a six-way valve. The FC step comprised tandem reversed phase columns, pre-packed with MCI gel (Mitsubishi Chemical Corp., Tokyo, Japan) and C18 (Fuji Silysia Chemical Ltd, Osaka, Japan) resin, respectively, and was designed to separate a crude Pueraria lobata extract into several preliminary fractions. Fractions containing the target compounds were then directly injected via the six-way valve into prep-HPLC columns, without further treatment, for final isolation and purification. Nine isoflavonoids were successfully isolated, three through an online mode and the other six through an offline mode. The purities of all compounds exceeded 95.0%, as determined by HPLC with an UV-vis photodiode array detector. The convenience, low solvent consumption, and time-saving advantages of this method offer an attractive and promising approach to the isolation of natural products.

  7. Gas chromatographic analysis of polyhydroxybutyrate in activated sludge: a round-robin test.

    PubMed

    Baetens, D; Aurola, A M; Foglia, A; Dionisi, D; van Loosdrecht, M C M

    2002-01-01

    Polyhydroxyalkanoates (PHA) and poly-beta-hydroxybutyrate (PHB) in particular have become compounds which is routinely investigated in wastewater research. The PHB analysis method has only recently been applied to activated sludge samples where PHA contents might be relatively low. This urges the need to investigate the reproducibility of the gas chromatographic method for PHB analysis. This was evaluated in a round-robin test in 5 European laboratories with samples from lab-scale and full-scale enhanced biological phosphorus removal systems. It was shown that the standard deviation of measurements in each lab and the reproducibility between the labs was very good. Experimental results obtained by different laboratories using this analysis method can be compared. Sludge samples with PHB contents varying between 0.3 and 22.5 mg PHB/mg sludge were analysed. The gas chromatographic method allows for PHV, PH2MB and PH2MV analysis as well.

  8. Facile room-temperature solution-phase synthesis of a spherical covalent organic framework for high-resolution chromatographic separation.

    PubMed

    Yang, Cheng-Xiong; Liu, Chang; Cao, Yi-Meng; Yan, Xiu-Ping

    2015-08-07

    A simple and facile room-temperature solution-phase synthesis was developed to fabricate a spherical covalent organic framework with large surface area, good solvent stability and high thermostability for high-resolution chromatographic separation of diverse important industrial analytes including alkanes, cyclohexane and benzene, α-pinene and β-pinene, and alcohols with high column efficiency and good precision.

  9. Portable gas chromatograph mass spectrometer for on-site chemical analyses

    DOEpatents

    Haas, Jeffrey S.; Bushman, John F.; Howard, Douglas E.; Wong, James L.; Eckels, Joel D.

    2002-01-01

    A portable, lightweight (approximately 25 kg) gas chromatograph mass spectrometer, including the entire vacuum system, can perform qualitative and quantitative analyses of all sample types in the field. The GC/MS has a conveniently configured layout of components for ease of serviceability and maintenance. The GC/MS system can be transported under operating or near-operating conditions (i.e., under vacuum and at elevated temperature) to reduce the downtime before samples can be analyzed on-site.

  10. Gas chromatographic determination of pesticide residues in white mustard.

    PubMed

    Słowik-Borowiec, Magdalena; Szpyrka, Ewa; Walorczyk, Stanisław

    2015-04-15

    A new analytical method employing gas chromatography coupled to electron capture and nitrogen phosphorus detection (GC-ECD/NPD) has been developed and validated for the screening and quantification of 51 pesticides in a matrix of high chlorophyll content - white mustard (Sinapis alba L.). For preparation of the sample extract, the citrate buffered QuEChERS procedure was followed. However certain changes were made to adapt the method to our needs and available laboratory resources. The sample size was reduced to 5 g, 10 mL water was added and exchange of solvent before GC analysis was done. The samples spiked with the target pesticides at the concentration level 0.01 mg/kg and a higher level (depending on the compound) yielded average recoveries in the range of 70-120% with relative standard deviations (RSDs) 0-19% except for HCB, S-metolachlor and teflubenzuron, and displayed very good linearity (R(2)>0.99) for nearly all the analytes. Limit of quantification was 0.01 mg/kg for the majority of the analytes. The expanded measurement uncertainties were estimated employing a "top-down" empirical model as being between 6% and 32% and yielding an average value of 18% (coverage factor k=2, confidence level 95%).

  11. Gas Strut Separation Alternative for Ares I

    NASA Technical Reports Server (NTRS)

    Floyd, Brian; Owens, James

    2008-01-01

    This paper presents a design alternative and the rationale for a stage separation system based on Metering Adiabatic Gas Struts (MAG Struts) for the Ares 1 launch vehicle. The MAG Strut separation system was proposed as an alternative to the current Ares 1 separation system, which relies on small solid rocket motors to provide the main separation force. This paper will describe technical issues that were addressed during the trade study and present a conceptual design of the strut system that best resolved the issues. Needed development testing and programmatic considerations will be addressed as part of the paper.

  12. Gas chromatographic determination of triclopyr in fruits and vegetables.

    PubMed

    Ting, K C; Lee, C S

    1995-01-20

    This research was comprised of two parts: quantitative analyses, and confirmatory test. In the quantitative analyses, five classes of fruits and vegetables comprising 10 individual commodities were fortified with triclopyr herbicide at 0.4 and 0.8 ppm level. Triclopyr was extracted from the matrices and derivatized separately to 2-chloroethylene ester with 2-chloroethanol-BCl3 and methyl ester with diazomethane. The esters were then quantitated by GC-ECD and GC-NPD. The GC-ECD recoveries for 2-chloroethylene ester were 100.0% and 100.7% at 0.4 ppm and 0.8 ppm fortification levels, respectively, whereas methyl ester recovery was 103.9% at 0.4 ppm fortification level. Similarly, the GC-NPD recoveries for 2-chloroethylene ester were 99.0% and 97.9% at 0.4 ppm and 0.8 ppm fortification levels respectively, whereas methyl ester recovery was 102.0% at 0.4 ppm fortification level. In the confirmatory test, the 2-chloroethylene ester was introduced into a GC-ion trap. The EI mass spectrum was then interpreted based on the criteria of molecular ion, isotopes, base ion, characteristic ions and the nitrogen rule. Compared to existing methods, this method has reduced partition solvents to nearly one-tenth. In addition, this method proved to be simple, fast, safe and accurate.

  13. Comparison of gas chromatographic hyphenated techniques for mercury speciation analysis.

    PubMed

    Nevado, J J Berzas; Martín-Doimeadios, R C Rodríguez; Krupp, E M; Bernardo, F J Guzmán; Fariñas, N Rodríguez; Moreno, M Jiménez; Wallace, D; Ropero, M J Patiño

    2011-07-15

    In this study, we evaluate advantages and disadvantages of three hyphenated techniques for mercury speciation analysis in different sample matrices using gas chromatography (GC) with mass spectrometry (GC-MS), inductively coupled plasma mass spectrometry (GC-ICP-MS) and pyrolysis atomic fluorescence (GC-pyro-AFS) detection. Aqueous ethylation with NaBEt(4) was required in all cases. All systems were validated with respect to precision, with repeatability and reproducibility <5% RSD, confirmed by the Snedecor F-test. All methods proved to be robust according to a Plackett-Burnham design for 7 factors and 15 experiments, and calculations were carried out using the procedures described by Youden and Steiner. In order to evaluate accuracy, certified reference materials (DORM-2 and DOLT-3) were analyzed after closed-vessel microwave extraction with tetramethylammonium hydroxide (TMAH). No statistically significant differences were found to the certified values (p=0.05). The suitability for water samples analysis with different organic matter and chloride contents was evaluated by recovery experiments in synthetic spiked waters. Absolute detection and quantification limits were in the range of 2-6 pg for GC-pyro-AFS, 1-4 pg for GC-MS, with 0.05-0.21 pg for GC-ICP-MS showing the best limits of detection for the three systems employed. However, all systems are sufficiently sensitive for mercury speciation in environmental samples, with GC-MS and GC-ICP-MS offering isotope analysis capabilities for the use of species-specific isotope dilution analysis, and GC-pyro-AFS being the most cost effective alternative.

  14. Separation of gas mixtures by supported complexes

    SciTech Connect

    Nelson, D.A.; Lilga, M.A.; Hallen, R.T.; Lyke, S.E.

    1986-08-01

    The goal of this program is to determine the feasibility of solvent-dissolved coordination complexes for the separation of gas mixtures under bench-scale conditions. In particular, mixtures such as low-Btu gas are examined for CO and H/sub 2/ separation. Two complexes, Pd/sub 2/(dpm)/sub 2/Br/sub 2/ and Ru(CO)/sub 2/(PPh/sub 3/)/sub 3/, were examined in a bench-scale apparatus for the separation of binary (CO-N/sub 2/ or H/sub 2/-N/sub 2/) and quinary (H/sub 2/, CO, CO/sub 2/, CH/sub 4/, and N/sub 2/) mixtures. The separation of CO-N/sub 2/ was enhanced by the presence of the palladium complex in the 1,1,2-trichloroethane (TCE) solvent, especially at high gas and low liquid rates. The five-component gas mixture separation with the palladium complex in TCE provided quite unexpected results based on physical solubility and chemical coordination. The complex retained CO, while the solvent retained CO/sub 2/, CH/sub 4/, and N/sub 2/ to varying degrees. This allowed the hydrogen content to be enhanced due to its low solubility in TCE and inertness to the complex. Thus, a one-step, hydrogen separation can be achieved from gas mixtures with compositions similar to that of oxygen-blown coal gas. A preliminary economic evaluation of hydrogen separation was made for a system based on the palladium complex. The palladium system has a separation cost of 50 to 60 cents/MSCF with an assumed capital investment of $1.60/MSCF of annual capacity charged at 30% per year. This assumes a 3 to 4 year life for the complex. Starting with a 90% hydrogen feed, PSA separation costs are in the range of 30 to 50 cents/MSCF. The ruthenium complex was not as successful for hydrogen or carbon monoxide separation due to unfavorable kinetics. The palladium complex was found to strip hydrogen gas from H/sub 2/S. The complex could be regenerated with mild oxidants which removed the sulfur as SO/sub 2/. 24 refs., 26 figs., 10 tabs.

  15. Development of High Precision Metal Micro-Electro-Mechanical-Systems Column for Portable Surface Acoustic Wave Gas Chromatograph

    NASA Astrophysics Data System (ADS)

    Iwaya, Takamitsu; Akao, Shingo; Sakamoto, Toshihiro; Tsuji, Toshihiro; Nakaso, Noritaka; Yamanaka, Kazushi

    2012-07-01

    In the field of environmental measurement and security, a portable gas chromatograph (GC) is required for the on-site analysis of multiple hazardous gases. Although the gas separation column has been downsized using micro-electro-mechanical-systems (MEMS) technology, an MEMS column made of silicon and glass still does not have sufficient robustness and a sufficiently low fabrication cost for a portable GC. In this study, we fabricated a robust and inexpensive high-precision metal MEMS column by combining diffusion-bonded etched stainless-steel plates with alignment evaluation using acoustic microscopy. The separation performance was evaluated using a desktop GC with a flame ionization detector and we achieved the high separation performance comparable to the best silicon MEMS column fabricated using a dynamic coating method. As an application, we fabricated a palm-size surface acoustic wave (SAW) GC combining this column with a ball SAW sensor and succeeded in separating and detecting a mixture of volatile organic compounds.

  16. Ion Exchange and Thin Layer Chromatographic Separation and Identification of Amino Acids in a Mixture: An Experiment for General Chemistry and Biotechnology Laboratories

    ERIC Educational Resources Information Center

    Brunauer, Linda S.; Caslavka, Katelyn E.; Van Groningen, Karinne

    2014-01-01

    A multiday laboratory exercise is described that is suitable for first-year undergraduate chemistry, biochemistry, or biotechnology students. Students gain experience in performing chromatographic separations of biomolecules, in both a column and thin layer chromatography (TLC) format. Students chromatographically separate amino acids (AA) in an…

  17. UPGRADING NATURAL GAS VIA MEMBRANE SEPARATION PROCESSES

    SciTech Connect

    S.A.Stern; P.A. Rice; J. Hao

    2000-03-01

    The objective of the present study is to assess the potential usefulness of membrane separation processes for removing CO{sub 2} and H{sub 2}S from low-quality natural gas containing substantial amounts of both these ''acid'' gases, e.g., up to 40 mole-% CO{sub 2} and 10 mole-% H{sub 2}S. The membrane processes must be capable of upgrading the crude natural gas to pipeline specifications ({le} 2 mole-% CO{sub 2}, {le} 4 ppm H{sub 2}S). Moreover, these processes must also be economically competitive with the conventional separation techniques, such as gas absorption, utilized for this purpose by the gas industry.

  18. Crosslinked Polybenzimidazole Membrane For Gas Separation

    SciTech Connect

    Jorgensen, Betty S.; Young, Jennifer S.; Espinoza, Brent F.

    2005-09-20

    A cross-linked, supported polybenzimidazole membrane for gas separation is prepared by layering a solution of polybenzimidazole (PBI) and a,a'dibromo-p-xylene onto a porous support and evaporating solvent. A supported membrane of cross-linked poly-2,2'-(m-phenylene)-5,5'-bibenzimidazole unexpectedly exhibits an enhanced gas permeability compared to the non-cross linked analog at temperatures over 265° C.

  19. A Gas Chromatograph/Mass Spectrometer System for UltraLow-Emission Combustor Exhaust Studies

    NASA Technical Reports Server (NTRS)

    Brabbs, Theodore A.; Wey, Chowen Chou

    1996-01-01

    A gas chromatograph (GC)/mass spectrometer (MS) system that allows the speciation of unburnt hydrocarbons in the combustor exhaust has been developed at the NASA Lewis Research Center. Combustion gas samples are withdrawn through a water-cooled sampling probe which, when not in use, is protected from contamination by a high-pressure nitrogen purge. The sample line and its connecting lines, filters, and valves are all ultraclean and are heated to avoid condensation. The system has resolution to the parts-per-billion (ppb) level.

  20. Optimization of the Finnigan MAT 5100 Capillary Gas Chromatograph-Mass Spectrometer for the Analysis of Polychlorinated Biphenyls.

    DTIC Science & Technology

    1986-11-01

    FINNIGAN MAT 5100 CAPILLARY GAS CHROMATOGRAPH-MASS SPECTROMETER FOR THE ANALYSIS OF POLYCHLORINATED BIPHENYLS J.A. Hiltz - J. Power ,¢., DJ : .,:.JAN 1 4...CAPILLARY GAS CHROMATOGRAPH-MASS SPECTROMETER FOR THE ANALYSIS OF POLYCHLORINATED BIPHENYLS J.A. Hiltz - J.J. Power November 1986 Approved by B.F. Peters A...INTRODUCTION The use of polychlorinated biphenyls (PCBs) as dielectric fluids in electrical transformers and capacitors has been commomplace over the

  1. A method for the analysis of tabun in multisol using gas chromatographic flame photometric detection.

    PubMed

    Logan, Thomas P; Allen, Edward D; Way, Mark R; Swift, Austin T; Soni, Sunil-Datta; Koplovitz, Irwin

    2006-01-01

    Preparation and analysis of tabun (GA) solutions are necessary for the continued development of countermeasures to this nerve agent. GA solutions must be stable and compatible for use in the test systems chosen for study; however, GA is very unstable in saline solutions. In the past we have found GA in saline at 2 mg/mL to be stable for a month or less at -70 degrees C, whereas saline solutions of sarin (GB), soman (GD), and cyclosarin (GF) were stable for many months. Previous studies have shown that Multisol (48.5% H(2)O, 40% propylene glycol, 10% ethanol, and 1.5% benzyl alcohol) provides stable solutions of GA. We confirmed the stability of GA in Multisol with phosphorus nuclear magnetic resonance (P horizontal line NMR) and developed a method for the analysis of GA in Multisol using gas chromatographic flame photometric detection (GCFPD) in the phosphorus mode. The GC method used acetonitrile (CH(3)CN) for a dilution solvent because of its miscibility with GA in chloroform (CHCl(3)) standards and GA in Multisol samples at 1% (v/v). Furthermore, the dilutions with CH(3)CN made the phosphorus mode interference peak present in CHCl(3) analytically manageable, reduced the interferences of Multisol in the GC separation, and contributed to a safe and reliable analysis of GA at 20 mug/mL. We demonstrated the stability of GA in Multisol stored for more than a year at 70 degrees C. This method contributes a suitable technique for the preparation and analysis of reliable solutions of GA in nerve agent medical research and demonstrates the extended stability of GA in Multisol.

  2. Toward a microfabricated preconcentrator-focuser for a wearable micro-scale gas chromatograph.

    PubMed

    Bryant-Genevier, Jonathan; Zellers, Edward T

    2015-11-27

    This article describes work leading to a microfabricated preconcentrator-focuser (μPCF) designed for integration into a wearable microfabricated gas chromatograph (μGC) for monitoring workplace exposures to volatile organic compounds (VOCs) ranging in vapor pressure from ∼0.03 to 13kPa at concentrations near their respective Threshold Limit Values. Testing was performed on both single- and dual-cavity, etched-Si μPCF devices with Pyrex caps and integrated resistive heaters, packed with the graphitized carbons Carbopack X (C-X) and/or Carbopack B (C-B). Performance was assessed by measuring the 10% breakthrough volumes and injection bandwidths of a series of VOCs, individually and in mixtures, as a function of the VOC air concentrations, mixture complexity, sampling and desorption flow rates, adsorbent masses, temperature, and the injection split ratio. A dual-cavity device containing 1.4mg of C-X and 2.0mg of C-B was capable of selectively and quantitatively capturing a mixture of 14 VOCs at low-ppm concentrations in a few minutes from sample volumes sufficiently large to permit detection at relevant concentrations for workplace applications with the μGC detector that we ultimately plan to use. Thermal desorption at 225°C for 40s yielded ≥99% desorption of all analytes, and injected bandwidths as narrow as 0.6s facilitated efficient separation on a downstream 6-m GC column in <3min. A preconcentration factor of 620 was achieved for benzene from a sample of just 31mL. Increasing the mass of C-X to 2.3mg would be required for exhaustive capture of the more volatile target VOCs at high-ppm concentrations.

  3. Novel chromatographic separation and carbon solid-phase extraction of acetanilide herbicide degradation products.

    PubMed

    Shoemaker, Jody A

    2002-01-01

    One acetamide and 5 acetanilide herbicides are currently registered for use in the United States. Over the past several years, ethanesulfonic acid (ESA) and oxanilic acid (OA) degradation products of these acetanilide/acetamide herbicides have been found in U.S. ground waters and surface waters. Alachlor ESA and other acetanilide degradation products are listed on the U.S. Environmental Protection Agency's (EPA) 1998 Drinking Water Contaminant Candidate List. Consequently, EPA is interested in obtaining national occurrence data for these contaminants in drinking water. EPA currently does not have a method for determining these acetanilide degradation products in drinking water; therefore, a research method is being developed using liquid chromatography/negative ion electrospray/mass spectrometry with solid-phase extraction (SPE). A novel chromatographic separation of the acetochlor/alachlor ESA and OA structural isomers was developed which uses an ammonium acetate-methanol gradient combined with heating the analytical column to 70 degrees C. Twelve acetanilide degradates were extracted by SPE from 100 mL water samples using carbon cartridges with mean recoveries >90% and relative standard deviations < or =16%.

  4. Using precipitation by polyamines as an alternative to chromatographic separation in antibody purification processes.

    PubMed

    Ma, Junfen; Hoang, Hai; Myint, Thomas; Peram, Thanmaya; Fahrner, Robert; Chou, Judy H

    2010-03-15

    Polyamine precipitation conditions for removing host cell protein impurities from the cell culture fluid containing monoclonal antibody were studied. We examined the impact of polyamine concentration, size, structure, cell culture fluid pH and ionic strength. A 96-well microtiter plate based high throughput screening method was developed and used for evaluating different polyamines. Polyallylamine, polyvinylamine, branched polyethyleneimine and poly(dimethylamine-co-epichlorohydrin-ethylenediamine) were identified as efficient precipitants in removing host cell protein impurities. Leveraging from the screening results, we incorporated a polyamine precipitation step into a monoclonal antibody purification process to replace the Protein A chromatography step. The optimization of the overall purification process was performed by taking the mechanisms of both precipitation and chromatographic separation into account. The precipitation-containing process removed a similar amount of process-related impurities, including host cell proteins, DNA, insulin and gentamicin and maintained similar product quality in respect of size and charge variants to chromatography based purification. Overall recovery yield was comparable to the typical Protein A affinity chromatography based antibody purification process.

  5. Surface-modified polystyrene beads as photografting imprinted polymer matrix for chromatographic separation of proteins.

    PubMed

    Qin, Lei; He, Xi-Wen; Zhang, Wei; Li, Wen-You; Zhang, Yu-Kui

    2009-01-30

    A new and facile fabricating method for lysozyme molecularly imprinted polymer beads (lysozyme-MIP beads) in aqueous media was presented. Mesoporous chloromethylated polystyrene beads (MCP beads) containing dithiocarbamate iniferter (initiator transfer agent terminator) were used as supports for the grafting of lysozyme imprinted copolymers with acrylamide and N,N'-methylenebisacrylamide through surface initiated living-radical polymerization (SIP). After the polymerization, a layer of lysozyme-MIP was formed on the MCP beads. The SIP allowed an efficient control of the grafting process and suppressed solution propagation. Therefore, the obtained lysozyme-MIP beads had a large quantity of well-distributed pores on the surface without any visible gel formation in solution and were more advantageous comparing with traditional MIPs which were prepared by traditionally initiated radical polymerization. The obtained composites were characterized by Fourier transform infrared spectroscopy, elemental analysis, nitrogen sorption analysis and scanning electron microscopy. Chromatographic behaviors of the column packed with lysozyme-MIP beads exhibited ability in separating lysozyme from competitive protein (bovine hemoglobin, bovine serum albumin, ovalbumin or cytochrome c) in aqueous mobile phase.

  6. Metal oxide membranes for gas separation

    DOEpatents

    Anderson, M.A.; Webster, E.T.; Xu, Q.

    1994-08-30

    A method for formation of a microporous ceramic membrane onto a porous support includes placing a colloidal suspension of metal oxide particles on one side of the porous support and exposing the other side of the porous support to a drying stream of gas or a reactive gas stream so that the particles are deposited on the drying side of the support as a gel. The gel so deposited can be sintered to form a supported ceramic membrane having mean pore sizes less than 30 Angstroms and useful for ultrafiltration, reverse osmosis, or gas separation. 4 figs.

  7. Metal oxide membranes for gas separation

    DOEpatents

    Anderson, Marc A.; Webster, Elizabeth T.; Xu, Qunyin

    1994-01-01

    A method for permformation of a microporous ceramic membrane onto a porous support includes placing a colloidal suspension of metal oxide particles on one side of the porous support and exposing the other side of the porous support to a drying stream of gas or a reactive gas stream so that the particles are deposited on the drying side of the support as a gel. The gel so deposited can be sintered to form a supported ceramic membrane having mean pore sizes less than 30 Angstroms and useful for ultrafiltration, reverse osmosis, or gas separation.

  8. Development and assessment of a miniaturised centrifugal chromatograph for reversed-phase separations in micro-channels.

    PubMed

    Penrose, Andrew; Myers, Peter; Bartle, Keith; McCrossen, Sean

    2004-08-01

    This paper describes the micro-fabrication and preliminary assessment of a miniature polydimethylsiloxane (PDMS) device for performing rapid, parallel liquid phase chromatographic separations driven by centrifugal force in microchannels. Device components include a main separating channel, into which a high performance liquid chromatography (HPLC) particulate stationary phase was packed under pressure by application of centrifugal force, in addition to solvent and sample reservoirs. Also described are methods for sealing such devices based upon partial polymerisation of PDMS. The mobile phase flow rate through a typical device was measured and several important chromatographic parameters determined from a test separation. An expression describing mobile phase flow through packed channels was also developed, based upon work on liquid flow in open micro-channels. Good agreement between predicted and measured flow rates were observed. Some predictions for potential uses of such devices and possibilities for further miniaturisation are discussed.

  9. Metering Gas Strut for Separating Rocket Stages

    NASA Technical Reports Server (NTRS)

    Floyd, Brian

    2010-01-01

    A proposed gas strut system would separate a liquid-fueled second rocket stage from a solid-fueled first stage using an array of pre-charged struts. The strut would be a piston-and-cylinder mechanism containing a compressed gas. Adiabatic expansion of the gas would drive the extension of the strut. The strut is designed to produce a force-versus-time profile, chosen to prevent agitation of the liquid fuel, in which the force would increase from an initial low value to a peak value, then decay toward the end of the stroke. The strut would include a piston chamber and a storage chamber. The piston chamber would initially contain gas at a low pressure to provide the initial low separation force. The storage chamber would contain gas at a higher pressure. The piston would include a longitudinal metering rod containing an array of small holes, sized to restrict the flow gas between the chambers, that would initially not be exposed to the interior of the piston chamber. During subsequent expansion, the piston motion would open more of the metering holes between the storage and piston chambers, thereby increasing the flow of gas into the piston chamber to produce the desired buildup of force.

  10. Gas separation using ultrasound and light absorption

    DOEpatents

    Sinha, Dipen N [Los Alamos, NM

    2012-07-31

    An apparatus and method for separating a chosen gas from a mixture of gases having no moving parts and utilizing no chemical processing is described. The separation of particulates from fluid carriers thereof has been observed using ultrasound. In a similar manner, molecular species may be separated from carrier species. It is also known that light-induced drift may separate light-absorbing species from carrier species. Therefore, the combination of temporally pulsed absorption of light with ultrasonic concentration is expected to significantly increase the efficiency of separation by ultrasonic concentration alone. Additionally, breaking the spatial symmetry of a cylindrical acoustic concentrator decreases the spatial distribution of the concentrated particles, and increases the concentration efficiency.

  11. Pump Propels Liquid And Gas Separately

    NASA Technical Reports Server (NTRS)

    Harvey, Andrew; Demler, Roger

    1993-01-01

    Design for pump that handles mixtures of liquid and gas efficiently. Containing only one rotor, pump is combination of centrifuge, pitot pump, and blower. Applications include turbomachinery in powerplants and superchargers in automobile engines. Efficiencies lower than those achieved in separate components. Nevertheless, design is practical and results in low consumption of power.

  12. First Results From the Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe

    NASA Technical Reports Server (NTRS)

    Niemann, Hasso B.; Demick, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Raaen, E.; Way, S.; Atreya, S.; Carignan, G.; Bauer, S.

    2005-01-01

    The Huygens Probe of the Cassini Huygens Mission entered the atmosphere of the moon Titan on January 14,2005. The GCMS was part of the instrument complement on the Probe to measure in situ the chemical composition of the atmosphere during the probe descent and to support the Aerosol Collector Pyrolyser (ACP) experiment by serving as detector for the pyrolization products. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns. The mass spectrometer employed five electron impact ion sources with available electron energies of either 70 or 25 eV. Three ion sources served as detectors for the GC columns and two were dedicated to direct atmosphere sampling and ACP gas sampling, respectively. The GCMS gas inlet was heated to prevent condensation, and served to evaporate surface constituents after impact.

  13. Separation studies of As(III), Sb(III) and Bi(III) by reversed-phase paper chromatographic technique

    SciTech Connect

    Raman, B.; Shinde, V.M.

    1987-07-01

    Reversed-phase paper chromatographic separations of As(III), Sb(III) and Bi(III) have been carried out on Whatman No 1 filter paper impregnated with triphenylphosphine oxide as stationary phase and using organic complexing agents such as sodium acetate, sodium succinate and sodium malonate solutions as active mobile phases. Results for the separation of binary and ternary mixtures are reported and the method has been successfully applied to the separation and detection of these elements present in real samples and at ppm level concentration.

  14. [Investigation of a gas chromatographic column system for the on-line analysis of gaseous components in de-propane tower of pyrolysis equipment].

    PubMed

    Cai, H; Liu, L J; Yan, J; Lu, X; Ye, F; Xu, G W

    2000-03-01

    Multi-dimensional gas chromatograph has become an important process analyzer due to the advantages of high resolution and fast speed. According to the production requirement, a gas chromatographic column switching system has been investigated for the on-line analysis of gaseous components from high-pressure and lower-pressure de-propane towers of pyrolysis equipment. By using two different injection times on three injectors, and fore-flush and back-flush techniques, C2-hydrocarbons, propane, propene, methylacetylene, propadiene and C4-hydrocarbons can be separated on 7 columns in 7 minutes. The practical application showed the developed column system is suitable for the on-line monitoring of the production process.

  15. Gas chromatographic-mass spectrometric determination of brain levels of alpha-cholest-8-en-3beta-ol (lathosterol).

    PubMed

    Luzón-Toro, Berta; Zafra-Gómez, Alberto; Ballesteros, Oscar

    2007-05-01

    A gas chromatographic-mass spectrometric (GC-MS) method is proposed for the detection and quantification of lathosterol in rabbit brain. This compound is one of the most important precursors of the cholesterol synthesis. The interest in brain cholesterol metabolism is growing nowadays since it was described to play an important role in some neurodegenerative disorders such as Alzheimer's disease and Multiple Sclerosis. The analytical methodology proposed involves a liquid-liquid extraction procedure (LLE) followed by a silylation step previous to the GC-MS analysis. The chromatographic separation was performed by using a low bleed HP5-MS fused silica capillary column. A clean up is not necessary when using single-ion monitoring (SIM) mode. The molecular ion appears at 458 m/z; being as well the base peak. Alpha-naphtol was used as an internal standard. The detection limit obtained was 0.09 microg mL(-1). The method was applied to the determination of brain lathosterol levels in rabbits fed with different types of diets (control and atherogenic, supplemented or not with natural polyphenolic antioxidants). The quantification of the compound in samples showed a reduction, after 1 month, of this precursor of cholesterol synthesis in groups fed with antioxidant supplemented diets.

  16. Experimental Confirmation of Isotope Fractionation in Thiomolybdates Using Ion Chromatographic Separation and Detection by Multicollector ICPMS.

    PubMed

    Kerl, Carolin F; Lohmayer, Regina; Bura-Nakić, Elvira; Vance, Derek; Planer-Friedrich, Britta

    2017-03-07

    Molybdenum (98)Mo/(95)Mo isotope ratios are a sediment paleo proxy for the redox state of the ancient ocean. Under sulfidic conditions, no fractionation between seawater and sediment should be observed if molybdate (MoO4(2-)) is quantitatively transformed to tetrathiomolybdate (MoS4(2-)) and precipitated. However, quantum mechanical calculations previously suggested that incomplete sulfidation could be associated with substantial fractionation. To experimentally confirm isotope fractionation in thiomolybdates, a new approach for determination of isotope ratios of individual thiomolybdate species was developed that uses chromatography (HPLC-UV) to separate individual thiomolybdates, collecting each peak and analyzing isotope ratios with multicollector inductively coupled plasma mass spectrometry (MC-ICPMS). Using commercially available MoO4(2-) and MoS4(2-) standards, the method was evaluated and excellent reproducibility and accuracy were obtained. For species with longer retention times, complete chromatographic peaks had to be collected to avoid isotope fractionation within peaks. Isotope fractionation during formation of thiomolybdates could be experimentally proven for the first time in the reaction of MoO4(2-) with 20-fold or 50-fold excess of sulfide. The previously calculated isotope fractionation for MoS4(2-) was confirmed, and the result for MoO2S2(2-) was in the predicted range. Isotopic fractionation during MoS4(2-) transformation with pressurized air was dominated by kinetic fractionation. Further optimization and online-coupling of the HPLC-MC-ICPMS approach for determination of low concentrations in natural samples will greatly help to obtain more accurate species-selective isotope information.

  17. High-performance reversed-phase ion-pair chromatographic study of myo-inositol phosphates. Separation of myo-inositol phosphates, some common nucleotides and sugar phosphates.

    PubMed

    Patthy, M; Balla, T; Arányi, P

    1990-12-07

    A detailed study of all the major chromatographic variables affecting the retention behaviour and separation of myo-inositol phosphates in reversed-phase ion-pair chromatographic systems was carried out. The parameters studied included the eluent concentration of the pairing ion, the eluent concentration of the organic modifier and the buffer salt, the pH of the eluent, the minimum column plate count necessary for the separation of the inositol trisphosphate isomers and isocratic and gradient modes of separation. The retention behaviour of some common nucleotides and sugar phosphates was also investigated as these phosphates present chromatographic interference problems in biochemical studies based on the cellular incorporation of [32P]Pi. The separation methods developed appear to be superior to established anion-exchange separation techniques in terms of separation speed and "mildness" of the chromatographic conditions.

  18. Adsorption Model for Off-Gas Separation

    SciTech Connect

    Veronica J. Rutledge

    2011-03-01

    The absence of industrial scale nuclear fuel reprocessing in the U.S. has precluded the necessary driver for developing the advanced simulation capability now prevalent in so many other countries. Thus, it is essential to model complex series of unit operations to simulate, understand, and predict inherent transient behavior and feedback loops. A capability of accurately simulating the dynamic behavior of advanced fuel cycle separation processes will provide substantial cost savings and many technical benefits. The specific fuel cycle separation process discussed in this report is the off-gas treatment system. The off-gas separation consists of a series of scrubbers and adsorption beds to capture constituents of interest. Dynamic models are being developed to simulate each unit operation involved so each unit operation can be used as a stand-alone model and in series with multiple others. Currently, an adsorption model has been developed in gPROMS software. Inputs include gas stream constituents, sorbent, and column properties, equilibrium and kinetic data, and inlet conditions. It models dispersed plug flow in a packed bed under non-isothermal and non-isobaric conditions for a multiple component gas stream. The simulation outputs component concentrations along the column length as a function of time from which the breakthrough data is obtained. It also outputs temperature along the column length as a function of time and pressure drop along the column length. Experimental data will be input into the adsorption model to develop a model specific for iodine adsorption on silver mordenite as well as model(s) specific for krypton and xenon adsorption. The model will be validated with experimental breakthrough curves. Another future off-gas modeling goal is to develop a model for the unit operation absorption. The off-gas models will be made available via the server or web for evaluation by customers.

  19. A theoretical model for the separation of glucose and fructose mixtures by using a semicontinuous chromatographic refiner

    SciTech Connect

    Lee, Kwang Nam; Lee, Won Kook )

    1992-03-01

    The separation of a glucose and fructose mixture was experimentally performed by using a semicontinuous chromatographic refiner (SCCR) packed with Ca{sup 2+} ion in the form of DOWEX 50W 12X resin. The plug flow model with velocity-dependent mass transfer resistance was resistance was presented for calculating both products and on-concentrations in the SCCR unit, and the validity of the model was experimentally confirmed.

  20. Screening of ground water samples for volatile organic compounds using a portable gas chromatograph

    USGS Publications Warehouse

    Buchmiller, R.C.

    1989-01-01

    A portable gas chromatograph was used to screen 32 ground water samples for volatile organic compounds. Seven screened samples were positive; four of the seven samples had volatile organic substances identified by second-column confirmation. Four of the seven positive, screened samples also tested positive in laboratory analyses of duplicate samples. No volatile organic compounds were detected in laboratory analyses of samples that headspace screening indicated to be negative. Samples that contained volatile organic compounds, as identified by laboratory analysis, and that contained a volatile organic compound present in a standard of selected compounds were correctly identified by using the portable gas chromatography. Comparisons of screened-sample data with laboratory data indicate the ability to detect selected volatile organic compounds at concentrations of about 1 microgram per liter in the headspace of water samples by use of a portable gas chromatography. -Author

  1. Structure, gas chromatographic measurement, and function of suberin synthesized by potato tuber tissue slices.

    PubMed

    Kolattukudy, P E; Dean, B B

    1974-07-01

    The polymeric material (suberin) of the wound periderm of potato tuber slices was analyzed after depolymerization with LiAIH(4) in tetrahydrofuran or BF(3) in methanol with the use of thin layer chromatography, chemical modification, and combined gas-liquid chromatography and mass spectrometry. Fatty acids (C(16) to C(26)), fatty alcohols (C(16) to C(26)), octadec-9-ene-1, 18-dioic acid, and 18-hydroxy-octadec-9-enoic acid were identified to be the major components. Based on the structural information that the two bifunctional C(18) molecules constituted a major portion of suberin, a gas chromatographic method of measuring suberization was developed. This method consisted of hydrogenolysis of powdered tissue followed by thin layer chromatography and gas chromatographic measurement of octadecene-1, 18-diol as the trimethylsilyl ether. With this assay it was shown that the development of resistance to water loss by the tissue slices was directly proportional to the quantity of the bifunctional C(18) molecules, thus providing evidence that a function of suberin is prevention of water loss.

  2. Gas chromatographic determination of propionates as paranitrobenzyl ester in bakery products.

    PubMed

    Takatsuki, K; Sakai, K

    1982-07-01

    A procedure was developed to determine propionates used as mold inhibitors and preservatives in bakery products. Propionates were extracted from the sample with water alkalinized by potassium carbonate. Water was evaporated, and the residue was reacted with paranitrobenzyl bromide in dimethyl-formamide-water (90 + 10) at room temperature to convert propionates to paranitrobenzyl ester, which was determined with a gas chromatograph equipped with a flame ionization detector. Bakery products, such as bread, sponge cake, cookies, and biscuits, were analyzed by this procedure. Recoveries from samples fortified with propionates ranged from 94 to 101%, with a standard deviation of 3.32. The concentrations determined were 50 to 2500 micrograms/g sample.

  3. Miniature triaxial metastable ionization detector for gas chromatographic trace analysis of extraterrestrial volatiles

    NASA Technical Reports Server (NTRS)

    Woeller, F. H.; Kojiro, D. R.; Carle, G. C.

