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Sample records for gas chromatographic detection

  1. 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.

  2. 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.

  3. EVALUATION OF PORTABLE GAS CHROMATOGRAPHS

    EPA Science Inventory

    Limits of detection, linearity of responses, and stability of response factors and retention times for five commercially-available portable gas chromatographs (PGC) were determined during laboratory evaluation. he PGCs were also operated at the French Limited Superfund site near ...

  4. Gas chromatographic identification of Clostridium difficile and detection of cytotoxin from a modified selective medium.

    PubMed Central

    Levett, P N; Phillips, K D

    1985-01-01

    A modification of an existing selective medium for Clostridium difficile is described. Inclusion in the medium of DL nor-leucine and p-hydroxyphenylacetic acid enables identification of C difficile to be made directly from primary isolation plates by gas chromatographic detection of caproic acid and p-cresol. Plugs of agar withdrawn from the selective medium also allow the detection of cytotoxin production in vitro. PMID:3968212

  5. 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.

  6. 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.

  7. Protecting Gas Chromatographic Syringes

    NASA Astrophysics Data System (ADS)

    Ruekberg, Ben

    1995-12-01

    This article describes the construction of a device which protects gas chromatographic syringes. The device lessens the likelihood of syringes rolling off tables and breaking. If the syringe is dropped, the glass barrel is less apt to be struck and shattered.

  8. 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.

  9. 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.

  10. 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...

  11. Derivatization and gas chromatographic-mass spectrometric detection of anabolic steroid residues isolated from edible muscle tissues.

    PubMed

    Daeseleire, E; De Guesquière, A; Van Peteghem, C

    1991-01-01

    A method was developed for the detection of anabolic steroid residues in edible muscle tissues. After enzymic digestion of the tissue and purification on disposable C18 solid-phase extraction columns, the extract was injected onto a C18 reversed-phase high-performance liquid chromatographic column. Three fractions or windows were collected, each containing specific analytes. After evaporation to dryness, the residues were subjected to a derivatization procedure which yielded suitable derivatives. After gas chromatographic-mass spectrometric analysis, both gas chromatographic retention data and mass spectral data were used for the detection and identification of nortestosterone, testosterone, estradiol, ethinylestradiol, trenbolone, methyltestosterone, chlormadinone acetate, medroxyprogesterone acetate and megestrol acetate. PMID:2026730

  12. Headspace gas chromatographic determination of methylene chloride in decaffeinated tea and coffee, with electrolytic conductivity detection.

    PubMed

    Page, B D; Charbonneau, C F

    1984-01-01

    A headspace gas chromatographic procedure is described for the determination of methylene chloride (MC) in decaffeinated tea and coffee. The tea or coffee sample, with added methylene bromide (MB) internal standard, is equilibrated for 1.5 h at 100 degrees C in aqueous sodium sulfate before manual headspace sampling. MC and MB are separated on a Porasil A column at 160 degrees C and detected by using a Coulson electrolytic conductivity detector. For coffee and tea samples spiked at 1.3 ppm MC, as well as commercially decaffeinated teas and coffees containing up to 8 ppm MC, coefficients of variation were 10% or less. For decaffeinated teas, problems involving sample homogeneity and loss of MC before sealing the headspace vial had to be overcome. Similar problems with decaffeinated instant and ground coffees were minimal. The headspace procedure was superior to a previously reported distillation technique. MC was readily detected at 0.05 ppm. Fourteen decaffeinated teas and 15 decaffeinated coffees were analyzed; MC was detected at levels that ranged up to 15.9 and 4.0 ppm, respectively. PMID:6469909

  13. The gas-liquid chromatograph and the electron capture detection in equine drug testing.

    PubMed Central

    Blake, J. W.; Tobin, T.

    1976-01-01

    Three gas-liquid chromatographic (G.L.C.) procedures discussed have been designed around the four "esses" of detection tests--speed, sensitivity, simplicity, and specificity. These techniques are admirably applicable to the very low plasma drug levels encountered in blood testing under pre-race conditions. The methods are equally applicable to post-race testing procedures, where both blood and urine samples are tested. Drugs can only rarely be detected by the electron capture detector (E.C.D.) without a prior derivatization step, which conveys to the drug(s) high electron affinity. Because of broad applicability, two derivatizing agents, heptafluorobutyric (HFBA) and pentafluorpropionic (PFPA) anhydrides are employed. The three techniques, allowing broad coverage of various drug classes are: 1) direct derivatization of drugs to form strongly electron capturing amides and esters. 2) reductive fragmentation of drugs with lithium aluminum hydride to form alcohols, with conversion to ester derivatives. 3) oxidative fragmentation of drugs with potassium dichromate to form derivatizable groups, followed by direct derivatization. PMID:1000157

  14. Microfabricated packed gas chromatographic column

    DOEpatents

    Kottenstette, Richard; Matzke, Carolyn M.; Frye-Mason, Gregory C.

    2003-12-16

    A new class of miniaturized gas chromatographic columns has been invented. These chromatographic columns are formed using conventional micromachining techniques, and allow packed columns having lengths on the order of a meter to be fabricated with a footprint on the order of a square centimeter.

  15. Microminiature gas chromatographic column

    NASA Technical Reports Server (NTRS)

    Donaldson, R. W., Jr.

    1972-01-01

    Techniques commonly used for fabrication of integrated circuits are utilized to produce long capillary tubes for microminiature chromatographs. Method involves bonding of flat silicon plate to top of spirally grooved silicon chip to close groove and form capillary column.

  16. 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.

  17. Evaluation of portable gas chromatographs

    SciTech Connect

    Berkley, R.E.; Miller, M.; Chang, J.C.; Oliver, K.; Fortune, C.

    1993-01-01

    Limits of detection, linearity of responses, and stability of response factors and retention times for five commercially-available portable gas chromatographs (PGC) were determined during laboratory evaluation. The PGCs were also operated at the French Limited Superfund site near Houston, TX during startup of bioremediation. Concentrations of volatile organic compounds (VOC) at the site were slightly above ambient background levels. Concurrent collocated grab samples were collected periodically in canisters and analyzed by Method TO-14 using a mass-selective detector. Canister data were taken to indicate correct concentrations and were used to assess the accuracy of PGC data. Durability, reliability, and complexity of operation of PGCs were also evaluated. The principal goal of the study was to determine the best way to use each instrument as a monitor for airborne VOCs.

  18. Detection of discoloration in diesel fuel based on gas chromatographic fingerprints.

    PubMed

    Krakowska, Barbara; Stanimirova, Ivana; Orzel, Joanna; Daszykowski, Michal; Grabowski, Ireneusz; Zaleszczyk, Grzegorz; Sznajder, Miroslaw

    2015-02-01

    In the countries of the European Community, diesel fuel samples are spiked with Solvent Yellow 124 and either Solvent Red 19 or Solvent Red 164. Their presence at a given concentration indicates the specific tax rate and determines the usage of fuel. The removal of these so-called excise duty components, which is known as fuel "laundering", is an illegal action that causes a substantial loss in a government's budget. The aim of our study was to prove that genuine diesel fuel samples and their counterfeit variants (obtained from a simulated sorption process) can be differentiated by using their gas chromatographic fingerprints that are registered with a flame ionization detector. To achieve this aim, a discriminant partial least squares analysis, PLS-DA, for the genuine and counterfeit oil fingerprints after a baseline correction and the alignment of peaks was constructed and validated. Uninformative variables elimination (UVE), variable importance in projection (VIP), and selectivity ratio (SR), which were coupled with a bootstrap procedure, were adapted in PLS-DA in order to limit the possibility of model overfitting. Several major chemical components within the regions that are relevant to the discriminant problem were suggested as being the most influential. We also found that the bootstrap variants of UVE-PLS-DA and SR-PLS-DA have excellent predictive abilities for a limited number of gas chromatographic features, 14 and 16, respectively. This conclusion was also supported by the unitary values that were obtained for the area under the receiver operating curve (AUC) independently for the model and test sets. PMID:25407430

  19. 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.

  20. Electron capture gas chromatographic detection of acethylmethylcarbinol produced by neisseria gonorrhoeae.

    PubMed

    Morse, C D; Brooks, J B; Kellogg, D S

    1976-01-01

    Acetylmethylcarbinol (acetoin) production by Neisseria gonorrhoeae and other Neisseria species was established by gas-liquid chromatography and by mass spectrometric data. Sixty-nine isolates of Neisseria were tested by incubating them in a chemically defined fluid medium. The medium was extracted with organic solvents and derivatized with heptafluorobutryic anhydride for gas chromatography and mass spectrometry. Cultures of 58 of the same strains were tested with the conventional Voges-Proskauer reagents, and results were compared with those of gas-liquid chromatography. When glucose was used as an energy source, N. gonorrhoeae, some N. meningitidis, and N. lactamica produced enough acetoin in 16 h to be detectable by either method, whereas other Neisseria species produce amounts detectable only by gas chromatography. The conventional acetylmethylcarbinol test with the chemically defined medium and maltose as an energy source might be used to develop methods that would differentiate certain members of the genus, including the pathogenic species. PMID:815266

  1. Capillary gas chromatography of amino acids, including asparagine and glutamine: sensitive gas chromatographic-mass spectrometric and selected ion monitoring gas chromatographic-mass spectrometric detection of the N,O(S)-tert.-butyldimethylsilyl derivatives.

    PubMed

    Chaves Das Neves, H J; Vasconcelos, A M

    1987-04-17

    Amino acids and the amino acid amides glutamine and asparagine can be simultaneously derivatized to the corresponding N,O(S)-tert.-butyldimethylsilyl derivatives in a one-step reaction with N-methyl-N-(tert.-butyldimethylsilyl)trifluoroacetamide in acetonitrile. The solution is used directly for gas chromatography (GC). Losses due to evaporation steps are avoided. Except for the more basic amino acids, derivatization occurs at room temperature. Lysine, arginine and histidine require additional heating at 150 degrees C for 2.5 h in order to complete derivatization. The derivatization has high reproducibility. The response factors relative to norvaline or cycloleucine lie between 0.40 and 1.30. Arginine is the most difficult amino acid to derivatize. The size of the tert.-butyldimethylsilyl (TBDMS) group prevents multiple silylation of the nitrogen atoms. Only a single peak is observed for each compound. Twenty-seven amino acid (and glutamine and asparagine) derivatives were simultaneously chromatographed and well separated in a single run on a 25 m X 0.20 mm I.D. glass capillary column coated with OV-1. The TBDMS derivatives possess very characteristic EI mass spectra at 70 eV, with intense diagnostic ions. This makes them very appropriate for GC-mass spectrometric (MS) work and selected ion monitoring GC-MS at the picomole level. The detection limit for arginine as the TBDMS derivative is less than 0.3 ng. The usefulness of the method is illustrated by the detection of amino acids in a peptide hydrolysate obtained from 1 microgram of bovin insulin B-chain. PMID:3597576

  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. 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. PMID:16509343

  4. Gas chromatograph injection port protective device

    NASA Technical Reports Server (NTRS)

    Robertson, M. D.; Welz, E. A.

    1969-01-01

    To prevent samples containing foreign matter from poisoning the gas chromatographic columns, a pre-filter insertion is placed in the injection port. The packing becomes a variable reactant, for example, acids are removed by using an alkaline liquid.

  5. 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)

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

    PubMed

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

    2001-03-01

    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. PMID:11269587

  7. 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.

  8. 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.

  9. 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...

  10. 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...

  11. 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.

  12. 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.

  13. 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.

  14. [A gas chromatographic method for determining acetaldehyde in cadaver blood].

    PubMed

    Savich, V I; Valladares, Kh A; Gusakov, Iu A; Skachko, Z M

    1990-01-01

    Gas-chromatographic method of acetaldehyde detection in blood of subjects who died of alcoholic intoxication is suggested. Method is simple, does not require additional expenses, can be readily used in medicolegal practice and in difficult cases it may help the expert to make an objective conclusion on the cause of death. PMID:2087747

  15. Simple gas chromatographic method for furfural analysis.

    PubMed

    Gaspar, Elvira M S M; Lopes, João F

    2009-04-01

    A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSD<8%), showed good recoveries (77-107%) and good limits of detection (GC-FID: 1.37 microgL(-1) for 2-F, 8.96 microgL(-1) for 5-MF, 6.52 microgL(-1) for 5-HMF; GC-TOF-MS: 0.3, 1.2 and 0.9 ngmL(-1) for 2-F, 5-MF and 5-HMF, respectively). It was applied to different commercial food matrices: honey, white, demerara, brown and yellow table sugars, and white and red balsamic vinegars. This one-step, sensitive and direct method for the analysis of furfurals will contribute to characterise and quantify their presence in the human diet. PMID:18976770

  16. 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.