    1984-01-01

    The present investigation is concerned with a miniature metastable ionization detector featuring an unconventional electrode configuration, whose performance characteristics parallel those of traditional design. The ionization detector is to be incorporated in a flight gas chromatograph (GC) for use in the Space Shuttle. The design of the detector is discussed, taking into account studies which verified the sensitivity of the detector. The triaxial design of the detector is compared with a flat-plate style. The obtained results show that the principal goal of developing a miniature, highly sensitive ionization detector for flight applications was achieved. Improved fabrication techniques will utilize glass-to-metal seals and brazing procedures.

  4. [Gas chromatographic analysis of methyl methacrylate and methanol in its esterification mixture].

    PubMed

    Wu, C; Zeng, C

    1997-09-01

    A fast, simple and accurate gas chromatographic method is established for determining the content of methyl methacrylate (MMA) and methanol in the esterification mixture of methacrylic acid with methanol in the presence of sulfuric acid. In the measurement, polyethylene glycol-20M/sodium hydroxide was adopted as liquid phase, coated on the acid-washed 201 pink support. n-Heptane was used as the internal standard and the correction factors of MMA and methanol obtained were 1.65 and 4.10, respectively. It is significant for this method to be used to control MMA production by acetone cyanohydrin method and to improve the production technology.

  5. Improvement of the chromatographic separation of several 1,4-dihydropyridines calcium channel antagonist drugs by experimental design.

    PubMed

    Baranda, Ana B; Etxebarria, Nestor; Jiménez, Rosa M; Alonso, Rosa M

    2005-01-01

    A high-performance liquid chromatographic method with diode array detection has been developed and optimized for the separation of five calcium channel blockers belonging to the 1,4-dihydropyridine subgroup (nifedipine and related drugs). The possibility of the simultaneous drug analysis allows a decrease of time during the assay as well as a saving of reagents and solvents. In this work, the effect of four experimental parameters (organic modifier percentage, pH value, concentration of the buffer in the mobile phase, and column temperature) on the chromatographic resolution are investigated by experimental design in order to optimize the chromatographic separation of five 1,4-dihydropyridines (amlodipine, nitrendipine, felodipine, lacidipine, and lercanidipine). Fractional factorial design, central composite design, and finally the Multisimplex program are used to establish the optimal conditions in terms of resolution and minimum analysis time. Optimal separation of the five compounds under study is achieved in less than 12 min using a Sulpecosil LC-ABZ+Plus C18 column, a composition of mobile phase of acetonitrile-10mM acetic acid acetate buffer pH 5 (72:28, v/v) at a flow rate of 1 mL/min, a column temperature of 30 degrees C +/- 0.1 degrees C, and a detection wavelength of 238 nm.

  6. Gas chromatograph analysis on closed air and nitrogen oxide storage atmospheres of recalcitrant seeds of Quercus Alba

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Storage of recalcitrant seeds remains an unsolved problem. This study investigated the quantitative gas analysis of nitrous oxide (N2O) and air atmospheres on the recalcitrant seeds of Quercus alba by using gas chromatograph. Ten seeds were placed in each sealed atmospheric system of air and 98/2% N...

  7. Synthesis of a further improved porous polymer for the separation of nitrogen, oxygen, argon, and carbon monoxide by gas chromatography

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.

    1986-01-01

    A further improvement has been made in the synthesis of an N-type porous polymer for the separation of permanent gases. Changing the ratios of reactants and diluting the Hi-DVB with styrene led to a porous polymer gas chromatographic packing which is superior to commercial products and to the author's own previously reported custom-made polymer.

  8. Four-port gas separation membrane module assembly

    DOEpatents

    Wynn, Nicholas P.; Fulton, Donald A.; Lokhandwala, Kaaeid A.; Kaschemekat, Jurgen

    2010-07-20

    A gas-separation membrane assembly, and a gas-separation process using the assembly. The assembly incorporates multiple gas-separation membranes in an array within a single vessel or housing, and is equipped with two permeate ports, enabling permeate gas to be withdrawn from both ends of the membrane module permeate pipes.

  9. Headspace gas chromatographic method for determination of methyl bromide in food ingredients

    SciTech Connect

    DeVries, J.W.; Broge, J.M.; Schroeder, J.P.; Bowers, R.H.; Larson, P.A.; Burns, N.M.

    1985-11-01

    A headspace gas chromatographic (GC) method, which can be automated, has been developed for determination of methyl bromide. This method has been applied to wheat, flour, cocoa, and peanuts. Samples to be analyzed are placed in headspace sample vials, water is added, and the vials are sealed with Teflon-lined septa. After an appropriate equilibration time at 32 degrees C, the samples are analyzed within 10 h. A sample of the headspace is withdrawn and analyzed on a gas chromatograph equipped with an electron capture detector (ECD). Methyl bromide levels were quantitated by comparison of peak area with a standard. The standard was generated by adding a known amount of methyl bromide to a portion of the matrix being analyzed and which was known to be methyl bromide free. The detection limit of the method was 0.4 ppb. The coefficient of variation (CV) was 6.5% for wheat, 8.3% for flour, 3.3% for cocoa, and 11.6% for peanuts.

  10. Microfabricated gas chromatograph for on-site determination of trichloroethylene in indoor air arising from vapor intrusion. 1. Field evaluation.

    PubMed

    Kim, Sun Kyu; Burris, David R; Chang, Hungwei; Bryant-Genevier, Jonathan; Zellers, Edward T

    2012-06-05

    Results are presented of inaugural field tests of two identical prototype microfabricated gas chromatographs (μGC) adapted for the in situ determination of trichloroethylene (TCE) in indoor air in support of vapor intrusion (VI) investigations. Each μGC prototype has a pretrap and partially selective high-volume sampler of conventional design, a micromachined-Si focuser for injection, dual micromachined-Si columns for separation, and an integrated array of four microscale chemiresistors with functionalized gold nanoparticle interface films for multichannel detection. Scrubbed ambient air is used as the carrier gas. Field-generated calibration curves were linear for injected TCE masses of 26-414 ng (4.8-77 ppb·L; r(2) > 0.98) and the projected single-sensor detection limit was 0.052 ppb for an 8-L air sample collected and analyzed in 20 min. Consistent performance between the prototypes and good medium-term stability were shown. Above the mitigation action level (MAL) of 2.3 ppb for the field-test site, μGC TCE determinations fell within ±25% of those from the reference method for 21 of 26 measurements, in the presence of up to 37 documented background VOCs. Below the MAL, positive biases were consistently observed, which are attributable to background VOCs that were unresolvable chromatographically or by analysis of the sensor-array response patterns. Results demonstrate that this type of μGC instrument could serve the need for routine TCE determinations in VI-related assessment and mitigation efforts.

  11. Fast low-pressure microwave assisted extraction and gas chromatographic determination of polychlorinated biphenyls in soil samples.

    PubMed

    Bruzzoniti, M C; Maina, R; Tumiatti, V; Sarzanini, C; Rivoira, L; De Carlo, R M

    2012-11-23

    A new technology equipment for low-pressure microwave assisted extraction (usually employed for organic chemistry reactions), recently launched in the market, is used for the first time in environmental analysis for the extraction of commercial technical Aroclor mixtures from soil. Certified reference materials of Aroclor 1260, Aroclor 1254 and Aroclor 1242 in transformer oils were used to contaminate the soil samples and to optimize the extraction method as well as the subsequent gas chromatographic electron capture detection (GC-ECD) analytical method. The study was performed optimizing the extraction, the purification and the gas chromatographic separation conditions to enhance the resolution of difficult pairs of congeners (C28/31 and C141/179). After optimization, the recovery yields were included within the range 79-84%. The detection limits, evaluated for two different commercial polychlorinated biphenyl (PCB) mixtures (Aroclor 1260 and Aroclor 1242) were 0.056 ± 0.001 mg/kg and 0.290 ± 0.006 mg/kg, respectively. The method, validated with certified soil samples, was used to analyze a soil sample after an event of failure of a pole-mounted transformer which caused the dumping of PCB contaminated oil in soil. Moreover, the method provides simple sample handling, fast extraction with reduced amount of sample and solvents than usually required, and simple purification step involving the use of solvent (cyclohexane) volumes as low as 5 mL. Reliability and reproducibility of extraction conditions are ensured by direct and continuous monitoring of temperature and pressure conditions.

  12. Gas chromatographic investigation of volatile nitrogen containing bases of Antarctic krill Euphausia superba Dana.

    PubMed

    Svetlova, N I; Golovnya, R V; Zhuravleva, I L; Grigorieva, D N; Samusenko, A L

    1985-01-01

    The composition of the volatile nitrogen-containing bases of fresh-caught Antarctic krill E. superba has been investigated by gas chromatography. The analysis was carried out on three packed columns with Apiezon L, Triton X-305, PEG-1000 and one glass capillary column with Triton X-305. The components were identified by standardless gas chromatographic method with a special computer program. No less than 63 compounds have been found and 54 compounds have been identified, among these primary, secondary and tertiary aliphatic amines as well as heterocyclic bases. The presence of 5 compounds has been confirmed by GC/MS technique. Analysis with the help of a specific flame-photometric detector has shown the presence of 9 bi-functional nitrogen- and sulfur-containing compounds.

  13. Gas chromatographic determination of polysaccharide gums in foods after hydrolysis and derivatization.

    PubMed

    Lawrence, J F; Iyengar, J R

    1985-12-20

    A gas chromatographic method was evaluated for the determination of food grade gums in dairy products, salad dressings and meat sauces. The gums studied were tragacanth, karaya, ghatti, carob, guar, arabic and xanthan gum. The extraction method included removal of fat followed by starch degradation then precipitation of protein. The isolated gums were hydrolysed with trifluoroacetic acid and the resulting neutral monosaccharides converted to their aldonitrile acetate derivatives for determination by gas chromatography. Recoveries from thirteen different commodities averaged 85%. However, the recovery of guar gum from ice cream and cold pack cheese was 42 and 50%, respectively. In a comparison of enzyme hydrolysis and iodine complexation for the removal of starch the former was simpler and provided cleaner extracts than the iodine treatment. Both gave similar results.

  14. Quantitative gas chromatographic analysis of volatile fatty acids in spent culture media and body fluids.

    PubMed Central

    van den Bogaard, A E; Hazen, M J; Van Boven, C P

    1986-01-01

    Gas chromatographic analysis of volatile fatty acids for identification of obligately anaerobic bacteria and for presumptive diagnosis of anaerobic infections is now widely practiced. However, it is difficult to compare data because only a qualitative analysis is done or only chromatograms are presented instead of quantitative data on volatile fatty acid production. We compared three stationary phases for volatile fatty acid analysis of aqueous solutions and four methods of pretreating samples for gas chromatography. Quantitative analysis could be done accurately by using Carbowax as the stationary phase after pretreatment of spent culture media with Dowex columns. If only qualitative analysis is required (e.g., for presumptive diagnosis of anaerobic infections), ether extraction and headspace analysis are equally suitable. The overall variation coefficient for volatile fatty acid production by four reference strains of obligately anaerobic bacteria after 24 h of incubation was approximately 10%. PMID:3958144

  15. Detection system for a gas chromatograph. [. cap alpha. -methylnaphthalene,. beta. -methylnapthalene

    DOEpatents

    Hayes, J.M.; Small, G.J.

    1982-04-26

    A method and apparatus are described for the quantitative analysis of vaporizable compounds, and in particular of polycyclic aromatic hydrocarbons which may be induced to fluoresce. The sample to be analyzed is injected into a gas chromatography column and is eluted through a narrow orifice into a vacuum chamber. The free expansion of the eluted sample into the vacuum chamber creates a supersonic molecular beam in which the sample molecules are cooled to the extent that the excited vibrational and rotational levels are substantially depopulated. The cooled molecules, when induced to fluoresce by laser excitation, give greatly simplified spectra suitable for analytical purposes. The laser induced fluorimetry provides great selectivity, and the gas chromatograph provides quantitative transfer of the sample to the molecular beam. 3 figures, 2 tables.

  16. Gas storage and separation by electric field swing adsorption

    DOEpatents

    Currier, Robert P; Obrey, Stephen J; Devlin, David J; Sansinena, Jose Maria

    2013-05-28

    Gases are stored, separated, and/or concentrated. An electric field is applied across a porous dielectric adsorbent material. A gas component from a gas mixture may be selectively separated inside the energized dielectric. Gas is stored in the energized dielectric for as long as the dielectric is energized. The energized dielectric selectively separates, or concentrates, a gas component of the gas mixture. When the potential is removed, gas from inside the dielectric is released.

  17. [Contamination mechanism and regeneration strategies of chromatographic resin in separation process for expression product from mammary gland bioreactor].

    PubMed

    Sun, Xiyan; Zhang, Yan; Li, Yan; Luo, Jian; Qin, Peiyong; Su, Zhiguo

    2011-11-01

    This study focused on the contamination mechanism and regeneration strategies of sulfopropyl ion exchange resin (SP Sepharose FF) during the separation of recombinant human lactoferrin from transgenic bovine milk. We analyzed primary constituents' contents in chromatorgraphic material and fractions. The results showed that the lipid in milk can clog the column or adhere to the resin through hydrophobic interaction, leading to an increase in column pressure. Some casein molecules were found to adsorb onto the resin through electrostatic interaction, therefore the adsorption capacity was decreased. There was no direct interaction between lactose and the resin in the chromatorgraphic process. Increased continuous chromatographic cycles and prolonged time interval between protein purification and column regeneration could enhance the undesirable interaction between the contaminants and resin, thus lowering the regeneration efficiency. NaOH was found to be effective in the removal of lipid and casein molecules from the column. Furthermore, normal microstructure and chromatographic performance of the ion exchanger was recovered after this cleaning procedure.

  18. Hyperthin Organic Membranes for Gas Separations

    NASA Astrophysics Data System (ADS)

    Wang, Minghui

    Gas separation is practically important in many aspects, e.g., clean energy production and global warming prevention. Compared to other separation technologies like cryogenic distillation and pressure swing adsorption, membrane separation is considered to be more energy efficient. For practical purposes, the ultimate goal is to construct membranes producing high flux and high gas permeation selectivity at the same time. Based on the inverse relationship between flux and membrane thickness, it is clear that fabricating highly selective membranes as thin as possible could increase the flux through the membrane without sacrificing selectivity. But it has proven to be challenging to manufacture selective membranes in the hyperthin (< 100nm) region. [Note: 100 nm is the typical dense layer thickness of commercial membranes to separation gases.] In this dissertation, the focus is on the development of hyperthin selective membranes that were supported by poly(1-trimethylsilyl-1-propyne) (PTMSP), using Langmuir-Blodgett (LB) and Layer-by-Layer (LbL) deposition methods. A "gluing" strategy has been successfully introduced into LB films by our laboratory recently, in which LB monolayers are ionically crosslinked with polyelectrolytes. This success stimulated the pursuance of LB films with improved gas separation properties by: (i) examining calix[n]arene-based surfactants with different sizes (ii) using polymeric surfactants as LB forming materials, and (iii) optimizing the condition of the subphase containing polyelectrolytes. Both a strong polyelectrolyte poly(4-styrene sulfonate) (PSS) and a weak polyelectrolyte poly(acrylic acid) (PAA) were used to create glued LB bilayers. The gas permeation through PSS or PAA-glued LB bilayers made of calix[n]arenes was found to be dominated by solution-diffusion rather than molecular-sieving mechanism. The porous nature of calix[n]arene-based surfactants also turned out to be unnecessary for constructing LB films with high gas

  19. Feasibility of the preparation of silica monoliths for gas chromatography: fast separation of light hydrocarbons.

    PubMed

    Azzouz, Imadeddine; Essoussi, Anouar; Fleury, Joachim; Haudebourg, Raphael; Thiebaut, Didier; Vial, Jerome

    2015-02-27

    The preparation conditions of silica monoliths for gas chromatography were investigated. Silica-based monolithic capillary columns based on sol-gel process were tested in the course of high-speed gas chromatographic separations of light hydrocarbons mixture (C1-C4). The impact of modifying the amount of porogen and/or catalyst on the monolith properties were studied. At the best precursor/catalyst/porogen ratio evaluated, a column efficiency of about 6500 theoretical plates per meter was reached with a very good resolution (4.3) for very light compounds (C1-C2). The test mixture was baseline separated on a 70cm column. To our knowledge for the first time a silica-based monolithic capillary column was able to separate light hydrocarbons from methane to n-butane at room temperature with a back pressure in the range of gas chromatography facilities (under 4.1bar).

  20. Thin-layer chromatographic specification and separation of Cu(1+), Cu(2+), Ni(2+), and Co(2+) cations.

    PubMed

    Savasci, Sahin; Akçay, Mehmet; Ergül, Soner

    2010-07-01

    The M(PyDTC)(2) (M: Cu, Co, or Ni) and CuPyDTC complexes, prepared by reactions of ammonium pyrrolidinedithiocarbamate with metal nitrates, are examined for qualitative analysis, speciation, and mutual separation using thin-layer chromatography systems. These complexes and their mixtures are spotted to the activated and non-activated thin layers of silica gel 60GF(254) (Si-60GF(254)) with a 250-microm thickness. Toluene-dichloromethane mixtures (4:1, 1:1, 1:4 v/v) are used as mobile phases for running of the complexes. All of these chromatographic systems are successfully used for speciation of Cu(2+) and Cu(1+) cations. The best analytical separation for the qualitative analysis of corresponding metal cations and mutual separation of components in M(PyDTC)(2) and CuPyDTC complexes are obtained when using pure toluene-dichloromethane (1:1 v/v) on the activated layer. This study shows that it is possible to qualitatively analyze and satisfactorily separate a mixture of Cu(1+), Cu(2+), Ni(2+), and Co(2+) cations on cited chromatographic systems. These results may be also said for the adaptability or validity on column chromatography.

  1. Chromatographic separation of platinum group metals from simulated high level liquid waste using macroporous silica-based adsorbents.

    PubMed

    Xu, Yuanlai; Kim, Seong-Yun; Ito, Tatsuya; Tokuda, Haruki; Hitomi, Keitaro; Ishii, Keizo

    2013-10-18

    To separate platinum group metals (PGMs) from high level liquid waste, three novel macroporous silica-based adsorbents, namely, (Crea+Dodec)/SiO2-P, (Crea+TOA)/SiO2-P and (MOTDGA+TOA)/SiO2-P, were synthesized by introducing extractants Crea (N',N'-di-n-hexyl-thiodiglycolamide), TOA (Tri-n-octylamine), MOTDGA (N,N'-dimethyl-N,N'-di-n-octyl-thiodiglycolamide) along with theirs modifier, Dodec (n-dodecyl alcohol), into 50μm diameter SiO2-P particles by impregnation. Chromatographic separation of PGMs from simulated high level liquid waste was investigated by column method. It was found that 100% of Pd(II) and Re(VII) could be eluted out from simulate HLLW in 3.0M HNO3 solution using three adsorbents. For Ru(III) and Rh(III), high temperature has distinct effect on the adsorption rate and a further study for Ru(III) and Rh(III) is necessary to separate them from HLLW completely. In all six column experiments, a relatively satisfactory chromatographic separation operating for PGMs from simulated HLLW was obtained using (Crea+TOA)/SiO2-P adsorbent packed column at 323K.

  2. Permeable polyaniline articles for gas separation

    DOEpatents

    Wang, Hsing-Lin; Mattes, Benjamin R.

    2004-09-28

    Immersion precipitation of solutions having 15%-30% (w/w) and various molecular weights of the emeraldine base form of polyaniline in polar aprotic solvents are shown to form integrally skinned asymmetric membranes and fibers having skin layers <1 .mu.m thick which exhibit improved rates of gas transport while preserving good selectivity. These membranes can be further transformed by an acid doping process after fabrication to achieve excellent permeation rates and high selectivities for particular gas separations. Prior to the use of concentrated EB solutions, the formation of integrally skinned asymmetric membranes was not possible, since films and fibers made from <5% w/w polyaniline solutions were found to disintegrate during the IP process.

  3. Permeable polyaniline articles for gas separation

    DOEpatents

    Wang, Hsing-Lin; Mattes, Benjamin R.

    2009-07-21

    Immersion precipitation of solutions having 15%-30% (w/w) and various molecular weights of the emeraldine base form of polyaniline in polar aprotic solvents are shown to form integrally skinned asymmetric membranes and fibers having skin layers <1 .mu.m thick which exhibit improved rates of gas transport while preserving good selectivity. These membranes can be further transformed by an acid doping process after fabrication to achieve excellent permeation rates and high selectivities for particular gas separations. Prior to the use of concentrated EB solutions, the formation of integrally skinned asymmetric membranes was not possible, since films and fibers made from <5% w/w polyaniline solutions were found to disintegrate during the IP process.

  4. Kinetic optimisation of the reversed phase liquid chromatographic separation of rooibos tea (Aspalathus linearis) phenolics on conventional high performance liquid chromatographic instrumentation.

    PubMed

    Beelders, Theresa; Sigge, Gunnar O; Joubert, Elizabeth; de Beer, Dalene; de Villiers, André

    2012-01-06

    Rooibos tea, produced from the endemic South African shrub Aspalathus linearis, has various health-promoting benefits which are attributed to its phenolic composition. Generating reliable, quantitative data on these phenolic constituents is the first step towards documenting the protective effects associated with rooibos tea consumption. Reversed phase liquid chromatographic (RP-LC) methods currently employed in the quantitative analysis of rooibos are, however, hampered by limited resolution and/or excessive analysis times. In order to overcome these limitations, a systematic approach towards optimising the RP-LC separation of the 15 principal rooibos tea phenolics on a 1.8 μm phase using conventional HPLC instrumentation was adopted. Kinetic plots were used to obtain the optimal configuration for the separation of the target analytes within reasonable analysis times. Simultaneous optimisation of temperature and gradient conditions provided complete separation of these rooibos phenolics on a 1.8 μm C18 phase within 37 min. The optimised HPLC-DAD method was validated and successfully applied in the quantitative analysis of aqueous infusions of unfermented and fermented rooibos. Major phenolic constituents of fermented rooibos were found to be a phenylpropanoid phenylpyruvic acid glucoside (PPAG), the dihydrochalcone C-glycoside aspalathin, the flavones isoorientin and orientin, and a flavonol O-diglycoside tentatively identified as quercetin-3-O-robinobioside. Content values for PPAG, ferulic acid and quercetin-3-O-robinobioside in rooibos are reported here for the first time. Mass spectrometric (MS) and tandem MS detection were used to tentatively identify 13 additional phenolic compounds in rooibos infusions, including a new luteolin-6-C-pentoside-8-C-hexoside and a novel C-8-hexosyl derivative of aspalathin reported here for the first time.

  5. Interfacing a robotic station with a gas chromatograph for the full automation of the determination of organochlorine pesticides in vegetables

    SciTech Connect

    Torres, P.; Luque de Castro, M.D.

    1996-12-31

    A fully automated method for the determination of organochlorine pesticides in vegetables is proposed. The overall system acts as an {open_quotes}analytical black box{close_quotes} because a robotic station performs the prelimninary operations, from weighing to capping the leached analytes and location in an autosampler of an automated gas chromatograph with electron capture detection. The method has been applied to the determination of lindane, heptachlor, captan, chlordane and metoxcychlor in tea, marjoram, cinnamon, pennyroyal, and mint with good results in most cases. A gas chromatograph has been interfaced to a robotic station for the determination of pesticides in vegetables. 15 refs., 4 figs., 2 tabs.

  6. Simultaneous gas chromatographic determination of four toxic gases generally present in combustion atmospheres.

    PubMed

    Endecott, B R; Sanders, D C; Chaturvedi, A K

    1996-01-01

    The measurement of combustion gases produced by burning aircraft cabin materials poses a continuing limitation for smoke toxicity research. Because toxic effects of gases depend on both their concentrations and the duration of exposure, frequent atmosphere sampling is necessary to define the gas concentration-exposure time curve. A gas chromatographic (GC) method was developed for the simultaneous analyses of carbon monoxide (CO), hydrogen sulfide (H2S), sulfur dioxide (SO2), and hydrogen cyanide (HCN). The method used an MTI M200 dual-column gas chromatograph equipped with 4-m molecular sieve-5A and 8-m PoraPlot-U wall-coated capillary columns and two low-volume, high-sensitivity thermal conductivity detectors. Detectability (in parts per million [ppm]) and retention times (in seconds) for the gases were as follows: CO, 100 ppm, 28 s; H2S, 50 ppm, 26 s; SO2, 125 ppm, 76 s; and HCN, 60 ppm, 108 s. The method was effective for determining these gases in mixtures and in the combustion atmospheres generated by burning wool (CO, HCN, and H2S) and modacrylic fabrics (CO and HCN). Common atmospheric gaseous or combustion products (oxygen, carbon dioxide, nitrogen, water vapor, and other volatiles) did not interfere with the analyses. However, filtration of the combustion atmospheres was necessary to prevent restriction of the GC sampling inlet by smoke particulates. The speed, sensitivity, and selectivity of this method make it suitable for smoke toxicity research and for evaluating performance of passenger protective breathing equipment. Also, this method can potentially be modified to analyze these gases when they are liberated from biosamples.

  7. [The development of a static water/gas separator].

    PubMed

    Zhou, K H; Ai, S K; Lu, X Y; Liu, C L

    2000-10-01

    Objective. To develop a device for separating water from gas in small flow rate under zero "G". Method. Beginning with the study of surface characteristic of materials, a capillary material was developed according to the requirement and the water/gas separator using this single separating material was designed. Result. The water/gas separator worked well in the range of gas flow below 10.0 L/min and water flow below 10.0 ml/min. No gas was found in the separated water and no water was found in the separated gas. Conclusion. The structure of the separator was reasonable and the water/gas separating method using a single separating material was feasible.

  8. Gas chromatographic determination of volatile congeners in spirit drinks: interlaboratory study.

    PubMed

    Kelly, J; Chapman, S; Brereton, P; Bertrand, A; Guillou, C; Wittkowski, R

    1999-01-01

    An interlaboratory study of a gas chromatographic (GC) method for the determination of volatile congeners in spirit drinks was conducted; 31 laboratories from 8 countries took part in the study. The method uses GC with flame ionization detection and incorporates several quality control measures which permit the choice of chromatographic system and conditions to be selected by the user. Spirit drink samples were prepared and sent to participants as 10 blind duplicate or split-level test materials for the determination of 1,1-diethoxyethane (acetal), 2-methylbutan-1-ol (active amyl alcohol), 3-methylbutan-1-ol (isoamyl alcohol), methanol (methyl alcohol), ethyl ethanoate (ethyl acetate), butan-1-ol (n-butanol), butan-2-ol (sec-butanol), 2-methylpropan-1-ol (isobutyl alcohol), propan-1-ol (n-propanol), and ethanal (acetaldehyde). The precision of the method for 9 of the 10 analytes was well within the range predicted by the Horwitz equation. The precision of the most volatile analyte, ethanal, was just above statistically predicted levels. This method is recommended for official regulatory purposes.

  9. Gas-solid chromatographic analysis of automobile tailpipe emissions as a function of different engine and exhaust system modifications

    SciTech Connect

    Kang, L.; Armstrong, D.W.

    1994-12-31

    The authors developed a single, relatively short gas-solid chromatographic PLOT column and used it to separate aliphatic hydrocarbons, aromatic hydrocarbons and some inorganic gases (O{sub 2}, N{sub 2}, CO and CO{sub 2}) found in automobile exhaust. In the case of hydrocarbons, both aliphatic and aromatic components (up through alkylated-benzenes) were done in one run. Subambient temperature was needed for the oxygen-nitrogen separation, but they were easily resolved from each other and the other compounds present. The effects of different engine and exhaust system modifications on the level of compounds in the exhaust were tested. The concentrations of the emission gases varied considerably with changes in air/fuel ratio, coil voltage, use of catalytic converters and so forth. The results showed that the use of catalytic converter and a higher voltage coil tended to produce the most pronounced decreases in emissions of hydrocarbons and the catalytic converter produced the significant decrease in carbon monoxide concentrations. The results of the GSC analyses were compared to those of a commercial emission analyzer (i.e., sniffer). They showed similar trends and relative concentrations but somewhat different absolute concentrations. This may have been due to differences in the calibration of these methods.

  10. Gas-chromatographic measurement of carboxyhemoglobin in blood from mothers and newborns.

    PubMed

    Fogh-Andersen, N; Eriksen, P S; Grinsted, J; Siggaard-Andersen, O

    1988-01-01

    HbCO in blood sampled from 20 mothers and newborns immediately after birth was measured with a new, simple gas-chromatographic method for CO. The mean ratio of HbCO to total hemoglobin for 13 non-smoking mothers did not differ significantly from that for their infants (mean 0.38%, SD 0.26% vs 0.38%, SD 0.13%), but the HbCO ratio varied more in the mothers than in the infants (P less than 0.05). The infants of seven cigarette-smoking mothers, tobacco-abstinent for 7 h during labor, had higher HbCO ratios than their mothers (mean 1.88% vs 1.28%, P less than 0.05). The results are in harmony with the concept of equal affinities of fetal and adult hemoglobin for CO and a long time for passage of CO across the placenta.

  11. 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.

  12. The current practice in the application of chemometrics for correlation of sensory and gas chromatographic data.

    PubMed

    Seisonen, Sirli; Vene, Kristel; Koppel, Kadri

    2016-11-01

    A lot of research has been conducted in correlating the sensory properties of food with different analytical measurements in recent years. Various statistical methods have been used in order to get the most reliable results and to create prediction models with high statistical performance. The current review summarises the latest practices in the field of correlating attributes from sensory analysis with volatile data obtained by gas chromatographic analysis. The review includes the origin of the data, different pre-processing and variable selection methods and finally statistical methods of analysis and validation. Partial least squares regression analysis appears as the most commonly used statistical method in the area. The main shortcomings were identified in the steps of pre-processing, variable selection and also validation of models that have not gained enough attention. As the association between volatiles and sensory perception is often nonlinear, future studies should test the application of different nonlinear techniques.

  13. Determination and discrimination of biodiesel fuels by gas chromatographic and chemometric methods

    NASA Astrophysics Data System (ADS)

    Milina, R.; Mustafa, Z.; Bojilov, D.; Dagnon, S.; Moskovkina, M.

    2016-03-01

    Pattern recognition method (PRM) was applied to gas chromatographic (GC) data for a fatty acid methyl esters (FAME) composition of commercial and laboratory synthesized biodiesel fuels from vegetable oils including sunflower, rapeseed, corn and palm oils. Two GC quantitative methods to calculate individual fames were compared: Area % and internal standard. The both methods were applied for analysis of two certified reference materials. The statistical processing of the obtained results demonstrates the accuracy and precision of the two methods and allows them to be compared. For further chemometric investigations of biodiesel fuels by their FAME-profiles any of those methods can be used. PRM results of FAME profiles of samples from different vegetable oils show a successful recognition of biodiesels according to the feedstock. The information obtained can be used for selection of feedstock to produce biodiesels with certain properties, for assessing their interchangeability, for fuel spillage and remedial actions in the environment.

  14. Bio-sample preparation and gas chromatographic determination of benzodiazepines--a review.

    PubMed

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

    2013-08-01

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

  15. Thermal Modulation Methods To Improve the Efficiency of a Gas Chromatograph

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.; Dimandja, J. D.; Do, M. T.; Kaljurand, M.; Chang, Sherwood (Technical Monitor)

    1995-01-01

    Thermal modulation techniques can be used to improve capacity, resolution, and time of analysis of a gas chromatograph. Two of-the techniques developed in our laboratories include using a GC column to store a sample (sample storage system) and applying temperature programming directly onto the wall of a capillary column. The storage system developed allowed the continuous collection of a sample profile for about 3 hours and storing it for as long as 20 hours. Thereafter, the samples were eluted maintaining the individual characteristics of the components present in it. Moreover, temperature programming was done directly on a capillary column improving the time of analysis and resolution of a mixture containing light hydrocarbons.

  16. Linear solvation energy relationships as classifiers in non-target analysis - a gas chromatographic approach.

    PubMed

    Ulrich, Nadin; Mühlenberg, Jana; Retzbach, Heiko; Schüürmann, Gerrit; Brack, Werner

    2012-11-16

    Linear solvation energy relationships (LSERs) are applied as classifiers to predict the logarithmic retention factors logk from the structures of candidate compounds in non-target analysis. By comparison of the predicted value with the experimentally determined logk, progressive exclusion of candidates is done. The approach is based on the determination of stationary phase parameters to describe ten different gas chromatographic columns under four isothermal conditions. To demonstrate retention prediction and the application of the classifier model, twelve compounds with the molecular formula C(12)H(10)O(2) were selected, while experimental logk values were compared to the predicted values and exclusion of potential candidate compounds was performed. The analytical power of the approach was demonstrated on the basis of experimentally determined compound descriptors achieved from gas chromatographic measurements. The prediction got less accurate when calculated compound descriptors were employed. For the time being insufficient precision in estimating the descriptors limits the possibility to exclude candidate compounds in non-target analysis. It is expected that new approaches to estimate compound descriptors, will improve this situation. At present, the insufficient accuracy of descriptor estimates can be dealt with larger prognosis intervals. Furthermore, the combination of two stationary phases with corresponding retention prediction further advanced the exclusion of potential candidates. The most appropriate pair of stationary phases was selected by the application of four different orthogonal strategies. In addition, the classifier was applied for a validation set with different molecular composition, where column selection was considered on the basis of the differences in the compound descriptors of the corresponding candidate compounds.

  17. Convenient headspace gas chromatographic determination of azide in blood and plasma.

    PubMed

    Meatherall, Robert; Palatnick, Wes

    2009-10-01

    Azide in human blood and plasma samples was derivatized with propionic anhydride in a headspace vial without prior sample preparation. The reaction proceeds quickly at room temperature to form propionyl azide. A portion of the headspace was assayed by gas chromatography with a nitrogen-phosphorus detector. In the heated injector of the gas chromatograph, the propionyl azide undergoes thermal rearrangement, forming ethyl isocyanate, which is subsequently chromatographed and detected. Propionitrile was used as the internal standard. The method is linear to at least 20 microg/mL. Limit of quantitation was 0.04 microg/mL, and the within-run coefficient of variation was 5.6% at 1 microg/mL. There was no interference from cyanide. A fatality report in which blood and plasma azide concentrations from a 59-year-old man were monitored for 24 h following the ingestion of an unknown amount of sodium azide is presented. The patient became critically ill after his self-inflicted sodium azide ingestion. He was intubated and treated with vasopressors and aggressive supportive care, including extracorporeal membrane oxygenation therapy, in the intensive care facility but died from neurological brain damage secondary to anoxia. On admission, 1.4 h after ingestion, his azide level was 5.6 microg/mL (blood); shortly thereafter, it had risen to 13.7 microg/mL (plasma) and, subsequently, was projected to have been eliminated by 16.7 h. No azide was detected in the postmortem blood and vitreous humor.

  18. DETERMINATION OF PESTICIDES IN COMPOSITE DIETARY SAMPLES BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY IN THE SELECTED ION MONITORING MODE USING A TEMPERATURE PROGRAMMABLE LARGE VOLUME INJECTOR WITH PRE-SEPARATION COLUMN

    EPA Science Inventory

    Use of a temperature-programmable pre-separation column in the gas chromatographic injection port permits determination of a wide range of semi-volatile pesticides including organochlorines, organophosphates, triazines, and anilines in fatty composite dietary samples while reduci...

  19. How to compare separation selectivity of high-performance liquid chromatographic columns properly?

    PubMed

    Andrić, Filip; Héberger, Károly

    2017-03-10

    Comparison and selection of chromatographic columns is an important part of development as well as validation of analytical methods. Presently there is abundant number of methods for selection of the most similar and orthogonal columns, based on the application of limited number of test compounds as well as quantitative structure retention relationship models (QSRR), from among Snyder's hydrophobic-subtraction model (HSM) have been most extensively used. Chromatographic data of 67 compounds were evaluated using principal component analysis (PCA), hierarchical cluster analysis (HCA), non-parametric ranking methods as sum of ranking differences (SRD) and generalized pairwise correlation method (GPCM), both applied as a consensus driven comparison, and complemented by the comparison with one variable at a time (COVAT) approach. The aim was to compare the ability of the HSM approach and the approach based on primary retention data of test solutes (logk values) to differentiate among ten highly similar C18 columns. The ranking (clustering) pattern of chromatographic columns based on primary retention data and HSM parameters gave different results in all instances. Patterns based on retention coefficients were in accordance with expectations based on columns' physicochemical parameters, while HSM parameters provided a different clustering. Similarity indices calculated from the following dissimilarity measures: SRD, GPCM Fisher's conditional exact probability weighted (CEPW) scores; Euclidian, Manhattan, Chebyshev, and cosine distances; Pearson's, Spearman's, and Kendall's, correlation coefficients have been ranked by the consensus based SRD. Analysis of variance confirmed that the HSM model produced statistically significant increases of SRD values for the majority of similarity indices, i.e. HS transformation of original retention data yields significant loss of information, and finally results in lower performance of HSM methodology. The best similarity measures were

  20. Screening Brazilian C gasoline quality: application of the SIMCA chemometric method to gas chromatographic data.

    PubMed

    Flumignan, Danilo Luiz; Tininis, Aristeu G; Ferreira, Fabrício de O; de Oliveira, José Eduardo

    2007-07-09

    A total of 2400 samples of commercial Brazilian C gasoline were collected over a 6-month period from different gas stations in the São Paulo state, Brazil, and analysed with respect to 12 physicochemical parameters according to regulation 309 of the Brazilian Government Petroleum, Natural Gas and Biofuels Agency (ANP). The percentages (v/v) of hydrocarbons (olefins, aromatics and saturated) were also determined. Hierarchical cluster analysis (HCA) was employed to select 150 representative samples that exhibited least similarity on the basis of their physicochemical parameters and hydrocarbon compositions. The chromatographic profiles of the selected samples were measured by gas chromatography with flame ionisation detection and analysed using soft independent modelling of class analogy (SIMCA) method in order to create a classification scheme to identify conform gasolines according to ANP 309 regulation. Following the optimisation of the SIMCA algorithm, it was possible to classify correctly 96% of the commercial gasoline samples present in the training set of 100. In order to check the quality of the model, an external group of 50 gasoline samples (the prediction set) were analysed and the developed SIMCA model classified 94% of these correctly. The developed chemometric method is recommended for screening commercial gasoline quality and detection of potential adulteration.

  1. [Pyrolysis-gas chromatographic fingerprints with hierarchical cluster analysis for Dendrobium candidum Wall. ex Lindl].

    PubMed

    Wang, Lili; Wang, Cong; Pan, Zaifa; Sun, Fa

    2008-09-01

    The pyrogram fingerprints of Dendrobium candidum Wall. ex Lindl. from different regions were studied by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and compared with hierarchical cluster analysis. The effect of pyrolysis temperature on the fingerprint was examined by evolved gas analysis, and then 450 degrees C was selected as the optimized pyrolysis temperature. An amount of 0.4 mg of raw drug powder was pyrolysed in a vertical microfurnace pyrolyzer, and the products were directly introduced into a gas chromatograph equipped with a flame ionization detector (FID) and a fused-silica capillary column (30 m x 0.25 mm x 0.25 microm). The pyrogram fingerprints of 10 samples from different regions showed a high similarity and a good reproducibility with the relative standard deviations (RSDs) of the retention times less than 0.33% and the RSDs of the relative peak areas less than 4.8%. Therefore, each sample was characterized by the peak area of 31 peaks in each pyrogram and these peaks were employed for hierarchical cluster analysis. Furthermore, the discrimination of the sample from different regions was achieved by hierarchical cluster analysis via recognizing the 10 x 31 data matrix. Thus, the results proved it is a simple, rapid and accurate method suitable for the quality control of the traditional Chinese medicines.

  2. Comparison of nano and conventional liquid chromatographic methods for the separation of (+)-catechin-ethyl-malvidin-3-glucoside diastereoisomers.

    PubMed

    Kučera, Lukáš; Fanali, Salvatore; Aturki, Zeineb; Pospíšil, Tomáš; Bednář, Petr

    2016-01-08

    Nano-liquid chromatography and conventional HPLC were used for the separation of diastereomers of (+)-catechin-ethyl-malvidin-3-glucoside. Those bridged anthocyanin dyes were obtained by reaction of (+)-catechin with malvidin-3-glucoside in the presence of acetaldehyde. Both diastereomers were isolated with semipreparative chromatography and their structures were confirmed by nuclear magnetic resonance and mass spectrometry. In-laboratory prepared capillary columns packed with fully porous particles Chromosphere C18, dp=3μm, core-shell particles Kinetex C18, dp=2.6μm (100μm i.d.) and monolithic column Chromolith CapRod (100μm i.d.) were used for the separation of (+)-catechin, malvidin-3-glucoside and both diastereomers. Chromosphere C18 stationary phase provided the best chromatographic performance. Mobile phase containing water:acetonitrile (80:20) acidified with trifluoroacetic acid (0.1%, v/v/v) was used in an isocratic elution mode with a flow rate of 360nLmin(-1). Separation of studied compounds was achieved in less than 7min under optimized conditions. The nano-liquid chromatographic method and a conventional HPLC one using the same fully porous particles (Chromosphere C18, 3μm, 100mm×4.6mm) were compared providing higher separation efficiency with the first analytical method and similar selectivity. A better peak symmetry and higher resolution of the studied diastereomers was achieved by conventional chromatography. Nevertheless, nano-liquid chromatography appeared to be useful for the separation of complex anthocyanin dyes and can be utilized for their analysis in plant and food micro-samples. The developed method was used for analysis of red wine grape pomace.

  3. Gas purge microsyringe extraction for quantitative direct gas chromatographic-mass spectrometric analysis of volatile and semivolatile chemicals.

    PubMed

    Yang, Cui; Piao, Xiangfan; Qiu, Jinxue; Wang, Xiaoping; Ren, Chunyan; Li, Donghao

    2011-03-25

    Sample pretreatment before chromatographic analysis is the most time consuming and error prone part of analytical procedures, yet it is a key factor in the final success of the analysis. A quantitative and fast liquid phase microextraction technique termed as gas purge microsyringe extraction (GP-MSE) has been developed for simultaneous direct gas chromatography-mass spectrometry (GC-MS) analysis of volatile and semivolatile chemicals without cleanup process. Use of a gas flowing system, temperature control and a conventional microsyringe greatly increased the surface area of the liquid phase micro solvent, and led to quantitative recoveries of both volatile and semivolatile chemicals within short extraction time of only 2 min. Recoveries of polycyclic aromatic hydrocarbons (PAHs), organochlorine pesticides (OCPs) and alkylphenols (APs) determined were 85-107%, and reproducibility was between 2.8% and 8.5%. In particular, the technique shows high sensitivity for semivolatile chemicals which is difficult to achieve in other sample pretreatment techniques such as headspace-liquid phase microextraction. The variables affecting extraction efficiency such as gas flow rate, extraction time, extracting solvent type, temperature of sample and extracting solvent were investigated. Finally, the technique was evaluated to determine PAHs, APs and OCPs from plant and soil samples. The experimental results demonstrated that the technique is economic, sensitive to both volatile and semivolatile chemicals, is fast, simple to operate, and allows quantitative extraction. On-site monitoring of volatile and semivolatile chemicals is now possible using this technique due to the simplification and speed of sample treatment.

  4. Immobilized fluid membranes for gas separation

    SciTech Connect

    Liu, Wei; Canfield, Nathan L; Zhang, Jian; Li, Xiaohong Shari; Zhang, Jiguang

    2014-03-18

    Provided herein are immobilized liquid membranes for gas separation, methods of preparing such membranes and uses thereof. In one example, the immobilized membrane includes a porous metallic host matrix and an immobilized liquid fluid (such as a silicone oil) that is immobilized within one or more pores included within the porous metallic host matrix. The immobilized liquid membrane is capable of selective permeation of one type of molecule (such as oxygen) over another type of molecule (such as water). In some examples, the selective membrane is incorporated into a device to supply oxygen from ambient air to the device for electrochemical reactions, and at the same time, to block water penetration and electrolyte loss from the device.

  5. Multidimensional gas chromatography beyond simple volatiles separation.

    PubMed

    Chin, Sung-Tong; Marriott, Philip J

    2014-08-18

    Multidimensional separation in gas chromatography (MDGC) plays an important role in chemical analysis. This review presents selected literature on MDGC development and examples of the range of functionality reported for MDGC methods over the past 2 decades. With the most obvious advantage of providing much greater capacity for resolving constituents of a sample, MDGC extends analytical efficiency to a more substantial molecular coverage, combined with operational flexibility. But by judicious choice of implementation method, important chemical information relating to the sample, its components, potentially physico-chemical properties, and improved capacity for absolute identification may be realised. Sample-to-sample comparison is improved, and sample characterisation is facilitated especially when MDGC is combined with the informing power of modern mass spectrometry. Innovative MDGC arrangements allow high resolution coupled with spectroscopy and alternative bioassays, and delivers molecular elucidation in ways that are beyond just simple analysis of volatiles.

  6. TUNABLE COMPOSITE MEMBRANES FOR GAS SEPARATIONS

    SciTech Connect

    J.P. Ferraris; K.J. Balkus, Jr.; I.H. Musselman

    1999-01-01

    Poly 2-(3-thienyl)ethylacetate (PAET) was synthesized and solution cast as thin films to form dense membranes. These membranes are mechanically robust and are redox active, holding out promise as gas separation materials. The permeability properties of PAET membranes were evaluated for N{sub 2} (0.048 {+-} 0.008 Barrers), O{sub 2} (0.24 {+-} 0.02 Barrers), CH{sub 4} (0.081 {+-} 0.005 Barrers), and CO{sub 2} (1.4 {+-} 0.1 Barrers). The corresponding selectivity values ({alpha}) were: O{sub 2}/N{sub 2} = 5.1, CO{sub 2}/N{sub 2} = 29, and CO{sub 2}/CH{sub 4} = 18.

  7. Results from the Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe

    NASA Technical Reports Server (NTRS)

    Niemann, H.; Atreya, S.; Demick-Montelara, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Owen, T.; Raaen, E.; Way, S.

    2006-01-01

    The Gas Chromatograph Mass Spectrometer was one of six instruments on the Cassini-Huygens Probe mission to Titan. The GCMS measured in situ the chemical composition of the atmosphere during the probe descent and served as the detector for the pyrolization products for the Aerosol Collector Pyrolyser (ACP) experiment to determine the composition of the aerosol particles. The GCMS collected data from an altitude of 146 km to ground impact. The Probe and the GCMS survived impact and collected data for 1 hour and 9 minutes on the surface. Mass spectra were collected during descent and on the ground over a range of m/z from 2 to 141. The major constituents of the lower atmosphere were confirmed to be N2 and CH4. The methane mole fraction was uniform in the stratosphere. It increased below the tropopause, at about 32 km altitude, monotonically toward the surface, reaching a plateau at about 8 km at a level near saturation. After surface impact a steep increase of the methane signal was observed, suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. The measured mole fraction of Ar-40 is 4.3x10(exp -5) and of Ar-36 is 2.8x10(exp -7). The other primordial noble gases were below 10(exp -8) mole fraction. The isotope ratios of C-12/C-13 determined from methane measurements are 82.3 and of N-14/N-15 determined from molecular nitrogen are 183. The D/H isotope ratio determined from the H2 and HD measurements is 2.3x10(exp -4). Carbon dioxide, methane, acetylene and cyanogen were detected evaporating from the surface in addition to methane. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns, a chemical scrubber and a hydrocarbon enrichment cell. The GCMS gas inlet was heated to prevent condensation, and to evaporate volatiles from the

  8. Results from the Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe

    NASA Technical Reports Server (NTRS)

    Niemann, Hasso; Atreya, S.; Demick-Monelara, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Owen, T.; Raaen, E.; Way, S.

    2006-01-01

    The Gas Chromatograph Mass Spectrometer was one of six instruments on the Cassini-Huygens Probe mission to Titan. The GCMS measured in situ the chemical composition of the atmosphere during the probe descent and served as the detector for the pyrolization products for the Aerosol Collector Pyrolyser (ACP) experiment to determine the composition of the aerosol particles. The GCMS collected data from an altitude of 146 km to ground impact. The Probe and the GCMS survived impact and collected data for 1 hour and 9 minutes on the surface. Mass spectra were collected during descent and on the ground over a range of mlz from 2 to 141. The major constituents of the lower atmosphere were confirmed to be N2 and CH4. The methane mole fraction was uniform in the stratosphere. It increased below the tropopause, at about 32 km altitude, monotonically toward the surface, reaching a plateau at about 8 km at a level near saturation. After surface impact a steep increase of the methane signal was observed, suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. The measured mole fraction of Ar-40 is 4.3x10(exp -5) and of Ar-36 is 2.8x10(exp -7). The other primordial noble gases were below 10(exp -8) mole fraction. The isotope ratios of C-12/C-13 determined from methane measurements are 82.3 and of N-14/N-15 determined from molecular nitrogen are 183. The D/H isotope ratio determined from the H2 and HD measurements is 2.3x10(exp -4). Carbon dioxide, ethane, acetylene and cyanogen were detected evaporating from the surface in addition to methane. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns, a chemical scrubber and a hydrocarbon enrichment cell. The GCMS gas inlet was heated to prevent condensation, and to evaporate volatiles from the

  9. A Gas Chromatographic Method for the Determination of Aldose and Uronic Acid Constituents of Plant Cell Wall Polysaccharides 1

    PubMed Central

    Jones, Thomas M.; Albersheim, Peter

    1972-01-01

    A major problem in determining the composition of plant cell wall polysaccharides has been the lack of a suitable method for accurately determining the amounts of galacturonic and glucuronic acids in such polymers. A gas chromatographic method for aldose analysis has been extended to include uronic acids. Cell wall polysaccharides are depolymerized by acid hydrolysis followed by treatment with a mixture of fungal polysaccharide-degrading enzymes. The aldoses and uronic acids released by this treatment are then reduced with NaBH4 to alditols and aldonic acids, respectively. The aldonic acids are separated from the alditols with Dowex-1 (acetate form) ion exchange resin, which binds the aldonic acids. The alditols, which do not bind, are washed from the resin and then acetylated with acetic anhydride to form the alditol acetate derivatives. The aldonic acids are eluted from the resin with HCl. After the resin has been removed, the HCl solution of the aldonic acids is evaporated to dryness, converting the aldonic acids to aldonolactones. The aldonolactones are reduced with NaBH4 to the corresponding alditols, dried and acetylated. The resulting alditol acetate mixtures produced from the aldoses and those from the uronic acids are analyzed separately by gas chromatography. This technique has been used to determine the changes in composition of Red Kidney bean (Phaseolus vulgaris) hypocotyl cell walls during growth, and to compare the cell wall polysaccharide compositions of several parts of bean plants. Galacturonic acid is found to be a major component of all the cell wall polysaccharides examined. PMID:16658086

  10. Post-synthetic modification of MIL-101(Cr) with pyridine for high-performance liquid chromatographic separation of tocopherols.

    PubMed

    Yang, Fang; Yang, Cheng-Xiong; Yan, Xiu-Ping

    2015-05-01

    Effective separation of tocopherols is challenging and significant due to their structural similarity and important biological role. Here we report the post-synthetic modification of metal-organic framework (MOF) MIL-101(Cr) with pyridine for high-performance liquid chromatographic (HPLC) separation of tocopherols. Baseline separation of four tocopherols was achieved on a pyridine-grafted MIL-101(Cr) packed column within 10 min using hexane/isopropanol (96:4, v/v) as the mobile phase at a flow rate of 0.5 mL min(-1). The pyridine-grafted MIL-101(Cr) packed column gave high column efficiency (85,000 plates m(-1) for δ-tocopherol) and good precision (0.2-0.3% for retention time, 1.8-3.4% for peak area, 2.6-2.7% for peak height), and also offered much better performance than unmodified MIL-101(Cr) and commercial amino-bonded silica packed column for HPLC separation of tocopherols. The results not only show the promising application of pyridine-grafted MIL-101(Cr) as a novel stationary phase for HPLC separation of tocopherols, but also reveal a facile post-modification of MOFs to expand the application of MOFs in separation sciences.

  11. 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.

  12. Countercurrent Chromatographic Separation of Proteins Using an Eccentric Coiled Column with Synchronous and Nonsynchronous Type-J Planetary Motions

    PubMed Central

    SHINOMIYA, Kazufusa; YOSHIDA, Kazunori; TOKURA, Koji; TSUKIDATE, Etsuhiro; YANAGIDAIRA, Kazuhiro; ITO, Yoichiro

    2015-01-01

    Protein separation was performed using the high-speed counter-current chromatograph (HSCCC) at both synchronous and nonsynchronous type-J planetary motions. The partition efficiency was evaluated with two different column configurations, eccentric coil and toroidal coil, on the separation of a set of stable protein samples including cytochrome C, myoglobin and lysozyme with a polymer phase system composed of 12.5% (w/w) polyethylene glycol 1000 and 12.5% (w/w) dibasic potassium phosphate. Better peak resolution was obtained by the eccentric coil than by the toroidal coil using either lower or upper phase as the mobile phase. The peak resolution was further improved using the eccentric coil by the nonsynchronous type-J planetary motion with the combination of 1066 rpm of column rotation and 1000 rpm of revolution. PMID:25765276

  13. Liquid chromatographic enantiomer separation of 1-naphthylamides of chiral acids using several amylose- and cellulose-derived chiral stationary phases.

    PubMed

    Islam, Md F; Adhikari, Suraj; Paik, Man-Jeong; Lee, Wonjae

    2017-03-01

    The liquid chromatographic enantiomer separation of various chiral acids as 1-naphthylamides was performed using several chiral stationary phases (CSPs). The CSPs used in this study were six covalently bonded and four coated type CSPs derived from amylose and cellulose derivatives as chiral selectors. The degree of enantioseparation is affected by the structure of chiral acids and the CSPs used, which have different chiral selectors and types of immobilization. For the enantiomer resolution of chiral acids as 1-naphthylamide derivatives, the performance of the coated type Lux Cellulose-1 was superior to those of the other CSPs, except for 2-aryloxypropionic acid derivatives. Owing to the strong ultraviolet absorbance of the 1-naphthyl group, the convenient analytical method developed and validated in this study could be expected to be very useful for the enantiomer separation of various chiral acids as 1-naphthylamide derivatives using polysaccharide-derived CSPs.

  14. Quantitative structure-retention relationships of polycyclic aromatic hydrocarbons gas-chromatographic retention indices.

    PubMed

    Drosos, Juan Carlos; Viola-Rhenals, Maricela; Vivas-Reyes, Ricardo

    2010-06-25

    Polycyclic aromatic compounds (PAHs) are of concern in environmental chemistry and toxicology. In the present work, a QSRR study was performed for 209 previously reported PAHs using quantum mechanics and other sources descriptors estimated by different approaches. The B3LYP/6-31G* level of theory was used for geometrical optimization and quantum mechanics related variables. A good linear relationship between gas-chromatographic retention index and electronic or topologic descriptors was found by stepwise linear regression analysis. The molecular polarizability (alpha) and the second order molecular connectivity Kier and Hall index ((2)chi) showed evidence of significant correlation with retention index by means of important squared coefficient of determination, (R(2)), values (R(2)=0.950 and 0.962, respectively). A one variable QSRR model is presented for each descriptor and both models demonstrates a significant predictive capacity established using the leave-many-out LMO (excluding 25% of rows) cross validation method's q(2) cross-validation coefficients q(2)(CV-LMO25%), (obtained q(2)(CV-LMO25%) 0.947 and 0.960, respectively). Furthermore, the physicochemical interpretation of selected descriptors allowed detailed explanation of the source of the observed statistical correlation. The model analysis suggests that only one descriptor is sufficient to establish a consistent retention index-structure relationship. Moderate or non-significant improve was observed for quantitative results or statistical validation parameters when introducing more terms in predictive equation. The one parameter QSRR proposed model offers a consistent scheme to predict chromatographic properties of PAHs compounds.

  15. Establishing high temperature gas chromatographic profiles of non-polar metabolites for quality assessment of African traditional herbal medicinal products.

    PubMed

    Bony, Nicaise F; Libong, Danielle; Solgadi, Audrey; Bleton, Jean; Champy, Pierre; Malan, Anglade K; Chaminade, Pierre

    2014-01-01

    The quality assessment of African traditional herbal medicinal products is a difficult challenge since they are complex mixtures of several herbal drug or herbal drug preparations. The plant source is also often unknown and/or highly variable. Plant metabolites chromatographic profiling is therefore an important tool for quality control of such herbal products. The objective of this work is to propose a protocol for sample preparation and gas chromatographic profiling of non-polar metabolites for quality control of African traditional herbal medicinal products. The methodology is based on the chemometric assessment of chromatographic profiles of non-polar metabolites issued from several batches of leaves of Combretum micranthum and Mitracarpus scaber by high temperature gas chromatography coupled to mass spectrometry, performed on extracts obtained in refluxed dichloromethane, after removal of chlorophyll pigments. The method using high temperature gas chromatography after dichloromethane extraction allows detection of most non-polar bioactive and non-bioactive metabolites already identified in leaves of both species. Chemometric data analysis using Principal Component Analysis and Partial Least Squares after Orthogonal Signal Correction applied to chromatographic profiles of leaves of Combretum micranthum and Mitracarpus scaber showed slight batch to batch differences, and allowed clear differentiation of the two herbal extracts.

  16. Autonomous gas chromatograph system for Thermal Enhanced Vapor Extraction System (TEVES) proof of concept demonstration

    SciTech Connect

    Peter, F.J.; Laguna, G.R.

    1996-09-01

    An autonomous gas chromatograph system was designed and built to support the Thermal Enhanced Vapor Extraction System (TEVES) demonstration. TEVES is a remediation demonstration that seeks to enhance an existing technology (vacuum extraction) by adding a new technology (soil heating). A pilot scale unit was set up at one of the organic waste disposal pits at the Sandia National Laboratories Chemical Waste Landfill (CWL) in Tech Area 3. The responsibility for engineering a major part of the process instrumentation for TEVES belonged to the Manufacturing Control Subsystems Department. The primary mission of the one-of-a-kind hardware/software system is to perform on-site gas sampling and analysis to quantify a variety of volatile organic compounds (VOCs) from various sources during TEVES operations. The secondary mission is to monitor a variety of TEVES process physical parameters such as extraction manifold temperature, pressure, humidity, and flow rate, and various subsurface pressures. The system began operation in September 1994 and was still in use on follow-on projects when this report was published.

  17. Gas chromatographic and mass spectrometric analysis of polychlorinated biphenyls in human placenta and cord blood

    SciTech Connect

    Ando, M.; Saito, H.; Wakisaka, I.

    1986-10-01

    Gas chromatographic and mass spectrometric analyses of polychlorinated biphenyls (PCBs) in placenta, maternal blood, cord blood, and milk were carried out. Trichlorobiphenyl, tetrachlorobiphenyl, pentachlorobiphenyls, and hexachlorobiphenyls were identified by the mass chromatogram and the mass spectra. Some minor peaks of PCBs were identified by gas chromatography. The relationship between the PCB concentration in placenta and that in milk is different in each PCB congener. The higher the chlorine content of the PCB congener, the more significant the correlation. No significant but a low negative correlation exists between the concentration of some PCB congeners in the placenta and that in cord blood. On the other hand, a significant linear correlation exists between the concentration of hexachlorobenzene in the placenta and that in cord blood. The transplacental transport of each PCB congener varied depending upon its chemical nature. Trichlorobiphenyl and tetrachlorobiphenyl were more transferable than hexachlorobiphenyls. The results show that the placenta and cord blood are useful human samples to analyze the body burden of environmental pollutants and to estimate their transfer from mother to fetus.

  18. A specific gas chromatographic detector for carbonyl compounds, based on polarography.

    PubMed

    Fleet, B; Risby, T H

    1969-07-01

    The evaluation of a specific gas Chromatographie detector for carbonyl compounds is described. This is based on the polarographic reduction of the Girard T hydrazone derivative which is formed when the carbonyl compound is absorbed in a buffered supporting electrolyte containing the carbonyl reagent. The detector was used to monitor the separation of a homologous series of alkanals.

  19. Gas chromatographic/thermal energy analyzer method for N-nitrosodibenzylamine in hams processed in elastic rubber netting.

    PubMed

    Pensabene, J W; Fiddler, W

    1994-01-01

    We previously described a solid-phase extraction (SPE) procedure for determining volatile nitrosamines in hams processed in elastic rubber nettings. This same procedure was found to successfully isolate N-nitrosodibenzylamine (NDBzA), a semivolatile nitrosamine. This nitrosamine may form as a result of the reformulated rubber now used in nettings. Reformulation became necessary because of the reported presence of N-nitrosodibutylamine in both the old nettings and on the exterior portion of commercial hams. After SPE, NDBzA was quantitated by using a gas chromatographic (GC) system interfaced to a nitrosamine-specific chemiluminescence detector [thermal energy analyzer (TEA)]. The GC system was equipped with a heated interface external to the TEA furnace to facilitate quantitation of NDBzA. With separation on a packed column, the method can be used to analyze 10 volatile nitrosamines and NDBzA. Repeatability of the method for NDBzA was found to be 2.1 ppb, and the coefficient of variation (CV) was 10.6%. Analysis of 18 commercial hams from 9 different producers, purchased from local retailers, indicated that 12 were positive for NDBzA (range, 2.6-128.5 ppb). NDBzA was confirmed by GC/mass spectrometry.

  20. Improving accuracy and precision of ice core δD(CH4) analyses using methane pre-pyrolysis and hydrogen post-pyrolysis trapping and subsequent chromatographic separation

    NASA Astrophysics Data System (ADS)

    Bock, M.; Schmitt, J.; Beck, J.; Schneider, R.; Fischer, H.

    2014-07-01

    Firn and polar ice cores offer the only direct palaeoatmospheric archive. Analyses of past greenhouse gas concentrations and their isotopic compositions in air bubbles in the ice can help to constrain changes in global biogeochemical cycles in the past. For the analysis of the hydrogen isotopic composition of methane (δD(CH4) or δ2H(CH4)) 0.5 to 1.5 kg of ice was hitherto used. Here we present a method to improve precision and reduce the sample amount for δD(CH4) measurements in (ice core) air. Pre-concentrated methane is focused in front of a high temperature oven (pre-pyrolysis trapping), and molecular hydrogen formed by pyrolysis is trapped afterwards (post-pyrolysis trapping), both on a carbon-PLOT capillary at -196 °C. Argon, oxygen, nitrogen, carbon monoxide, unpyrolysed methane and krypton are trapped together with H2 and must be separated using a second short, cooled chromatographic column to ensure accurate results. Pre- and post-pyrolysis trapping largely removes the isotopic fractionation induced during chromatographic separation and results in a narrow peak in the mass spectrometer. Air standards can be measured with a precision better than 1‰. For polar ice samples from glacial periods, we estimate a precision of 2.3‰ for 350 g of ice (or roughly 30 mL - at standard temperature and pressure (STP) - of air) with 350 ppb of methane. This corresponds to recent tropospheric air samples (about 1900 ppb CH4) of about 6 mL (STP) or about 500 pmol of pure CH4.

  1. Improving accuracy and precision of ice core δD (CH4) analyses using methane pre- and hydrogen post-pyrolysis trapping and subsequent chromatographic separation

    NASA Astrophysics Data System (ADS)

    Bock, M.; Schmitt, J.; Beck, J.; Schneider, R.; Fischer, H.

    2013-12-01

    Firn and polar ice cores offer the only direct paleoatmospheric archive. Analyses of past greenhouse gas concentrations and their isotopic compositions in air bubbles in the ice can help to constrain changes in global biogeochemical cycles in the past. For the analysis of the hydrogen isotopic composition of methane (δD (CH4)) 0.5 to 1.5 kg of ice was previously necessary to achieve the required precision. Here we present a method to improve precision and reduce the sample amount for δD (CH4) measurements on (ice core) air. Pre-concentrated methane is focused before a high temperature oven (pre pyrolysis trapping), and molecular hydrogen formed by pyrolysis is trapped afterwards (post pyrolysis trapping), both on a carbon-PLOT capillary at -196 °C. A small amount of methane and krypton are trapped together with H2 and must be separated using a short second chromatographic column to ensure accurate results. Pre and post pyrolysis trapping largely removes the isotopic fractionation induced during chromatographic separation and results in a narrow peak in the mass spectrometer. Air standards can be measured with a precision better than 1‰. For polar ice samples from glacial periods we estimate a precision of 2.2‰ for 350 g of ice (or roughly 30 mL (at standard temperature and pressure (STP)) of air) with 350 ppb of methane. This corresponds to recent tropospheric air samples (about 1900 ppb CH4) of about 6 mL (STP) or about 500 pmol of pure CH4.

  2. Investigation of porous polymer gas chromatographic packings for atmospheric analysis of extraterrestrial bodies

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.

    1986-01-01

    Measurement of the permanent gases in the atmospheres of mission targets is a major objective. A 16 meter long Porapak N column was used on the Venus probe and required a rather high carrier gas flow rate. The researchers have, therefore, surveyed commercial porous polymer types which had some ability to resolve nitrogen, oxygen, argon and carbon monoxide gases. Porapaks N and Q appeared superior to most. Batch to batch variation, however, was quite wide, so the researchers learned how to synthesize porous polymer and investigated some of the factors affecting the separations. A polymer was synthesized which was superior to all commercial products and allowed at least a 50% reduction in length and flow rate of carrier gas. Similar studies were made concerning the separation of hydrocarbons and new porous polymers have been synthesized which represent significant improvements in time of analysis, column, and carrier gas flow rate.

  3. Statistical learning of peptide retention behavior in chromatographic separations: a new kernel-based approach for computational proteomics

    PubMed Central

    Pfeifer, Nico; Leinenbach, Andreas; Huber, Christian G; Kohlbacher, Oliver

    2007-01-01

    Background High-throughput peptide and protein identification technologies have benefited tremendously from strategies based on tandem mass spectrometry (MS/MS) in combination with database searching algorithms. A major problem with existing methods lies within the significant number of false positive and false negative annotations. So far, standard algorithms for protein identification do not use the information gained from separation processes usually involved in peptide analysis, such as retention time information, which are readily available from chromatographic separation of the sample. Identification can thus be improved by comparing measured retention times to predicted retention times. Current prediction models are derived from a set of measured test analytes but they usually require large amounts of training data. Results We introduce a new kernel function which can be applied in combination with support vector machines to a wide range of computational proteomics problems. We show the performance of this new approach by applying it to the prediction of peptide adsorption/elution behavior in strong anion-exchange solid-phase extraction (SAX-SPE) and ion-pair reversed-phase high-performance liquid chromatography (IP-RP-HPLC). Furthermore, the predicted retention times are used to improve spectrum identifications by a p-value-based filtering approach. The approach was tested on a number of different datasets and shows excellent performance while requiring only very small training sets (about 40 peptides instead of thousands). Using the retention time predictor in our retention time filter improves the fraction of correctly identified peptide mass spectra significantly. Conclusion The proposed kernel function is well-suited for the prediction of chromatographic separation in computational proteomics and requires only a limited amount of training data. The performance of this new method is demonstrated by applying it to peptide retention time prediction in IP

  4. Robust isocratic liquid chromatographic separation of functional poly(methyl methacrylate).

    PubMed

    Jiang, Xulin; Lima, Vincent; Schoenmakers, Peter J

    2003-11-07

    The separation of telechelic poly(methyl methacrylate) (PMMA) prepolymers based on the number of end-groups under critical liquid chromatography (LC) conditions has been studied using a bare-silica column, which can interact with polar functional groups. The critical solvent compositions for non-functional, mono-functional and bi-functional PMMAs were determined in normal-phase LC using mixtures of acetonitrile and dichloromethane (DCM) of varying composition as the mobile phase. The telechelic prepolymers were successfully separated according to hydroxyl (OH) functionality (with zero, one, or two OH groups, respectively) under the critical conditions, in which fast (5 min), base-line separations were obtained independent of molecular weight. Changing the column temperature, flow rate, and mobile-phase composition within a certain range did not affect the functionality separation. Therefore this isocratic LC separation method is quite robust. Evaporative light-scattering detector (ELSD) calibration curves were used for the quantitative analysis of functional PMMA prepolymers.

  5. Comprehensive multi-dimensional liquid chromatographic separation in biomedical and pharmaceutical analysis: a review.

    PubMed

    Dixon, Steven P; Pitfield, Ian D; Perrett, David

    2006-01-01

    'Multi-dimensional' liquid separations have a history almost as long as chromatography. In multi-dimensional chromatography the sample is subjected to more than one separation mechanism; each mechanism is considered an independent separation dimension. The separations can be carried out either offline via fraction collection, or directly coupled online. Early multi-dimensional separations using combinations of paper chromatography, electrophoresis and gels, in both planar and columnar modes are reviewed. Developments in HPLC have increased the number of measurable analytes in ever more complex matrices, and this has led to the concept of 'global metabolite profiling'. This review focuses on the theory and practice of modern 'comprehensive' multi-dimensional liquid chromatography when applied to biomedical and pharmaceutical analysis.

  6. Gas chromatographic methods for determination of gamma-BHC in technical emulsifiable concentrates and water-dispersible powder formulations and in lindane shampoo and lotion: collaborative study.

    PubMed

    Miles, J W; Mount, D L; Beckmann, T J; Carrigan, S K; Galoux, I M; Hitos, P; Hodge, M C; Kissler, K; Martijn, A; Sanchez-Rasero, F

    1984-01-01

    Although the gas chromatographic separation of the isomers of BHC was demonstrated two decades ago, the present AOAC method of analysis of BHC for gamma-isomer (lindane) content is based on a separation carried out on a liquid chromatographic partition column. A method of analysis has been developed that uses an OV-210 column for separation of the gamma-isomer from the other isomers and impurities in technical BHC. Di-n-propyl phthalate was chosen as an internal standard. The same system allows quantitation of lindane in lotion and shampoo after these products are extracted with ethyl acetate-isooctane (1 + 4). The analytical methods were subjected to a collaborative trial with 10 laboratories. The coefficient of variation for technical BHC was 2.83%. For the water-dispersible powder and emulsifiable concentrate, the coefficients of variation were 2.89% and 4.62%, respectively. Coefficients of variation for 1% lindane lotion and shampoo were 4.36% and 11.92%, respectively. The method has been adopted official first action.

  7. Single-walled carbon nanotube-based polymer monoliths for the enantioselective nano-liquid chromatographic separation of racemic pharmaceuticals.

    PubMed

    Ahmed, Marwa; Yajadda, Mir Massoud Aghili; Han, Zhao Jun; Su, Dawei; Wang, Guoxiu; Ostrikov, Kostya Ken; Ghanem, Ashraf

    2014-09-19

    Single-walled carbon nanotubes were encapsulated into different polymer-based monolithic backbones. The polymer monoliths were prepared via the copolymerization of 20% monomers, glycidyl methacrylate, 20% ethylene glycol dimethacrylate and 60% porogens (36% 1-propanol, 18% 1,4-butanediol) or 16.4% monomers (16% butyl methacrylate, 0.4% sulfopropyl methacrylate), 23.6% ethylene glycol dimethacrylate and 60% porogens (36% 1-propanol, 18% 1,4-butanediol) along with 6% single-walled carbon nanotubes aqueous suspension. The effect of single-walled carbon nanotubes on the chiral separation of twelve classes of pharmaceutical racemates namely; α- and β-blockers, antiinflammatory drugs, antifungal drugs, dopamine antagonists, norepinephrine-dopamine reuptake inhibitors, catecholamines, sedative hypnotics, diuretics, antihistaminics, anticancer drugs and antiarrhythmic drugs was investigated. The enantioselective separation was carried out under multimodal elution to explore the chiral recognition capabilities of single-walled carbon nanotubes using reversed phase, polar organic and normal phase chromatographic conditions using nano-liquid chromatography. Baseline separation was achieved for celiprolol, chlorpheniramine, etozoline, nomifensine and sulconazole under multimodal elution conditions. Satisfactory repeatability was achieved through run-to-run, column-to-column and batch-to-batch investigations. Our findings demonstrate that single-walled carbon nanotubes represent a promising stationary phase for the chiral separation and may open the field for a new class of chiral selectors.

  8. Characterization of thermal desorption with the Deans-switch technique in gas chromatographic analysis of volatile organic compounds.

    PubMed

    Ou-Yang, Chang-Feng; Huang, Ying-Xue; Huang, Ting-Jyun; Chen, Yong-Shen; Wang, Chieh-Heng; Wang, Jia-Lin

    2016-09-02

    This study presents a novel application based on the Deans-switch cutting technique to characterize the thermal-desorption (TD) properties for gas chromatographic (GC) analysis of ambient volatile organic compounds (VOCs). Flash-heating of the sorbent bed at high temperatures to desorb trapped VOCs to GC may easily produce severe asymmetric or tailing GC peaks affecting resolution and sensitivity if care is not taken to optimize the TD conditions. The TD peak without GC separation was first examined for the quality of the TD peak by analyzing a standard gas mixture from C2 to C12 at ppb level. The Deans switch was later applied in two different stages. First, it was used to cut the trailing tail of the TD peak, which, although significantly improved the GC peak symmetry, led to more loss of the higher boiling compounds than the low boiling ones, thus suggesting compound discrimination. Subsequently, the Deans switch was used to dissect the TD peak into six 30s slices in series, and an uneven distribution in composition between the slices were found. A progressive decrease in low boiling compounds and increase in higher boiling ones across the slices indicated severe inhomogeneity in the TD profile. This finding provided a clear evidence to answer the discrimination problem found with the tail cutting approach to improve peak symmetry. Through the use of the innovated slicing method based on the Deans-switch cutting technique, optimization of TD injection for highly resolved, symmetric and non-discriminated GC peaks can now be more quantitatively assessed and guided.

  9. Potential for Measurement of Trace Volatile Organic Compounds in Closed Environments Using Gas Chromatograph/Differential Mobility Spectrometer

    NASA Technical Reports Server (NTRS)

    Limero, Thomas; Cheng, Patti

    2007-01-01

    For nearly 3.5 years, the Volatile Organic Analyzer (VOA) has routinely analyzed the International Space Station (ISS) atmosphere for a target list of approximately 20 volatile organic compounds (VOCs). Additionally, an early prototype of the VOA collected data aboard submarines in two separate trials. Comparison of the data collected on ISS and submarines showed a surprising similarity in the atmospheres of the two environments. Furthermore, in both cases it was demonstrated that the VOA data can detect hardware issues unrelated to crew health. Finally, it was also clear in both operations that the VOA s size and resource consumption were major disadvantages that would restrict its use in the future. The VOA showed the value of measuring VOCs in closed environments, but it had to be shrunk if it was to be considered for future operations in these environments that are characterized by cramped spaces and limited resources. The Sionex Microanalyzer is a fraction of the VOA s size and this instrument seems capable of maintaining or improving upon the analytical performance of the VOA. The two design improvements that led to a smaller, less complex instrument are the Microanalyzer s use of recirculated air as the gas chromatograph s carrier gas and a micromachined detector. Although the VOA s ion mobility spectrometer and the Microanalyzer s differential mobility spectrometer (DMS) are related detector technologies, the DMS was more amenable to micromachining. This paper will present data from the initial assessment of the Microanalyzer. The instrument was challenged with mixtures that simulated the VOCs typically detected in closed-environment atmospheres.