  17. A nonlinear model for gas chromatograph systems

    NASA Technical Reports Server (NTRS)

    Feinberg, M. P.

    1975-01-01

    Fundamental engineering design techniques and concepts were studied for the optimization of a gas chromatograph-mass spectrometer chemical analysis system suitable for use on an unmanned, Martian roving vehicle. Previously developed mathematical models of the gas chromatograph are found to be inadequate for predicting peak heights and spreading for some experimental conditions and chemical systems. A modification to the existing equilibrium adsorption model is required; the Langmuir isotherm replaces the linear isotherm. The numerical technique of Crank-Nicolson was studied for use with the linear isotherm to determine the utility of the method. Modifications are made to the method eliminate unnecessary calculations which result in an overall reduction of the computation time of about 42 percent. The Langmuir isotherm is considered which takes into account the composition-dependent effects on the thermodynamic parameter, mRo.

  18. Coupling of a gas chromatograph to a simultaneous-detection inductively coupled plasma mass spectrograph for speciation of organohalide and organometallic compounds

    SciTech Connect

    Barnes, James H.; Schilling, G; Sperline, Roger; Denton, M Bonner B.; Young, Erick T.; Barinaga, Charles J.; Koppenaal, David W.; Hieftje, Gary M.

    2004-06-01

    A gas chromatograph (GC) has been coupled to an inductively coupled plasma Mattauch-Herzog geometry mass spectrograph (ICP-MHMS) equipped with a novel detector array. In its current state of development the detector array, termed the focal plan camera (FPC), permits the simultaneous monitoring of up to 15 m/z values. A heated line was used to transfer the capillary-column effluent from the GC to the ICP torch, though due to instrument operating conditions, the transfer line was terminated 50 mm ahead of the ICP torch. Minimal tailing was observed, with the most severe effect seen for high-boiling analytes. With the coupling, absolute limits of detection are in the tens to hundreds of femtogram regime for organometallic species and in the single pictogram regime for halogenated hydrocarbons.

  19. 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

  20. Development of Gas Chromatographic Mass Spectrometry.

    PubMed

    Hites, Ronald A

    2016-07-19

    Gas chromatographic mass spectrometry is now widely used for the quantitation and identification of organic compounds in almost any imaginable sample. These applications include the measurement of chlorinated dioxins in soil samples, the identification of illicit drugs in human blood, and the quantitation of accelerants in arson investigations, to name just a few. How did GC/MS get so popular? It turns out that it required parallel developments in mass spectrometry, gas chromatography, and computing and that no one person "invented" the technique. This Perspective traces this history from the 1950s until today. PMID:27384908

  1. 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.

  2. Economic gas chromatograph system for subambient pressure gas sampling

    NASA Technical Reports Server (NTRS)

    Mitchell, S. M.

    1970-01-01

    Gas chromatograph sampling system consists of a manifold with a gas-sample valve, a minimum-volume pressure transducer with a portable monitor, a vacuum-source valve, and a sample inlet valve. Increased accuracy of analysis is obtained by better control of sample size.

  3. 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

  4. Gas chromatographic-mass spectrometry method for the detection of busulphan and its metabolites in plasma and urine.

    PubMed

    El-Serafi, Ibrahim; Terelius, Ylva; Twelkmeyer, Brigitte; Hagbjörk, Ann-Louise; Hassan, Zuzana; Hassan, Moustapha

    2013-01-15

    Busulphan is an alkylating agent used as conditioning regimen prior to stem cell transplantation. Busulphan is metabolized in the liver and four major metabolites have been identified. The first metabolite is tetrahydrothiophene which is oxidized to tetrahydrothiophene 1-oxide, then sulfolane and finally 3-hydroxy sulfolane. Despite the low molecular weight and wide polarity range of busulphan and its four metabolites, the use of a fused silica non-polar column significantly enhanced the automated gas chromatography-mass spectrometry of their detection in one simple method. The limit of quantification was 0.5μM for busulphan and all its metabolites except 3-OH sulfolane, which was 1.25μM. This method was validated for all the compounds in both human plasma and urine. Lower limits of quantifications (LLOQs) were run in pentaplicate per compound and all results were within 20% of the nominal values. The recovery was determined by comparing the peak area of two quality control (QC) samples, before and after extraction in plasma and urine, in triplicate. Acceptable precision and accuracy have been obtained; at least 3 standard curves have been run for each compound using three different QCs covering the calibration curve in triplicate. The QC values were within 15% (SD) of the nominal values. Selectivity and sensitivity of all compounds have been measured. Compounds were stable up to 50 days after extraction in -20°C and 48h at RT. Moreover, the compounds were stable for three cycles of freezing and thawing. The method was applied in a clinical case where the patient received high dose busulphan; all the compounds have been detected, identified and quantified both in plasma and urine. PMID:23286981

  5. The Gas Chromatograph Mass Spectrometer for the Huygens Probe

    NASA Astrophysics Data System (ADS)

    Niemann, H. B.; Atreya, S. K.; Bauer, S. J.; Biemann, K.; Block, B.; Carignan, G. R.; Donahue, T. M.; Frost, R. L.; Gautier, D.; Haberman, J. A.; Harpold, D.; Hunten, D. M.; Israel, G.; Lunine, J. I.; Mauersberger, K.; Owen, T. C.; Raulin, F.; Richards, J. E.; Way, S. H.

    2002-07-01

    The Gas Chromatograph Mass Spectrometer (GCMS) on the Huygens Probe will measure the chemical composition of Titan's atmosphere from 170 km altitude (˜1 hPa) to the surface (˜1500 hPa) and determine the isotope ratios of the major gaseous constituents. The GCMS will also analyze gas samples from the Aerosol Collector Pyrolyser (ACP) and may be able to investigate the composition (including isotope ratios) of several candidate surface materials. The GCMS is 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 employs five ion sources sequentially feeding the mass analyzer. Three ion sources serve as detectors for the GC columns and two are dedicated to direct atmosphere sampling and ACP gas sampling respectively. The instrument is also equipped with a chemical scrubber cell for noble gas analysis and a sample enrichment cell for selective measurement of high boiling point carbon containing constituents. The mass range is 2 to 141 Dalton and the nominal detection threshold is at a mixing ratio of 10- 8. The data rate available from the Probe system is 885 bit/s. The weight of the instrument is 17.3 kg and the energy required for warm up and 150 minutes of operation is 110 Watt-hours.

  6. The Gas Chromatograph Mass Spectrometer for the Huygens Probe

    NASA Astrophysics Data System (ADS)

    Niemann, H. B.; Atreya, S. K.; Bauer, S. J.; Biemann, K.; Block, B.; Carignan, G. R.; Donahue, T. M.; Frost, R. L.; Gautier, D.; Haberman, J. A.; Harpold, D.; Hunten, D. M.; Israel, G.; Lunine, J. I.; Mauersberger, K.; Owen, T. C.; Raulin, F.; Richards, J. E.; Way, S. H.

    2002-07-01

    The Gas Chromatograph Mass Spectrometer (GCMS) on the Huygens Probe will measure the chemical composition of Titan's atmosphere from 170 km altitude (~1 hPa) to the surface (~1500 hPa) and determine the isotope ratios of the major gaseous constituents. The GCMS will also analyze gas samples from the Aerosol Collector Pyrolyser (ACP) and may be able to investigate the composition (including isotope ratios) of several candidate surface materials. The GCMS is 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 employs five ion sources sequentially feeding the mass analyzer. Three ion sources serve as detectors for the GC columns and two are dedicated to direct atmosphere sampling and ACP gas sampling respectively. The instrument is also equipped with a chemical scrubber cell for noble gas analysis and a sample enrichment cell for selective measurement of high boiling point carbon containing constituents. The mass range is 2 to 141 Dalton and the nominal detection threshold is at a mixing ratio of 10- 8. The data rate available from the Probe system is 885 bit/s. The weight of the instrument is 17.3 kg and the energy required for warm up and 150 minutes of operation is 110 Watt-hours.

  7. 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.

  8. FIELD COMPARISON OF PORTABLE GAS CHROMATOGRAPHS WITH METHOD TO-14

    EPA Science Inventory

    A field-deployable prototype fast gas chromatograph (FGC) and two commercially-available portable gas chromatographs (PGC) were evaluated by measuring organic vapors in ambient air at a field monitoring site in metropolitan San Juan, Puerto Rico. he data were compared with simult...

  9. Gas-Chromatographic Determination Of Water In Freon PCA

    NASA Technical Reports Server (NTRS)

    Melton, Donald M.

    1994-01-01

    Gas-chromatographic apparatus measures small concentrations of water in specimens of Freon PCA. Testing by use of apparatus faster and provides greater protection against accidental contamination of specimens by water in testing environment. Automated for unattended operation. Also used to measure water contents of materials, other than Freon PCA. Innovation extended to development of purgeable sampling accessory for gas chromatographs.

  10. Development of a Low Power Gas Chromatograph-Mass Spectrometer for In-Situ Detection of Organics in Martian Soil

    NASA Technical Reports Server (NTRS)

    Pinnick, Veronica; Buch, Arnaud; VanAmerom, Friso H. W.; Danell, Ryan M.; Brinckerhoff, William; Mahaffy, Paul; Cotter, Robert J.

    2011-01-01

    The Mars Organic Molecule Analyzer (MOMA) is a joint venture by NASA and the European Space Agency (ESA) to develop a sensitive, light-weight, low-power mass spectrometer for chemical analysis on Mars. MOMA is a key analytical instrument aboard the 2018 ExoMars rover mission seeking signs of past or present life. The current prototype was built to demonstrate operation of gas chromatography (OC) and laser desorption (LD) mass spectrometry under martian ambient conditions (5-7 Torr of CO2-rich atmosphere). Recent reports have discussed the MO MA concept, design and performance. Here, we update the current prototype performance, focusing specifically on the GCMS mode.

  11. Gas chromatographic concepts for the analysis of planetary atmospheres

    NASA Technical Reports Server (NTRS)

    Valentin, J. R.; Cullers, D. K.; Hall, K. W.; Krekorian, R. L.; Phillips, J. B.

    1991-01-01

    Over the last few years, new gas chromatographic (GC) concepts were developed for use on board spacecraft or any other restricted environments for determining the chemical composition of the atmosphere and surface material of various planetary bodies. Future NASA Missions include an entry probe that will be sent to Titan and various spacecraft that will land on Mars. In order to be able to properly respond to the mission science requirements and physical restrictions imposed on the instruments by these missions, GC analytical techniques are being developed. Some of these techniques include hardware and mathematical techniques that will improve GC sensitivity and increase the sampling rate of a GC descending through a planetary atmosphere. The technique of Multiplex Gas Chromatography (MGC) is an example of a technique that was studied in a simulated Titan atmosphere. In such an environment, the atmospheric pressure at instrument deployment is estimated to be a few torr. Thus, at such pressures, the small amount of sample that is acquired might not be enough to satisfy the detection requirements of the gas chromatograph. In MGC, many samples are pseudo-randomly introduced to the chromatograph without regard to elution of preceding components. The resulting data is then reduced using mathematical techniques such as cross-correlation of Fourier Transforms. Advantages realized from this technique include: improvement in detection limits of several orders of magnitude and increase in the number of analyses that can be conducted in a given period of time. Results proving the application of MGC at very low pressures emulating the same atmospheric pressures that a Titan Probe will encounter when the instruments are deployed are presented. The sample used contained hydrocarbons that are expected to be found in Titan's atmosphere. In addition, a new selective modulator was developed to monitor water under Martian atmospheric conditions. Since this modulator is selective only

  12. On-line gas chromatographic analysis of airborne particles

    DOEpatents

    Hering, Susanne V.; Goldstein, Allen H.

    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.

  13. 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)

  14. GAS CHROMATOGRAPHIC TECHNIQUES FOR THE MEASUREMENT OF ISOPRENE IN AIR

    EPA Science Inventory

    The chapter discusses gas chromatographic techniques for measuring isoprene in air. Such measurement basically consists of three parts: (1) collection of sufficient sample volume for representative and accurate quantitation, (2) separation (if necessary) of isoprene from interfer...

  15. Gas chromatographic determination of residual methylene chloride and trichloroethylene in decaffeinated instant and ground coffee with electrolytic conductivity and electron capture detection.

    PubMed

    Page, B D; Charbonneau, C F

    1977-05-01

    A method is described for the quantitative determination of residual methylene chloride (MC) and trichloroethylene (TCE) in decaffeinated instant and ground roasted coffees. The residual solvents were isolated by a closed system vacuum distillation technique with toluene as a carrier solvent, chromatographed on Chromosorb 102, detected by both electron capture and electrolytic conductivity detectors, and quantitated by comparison with an internal standard. Average recoveries of MC from instant and ground coffees spiked at 1, 10, and 25 ppm were 100.0 (88-113), 93.2 (92-95), and 97.7% (94-102%); and for TCE, 97.2 (92-101), 96.2 (95-99), and 96.5% (92-100%), respectively. The results from both detectors are compared. At lower attenuations, levels less than 1 ppm can be readily measured. The procedure developed was applied to domestic and imported coffee samples. PMID:858707

  16. Gas chromatographic detection of D-(-)-2,3-butanediol and butyric acid produced by sporeformers in cream-style corn and canned beef noodle soup: collaborative study.