  10. Design of chiral monochloro-s-triazine reagents for the liquid chromatographic separation of amino acid enantiomers.

    PubMed

    Brückner, H; Wachsmann, M

    2003-05-23

    A series of chiral derivatizing reagents (CDRs) was synthesized by nucleophilic replacement of one chlorine atom in cyanuric chloride (2,4,6-trichloro-1,3,5-triazine; s-triazine) by alkoxy (methoxy, butoxy, 1,1,1-trifluoroethoxy) or aryloxy groups (phenoxy, nitrophenoxy, phenylphenoxy, 4-methylcoumaryloxy), and displacement of a second chlorine by L-alanine amide, L-phenylalanine amide, L-proline tert.-butyl ester, or Boc-L-lysine tert.-butyl ester. Further, CDRs were investigated in which two chlorine atoms in cyanuric chloride were substituted consecutively by L-valine amide and L-phenylalanine amide. The resulting CDRs having a remaining reactive chlorine were tested for their capability of derivatizing DL-amino acids followed by liquid chromatographic separation of the resulting diastereomers.

  11. Device for separation of vortex gas-dynamic energy

    NASA Astrophysics Data System (ADS)

    Leontiev, A. I.; Burtsev, S. A.

    2015-10-01

    A device for separation of vortex gas-dynamic energy, which combines the mechanism of separation of vortex energy used in the Ranque-Hilsch tubes and the mechanism of separation of gas-dynamic energy, is proposed for supersonic flows. A method of calculation of this device is developed. A comparison is made that showed that, when working with natural gas, the cooling depth of half of the mass flow rate proves to be 1.3 times higher than that for the vortex tube and three times higher than that for the device for separation of the gas-dynamic energy.

  12. Gas chromatographic-mass spectrometric assay for 6-hydroxymelatonin sulfate and 6-hydroxymelatonin glucuronide in urine

    SciTech Connect

    Francis, P.L.; Leone, A.M.; Young, I.M.; Stovell, P.; Silman, R.E.

    1987-04-01

    Circulating melatonin is hydroxylated to 6-hydroxymelatonin and excreted in urine as the sulfate and glucuronide conjugates. We extracted these two compounds from urine by using octadecylsilane-bonded silica cartridges to eliminate most of the urea and electrolytes, and silica cartridges to separate the sulfate and glucuronide conjugates. After hydrolyzing the separated conjugates enzymically, we determined the free hydroxymelatonin by gas chromatography-mass spectrometry. Though recoveries were low and variable, we were able to quantify the analyte in the original sample by adding deuterated sulfate and glucuronide conjugates to the urines before extraction.

  13. Application of a Modified Gas Chromatograph to Analyze Space Experiment Combustion Gases on Space Shuttle Mission STS-94

    NASA Technical Reports Server (NTRS)

    Coho, William K.; Weiland, Karen J.; VanZandt, David M.

    1998-01-01

    A space experiment designed to study the behavior of combustion without the gravitational effects of buoyancy was launched aboard the Space Shuttle Columbia on July 1, 1997. The space experiment, designated as Combustion Module-1 (CM-1), was one of several manifested on the Microgravity Sciences Laboratory - 1 (MSL-1) mission. The launch, designated STS-94, had the Spacelab Module as the payload, in which the MSL-1 experiments were conducted by the Shuttle crewmembers. CM-1 was designed to accommodate two different combustion experiments during MSL-1. One experiment, the Structure of Flame Balls at Low Lewis-number experiment (SOFBALL), required gas chromatography analysis to verify the composition of the known, premixed gases prior to combustion, and to determine the remaining reactant and the products resulting from the combustion process in microgravity. A commercial, off-the-shelf, dual-channel micro gas chromatograph was procured and modified to interface with the CM-1 Fluids Supply Package and the CM-1 Combustion Chamber, to accommodate two different carrier gases, each flowing through its own independent column module, to withstand the launch environment of the Space Shuttle, to accept Spacelab electrical power, and to meet the Spacelab flight requirements for electromagnetic interference (EMI) and offgassing. The GC data was down linked to the Marshall Space Flight Center for near-real time analysis, and stored on-orbit for post-flight analysis. The gas chromatograph operated successfully during the entire SOFBALL experiment and collected 309 runs. Because of the constraints imposed upon the gas chromatograph by the CM-1 hardware, system and operations, it was unable to measure the gases to the required accuracy. Future improvements to the system for a re-flight of the SOFBALL experiment are expected to enable the gas chromatograph to meet all the requirements.

  14. Prototype of the gas chromatograph - mass spectrometer to investigate volatile species in the lunar soil for the Luna-Glob and Luna-Resurs missions.

    NASA Astrophysics Data System (ADS)

    Hofer, L.; Lasi, D.; Tulej, M.; Wurz, P.; Cabane, M.; Cosica, D.; Gerasimov, M.; Rodinov, D.

    2013-09-01

    In preparation for the Russian Luna-Glob and Luna-Resurs missions we combined our compact time-offlight mass spectrometer (TOF-MS) with a chemical pre-separation of the species by gas chromatography (GC). Combined measurements with both instruments were successfully performed with the laboratory prototype of the mass spectrometer and a flight-like gas chromatograph. Due to its capability to record mass spectra over the full mass range at once with high sensitivity and a dynamic range of up to 106 within 1s, the TOF-MS system is a valuable extension of the GC analysis. The combined GC-MS complex is able to detect concentrations of volatile species in the sample of about 2·10^-9 by mass.

  15. Determination of vapor pressures for nonpolar and semipolar organic compounds from gas chromatographic retention data

    USGS Publications Warehouse

    Hinckley, D.A.; Bidleman, T.F.; Foreman, W.T.; Tuschall, J.R.

    1990-01-01

    Vapor pressures for nonpolar and moderately polar organochlorine, pyrethroid, and organophosphate insecticides, phthalate esters, and organophosphate flame retardants were determined by capillary gas chromatography (GC). Organochlorines and polycyclic aromatic hydrocarbons with known liquid-phase vapor pressures (P??L) (standard compounds) were chromatographed along with two reference compounds n-C20 (elcosane) and p,p???-DDT on a 1.0-m-long poly(dimethylsiloxane) bonded-phase (BP-1) column to determine their vapor pressures by GC (P??GC). A plot of log P??L vs log P??GC for standard compounds was made to establish a correlation between measured and literature values, and this correlation was then used to compute P??L of test compounds from their measured P??GC. P??L of seven major components of technical chlordane, endosulfan and its metabolites, ??-hexachlorocyclohexane, mirex, and two components of technical toxaphene were determined by GC. This method provides vapor pressures within a factor of 2 of average literature values for nonpolar compounds, similar to reported interlaboratory precisions of vapor pressure determinations. GC tends to overestimate vapor pressures of moderately polar compounds. ?? 1990 American Chemical Society.

  16. Cross-column prediction of gas-chromatographic retention indices of saturated esters.

    PubMed

    D'Archivio, Angelo Antonio; Maggi, Maria Anna; Ruggieri, Fabrizio

    2014-08-15

    We combine computational molecular descriptors and variables related with the gas-chromatographic stationary phase into a comprehensive model able to predict the retention of solutes in external columns. To explore the quality of various approaches based on alternative column descriptors, we analyse the Kováts retention indices (RIs) of 90 saturated esters collected with seven columns of different polarity (SE-30, OV-7, DC-710, OV-25, XE-60, OV-225 and Silar-5CP). Cross-column retention prediction is evaluated on an internal validation set consisting of data of 40 selected esters collected with each of the seven columns, sequentially excluded from calibration. The molecular descriptors are identified by a genetic algorithm variable selection method applied to a large set of non-empirical structural quantities aimed at finding the best multi-linear quantitative structure-retention relationship (QSRR) for the column OV-25 having intermediate polarity. To describe the columns, we consider the sum of the first five McReynolds phase constants and, alternatively, the coefficients of the corresponding QSRRs. Moreover, the mean RI value for the subset of esters used in QSRR calibration or RIs of a few selected compounds are used as column descriptors. For each combination of solute and column descriptors, the retention model is generated both by multi-linear regression and artificial neural network regression.

  17. Enantiospecific gas chromatographic-mass spectrometric analysis of urinary methylphenidate: implications for phenotyping.

    PubMed

    LeVasseur, Natalie L; Zhu, Hao-Jie; Markowitz, John S; DeVane, C Lindsay; Patrick, Kennerly S

    2008-02-01

    A chiral derivatization gas chromatographic-mass spectrometric (GC-MS) method for urine methylphenidate (MPH) analysis was developed and validated to investigate preliminary findings regarding a novel MPH poor metabolizer (PM). Detection was by electron impact (EI) ionization-selected ion monitoring of the N-trifluoroacetylprolylpiperidinium fragments from MPH and the piperidine-deuterated MPH internal standard. The PM eliminated approximately 70 times more l-MPH in urine (9% of the dose over 0-10h), and approximately 5 times more of the d-isomer (10% of the dose), than the mean values determined from 10 normal metabolizers of MPH. Only minor amounts of the metabolite p-hydroxy-MPH were found in the urine of both the PM and normal metabolizers, while the concentration of MPH lactam was not high enough to be detectable. The described method indirectly gauges the functional carboxylesterase-1 status of patients receiving MPH based on the evaluation of relative urine concentrations of d-MPH:l-MPH. Clinical implications concerning rational drug selection for an identified or suspected MPH PM are discussed.

  18. Gas chromatographic quantitative analysis of methanol in wine: operative conditions, optimization and calibration model choice.

    PubMed

    Caruso, Rosario; Gambino, Grazia Laura; Scordino, Monica; Sabatino, Leonardo; Traulo, Pasqualino; Gagliano, Giacomo

    2011-12-01

    The influence of the wine distillation process on methanol content has been determined by quantitative analysis using gas chromatographic flame ionization (GC-FID) detection. A comparative study between direct injection of diluted wine and injection of distilled wine was performed. The distillation process does not affect methanol quantification in wines in proportions higher than 10%. While quantification performed on distilled samples gives more reliable results, a screening method for wine injection after a 1:5 water dilution could be employed. The proposed technique was found to be a compromise between the time consuming distillation process and direct wine injection. In the studied calibration range, the stability of the volatile compounds in the reference solution is concentration-dependent. The stability is higher in the less concentrated reference solution. To shorten the operation time, a stronger temperature ramp and carrier flow rate was employed. With these conditions, helium consumption and column thermal stress were increased. However, detection limits, calibration limits, and analytical method performances are not affected substantially by changing from normal to forced GC conditions. Statistical data evaluation were made using both ordinary (OLS) and bivariate least squares (BLS) calibration models. Further confirmation was obtained that limit of detection (LOD) values, calculated according to the 3sigma approach, are lower than the respective Hubaux-Vos (H-V) calculation method. H-V LOD depends upon background noise, calibration parameters and the number of reference standard solutions employed in producing the calibration curve. These remarks are confirmed by both calibration models used.

  19. Analytical bias among different gas chromatographic approaches using standard BTX gases and exhaust samples.

    PubMed

    Kim, Ki-Hyun; Pandey, Sudhir Kumar; Pal, Raktim

    2009-02-01

    In this study, the analytical compatibility of the gas chromatographic (GC) approach was evaluated through a cross-calibration exercise. To this end, three aromatic volatile organic compounds (VOCs: benzene, toluene, and p-xylene (BTX)) were simultaneously analyzed with four individual instrumental setups (type I = GC with MS plus solid phase microextraction (SPME) method, II = GC with flame ionization detection (FID) plus SPME, III = fast GC-FID plus SPME, and IV = GC-FID plus air server/thermal desorption (AS/TD) method). A comparison of basic quality assurance (QA) data revealed considerable differences in DL values among the methods with moderate variabilities in the intercompound sensitivity. In light of the differences in detection properties, the analytical bias involved for each methodological approach was assessed by the relative relationship between analytes and basic operating conditions. The results suggest that the analysis of environmental samples at ultra-low concentration levels (at or below ppb level) can be subject to diverse sources of bias. Although detection properties of target compounds seem to be affected by the combined effects of various factors, changes in the sample concentration levels were seen to be the most consistent under the experimental setups analyzed in this study.

  20. Different reactivities of amphetamines with N-methyl-bis(trifluoroacetamide) in heated gas chromatographic injectors.

    PubMed

    Hidvégi, E; Hideg, Zs; Somogyi, G P

    2008-03-01

    A fast gas chromatographic mass spectrometric method has been developed earlier for the determination of amphetamine derivatives in human serum and urine. For derivatization, N-methyl-bis(trifluoroacetamide) (MBTFA) was used. Derivatization was performed using an on-line mode, since 1 microl of MBTFA and 1 microl sample extract, dissolved in toluene were injected simultaneously. In this study, the reactivity of the several amphetamine type analytes with MBTFA was investigated. MBTFA used for flash derivatization was applied undiluted on the one hand and diluted 4--4096-fold with acetonitrile on the other hand. Studying several amphetamines in the test sample spiked at the same concentrations we found that they could be divided into 3 groups based on relative target ion peak areas as a function of MBTFA dilution. Group 1, containing only primary amines showed an early increase of the relative peak areas if we increased MBTFA concentration, where group 2 (mainly N-methyl secondary amines) showed that relative peak areas started to increase intensively at higher MBTFA concentrations. Finally, MDEA as an N-ethyl secondary amine, representing group 3, showed significant increase if only slightly diluted MBTFA was used as a flash reagent. This phenomenon can be explained mainly with the less and less reactivity of amine groups in the case of groups 2 and 3, compared to group 1. These findings could help to optimise analytical methods involving flash derivatization processes.

  1. Gas chromatographic mass analysis and further pharmacological actions of Cymbopogon proximus essential oil.

    PubMed

    Al-Taweel, A M; Fawzy, G A; Perveen, S; El Tahir, K E H

    2013-09-01

    The present study reports Gas chromatographic mass analysis (GC-MS) as well as important biological activities of Cymbopogon proximus essential oil. The chemical composition of the essential oil of Cymbopogon proximus was investigated by GC-MS. Furthermore, the effects of Cymbopogon proximus essential oil on the cardiac parasympathetic ganglia in rats, the intra-tracheal pressure in guinea-pigs and on carrageenan-induced inflammation in the rats paw, were studied. The GC-MS study led to the identification of 22 components with Piperitone representing (73.81%), Elemol (9.32%), alpha-Eudesmol (5.21%) and alpha-Terpineol (3.01%) of the oils composition. The percentage protective effect of the oil on the vagus-induced bradycardia in rats was 90.1±3.1%, which represents a significant protection. As for the effect of Cymbopogon oil on bronchoconstrictors-induced increase in intra-tracheal pressure in guinea-pigs, the oil antagonized the actions of 5-HT and histamine by 80±3.7 and 93±8.3%, respectively. Pharmacological investigations using Cymbopogon oil revealed its inherent ability to possess a bronchodilator activity mediated via blockade of both histamine and serotonin receptors. It possessed a significant ganglionic blocking action and a limited anti-inflammatory activity that seemed to involve blockade of histamine and serotonin receptors in the rats' paws.

  2. Oil/gas collector/separator for underwater oil leaks

    SciTech Connect

    Henning, C.D.

    1992-12-31

    This invention is comprised of an oil/gas collector/separator for recovery of oil leaking, for example, from an offshore or underwater oil well. The separator is floated over the point of the leak and tethered in place so as to receive oil/gas floating, or forced under pressure, toward the water surface from either a broken or leaking oil well casing, line, or sunken ship. The separator is provided with a downwardly extending skirt to contain the oil/gas which floats or is forced upward into a dome wherein the gas is separated from the oil/water, with the gas being flared (burned) at the top of the dome, and the oil is separated from water and pumped to a point of use. Since the density of oil is less than that of water it can be easily separated from any water entering the dome.

  3. Oil/gas collector/separator for underwater oil leaks

    DOEpatents

    Henning, Carl D.

    1993-01-01

    An oil/gas collector/separator for recovery of oil leaking, for example, from an offshore or underwater oil well. The separator is floated over the point of the leak and tethered in place so as to receive oil/gas floating, or forced under pressure, toward the water surface from either a broken or leaking oil well casing, line, or sunken ship. The separator is provided with a downwardly extending skirt to contain the oil/gas which floats or is forced upward into a dome wherein the gas is separated from the oil/water, with the gas being flared (burned) at the top of the dome, and the oil is separated from water and pumped to a point of use. Since the density of oil is less than that of water it can be easily separated from any water entering the dome.

  4. Application of chiral derivatizing agents in the high-performance liquid chromatographic separation of amino acid enantiomers: a review.

    PubMed

    Ilisz, István; Berkecz, Robert; Péter, Antal

    2008-05-12

    The past 20 years has seen an explosive growth in the field of chirality, as illustrated by the rapid progress in the various facets of this intriguing field. The impetus for advances in chiral separation has been highest in the past decade and this still continues to be an area of high focus. This paper reviews indirect separation approaches, i.e. derivatization reactions aimed at creating the basis for the chromatographic resolution of biologically and pharmaceutically important enantiomers, with emphasis on the literature published in the last 12 years. The main aspects of the chiral derivatization of amino acids are discussed, i.e. derivatization on the amino group, transforming the molecules into covalently bonded diastereomeric derivatives through the use of homochiral derivatizing agents. The diastereomers formed (amides, urethanes, urea, thiourea derivatives, etc.) can be separated on achiral stationary phases. The applications are considered, and in some cases different derivatizing agents for the resolution of complex mixtures of proteinogenic d,l-amino acids, non-proteinogenic amino acids and peptides/amino acids from peptide syntheses or microorganisms are compared.

  5. Capillary gas chromatographic assay of residual methenamine hippurate in equipment cleaning validation swabs.

    PubMed

    Mirza, T; George, R C; Bodenmiller, J R; Belanich, S A

    1998-02-01

    A capillary gas chromatographic method is described for the determination of methenamine hippurate residue in swabs collected from manufacturing equipment surfaces. Any residual methenamine hippurate remaining on process equipment after cleaning is removed by swabbing with one wet polyester Absorbond swab (4" x 4") pre-moistened with water followed by a dry Absorbond swab. The residual methenamine hippurate is chromatographed on a 30 x 0.32 mm (i.d.) Supelcowax-10 capillary column of 0.25-micron film thickness. The amount of residual methenamine hippurate is determined by comparing the ratio of methenamine hippurate peak area response to that of p-cresol (internal standard) obtained for the sample to a linear calibration curve obtained for a series of standard solutions. The method is demonstrated to be sufficiently linear, accurate, precise, sensitive and rugged for the determination of low levels of methenamine hippurate on equipment surfaces. Using this method, the mean recovery of methenamine hippurate from spiked Absorbond swab samples contained in high density polyethylene bottles was 105.2%, with a relative standard deviation (RSD) of +/- 7.1% (n = 25). The mean recoveries of methenamine hippurate from spiked test plates for '180 Grit' Stainless Steel, Teflon and WARCO White (neoprene and PVC) gasket material were 77.2, 96.1 and 50.6%, with RSDs of +/- 9.4 (n = 25), +/- 4.3 (n = 25) and +/- 36% (n = 20), respectively. Recovery correction factors have been incorporated into the method. The method was successfully applied to the assay of actual equipment cleaning validation swab samples. Stability studies demonstrate that methenamine hippurate is not very stable on the equipment surfaces or in the swabs. It is recommended that the surfaces be swabbed immediately after cleaning and the swabs analyzed within 24 h after sample collection. The results demonstrate that in order to fully validate the cleaning procedures, it is not only necessary to investigate the

  6. Chromatographic separation of arsenic species with pentafluorophenyl column and application to rice.

    PubMed

    Baba, Koji; Arao, Tomohito; Yamaguchi, Noriko; Watanabe, Eiki; Eun, Heesoo; Ishizaka, Masumi

    2014-08-08

    Arsenic species, including arsenous acid, arsenic acid, methylarsonic acid, and dimethylarsinic acid, were determined using HPLC-ICPMS. The species were separated with a Discovery HS F5 column and a simple, volatile, and isocratic mobile phase of 0.1% (v/v) formic acid and 1% (v/v) methanol. The Discovery HS F5 column with a pentafluorophenyl (PFP) stationary phase gave sharp peaks and full separation of the arsenic species in 5min, and other PFP columns showed lower performance. This separation method was applied to arsenic species analysis in rice. The extraction of arsenic from rice samples was performed using 0.15M nitric acid. The methodology was validated by use of certified reference materials, NMIJ CRM 7503-a and NIST SRM 1568a, and extremely low arsenic rice samples as blank samples.

  7. A novel derivatization procedure and chiral gas chromatographic method for enantiomeric purity screening of L-carnitine.

    PubMed

    Albreht, Alen; Zupančič, Borut; Vovk, Irena

    2014-01-01

    L-Carnitine is used extensively in functional foods and food supplements; consequently, the control of its enantiomeric purity is of paramount importance. A new derivatization procedure and chiral gas chromatographic method with flame ionization detection, using a cyclodextrin based stationary phase, enables prompt, simple, and inexpensive screening of the enantiomeric ratio of L- and D-carnitine in samples with different matrices. Conversion of carnitine to beta-acetoxy-gama-butyrolactone was optimized for maximum conversion (98% of the desired product lactone was formed and 2% of the side product gama-crotonolactone) and minimum racemization (no changes at the chiral center were detected) and time consumption. As it is shown in this study, a fast gas chromatographic method, with total run time of 7 min, together with the new derivatization procedure enables an effective enantiomeric purity screening of L-carnitine in real samples such as food supplements and L-carnitine raw ingredient.

  8. Gas chromatographic simulated distillation-mass spectrometry for the determination of the boiling point distributions of crude oils

    PubMed

    Roussis; Fitzgerald

    2000-04-01

    The coupling of gas chromatographic simulated distillation with mass spectrometry for the determination of the distillation profiles of crude oils is reported. The method provides the boiling point distributions of both weight and volume percent amounts. The weight percent distribution is obtained from the measured total ion current signal. The total ion current signal is converted to weight percent amount by calibration with a reference crude oil of a known distillation profile. Knowledge of the chemical composition of the crude oil across the boiling range permits the determination of the volume percent distribution. The long-term repeatability is equivalent to or better than the short-term repeatability of the currently available American Society for Testing and Materials (ASTM) gas chromatographic method for simulated distillation. Results obtained by the mass spectrometric method are in very good agreement with results obtained by conventional methods of physical distillation. The compositional information supplied by the method can be used to extensively characterize crude oils.

  9. Gas chromatographic ion trap mass spectrometry determination of zoxamide residues in grape, grape processing, and in the fermentation process.

    PubMed

    Angioni, Alberto; Garau, Anna; Caboni, Pierluigi; Russo, Maria Teresa; Farris, Giovanni Antonio; Zara, Severino; Cabras, Paolo

    2005-12-02

    A gas chromatographic ion-trap mass spectrometry (GC-ITMS) method was developed for the determination of the fungicide zoxamide in grape, must, wine, and spirits. Samples were extracted with hexane and analyzed without any clean up. The gas chromatograph was fitted with a carbofrit inserted into the glass liner to allow large volume injections. Analyses were carried out both in EI and CI mode. Recoveries from fortified samples ranged between 86 and 114% at four different fortification levels (n=6 each), ranging between 0.05 and 2.00 mg/kg. The relative standard deviation was below 19%. Both in EI and CI mode the calculated limit of detection (LOD) and quantification (LOQ) were 0.01 and 0.05 mg/kg (0.08 mg/kg in CI), respectively. Moreover the influence of yeasts and bacteria fermentation was evaluated.

  10. Evaluation of Comprehensive 2-D Gas Chromatography-Time-Of-Flight Mass Spectrometry for 209 Chlorinated Biphenyl Congeners in Two Chromatographic Runs

    EPA Science Inventory

    This research evaluates a recently developed comprehensive 2-D GC coupled with a time-of-flight (TOF) mass spectrometer for the potential separation of 209 PCB congeners, using a sequence of 1-D and 2-D chromatographic modes. In two consecutive chromatographic runs, using a 40 m,...

  11. Chromatographic separation of selenium and arsenic: A potential (72)Se/(72)As generator.

    PubMed

    Wycoff, Donald E; Gott, Matthew D; DeGraffenreid, Anthony J; Morrow, Ryan P; Sisay, Nebiat; Embree, Mary F; Ballard, Beau; Fassbender, Michael E; Cutler, Cathy S; Ketring, Alan R; Jurisson, Silvia S

    2014-05-02

    An anion exchange method was developed to separate selenium and arsenic for potential utility in a (72)Se/(72)As generator. The separation of the daughter (72)As from the (72)Se parent is based on the relative acid-base behavior of the two oxo-anions in their highest oxidation states. At pH 1.5, selenate is retained on strongly basic anion exchange resin as HSeO4(-) and SeO4(2-), while neutral arsenic acid, H3AsO4, is eluted.

  12. Chromatographic Separation of Selenium and Arsenic: A Potential 72Se/72As Generator

    PubMed Central

    Wycoff, Donald E.; Gott, Matthew D.; DeGraffenreid, Anthony J.; Morrow, Ryan P.; Sisay, Nebiat; Embree, Mary F.; Ballard, Beau; Fassbender, Michael E.; Cutler, Cathy S.; Ketring, Alan R.; Jurisson, Silvia S.

    2014-01-01

    Summary An anion exchange method was developed to separate selenium and arsenic for potential utility in a 72Se/72As generator. The separation of the daughter 72As from the 72Se parent is based on the relative acid-base behavior of the two oxo-anions in their highest oxidation states. At pH 1.5, selenate is retained on strongly basic anion exchange resin as HSeO4− and SeO42−, while neutral arsenic acid, H3AsO4, is eluted. PMID:24679827

  13. Field-portable Gas Chromatograph Mass Spectrometer (GC-MS) Unit for Semi-volatile Compound Analysis in Groundwater

    DTIC Science & Technology

    2011-09-01

    Program ERDC TR-11-11 September 2011 Field-portable Gas Chromatograph Mass Spectrometer (GC-MS) Unit for Semi-volatile Compound Analysis in...fixed laboratories that perform regulatory-approved analytical methods . The typical analysis and data reporting time at most analytical laboratories...USEPA method 8330. Technology description Mass spectrometry (MS) analysis systems can provide valuable chemical information on almost any type of

  14. Fitting formula for the injection volume of a gas chromatograph for radio-xenon sampling in the lower troposphere.

    PubMed

    Shu-jiang, Liu; Zhan-ying, Chen; Shi-lian, Wang; Yin-zhong, Chang; Qi, Li; Yuan-qing, Fan; Yun-gang, Zhao; Huai-mao, Jia; Xin-jun, Zhang; Jun, Wang

    2014-06-01

    GC is usually used for xenon concentration and radon removal in the International Monitoring System of the Comprehensive Nuclear-Test-Ban Treaty. In a gas chromatograph, the injection volume is defined to calculate the column capacity. In this paper, the injection volume was investigated and a fitting formula for the injection volume was derived and discussed subsequently. As a consequence, the xenon injection volume exponentially decreased with the column temperature increased, but exponentially increased as the flow rate increased.

  15. Thin-layer chromatographic (TLC) separations and bioassays of plant extracts to identify antimicrobial compounds

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungal spores in nutrient solution or bacteria in liquefied agar), allowing time for the microbes to gr...

  16. Development of an Exhaled Breath Monitoring System with Semiconductive Gas Sensors, a Gas Condenser Unit, and Gas Chromatograph Columns

    PubMed Central

    Itoh, Toshio; Miwa, Toshio; Tsuruta, Akihiro; Akamatsu, Takafumi; Izu, Noriya; Shin, Woosuck; Park, Jangchul; Hida, Toyoaki; Eda, Takeshi; Setoguchi, Yasuhiro

    2016-01-01

    Various volatile organic compounds (VOCs) in breath exhaled by patients with lung cancer, healthy controls, and patients with lung cancer who underwent surgery for resection of cancer were analyzed by gas condenser-equipped gas chromatography-mass spectrometry (GC/MS) for development of an exhaled breath monitoring prototype system involving metal oxide gas sensors, a gas condenser, and gas chromatography columns. The gas condenser-GC/MS analysis identified concentrations of 56 VOCs in the breath exhaled by the test population of 136 volunteers (107 patients with lung cancer and 29 controls), and selected four target VOCs, nonanal, acetoin, acetic acid, and propanoic acid, for use with the condenser, GC, and sensor-type prototype system. The prototype system analyzed exhaled breath samples from 101 volunteers (74 patients with lung cancer and 27 controls). The prototype system exhibited a level of performance similar to that of the gas condenser-GC/MS system for breath analysis. PMID:27834896

  17. Development of an Exhaled Breath Monitoring System with Semiconductive Gas Sensors, a Gas Condenser Unit, and Gas Chromatograph Columns.

    PubMed

    Itoh, Toshio; Miwa, Toshio; Tsuruta, Akihiro; Akamatsu, Takafumi; Izu, Noriya; Shin, Woosuck; Park, Jangchul; Hida, Toyoaki; Eda, Takeshi; Setoguchi, Yasuhiro

    2016-11-10

    Various volatile organic compounds (VOCs) in breath exhaled by patients with lung cancer, healthy controls, and patients with lung cancer who underwent surgery for resection of cancer were analyzed by gas condenser-equipped gas chromatography-mass spectrometry (GC/MS) for development of an exhaled breath monitoring prototype system involving metal oxide gas sensors, a gas condenser, and gas chromatography columns. The gas condenser-GC/MS analysis identified concentrations of 56 VOCs in the breath exhaled by the test population of 136 volunteers (107 patients with lung cancer and 29 controls), and selected four target VOCs, nonanal, acetoin, acetic acid, and propanoic acid, for use with the condenser, GC, and sensor-type prototype system. The prototype system analyzed exhaled breath samples from 101 volunteers (74 patients with lung cancer and 27 controls). The prototype system exhibited a level of performance similar to that of the gas condenser-GC/MS system for breath analysis.

  18. Determination of hexanal as an oxidative marker in vegetable oils using an automated dynamic headspace sampler coupled to a gas chromatograph/mass spectrometer.

    PubMed

    Ha, Jaeho; Seo, Dong-Won; Chen, Xi; Hwang, Jin-Bong; Shim, You-Shin

    2011-01-01

    An automated dynamic headspace sampler coupled to a gas chromatograph/mass spectrometer was evaluated as an oxidative marker to determine hexanal content in vegetable oils. For the effective analysis, a cooled injection system (CIS) was used to focus and to introduce the hexanal desorbed from the Tenax TA. The temperature of the CIS was maintained at -60 °C for 12 min before desorbing the hexanal. Hexanal was separated on a capillary column (DB-5, 0.25 mm × 60 m, 0.25 µm in film thickness) from 50 to 230 °C, followed by mass spectrometer-selected ion monitoring analysis at m/z 56. The instrumental response to hexanal was highly linear from 10 ng mL(-1) to 1 µg mL(-1) (r(2) = 0.9999). The relative standard deviation (RSD) of intra- and inter-day repeatability was acceptable, with values of less than 3.88 and 4.25%, respectively. The LOD and LOQ of hexanal were determined by gas chromatograph/mass spectrometer-selected ion monitoring to be 3.3 and 9.8 ng mL(-1), respectively. The acid value, peroxide value and fatty acid composition revealed a good correlation with the hexanal concentration.

  19. Sequential determination of triglycerides and free fatty acids in biological fluids by use of a continuous pretreatment module coupled to a gas chromatograph.

    PubMed

    Cárdenas, M S; Ballesteros, E; Gallego, M; Valcárcel, M

    1994-11-01

    A continuous system coupled to a gas-liquid chromatograph was used for the sequential determination of triglycerides and free fatty acids in serum and urine. The module provides compositional information and hence more detailed information on lipid metabolism changes in patients suffering metabolic disorders. Lipids in biological samples are manually extracted in methanol-n-hexane and introduced into the flow system; free fatty acids are then separated by retention on an ion-exchange resin and triglycerides (not retained) are transesterified with acetyl chloride in methanol. The resulting methyl esters are continuously injected into the gas chromatograph and determined by using a flame ionization detector. In a second step, retained free fatty acids are eluted and derivatized (also with acetyl chloride in methanol) and subsequently determined similarly as the triglycerides. The proposed method was applied to the determination of triglycerides in a lipid control serum; free fatty acids were determined in a human pool serum by the proposed method and compared with the volumetric method used in clinical practice. The results obtained in both instances showed good agreement between the results provided for triglycerides and free fatty acids. The proposed method was also applied to urine samples; a parallel recovery study was also made in order to assess the performance of the method.

  20. Exploring atmospheric photooxidation with a new Gas Chromatograph Time-of-Flight Chemical Ionization Mass Spectrometer (GC-ToF-CIMS)

    NASA Astrophysics Data System (ADS)

    Nölscher, A. C.; Allen, H. M.; Teng, A.; Crounse, J.; Wennberg, P. O.

    2015-12-01

    Atmospheric photooxidation is a fundamental process that effectively removes pollutants and greenhouse gases from the air we breathe. One way to explore these processes is to directly measure the stable intermediate oxidation products. Chemical Ionization Mass Spectrometry (CIMS) has proven to be a powerful tool to sensitively detect with high time resolution photooxidation products in the atmosphere such as hydroperoxides, acids, nitrates, and other oxygenated volatile organic compounds. Despite the potential to elucidate atmospheric photooxidation in detail, field observations of such compounds are sparse. Here we present the development of a new Gas Chromatograph Time-of-Flight Chemical Ionization Mass Spectrometer (GC-ToF-CIMS) for field deployment. Using low pressure gas chromatography and CF3O- ionization chemistry, the selective operation of a GC is combined with the sensitive, specific, and fast detection of a high-resolution ToF-CIMS. The combination of chromatographic separation and exact mass identification allows detecting isomer resolved photooxidation products. Direct measurements in the atmosphere of such isomer distributions are particularly interesting due to the broad range of their individual atmospheric lifetimes and impacts.

  1. Ion-exchange chromatographic separation of einsteinium from irradiated californium targets

    SciTech Connect

    Elesin, A.A.; Nikolaev, V.M.; Shalimov, V.V.; Popov, Yu.S.; Kovantsev, V.N.; Tselishchev, I.V.; Filimonov, V.T.; Mishenev, V.B.; Yadovin, A.A.; Golosovskii, L.S.; Chetverikov, A.P.

    1987-07-01

    Einsteinium was obtained by preparing two experimental californium targets and subjecting them to neutron irradiation in a high-flux reactor. The einsteinium was separated from the bombarded targets on a column packed with KU-2U sulfonated cation-exchange resin (20-50 ..mu..m) and eluted at room temperature with an ammonium ..cap alpha..-hydroxyisobutyrate solution. Three successive separation cycles removed californium to produce einsteinium in 68% yield with a decontamination factor of 5.3 x 10/sup 6/. About 20% of the einsteinium was used up by analysis and 11% remained in intermediate fractions. The method developed yielded pure einsteinium with little fission products present. The contribution of the fission products to the total einsteinium gamma-irradiation dose rate was no greater than 81%, due primarily to the radioisotope terbium-160.

  2. Electrochemically modulated liquid chromatographic separation of triazines and the effect of pH on retention.

    PubMed

    Yakes, Betsy Jean; Keller, David W; Porter, Marc D

    2010-06-25

    Electrochemically modulated liquid chromatography (EMLC) manipulates analyte retention by changing the potential applied (E(app)) to a conductive stationary phase. This paper applies EMLC to the separation of a set of seven triazines which are commonly used but environmentally hazardous herbicides. Experiments herein examine the influence of E(app) and the pH of the mobile phase on triazine retention. The results are discussed in terms of: (1) retention of triazines of dissimilar acid strengths and by correlations with the pH of the mobile phase; (2) how changes in E(app) and acid-base equilibria modulate elution; (3) qualitative insights into EMLC-based retention; and (4) potential merits of EMLC in realizing the rapid separation of the seven-component triazine mixture.

  3. A Novel Micellar Electrokinetic Chromatographic Method for Separation of Metal-DDTC Complexes

    PubMed Central

    Mallah, Arfana; Memon, Saima Q.; Solangi, Amber R.; Memon, Najma; Abbassi, Kulsoom; Khuhawar, Muhammad Yar

    2012-01-01

    Micellar electrokinetic chromatography (MEKC) was examined for the separation and determination of Mo(VI), Cr(VI), Ni(II), Pd(II), and Co(III) as diethyl dithiocarbamate (DDTC) chelates. The separation was achieved from fused silica capillary (52 cm × 75 μm id) with effective length 40 cm, background electrolyte (BGE) borate buffer pH 9.1 (25 mM), CTAB 30% (100 mM), and 1% butanol in methanol (70 : 30 : 5 v/v/v) with applied voltage of −10 kV using reverse polarity. The photodiode array detection was achieved at 225 nm. The linear calibration for each of the element was obtained within 0.16–10 μg/mL with a limit of detection (LOD) 0.005–0.0167 μg/mL. The separation and determination was repeatable with relative standard deviation (RSD) within 2.4–3.3% (n = 4) in terms of migration time and peak height/peak area. The method was applied for the determination of Mo(VI) from potatoes and almond, Ni(II) from hydrogenated vegetable oil, and Co(III) from pharmaceutical preparations with RSD within 3.9%. The results obtained were checked by standard addition and rechecked by atomic absorption spectrometry. PMID:22649320

  4. Liquid-chromatographic separation and on-line bioluminescence detection of creatine kinase isoenzymes

    SciTech Connect

    Bostick, W.D.; Denton, M.S.; Dinsmore, S.R.

    1980-01-01

    Isoenzymes of creatine kinase were separated by anion-exchange chromatography, with use of an elution gradient containing lithium acetate (0.1 to 0.6 mol/L). A stream splitter was used to divert a 5% side stream of column effluent, which was subsequently mixed with the reagents necessary for bioluminescence assay of the separated isoenzymes. The use of the stream splitter greatly decreased the rate of consumption of reagent and, when combined with a peristaltic pumping system, permitted independent control of the side-stream flow rate. Thus both the residence interval in a delay coil in which the ATP reaction product is formed and the bioluminescence emission was monitored in a flow-through fluorometer without use of an external light source or filters. Separation and detection of the isoenzymes of creatine kinase were rapid, sensitive, and highly selective. The incremental decrease of bioluminescence response owing to inhibition by the ions in the eluent was less than 31% across the entire gradient.

  5. Triticonazole enantiomers: Separation by supercritical fluid chromatography and the effect of the chromatographic conditions.

    PubMed

    He, Jianfeng; Fan, Jun; Yan, Yilun; Chen, Xiaodong; Wang, Tai; Zhang, Yaomou; Zhang, Weiguang

    2016-11-01

    Enantiomeric pairs of triticonazole have been successfully separated by supercritical fluid chromatography coupled with a tris(3,5-dimethylphenylcarbamoyl) cellulose-coated chiral stationary phase in this work. The effects of co-solvent, dissolution solvent, flow rate, backpressure, and column temperature have been studied in detail with respect to retention, selectivity, and resolution of triticonazole. As indicated, the co-solvents mostly affected the retention factors and resolution, due to the different molecular structure and polarity. In addition, the dissolution solvents, namely, chloromethanes and alcohols, have been also important for enantioseparation because of the different interaction with stationary phase. Higher flow rate and backpressure led to faster elution of the triticonazole molecules, and the change of column temperature showed slight effect on the resolution of triticonazole racemate. Moreover, a comparative separation experiment between supercritical fluid chromatography and high performance liquid chromatography revealed that chiral supercritical fluid chromatography gave the 3.5 times value of Rs /tR2 than high performance liquid chromatography, which demonstrated that supercritical fluid chromatography had much higher separation efficiency.

  6. Results from the Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe

    NASA Technical Reports Server (NTRS)

    Niemann, Hasso B.

    2006-01-01

    The GCMS was part of the instrument complement on the Cassini-Huygens Probe to measure in situ the chemical composition of the atmosphere during the probe descent and coupled with the Aerosol Collector Pyrolyser (ACP) experiment by serving as detector for the pyrolization products to determine the composition of the aerosol particles. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns, a chemical scrubber and a hydrocarbon enrichment cell. The GCMS gas inlet was heated to prevent condensation, and to evaporate volatiles from the surface after impact. The GCMS collected data from an altitude of 146 km to ground impact. The Probe and the GCMS survived impact and collected data for 1 hour and 9 minutes on the surface. Mass spectra were collected during descent and on the ground over a range of m/z from 2 to 141. The major constituents of the lower atmosphere were confirmed to be NP and CH4. The methane mole fraction was uniform in the stratosphere. It increased below the tropopause, at about 32 km altitude, monotonically toward the surface, reaching a plateau at about 8 km at a level near saturation. After surface impact a steep increase of the methane signal was observed, suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. The measured mole fraction of Ar-40 is 4.3 x 10(exp-5) and of Ar-36 is 2.8 x 10(exp -7). The other primordial noble gases were below mole fraction. The isotope ratios of C-12/C-13 determined from methane measurements are 82.3 and of N-14/N-15 determined from molecular nitrogen are 183. The D/H isotope ratio determined from the H2 and HD measurements is 2.3 x l0(exp -4). Carbon dioxide, ethane, acetylene and cyanogen were detected evaporating from the surface in addition to methane.

  7. Oil/gas separator for installation at burning wells

    DOEpatents

    Alonso, Carol T.; Bender, Donald A.; Bowman, Barry R.; Burnham, Alan K.; Chesnut, Dwayne A.; Comfort, III, William J.; Guymon, Lloyd G.; Henning, Carl D.; Pedersen, Knud B.; Sefcik, Joseph A.; Smith, Joseph A.; Strauch, Mark S.

    1993-01-01

    An oil/gas separator is disclosed that can be utilized to return the burning wells in Kuwait to production. Advantageously, a crane is used to install the separator at a safe distance from the well. The gas from the well is burned off at the site, and the oil is immediately pumped into Kuwait's oil gathering system. Diverters inside the separator prevent the oil jet coming out of the well from reaching the top vents where the gas is burned. The oil falls back down, and is pumped from an annular oil catcher at the bottom of the separator, or from the concrete cellar surrounding the well.

  8. Oil/gas separator for installation at burning wells

    DOEpatents

    Alonso, C.T.; Bender, D.A.; Bowman, B.R.; Burnham, A.K.; Chesnut, D.A.; Comfort, W.J. III; Guymon, L.G.; Henning, C.D.; Pedersen, K.B.; Sefcik, J.A.; Smith, J.A.; Strauch, M.S.

    1993-03-09

    An oil/gas separator is disclosed that can be utilized to return the burning wells in Kuwait to production. Advantageously, a crane is used to install the separator at a safe distance from the well. The gas from the well is burned off at the site, and the oil is immediately pumped into Kuwait's oil gathering system. Diverters inside the separator prevent the oil jet coming out of the well from reaching the top vents where the gas is burned. The oil falls back down, and is pumped from an annular oil catcher at the bottom of the separator, or from the concrete cellar surrounding the well.

  9. Optimization to eliminate the interference of migration isomers for measuring 1-O-beta-acyl glucuronide without extensive chromatographic separation.

    PubMed

    Xue, Y-J; Akinsanya, J Billy; Raghavan, Nirmala; Zhang, Donglu

    2008-01-01

    A highly selected reaction monitoring (SRM) method has been investigated for the determination of muraglitazar 1-O-beta-acyl glucuronide in animal and human plasma without chromatographic separation of this naturally formed acyl glucuronide from its migration isomers. In the ion source or the collision cell, glucuronides are often prone to lose the dehydrated glucuronic acid (176 Da) and convert back into the parent drug (aglycone). The extent of loss of the glucuronide moiety can differ among glucuronides. For the naturally occurring muraglitazar 1-O-beta-acyl glucuronide, or its synthetic anomer 1-O-alpha-glucuronide, the loss of the glucuronide moiety was a major fragment ion. The loss of the glucuronide moiety was greater for the 1-O-beta-acyl glucuronide than the 1-O-alpha-anomer. In addition, the loss of the glucuronide moiety was insignificant (less than 0.01%) with the other glucuronide isomers (2-, 3- or 4-O, alpha or beta). Given the fact that the 1-O-alpha-anomer was a minor impurity in the muraglitazar 1-O-beta-acyl glucuronide reference standard, and not either a conversion product of 1-O-beta-acyl glucuronide or endogenously formed, the SRM transition corresponding to the loss of the glucuronide moiety was very specific for 1-O-beta-acyl glucuronide, and practically free from interference of the other isomers under optimized collision-cell conditions. As a result, extensive chromatographic separation of 1-O-beta-acyl glucuronide from its migration isomers was not required. The use of this specific SRM transition effectively reduced the separation time from 12.0 min of a long-column high-performance liquid chromatography (HPLC) method to 2.5 min by use of a shorter column. The standard curve performance and analysis results of 1-O-beta-acyl glucuronide incubation samples showed that the short-column method could produce equivalent results to the long-column method but with a 4.5-fold improvement in sample throughput. This approach may be useful for

  10. Determination of mercurial species in fish by inductively coupled plasma mass spectrometry with anion exchange chromatographic separation.

    PubMed

    Chen, Xiaopan; Han, Chao; Cheng, Heyong; Liu, Jinhua; Xu, Zigang; Yin, Xuefeng

    2013-09-24

    This work demonstrated the feasibility of mercury speciation analysis by anion exchange chromatographic separation with inductively coupled plasma mass spectrometry detection. For the first time, by complexing with the mobile phase containing 3-mercapto-1-propanesulfonate into negatively charged complexes, fast separation of inorganic mercury (Hg(2+)), monomethylmercury (MeHg), ethylmercury (EtHg) and phenylmercury (PhHg) was achieved within 5 min on a 12.5-mm strong anion exchange column. The detection limits for Hg(2+), MeHg, EtHg and PhHg were 0.008, 0.024, 0.029 and 0.034 μg L(-1), respectively. The relative standard deviations of peak height and peak area (5.0 μg L(-1) for each Hg species) were all below 3%. The determined contents of Hg(2+), MeHg and total Hg in a certified reference material of fish tissue by the proposed method were in good accordance with the certified values with satisfactory recoveries. The relative errors for determining MeHg and total mercury were -2.4% and -1.2%, respectively, with an acceptable range for spike recoveries of 94-101%. Mercury speciation in 11 fish samples were then analyzed after the pretreated procedure. The mercury contents in all fish samples analyzed were found compliant with the criteria of the National Standards of China.

  11. Discovery of active components in herbs using chromatographic separation coupled with online bioassay.

    PubMed

    De-Qiang, Li; Zhao, Jing; Wu, Dong; Shao-Ping, Li

    2016-05-15

    Discovery of bioactive compounds from complex mixtures is a challenge. In past decades, several strategies were developed and implemented for rapid and effective screening and characterization of bioactive components in complex matrices. This review mainly focused on the online strategies, which integrated the separation science, mass spectrometry, and bioactivity screening in a single platform, allowing simultaneous screening and characterization of active compounds from complex matrices, especially from the herbs. The online screening methodologies, including pre-column affinity-based screening and post-column bioassay, were discussed and their applied examples were also presented to illustrate the strengths and limitations of these approaches.

  12. Measurement of Ethanol in Gaseous Breath Using a Miniature Gas Chromatograph

    PubMed Central

    Morey, Timothy E.; Booth, Matthew M.; Prather, Robert A.; Nixon, Sara J.; Boissoneault, Jeff; Melker, Richard J.; Goldberger, Bruce A.; Wohltjen, Hank; Dennis, Donn M.

    2011-01-01

    We designed and built a novel, miniature gas chromatograph (mGC) to use exhaled breath to estimate blood ethanol concentrations that may offer GC quality sensitivity and specificity, but with portability, reduced size, and decreased cost. We hypothesized that the mGC would accurately estimate the serum ethanol concentration using exhaled breath. Human subjects (n = 8) were dosed with ethanol employing the Widmark criteria, targeting a blood concentration of 0.08 g/dL. Serum and breath samples were collected concurrently over an hour. Ethanol concentrations in serum were measured using a CLIA-approved laboratory. Ethanol concentrations in conventional breath were assayed using a calibrated mGC or Intoxilyzer 400PA. Data were analyzed using Bland-Altman analysis using serum concentrations as a “gold standard”. For the mGC, the regression line (correlation coefficient), bias, and 95% limits of agreement were y = 1.013x − 0.009 (r = 0.91), −0.008 g/dL, and −0.031 to 0.016 g/dL, respectively, for 30 specimens. For the Intoxilyzer 400PA, the regression line (correlation coefficient), bias, and 95% limits of agreement were y = 0.599x + 0.008 (r = 0.86), −0.024 g/dL, and −0.049 to 0.002 g/dL, respectively, for 71 specimens with a large magnitude effect. We concluded that the mGC, using exhaled breath, performed well to estimate the serum ethanol concentrations. PMID:21439148

  13. The Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe: First Results

    NASA Technical Reports Server (NTRS)

    Niemann, H.; Demick, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Raaen, E.; Way, S.; Atreya, S.; Carignan, G.; Bauer, S.

    2005-01-01

    The Huygens Probe of the Cassini Huygens Mission entered the atmosphere of the moon Titan on January 14, 2005. The GCMS was part of the instrument complement on the Probe to measure in situ the chemical composition of the atmosphere during the probe descent and to support the Aerosol Collector Pyrolyzer (ACP) experiment by serving as detector for the pyrolization products. The GCMS collected data from an altitude of 146 km to ground impact for a time interval of 2 hours and 37 minutes. The Probe and the GCMS survived the ground impact and collected data for 1 hour and 9 minutes on the surface in the near surface environment until signal loss by the orbiter. The instrument collected 5634 mass spectra during descent and 2692 spectra on the ground over a range of m/z from 2 to 141. Eight gas chromatograph samples were taken during the descent and two on the ground. This is a report on work in progress. The major constituents of the lower atmosphere were found to be N2 and CH4. The methane-mixing ratio was found to increase below the turbopause, about 35 km altitude, monotonically toward the surface to levels near saturation. After surface impact a steep increase of the mixing ratio was observed suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. Other constituents were found to be in very low concentrations, below ppm levels. The presence of Argon 40 was confirmed. The results for the other noble gases are still being evaluated. Other hydrocarbons and nitriles were also observed and quantitative evaluation is in progress. Preliminary ratios for the major carbon and nitrogen isotopes were computed from methane and molecular nitrogen measurements.

  14. Cassini-Huygens Probe Gas Chromatograph Mass Spectrometer (GCMS) Experiment: First Results

    NASA Technical Reports Server (NTRS)

    Niemann, H.; Demick, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Raaen, E.; Way, S.; Atreya, S.; Carignan, G.; Bauer, S.

    2005-01-01

    The Huygens Probe of the Cassini Huygens Mission entered the atmosphere of the moon Titan on January 14, 2005. The GCMS was part of the instrument complement on the probe to measure in situ the chemical composition of the atmosphere during the probe descent and to support the Aerosol Collector Pyrolyzer (ACP) experiment by serving as detector for the pyrolization products. The GCMS collected data from an altitude of 146 km to ground impact for a time interval of 2hours and 37minutes. The Probe and the GCMS survived the ground impact and collected data for 1hour and 9 minutes on the surface in the near surface environment until signal loss by the orbiter. The major constituents of the lower atmosphere were found to be N2 and CH4. The methane-mixing ratio was found to increase below the turbopause, about 35 km altitude, monotonically toward the surface to levels near saturation. After surface impact a steep increase of the mixing ratio was observed suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. Other constituents were found to be in very low concentrations, below ppm levels. The presence of Argon 40 was confirmed. The results for the other noble gases are still being evaluated. Other hydrocarbons and nitriles were also observed and quantitative evaluation is in progress. Preliminary ratios for the major carbon and nitrogen isotopes were computed from methane and molecular nitrogen measurements. The instrument collected 5634 mass spectra during descent and 2692 spectra on the ground over a range of m/z from 2 to 141. Eight gas chromatograph samples were taken during the descent and two on the ground.

  15. Gas chromatographic and mass spectrometric investigations of organic residues from Roman glass unguentaria.

    PubMed

    Ribechini, Erika; Modugno, Francesca; Colombini, Maria Perla; Evershed, Richard P

    2008-03-07

    A combination of gas chromatographic (GC) and mass spectrometric (MS) techniques, including direct exposure-MS (DE-MS), high-temperature GC-MS (HTGC-MS) and GC-MS of neutral and acid fractions, was employed to study the composition and recognise origin of the organic materials used to manufacture balm residues surviving in a series of glass unguentaria recovered from excavations of a Roman villa (Villa B) in the ancient town of Oplontis (Naples, Italy). DE-MS provided comprehensive 'fingerprint' information on the solvent soluble components of the contents of the unguentaria, while GC-MS analyses provided detailed molecular compositions, highlighting the presence of a wide range of compound classes including mid- and long-chain fatty acids, long-chain hydroxy-acids, n-alkanols, alkandiols, n-alkanes, long-chain monoesters, phytosterols and diterpenoid acids. Characteristic biomarkers and their distributions indicate the presence of beeswax, Pinaceae resin and another wax, as the main organic constituents of all of the preparations examined. In particular, the occurrence of phytosterols and long-chain monoesters, in which the acyl moiety was not exclusively palmitic acid, suggested the presence of a second waxy-lipid constituent of plant origin. The results are consistent with beeswax being used in the preparation of the cosmetics preserved in the unguentaria, while the other lipids are most likely the residue of some as yet unidentified plant extract(s), possibly deriving from the cuticular waxes of flowers and/or leaves. The composition of the extracts are consistent with the ancient practices of maceration and/or "enfleurage", in which lipid-based materials, such as beeswax, animal fat or vegetables oils, were used to extract aromatic and fragrant substances from resin, flowers, spices and scented wood, in order to produce unguents and balms.

  16. Improved micromachined column design and fluidic interconnects for programmed high-temperature gas chromatography separations.

    PubMed

    Gaddes, David; Westland, Jessica; Dorman, Frank L; Tadigadapa, Srinivas

    2014-07-04

    This work focuses on the development and experimental evaluation of micromachined chromatographic columns for use in a commercial gas chromatography (GC) system. A vespel/graphite ferrule based compression sealing technique is presented using which leak-proof fluidic interconnection between the inlet tubing and the microchannel was achieved. This sealing technique enabled separation at temperatures up to 350°C on a μGC column. This paper reports the first high-temperature separations in microfabricated chromatographic columns at these temperatures. A 2m microfabricated column using a double Archimedean spiral design with a square cross-section of 100μm×100μm has been developed using silicon microfabrication techniques. The microfabricated column was benchmarked against a 2m 100μm diameter commercial column and the performance between the two columns was evaluated in tests performed under identical conditions. High temperature separations of simulated distillation (ASTM2887) and polycyclic aromatic hydrocarbons (EPA8310) were performed using the μGC column in temperature programmed mode. The demonstrated μGC column along with the high temperature fixture offers one more solution toward potentially realizing a portable μGC device for the detection of semi-volatile environmental pollutants and explosives without the thermal limitations reported to date with μGC columns using epoxy based interconnect technology.

  17. Gas chromatographic-mass spectrometric analysis of creosotes extracted from wooden sleepers installed in playgrounds

    SciTech Connect

    Rotard, W.; Mailahn, W.

    1987-01-01

    In order to evaluate their hygienic risk, wood samples from sleepers (railroad cross ties) impregnated with coal tar creosote were taken from playgrounds and investigated for hazardous compounds. The samples were extracted with ether, and acid-base-neutral separations were made on the creosote extracts. Water-soluble compounds were also isolated. All the fractions were investigated by capillary gas chromatography-mass spectrometry. Besides phenols in the acidic fractions and N-heterocyclic polynuclear aromatic hydrocarbons (PAH) in the basic fractions, high amounts of neutral PAH and also, in several samples high levels of carcinogenic and cocarcinogenic PAH were determined.

  18. Evaluation of two approaches to characterise liquid chromatographic columns using pharmaceutical separations.

    PubMed

    Dragovic, Sanja; Haghedooren, Erik; Németh, Tamás; Palabiyik, I Murat; Hoogmartens, Jos; Adams, Erwin

    2009-04-10

    In this paper a comparison of two column characterisation systems is reported: the method based on the hydrophobic-subtraction model of Dolan and Snyder (HS method) versus the method developed at the Katholieke Universiteit Leuven (KUL method). Comparison was done for seven different pharmaceutical separations (fluoxetine, gemcitabine, erythromycin, tetracycline, tetracaine, amlodipine and bisacodyl), using a set of 59 columns. A ranking was built based on an F value (KUL) or F(s) value (HS) versus a (virtual) reference column. Both methods showed similar probabilities of ranking patterns. Correlation of the respective test parameters of both approaches was poor. Both methods are not perfect and do not match well, but anyhow yield results which allow, with a relatively high certainty, the selection of similar or dissimilar columns as compared to a reference column. An analyst that uses either of the two methods will end up with a similar probability to choose an adequate column. From a practical point of view, it must be noted that the KUL method is easier to use.

  19. Preparation of weak cation exchange packings for chromatographic separation of proteins using "click chemistry''.

    PubMed

    Zhao, Kailou; Bai, Quan; Song, Chao; Wang, Fei; Yang, Fan

    2012-04-01

    "Click chemistry" is defined as a class of robust and selective chemical reactions affording high yields and is tolerant to a variety of solvents (including water), functional groups, and air. In this study, click chemistry was used as an effective strategy for coupling three alkyne-carboxylic acids onto the azide-silica to obtain three novel stationary phases of weak cation exchange chromatography, which were characterized with FTIR and elemental analysis. Six kinds of standard proteins, such as myoglobin, RNase A, RNase B, cytochrome C, α-chymotrypsin A, and lysozyme, were separated completely with the three novel weak cation exchange chromatography stationary phases. Compared with commercial weak cation exchange chromatography columns, the three kinds of novel weak cation exchange chromatography packings prepared by click chemistry approach have better resolution and selectivity. The mass recovery of more than 97% was obtained for all the tested proteins, and the bioactivity recovery of lysozyme on the prepared column was determined to be 96%. In addition, lysozyme was purified successfully from egg white with the novel weak cation exchange chromatography column by one step. The purity was more than 97% and a high specific activity was achieved to be 81 435 U/mg. The results illustrate the potential of click chemistry for preparing stationary phase for ion-exchange chromatography.

  20. Gas separation applications to METC-supported technologies

    SciTech Connect

    Poku, J.A.; Plunkett, J.E.

    1989-12-01

    The objectives of this study were to catalog both hot and cold gas separation technologies, to identify the status and the developers of each, and to identify how these separation processes might be applied to METC-supported technologies for removal of trace contaminants, or purification of gases used in or generated by coal processing. Discussions on gas separation process names, typical feeds, process developers, and operating conditions are provided in the following sections of this report, as well as descriptions of how these gas cleanup techniques would be used in developmental coal conversion technologies. 82 refs., 22 figs., 14 tabs.

  1. High-temperature separation with polymer-coated fiber in packed capillary gas chromatography.

    PubMed

    Saito, Yoshihiro; Ogawa, Mitsuhiro; Imaizumi, Motohiro; Ban, Kazuhiro; Abe, Akira; Takeichi, Tsutomu; Wada, Hiroo; Jinno, Kiyokatsu

    2005-06-01

    High-temperature gas chromatographic separation of several synthetic polymer mixtures with Dexsil-coated fiber-packed columns was studied. A bundle of heat-resistant filaments, Zylon, was longitudinally packed into a short metal capillary, followed by the conventional coating process with Dexsil 300 material. Prior to the packing process the metal capillary was deactivated by the formation of a silica layer. The typical size of the resulting column was 0.3-mm i.d., 0.5-mm o.d., 1-m length, and packed with about 170 filaments of the Dexsil-coated Zylon. The column temperature could be elevated up to 450 degrees C owing to the good thermal stability of the fiber, Dexsil coating, and metal capillary; furthermore, this allowed the separation of low-volatile compounds to be studied.

  2. Quantitative Mass Spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation

    PubMed Central

    Salama, Nahla N.; Wang, Shudong

    2009-01-01

    The present study employs time of flight mass and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL−1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%–102.75% was obtained. The method is accurate (% RE < 5%) and reproducible with intra- and inter-assay precision (RSD% < 8.0%). The quantification limit is 23.8 ng mL−1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs. PMID:19652756

  3. Quantitative mass spectrometric analysis of ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma without chromatographic separation.

    PubMed

    Salama, Nahla N; Wang, Shudong

    2008-05-28

    The present study employs time of flight mass and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL(-1) for both drugs. The correlation coefficient was >or=0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%-102.75% was obtained. The method is accurate (% RE < 5%) and reproducible with intra- and inter-assay precision (RSD% < 8.0%). The quantification limit is 23.8 ng mL(-1) for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.

  4. High-performance liquid chromatographic separation of paclitaxel intermediate phenylisoserine derivatives on macrocyclic glycopeptide and cyclofructan-based chiral stationary phases.

    PubMed

    Ilisz, István; Grecsó, Nóra; Forró, Enikő; Fülöp, Ferenc; Armstrong, Daniel W; Péter, Antal

    2015-10-10

    High-performance liquid chromatographic methods were developed for the separation of enantiomers of four unnatural paclitaxel precursor phenylisoserine analogs on chiral stationary phases containing macrocyclic glycopeptides and cyclofructans as chiral selectors. The effects of the mobile phase composition, the nature and concentration of different mobile phase additives (alcohols, amines and acids) in different chromatographic modes, temperature and the structures of the analytes on the separations were investigated. Separations were carried out at constant mobile phase compositions in the temperature range 10-50°C on macrocyclic antibiotic-based and 5-35°C on cyclofructan-based columns and the changes in enthalpy, Δ(ΔH°), entropy, Δ(ΔS°), and free energy, Δ(ΔG°), were calculated. The elution sequence was determined in most cases; no general rule could be observed.

  5. Liquid absorbent solutions for separating nitrogen from natural gas

    DOEpatents

    Friesen, Dwayne T.; Babcock, Walter C.; Edlund, David J.; Lyon, David K.; Miller, Warren K.

    2000-01-01

    Nitrogen-absorbing and -desorbing compositions, novel ligands and transition metal complexes, and methods of using the same, which are useful for the selective separation of nitrogen from other gases, especially natural gas.

  6. Gas Phase Chiral Separations By Ion Mobility Spectrometry

    PubMed Central

    Dwivedi, Prabha; Wu, Ching; Hill, Herbert H.

    2013-01-01

    This manuscript introduces the concept of Chiral Ion Mobility Spectrometry (CIMS) and presents examples demonstrating the gas phase separation of enantiomers of a wide range of racemates including pharmaceuticals, amino acids and carbohydrates. CIMS is similar to traditional ion mobility spectrometry (IMS), where gas phase ions, when subjected to a potential gradient are separated at atmospheric pressure due to differences in their shapes and sizes. In addition to size and shape, CIMS separates ions based on their stereospecific interaction with a chiral gas. In order to achieve chiral discrimination by CIMS, an asymmetric environment was provided by doping the drift gas with a volatile chiral reagent. In this study S-(+)-2-butanol was used as a chiral modifier to demonstrate enantiomeric separations of atenolol, serine, methionine, threonine, methyl-α-glucopyranoside, glucose, penicillamine, valinol, phenylalanine, and tryptophan from their respective racemic mixtures. PMID:17165808

  7. Gas-Liquid Flows and Phase Separation

    NASA Technical Reports Server (NTRS)

    McQuillen, John

    2004-01-01

    Common issues for space system designers include:Ability to Verify Performance in Normal Gravity prior to Deployment; System Stability; Phase Accumulation & Shedding; Phase Separation; Flow Distribution through Tees & Manifolds Boiling Crisis; Heat Transfer Coefficient; and Pressure Drop.The report concludes:Guidance similar to "A design that operates in a single phase is less complex than a design that has two-phase flow" is not always true considering the amount of effort spent on pressurizing, subcooling and phase separators to ensure single phase operation. While there is still much to learn about two-phase flow in reduced gravity, we have a good start. Focus now needs to be directed more towards system level problems .

  8. QbD-oriented development and validation of a bioanalytical method for nevirapine with enhanced liquid-liquid extraction and chromatographic separation.

    PubMed

    Beg, Sarwar; Chaudhary, Vandna; Sharma, Gajanand; Garg, Babita; Panda, Sagar Suman; Singh, Bhupinder

    2016-06-01

    The present studies describe the systematic quality by design (QbD)-oriented development and validation of a simple, rapid, sensitive and cost-effective reversed-phase HPLC bioanalytical method for nevirapine in rat plasma. Chromatographic separation was carried out on a C18 column using isocratic 68:9:23% v/v elution of methanol, acetonitrile and water (pH 3, adjusted by orthophosphoric acid) at a flow rate of 1.0 mL/min using UV detection at 230 nm. A Box-Behnken design was applied for chromatographic method optimization taking mobile phase ratio, pH and flow rate as the critical method parameters (CMPs) from screening studies. Peak area, retention time, theoretical plates and peak tailing were measured as the critical analytical attributes (CAAs). Further, the bioanalytical liquid-liquid extraction process was optimized using an optimal design by selecting extraction time, centrifugation speed and temperature as the CMPs for percentage recovery of nevirapine as the CAA. The search for an optimum chromatographic solution was conducted through numerical desirability function. Validation studies performed as per the US Food and Drug Administration requirements revealed results within the acceptance limit. In a nutshell, the studies successfully demonstrate the utility of analytical QbD approach for the rational development of a bioanalytical method with enhanced chromatographic separation and recovery of nevirapine in rat plasma. Copyright © 2015 John Wiley & Sons, Ltd.

  9. Sorption characteristics and chromatographic separation of gold (I and III) from silver and base metal ions using polyurethane foams.

    PubMed

    Farag, A B; Soliman, M H; Abdel-Rasoul, O S; el-Shahawi, M S

    2007-10-10

    The influence of different parameters on the sorption profiles of trace and ultra traces of gold (I) species from the aqueous cyanide media onto the solid sorbents ion exchange polyurethane foams (IEPUFs) and commercial unloaded polyurethane foams (PUFs) based polyether type has been investigated. The retention of gold (I) species onto the investigated solid sorbents followed a first-order rate equation with an overall rate constant k in the range 2.2-2.8+/-0.2 s(-1). The sorption data of gold (I) followed Freundlich and Langmuir isotherm models. Thus, the a dual-mode of sorption mechanism involving absorption related to "weak base anion exchanger" and an added component for "surface adsorption" seems the most likely proposed dual mechanism for retention profile of gold (I) by the IEPUFs and PUFs solid sorbents. The capacity of the IEPUFs and PUFs towards gold (I) sorption calculated from the sorption isotherms was found to be 11.21+/-1.8 and 5.29+/-0.9 mg g(-1), respectively. The chromatographic separation of the spiked inorganic gold (I) from de ionized water at concentrations 5-15 microg mL(-1) onto the developed IEPUFs and PUFs packed columns at 10 mL min(-1) flow rate was successfully achieved. The retained gold (I) species were then recovered quantitatively from the IEPUFs (98.4+/-2.4%, n=5) and PUFs (95.4+/-3.4%, n=5) packed columns using perchloric acid (60 mL, 1.0 mol L(-1)) as a proper eluting agent. Thiourea (1.0 mol L(-1))-H2SO4 (0.1 mol L(-1)) system was also used as eluting agent for the recovery of gold (I) from IEPUFS (95.4+/-5.4%, n=3) and also PUFs (93.4+/-4.4%, n=3) packed columns. The performance of the IEPUFs and PUFs packed columns in terms of the height equivalent to the theoretical plates (HETP), number of plates (N), and critical and breakthrough capacities towards gold (I) species were evaluated. The developed IEPUFs packed column was applied successfully for complete retention and recovery (98.5+/-2.7) of gold (III) species spiked onto

  10. Modified ion source triple quadrupole mass spectrometer gas chromatograph for polycyclic aromatic hydrocarbon analyses

    PubMed Central

    Anderson, Kim A.; Szelewski, Michael J.; Wilson, Glenn; Quimby, Bruce D.; Hoffman, Peter D.

    2015-01-01

    We describe modified gas chromatography electron-impact/triple-quadrupole mass spectrometry (GC–EI/MS/MS) utilizing a newly developed hydrogen-injected self-cleaning ion source and modified 9 mm extractor lens. This instrument, with optimized parameters, achieves quantitative separation of 62 polycyclic aromatic hydrocarbons (PAHs). Existing methods historically limited rigorous identification and quantification to a small subset, such as the 16 PAHs the US EPA has defined as priority pollutants. Without the critical source and extractor lens modifications, the off-the-shelf GC–EI/MS/MS system was unsuitable for complex PAH analysis. Separations were enhanced by increased gas flow, a complex GC temperature profile incorporating multiple isothermal periods, specific ramp rates, and a PAH-optimized column. Typical determinations with our refined GC–EI/MS/MS have a large linear range of 1–10,000 pg μl−1 and detection limits of <2 pg μl−1. Included in the 62 PAHs, multiple-reaction-monitoring (MRM) mode enabled GC-EI/MS/MS identification and quantitation of several constituents of the MW 302 PAHs isomers. Using calibration standards, values determined were within 5% of true values over many months. Standard curve r2 values were typically >0.998, exceptional for compounds which are archetypally difficult. With this method benzo[a]fluorene, benzo[b]fluorene, benzo[c]fluorene were fully separated as was benzo[b]fluoranthene, benzo[k]fluoranthene, and benzo[j]fluoranthene. Chrysene and triphenylene, were sufficiently separated to allow accurate quantitation. Mean limits of detection (LODs) across all PAHs were 1.02 ± 0.84 pg μl−1 with indeno[1,2,3-c,d] pyrene having the lowest LOD at 0.26 pg μl−1 and only two analytes above 2.0 pg μl−1; acenaphthalene (2.33 pg μl−1) and dibenzo[a,e]pyrene (6.44 pg μl−1). PMID:26454790

  11. In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water.

    PubMed

    Varanusupakul, Pakorn; Vora-Adisak, Narongchai; Pulpoka, Bancha

    2007-08-13

    An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 degrees C for 60 min with 20% Na2SO4. The linear calibration curves were observed for the concentrations ranging from 1 to 300 microg L(-1) with the correlation coefficients (R2) being greater than 0.99. The method detection limits of most analytes were below 1 microg L(-1) except DCAA and MCAA that were 2 and 18 microg L(-1), respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water.

  12. Process for separating aggressive gases from gas mixtures

    SciTech Connect

    Graham, T.E.

    1984-03-06

    A process for separating large percentages of aggressive gases such as carbon dioxide from low temperature gas mixtures wherein the gas mixture is passed through a plurality of treatment zones in series. In each treatment zone the gas mixture is first compressed to a pressure such that the partial pressure of the carbon dioxide is not greater than the critical carbon dioxide partial pressure and the compressed gas mixture is then brought into contact with a membrane more permeable to carbon dioxide than other gases of the mixture such that carbon dioxide permeates the membrane to the other side thereof. The gas mixture is maintained in contact with the membrane a sufficient time to lower the partial pressure of the carbon dioxide in the non-permeated gas mixture to less than about 40 percent of said critical carbon dioxide partial pressure. The process is especially useful for separating carbon dioxide from methane and other gases.

  13. Liquid chromatographic analysis of a formulated ester from a gas-turbine engine test

    NASA Technical Reports Server (NTRS)

    Jones, W. R., Jr.; Morales, W.

    1983-01-01

    Size exclusion chromatography (SEC) utilizing mu-Bondagel and mu-Styragel columns with a tetrahydrofuran mobile phase was used to determine the chemical degradation of lubricant samples from a gas-turbine engine test. A MIL-L-27502 candidate, ester-based lubricant was run in a J57-29 engine at a bulk oil temperature of 216 C. In general, the analyses indicated a progressive loss of primary ester, additive depletion, and formation of higher molecular weight material. An oil sample taken at the conclusion of the test showed a reversal of this trend because of large additions of new oil. The high-molecular-weight product from the degraded ester absorbed strongly in the ultraviolet region at 254 nanometers. This would indicate the presence of chromophoric groups. An analysis of a similar ester lubricant from a separate high-temperature bearing test yielded qualitatively similar results.

  14. 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.

  15. Preliminary results of investigations into the use of artificial neural networks for discriminating gas chromatograph mass spectra of remote samples

    NASA Technical Reports Server (NTRS)

    Geller, Harold A.; Norris, Eugene; Warnock, Archibald, III

    1991-01-01

    Neural networks trained using mass spectra data from the National Institute of Standards and Technology (NIST) are studied. The investigations also included sample data from the gas chromatograph mass spectrometer (GCMS) instrument aboard the Viking Lander, obtained from the National Space Science Data Center. The work performed to data and the preliminary results from the training and testing of neural networks are described. These preliminary results are presented for the purpose of determining the viability of applying artificial neural networks in discriminating mass spectra samples from remote instrumentation such as the Mars Rover Sample Return Mission and the Cassini Probe.

  16. Multiresidue method for the gas chromatographic determination of pesticides in honey after solid-phase extraction cleanup.

    PubMed

    Jansson, C

    2000-01-01

    A new multiresidue method is described for the determination of pesticides in honey. The method involves dissolution of the honey in a methanol-water mixture, followed by solid-phase extraction cleanup and gas chromatographic determination. Twenty-six pesticides used on flowering field crops, on flowering fruit and vegetables, or as acaricides to control Varroa jacobsoni in beehives are determined by the method. Recoveries from honey, spiked at 0.02-1.6 mg/kg, ranged from 85 to 127% with a relative standard deviation (RSD) of 2-16%, except for the RSD of 27% for captan at 0.05 mg/kg.

  17. Gas chromatographic/mass spectrometric analyses of unknown analytical response in imported Fava beans: 4-chloro-6-methoxyindole.

    PubMed

    Petzinger, G; Barry, T L; Roach, J A; Musser, S M; Sphon, J

    1995-01-01

    A halogenated unidentified analytical response (UAR) was encountered in a number of imported Fava bean samples during the Food and Drug Administration's routine pesticide-monitoring program. Gas chromatographic/mass spectrometric (GC/MS) analyses identified the halogenated component as 4-chloro-6-methoxyindole, a naturally occurring promutagen in Fava beans that has been linked to incidents of gastric cancer. Data from electron impact, positive and negative chemical ionization, collision-induced dissociation, and deuteration studies of this compound are presented, along with GC retention time data.

  18. Functionalized inorganic membranes for gas separation

    DOEpatents

    Ku, Anthony Yu-Chung; Ruud, James Anthony; Molaison, Jennifer Lynn; Schick, Louis Andrew ,; Ramaswamy, Vidya

    2008-07-08

    A porous membrane for separation of carbon dioxide from a fluid stream at a temperature higher than about 200.degree. C. with selectivity higher than Knudsen diffusion selectivity. The porous membrane comprises a porous support layer comprising alumina, silica, zirconia or stabilized zirconia; a porous separation layer comprising alumina, silica, zirconia or stabilized zirconia, and a functional layer comprising a ceramic oxide contactable with the fluid stream to preferentially transport carbon dioxide. In particular, the functional layer may be MgO, CaO, SrO, BaO, La.sub.2O.sub.3, CeO.sub.2, ATiO.sub.3, AZrO.sub.3, AAl.sub.2O.sub.4, A.sup.1FeO.sub.3, A.sup.1MnO.sub.3, A.sup.1CoO.sub.3, A.sup.1NiO.sub.3, A.sup.2HfO.sub.3, A.sup.3CeO.sub.3, Li.sub.2ZrO.sub.3, Li.sub.2SiO.sub.3, Li.sub.2TiO.sub.3 or a mixture thereof; wherein A is Mg, Ca, Sr or Ba; A.sup.1 is La, Ca, Sr or Ba; A.sup.2 is Ca, Sr or Ba; and A.sup.3 is Sr or Ba.