    PubMed

    Schafer, M L; Peeler, J T; Bradshaw, J G; Hamilton, C H; Carver, R B

    1985-01-01

    A gas chromatographic method that identifies sporeformers as the cause of spoilage in swollen cans of low-acid foods was collaboratively studied in 2 stages. Two organic compounds produced by sporeformers, D-(-)-2,3-butanediol and butyric acid, are measured in the upper phase after centrifugation of the liquid portion of the can contents. Each sample is assayed on 2 packed columns designed for the assay of aqueous solutions of volatile fatty acids, using flame ionization detectors. For study 1, 16 duplicate inoculated cans of cream-style corn and beef noodle soup were sent to 9 collaborators. For study 2, 7 collaborators received 11 duplicate inoculated cans of the 2 foods. Duplicate uninoculated cans of each food served as negative controls. The inocula were 6 sporeforming organisms (4 Clostridium and 2 gas-forming Bacillus species) and 2 nonsporeformers. After the deletion of marginal samples, the percentages of correctly identified sporeformers and nonsporeformers in beef noodle soup were 83 (110/132) and 90 (54/60), respectively; corresponding percentages for cream-style corn were 80 (98/123) and 100 (35/35). The method has been adopted official first action. PMID:4030630

  17. Gas chromatographic mass spectrometric detection of dihydroxy fatty acids preserved in the 'bound' phase of organic residues of archaeological pottery vessels.

    PubMed

    Hansel, Fabricio A; Bull, Ian D; Evershed, Richard P

    2011-07-15

    A methodology is presented for the determination of dihydroxy fatty acids preserved in the 'bound' phase of organic residues preserved in archaeological potsherds. The method comprises saponification, esterification, silica gel column chromatographic fractionation, and analysis by gas chromatography/mass spectrometry. The electron ionisation mass spectra of the trimethylsilyl ether methyl ester derivatives are characterised by fragment ions arising from cleavage of the bond between the two vicinal trimethylsiloxy groups. Other significant fragment ions are [M-15](+.), [M-31](+.), m/z 147 and ions characteristic of vicinal disubstituted (trimethylsiloxy) TMSO- groups (Δ(7,8), Δ(9,10), Δ(11,12) and Δ(13,14): m/z 304, 332, 360 and 388, respectively). The dihydroxy fatty acids identified in archaeological extracts exhibited carbon numbers ranging from C(16) to C(22) and concentrations varying from 0.05 to 14.05 µg g(-1) . The wide range of dihydroxy fatty acids observed indicates that this approach may be applied confidently in screening archaeological potsherds for the degradation products of monounsaturated fatty acids derived from commodities processed in archaeological pottery vessels. PMID:21638365

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

    PubMed

    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 conclusions 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 inclusion on 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 crushing 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 processes involved in the history of the samples analyzed. PMID:11541990

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

    USGS Publications Warehouse

    Andrawes, F.; Holzer, G.; Roedder, E.; Gibson, E.K., Jr.; 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.

  20. GAS CHROMATOGRAPHIC MICROMETHOD FOR TRACE DETERMINATIONS OF PHENOLS

    EPA Science Inventory

    A gas chromatographic procedure is described for the analysis of a variety of substituted phenols from water samples. The method was designed for situations when the sample size is very limited (0.5 to 1.0 ml), such as in laboratory microcosm experiments on transport and fate of ...

  1. Gas chromatographic column for the Viking 1975 molecular analysis experiment

    NASA Technical Reports Server (NTRS)

    Novotny, M.; Hayes, J. M.; Bruner, F.; Simmonds, P. G.

    1975-01-01

    A gas chromatographic column has been developed for use in the remote analysis of the Martian surface. The column, which utilizes a liquid-modified organic adsorbent (Tenax) as the stationary phase, provides efficient transmission and resolution of nanogram quantities of organic materials in the presence of millionfold excesses of water and carbon dioxide.

  2. 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.

  3. 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.

  4. Gas-liquid chromatographic determination of morphine, heroin, and cocaine.

    PubMed

    Prager, M J; Harrington, S M; Governo, T F

    1979-03-01

    Morphine, heroin, and cocaine are quantitatively determined with the same gas-liquid chromatographic system. The compounds are separated on a 6 ft X 2 mm id glass column packed with a 1:1 mixture of 5% SE-30 on 80--100 mesh Chromosorb W and 3% OV-17 on 80--100 mesh Varaport 30. The column is temperature-programmed. Flame ionization detector responses are measured with a computer-based data system. Heroin and cocaine are chromatographed directly; morphine is derivatized first. The procedure was evaluated with previously analyzed commercial and forensic samples. Accuracy and precision were 5 and 3%, respectively. PMID:447602

  5. Analytical Method for the Detection of Ozone Depleting Chemicals (ODC) in Commercial Products Using a Gas Chromatograph with an Electron Capture Detector (GC-ECD)

    SciTech Connect

    Lee, Richard N.; Dockendorff, Brian P.; Wright, Bob W.

    2008-08-01

    This document describes an analytical procedure that was developed for the trace level detection of residual ozone depleting chemicals (ODC) associated with the manufacture of selected commercial products. To ensure the United States meets it obligation under the Montreal Protocol, Congress enacted legislation in 1989 to impose an excise tax on electronic goods imported into the United States that were produced with banned chemicals. This procedure was developed to technically determine if residual ODC chemicals could be detected on electronic circuit boards. The analytical method utilizes a “purge and trap” technique followed by gas chromatography with electron capture detection to capture and analyze the volatile chemicals associated with the matrix. The method describes the procedure, the hardware, operating conditions, calibration, and quality control measures in sufficient detail to allow the capability to be replicated. This document corresponds to internal Standard Operating Procedure (SOP) EFL-130A, Rev 4.

  6. 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.

  7. Ion chromatographic separation and quantitation of alkyl methylamines and ethylamines in atmospheric gas and particulate matter using preconcentration and suppressed conductivity detection.

    PubMed

    VandenBoer, T C; Markovic, M Z; Petroff, A; Czar, M F; Borduas, N; Murphy, J G

    2012-08-24

    Two methods based on ion chromatography (IC) were developed for the detection of methyl and ethyl alkyl amines (methylamine (MA), ethylamine (EA), dimethylamine (DMA), diethylamine (DEA), trimethylamine (TMA) and triethylamine (TEA)) and NH(3)/NH(4)(+) in online atmospheric gas-particle and size-resolved particulate samples. The two IC methods were developed to analyze samples collected with an ambient ion monitor (AIM), an online gas-particle collection system, or with a Micro Orifice Uniform Deposit Impactor (MOUDI) for size-resolved particle samples. These methods enable selective and (semi-) quantitative detection of alkyl amines at ambient atmospheric concentrations (pptv and pgm(-3)) in samples where significant interferences can be expected from Na(+) and NH(4)(+), for example marine and rural air masses. Sample pre-concentration using a trace cation column enabled instrumental detection limits on the order of pmol (sub-ng) levels per sample, an improvement of up to 10(2) over current IC methods. Separation was achieved using a methanesulfonic acid gradient elution on Dionex CS12A and CS17 columns. The relative standard deviations in retention times during 3 weeks continuous (hourly) sampling campaigns ranged from 0.1 to 0.5% and 0.2 to 5% for the CS12A and CS17 across a wide dynamic range of atmospheric concentrations. Resolution of inorganic and organic cations is limited to 25min for online samples. Mass-dependent coelution of NH(4)(+)/MA/EA occurred on the CS12A column and DEA/TMA coeluted on both columns. Calibrations of ammonium show a non-linear response across the entire calibration range while all other analytes exhibit high linearity (R(2)=0.984-0.999), except for EA and TEA on the CS12A (R(2)=0.960 and 0.941, respectively). Both methods have high analytical accuracy for the nitrogenous bases ranging from 9.5 to 20% for NH(3) and <5-15% for the amines. Hourly observations of amines at Egbert, ON in October 2010 showed gaseous DMA and TMA+DEA at 1

  8. A sensitive gas chromatographic-tandem mass spectrometric method for detection of alkylating agents in water: application to acrylamide in drinking water, coffee and snuff.

    PubMed

    Pérez, Hermes Licea; Osterman-Golkar, Siv

    2003-08-01

    A sensitive analytical method for the analysis of acrylamide and other electrophilic agents in water has been developed. The amino acid L-valine served as a nucleophilic trapping agent. The method was applied to the analysis of acrylamide in 0.2-1 mL samples of drinking water or Millipore-filtered water, brewed coffee, or water extracts of snuff. The reaction product, N-(2-carbamoylethyl)valine, was incubated with pentafluorophenyl isothiocyanate to give a pentafluorophenylthiohydantoin (PFPTH) derivative. This derivative was extracted with diethyl ether, separated from excess reagent and impurities by a simple extraction procedure, and analyzed by gas chromatography-tandem mass spectrometry. (2H3)Acrylamide, added before the reaction with L-valine, was used as internal standard. Acrylamide and the related compound, N-methylolacrylamide, gave the same PFPTH derivative. The concentrations of acrylamides were < or = 0.4 nmol L(-1) (< or = 0.03 microg acrylamide L(-1)) in water, 200 to 350 nmol L(-1) in brewed coffee, and 10 to 34 nmol g(-1) snuff in portion bags, respectively. The precision (the coefficient of variation was 5%) and accuracy of the method were good. The detection limit was considerably lower than that of previously published methods for the analysis of acrylamide. PMID:12964603

  9. Gas chromatographic method using nitrogen-phosphorus detection for the measurement of tramadol and its O-desmethyl metabolite in plasma and brain tissue of mice and rats.

    PubMed

    Tao, Q; Stone, D J; Borenstein, M R; Jean-Bart, V; Codd, E E; Coogan, T P; Desai-Krieger, D; Liao, S; Raffa, R B

    2001-11-01

    A method that allows the measurement of plasma and brain levels of the centrally-acting analgesic tramadol and its major metabolite (O-desmethyl tramadol) in mice and rats was developed using gas chromatography equipped with nitrogen-phosphorus detection (GC-NPD). Plasma samples were extracted with methyl tert.-butyl ether (MTBE) and were injected directly into the GC system. Brain tissue homogenates were precipitated with methanol, the resulting supernatant was dried then acidified with hydrochloric acid. The aqueous solution was washed with MTBE twice, alkalinized, and extracted with MTBE. The MTBE layer was dried, reconstituted and injected into the GC system. The GC assay used a DB-1 capillary column with an oven temperature ramp (135 to 179 degrees C at 4 degrees C/min). Dextromethorphan was used as the internal standard. The calibration curves for tramadol and O-desmethyl tramadol in plasma and brain tissue were linear in the range of 10 to 10000 ng/ml (plasma) and ng/g (brain). Assay accuracy and precision of back calculated standards were within +/- 15%. PMID:11710575

  10. 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.

  11. Gas chromatographic determination of nitrogen oxide and dioxide using a photoionization detector

    SciTech Connect

    Bulycheva, Z.Yu.; Panina, L.I.; Rudenko, B.A.

    1995-01-01

    Recently, fundamentally new possibilities of detecting NO and NO{sub 2} have been connected with the use of a photoionization detector (PID), which is based on the ionization of analyzed components under vacuum UV radiation. The extensive experimental material on the employment of PID in the gas chromatographic analysis of different samples of organic and inorganic origin is given earlier. However there is no information about the practical use of PIDs for the analysis of NO and NO{sub 2}. The results obtained by using a PID for the gas-chromatographic analysis of a mixture of NO and NO{sub 2} are presented in this work. A specific Kuprumsorb sorbent based on a macroporous sulfonated cation-exchange resin in the Cu{sup 2+} form was used.

  12. Gas chromatographic characterization of vegetable oil deodorization distillate.

    PubMed

    Verleyen, T; Verhe, R; Garcia, L; Dewettinck, K; Huyghebaert, A; De Greyt, W

    2001-07-01

    Because of its complex nature, the analysis of deodorizer distillate is a challenging problem. Deodorizer distillate obtained from the deodorization process of vegetable oils consists of many components including free fatty acids, tocopherols, sterols, squalene and neutral oil. A gas chromatographic method for the analysis of deodorizer distillate without saponification of the sample is described. After a concise sample preparation including derivatization and silylation, distillate samples were injected on column at 60 degrees C followed by a gradual increase of the oven temperature towards 340 degrees C. The temperature profile of the oven was optimized in order to obtain a baseline separation of the different distillate components including free fatty acids, tocopherols, sterols, squalene and neutral oil. Good recoveries for delta-tocopherol, alpha-tocopherol, stigmasterol and cholesteryl palmitate of 97, 94.4, 95.6 and 92%, respectively were obtained. Repeatability of the described gas chromatographic method was evaluated by analyzing five replicates of a soybean distillate. Tocopherols and sterols had low relative standard deviations ranging between 1.67 and 2.25%. Squalene, mono- and diacylglycerides had higher relative standard deviations ranging between 3.33 and 4.12%. Several industrial deodorizer distillates obtained from chemical and physical refining of corn, canola, sunflower and soybean have been analyzed for their composition. PMID:11471811

  13. 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

  14. 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

  15. 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.

  16. Gas and liquid chromatographic analyses of nimodipine calcium antagonist in blood plasma and cerebrospinal fluid.

    PubMed

    Krol, G J; Noe, A J; Yeh, S C; Raemsch, K D

    1984-01-13

    Gas (GC) and liquid chromatographic (LC) assay procedures were developed for analysis of nimodipine (1,4-dihydropyridine calcium antagonist, BAY e 9736) in blood plasma at low nanogram concentration levels. To avoid decomposition during gas chromatography, nimodipine was oxidized to nimodipine pyridine (P) analogue before it was chromatographed on the OV-17 column and quantitated using an electron-capture detector. In contrast, the LC procedure involved chromatographic separation and quantitation of the underivatized nimodipine and of the endogenous P analogue using a 3-micron Spherisorb ODS column and UV detection. The same plasma extract and three alternative internal standards were used for both assays. Taking into consideration the fact that the GC assay result includes endogenous P analogue as well as nimodipine, good correlation between GC and LC assay data was obtained. Comparison of the results observed with the two procedures confirmed the accuracy of each procedure and provided an alternative when one of the assay results was subject to patient plasma constituent interference. The LC assay was also used for analysis of the demethylated metabolites of nimodipine. To detect sub-nanogram concentrations of nimodipine in cerebrospinal fluid a combined LC-GC procedure using an LC clean-up step and a GC quantitation step was also developed. The above GC and LC procedures were used to obtain preliminary pharmacokinetic data. PMID:6707134

  17. A bubble-based microfluidic gas sensor for gas chromatographs.

    PubMed

    Bulbul, Ashrafuzzaman; Kim, Hanseup

    2015-01-01

    We report a new proof-of-concept bubble-based gas sensor for a gas chromatography system, which utilizes the unique relationship between the diameters of the produced bubbles with the gas types and mixture ratios as a sensing element. The bubble-based gas sensor consists of gas and liquid channels as well as a nozzle to produce gas bubbles through a micro-structure. It utilizes custom-developed software and an optical camera to statistically analyze the diameters of the produced bubbles in flow. The fabricated gas sensor showed that five types of gases (CO2, He, H2, N2, and CH4) produced (1) unique volumes of 0.44, 0.74, 1.03, 1.28, and 1.42 nL (0%, 68%, 134%, 191%, and 223% higher than that of CO2) and (2) characteristic linear expansion coefficients (slope) of 1.38, 2.93, 3.45, 5.06, and 5.44 nL/(kPa (μL s(-1))(-1)). The gas sensor also demonstrated that (3) different gas mixture ratios of CO2 : N2 (100 : 0, 80 : 20, 50 : 50, 20 : 80 and 0 : 100) generated characteristic bubble diameters of 48.95, 77.99, 71.00, 78.53 and 99.50 μm, resulting in a linear coefficient of 10.26 μm (μL s(-1))(-1). It (4) successfully identified an injection (0.01 μL) of pentane (C5) into a continuous carrier gas stream of helium (He) by monitoring bubble diameters and creating a chromatogram and demonstrated (5) the output stability within only 5.60% variation in 67 tests over a month. PMID:25350655

  18. Gas chromatographic separation of methoxylated polychlorinated biphenyl atropisomers

    PubMed Central

    Kania-Korwel, Izabela; Vyas, Sandhya M.; Song, Yang; Lehmler, Hans-Joachim

    2008-01-01

    Several polychlorinated biphenyls (PCBs) and their hydroxylated metabolites display axial chirality. Here we describe an enantioselective, gas chromatographic separation of methylated derivatives of hydroxylated (OH-)PCB atropisomers (MeO-PCB) using a chemically bonded β-cyclodextrin column (Chirasil-Dex). The atropisomers of several MeO-PCBs could be separated on this column with resolutions ranging from 0.42–0.87 under isothermal or temperature-programmed conditions. In addition, the enantiomeric fraction of OH-PCB 136 metabolites was determined in male and female rats treated with racemic PCB 136. The methylated derivatives of two OH-PCB 136 metabolites showed an enantiomeric enrichment in liver tissue, whereas PCB 136 itself was near racemic. PMID:18760792

  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. Prediction of gas chromatographic retention data for hydrocarbons from naphthas

    SciTech Connect

    Woloszyn, T.F.; Jurs, P.C. )

    1993-03-01

    Regression equations that model the gas chromatographic retention behavior of hydrocarbons found in complex petrochemical mixtures were developed for two different stationary phases, SE-30 and Carbowax 20M. The models had relative standard errors in the range 1--2%. This quantitative structure-retention relationship (QSRR) study focused on a relatively heterogeneous data set and resulted in the generation of several statistical models that related Kovats' retention index with descriptors that encode molecular structure. Also investigated was the addition of boiling point as a physicochemical descriptor. These models bore a significant improvement over the models containing only structural descriptors, with R values of 0.996. 27 refs., 4 figs., 8 tabs.

  1. 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.

  2. 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.

  3. 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

  4. 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

  5. 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.

  6. 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.

  7. 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

  8. Capillary gas chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco*

    PubMed Central

    Liu, Hong-cheng; Li, Qi-wan; Tang, Li-bin

    2007-01-01

    Simple procedures for extraction and chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco are described. The determination was carried out by capillary gas chromatography (GC) with electron capture detection (ECD) and confirmed by GC-MS. The mean recoveries and relative standard deviation (RSD) were 93.2%~112.9% and 3.5%~6.7%, respectively at levels ranging from 0.01 to 0.1 mg/kg. The limit of determination was 0.001 mg/kg. Tobacco samples in routine check were successfully analyzed using the proposed method. PMID:17444603

  9. Application of gas chromatographic method in simultaneous measurements of helium, argon and neon concentration in groundwaters

    NASA Astrophysics Data System (ADS)

    Najman, J.; Bielewski, J.; Sliwka, I.

    2012-04-01

    Helium concentration in groundwater is a fine indicator in water dating in a range from a hundred to tens of thousands of years. Gas chromatography (GC) measurements of helium can be used as an alternative to mass spectrometry (MS) determinations of 4He for groundwater dating [1]. Argon and neon concentrations mainly serve for determining the temperature of recharge and the air excess which is needed to correct measured values of helium concentration [2] . A chromatographic measurement system of helium, argon and neon concentration in groundwater is presented [3]. Water samples are taken from groundwater with a precise procedure without contamination with air in a special stainless steel vessels of volume equal to 2900 cm3. Helium is extracted from water samples using the head-space method. After enrichment by cryotrap method helium is analyzed in the gas chromatograph equipped with the thermal conductivity detector (TCD) with detection limit of about 2.8 ng He. The helium limit of detection of presented method is 1,2·10-8 cm3STP/gH2O [4]. We are currently working on adapting the method of cryogenic enrichment of helium concentration for simultaneous measurements of the concentration of helium, argon and neon using single sample of groundwater. Neon will be measured with the thermal conductivity detector and capillary column filled with molecular sieve 5A. Argon will be analyzed also with the thermal conductivity detector and packed column filled with molecular sieve 5A. This work was supported by grant No. N N525 3488 38 from the polish National Science Centre. [1] A. Zuber, W. Ciężkowski, K. Różański (red.), Tracer methods in hydrogeological studies - a methodological guide. Wroclaw University of Technology Publishing House, Wroclaw, 2007 (in polish). [2] P. Mochalski, Chromatographic method for the determination of Ar, Ne and N2 in water, Ph.D. thesis, Institute of Nuclear Physics Polish Academy of Sciences in Krakow, 2003 (in polish). [3] A. Żurek, P

  10. Chromatographic detection and analysis of traces of hydrocarbons

    NASA Technical Reports Server (NTRS)

    Fickey, E. W.; Mullins, H. E.

    1969-01-01

    Special analytical column having in series two separate absorption sections charged with beads of porous polymer and a sample of gas detects traces of hydrocarbons. New method requires only 15 minutes for execution.

  11. Mars Solar Balloon Landed Gas Chromatograph Mass Spectrometer

    NASA Technical Reports Server (NTRS)

    Mahaffy, P.; Harpold, D.; Niemann, H.; Atreya, S.; Gorevan, S.; Israel, G.; Bertaux, J. L.; Jones, J.; Owen, T.; Raulin, F.

    1999-01-01

    A Mars surface lander Gas Chromatograph Mass Spectrometer (GCMS) is described to measure the chemical composition of abundant and trace volatile species and isotope ratios for noble gases and other elements. These measurements are relevant to the study of atmospheric evolution and past climatic conditions. A Micromission plan is under study where a surface package including a miniaturized GCMS would be delivered to the surface by a solar heated hot air balloon based system. The balloon system would be deployed about 8 km above the surface of Mars, wherein it would rapidly fill with Martian atmosphere and be heated quickly by the sun. The combined buoyancy and parachuting effects of the solar balloon result in a surface package impact of about 5 m/sec. After delivery of the package to the surface, the balloon would ascend to about 4 km altitude, with imaging and magnetometry data being taken for the remainder of the daylight hours as the balloon is blown with the Martian winds. Total atmospheric entry mass of this mission is estimated to be approximately 50 kg, and it can fit as an Ariane 5 piggyback payload. The GCMS would obtain samples directly from the atmosphere at the surface and also from gases evolved from solid phase material collected from well below the surface with a Sample Acquisition and Transport Mechanism (SATM). The experiment envisioned in the Mars Micromission described would obtain samples from a much greater depth of up to one meter below the surface, and would search for organic molecules trapped in ancient stratified layers well below the oxidized surface. Insitu instruments on upcoming NASA missions working in concert with remote sensing measurement techniques have the potential to provide a more detailed investigation of mineralogy and the extent of simple volatiles such as CO2 and H2O in surface and subsurface solid phase materials. Within the context of subsequent mission opportunities such as those provided by the Ariane 5 piggyback

  12. 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.

  13. Toward a Micro Gas Chromatograph/Mass Spectrometer (GC/MS) System

    NASA Astrophysics Data System (ADS)

    Wiberg, D. V.; Eyre, F. B.; Orient, O.; Chutjian, A.; Garkarian, V.

    2001-01-01

    Miniature mass filters (e.g., quadrupoles, ion traps) have been the subject of several miniaturization efforts. A project is currently in progress at JPL to develop a miniaturized Gas Chromatograph/Mass Spectrometer (GC/MS) system, incorporating and/or developing miniature system components including turbomolecular pumps, scroll type roughing pump, quadrupole mass filter, gas chromatograph, precision power supply and other electronic components. The preponderance of the system elements will be fabricated using microelectromechanical systems (MEMS) techniques. The quadrupole mass filter will be fabricated using an X-ray lithography technique producing high precision, 5x5 arrays of quadrupoles with pole lengths of about 3 mm and a total volume of 27 cubic mm. The miniature scroll pump will also be fabricated using X-ray lithography producing arrays of scroll stages about 3 mm in diameter. The target detection range for the mass spectrometer is 1 to 300 atomic mass units (AMU) with are solution of 0.5 AMU. This resolution will allow isotopic characterization for geochronology, atmospheric studies and other science efforts dependant on the understanding of isotope ratios of chemical species. This paper will discuss the design approach, the current state-of-the art regarding the system components and the progress toward development of key elements. The full system is anticipated to be small enough in mass, volume and power consumption to allow in situ chemical analysis on highly miniaturized science craft for geochronology, atmospheric characterization and detection of life experiments applicable to outer planet roadmap missions.

  14. 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.

  15. Absolutely Exponential Stability and Temperature Control for Gas Chromatograph System Under Dwell Time Switching Techniques.