  19. Evaluation of Mars CO2 Capture and Gas Separation Technologies

    NASA Technical Reports Server (NTRS)

    Muscatello, Anthony C.; Santiago-Maldonado, Edgardo; Gibson, Tracy; Devor, Robert; Captain, James

    2011-01-01

    Recent national policy statements have established that the ultimate destination of NASA's human exploration program is Mars. In Situ Resource Utilization (ISRU) is a key technology required to ,enable such missions and it is appropriate to review progress in this area and continue to advance the systems required to produce rocket propellant, oxygen, and other consumables on Mars using the carbon dioxide atmosphere and other potential resources. The Mars Atmospheric Capture and Gas separation project is selecting, developing, and demonstrating techniques to capture and purify Martian atmospheric gases for their utilization for the production of hydrocarbons, oxygen, and water in ISRU systems. Trace gases will be required to be separated from Martian atmospheric gases to provide pure CO2 to processing elements. In addition, other Martian gases, such as nitrogen and argon, occur in concentrations high enough to be useful as buffer gas and should be captured as well. To achieve these goals, highly efficient gas separation processes will be required. These gas separation techniques are also required across various areas within the ISRU project to support various consumable production processes. The development of innovative gas separation techniques will evaluate the current state-of-the-art for the gas separation required, with the objective to demonstrate and develop light-weight, low-power methods for gas separation. Gas separation requirements include, but are not limited to the selective separation of: (1) methane and water from unreacted carbon oxides (C02-CO) and hydrogen typical of a Sabatier-type process, (2) carbon oxides and water from unreacted hydrogen from a Reverse Water-Gas Shift process, (3)/carbon oxides from oxygen from a trash/waste processing reaction, and (4) helium from hydrogen or oxygen from a propellant scavenging process. Potential technologies for the separations include' freezers, selective membranes, selective solvents, polymeric sorbents

  20. Thermophoretic separation of aerosol particles from a sampled gas stream

    DOEpatents

    Postma, Arlin K.

    1986-01-01

    A method for separating gaseous samples from a contained atmosphere that includes aerosol particles uses the step of repelling particles from a gas permeable surface or membrane by heating the surface to a temperature greater than that of the surrounding atmosphere. The resulting thermophoretic forces maintain the gas permeable surface clear of aerosol particles. The disclosed apparatus utilizes a downwardly facing heated plate of gas permeable material to combine thermophoretic repulsion and gravity forces to prevent particles of any size from contacting the separating plate surfaces.

  1. Continuous countercurrent chromatographic separator for the purification of sugars from biomass hydrolyzate. Final project report, July 1, 1996--September 30, 1997

    SciTech Connect

    Wooley, R J

    1997-12-01

    Production of pure sugars is required to enable production of fuels and chemicals from biomass feedstocks. Hydrolysis of cellulose and hemicellulose (principal constituents of biomass) produces sugars that can be utilized in various fermentation process to produce valuable chemicals. Unfortunately, the hydrolysis process also liberates chemicals from the biomass that can be toxic to the fermenting organisms. The two primary toxic components of biomass hydrolyzate are sulfuric acid (catalyst used in the hydrolysis) and acetic acid (a component of the feed biomass). In the standard batch chromatographic separation of these three components, sugar elutes in the middle. Batch chromatographic separations are not practical on a commercial scale, because of excess dilution and high capital costs. Because sugar is the {open_quotes}center product,{close_quotes} a continuous separation would require two costly binary separators. However, a single, slightly larger separator, configured to produce three products, would be more economical. This FIRST project develops a cost-effective method for purifying biomass hydrolyzate into fermentable sugars using a single continuous countercurrent separator to separate this ternary mixture.

  2. Development of fast enantioselective gas-chromatographic analysis using gas-chromatographic method-translation software in routine essential oil analysis (lavender essential oil).

    PubMed

    Bicchi, Carlo; Blumberg, Leonid; Cagliero, Cecilia; Cordero, Chiara; Rubiolo, Patrizia; Liberto, Erica

    2010-02-26

    The study aimed to find the best trade-off between separation of the most critical peak pair and analysis time, in enantioselective GC-FID and GC-MS analysis of lavender essential oil, using the GC method-translation approach. Analysis conditions were first optimized for conventional 25 m x 0.25 mm inner diameter (dc) column coated with 6(I-VII)-O-tert-butyldimethylsilyl-2(I-VII)-3(I-VII)-O-ethyl-beta-cyclodextrin (CD) as chiral stationary phase (CSP) diluted at 30% in PS086 (polymethylphenylpolysiloxane, 15% phenyl), starting from routine analysis. The optimal multi-rate temperature program for a pre-set column pressure was determined and then used to find the pressures producing the efficiency-optimized flow (EOF) and speed-optimized flow (SOF). This method was transferred to a shorter narrow-bore (NB) column (11 m x 0.10 mm) using method-translation software, keeping peak elution order and separation. Optimization of the enantioselective GC method with the translation approach markedly reduced the analysis time of the lavender essential oil, from about 87 min with the routine method to 40 min with an optimal multi-rate temperature program and initial flow with a conventional inner diameter column, and to 15 min with FID as detector or 13.5 min with MS with a corresponding narrow-bore column, while keeping enantiomer separation and efficiency.

  3. Prototype of the gas chromatograph-mass spectrometer to investigate volatile species in the lunar soil for the Luna-Resurs mission

    NASA Astrophysics Data System (ADS)

    Hofer, L.; Wurz, P.; Buch, A.; Cabane, M.; Coll, P.; Coscia, D.; Gerasimov, M.; Lasi, D.; Sapgir, A.; Szopa, C.; Tulej, M.

    2015-06-01

    In preparation for the Russian Luna-Resurs mission we combined our compact time-of-flight mass spectrometer (TOF-MS) with a chemical pre-separation of the species by gas chromatography (GC). Coupled measurements with both instruments were successfully performed with the prototype of the mass spectrometer and a flight-like gas chromatograph. The system was tested with two test gas mixtures, a mixture of hydrocarbons and a mixture of noble gases. Due to its capability to record mass spectra over the full mass range at once with high sensitivity and a dynamic range of up to 106 within 1 s, the TOF-MS system is a valuable extension of the GC analytical system. Based on the measurements with calibration gases performed with the combined GC-MS prototype and under assumption of mean characteristics for the Moon's regolith, the detection limit for volatile species in a soil sample is estimated to 2·10-10 by mass for hydrocarbons and 2·10-9 by mass for noble gases.

  4. High-resolution hydrodynamic chromatographic separation of large DNA using narrow, bare open capillaries: a rapid and economical alternative technology to pulsed-field gel electrophoresis?

    PubMed

    Liu, Lei; Veerappan, Vijaykumar; Pu, Qiaosheng; Cheng, Chang; Wang, Xiayan; Lu, Liping; Allen, Randy D; Guo, Guangsheng

    2014-01-07

    A high-resolution, rapid, and economical hydrodynamic chromatographic (HDC) method for large DNA separations in free solution was developed using narrow (5 μm diameter), bare open capillaries. Size-based separation was achieved in a chromatographic format with larger DNA molecules being eluting faster than smaller ones. Lambda DNA Mono Cut Mix was baseline-separated with the percentage resolutions generally less than 9.0% for all DNA fragments (1.5 to 48.5 kbp) tested in this work. High efficiencies were achieved for large DNA from this chromatographic technique, and the number of theoretical plates reached 3.6 × 10(5) plates for the longest (48.5 kbp) and 3.7 × 10(5) plates for the shortest (1.5 kbp) fragments. HDC parameters and performances were also discussed. The method was further applied for fractionating large DNA fragments from real-world samples (SacII digested Arabidopsis plant bacterial artificial chromosome (BAC) DNA and PmeI digested Rice BAC DNA) to demonstrate its feasibility for BAC DNA finger printing. Rapid separation of PmeI digested Rice BAC DNA covering from 0.44 to 119.041 kbp was achieved in less than 26 min. All DNA fragments of these samples were baseline separated in narrow bare open capillaries, while the smallest fragment (0.44 kbp) was missing in pulsed-field gel electrophoresis (PFGE) separation mode. It is demonstrated that narrow bare open capillary chromatography can realize a rapid separation for a wide size range of DNA mixtures that contain both small and large DNA fragments in a single run.

  5. Classification of gasoline by octane number and light gas condensate fractions by origin with using dielectric or gas-chromatographic data and chemometrics tools.

    PubMed

    Rudnev, Vasiliy A; Boichenko, Alexander P; Karnozhytskiy, Pavel V

    2011-05-15

    The approach for classification of gasoline by octane number and light gas condensate fractions by origin with using dielectric permeability data has been proposed and compared with classification of same samples on the basis of gas-chromatographic data. The precision of dielectric permeability measurements was investigated by using ANOVA. The relative standard deviation of dielectric permeability was in the range from 0.3 to 0.5% for the range of dielectric permeability from 1.8 to 4.4. The application of exploratory chemometrics tools (cluster analysis and principal component analysis) allow to explicitly differentiate the gasoline and light gas condensate fractions into groups of samples related to specific octane number or origin. The neural networks allow to perfectly classifying the gasoline and light gas condensate fractions.

  6. Measurement of dissolved H2, O2, and CO2 in groundwater using passive samplers for gas chromatographic analyses.

    PubMed

    Spalding, B P; Watson, D B

    2006-12-15

    A simple in-situ passive dissolved gas groundwater sampler, comprised of a short length of silicone tubing attached to a gastight or other syringe, was adapted and tested for in-situ collection of equilibrium gas samples. Sampler retrieval after several days of immersion in groundwater allowed the direct injection of the sample onto a gas chromatograph (GC), simplifying field collection and sample handling over the commonly used "bubble stripping" method for H2 analyses. A GC was modified by sequencing a thermal conductivity (TC) detector followed by a reductive gas (RG) detector so that linear calibration of H2 over the range 0.2-200,000 ppmv was attained using a 0.5-mL gas sample; inclusion of the TC detector allowed the simultaneous quantification of other fixed gases (O2, CO2, He, and Ne) to which the RG detector was not responsive. Uptake kinetics for H2 and He indicated that the passive sampler reached equilibrium within 12 h of immersion in water. Field testing of these passive samplers revealed unusually large equilibrium gas-phase H2 concentrations in groundwater, ranging from 0.1 to 13.9%, by volume, in 11 monitoring wells surrounding four former radiological wastewater disposal ponds at the Y-12 plant in Oak Ridge, Tennessee.

  7. Evaluation of poly(90% biscyanopropyl/10% cyanopropylphenyl siloxane) capillary columns for the gas chromatographic quantification of trans fatty acids in non-hydrogenated vegetable oils.

    PubMed

    Delmonte, Pierluigi

    2016-08-19

    Current gas chromatographic (GC) methods for the analysis of fatty acids (FA) were optimized primarily for the quantification of the trans 18:1 FAs (18:1 tFAs) produced during the partial hydrogenation of fats and oils. Recent regulatory action regarding the application of partial hydrogenation in the processing of edible fats and oils may reshape the FA composition of these products. The higher content in 18:3 tFAs compared to 18:1 tFAs of most refined non-hydrogenated vegetable oils (RNHVO), and the challenge in their quantification applying current methods, suggest the need for new methodologies. This manuscript describes a simple GC method for the analysis of FAs in RNHVOs utilizing a 100m (0.25mm I.D.) capillary column coated with poly(90% biscyanopropyl/10% cyanopropylphenyl siloxane) (90% BCS). The optimization of the chromatographic conditions and the detection of co-eluting compounds were carried out by applying comprehensive two dimensional gas chromatography with online reduction (GC-OR×GC). Results showed that 90% BCS capillary columns operated at the elution temperature of 162°C provide the separation of the 18:1, 18:2 and 18:3 tFAs, contained in RNHVOs, from other components. A minor constituent of Canola oil, 16:3n-3, partially co-eluted with trans-18:1 FAMEs. This simple GC method showed the ability to measure trans-fat in RNHVOs at the level of 0.5g/100g, providing comparable quantitative results to the more complex GC×GC methodology.

  8. Solid phase micro extraction - A new technique coupled with gas chromatograph for chloroethene analysis from aqueous samples

    SciTech Connect

    Xu, N.; Sewell, G.W.

    1996-10-01

    Once the chloroethenes (tetrachloroethene and trichloroethene) contamination occurs in the subsurface environment, they tend to retain and form a Pollution plum in the aquifer because of their recalcitrance to aerobic oxidation. Currently, the most promising bioremediation method for chlorinated compounds is through anaerobic reductive biotransformation, in which each chlorine is replaced by a hydrogen. To study the biodegradation process, it is essential to monitor tetrachloroethene and its degradation daughter products frequently. An analytical method has been modified for chloroethene analysis by gas chromatography. Solid Phase Micro Extraction technique has been used to extract aqueous sample onto a fiber and then to desorb the sample directly into a gas chromatograph injection port. The total run time is less than 17 minutes.

  9. Development of a switchable multidimensional/comprehensive two-dimensional gas chromatographic analytical system.

    PubMed

    Maikhunthod, Bussayarat; Morrison, Paul D; Small, Darryl M; Marriott, Philip J

    2010-02-26

    In this study, a new system for analysis using a dual comprehensive two-dimensional gas chromatography/targeted multidimensional gas chromatography (switchable GC x GC/targeted MDGC) analysis was developed. The configuration of this system not only permits the independent operation of GC, GC x GC and targeted MDGC analyses in separate analyses, but also allows the mode to be switched from GC x GC to targeted MDGC any number of times through a single analysis. By incorporating a Deans switch microfluidics transfer module prior to a cryotrapping device, the flow stream from the first dimension column can be directed to either one of two second dimension columns in a classical heart-cutting operation. Both second columns pass through the cryotrap to allow solute bands to be focused and then rapidly remobilized to the respective second columns. A short second column enables GC x GC operation, whilst a longer column is used for targeted MDGC. Validation of the system was performed using a standard mixture of compounds relevant to essential oil analysis, and then using compounds present at different abundances in lavender essential oil. Reproducibility of retention times and peak area responses demonstrated that there was negligible variation in the system over the course of multiple heart-cuts, and proved the reliable operation of the system. An application of the system to lavender oil, as a more complex sample, was carried out to affirm system feasibility, and demonstrate the ability of the system to target multiple components in the oil. The system was proposed to be useful for study of aroma-impact compounds where GC x GC can be incorporated with MDGC to permit precise identification of aroma-active compounds, where heart-cut multidimensional GC-olfactometry detection (MDGC-O) is a more appropriate technology for odour assessment.

  10. Gas chromatographic metabolic profiling: a sensitive tool for functional microbial ecology.

    PubMed

    Coucheney, Elsa; Daniell, Tim J; Chenu, Claire; Nunan, Naoise

    2008-12-01

    Microbial metabolomics, which consists of a non-targeted analysis of the metabolites released from ('exometabolome') or existing in ('endometabolome') a cell has mostly been used to study the metabolism of particular microbes. Metabolomes also represent a picture of microbial activity and we suggest that the exometabolome may also contain pertinent information for studying microbial interaction networks. Gas chromatography coupled to mass spectrometry is the most commonly used technique in metabolomics studies. It allows a wide range of metabolites to be detected but requires the derivatisation of compounds prior to detection. This type of non-targeted analysis can introduce biases to the detection and quantification of the different metabolites, particularly at the extraction and derivatisation steps. The aims of this study, therefore, were to quantify the sources of variability and to test the sensitivity of the GC metabolic profiling approach to small environmental changes such as shifts in temperature. The temperature sensitivity of metabolic profiles was compared with that of catabolic profiles obtained using Biolog microplates. Analytical variability was compared with biological variability by incubating bacterial strains isolated from soil with fructose at 20 degrees C and by replicating each step of the protocol (incubation, extraction and derivatisation). For both the endo- and the exometabolome, more than 70% of the total variability was of biological origin and principal components analysis clearly separated the strains along the first ordination axis. The endometabolome distinguished bacterial strains at the species level only, whereas separation was evident at the species and group level with the exometabolome. Temperature had a significant but differential effect on the metabolite production of the bacterial strains whilst their catabolic profiles remained relatively unaffected. The exometabolome was more sensitive to temperature shifts than the

  11. [Development of an automatic vacuum liquid chromatographic device and its application in the separation of the components from Schisandra chinensis (Turz) Baill].

    PubMed

    Zhu, Jingbo; Liu, Baoyue; Shan, Shibo; Ding, Yanl; Kou, Zinong; Xiao, Wei

    2015-08-01

    In order to meet the needs of efficient purification of products from natural resources, this paper developed an automatic vacuum liquid chromatographic device (AUTO-VLC) and applied it to the component separation of petroleum ether extracts of Schisandra chinensis (Turcz) Baill. The device was comprised of a solvent system, a 10-position distribution valve, a 3-position changes valve, dynamic axis compress chromatographic columns with three diameters, and a 10-position fraction valve. The programmable logic controller (PLC) S7- 200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection, separation time setting and fraction collection. The separation results showed that six fractions (S1-S6) of different chemical components from 100 g Schisandra chinensis (Turcz) Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The initial mobile phase of AUTO-VLC was selected by taking Rf of all the target compounds ranging from 0 to 0.45 for fist development on the TLC; gradient elution ratio was selected according to k value (the slope of the linear function of Rf value and development times on the TLC) and the resolution of target compounds; elution times (n) were calculated by the formula n ≈ ΔRf/k. A total of four compounds with the purity more than 85% and 13 other components were separated from S5 under the selected conditions for only 17 h. Therefore, the development of the automatic VLC and its method are significant to the automatic and systematic separation of traditional Chinese medicines.

  12. Gas chromatographic isolation of individual compounds from complex matrices for radiocarbon dating

    SciTech Connect

    Eglinton, T.I.; Aluwihare, L.I.; McNichol, A.P.; Bauer, J.E.; Druffel, E.R.M.

    1996-03-01

    This paper describes the application of a novel, practical approach for isolation of individual compounds from complex organic matrices for natural abundance radiocarbon measurement. This is achieved through the use of automated pereparative capillary gas chromatography (PCGC) to separate and recover sufficient quantities of individual target compounds for {sup 14}C analysis by accelerator mass spectrometry (AMS). We developed and tested this approach using a suite of samples (plant lipids, petroleums) whose ages spanned the {sup 14}C time scale and which contained a variety of compound types (fatty acids, sterols, hydrocarbons). Comparison of individual compound and bulk radiocarbon signatures for the isotopically homogeneous samples studied revealed that {Delta}{sup 14}C values generally agreed well ({+-}10%). Background contamination was assessed at each stage of the isolation procedure, and incomplete solvent removal prior to combustion was the only significant source of additional carbon. Isotope fractionation was addressed through compound-specific stable carbon isotopic analyses. Fractionation of isotopes during isolation of individual compounds was minimal (<5% for {delta}{sup 13}C), provided the entire peak was collected during PCGC. Trapping of partially coeluting peaks did cause errors, and these results highlight the importance of conducting stable carbon isotopic measurements of each trapped compound in concert with AMS for reliable radiocarbon measurements. 29 refs., 9 figs., 2 tabs.

  13. Advanced Sorbents as a Versatile Platform for Gas Separation

    SciTech Connect

    Neil Stephenson

    2003-09-30

    The program objective was to develop materials and processes for industrial gas separations to reduce energy use and enable waste reduction. The approach chosen combined novel oxygen selective adsorbents and pressure swing adsorption (PSA) processes. Preliminary materials development and process simulation results indicated that oxygen selective adsorbents could provide a versatile platform for industrial gas separations. If fully successful, this new technology offered the potential for reducing the cost of producing nitrogen/oxygen co-products, high purity nitrogen, argon, and possibly oxygen. The potential energy savings for the gas separations are appreciable, but the end users are the main beneficiaries. Lowering the cost of industrial gases expands their use in applications that can employ them for reducing energy consumption and emissions.

  14. Refined separation of combined Fe–Hf from rock matrices for isotope analyses using AG-MP-1M and Ln-Spec chromatographic extraction resins

    PubMed Central

    Cheng, Ting; Nebel, Oliver; Sossi, Paolo A.; Chen, Fukun

    2014-01-01

    A combined procedure for separating Fe and Hf from a single rock digestion is presented. In a two-stage chromatographic extraction process, a purified Fe fraction is first quantitatively separated from the rock matrix using AG-MP-1M resin in HCl. Hafnium is subsequently isolated using a modified version of a commonly applied method using Eichrom LN-Spec resin. Our combined method includes:•Purification of Fe from the rock matrix using HCl, ready for mass spectrometric analysis.•Direct loading of the matrix onto the resin that is used for Hf purification.•Collection of a Fe-free Hf fraction. PMID:26150946

  15. An efficient polymer molecular sieve for membrane gas separations.

    PubMed

    Carta, Mariolino; Malpass-Evans, Richard; Croad, Matthew; Rogan, Yulia; Jansen, Johannes C; Bernardo, Paola; Bazzarelli, Fabio; McKeown, Neil B

    2013-01-18

    Microporous polymers of extreme rigidity are required for gas-separation membranes that combine high permeability with selectivity. We report a shape-persistent ladder polymer consisting of benzene rings fused together by inflexible bridged bicyclic units. The polymer's contorted shape ensures both microporosity-with an internal surface area greater than 1000 square meters per gram-and solubility so that it is readily cast from solution into robust films. These films demonstrate exceptional performance as molecular sieves with high gas permeabilities and good selectivities for smaller gas molecules, such as hydrogen and oxygen, over larger molecules, such as nitrogen and methane. Hence, this polymer has excellent potential for making membranes suitable for large-scale gas separations of commercial and environmental relevance.

  16. Ceramic membranes for gas separation at high temperatures. Final report

    SciTech Connect

    Wang, C.J.

    1994-03-01

    Superior heat, wear, erosion, and corrosion resistance of ceramic materials have motivated the studies of processing-structure-performance interrelationships of ceramic membranes for high temperature gas separations. A literature review on pore transport mechanisms, physical structure of membranes, and module configuration of industrial membrane processes has been made to obtain a better understanding of membrane performance in gas separations. The research experience in decomposing polymer resins for ablative composites has stimulated a research interest in developing a dynamic model for membrane processes, incorporating a temperature effects on material and fluid properties. Brief summaries of the reviewed literature, permeability experiments, and process modeling are presented in this report.

  17. Porous liquids: A promising class of media for gas separation

    SciTech Connect

    Zhang, Jinshui; Chai, Song -Hai; Qiao, Zhen -An; Mahurin, Shannon M.; Chen, Jihua; Fang, Youxing; Wan, Shun; Nelson, Kimberly; Zhang, Pengfei; Dai, Sheng

    2014-11-17

    In porous liquids with empty cavities we successfully has been successfully fabricated by surface engineering of hollow structures with suitable corona and canopy species. By taking advantage of the liquid-like polymeric matrices as a separation medium and the empty cavities as gas transport pathway, this unique porous liquid can function as a promising candidate for gas separation. A facile synthetic strategy can be further extended to other types of nanostructure-based porous liquid fabrication, opening up new opportunities for preparation of porous liquids with attractive properties for specific tasks.

  18. Microporous organic polymers for gas storage and separation applications.

    PubMed

    Chang, Ze; Zhang, Da-Shuai; Chen, Qiang; Bu, Xian-He

    2013-04-21

    Microporous organic polymers (MOPs), an emerging class of functional porous materials featured with the pure organic component have been widely studied in recent years. These materials have potential uses in areas such as storage, separation, and catalysis. In this Perspective, we focused on the gas storage and separation of MOPs. The targeted design and synthesis of MOPs toward the enhancement of gas capacity and selectivity are discussed. Furthermore, special emphasis is given to the post-synthesis modification of MOPs which have been proved to be effective methods to accurately tune the desired properties.

  19. Sulfolane-Cross-Polybenzimidazole Membrane For Gas Separation

    SciTech Connect

    Young, Jennifer S.; Long, Gregory S.; Espinoza, Brent F.

    2006-02-14

    A cross-linked, supported polybenzimidazole membrane for gas separation is prepared by reacting polybenzimidazole (PBI) with the sulfone-containing crosslinking agent 3,4-dichloro-tetrahydro-thiophene-1,1-dioxide. The cross-linked reaction product exhibits enhanced gas permeability to hydrogen, carbon dioxide, nitrogen, and methane as compared to the unmodified analog, without significant loss of selectivity, at temperatures from about 20 degrees Celsius to about 400 degrees Celsius.

  20. Separation of gas from solvent by membrane technology

    SciTech Connect

    Beaupre, R.F.; Jung, D.Y.

    1991-02-26

    This patent describes the method of separating a charge rich liquid containing gas dissolved in solvent. It comprises: maintaining the charge rich liquid containing gas dissolved in solvent therefore in liquid phase in contact with a gas-permeable, essentially solvent impermeable membrane of pore size of less than about 1000 A and molecular weight cutoff of below about 1,000 selected from the group consisting of cellulose acetate membrane, hydrolyzed cellulose membrane, and polyethyleneimine membrane, and; maintaining a pressure drop across the gas-permeable essentially solvent-impermeable membrane; passing the gas from the charge rich liquid containing gas dissolved in solvent therefore at the higher pressure side of the membrane through the membrane thereby forming lean liquid containing decreased quantities of gas dissolved in solvent on the higher pressure side of the membrane and, on the lower pressure side of the membrane, gas containing decreased quantities of liquid; recovering lean liquid containing decreased quantities of gas dissolved in solvent from the high pressure side of the membrane; and recovering gas containing decreased quantities of liquid from the lower pressure side of the membrane.

  1. Separation of Carbon Dioxide from Flue Gas Using Ion Pumping

    SciTech Connect

    Aines, R; Bourcier, W L; Johnson, M R

    2006-04-21

    We are developing a new way of separating carbon dioxide from flue gas based on ionic pumping of carbonate ions dissolved in water. Instead of relying on large temperature or pressure changes to remove carbon dioxide from solvent used to absorb it from flue gas, the ion pump increases the concentration of dissolved carbonate ion in solution. This increases the overlying vapor pressure of carbon dioxide gas, which can be removed from the downstream side of the ion pump as a nearly pure gas. This novel approach to increasing the concentration of the extracted gas permits new approaches to treating flue gas. The slightly basic water used as the extraction medium is impervious to trace acid gases that destroy existing solvents, and no pre-separation is necessary. The simple, robust nature of the process lends itself to small separation plants. Although the energy cost of the ion pump is significant, we anticipate that it will be compete favorably with the current 35% energy penalty of chemical stripping systems in use at power plants. There is the distinct possibility that this simple method could be significantly more efficient than existing processes.

  2. Equations for nickel-chromium wire heaters of column transfer lines in gas chromatographic-electroantennographic detection (GC-EAD).

    PubMed

    Byers, John A

    2004-05-30

    Heating of chromatographic columns, transfer lines, and other devices is often required in neuroscience research. For example, volatile compounds passing through a capillary column of a gas chromatograph (GC) can be split, with half exiting the instrument through a heated transfer line to an insect antenna or olfactory sensillum for electroantennographic detector (GC-EAD) recordings. The heated transfer line is used to prevent condensation of various chemicals in the capillary that would otherwise occur at room temperature. Construction of such a transfer line heater is described using (80/20%) nickel-chromium heating wire wrapped in a helical coil and powered by a 120/220 V ac rheostat. Algorithms were developed in a computer program to estimate the voltage at which a rheostat should be set to obtain the desired heater temperature for a specific coil. The coil attributes (radius, width, number of loops, or length of each loop) are input by the user, as well as AWG size of heating wire and desired heater temperature. The program calculates total length of wire in the helix, resistance of the wire, amperage used, and the voltage to set the rheostat. A discussion of semiochemical isolation methods using the GC-EAD and bioassays is presented.

  3. Capillary gas chromatographic determination of prometryn and its degradation products in parsley.

    PubMed

    Bardalaye, P C; Wheeler, W B

    1985-01-01

    Residue analysis of the herbicide prometryn (2,4-bis(isopropylamino)-6-methylthio-1,3,5-triazine) is widely known, but an analytical method for determining its metabolities or degradation products in addition to the parent chemical has not yet been reported in the literature. The procedure reported here is for the extraction and determination of prometryn and 2 metabolites, 2-amino-4-isopropylamino-6-methyl-thio-1,3,5-triazine and 2,4-diamino-6-methylthio-1,3,5-triazine, in parsley. Crops were extracted with 2-propanol followed by concentration of the extract and partitioning with a minimum amount of hexane in the presence of a large excess of water to remove most of the green pigment. The aqueous phase was divided into 2 equal halves: (A) One-half portion was partitioned with dichloromethane in the presence of saturated sodium chloride solution, the dichloromethane phase was separated, and the aqueous phase was discarded. The organic solvent was evaporated, and the contents were reconstituted in petroleum ether before prometryn analysis. (B) The other half was made slightly alkaline with ammonium hydroxide solution and was partitioned with ethyl acetate in the presence of saturated sodium chloride solution. The ethyl acetate phase was concentrated, centrifuged to remove any turbidity, and analyzed for the 2 metabolities above. Fused silica capillary gas chromatography (GC) with nitrogen-phosphorus (N-P) detection was used for quantitation. The limit of detection was 0.05 mg/kg for all the compounds examined. Recoveries from fortified parsley samples ranged from 59 to 73% at fortification levels of 0.05 to 1.0 mg/kg.

  4. Determination of volatile organic compounds in ambient air with gas chromatograph-flame ionization and ion trap detection

    SciTech Connect

    Liu, S.; Carley, R.J.; Kang, J.; Chen, J.; Stuart, J.D.

    1994-12-31

    Two new techniques are utilized to integrate the following three equipments: an Entech 2000 automated air concentrator, a Hewlett Packard gas chromatograph (GC) with flame ionization detector (FID) and an ion trap mass spectrometer detector (ITD). This combined analytical system is used to determine low ppb level volatile organic compounds (VOC) in ambient air. The first technique is to configure the inlet system of the GC, so that the pressure regulated flow control system of the GC injection port is used to control the flow of both the desorb gas of the automated air concentrator and the carrier gas of the GC column. The injection port still can be used to inject gas and liquid samples directly. The second technique is to split the effluent of GC column at a 1:1 ratio to the ITD and the FID. In this way, both FID and ITD data can be obtained for each analysis. For ambient air non-methane hydrocarbons monitoring, the FID detector is widely used. Oxygen containing and halogenated organic compounds cannot be differentiated by FID detector and would be quantified as coeluting hydrocarbons. However, volatile organic compounds other than target hydrocarbons can be identified by ITD. This analytical system is very valuable research tool for non-methane hydrocarbons and urban air toxic monitoring. The performances of this developed system have been presented.

  5. Process for separating carbon dioxide from flue gas using sweep-based membrane separation and absorption steps

    DOEpatents

    Wijmans, Johannes G.; Baker, Richard W.; Merkel, Timothy C.

    2012-08-21

    A gas separation process for treating flue gases from combustion processes, and combustion processes including such gas separation. The invention involves routing a first portion of the flue gas stream to be treated to an absorption-based carbon dioxide capture step, while simultaneously flowing a second portion of the flue gas across the feed side of a membrane, flowing a sweep gas stream, usually air, across the permeate side, then passing the permeate/sweep gas to the combustor.

  6. Ligand-modified metal clusters for gas separation and purification

    DOEpatents

    Okrut, Alexander; Ouyang, Xiaoying; Runnebaum, Ron; Gates, Bruce C.; Katz, Alexander

    2017-02-21

    Provided is an organic ligand-bound metal surface that selects one gaseous species over another. The species can be closely sized molecular species having less than 1 Angstrom difference in kinetic diameter. In one embodiment, the species comprise carbon monoxide and ethylene. Such organic ligand-bound metal surfaces can be successfully used in gas phase separations or purifications, sensing, and in catalysis.

  7. Poly(triallyl isocyanurate-co-ethylene dimethacrylate-co-alkyl methacrylate) stationary phases in the chromatographic separation of hydrophilic solutes.

    PubMed

    Lin, Cheng-Lan; Singco, Brenda; Wu, Ching-Yi; Liang, Pei-Zhu; Cheng, Yi-Jie; Huang, Hsi-Ya

    2013-01-11

    This study describes the ability of triallyl isocyanurate (TAIC)-co-methacrylate ester polymer monoliths as stationary phases for the separation of hydrophilic compounds (phenolic acids, amino acids and catecholamines) in capillary electrochromatography (CEC) and ultra high pressure liquid chromatography (UHPLC). Several TAIC-co-methacrylate ester polymer monoliths prepared by single-step in situ copolymerization of TAIC, ethylene dimethacrylate (EDMA) and 2-acrylamido-2-methylpropane sulfonic acid (AMPS), with or without alkyl methacrylates were characterized by examining the SEM image, surface area, contact angle, and the thermal decomposition temperature. Compared to the conventional methacrylate ester-based monoliths, these proposed monoliths possessed hydrophilic character thus increased wettability which improved chromatographic separation selectivity of polar phenolic acids. Among the proposed TAIC-co-methacrylate monoliths, poly(TAIC-co-EDMA-AMPS-co-stearyl methacrylate (SMA)) showed separation selectivity with an increased analyte resolution from 0.0 to 0.92 for 4-hydroxybenzoic acid and vanillic acid, which were consistently difficult to resolve in the reversed-phase chromatographic mechanism of these monoliths in aqueous mobile phases. Moreover, stable ionization efficiencies were observed when this monolith was combined with ESI-MS detector possibly because an organic solvent-rich sheath liquid was used in the CEC-MS. This study demonstrates the potentiality of novel TAIC-co-methacrylate polymer monoliths in hydrophilic solute separation either in CEC or UHPLC mode.

  8. Ambient Atmospheric Hydrocarbon Content as Determined by Gas Chromatographic Techniques from Rural Tidewater Virginia in Late Spring 1974

    NASA Technical Reports Server (NTRS)

    Copeland, G. E.; Davis, R.; Maroulis, P.; Bandy, A. R.; Denyszyn, R.; Kindle, E. C.

    1975-01-01

    In an attempt to ascertain the naturally generated hydrocarbon contribution to the air quality of the Hampton Roads region of Tidewater Virginia, a series of 27 air samples was obtained in two rural locations during late spring of 1974. These samples were analyzed for their hydrocarbon content (carbon number range C5 to C10) using gas chromatographic techniques. The thirty different hydrocarbon species were identified and monitored in the experiment. Preliminary analysis of the data indicates an average concentration of 397 parts per billion by weight (carbon) for the total non-methane hydrocarbon loading for C5 to C10 during the experiment. This value exceeds the National Primary Air Quality Standards as set by the Environmental Protection Agency.

  9. Gas chromatographic/mass spectrometric analysis of morphine and codeine in human urine of poppy seed eaters.

    PubMed

    elSohly, H N; Stanford, D F; Jones, A B; elSohly, M A; Snyder, H; Pedersen, C

    1988-03-01

    In this study, poppy seeds were examined for a natural constituent that might serve as a maker for the seeds' ingestion as opposed to opiate abuse. Thebaine was selected as possible marker, since it was found to be a component of all poppy seeds examined and was not a natural component of different heroin samples. During the course of this investigation, a new extraction and cleanup procedure was developed for the gas chromatographic/nitrogen phosphorus detection (GC/NPD) and gas chromatographic/mass spectrometric (GC/MS) analysis of morphine and codeine in urine. A linear response, over a concentration range of 25 to 600 ng/mL, was obtained for codeine and morphine (r = 0.9982 and 0.9947, respectively). The minimum detectable level (LOD) and limit of quantitation (LOQ) for morphine were 10 and 30 ng/mL, respectively; whereas LOD and LOQ for codeine were 2 and 8 ng/mL, respectively. The coefficients of variance (CV, n = 6) for morphine and codeine analyses at the 100-ng/mL level were 13.3 and 4.6%, respectively. This procedure was used for the analysis of urine samples from five poppy seed eaters who each ingested 200 g of poppy seed cake. Results indicated that significant amounts of morphine and codeine are excreted in urine and that in all subjects, at least at one point in time, the apparent morphine concentration as determined by radioimmunoassay (RIA) analysis exceeded the cutoff value (300 ng/mL) established for screening. Thebaine was not detected in urine specimens collected following poppy seeds ingestion and thus could not be used as a marker.

  10. Gas adsorption and gas mixture separations using mixed-ligand MOF material

    DOEpatents

    Hupp, Joseph T.; Mulfort, Karen L.; Snurr, Randall Q.; Bae, Youn-Sang

    2011-01-04

    A method of separating a mixture of carbon dioxiode and hydrocarbon gas using a mixed-ligand, metal-organic framework (MOF) material having metal ions coordinated to carboxylate ligands and pyridyl ligands.

  11. Evaluation of a gas chromatograph with a novel surface acoustic wave detector (SAW GC) for screening of volatile organic compounds in Hanford waste tank samples

    SciTech Connect

    Lockrem, L.L.

    1998-01-12

    A novel instrument, a gas chromatograph with a Surface Acoustic Wave Detector (SAW GC), was evaluated for the screening of organic compounds in Hanford tank headspace vapors. Calibration data were developed for the most common organic compounds, and the accuracy and precision were measured with a certified standard. The instrument was tested with headspace samples collected from seven Hanford waste tanks.

  12. Integration of gas chromatographs into the Federal Highway Administration/Environmental Protection Agency near road MSAT study in Las Vegas, NV

    EPA Science Inventory

    This paper documents the technical evaluation of a semi-continuous gas chromatograph (GC) for the measurement of benzene and 1,33butadiene in the near road environment. This paper will also consider the some of the non-technical implications associated with the operation of a GC ...