    PubMed

    Sun, Xi-Ming; Wang, Xue-Fang; Tan, Ying; Wang, Xiao-Liang; Wang, Wei

    2016-06-01

    This paper provides a design strategy for temperature control of the gas chromatograph. Usually gas chromatograph is modeled by a simple first order system with a time-delay, and a proportion integration (PI) controller is widely used to regulate the output of the gas chromatograph to the desired temperature. As the characteristics of the gas chromatograph varies at the different temperature range, the single-model based PI controller cannot work well when output temperature varies from one range to another. Moreover, the presence of various disturbance will further deteriorate the performance. In order to improve the accuracy of the temperature control, multiple models are used at the different temperature ranges. With a PI controller designed for each model accordingly, a delay-dependent switching control scheme using the dwell time technique is proposed to ensure the absolute exponential stability of the closed loop. Experiment results demonstrate the effectiveness of the proposed switching technique. PMID:26316283

  16. GAS CHROMATOGRAPH-BASED SYSTEM FOR MEASURING THE METHANE FRACTION OF DIESEL ENGINE HYDROCARBON EMISSIONS

    EPA Science Inventory

    An instrument has been developed (termed the 'methane analytical system') enabling diesel methane emissions to be quatified separately from total unburned hydrocarbon emissions. The instrument employed gas chromatographic principles whereby a molecular sieve column operating isot...

  17. Miniaturized gas chromatograph-Paul ion trap system: applications to environmental monitoring

    NASA Technical Reports Server (NTRS)

    Shortt, B. J.; Darrach, M. R.; Holland, Paul M.; Chutjian, A.

    2004-01-01

    A miniature gas chromatograph (GC) and miniature Paul ion trap (PT) mass spectrometer system has been developed for identifying and quantifying chemical species present in closed environments having a complex mixture of gases.

  18. Simultaneous gas-chromatographic determination of four toxic gases generally present in combustion atmospheres. Final report

    SciTech Connect

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

    1994-09-01

    Measurement of combustion gases produced by burning aircraft cabin materials poses a continuing limitation for smoke toxicity research. Since toxic effects of gases depend on both their concentrations and duration of exposures, frequent atmosphere sampling is necessary to define the concentration-time curve. A gas chromatographic method was developed for the simultaneous analyses of carbon monoxide (CO), hydrogen sulfide (H2S), sulfur dioxide (SO2), and hydrogen cyanide (HCN). The method utilized an MTI M200 dual-column gas chromatograph (GC) equipped with 4-m molecular sieve-5A and 8-m PoraPlot-U capillary columns and two low-volume, high-sensitivity thermal conductivity detectors. Detectability (ppm)/retention times (seconds) for the gases were: CO (100/28); H2S (50/26); SO2 (125/76); HCN (60/108). 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 (CO and HCN) fabrics. 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.

  19. 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.

  20. NEW LIQUID CHROMATOGRAPHIC DETECTION SYSTEM FOR ENVIRONMENTAL POLLUTANTS

    EPA Science Inventory

    Resonance enhanced coherent anti-Stokes Raman spectrometry (CARS) has been demonstrated as a specific identification system for liquid chromatography for water pollution identification. To achieve this, liquid chromatographic preconcentration and separation and computer control o...

  1. 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. PMID:24211706

  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. Programmed automation of modulator cold jet flow for comprehensive two-dimensional gas chromatographic analysis of vacuum gas oils.

    PubMed

    Rathbun, Wayne

    2007-01-01

    A method is described for automating the regulation of cold jet flow of a comprehensive two-dimensional gas chromatograph (GCxGC) configured with flame ionization detection. This new capability enables the routine automated separation, identification, and quantitation of hydrocarbon types in petroleum fractions extending into the vacuum gas oil (VGO) range (IBP-540 degrees C). Chromatographic data acquisition software is programmed to precisely change the rate of flow from the cold jet of a nitrogen cooled loop modulator of a GCxGC instrument during sample analysis. This provides for the proper modulation of sample compounds across a wider boiling range. The boiling point distribution of the GCxGC separation is shown to be consistent with high temperature simulated distillation results indicating recovery of higher boiling semi-volatile VGO sample components. GCxGC configured with time-of-flight mass spectrometry is used to determine the molecular identity of individual sample components and boundaries of different molecular types. PMID:18078570

  4. Advances in Gas Chromatographic Methods for the Identification of Biomarkers in Cancer

    PubMed Central

    Kouremenos, Konstantinos A.; Johansson, Mikael; Marriott, Philip J.

    2012-01-01

    Screening complex biological specimens such as exhaled air, tissue, blood and urine to identify biomarkers in different forms of cancer has become increasingly popular over the last decade, mainly due to new instruments and improved bioinformatics. However, despite some progress, the identification of biomarkers has shown to be a difficult task with few new biomarkers (excluding recent genetic markers) being considered for introduction to clinical analysis. This review describes recent advances in gas chromatographic methods for the identification of biomarkers in the detection, diagnosis and treatment of cancer. It presents a general overview of cancer metabolism, the current biomarkers used for cancer diagnosis and treatment, a background to metabolic changes in tumors, an overview of current GC methods, and collectively presents the scope and outlook of GC methods in oncology. PMID:23074381

  5. [Gas chromatographic determination of formic acid in urine as carbon monoxide (author's transl)].

    PubMed

    Angerer, J

    1976-02-01

    A gas chromatographic method for determining formic acid in human urine is described. The analytical reliability of this method fullfills the criteria of statistical quality control. The rate of recovery is 101.2 to 105.7% the variability coefficients lie between 2.9 and 7.2%. The selectivity of this method is demonstrated by analysing a group of components normally occuring in urine which did not interfere with the determination of formic acid. The detection limit of about 4.3 mumol/1 formic acid in urine permits the determination of the concentration of formic acid in the urine of normal persons. The concentrations of formic acid in the urine of a group of normal persons lies between 0 and 2.79 mmol/1. The average concentration was 0.39 +/- 0.60 mmol/1. PMID:1249528

  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. PMID:8735201

  7. Evaluation of two commercial capillary columns for the enantioselective gas chromatographic separation of organophosphorus pesticides.

    PubMed

    Fidalgo-Used, Natalia; Blanco-González, Elisa; Sanz-Medel, Alfredo

    2006-12-15

    The separation of the enantiomers of 13 organophosphorus pesticides (OPPs) has been investigated by gas chromatography (GC) with flame ionisation detection (FID) using two different commercially available chiral columns, Chirasil-Val (l-valine-tert-butylamide) and CP-Chirasil-Dex CB (heptakis (2,3,6-tri-O-metil)-beta-cyclodextrin). Using the Chirasil-Val column no chiral resolution was obtained for the OPPs investigated under any tested experimental condition. The use of the CP-Chirasil-Dex CB stationary phase enabled good individual enantiomeric separation of two OPPs, ruelene and trichlorfon and partial separation of naled, chloretoxyphos, isophenphos and metamidophos. Also, the obtained chromatographic results showed that Chirasil-Dex could resolve enantiomers through the combination of different mechanism (e.g. formation of inclusion complexes and/or interactions outside the cyclodextrin cavity). Under optimised conditions, precision, linearity range and detection limits were evaluated for the enantiomers of ruelene and trichlorfon using CP-Chirasil-Dex CB column and electron capture detection (ECD). By using the GC-ECD method the enantiomers of these OPPs could be satisfactorily detected at very low concentration levels. The detection limits observed were 1.5ngmL(-1) and 11.5ngmL(-1) for the enantiomers of trichlorfon and ruelene, respectively. PMID:18970881

  8. Accelerated solvent extraction for gas chromatographic analysis of nicotine and cotinine in meconium samples.

    PubMed

    Sant'anna, Simone Gomes; Oliveira, Carolina Dizioli Rodrigues; Diniz, Edna Maria de Albuquerque; Yonamine, Mauricio

    2012-01-01

    Adverse effects associated with smoking during pregnancy are well documented. Although self-report surveys on drug consumption during pregnancy have been improved with new interviewing techniques, underreporting is still a concern. Therefore, a series of biological markers and specimens to diagnose fetal exposure to tobacco have been studied. In the present study, an analytical method was developed to detect nicotine and cotinine (the main nicotine metabolite) in meconium samples. Accelerated solvent extraction (ASE) followed by solid-phase extraction (SPE) were used as sample preparation techniques. The analytes were detected by gas-chromatography with nitrogen-phosphorus detection. The limits of detection were 3.0 and 30 ng/g for cotinine and nicotine, respectively. The method showed good linearity (r(2) > 0.98) in the concentration range studied (LOQ-500 ng/g). The intraday precision, given by the RSD of the method, was less than 15% for cotinine and nicotine. The method proved to be fast, practical, and sensitive. Smaller volumes of organic solvents are necessary compared to other chromatographic methods published in the scientific literature. This is the first report in which ASE was used as sample preparation technique in methods to detect xenobiotics in meconium. PMID:22290748

  9. 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.

  10. 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. PMID:21641604

  11. 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. PMID:19572555

  12. Oral intake of a toluene-containing thinner. Effects and headspace gas chromatographic analytical diagnosis.

    PubMed

    Zahlsen, K; Rygnestad, T; Nilsen, O G

    1985-01-01

    After an accidental oral intake of a paint thinner, the constituents were identified in stomach content using headspace gas chromatography. The composition indicated ingestion of a commonly used thinner containing 60-70% toluene, 20-25% n-butylacetate and 10-15% of ethanol. A toluene concentration of 22.0 mg/kg was measured in serum in contrast to n-butylacetate which was not detected. Ethanol concentration was 1.85 g/kg, most of this was due to ethanol ingestion before the intake of thinner. The half life of toluene in serum was 8.5 h initially, which increased to 14 h after 19 h. An effect on liver function was demonstrated by increased activity of serum transaminases. Compared with the upper normal limits ASAT and ALAT were increased by 6 and 2.5 times, respectively. For both parameters the highest activity was seen 40 hours after admission and normal levels were achieved after 7 days. It is concluded that toluene is readily absorbed by ingestion of toluene-containing thinners, and that the function of the human liver is transiently affected. For screening purposes gas chromatography proved to be a useful method for the analytical diagnosis in cases of organic solvent intoxication. The use of the headspace technique further improved the speed of analysis and eliminated contamination of the gas chromatographic system. PMID:3868371

  13. 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

  14. 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

  15. 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.

  16. Minimizing thermal degradation in gas chromatographic quantitation of pentaerythritol tetranitrate.

    PubMed

    Lubrano, Adam L; Field, Christopher R; Newsome, G Asher; Rogers, Duane A; Giordano, Braden C; Johnson, Kevin J

    2015-05-15

    An analytical method for establishing calibration curves for the quantitation of pentaerythriol tetranitrate (PETN) from sorbent-filled thermal desorption tubes by gas chromatography with electron capture detection (TDS-GC-ECD) was developed. As PETN has been demonstrated to thermally degrade under typical GC instrument conditions, peaks corresponding to both PETN degradants and molecular PETN are observed. The retention time corresponding to intact PETN was verified by high-resolution mass spectrometry with a flowing atmospheric pressure afterglow (FAPA) ionization source, which enabled soft ionization of intact PETN eluting the GC and subsequent accurate-mass identification. The GC separation parameters were transferred to a conventional GC-ECD instrument where analytical method-induced PETN degradation was further characterized and minimized. A method calibration curve was established by direct liquid deposition of PETN standard solutions onto the glass frit at the head of sorbent-filled thermal desorption tubes. Two local, linear relationships between detector response and PETN concentration were observed, with a total dynamic range of 0.25-25ng. PMID:25841610

  17. 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)

  18. [Molecular topology study of gas chromatographic retention indices of alkane series].

    PubMed

    Nie, Changming; Dai, Yimin; Wen, Songnian; Li, Zhonghai

    2005-01-01

    The gas chromatographic retention indices can be used to qualify some organic compounds. A new topological index based on distance matrix and branch vertex of the atoms in a molecule is proposed by defining equilibrium electronegativity of atoms in the molecule and coloring atoms in the molecular graph with equilibrium electronegativity, which appears unique to the molecular structures and has excellent structural selectivity. The multivariate linear equations of gas chromatographic retention indices are as follows: I(Squalane) = 23.97842N1 - 3.86562N2 + 0.787379N3 + 42.33061, R = 0.9922, n = 70, S = 13.70405, F = 1396.601; I(SE-30) = 23.83937N1 - 3.5687N2 + 0.939876N3 + 22.11952, R = 0.9919, n = 37, S = 11.96088, F = 668.8781; where the N1, N2 and N3 are a group of topological indices; n, R, S and F are sample number, regression coefficient, residual standard deviation and F-statistic value, respectively. The calculated results by the formulae indicate that the average relative deviations between calculated values and experimental data of gas chromatographic retention indices of alkane series on both squalane (column temperature 50 degrees C) and SE-30 (column temperature 80 degrees C) were all 1.31% and the errors were within experimental deviations. The equations can express well the change rule of the relative gas chromatographic retention indices of alkane series. PMID:15881357

  19. ON-LINE MEASUREMENT OF THE INFRARED SPECTRA OF GAS CHROMATOGRAPHIC ELUENTS

    EPA Science Inventory

    Techniques for increasing the sensitivity of the interface between a gas chromatograph and a rapid-scanning Fourier transform infrared spectrometer (GC-IR) have been developed. A single-beam system, in which a triglycine sulfate (TGS) detector is used to measure the interferogram...

  20. A Microporous Metal-Organic Framework for Gas Chromatographic Separation of Alkanes

    SciTech Connect

    Chen, Banglin; Liang, Chengdu; Yang, Jun; Contreras, Damacio; Clancy, Yvette; Lobkovsky, Emil B.; Yaghi, Omar; Dai, Sheng

    2006-01-01

    A zinc-based metal-organic framework (MOF) can be transformed reversibly from an open (a) to a dense (b) configuration. The microporous solid is the first example of a MOF that is highly selective in the gas-chromatographic separation of alkanes.

  1. 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...

  2. AN EVALUATION OF THE HEWLETT-PACKARD 5993B GAS CHROMATOGRAPH-MASS SPECTROMETER

    EPA Science Inventory

    This report gives the results of an evaluation of a Hewlett-Packard Model 5993B computerized gas chromatograph/mass spectrometer. The evaluation was done according to the procedures found in EPA research report number EPA-600/4-80-025, 'Performance Tests for the Evaluation of Com...

  3. 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...

  4. 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...

  5. 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...

  6. 1993 FIELD STUDY/DEMONSTRATION OF AUTOMATED GAS CHROMATOGRAPH IN CONNECTICUT AND OTHER LABORATORIES

    EPA Science Inventory

    The objectives of this study were to install, test and demonstrate two automated gas chromatographic (GC) systems to state and regional EPA groups. he two GC systems required no liquid cryogen for operational purposes. he Dynatherm/Hewlett Packard GC system was designed for the m...

  7. 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.

  8. Rapid and sensitive gas-chromatographic determination of caffeine in blood plasma, saliva, and xanthine beverages.

    PubMed

    Teeuwen, H W; Elbers, E L; van Rossum, J M

    1991-02-01

    A gas chromatographic procedure is reported for the determination of caffeine in plasma, saliva, and xanthine beverages. Using a 75 cm column packed with OV-17, nitrogen-sensitive detection, and 1 ml samples, a suitable limit of analysis (coefficient of variation (CV) = 10.2%) of 50 ng/ml was obtained in plasma. Within-day CVs at caffeine concentrations of 0.1-0.5-2.0-7.5-15.0 micrograms/ml in plasma were 7.7-5.6-4.8-3.8-3.4%, respectively. The limit of detection, defined as the injected quantity of caffeine giving rise to a signal to noise ratio of 2, is 40 pg, corresponding to a plasma concentration of 1 ng/ml. The procedure involves addition of the internal standard 7-pentyl theophylline and alkaline extraction of the sample with dichloromethane. The method described rivals any gaschromatographic assay published so far in rapidness and accuracy. Plasma and saliva caffeine concentrations were determined in a healthy male volunteer after swallowing 400 ml of coffee. The calculated pharmacokinetic parameters, assuming complete absorption of caffeine from the G.I. tract, agree well with previously published values. PMID:1875916

  9. 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.

  10. A gas chromatographic air analyzer fabricated on a silicon wafer

    NASA Technical Reports Server (NTRS)

    Terry, S. C.; Jerman, J. H.; Angell, J. B.

    1979-01-01

    A miniature gas analysis system has been built based on the principles of gas chromatography (GC). The major components are fabricated in silicon using photolithography and chemical etching techniques, which allows size reductions of nearly three orders of magnitude compared to conventional laboratory instruments. The chromatography system consists of a sample injection valve and a 1.5-m-long separating capillary column, which are fabricated on a substrate silicon wafer. The output thermal conductivity detector is separately batch fabricated and integrably mounted on the substrate wafer. The theory of gas chromatography has been used to optimize the performance of the sensor so that separations of gaseous hydrocarbon mixtures are performed in less than 10 s. The system is expected to find application in the areas of portable ambient air quality monitors, implanted biological experiments, and planetary probes.

  11. 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}.

  12. 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].

  13. 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.…

  14. Factorial-design optimization of gas chromatographic analysis of tetrabrominated to decabrominated diphenyl ethers. Application to domestic dust.

    PubMed

    Regueiro, Jorge; Llompart, Maria; Garcia-Jares, Carmen; Cela, Rafael

    2007-07-01

    Gas chromatographic analysis of polybrominated diphenyl ethers (PBDEs) has been evaluated in an attempt to achieve better control of the separation process, especially for highly substituted congeners. Use of a narrow-bore capillary column enabled adequate determination of tetra, penta, hexa, hepta, octa, nona and decaBDE congeners in only one chromatographic run while maintaining resolution power similar to that of conventional columns. A micro electron-capture detector (GC-microECD) was used. Chromatographic conditions were optimized by multifactorial experimental design, with the objective of obtaining not only high sensitivity but also good precision. In this way two different approaches to maximizing response and minimizing variability were tested, and are fully discussed. These optimum chromatographic conditions were then used to determine PBDEs extracted from domestic dust samples by microwave-assisted solvent extraction (MASE). Quantitative recovery (90-108%) was achieved for all the PBDEs and method precision (RSD < 13%) was satisfactory. Accuracy was tested by use of the standard reference material SRM 2585, and sub-ng g(-1) limits of detection were obtained for all compounds except BDE-209 (1.44 ng g(-1)). Finally, several samples of house dust were analysed by use of the proposed method and all the target PBDEs were detected in all the samples. BDE-209 was the predominant congener. Amounts varied from 58 to 1615 ng g(-1) and the average contribution to the total PBDE burden of 52%. The main congeners of the octaBDE mixture (BDE-183, BDE-197, BDE-207 and BDE-196) also made an important contribution (29%) to the total. These are the first data about the presence of these compounds in European house-dust samples. Finally, the sum of the main congeners in the pentaBDE commercial mixture (BDE-47, BDE-99, and BDE-100) contributed 14% to the total. Figure Polybrominated diphenyl ethers in House Dust. PMID:17541561

  15. 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. PMID:21347675

  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. Gas chromatographic determination of clopidol in chicken tissues.

    PubMed

    Ekström, L G; Kuivinen, J

    1984-01-01

    A method has been developed for the determination of clopidol residues in chicken tissues. After extraction and cleanup, clopidol is esterified in a 2-phase system to clopidol propionate, which is determined by gas chromatography. The 2-phase system includes, in addition to the clopidol dissolved in methanol, aqueous borax solution, hexane, propionic anhydride, and pyridine. Use of these reagents precludes the use of explosive or carcinogenic chemicals in the derivatization step, and the method is therefore suitable for routine laboratory analysis. Levels of 0.5 ppb clopidol in tissue can be determined. PMID:6501161

  18. Micro-machined planar field asymmetric ion mobility spectrometer as a gas chromatographic detector

    NASA Technical Reports Server (NTRS)

    Eiceman, G. A.; Nazarov, E. G.; Miller, R. A.; Krylov, E. V.; Zapata, A. M.

    2002-01-01

    A planar high field asymmetric waveform ion mobility spectrometer (PFAIMS) with a micro-machined drift tube was characterized as a detector for capillary gas chromatography. The performance of the PFAIMS was compared directly to that of a flame ionization detector (FID) for the separation of a ketone mixture from butanone to decanone. Effluent from the column was continuously sampled by the detector and mobility scans could be obtained throughout the chromatographic analysis providing chemical inforrmation in mobility scans orthogonal to retention time. Limits of detection were approximately I ng for measurement of positive ions and were comparable or slightly better than those for the FID. Direct comparison of calibration curves for the FAIMS and the FID was possible over four orders of magnitude with a semi-log plot. The concentration dependence of the PFAIMS mobility scans showed the dependence between ion intensity and ion clustering, evident in other mobility spectrometers and atmospheric pressure ionization technologies. Ions were identified using mass spectrometry as the protonated monomer and the proton bound dimer of the ketones. Residence time for column effluent in the PFAIMS was calculated as approximately 1 ms and a 36% increase in extra-column broadening versus the FID occurred with the PFAIMS.

  19. Computerized gas chromatographic-mass spectrometric analysis of polycyclic aromatic hydrocarbons in environmental samples.

    PubMed

    Lao, R C; Thomas, R S; Monkman, J L

    1975-10-29

    Substantial progress has been made in the last few years in the development of a rapid method for determining polycyclic aromatic hydrocarbons (PAH) in environmental samples. The three-step method consists of (i) a preliminary separation of PAH by solvent and/or column chromatography, (ii) identification by a combination of gas chromatography with quadrupole mass spectrometry and computer, and (iii) measurement by computerized gas chromatography using internal standards. Samples of industrial effluents, coke oven emissions, coal tar and airborne particulates have been investigated. The efficiencies of different gas chromatographic columns were evaluated during these investigations. PMID:1184696

  20. Inverse gas chromatography and other chromatographic techniques in the examination of engine oils.

    PubMed

    Fall, Jacek; Voelkel, Adam

    2002-09-01

    The emerging market of engine oils consists of a number of products from different viscosity and quality classes. Determination of the base oil used in manufacturing of the final product (engine oil) as well as estimation of mutual miscibility of oils and their solubility could be crucial problems. Inverse gas chromatography and other chromatographic techniques are presented as an interesting and fruitful extension of normalised standard analytical methods used in the oil industry. PMID:12385390

  1. 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.

  2. Gas chromatographic determination of residual solvents in lubricating oils and waxes

    SciTech Connect

    De Andrade Bruening, I.M.R.

    1983-10-01

    A direct gas-liquid chromatographic analysis of residual solvents is described, using tert-butylbenzene as an internal standard. The lube oils and waxes were prevented from contaminating the chromatographic column by injecting the samples directly into a precolumn containing a silicone stationary phase. The samples of lube oils and waxes were injected directly into the chromatographic column containing another stationary phase, 1,2,3-tris(2-cyanoethoxy)propane. (The waxy samples were dissolved in a light neutral oil). With proper operating conditions, analysis time was 7 min. The procedure has been applied in the control of a lube oil dewaxing plant; the chromatographic column showed no sign of deterioration after 1 h when the precolumn was removed. Known amounts of toluene and methylethyl ketone were added to the solvent-free lubricating oils and wax, and these mixtures were analyzed to evaluate the accuracy of the procedure. Precision and accuracy of these data are comparable to those of methods previously described. 1 figure, 1 table.

  3. Microfabricated silicon gas chromatographic micro-channels: fabrication and performance

    SciTech Connect

    Matzke, C.M.; Kottenstette, R.J.; Casalnuovo, S.A.; Frye-Mason, G.C.; Hudson, M.L.; Sasaki, D.Y.; Manginell, R.P.; Wong, C.C.

    1998-11-01

    Using both wet and plasma etching, we have fabricated micro-channels in silicon substrates suitable for use as gas chromatography (GC) columns. Micro-channel dimensions range from 10 to 80 {micro}m wide, 200 to 400 {micro}m deep, and 10 cm to 100 cm long. Micro-channels 100 cm long take up as little as 1 cm{sup 2} on the substrate when fabricated with a high aspect ratio silicon etch (HARSE) process. Channels are sealed by anodically bonding Pyrex lids to the Si substrates. We have studied micro-channel flow characteristics to establish model parameters for system optimization. We have also coated these micro-channels with stationary phases and demonstrated GC separations. We believe separation performance can be improved by increasing stationary phase coating uniformity through micro-channel surface treatment prior to stationary phase deposition. To this end, we have developed microfabrication techniques to etch through silicon wafers using the HARSE process. Etching completely through the Si substrate facilitates the treatment and characterization of the micro- channel sidewalls, which domminate the GC physico-chemical interaction. With this approach, we separately treat the Pyrex lid surfaces that form the top and bottom surfaces of the GC flow channel.

  4. Microfabricated silicon gas chromatographic microchannels: fabrication and performance

    NASA Astrophysics Data System (ADS)

    Matzke, Carolyn M.; Kottenstette, Richard J.; Casalnuovo, Stephen A.; Frye-Mason, Gregory C.; Hudson, Mary L.; Sasaki, Darryl Y.; Manginell, Ronald P.; Wong, C. Channy

    1998-08-01

    Using both wet and plasma etching, we have fabricated micro- channels in silicon substrates suitable for use as gas chromatography (GC) columns. Micro-channel dimensions range from 10 to 80 micrometer wide, 200 to 400 micrometer deep, and 10 cm to 100 cm long. Micro-channels 100 cm long take up as little as 1 cm2 on the substrate when fabricated with a high aspect ratio silicon etch (HARSE) process. Channels are sealed by anodically bonding Pyrex lids to the Si substrates. We have studied micro-channel flow characteristics to establish model parameters for system optimization. We have also coated these micro-channels with stationary phases and demonstrated GC separations. We believe separation performance can be improved by increasing stationary phase coating uniformity through micro-channel surface treatment prior to stationary phase deposition. To this end, we have developed microfabrication techniques to etch through silicon wafers using the HARSE process. Etching completely through the Si substrate facilitates the treatment and characterization of the micro-channel sidewalls, which dominate the GC physico- chemical interaction. With this approach, we separately treat the Pyrex lid surfaces that form the top and bottom surfaces of the GC flow channel.