  13. A water extraction, static headspace sampling, gas chromatographic method to determine MTBE in heating oil and diesel fuel.

    PubMed

    Cummins, T M; Robbins, G A; Henebry, B J; Goad, C R; Gilbert, E J; Miller, M E; Stuart, J D

    2001-03-15

    A method was developed to determine the fuel/water partition coefficient (KMTBE) of methyl tert-butyl ether (MTBE) and then used to determine low parts per million concentrations of MTBE in samples of heating oil and diesel fuel. A special capillary column designed for the separation of MTBE and to prevent coelution and a gas chromatograph equipped with a photoionization detector (PID) were used. MTBE was partitioned from fuel samples into water during an equilibration step. The water samples were then analyzed for MTBE using static headspace sampling followed by GC/PID. A mathematical relationship was derived that allowed a KMTBE value to be calculated by utilizing the fuel/water volume ratios and the corresponding PID signal. KMTBE values were found to range linearly from 3.8 to 10.9 over a temperature range of 5-40 degrees C. This analysis method gave a MDL of 0.7 ppm MTBE in the fuel and a relative average accuracy of +/-15% by comparison with an independent laboratory using purge and trap GC/ MS analysis. MTBE was found in home heating oil in residential tanks and in diesel fuel at service stations throughout the state of Connecticut. The levels of MTBE were found to vary significantly with time. Heating oil and diesel fuel from terminals were also found to contain MTBE. This research suggests thatthe reported widespread contamination of groundwater with MTBE may also be due to heating oil and diesel fuel releases to the environment. used extensively for the past 20 years as a gasoline additive (up to 15 wt %) to reduce automobile carbon monoxide and hydrocarbon emissions. The fact that MTBE is highly soluble in water (approximately 5 wt %) (3) and chemically inert when compared to other fuel constituents causes it to be often detected at high concentrations in groundwater in the vicinity of gasoline spills. The EPA has reported that low levels of MTBE in drinking water (above 40 microg/L) may cause unpleasant taste and odors and has designated MTBE as a

  14. Computational investigation of thermal gas separation for CO2 capture.

    SciTech Connect

    Gallis, Michail A.; Bryan, Charles R.; Brady, Patrick Vane; Torczynski, John Robert; Brooks, Carlton, F.

    2009-09-01

    This report summarizes the work completed under the Laboratory Directed Research and Development (LDRD) project 09-1351, 'Computational Investigation of Thermal Gas Separation for CO{sub 2} Capture'. Thermal gas separation for a binary mixture of carbon dioxide and nitrogen is investigated using the Direct Simulation Monte Carlo (DSMC) method of molecular gas dynamics. Molecular models for nitrogen and carbon dioxide are developed, implemented, compared to theoretical results, and compared to several experimental thermophysical properties. The molecular models include three translational modes, two fully excited rotational modes, and vibrational modes, whose degree of excitation depends on the temperature. Nitrogen has one vibrational mode, and carbon dioxide has four vibrational modes (two of which are degenerate). These models are used to perform a parameter study for mixtures of carbon dioxide and nitrogen confined between parallel walls over realistic ranges of gas temperatures and nominal concentrations of carbon dioxide. The degree of thermal separation predicted by DSMC is slightly higher than experimental values and is sensitive to the details of the molecular models.

  15. Modified normal-phase ion-pair chromatographic methods for the facile separation and purification of imidazolium-based ionic compounds

    SciTech Connect

    Urban, ND; Schenkel, MR; Robertson, LA; Noble, RD; Gin, DL

    2012-07-04

    lmidazolium- and oligo(imidazolium)-based ionic organic compounds are important in the design of room-temperature ionic liquid materials; however, the chromatographic analysis and separation of such compounds are often difficult. A convenient and inexpensive method for effective thin-layer chromatography (TLC) analysis and column chromatography separation of imidazolium-based ionic compounds is presented. Normal-phase ion-pair TLC is used to effectively analyze homologous mixtures of these ionic compounds. Subsequent separation of the mixtures is performed using ion-pair flash chromatography on normal-phase silica gel, yielding high levels of recovery. This method also results in a complete exchange of the counter anion on the imidazolium compounds to the anion of the ion-pair reagent. (C) 2012 Elsevier Ltd. All rights reserved.

  16. Catalyst assisted synthesis of initiator attached silica monolith particles via isocyanate-hydroxyl reaction for production of polystyrene bound chromatographic stationary phase of excellent separation efficiency.

    PubMed

    Ali, Faiz; Kim, Yune Sung; Lee, Jin Wook; Cheong, Won Jo

    2014-01-10

    Dibutyltin dichloride (DBTDC) was used as a catalyst to chemically bind 4-chloromehtylphenylisocynate (4-CPI) to porous monolithic silica particles via isocyanate-hydroxyl reaction, and the reaction product was reacted with sodium diethyldithiocarbamate (SDDC) to yield initiator attached silica monolith particles. Reversible addition-fragmentation transfer (RAFT) polymerization was taken place on them to result in polystyrene attached silica particles that showed excellent separation efficiency when packed in a chromatographic column (1.0 mm × 300 mm). The numbers of theoretical plates (N) of 56,500 is better than those of any commercially available HPLC or UHPLC column yet.

  17. Features of a truxene-based stationary phase in capillary gas chromatography for separation of some challenging isomers.

    PubMed

    Lv, Qing; Feng, Shuai; Jing, Lingmin; Zhang, Qing; Qi, Meiling; Wang, Jinliang; Bai, Hua; Fu, Ruonong

    2016-07-08

    Herein we report the first example of exploring truxene-based derivatives for gas chromatographic (GC) separations. The fabricated thiophene-functionalized truxene (TFT) column exhibited weak polarity and efficiencies as high as 4000plates/m for 0.250mm i.d. columns. TFT column showed preferential retention for halogenated and alkyl benzene analytes, and especially, high resolving capability for the xylene isomers, di- and trichlorobiphenyls (di-CB and tri-CB) isomers. Interestingly, its unique retentions for the latter analytes were found to be closely related with their dihedral angles and the locations of chlorine atoms. This finding on the retention trend has not been reported in GC separations, which may provide a new perspective in elucidating retention behaviours for specific analytes. Moreover, TFT column exhibited high thermal stability up to 320°C and excellent repeatability. This work demonstrates the promising future of truxene derivatives in the separation science.

  18. Dynamic Absorption Model for Off-Gas Separation

    SciTech Connect

    Veronica J. Rutledge

    2011-07-01

    Modeling and simulations will aid in the future design of U.S. advanced reprocessing plants for the recovery and recycle of actinides in used nuclear fuel. The specific fuel cycle separation process discussed in this report is the off-gas treatment system. The off-gas separation consists of a series of scrubbers and adsorption beds to capture constituents of interest. Dynamic models are being developed to simulate each unit operation involved so each unit operation can be used as a stand-alone model and in series with multiple others. Currently, a rate based, dynamic absorption model is being developed in gPROMS software. Inputs include liquid and gas stream constituents, column properties, liquid and gas phase reactions, number of stages, and inlet conditions. It simulates multiple component absorption with countercurrent flow and accounts for absorption by mass transfer and chemical reaction. The assumption of each stage being a discrete well-mixed entity was made. Therefore, the model is solved stagewise. The simulation outputs component concentrations in both phases as a function of time from which the rate of absorption is determined. Temperature of both phases is output as a function of time also. The model will be used able to be used as a standalone model in addition to in series with other off-gas separation unit operations. The current model is being generated based on NOx absorption; however, a future goal is to develop a CO2 specific model. The model will have the capability to be modified for additional absorption systems. The off-gas models, both adsorption and absorption, will be made available via the server or web for evaluation by customers.

  19. Gas Chromatographic Determination of Methyl Salicylate in Rubbing Alcohol: An Experiment Employing Standard Addition.

    ERIC Educational Resources Information Center

    Van Atta, Robert E.; Van Atta, R. Lewis

    1980-01-01

    Provides a gas chromatography experiment that exercises the quantitative technique of standard addition to the analysis for a minor component, methyl salicylate, in a commercial product, "wintergreen rubbing alcohol." (CS)

  20. Aging and analytical performances evolution of a gas chromatographic system at Mars

    NASA Astrophysics Data System (ADS)

    Bonnet, J.-Y.; Szopa, C.; Millan, M.; Coscia, D.; Cabane, M.; Belmahdi, I.; Buch, A.; Dequaire, T.; Coll, P.; Teinturier, S.; Mahaffy, P.

    2015-10-01

    Health data from the gas chromatography (GC) module onboard the SAM instrument [1] will be presented to assess the analytical performances evolution of a GC device in Martian environment through 3 years.

  1. Thermophoretic separation of aerosol particles from a sampled gas stream

    DOEpatents

    Postma, A.K.

    1984-09-07

    This disclosure relates to separation of aerosol particles from gas samples withdrawn from within a contained atmosphere, such as containment vessels for nuclear reactors or other process equipment where remote gaseous sampling is required. It is specifically directed to separation of dense aerosols including particles of any size and at high mass loadings and high corrosivity. The United States Government has rights in this invention pursuant to Contract DE-AC06-76FF02170 between the US Department of Energy and Westinghouse Electric Corporation.

  2. Gas separation and bubble behavior at a woven screen

    NASA Astrophysics Data System (ADS)

    Conrath, Michael; Dreyer, Michael E.

    Gas-liquid two phase flows are widespread and in many applications the separation of both phases is necessary. Chemical reactors, water treatment devices or gas-free delivery of liquids like propellant are only some of them. We study the performance of a woven metal screen in respect to its phase separation behavior under static and dynamic conditions. Beside hydraulic screen resistance and static bubble point, our study also comprises the bubble detachment from the screen upon gas breakthrough. Since a woven screen is essentially an array of identical pores, analogies to bubble detachment from a needle can be established. While the bubble point poses an upper limit for pressurized gas at a wetted screen to preclude gas breakthrough, the necessary pressure for growing bubbles to detach from the screen pores a lower limit when breakthrough is already in progress. Based on that inside, the dynamic bubble point effects were constituted that relate to a trapped bubble at such a screen in liquid flow. A trapped is caused to break through the screen by the flow-induced pressure drop across it. Our model includes axially symmetric bubble shapes, degree of coverage of the screen and bubble pressurization due to hydraulic losses in the rest of the circuit. We have built an experiment that consists of a Dutch Twilled woven screen made of stainless steel in a vertical acrylic glass tube. The liquid is silicon oil SF0.65. The screen is suspended perpendicular to the liquid flow which is forced through it at variable flow rate. Controlled injection of air from a needle allows us to examine the ability of the screen to separate gas and liquid along the former mentioned effects. We present experimental data on static bubble point and detachment pressure for breakthrough at different gas supply rates that suggest a useful criterion for reliable static bubble point measurements. Results for the dynamic bubble point are presented that include i) screen pressure drop for different

  3. Use of a modified Tenax GC column packing for the direct gas chromatographic analysis of phenols in water at the ppm level.

    PubMed

    Bartle, K D; Elstub, J; Novotny, M; Robinson, R J

    1977-05-21

    Dilute solutions of phenols in water at the ppm level may be analysed gas chromatographically by direct injection onto a column with a packing similar to that used in the Viking 1975 spacecraft: Tenax GC (2,6-diphenyl-p-phenylene oxide polymer) modified with polymetaphenyl ether liquid phase to eradicate irreversible adsorption. Symmetrical peaks were observed for injections of less than 1 ng of phenol and some of its alkylated derivatives. Chromatographic properties of modified Tenax GC columns are reported along with their application to the analysis of some industrial effluents with previous work-up.

  4. Capillary gas chromatographic analysis of alditol acetates of neutral and amino sugars in bacterial cell walls.

    PubMed

    Fox, A; Morgan, S L; Hudson, J R; Zhu, Z T; Lau, P Y

    1983-02-18

    Several improvements in the preparation of alditol acetates of neutral and amino sugars and in the preparation of glass capillary columns for their separation are described. Modifications in sample preparation permitted the simultaneous processing of multiple samples and eliminated extraneous background peaks. Efficient and inert columns were tailor-made for the separation of alditol acetates of neutral and amino sugars by leaching glass capillaries with aqueous hydrochloric acid and dynamically coating with SP-2330.

  5. Rare-gas-rich separates from carbonaceous chondrites

    NASA Technical Reports Server (NTRS)

    Reynolds, J. H.; Frick, U.; Neil, J. M.; Phinney, D. L.

    1978-01-01

    This paper describes an analysis of carbon-rich separates prepared by demineralization of colloidal fractions after disaggregation of bulk samples of the type C2 meteorites Murray, Murchison, and Cold Bokkeveld, as well as a methanol colloid extracted from acid-resistant residues of the Allende meteorite (type C3V) obtained by dissolution of most of the minerals in HCl and HF acids. The carbonaceous separates, or lAlates (a coined word designating colloids prepared sometimes before and sometimes after acid treatment), are characterized incompletely and with difficulty. A stepwise heating experiment on a Murray lAlate is discussed which revealed bimodal release of all noble gases, with similar patterns for Ar, Kr, and Xe. Chemical reactions are suggested as the likely mechanism for gas release. The results are shown to support the concept of a carbonaceous gas carrier uniformly present in meteorites of various types.

  6. Gas separation device based on electrical swing adsorption

    DOEpatents

    Judkins, Roddie R.; Burchell, Timothy D.

    1999-10-26

    A method and apparatus for separating one constituent, especially carbon dioxide, from a fluid mixture, such as natural gas. The fluid mixture flows through an adsorbent member having an affinity for molecules of the one constituent, the molecules being adsorbed on the adsorbent member. A voltage is applied to the adsorbent member, the voltage imparting a current flow which causes the molecules of the one constituent to be desorbed from the adsorbent member.

  7. Carbon-fiber composite molecular sieves for gas separation

    SciTech Connect

    Jagtoyen, M.; Derbyshire, F.; Kimber, G.; Fei, Y.Q.

    1995-08-01

    The progress of research in the development of novel, rigid, monolithic adsorbent carbon fiber composites is described. Carbon fiber composites are produced at ORNL and activated at the CAER using steam or CO{sub 2} under different conditions, with the aims of producing a uniform degree of activation through the material, and of closely controlling pore structure and adsorptive properties The principal focus of the work to date has been to produce materials with narrow porosity for use in gas separations.

  8. Ion-Gated Gas Separation through Porous Graphene.

    PubMed

    Tian, Ziqi; Mahurin, Shannon M; Dai, Sheng; Jiang, De-En

    2017-03-08

    Porous graphene holds great promise as a one-atom-thin, high-permeance membrane for gas separation, but to precisely control the pore size down to 3-5 Å proves challenging. Here we propose an ion-gated graphene membrane comprising a monolayer of ionic liquid-coated porous graphene to dynamically modulate the pore size to achieve selective gas separation. This approach enables the otherwise nonselective large pores on the order of 1 nm in size to be selective for gases whose diameters range from 3 to 4 Å. We show from molecular dynamics simulations that CO2, N2, and CH4 all can permeate through a 6 Å nanopore in graphene without any selectivity. But when a monolayer of [emim][BF4] ionic liquid (IL) is deposited on the porous graphene, CO2 has much higher permeance than the other two gases. We find that the anion dynamically modulates the pore size by hovering above the pore and provides affinity for CO2, while the larger cation (which cannot go through the pore) holds the anion in place via electrostatic attraction. This composite membrane is especially promising for CO2/CH4 separation, yielding a CO2/CH4 selectivity of about 42 and CO2 permeance of ∼10(5) GPU (gas permeation unit). We further demonstrate that selectivity and permeance can be tuned by the anion size, pore size, and IL thickness. The present work points toward a promising direction of using the atom-thin ionic liquid/porous graphene hybrid membrane for high-permeance, selective gas separation that allows a greater flexibility in substrate pore size control.

  9. Ion-Gated Gas Separation through Porous Graphene

    DOE PAGES

    Tian, Ziqi; Mahurin, Shannon M.; Dai, Sheng; ...

    2017-02-10

    Porous graphene holds great promise as an atom-thin, high-permeance membrane for gas separation, but to precisely control the pore size at three to five angstroms proves challenging. Here we propose an ion-gated graphene membrane comprising a monolayer of ionic liquid coated porous graphene to dynamically modulate the pore size to achieve selective gas separation. This approach enables the otherwise non-selective large pores on the order of 1 nm in size to be selective for gases whose diameters range from three to four angstroms. We show from molecular dynamics simulations that CO2, N2 and CH4 all can permeate through a 1-nmmore » pore in graphene without any selectivity. But when a monolayer of [emim][BF4] is deposited on the porous graphene, CO2 has much higher permeance than the other two gases. We find that the anion dynamically modulates the pore size by hovering above the pore and provides affinity for CO2 while the larger cation (which cannot go through the pore) holds the anion in place via electrostatic attraction. This composite membrane is especially promising for CO2/CH4 separation, with a CO2/CH4 selectivity of about 42 and CO2 permeance ~105 GPU (gas permeation unit). We further demonstrate that selectivity and permeance can be tuned by the anion size. The present work points toward a promising direction of using the atom-thin ionic-liquid/porous-graphene hybrid membrane for high-permeance, selective gas separation that allows a greater flexibility in substrate pore size control.« less

  10. On-line gas chromatographic analysis of Fischer-Tropsch synthesis products formed in a supercritical reaction medium

    SciTech Connect

    Snavely, K.; Subramaniam, B.

    1997-10-01

    C{sub 1}-C{sub 30} products from Fischer-Tropsch synthesis, conducted in a supercritical n-hexane medium over an Fe catalyst in a fixed-bed reactor, are analyzed using on-line gas chromatography. A Hewlett-Packard 5890 Series II gas chromatograph (GC) is modified to minimize the effects of condensation of the on-line sample in the transfer lines. The GC is configured with a Supelco Petrocol DH capillary column connected to a flame ionization detector (FID) and two 1.83 m {times} 3.18 mm stainless steel columns placed in series, packed with 80/100 mesh HayeSep D, connected to a thermal conductivity detector (TCD). It is shown that pressure and temperature affect the elution order of oxygenates relative to hydrocarbons in the nonpolar capillary column. This phenomenon is exploited for obtaining improved resolution; several distinct methods produce similar elution orders. Ar, added to the syngas feed, is used to calculate syngas conversion. All compounds eluting before hexane (C{sub 1}-C{sub 5}, other than 2-methylpropene/1-butene and propanal/propanone) and nearly all the major peaks eluting after hexane are resolved in the capillary column. H{sub 2}, Ar, CO, CH{sub 4}, CO{sub 2}, and H{sub 2}O are resolved in the packed columns. The method provides excellent quantitative measurement of component mole fractions that are within the range of calibration.

  11. Avoiding hard chromatographic segmentation: A moving window approach for the automated resolution of gas chromatography-mass spectrometry-based metabolomics signals by multivariate methods.

    PubMed

    Domingo-Almenara, Xavier; Perera, Alexandre; Brezmes, Jesus

    2016-11-25

    Gas chromatography-mass spectrometry (GC-MS) produces large and complex datasets characterized by co-eluted compounds and at trace levels, and with a distinct compound ion-redundancy as a result of the high fragmentation by the electron impact ionization. Compounds in GC-MS can be resolved by taking advantage of the multivariate nature of GC-MS data by applying multivariate resolution methods. However, multivariate methods have to be applied in small regions of the chromatogram, and therefore chromatograms are segmented prior to the application of the algorithms. The automation of this segmentation process is a challenging task as it implies separating between informative data and noise from the chromatogram. This study demonstrates the capabilities of independent component analysis-orthogonal signal deconvolution (ICA-OSD) and multivariate curve resolution-alternating least squares (MCR-ALS) with an overlapping moving window implementation to avoid the typical hard chromatographic segmentation. Also, after being resolved, compounds are aligned across samples by an automated alignment algorithm. We evaluated the proposed methods through a quantitative analysis of GC-qTOF MS data from 25 serum samples. The quantitative performance of both moving window ICA-OSD and MCR-ALS-based implementations was compared with the quantification of 33 compounds by the XCMS package. Results shown that most of the R(2) coefficients of determination exhibited a high correlation (R(2)>0.90) in both ICA-OSD and MCR-ALS moving window-based approaches.

  12. Limits of detections for the determination of mono- and dicarboxylic acids using gas and liquid chromatographic methods coupled with mass spectrometry

    PubMed Central

    Št’ávová, Jana; Beránek, Josef; Nelson, Eric P.; Diep, Bonnie A.; Kubátová, Alena

    2011-01-01

    The chromatographic separation and instrumental limits of detection (LODs) were obtained for a broad range of C1-C18 monocarboxylic (MCAs) and C2-C14 dicarboxylic acids (DCAs) employing either chemical derivatization followed by gas chromatography-mass spectrometry and flame ionization detection (GC-MS/FID) or direct analysis with liquid chromatography high resolution MS and tandem MS (LC-MS). Suitability, efficiency and stability of reaction products for several derivatization agents used for esterification (BF3/butanol), and trimethysilylation, including trimethylsilyl-N-N-dimethylcarbamate (TMSDMC) and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) were evaluated. The lowest limits of detection for the majority of compounds below 10 pg (with the exception of acetic acid) were obtained for derivatization with BF3/butanol followed by GC-MS in the total ion current (TIC) mode. Further improvements were achieved when applying either selected ion monitoring (SIM), which decreased the LODs to 1–4 pg or a combination of SIM and TIC (SITI) (2–5 pg). GC-FID provided LODs comparable to those obtained by GC-MS TIC. Both trimethylsilylation (followed by GC-MS) and direct LC-MS/MS analysis yielded LODs of 5– 40 pg for most of the acids. For volatile acids the LODs were higher, e.g., 25 and 590 ng for TMSDMC and BSTFA derivatized formic acid, respectively whereas the LC-MS methods did not allow for the analysis of formic acid at all. PMID:21185238

  13. Ammonia Analysis by Gas Chromatograph/Infrared Detector (GC/IRD)

    NASA Technical Reports Server (NTRS)

    Scott, Joseph P.; Whitfield, Steve W.

    2003-01-01

    Methods are being developed at Marshall Space Flight Center's Toxicity Lab on a CG/IRD System that will be used to detect ammonia in low part per million (ppm) levels. These methods will allow analysis of gas samples by syringe injections. The GC is equipped with a unique cryogenic-cooled inlet system that will enable our lab to make large injections of a gas sample. Although the initial focus of the work will be analysis of ammonia, this instrument could identify other compounds on a molecular level. If proper methods can be developed, the IRD could work as a powerful addition to our offgassing capabilities.

  14. Task 6.5 - Gas Separation and Hot-Gas Cleanup

    SciTech Connect

    Swanson, Michael L.; Ness Jr., Robert O.; Hurley, John P.; McCollor, Donald P.

    1997-06-01

    Catalytic gasification of coal to produce H{sub 2}- and CH{sub 4}-rich gases for consumption in molten carbonate fuel cells is currently under development; however, to optimize the fuel cell performance and extend its operating life, it is desired to separate as much of the inerts (i.e., CO{sub 2} and N{sub 2}) and impurities (i.e., H{sub 2}S and NH{sub 3}) as possible from the fuel gas before they enter the fuel cell. In addition, the economics of the integrated gasification combined cycle (IGCC) can be improved by separating as much of the hydrogen as possible from the fuel, since hydrogen is a high-value product. One process currently under development by the Energy & Environmental Research Center (EERC) for accomplishing this gas separation and hot-gas cleanup involves gas separation membranes. These membranes are operated at temperatures as high as 800 C and pressures up to 300 psig. Some of these membranes can have very small pores (30-50 {angstrom}), which inefficiently separate the undesired gases by operating in the Knudsen diffusion region of mass transport. Other membranes with smaller pore sizes (<5 {angstrom}) operate in the molecular sieving region of mass transport phenomena, Dissolution of atomic hydrogen into thin metallic membranes made of platinum and palladium alloys is also being developed. Technological and economic issues that must be resolved before gas separation membranes are commercially viable include improved gas separation efficiency, membrane optimization, sealing of membranes in pressure vessels, high burst strength of the ceramic material, pore thermal stability, and material chemical stability. Hydrogen separation is dependent on the temperature, pressure, pressure ratio across the membrane, and ratio of permeate flow to total flow. For gas separation under Knudsen diffusion, increasing feed pressure and pressure ratio across the membrane should increase gas permeability; decreasing the temperature and the permeate-to-total flow

  15. Polar Aprotic Modifiers for Chromatographic Separation and Back-Exchange Reduction for Protein Hydrogen/Deuterium Exchange Monitored by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Valeja, Santosh G.; Emmett, Mark R.; Marshall, Alan G.

    2012-04-01

    Hydrogen/deuterium exchange monitored by mass spectrometry is an important non-perturbing tool to study protein structure and protein-protein interactions. However, water in the reversed-phase liquid chromatography mobile phase leads to back-exchange of D for H during chromatographic separation of proteolytic peptides following H/D exchange, resulting in incorrect identification of fast-exchanging hydrogens as unexchanged hydrogens. Previously, fast high-performance liquid chromatography (HPLC) and supercritical fluid chromatography have been shown to decrease back-exchange. Here, we show that replacement of up to 40% of the water in the LC mobile phase by the modifiers, dimethylformamide (DMF) and N-methylpyrrolidone (NMP) (i.e., polar organic modifiers that lack rapid exchanging hydrogens), significantly reduces back-exchange. On-line LC micro-ESI FT-ICR MS resolves overlapped proteolytic peptide isotopic distributions, allowing for quantitative determination of the extent of back-exchange. The DMF modified solvent composition also improves chromatographic separation while reducing back-exchange relative to conventional solvent.

  16. Importance of MS selectivity and chromatographic separation in LC-MS/MS-based methods when investigating pharmaceutical metabolites in water. Dipyrone as a case of study.

    PubMed

    Ibáñez, M; Gracia-Lor, E; Sancho, J V; Hernández, F

    2012-08-01

    Pharmaceuticals are emerging contaminants of increasing concern because of their presence in the aquatic environment and potential to reach drinking-water sources. After human and/or veterinary consumption, pharmaceuticals can be excreted in unchanged form, as the parent compound, and/or as free or conjugated metabolites. Determination of most pharmaceuticals and metabolites in the environment is commonly made by liquid chromatography (LC) coupled to mass spectrometry (MS). LC coupled to tandem MS is the technique of choice nowadays in this field. The acquisition of two selected reaction monitoring (SRM) transitions together with the retention time is the most widely accepted criterion for a safe quantification and confirmation assay. However, scarce attention is normally paid to the selectivity of the selected transitions as well as to the chromatographic separation. In this work, the importance of full spectrum acquisition high-resolution MS data using a hybrid quadrupole time-of-flight analyser and/or a suitable chromatographic separation (to reduce the possibility of co-eluting interferences) is highlighted when investigating pharmaceutical metabolites that share common fragment ions. For this purpose, the analytical challenge associated to the determination of metabolites of the widely used analgesic dipyrone (also known as metamizol) in urban wastewater is discussed. Examples are given on the possibilities of reporting false positives of dypirone metabolites by LC-MS/MS under SRM mode due to a wrong assignment of identity of the compounds detected.

  17. Set-up of large laboratory-scale chromatographic separations of poly(ethylene glycol) derivatives of the growth hormone-releasing factor 1-29 analogue.

    PubMed

    Piquet, G; Gatti, M; Barbero, L; Traversa, S; Caccia, P; Esposito, P

    2002-01-25

    In this paper we report the scale-up of the purification of poly(ethylene glycol) (PEG) derivatives of the growth hormone-releasing factor 1-29, from laboratory scale (100 mg of bulk starting material) to larger scale (3 g of bulk), through the use of a cation-exchange TSK-SP-5PW chromatographic column. A one-step purification process capable of purifying large amounts of mono-PEGylated GRF species from the crude reaction mixture was developed. A simple, straightforward stepwise gradient elution separation was developed at laboratory scale and then scaled up with a larger column packed with a chromatographic resin with the same chemistry which maintained the laboratory-scale separation profile. Active material recovery and material purity remained constant through the scale-up from the 13-microm stationary phase to the 25-microm larger column. Overall, the gram GRF equivalent/batch process scale showed to be quite reproducible, and could be considered as a good platform for scale up to production scale.

  18. Polar Aprotic Modifiers for Chromatographic Separation and Back-Exchange Reduction for Protein Hydrogen/Deuterium Exchange Monitored by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

    PubMed Central

    Valeja, Santosh G.; Emmett, Mark R.; Marshall, Alan G.

    2013-01-01

    Hydrogen/deuterium exchange monitored by mass spectrometry is an important non-perturbing tool to study protein structure and protein–protein interactions. However, water in the reversed-phase liquid chromatography mobile phase leads to back-exchange of D for H during chromatographic separation of proteolytic peptides following H/D exchange, resulting in incorrect identification of fast-exchanging hydrogens as unexchanged hydrogens. Previously, fast high-performance liquid chromatography (HPLC) and supercritical fluid chromatography have been shown to decrease back-exchange. Here, we show that replacement of up to 40% of the water in the LC mobile phase by the modifiers, dimethylformamide (DMF) and N-methylpyrrolidone (NMP) (i.e., polar organic modifiers that lack rapid exchanging hydrogens), significantly reduces back-exchange. On-line LC micro-ESI FT-ICR MS resolves overlapped proteolytic peptide isotopic distributions, allowing for quantitative determination of the extent of back-exchange. The DMF modified solvent composition also improves chromatographic separation while reducing back-exchange relative to conventional solvent. PMID:22298288

  19. Application of Homochiral Alkylated Organic Cages as Chiral Stationary Phases for Molecular Separations by Capillary Gas Chromatography.

    PubMed

    Xie, Shengming; Zhang, Junhui; Fu, Nan; Wang, Bangjin; Hu, Cong; Yuan, Liming

    2016-11-08

    Molecular organic cage compounds have attracted considerable attention due to their potential applications in gas storage, catalysis, chemical sensing, molecular separations, etc. In this study, a homochiral pentyl cage compound was synthesized from a condensation reaction of (S,S)-1,2-pentyl-1,2-diaminoethane and 1,3,5-triformylbenzene. The imine-linked pentyl cage diluted with a polysiloxane (OV-1701) was explored as a novel stationary phase for high-resolution gas chromatographic separation of organic compounds. Some positional isomers were baseline separated on the pentyl cage-coated capillary column. In particular, various types of enantiomers including chiral alcohols, esters, ethers and epoxides can be resolved without derivatization on the pentyl cage-coated capillary column. The reproducibility of the pentyl cage-coated capillary column for separation was investigated using nitrochlorobenzene and styrene oxide as analytes. The results indicate that the column has good stability and separation reproducibility after being repeatedly used. This work demonstrates that molecular organic cage compounds could become a novel class of chiral separation media in the near future.

  20. Application of a gas-solid fluidized bed separator for shredded municipal bulky solid waste separation.

    PubMed

    Sekito, T; Matsuto, T; Tanaka, N

    2006-01-01

    A laboratory-scale gas-solid fluidized bed separator able to separate fractions of 5.6-50mm was used for separation of shredded municipal bulky waste (SBW) into combustibles and incombustibles. In batch-scale tests, it was found that accumulation of SBW in the bottom of the bed significantly reduced the separation efficiency. In this study, stirring was shown to be effective in preventing this accumulation. Flexible sheet materials such as paper and film plastics also significantly decreased the separation efficiency. In batch-scale tests, an overall efficiency of 90% was obtained when flexible materials such as film plastics and paper were excluded from the feed SBW. In continuous feeding tests, purities of the float and sink fractions attained 95% and 86% efficiencies, respectively, with an overall efficiency of 79%. The effect of feedstock shape on separation efficiency was also investigated. This study revealed that large particles can be properly separated on the basis of density, while the shape of the material significantly influenced behavior in the fluidizing bed.

  1. Gas Chromatographic Verification of a Mathematical Model: Product Distribution Following Methanolysis Reactions.

    ERIC Educational Resources Information Center

    Lam, R. B.; And Others

    1983-01-01

    Investigated application of binomial statistics to equilibrium distribution of ester systems by employing gas chromatography to verify the mathematical model used. Discusses model development and experimental techniques, indicating the model enables a straightforward extension to symmetrical polyfunctional esters and presents a mathematical basis…

  2. Current Developments in Analyzing Food Volatiles by Multidimensional Gas Chromatographic Techniques.

    PubMed

    Cordero, Chiara; Schmarr, Hans-Georg; Reichenbach, Stephen E; Bicchi, Carlo

    2017-02-02

    This paper presents current developments and future perspectives on the spread of advanced analytical tasks in the field of food volatile analysis. The topics outlined comprise (a) recent advances on miniaturized sampling techniques; (b) the potential and challenges of multidimensional gas chromatography coupled with mass spectrometric detection for volatile identification and quantitation in samples with complex matrices;

  3. On-line continuous sampling dynamic microwave-assisted extraction coupled with high performance liquid chromatographic separation for the determination of lignans in Wuweizi and naphthoquinones in Zicao.

    PubMed

    Gao, Shiqian; You, Jingyan; Wang, Ying; Zhang, Rui; Zhang, Hanqi

    2012-03-01

    The on-line continuous sampling dynamic microwave-assisted extraction (on-line CSDMAE) coupled with high-performance liquid chromatographic separation and determination of the lignans in Wuweizi and naphthoquinones in Zicao was developed. The extraction, separation and determination of target analytes were simultaneously carried out. The experimental parameters, including type of extraction solvent, microwave extraction power, solvent flow rate, amount of sample and particle size of the sample, were evaluated by the univariate method and orthogonal screening. The detection limits for schisandrin A, schisantherin A, deoxyschizandrin, shikonin and β,β'-dimethylacrylshikonin are 0.86, 0.90, 0.27, 0.42 and 0.92 μg mL⁻¹, respectively. Compared with the conventional extraction methods, such as off-line continuous microwave-assisted extraction, ultrasound-assisted extraction and Soxhlet extraction, the proposed method is quicker and more effective.

  4. Development and evaluation of gas and liquid chromatographic methods for the analysis of fatty amines.

    PubMed

    Breitbach, Zachary S; Weatherly, Choyce A; Woods, Ross M; Xu, Chengdong; Vale, Glenda; Berthod, Alain; Armstrong, Daniel W

    2014-03-01

    In contrast to the plethora of publications on the separation of fatty acids, analogous studies involving fatty amines are scarce. A recently introduced ionic-liquid-based capillary column for GC was used to separate trifluoroacetylated fatty amines focusing on the analysis of a commercial sample. Using the ionic liquid column (isothermal mode at 200 °C) it was possible to separate linear primary fatty amines from C12 to C22 chain length in less 25 min with MS identification. The log of the amine retention factors are linearly related to the alkyl chain length with a methylene selectivity of 0.117 kcal/mol for the saturated amines and 0.128 kcal/mol for the mono-unsaturated amines. The sp2 selectivity for unsaturated fatty amines also could be calculated as 0.107 kcal/mol for the ionic liquid column. The commercial sample was quantified by GC with flame ionization detection (FID). An LC method also was developed with a reversed phase gradient separation using acetonitrile/formate buffer mobile phases and ESI-MS detection. Native amines could be detected and identified by their single ion monitoring chromatograms even when partial coelution was observed. The analysis of the commercial sample returned results coherent with those obtained by GC-FID and with the manufacturer's data.

  5. Use of exhaust gas as sweep flow to enhance air separation membrane performance

    DOEpatents

    Dutart, Charles H.; Choi, Cathy Y.

    2003-01-01

    An intake air separation system for an internal combustion engine is provided with purge gas or sweep flow on the permeate side of separation membranes in the air separation device. Exhaust gas from the engine is used as a purge gas flow, to increase oxygen flux in the separation device without increasing the nitrogen flux.

  6. Separation of CO2 from flue gas using electrochemical cells

    SciTech Connect

    Pennline, H.W; Granite, E.J.; Luebke, D.R; Kitchin, J.R; Landon, J.; Weiland, L.M.

    2010-06-01

    ABSTRACT Past research with high temperature molten carbonate electrochemical cells has shown that carbon dioxide can be separated from flue gas streams produced by pulverized coal combustion for power generation, However, the presence of trace contaminants, i.e" sulfur dioxide and nitric oxides, will impact the electrolyte within the cell. If a lower temperature cell could be devised that would utilize the benefits of commercially-available, upstream desulfurization and denitrification in the power plant, then this CO2 separation technique can approach more viability in the carbon sequestration area, Recent work has led to the assembly and successful operation of a low temperature electrochemical cell. In the proof-of-concept testing with this cell, an anion exchange membrane was sandwiched between gas-diffusion electrodes consisting of nickel-based anode electrocatalysts on carbon paper. When a potential was applied across the cell and a mixture of oxygen and carbon dioxide was flowed over the wetted electrolyte on the cathode side, a stream of CO2 to O2 was produced on the anode side, suggesting that carbonate/ bicarbonate ions are the CO2 carrier in the membrane. Since a mixture of CO 2 and 02 is produced, the possibility exists to use this stream in oxy-firing of additional fuel. From this research, a novel concept for efficiently producing a carbon dioxide rich effiuent from combustion of a fossil fuel was proposed. Carbon dioxide and oxygen are captured from the flue gas of a fossilfuel combustor by one or more electrochemical cells or cell stacks. The separated stream is then transferred to an oxy-fired combustor which uses the gas stream for ancillary combustion, ultimately resulting in an effluent rich in carbon dioxide, A portion of the resulting flow produced by the oxy-fired combustor may be continuously recycled back into the oxy-fired combustor for temperature control and an optimal carbon dioxide rich effluent.

  7. A technique for rapid source apportionment applied to ambient organic aerosol measurements from a thermal desorption aerosol gas chromatograph (TAG)

    NASA Astrophysics Data System (ADS)

    Zhang, Yaping; Williams, Brent J.; Goldstein, Allen H.; Docherty, Kenneth S.; Jimenez, Jose L.