  5. AUTOMATED CALIBRATION AND ANALYSIS OF VOCS WITH A CAPILLARY COLUMN GAS CHROMATOGRAPH EQUIPPED FOR REDUCED TEMPERATURE TRAPPING

    EPA Science Inventory

    Recently an automated system for monitoring volatile organics by reduced temperature (-150C) preconcentration and capillary column/gas chromatographic analysis has been assembled and evaluated. The automation has now been extended to include multipoint calibration using single st...

  6. Construction of a cryogen-free thermal desorption gas chromatographic system with off-the-shelf components for monitoring ambient volatile organic compounds.

    PubMed

    Ou-Yang, Chang-Feng; Liao, Wei-Cheng; Wang, Pei-Chieh; Fan, Gang-Jei; Hsiao, Chien-Cheng; Chuang, Ming-Tung; Chang, Chih-Chung; Lin, Neng-Huei; Wang, Jia-Lin

    2016-04-01

    An automated gas chromatographic system aimed at performing unattended measurements of ambient volatile organic compounds was configured and tested. By exploiting various off-the-shelf components, the thermal desorption unit was easily assembled and can be connected with any existing commercial gas chromatograph in the laboratory to minimize cost. The performance of the complete thermal desorption gas chromatographic system was assessed by analyzing a standard mixture containing 56 target nonmethane hydrocarbons from C2 -C12 at sub-ppb levels. Particular attention was given to the enrichment efficiency of the C2 compounds, such as ethane (b.p. = -88.6°C) and ethylene (b.p. = -104.2°C), due to their extremely high volatilities. Quality assurance was performed in terms of the linearity, precision and limits of detection of the target compounds. To further validate the system, field measurements of target compounds in ambient air were compared with those of a commercial total hydrocarbon analyzer and a carbon monoxide analyzer. Highly coherent results from the three instruments were observed during a two-month period of synchronized measurements. Moreover, the phenomenon of opposite diurnal variations between the biogenic isoprene and anthropogenic species was exploited to help support the field applicability of the thermal desorption gas chromatographic method. PMID:26924196

  7. 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.

  8. A rapid paper chromatographic method for detection of anionic detergent in milk.

    PubMed

    Barui, Amit K; Sharma, Rajan; Rajput, Yudhishthir S; Singh, Smita

    2013-08-01

    A paper chromatographic method for the detection of adulteration of anionic detergent in milk is described. The method is based on the complexing of anionic detergent with methylene blue dye and separation of complex from free dye using simple paper chromatographic method. Since complexing of detergent is with dye, visualization is direct without involvement of subsequent detection of complex. The method is simple and results are available in 10 min. The method is sensitive to detect 0.1 % (w/v) labolene (laboratory grade detergent) or 0.01 % (w/v) sodium dodecylbenzene sulfonate (pure anionic detergent) in milk. The method can be adopted at quality control laboratories in dairies for ascertaining the quality of milk. PMID:24425989

  9. Determination of calcium stearate in polyolefin samples by gas chromatographic technique after performing dispersive liquid-liquid microextraction.

    PubMed

    Ranji, Ali; Ghorbani Ravandi, Mahboobeh; Farajzadeh, Mir Ali

    2008-05-01

    In this study, a gas chromatographic method is presented for the determination of calcium stearate after its conversion to stearic acid in a polymeric matrix. A solution of hydrochloric acid in 2-propanol is used as an extracting solvent of calcium stearate and its converter to stearic acid. For stearic acid preconcentration before its injection to a separation system, a recently presented extraction method, dispersive liquid-liquid microextraction, using carbon tetrachloride as an extracting solvent is used. Finally, 1 microL of the organic phase collected at the bottom of a conical test tube after centrifuging is injected into a gas chromatograph (GC) for quantification. This method has a relatively broad linear dynamic range (50 - 2000 mg/L) with a limit of detection (LOD) of 15 mg/L for stearic acid in solution. The LOD of the proposed method in a polymeric sample using 10 mg of polymer is 60 ppm as calcium stearate. Some effective parameters, such as the time and temperature of heating, the concentration of hydrochloric acid and the volume of distilled water, were studied. PMID:18469468

  10. 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. PMID:26530144

  11. Gas chromatographic determination of trace amounts of vinyl chloride and dichloroethenes in landfill-gas.

    PubMed

    Wittsiepe, J; Selenka, F; Jackwerth, E

    1996-03-01

    A method for the determination of vinyl chloride (VC) and dichloroethenes (DCE) in gas samples is presented. The analytes are preconcentrated from a gas-volume of up to 20 l on an adsorption tube filled with 1.0 g of a carbon molecular sieve at a flow rate of 80 l/h and are subsequently desorbed with carbon disulfide. Vinyl bromide is added as internal standard to the extract. The analytes are determined as their 1,2-dibromo-derivatives by capillary gas chromatography with electron capture detection. The detection limits have been found to be 82 ng/m(3) = 32 ppt (VC), 190 ng/m(3) = 48 ppt (1,1-DCE) and 96 ng/m(3) = 24 ppt (cis-/trans-1,2-DCE). The method has been used for the quantification of the anaerobic microbial degradation of tetra- (PCE) and trichloroethene (TCE) to dichloroethenes and vinyl chloride in landfill sites. The substances have been analyzed in landfill-gas as well as in gaseous emissions from the landfill surface. The mean emission rates of tetrachloroethene, trichloroethene and vinyl chloride from the landfill surface into the ambient air are about 0.5 microg/(m(2) x h). PMID:15048415

  12. Balloonborne in situ gas chromatograph for measurements in the troposphere and stratosphere

    NASA Astrophysics Data System (ADS)

    Moore, F. L.; Elkins, J. W.; Ray, E. A.; Dutton, G. S.; Dunn, R. E.; Fahey, D. W.; McLaughlin, R. J.; Thompson, T. L.; Romashkin, P. A.; Hurst, D. F.; Wamsley, P. R.

    2003-03-01

    An in situ gas chromatograph (GC) instrument on a balloonborne package is described in detail and data from seven science deployments are presented. This instrument, the Lightweight Airborne Chromatograph Experiment (LACE), operates on the Observations of the Middle Stratosphere (OMS) in situ gondola and has taken data from the upper troposphere to near 32 km with a vertical resolution of better than 300 m. LACE chromatography has been developed to measure halon-1211, the chlorofluorocarbons (CFC-11, CFC-113, CFC-12), nitrous oxide (N2O), and sulfur hexafluoride (SF6) every 70 s and methyl chloroform (CH3CCl3), carbon tetrachloride (CCl4), hydrogen (H2), methane (CH4), and carbon monoxide (CO) every 140 s. In the introduction we present scientific motivation for choosing this suite of molecules and for the use of faster sample rates resulting in unprecedented vertical resolution from an in situ GC. Results from an intercomparison with the Airborne Chromatograph for Atmospheric Trace Species (ACATS-IV) instrument are shown to quantitatively connect this LACE data set to the complementary data set generated on board the NASA ER-2 aircraft.

  13. Position sensitive radioactivity detection for gas and liquid chromatography

    DOEpatents

    Cochran, Joseph L.; McCarthy, John F.; Palumbo, Anthony V.; Phelps, Tommy J.

    2001-01-01

    A method and apparatus are provided for the position sensitive detection of radioactivity in a fluid stream, particularly in the effluent fluid stream from a gas or liquid chromatographic instrument. The invention represents a significant advance in efficiency and cost reduction compared with current efforts.

  14. 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

  15. 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.

  16. Gas chromatographic organic acid profiling analysis of brandies and whiskeys for pattern recognition analysis.

    PubMed

    Park, Y J; Kim, K R; Kim, J H

    1999-06-01

    An efficient gas chromatographic profiling and pattern recognition method is described for brandy and whiskey samples according to their organic acid contents. It involves solid-phase extraction of organic acids using Chromosorb P with subsequent conversion to stable tert-butyldimethylsilyl derivatives for the direct analysis by capillary column gas chromatography and gas chromatography-mass spectrometry. A total of 12 organic acids were reproducibly identified in liquor samples (1 mL). When the GC profiles were simplified to their retention index spectra, characteristic patterns were obtained for each liquor sample as well as for each group average. Stepwise discriminant analysis provided star symbols characteristic for each liquor sample and group average. As expected, canonical discriminant analysis correctly classified 23 liquor samples studied into two groups of either brandy or whiskey. PMID:10794629

  17. A gas chromatographic instrument for measurement of hydrogen cyanide in the lower atmosphere

    NASA Astrophysics Data System (ADS)

    Ambrose, J. L.; Zhou, Y.; Haase, K.; Mayne, H. R.; Talbot, R.; Sive, B. C.

    2012-06-01

    A gas-chromatographic (GC) instrument was developed for measuring hydrogen cyanide (HCN) in the lower atmosphere. The main features of the instrument are (1) a cryogen-free cooler for sample dehumidification and enrichment, (2) a porous polymer PLOT column for analyte separation, (3) a flame thermionic detector (FTD) for sensitive and selective detection, and (4) a dynamic dilution system for calibration. We deployed the instrument for a ∼4 month period from January-June, 2010 at the AIRMAP atmospheric monitoring station Thompson Farm 2 (THF2) in rural Durham, NH. A subset of measurements made during 3-31 March is presented here with a detailed description of the instrument features and performance characteristics. The temporal resolution of the measurements was ~20 min, with a 75 s sample capture time. The 1σ measurement precision was <10% and the instrument response linearity was excellent on a calibration scale of 0.10-0.75 ppbv (±5%). The estimated method detection limit (MDL) and accuracy were 0.021 ppbv and 15%, respectively. From 3-31 March 2010, ambient HCN mixing ratios ranged from 0.15-1.0 ppbv (±15%), with a mean value of 0.36 ± 0.16 ppbv (1σ). The approximate mean background HCN mixing ratio of 0.20 ± 0.04 ppbv appeared to agree well with tropospheric column measurements reported previously. The GC-FTD HCN measurements were strongly correlated with acetonitrile (CH3CN) measured concurrently with a proton transfer-reaction mass spectrometer (PTR-MS), as anticipated given our understanding that the nitriles share a common primary biomass burning source to the global atmosphere. The nitriles were overall only weakly correlated with carbon monoxide (CO), which is reasonable considering the greater diversity of sources for CO. However, strong correlations with CO were observed on several nights under stable atmospheric conditions and suggest regional combustion-based sources for the nitriles. These results demonstrate that the GC-FTD instrument is

  18. Application of Gas Chromatographic analysis to RPC detectors in the ATLAS experiment at CERN-LHC

    NASA Astrophysics Data System (ADS)

    de Asmundis, R.

    2007-06-01

    Starting from 2007 a large number (1200) Resistive Plate Chambers (RPC) detectors will be used as muon trigger detectors in the ATLAS Experiment at CERN-LHC accelerator. RPC are gaseous detector in which the quality and the stability of the gas mixture as well as the design of the gas supplying system, play a fundamental role in their functioning. RPC are foreseen to work more than ten years in the high radiation environment of ATLAS and the gas mixture acts really as a "lifeguard" for the detectors. For this reason a great attention has been devoted to the gas studies in order to optimize RPC performance, robustness and reliability in a high radiation environment. In this paper we describe the work done to decide how to supply and control in an optimal way the gas to the detectors, in order to ensure their best performance for a long time. The activity, based on Gas Chromatographic (GC) analysis, has been carried on a sample of final RPC working in radiation conditions much more intense than those foreseen for the ATLAS experiment. This has been possible using a high Gamma ray radiation facility available at CERN (GIF). The gas has been supplied using a system similar but at a reduced scale with respect to the final one and including: a recirculation circuit, a humidification module and a three stages purification subsystem.

  19. 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. PMID:23084486

  20. 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...