    2016-11-01

    We present a rapid method for apportioning the sources of atmospheric organic aerosol composition measured by gas chromatography-mass spectrometry methods. Here, we specifically apply this new analysis method to data acquired on a thermal desorption aerosol gas chromatograph (TAG) system. Gas chromatograms are divided by retention time into evenly spaced bins, within which the mass spectra are summed. A previous chromatogram binning method was introduced for the purpose of chromatogram structure deconvolution (e.g., major compound classes) (Zhang et al., 2014). Here we extend the method development for the specific purpose of determining aerosol samples' sources. Chromatogram bins are arranged into an input data matrix for positive matrix factorization (PMF), where the sample number is the row dimension and the mass-spectra-resolved eluting time intervals (bins) are the column dimension. Then two-dimensional PMF can effectively do three-dimensional factorization on the three-dimensional TAG mass spectra data. The retention time shift of the chromatogram is corrected by applying the median values of the different peaks' shifts. Bin width affects chemical resolution but does not affect PMF retrieval of the sources' time variations for low-factor solutions. A bin width smaller than the maximum retention shift among all samples requires retention time shift correction. A six-factor PMF comparison among aerosol mass spectrometry (AMS), TAG binning, and conventional TAG compound integration methods shows that the TAG binning method performs similarly to the integration method. However, the new binning method incorporates the entirety of the data set and requires significantly less pre-processing of the data than conventional single compound identification and integration. In addition, while a fraction of the most oxygenated aerosol does not elute through an underivatized TAG analysis, the TAG binning method does have the ability to achieve molecular level resolution on

  8. Gas chromatographic/mass spectrometric determination of lysergic acid diethylamide (LSD) in serum samples.

    PubMed

    Musshoff, F; Daldrup, T

    1997-08-04

    A sensitive method for the detection and quantification of lysergic acid diethylamide (LSD) in serum samples is described. After liquid-liquid extraction the trimethylsilyl derivative of LSD is detected by gas chromatography-mass spectrometry. Experiments with spiked samples resulted in a recovery of 76%, the coefficient of variation was 9.3%. Excellent linearity was obtained over the range 0.1-10 ng ml-1. Additionally experiments demonstrating the light sensitivity of LSD are presented together with casuistics.

  9. Separation of flue-gas scrubber sludge into marketable products

    SciTech Connect

    Kawatra, S.K.; Eisele, T.C.

    1997-08-31

    A tremendous amount of wet flue-gas desulfurization scrubber sludge (estimated 20 million metric tons per year in the US) is currently being landfilled at a huge cost to utility companies. Scrubber sludge is the solid precipitate produced during desulfurization of flue-gas from burning high sulfur coal. The amount of this sludge is expected to increase in the near future due to ever increasing governmental regulation concerning the amount of sulfur emissions. Scrubber sludge is a fine, grey colored powder that contains calcium sulfite hemihydrate (CaSO{sub 3} {center_dot} 1/2H{sub 2}), calcium sulfate dihydrate (CaSO{sub 4} {center_dot} 2H{sub 2}O), limestone (CaCO{sub 3}), silicates, and iron oxides. This material can continue to be landfilled at a steadily increasing cost, or an alternative for utilizing this material can be developed. This study explores the characteristics of a naturally oxidized wet flue-gas desulfurization scrubber sludge and uses these characteristics to develop alternatives for recycling this material. In order for scrubber sludge to be used as a feed material for various markets, it was necessary to process it to meet the specifications of these markets. A physical separation process was therefore needed to separate the components of this sludge into useful products at a low cost. There are several physical separation techniques available to separate fine particulates. These techniques can be divided into four major groups: magnetic separation, electrostatic separation, physico-chemical separation, and density-based separation. The properties of this material indicated that two methods of separation were feasible: water-only cycloning (density-based separation), and froth flotation (physico-chemical separation). These processes could be used either separately, or in combination. The goal of this study was to reduce the limestone impurity in this scrubber sludge from 5.6% by weight to below 2.0% by weight. The resulting clean calcium

  10. Gas chromatographic determination of urinary phenol conjugates after acid hydrolysis/extractive acetylation.

    PubMed

    Weber, L

    1992-02-14

    Phenolic metabolites of inhaled aromatic solvent vapours were liberated by acid hydrolysis of their urinary conjugates. Steam distillation enhanced by salting-out with MgSO4 gave good recoveries. After extractive acetylation, the derivatives of all cresols and xylenols were completely separated on a Se-54 capillary column. The overall recoveries of urinary phenols relative to the internal standard, 3-chlorophenol, were in the range 92-99%.

  11. Improved separation of fluorogenic derivatized intact proteins with high resolution and efficiency using a reversed-phase liquid chromatographic system.

    PubMed

    Ichibangase, Tomoko; Nakata, Katsunori; Imai, Kazuhiro

    2014-06-01

    Although the efficient separation of intact protein mixtures is extremely difficult, reversed-phase chromatography is an important technique for performing quantitative, accurate and reproducible proteomics analyses. Here, we show that, despite the operating constraints of conventional high-performance liquid chromatography, such as column temperature, operating pressure and separation time, comprehensive separation of fluorogenic derivatized intact proteins could be achieved with high resolution and separation efficiency. First, amylin was chosen as a model peptide and used to estimate the separation efficiency with respect to column temperature and flow rate, as indicated by peak capacity. Then, an extract of human primary hepatocytes was used to model complex component mixtures and the separation conditions were optimized. The effects of mobile-phase pH, the separation time and the column length were also investigated. Consequently, more than 890 peaks could be separated efficiently in the extract, which is 1.5-fold greater than when using conventional conditions. Finally, it was demonstrated that both longer separation time and column length contributed greatly to the effective separation of the protein mixture. These results are expected to provide insights into the separation of intact proteins.

  12. Evaluation of an electrochemical N2/H2 gas separator

    NASA Technical Reports Server (NTRS)

    Marshall, R. D.; Wynveen, R. A.; Carlson, J. N.

    1973-01-01

    A program was successfully completed to evaluate an electrochemical nitrogen/hydrogen (N2/H2) separator for use in a spacecraft nitrogen (N2) generator. Based on the technical data obtained a N2/H2 separator subsystem consisting of an organic polymer gas permeator first stage and an electrochemical second and third stage was estimated to have the lowest total spared equivalent weight, 257 kg (566 lb), for a 15 lb/day N2 generation rate. A pre-design analysis of the electrochemical N2/H2 separator revealed that its use as a first stage resulted in too high a power requirement to be competitive with the organic polymer membrane and the palladium-silver membrane separation methods. As a result, program emphasis was placed on evaluating the electrochemical. A parametric test program characterized cell performance and established second- and third-stage electrochemical N2/H2 separator operating conditions. A design verification test was completed on the second and third stages. The second stage was then successfully endurance tested for 200 hours.

  13. Optimizing the separation performance of a gas centrifuge

    NASA Astrophysics Data System (ADS)

    Wood, H. G.

    1997-11-01

    Gas centrifuges were originally developed for the enrichment of U^235 from naturally occurring uranium for the purpose of providing fuel for nuclear power reactors and material for nuclear weapons. This required the separation of a binary mixture composed of U^235 and U^238. Since the end of the cold war, a surplus of enriched uranium exists on the world market, but many centrifuge plants exist in numerous countries. These circumstances together with the growing demand for stable isotopes for chemical and physical research and in medical science has led to the exploration of alternate applications of gas centrifuge technology. In order to acieve these multi-component separations, existing centrifuges must be modified or new centrifuges must be designed. In either case, it is important to have models of the internal flow fields to predict the separation performance and algorithms to seek the optimal operating conditions of the centrifuges. Here, we use the Onsager pancake model of the internal flow field, and we present an optimization strategy which exploits a similarity parameter in the pancake model. Numerical examples will be presented.

  14. Simultaneous gas chromatographic determination of dibutyltin and tributyltin compounds in biological and sediment samples

    SciTech Connect

    Tsuda, T.; Nakanishi, H.; Morita, T.; Takebayashi, J.

    1986-11-01

    A method is described for the simultaneous determination of nanogram amounts of dibutyltin and tributyltin compounds in biological and sediment samples. These compounds are converted to the corresponding chlorides with HCl, extracted with ethyl acetate-hexane (3 + 2) for biological samples and with hexane for sediment samples, and hydrogenated with sodium borohydride. The corresponding hydrides, Bu2SnH2 and Bu3SnH, are detected by electron-capture gas chromatography after cleanup by silica gel column chromatography. Detection limits are 1.0-2.0 and 0.5-1.0 ng/g, respectively, for biological and sediment samples.

  15. Development of gas chromatographic methods for the analyses of organic carbonate-based electrolytes

    NASA Astrophysics Data System (ADS)

    Terborg, Lydia; Weber, Sascha; Passerini, Stefano; Winter, Martin; Karst, Uwe; Nowak, Sascha

    2014-01-01

    In this work, novel methods based on gas chromatography (GC) for the investigation of common organic carbonate-based electrolyte systems are presented, which are used in lithium ion batteries. The methods were developed for flame ionization detection (FID), mass spectrometric detection (MS). Further, headspace (HS) sampling for the investigation of solid samples like electrodes is reported. Limits of detection are reported for FID. Finally, the developed methods were applied to the electrolyte system of commercially available lithium ion batteries as well as on in-house assembled cells.

  16. 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.

  17. MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission: results and performance

    NASA Astrophysics Data System (ADS)

    Buch, A.; Pinnick, V. T.; Szopa, C.; Grand, N.; Humeau, O.; van Amerom, F. H.; Danell, R.; Freissinet, C.; Brinckerhoff, W.; Gonnsen, Z.; Mahaffy, P. R.; Coll, P.; Raulin, F.; Goesmann, F.

    2015-10-01

    The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquiring samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular and chiral) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis/chemical derivatization gas chromatography (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide information on elemental and molecular makeup, polarity, chirality and isotopic patterns of analyte species. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatographymass spectrometry (GC-MS) mode of operation.

  18. Miniaturized system of a gas chromatograph coupled with a Paul ion trap mass spectrometer

    NASA Technical Reports Server (NTRS)

    Shortt, B. J.; Darrach, M. R.; Holland, Paul M.; Chutjian, A.

    2005-01-01

    Miniature gas chromatography (GC) and miniature mass spectrometry (MS) instrumentation has been developed to identify and quantify the chemical compounds present in complex mixtures of gases. The design approach utilizes micro-GC components coupled with a Paul quadrupole ion trap (QIT) mass spectrometer. Inherent to the system are high sensitivity, good dynamic range, good QIT resolution, low GC flow-rates to minimize vacuum requirements and the need for consumables; and the use of a modular approach to adapt to volatile organic compounds dissolved in water or present in sediment. Measurements are reported on system response to gaseous species at concentrations varying over four orders of magnitude. The ability of the system to deal with complicated mixtures is demonstrated, and future improvements are discussed. The GC/QIT system described herein has a mass, volume and power that are, conservatively, one-twentieth of those of commercial off-the-shelf systems. Potential applications are to spacecraft cabin-air monitoring, robotic planetary exploration and trace-species detection for residual gas analysis and environmental monitoring.

  19. Enantioselective nano liquid chromatographic separation of racemic pharmaceuticals: a facile one-pot in situ preparation of lipase-based polymer monoliths in capillary format.

    PubMed

    Ahmed, Marwa; Ghanem, Ashraf

    2014-11-01

    New affinity monolithic capillary columns of 150 µm internal diameter were prepared in situ fused glass capillary via either immobilization or encapsulation of Candida antarctica lipase B (CALB) on or within polymer monoliths, respectively. The immobilized lipase-based monoliths were prepared via copolymerization of 19.1% monomers (8.9% MMA and 10.2% GMA), 19.8% EDMA, and 61.1% porogens (54.2% formamide and 6.9% 1-propanol) w/w or 20% GMA, 20% EDMA, and 60% porogens (51.6% cyclohexanol and 8.4% 1-dodecanol) in the presence of AIBN (1%) as a radical initiator. This was followed by pumping a solution of lipase through the capillaries and rinsing with potassium phosphate buffer. On the other hand, the encapsulated lipase-based monoliths were prepared via copolymerization of 20% monomers (GMA), 20% EDMA, and 60% porogens (48% 1-propanol, 6% 1,4-butanediol) or 16.4% monomers (16% BuMA, 0.4% SPMA), 23.6% EDMA, and 60% porogens (36% 1-propanol, 18% 1,4-butanediol along with 6% lipase aqueous solution in potassium phosphate buffer. The prepared capillary columns were investigated for the enantioselective nano liquid chromatographic separation of a set of different classes of racemic pharmaceuticals, namely, α- and β-blockers, antiinflammatory drugs, antifungal drugs, dopamine antagonists, norepinephrine-dopamine reuptake inhibitors, catecholamines, sedative hypnotics, diuretics, antihistaminics, anticancer drugs, and antiarrhythmic drugs. Run-to-run repeatability was quite satisfactory. The encapsulated lipase-based capillary monolith showed better enantioselective separations of most of the investigated compounds. Baseline separation was achieved for alprenolol, atenolol, bromoglutithimide, carbuterol, chloropheneramine, cizolertine carbinol, 4-hydroxy-3-methoxymandelic acid, desmethylcizolertine, nomifensine, normetanephrine, and sulconazole under reversed phase chromatographic conditions. A speculation about the understanding of the chiral recognition mechanism of

  20. Integration and Ruggedization of a Commercially Available Gas Chromatograph and Mass Spectrometer (GCMS) for the Resource Prospector Mission (RPM)

    NASA Technical Reports Server (NTRS)

    Loftin, Kathleen; Griffin, Timothy; Captain, Janine

    2013-01-01

    The Resource Prospector is a mission to prospect for lunar volatiles (primarily water) at one of the two lunar poles, as well as demonstrate In-Situ Resource Utilization (ISRU) on the Moon. The Resource Prospector consists of a lander, a rover, and a rover-borne scientific payload. The Regolith and Environment Science and Oxygen & Lunar Volatile Extraction (RESOLVE) payload, will be able to (1) locate near subsurface volatiles, (2) excavate and analyze samples of the volatile-bearing regolith, and (3) demonstrate the form, extractability and usefulness of the materials. The gas chromatograph mass spectrometer (GCMS) is the primary instrument in the RESOLVE instrumentation suite responsible for identification and quantification of the volatiles evolved from the lunar regolith. Specifically, this instrument must have: a low mass, a low power consumption, be able to perform fast analyses of samples ranging from less than one to greater than ninety nine percent water by mass, be autonomously controlled by the payload's software and avionics platform, and be able to operate in the harsh lunar environment. The RPM's short mission duration is the primary driver of the requirement for a very fast analysis time currently base lined at less than 2 minutes per sample. This presentation will discuss the requirements levied upon the GCMS design, lessons learned from a preliminary field demonstration deployment, the current design, and the path forward.

  1. Inverse gas chromatographic method for measurement of interactions between soy protein isolate and selected flavor compounds under controlled relative humidity.

    PubMed

    Zhou, Qiaoxuan; Cadwallader, Keith R

    2004-10-06

    An inverse gas chromatographic (IGC) method was developed to study the binding interactions between selected volatile flavor compounds and soy protein isolate (SPI) under controlled relative humidity (RH). Three volatile probes (hexane, 1-hexanol, and hexanal) at very low levels were used to evaluate and validate system performance. On the basis of the thermodynamic data and the isotherms measured at 0% RH, 1-hexanol and hexanal had higher binding affinities than hexane, which could be attributed to hydrogen-bonding interactions with SPI. At 30% RH, 1-hexanol and hexanal were retained less than at 0% RH, indicating possible competition for binding sites on the SPI surface between water and volatile probe molecules. Results showed that the thermodynamic data determined were comparable to the available literature values. Use of IGC allowed for the rapid and precise generation of sorption isotherms. Repeatability between replicate injections and reproducibility across columns were very good. IGC is a potentially high-throughput method for the sensitive, precise, and accurate measurement of flavor-ingredient interactions in low-moisture food systems.

  2. [Correlation between octanol-air partition coefficients and retention parameters of polychlorinated biphenyls on gas chromatographic columns].

    PubMed

    Zhang, Qing; Zhao, Hongxia; Chen, Jiping; Liang, Xinmiao

    2005-09-01

    Octanol-air partition coefficient (Koa) is a key descriptor for describing the partitioning of organic pollutants, especially persistent organic pollutants (POPs), between air and environmental organic phases. Thus it is necessary to determine or predict the Koa values of these compounds. A novel method was introduced to describe the quantitive relationship between the octanol-air partition coefficients and gas chromatographic (GC) retention parameters A, B values of polychlorinated diphenyls (PCBs) which are typical persistent organic pollutants. By the correlation analysis between GC retention parameters A, B values of PCBs on DB-1, DB-5 and DB-1701 columns, and their octanol-air partition coefficients, a good linear relationship was found. The stepwise multiple linear regression was used to derive binary equations with the correlation coefficients greater than 0.99, and the standard deviations are less than 0.11. In addition, based on the 153 experimental A, B values and 56 predicted A, B values, the Koa values of the remaining 190 PCBs were predicted.

  3. Development of a miniaturized diffusive sampler for true breathing-zone sampling and thermal desorption gas chromatographic analysis.

    PubMed

    Lindahl, Roger; Levin, Jan-Olof; Sundgren, Margit

    2009-07-01

    Exposure measurements should be performed as close as possible to the nose and mouth for a more correct assessment of exposure. User-friendly sampling equipment, with a minimum of handling before, during and after measurement, should not affect ordinary work. In diffusive (passive) sampling, no extra equipment as sampling pumps is needed, making the measurements more acceptable to the user. The diffusive samplers are normally attached on a shoulder, on a breast-pocket or on the lapel. There are, however, difficulties if true breathing-zone sampling is to be performed, since available diffusive samplers normally cannot be arranged close to the nose/mouth. The purpose of this work was to study the performance of a miniaturized tube type diffusive sampler attached to a headset for true breathing-zone sampling. The basis for this miniaturization was the Perkin Elmer ATD tube. Both the size of the tube and the amount of adsorbent was decreased for the miniaturized sampler. A special tube holder to be used with a headset was designed for the mini tube. The mini tube is thermally desorbed inside a standard PE tube. The new sampler was evaluated for the determination of styrene, both in laboratory experiments and in field measurements. As reference method, diffusive sampling with standard Perkin Elmer tubes, thermal desorption and gas chromatographic (GC) analysis was used. The sampling rate was determined to 0.356 mL min(-1) (CV 9.6%) and was not significantly affected by concentration, sampling time or relative humidity.

  4. Gas chromatographic fingerprinting of crude oil from Idu-Ekpeye oil spillage site in Niger-delta, Nigeria.

    PubMed

    Udoetok, Inimfon A; Osuji, Leo C

    2008-06-01

    Samples were collected from an oil polluted site in Niger-delta, Nigeria. Gas chromatographic analyses carried out on the samples revealed an abundance of n-alkanes within the n-C8-n-C23 region. The pristane/phytane ratio of 5.70 obtained for the samples depicted a plant/terrestrial source input and a possible oxic depositional environment. The n-C17/pristane and n-C18/phytane ratios of 2.80 and 2.77, respectively, suggested that the spilled oil was only slightly weathered, as corroborated by the presence of peaks in the aromatic hydrocarbon fingerprints. The polycyclic aromatic hydrocarbon (PAH) fractions showed that the hydrocarbon fractions might have undergone combustion and/or that there was bush burning at the site prior to the oil spill incidence. This is supported by the abundance of high-molecular-weight PAHs which are pyrogenic in nature. High molecular weight PAHs are products of the combustion of petroleum or its products. The phenanthrene/anthracene ratio of 0.95, fluorathene/pyrene ratio of 2.23 and the summation operator (other three to six ringed PAHs)/ summation operator (five alkylated PAHs) ratio far greater than unity (4.10) also affirm this. On the other hand, the benzo (a) anthracene to chrysene ratio of 0.24 confirms the petrogenic origin of the spilled oil because chrysene which is highly abundant is a fossil PAH.

  5. Separation of SF6 from gas mixtures using gas hydrate formation.

    PubMed

    Cha, Inuk; Lee, Seungmin; Lee, Ju Dong; Lee, Gang-woo; Seo, Yongwon

    2010-08-15

    This study aims to examine the thermodynamic feasibility of separating sulfur hexafluoride (SF(6)), which is widely used in various industrial fields and is one of the most potent greenhouse gases, from gas mixtures using gas hydrate formation. The key process variables of hydrate phase equilibria, pressure-composition diagram, formation kinetics, and structure identification of the mixed gas hydrates, were closely investigated to verify the overall concept of this hydrate-based SF(6) separation process. The three-phase equilibria of hydrate (H), liquid water (L(W)), and vapor (V) for the binary SF(6) + water mixture and for the ternary N(2) + SF(6) + water mixtures with various SF(6) vapor compositions (10, 30, 50, and 70%) were experimentally measured to determine the stability regions and formation conditions of pure and mixed hydrates. The pressure-composition diagram at two different temperatures of 276.15 and 281.15 K was obtained to investigate the actual SF(6) separation efficiency. The vapor phase composition change was monitored during gas hydrate formation to confirm the formation pattern and time needed to reach a state of equilibrium. Furthermore, the structure of the mixed N(2) + SF(6) hydrate was confirmed to be structure II via Raman spectroscopy. Through close examination of the overall experimental results, it was clearly verified that highly concentrated SF(6) can be separated from gas mixtures at mild temperatures and low pressure conditions.

  6. Method for measuring changes in the atmospheric O2/N2 ratio by a gas chromatograph equipped with a thermal conductivity detector

    NASA Astrophysics Data System (ADS)

    Tohjima, Yasunori

    2000-06-01

    We present a method for measuring changes in the atmospheric O2/N2 ratio based on data from a gas chromatograph (GC) equipped with a thermal conductivity detector (TCD). In this method, O2 and N2 in an air sample are separated on a column filled with molecular sieve 5A with H2 carrier gas. Since the separated O2 includes Ar, which has a retention time similar to that of O2, the (O2+Ar)/N2 ratio is actually measured. The change in the measured (O2+Ar)/N2 ratio can be easily converted to that in the O2/N2 ratio with a very small error based on the fact that the atmospheric Ar/N2 ratio is almost constant. The improvements to achieve the high-precision measurement include stabilization of the pressure at the GC column head and at the outlets of the TCD and the sample loop. Additionally, the precision is improved statistically by repeating alternate analyses of sample and a reference gas. The standard deviation of the replicate cycles of reference and sample analyses is about 18 per meg (corresponding to 3.8 parts per million (ppm) O2 in air). This means that the standard error is about 7 per meg (1.5 ppm O2 in air) for seven cycles of alternate analyses, which takes about 70 min. The response of this method is likely to have a 2% nonlinearity. Ambient air samples are collected under pressure in glass flasks equipped with two stopcocks sealed by Viton O-rings at both ends. Pressure depletion in the flask during the O2/N2 measurement does not cause any detectable change in the O2/N2 ratio, but the O2/N2 ratio in the flask was found to gradually decrease during the storage period. We also present preliminary results from air samples collected at Hateruma Island (latitude 24°03'N, longitude 123°49') from July 1997 through March 1999. The observed O2/N2 ratios clearly show a seasonal variation, increasing in spring and summer and decreasing in autumn and winter.

  7. Carbon Dioxide Separation from Flue Gas by Phase Enhanced Absorption

    SciTech Connect

    Liang Hu

    2006-06-30

    A new process, phase enhanced absorption, was invented. The method is carried out in an absorber, where a liquid carrier (aqueous solution), an organic mixture (or organic compound), and a gas mixture containing a gas to be absorbed are introduced from an inlet. Since the organic mixture is immiscible or at least partially immiscible with the liquid carrier, the organic mixture forms a layer or small parcels between the liquid carrier and the gas mixture. The organic mixture in the absorber improves mass transfer efficiency of the system and increases the absorption rate of the gas. The organic mixture serves as a transportation media. The gas is finally accumulated in the liquid carrier as in a conventional gas-liquid absorption system. The presence of the organic layer does not hinder the regeneration of the liquid carrier or recovery of the gas because the organic layer is removed by a settler after the absorption process is completed. In another aspect, the system exhibited increased gas-liquid separation efficiency, thereby reducing the costs of operation and maintenance. Our study focused on the search of the organic layer or transportation layer to enhance the absorption rate of carbon dioxide. The following systems were studied, (1) CO{sub 2}-water system and CO{sub 2}-water-organic layer system; (2) CO{sub 2}-Potassium Carbonate aqueous solution system and CO{sub 2}-Potassium Carbonate aqueous solution-organic layer system. CO{sub 2}-water and CO{sub 2}-Potassium Carbonate systems are the traditional gas-liquid absorption processes. The CO{sub 2}-water-organic layer and CO{sub 2}-Potassium Carbonate-organic layer systems are the novel absorption processes, phase enhanced absorption. As we mentioned early, organic layer (transportation layer phase) is used for the increase of absorption rate. Our study showed that the absorption rate can be increased by adding the organic layer. However, the enhanced factor is highly depended on the liquid mass transfer

  8. Carbon Dioxide Separation from Flue Gas by Phase Enhanced Absorption

    SciTech Connect

    Tim Fout

    2007-06-30

    A new process, phase enhanced absorption, was invented. The method is carried out in an absorber, where a liquid carrier (aqueous solution), an organic mixture (or organic compound), and a gas mixture containing a gas to be absorbed are introduced from an inlet. Since the organic mixture is immiscible or at least partially immiscible with the liquid carrier, the organic mixture forms a layer or small parcels between the liquid carrier and the gas mixture. The organic mixture in the absorber improves mass transfer efficiency of the system and increases the absorption rate of the gas. The organic mixture serves as a transportation media. The gas is finally accumulated in the liquid carrier as in a conventional gas-liquid absorption system. The presence of the organic layer does not hinder the regeneration of the liquid carrier or recovery of the gas because the organic layer is removed by a settler after the absorption process is completed. In another aspect, the system exhibited increased gas-liquid separation efficiency, thereby reducing the costs of operation and maintenance. Our study focused on the search of the organic layer or transportation layer to enhance the absorption rate of carbon dioxide. The following systems were studied, (1) CO{sub 2}-water system and CO{sub 2}-water-organic layer system; (2) CO{sub 2}-Potassium Carbonate aqueous solution system and CO{sub 2}-Potassium Carbonate aqueous solution-organic layer system. CO{sub 2}-water and CO{sub 2}-Potassium Carbonate systems are the traditional gas-liquid absorption processes. The CO{sub 2}-water-organic layer and CO{sub 2}-Potassium Carbonate-organic layer systems are the novel absorption processes, phase enhanced absorption. As we mentioned early, organic layer is used for the increase of absorption rate, and plays the role of transportation of CO{sub 2}. Our study showed that the absorption rate can be increased by adding the organic layer. However, the enhanced factor is highly depended on the

  9. Synthesis, pervaporation and gas separation studies of polyaniline blends

    SciTech Connect

    Huang, S.C.; Conklin, J.A.; Su, T.M.

    1995-12-01

    Membranes have been successfully produced from blends of polyaniline/polyacrylic acid and polyaniline/polyimide. The uniqueness of these membranes is the incorporation of {open_quotes}polymer dopants{close_quotes} in polyaniline. Conductivity measurements show that polyacrylic acid dopes the polyaniline. Pervaporation of water and water/acetic acid mixtures were performed using polyaniline and its polyacrylic acid blend. An improved flux over the polyaniline base form is observed. Polyaniline/polyimide blends were synthesized for gas permeability studies. These blends combine improved thermal stability relative to polyaniline with greater gas selectivity relative to polyimide. The blend shows an increase in permeability for all gases studied over both, polyaniline base and polyimide, while maintaining comparable separation factors.

  10. Counter pumping debris excluder and separator. [gas turbine shaft seals

    NASA Technical Reports Server (NTRS)

    Ludwig, L. P. (Inventor)

    1978-01-01

    A dirt separator and excluder for removing entrained debris from gas turbine shaft seals is described. A helical groove pattern is constructed on the rotating shaft with the pumping pattern such that it tends to pump seal pressurizing gas toward the gas turbine seal. A second helical groove pattern is provided on the stationary housing or counter rotating member coaxial with the shaft, and this pattern is designed to provide pumping in the direction opposite from that of the groove pattern on the shaft. Gas with entrained debris entering this grooved area will be subjected to high centrifugal forces due to the swirl motion induced by the groove pattern and the rotation of the shaft. This debris is centrifuged outwardly into the outer groove pattern on the housing or counter rotating member. Because the outer groove pattern has a pumping direction opposite from that of the seal, dirt is pumped away from the seal and can be collected in a suitable debris trap remote from the seal location.

  11. Hydrogen isotope separation installation for the regeneration of tritium from gas mixtures in tritium facilities

    SciTech Connect

    Andrew, B.M.; Perevezentsev, A.N.; Selivanenko, I.L.

    1994-12-31

    The advantages and disadvantages of different methods for hydrogen isotope separation are considered in terms of their applicability for tritium regeneration in a tritium facility. Due to low inventory, simplicity of operation, flexibility, and safety the methods of separation using solid phases are preferable for tritium facility. The detail consideration of the separation processes with a solid phase reveals that highest efficiency of separation should be achieved in a counter-current separation column, which allow multiplying the thermodynamic isotopic effect. Because of difficulties of the organization of a solid phase motion in a separation column this method did not found practical application for separation of hydrogen isotopic mixtures. The main efforts of a few researches groups were devoted to improve the chromatographic separation process and equipment. The detail comparison of the separation in sectioned column with that in chromatographic as well as in cryodistillation columns show that counter-current separation in a sectioned column is more effective and has other advantages when middle throughput is required. Complete regeneration of an isotopic mixture with separation into three practically pure isotopes independently from isotopic composition of feed can be provided using two sectioned separation columns. Separation installation can operate continuously as well as periodically.

  12. Optimization of liquid chromatographic method for the separation of nine hydrophilic and hydrophobic components in Salviae miltiorrhizae Radix et Rhizoma (Danshen) using microemulsion as eluent.

    PubMed

    Huang, Hongzhang; Xuan, Xueyi; Xu, Liyuan; Yang, Jianrui; Gao, Chongkai; Li, Ning

    2014-04-01

    In this study, we have proposed and developed a novel, environmental-friendly and simple method for separation of nine hydrophilic and hydrophobic components in Danshen using microemulsion liquid chromatography. The proposed method was optimized via the preliminary screening experiment and the experimental design. The following factors were investigated in preliminary screening experiment: pH of mobile phase, column type, the nature of surfactant, the nature of oil phase and additives. In order to simultaneously optimize resolution and analysis time, the chromatographic optimization function (COF) was adopted to evaluate chromatograms. The central composite design (CCD) was used to create the matrix of experiments for mapping the chromatographic response surface. Finally, the COF values were fitted into a second order polynomial model and the response surface methodology (RSM) was employed to find the optimal eluent constituents. The reliability of the established model was confirmed by the good agreement obtained between experimental data and predictive values. Based on the results from the preliminary screening experiment and the CCD optimization, the optimal mobile phase was identified as a solution consisting of 6.68% (w/w) polyoxyethylene lauryl ether (Brij35), 0.84% (w/w) cyclohexane, 6.92% (w/w) n-butanol, 85.56% (w/w) phosphate buffer (pH 6.60) and 8mM cetyltrimethyl ammonium bromide (CTAB).

  13. Synthesis and characterization of novel stationary phases for small scale liquid chromatographic separations of proteins and nanoparticles

    NASA Astrophysics Data System (ADS)

    Hutanu, Daniela

    The emerging field of nanotechnology strictly requires the micro-scaling of the available separation technology and the design of novel devices for separations of molecules of interest. The separation of proteins and nanoparticles is challenging due to their relatively large size, non-specific adherence to surfaces and instability in many solvents. This dissertation presents the synthesis and characterization of novel stationary phases for use in separations of proteins or nanoparticles in both capillary and microchip formats. In order to separate blood proteins with high specificity, a DNA aptamer selected for alpha-thrombin was employed as an affinity component of the stationary phases. Silica surfaces and organic monoliths were modified with the aptamer via an azlactone linkage and have demonstrated highly efficient separations of thrombin from a mixture in the microscale. The high efficiency of the protein separation (HETP = 276 mum, RS = 1.7) is comparable with macroscale results using antibodies as the affinity factor. Novel hybrid inorganic-organic polysilsesquioxane stationary phases were synthesized by way of surfactant templated polymerization of bridged alcoxy-silyl ethane monomers, in presence of sodium hydroxide. The novel materials were successful in size exclusion separation of polystyrene standards with molecular diameters of 0.3-2.4 nm. A hybrid inorganic-organic polysilsesquioxane sorbent also proved useful for small scale separations of triphenyl phosphine protected gold nanoparticles, based on a sorptive mechanism instead of a size exclusion mechanism. Polysilsesquioxanes were easily synthesized in-situ inside fused silica capillary columns and PMMA microchip channels in order to facilitate integration with a micro-reactor. The novel stationary phases proved efficient for separation of proteins and nanoparticles in the micro-scale format and can further be utilized for online purification and separation of these difficult compounds.

  14. Selectivity trend of gas separation through nanoporous graphene

    DOE PAGES

    Liu, Hongjun; Chen, Zhongfang; Dai, Sheng; ...

    2014-01-29

    We demonstrate that porous graphene can efficiently separate gases according to their molecular sizes using molecular dynamic (MD) simulations,. The flux sequence from the classical MD simulation is H2>CO2>>N2>Ar>CH4, which generally follows the trend in the kinetic diameters. Moreover, this trend is also confirmed from the fluxes based on the computed free energy barriers for gas permeation using the umbrella sampling method and kinetic theory of gases. Both brute-force MD simulations and free-energy calcualtions lead to the flux trend consistent with experiments. Case studies of two compositions of CO2/N2 mixtures further demonstrate the separation capability of nanoporous graphene.

  15. Selectivity trend of gas separation through nanoporous graphene

    SciTech Connect

    Liu, Hongjun; Chen, Zhongfang; Dai, Sheng; Jiang, De-en

    2014-01-29

    We demonstrate that porous graphene can efficiently separate gases according to their molecular sizes using molecular dynamic (MD) simulations,. The flux sequence from the classical MD simulation is H2>CO2>>N2>Ar>CH4, which generally follows the trend in the kinetic diameters. Moreover, this trend is also confirmed from the fluxes based on the computed free energy barriers for gas permeation using the umbrella sampling method and kinetic theory of gases. Both brute-force MD simulations and free-energy calcualtions lead to the flux trend consistent with experiments. Case studies of two compositions of CO2/N2 mixtures further demonstrate the separation capability of nanoporous graphene.

  16. Computing at the Dubna gas-filled recoil separator

    NASA Astrophysics Data System (ADS)

    Tsyganov, Yuri S.; Polyakov, Alexandr N.

    2006-03-01

    Simulation codes for the spectra of heavy implanted nuclei, applications for online data visualization and real time PC-based algorithms are considered. Special attention is paid to the application of real time techniques for radical suppression of background products in heavy-ion-induced nuclear reactions at the U-400 cyclotron of the Flerov Laboratory of Nuclear Reactions. The detection system of the Dubna gas-filled recoil separator (DGFRS) is also briefly described. Calculated heavy recoil spectra are compared with those measured in heavy-ion-induced nuclear reactions.

  17. Adsorption and Gas Separation of Molecules by Carbon Nanohorns.

    PubMed

    Gatica, Silvina M; Nekhai, Anton; Scrivener, Adam

    2016-05-19

    In this paper, we report the results of Monte Carlo simulations of the adsorption of neon, argon, methane and carbon dioxide in carbon nanohorns. We model the nanohorns as an array of carbon cones and obtained adsorption isotherms and isosteric heats. The main sites of adsorption are inside the cones and in the interstices between three cones. We also calculated the selectivity of carbon dioxide/methane, finding that nanohorns are a suitable substrate for gas separation. Our simulations are compared to available experimental data.

  18. Gas separation by composite solvent-swollen membranes

    DOEpatents

    Matson, S.L.; Lee, E.K.L.; Friesen, D.T.; Kelly, D.J.

    1989-04-25

    There is disclosed a composite immobilized liquid membrane of a solvent-swollen polymer and a microporous organic or inorganic support, the solvent being at least one highly polar solvent containing at least one nitrogen, oxygen, phosphorus or sulfur atom, and having a boiling point of at least 100 C and a specified solubility parameter. The solvent or solvent mixture is homogeneously distributed through the solvent-swollen polymer from 20% to 95% by weight. The membrane is suitable for acid gas scrubbing and oxygen/nitrogen separation. 3 figs.

  19. Gas separation by composite solvent-swollen membranes

    DOEpatents

    Matson, Stephen L.; Lee, Eric K. L.; Friesen, Dwayne T.; Kelly, Donald J.

    1989-01-01

    There is disclosed a composite immobulized liquid membrane of a solvent-swollen polymer and a microporous organic or inorganic support, the solvent being at least one highly polar solvent containing at least one nitrogen, oxygen, phosphorous or sulfur atom, and having a boiling point of at least 100.degree. C. and a specified solubility parameter. The solvent or solvent mixture is homogeneously distributed through the solvent-swollen polymer from 20% to 95% by weight. The membrane is suitable for acid gas scrubbing and oxygen/nitrogen separation.

  20. Methods of calculating engineering parameters for gas separations

    NASA Technical Reports Server (NTRS)

    Lawson, D. D.

    1980-01-01

    A group additivity method has been generated which makes it possible to estimate, from the structural formulas alone, the energy of vaporization and the molar volume at 25 C of many nonpolar organic liquids. From these two parameters and appropriate thermodynamic relationships it is then possible to predict the vapor pressure of the liquid phase and the solubility of various gases in nonpolar organic liquids. The data are then used to evaluate organic and some inorganic liquids for use in gas separation stages or as heat exchange fluids in prospective thermochemical cycles for hydrogen production.