  1. 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. PMID:4093481

  2. Comparison of a gas chromatographic and colorimetric method for the determination of plasma paracetamol.

    PubMed

    Chambers, R E; Jones, K

    1976-07-01

    Plasma paracetamol levels have generally been determined either by gas chromatography (Stewart and Willis, 1975), which relies on complex equipment, or by spectrophotometry (Knepil, 1974), which can be time-consuming. The introduction by Glynn and Kendal (1975) of a simple colorimetric method based on the reaction of paracetamol with nitrous acid to give 2-nitro-4-acetamidophenol appears to have overcome these disadvantages, thereby providing a suitable procedure for the rapid measurement of plasma paracetamol in cases of overdose. The method was reported to be specific for paracetamol, no interference being caused either by the sulphate and glucuronide conjugates of paracetamol or by a large number of other commonly found drugs. This communication presents the results of a study in which plasma paracetamol levels determined by the colorimetric method were compared with those determined by an established gas chromatographic technique. PMID:952476

  3. Gas chromatographic determination of sulfuric acid and application to urinary sulfate.

    PubMed

    Masuoka, N; Ubuka, T; Kinuta, M; Yoshida, S; Taguchi, T

    1988-10-01

    A new gas chromatographic method for the determination of sulfate was developed. In this method, sulfate was quantitatively converted to a volatile derivative, dimethyl sulfate, by a two-step procedure. First, sulfate was converted to silver sulfate by reaction with silver oxide, and then to dimethyl sulfate by reaction with methyl iodide. The derivative was analyzed by gas chromatography. Methyl methanesulfonate was used as an internal standard. The method was applied to the determination of total urinary sulfate. Phosphate and chloride ions, which interfered with the present method, were eliminated with the use of basic magnesium carbonate and an excess of silver oxide, respectively. Recovery was over 96% when 5 to 40 mumol/ml of sulfate was added to human urine samples. PMID:3223336

  4. Gas-Chromatographic analysis of Mars soil samples with the SAM instrument onboard Curiosity - the 359 first sols

    NASA Astrophysics Data System (ADS)

    Szopa, Cyril; Navarro-Gonzalez, Rafael; Mahaffy, Paul; Buch, Arnaud; Goutail, Jean Pierre; Cabane, Michel; Glavin, Daniel; Correia, Jean-Jacques; Coll, Patrice; Freissinet, Caroline; Meftah, Mustapha; Coscia, David; Teinturier, Samuel; Brunner, Anna; Bonnet, Jean-Yves; Millan, Maeva; Pascalin

    Amongst the SAM suite of instruments, SAM-GC (Gas Chromatograph) is devoted to identify and quantify volatiles evolved from the thermal/chemical treatment of any soil sample collected by the Curiosity rover. The first soil samples analyzed with SAM were composed of windblown dust and sand collected at the Rocknest site, while the second site analyzed was a basin called “Yellowknife Bay” where two holes were drilled (John Klein & Cumberland) and analysis showed these sites to be a fluvio-lacustrine sediment.. For their analysis, these samples were subjected to a pyrolysis at temperatures reaching about 850°C. For SAM-GC and GCMS analyses, different fractions of pyrolysates were collected at different temperature in the ambient-900°C range in order to discriminate potential different volatile fractions present in the solid sample. With the aim to search for potential organic molecules outgassed from the samples, a SAM-GC analytical channel composed of a thermal-desorption injector and a MXT-CLP chromatographic column was used as it was designed for the separation of a wide range of volatile organic molecules. This channel is also equipped with a thermal conductivity detector (TCD) capable to detect the most abundant species (with abundances down to approximately 10-10mol). His channel is thus complementary to the mass spectrometer detection for quantification of such species, as this last instrument does not have linear response in this domain of high abundance, whereas it is significantly more sensitive than the TCD. The results obtained with this instrument first show that the performances of SAM-GC is representative of those obtained during calibrations of the instrument in laboratory, and also that results are repeatable. Hence, the instrument performs nominally, making it the first GCMS running successfully on Mars since the Viking missions (middle of the 70’s). Moreover, the complementarity of GC towards MS is also shown, both by allowing the

  5. [Gas chromatographic method for the analysis of polychlorinated biphenyls in pine needles].

    PubMed

    Zhu, X; Zhang, X; Yao, J; Liu, Z; Lu, P

    1999-07-01

    Polychlorinated biphenyls (PCBs) are a class of 209 chemical compounds, in which 1-10 chlorine atoms are attached to a biphenyl molecule. PCBs are members of halogenated aromatic group of environmental pollutants that have been identified worldwide in diverse environmental matrices. PCBs in air, soils, sediment, water, transformer oils and other environmental matrices have been determined in the past years. In this work a method for routine analysis of PCBs in pine needles has been developed. First, extractions were carried out in Soxhlet apparatus with n-hexane as solvent. Then, a silica gel chromatographic column was applied to pretreat the pine needle samples. The reference standard used was clophen 50. The recovery was about 90%, so the feasibility and reliability were assured. After the analysis of PCBs in pine needle samples from four different regions, the distribution of PCBs in environment can be discussed and monitored. In this method, a Shimadzu GC-7A gas chromatograph equipped with a 63Ni electron capture detector was used for the analysis of PCBs. From the results, we can see the PCB pollution in different regions. So evaluation of air pollution level through foliage data is feasible. The sample preparation and analytical method mentioned in this paper is reliable and simple. PMID:12552848

  6. A gas chromatograph/mass spectrometry method for determining isotopic distributions in organic compounds used in the chemical approach to stable isotope separation

    SciTech Connect

    Martinez, A.M.; Spall, W.D.; Smith, B.F.

    1990-01-01

    A variety of gas chromatograph/mass spectrometry (GC/MS) methods have been developed to resolve benzene, benzophenone, anthracene, fluorenone, and their respective stable isotope analogs from other components by gas chromatography. The ratio of stable isotope-labeled material to natural isotopic abundance compounds is determined from the mass spectra averaged across the chromatographic peak. Both total ion and selective ion chromatographic approaches were used for relative data and comparison. 9 refs., 11 tabs.

  7. Capillary gas chromatographic determination of putrescine and cadaverine in serum of cancer patients using trifluoroacetylacetone as derivatizing reagent.

    PubMed

    Khuhawar, M Y; Memon, A A; Jaipal, P D; Bhanger, M I

    1999-02-19

    Trifluoroacetylacetone (FAA) derivatives of 1,4-diaminobutane (putrescine) (Pu) and 1,5-diaminopentane (cadaverine) (CA) were prepared and characterized by elemental microanalysis, IR, and mass spectrometry. Diamine derivatives were eluted from capillary gas chromatographic (CGC) column BP1 (12 m x 0.22 mm I.D.) or BP5 (50 m x 0.22 mm) with layer thickness 0.25 microm, using nitrogen as a carrier gas and flame ionization detection (FID). A solvent extraction procedure was developed for the extraction of Pu and CA from aqueous solution with a linear calibration range 0-20 microg/0.2 ml of extract with a detection limit of 0.5-0.6 ng/injection. The method was applied for the determination of Pu and CA in the serum of five cancer patients before and after radiotherapy. The serum of two healthy persons was also analyzed for Pu and CA contents. Pu and CA concentrations were found within the range 1.16-3.96 microg/ml and 0.88-1.46 microg/ml in cancer patients as compared to 0.11-0.16 microg/ml and 0.06-0.075 microg/ml respectively in healthy persons with a coefficient of variation (CV) within 0.62-5.47%. Pu and CA concentrations decreased on radiotherapy in cancer patients, but were much higher than in healthy persons. PMID:10080628

  8. Selectivity and sensitivity of some thin-layer chromatographic detection systems.

    PubMed

    Fodor-Csorba, K; Dutka, F

    1986-09-19

    The selectivity and sensitivity of some thin-layer chromatographic detection systems widely used internationally and developed in our laboratory were studied. Halogenated organophosphorus pesticides were found to interfere with the detection of organochlorine pesticides when using silver nitrate-2-phenoxyethanol. The stability of colours formed by the 4-(4'-nitrobenzyl)pyridine-tetraethylenepentamine system was enhanced by spraying with acetic acid and allowed densitometric evaluation. The most sensitive detection method for thiocarbamates is the reaction with 2,6-dichlorobenzoquinone-N-chloroimine or its dibromo analogue (50 ng). Application of this method for sulphur-containing organophosphorus insecticides results in the same or better sensitivity. Quantitation of these compounds was carried out by densitometry. PMID:3771705

  9. 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. PMID:27211679

  10. Gas chromatographic-mass spectrometric analysis and subsequent quality improvement of plastic infusion packaging materials.

    PubMed

    Fekete, Z; Rófusz, T; Angyal, V; Szabó-Révész, P; Aigner, Z

    2014-08-01

    Although the opalescence of sterile transparent plastic materials utilized for the packaging of parenteral infusion drugs is a serious quality problem, most suppliers do not report the exact compositions of such polymers, and no literature data are available. Similarly, no information is available as concerns the potential incompatibility of the inner bag and the overpouch. Our gas chromatographic-mass spectrometric study revealed that the cause of the opalescence is the presence of a low-molecular-weight slip additive, 13-docosenamide (erucamide), which is transferred into the primary infusion bag from the overpouch during the heat-sterilization process. Autoclaving trials confirmed the analytical results. In view of these findings, a new slip additive-free overpouch has been produced as secondary packaging material, which does not give rise to opalescence. PMID:24863371

  11. Rapid gas-liquid chromatographic method for determination of sulfathiazole in swine feed.

    PubMed

    Munns, R K; Roybal, J E

    1983-03-01

    A gas-liquid chromatographic (GLC) method for determining residues of sulfathiazole (STZ) in swine feed has been developed. Feed is extracted first with acetone and then with ammonia-acetone. STZ is isolated from other feed extractives on a Sephadex LH-20 column with methanol-toluene. The sulfa residues are methylated with diazomethane, and the eluate is evaporated to dryness. A solution containing an internal standard of methyl sulfasymazine is used to dilute the sample before injection onto an OV-25 GLC column. The precision of the method was determined by assaying 10 sets of feed spiked at 0.5, 1, 2, and 5 ppm STZ. The mean recoveries and coefficients of variation were 90.2 (5.90), 89.5 (4.67), 87.4 (5.62), and 87.7% (4.29), respectively. The critical steps of the method, including the stability of STZ, were also determined. PMID:6853414

  12. Rapid gas-liquid chromatographic method for determination of sulfamethazine in swine feed.

    PubMed

    Munns, R K; Roybal, J E

    1982-09-01

    A gas-liquid chromatographic method is described for the quantitative determination of trace amounts of sulfamethazine in swine feed. Sulfamethazine is extracted in ammoniated acetone and isolated from other extractants on a Sephadex LH-20 column. The eluate is methylated with diazomethane and evaporated to dryness. The residue is dissolved in a solvent containing an internal standard of methyl sulfasymazine before being injected onto an OV-25 GLC column. An estimation of precision was established by assaying 10 sets of swine feed fortified with 0.5, 1,2, and 5 ppm SMZ. Mean recoveries were 96.0, 94.3, 93.5, and 94.0%, respectively, with an average coefficient of variation of 3.07%. The critical steps and ruggedness of the method were also determined. PMID:7130074

  13. Recent development in chromatographic techniques

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Chromatographic techniques play a significant role in the determination of analytes in complex matrices, separating individual sample components prior to their detection. In the analysis of contaminants and chemical residues in foods, gas chromatography (GC) and liquid chromatography (LC) are two m...

  14. A preliminary report on the derivatization-gas chromatographic determination of nalidixic acid and 3,7-dicarboxynalidixic acid in urine.

    PubMed

    Wu, S M; Chen, S H; Wu, H L

    1989-11-01

    A preliminary study on the gas chromatographic analysis of urine spiked with nalidixic acid and 3,7-dicarboxynalidixic acid is described. The method is based on the transfer of an ion-pair of NA or CNA with tetradecyldimethylbenzylammonium chloride (benzalkonium chloride) from alkaline aqueous solution into methyl isobutyl ketone (MIBK), the organic phase, where these salts are derivatized with pentafluorobenzyl bromide. The derivatives formed by this process are chromatographed on an analytical column packed with 1.5% OV-101 and detected with a flame-ionization detector. Several parameters affecting the transfer and/or derivatization of NA or CNA were investigated. These parameters include the phase transfer catalyst employed, the organic solvent used, the concentration of the acid and base added, the amount of derivatizing agent required, and reaction time and temperature. PMID:2634117

  15. Development of a gas chromatographic test for the quantitation of the biomarker 2-butoxyacetic acid in urine samples.

    PubMed

    B'Hymer, C

    2007-08-01

    An accurate and precise method is developed and evaluated for the detection and quantitation of 2-butoxyacetic acid (2-BAA), a metabolite and biomarker for human exposure to 2-butoxyethanol. The solvent 2-butoxyethanol (2-BE) is extensively used in various industrial and domestic applications, and it is a health concern owing to its toxicity. Sample preparation consists of liquid-liquid extraction (LLE) of urine, then esterification of 2-BAA to produce the ethyl ester analog. The gas chromatographic conditions utilize a dimethyl polysiloxane phase (HP-1) capillary column and a mass spectrometer (MS) for detection of the analyte. Validation of this method includes a recovery study using fortified urine samples, which demonstrated good accuracy and precision; recovery varied between 100% and 102% of theory, with relative standard deviations of replicate samples at 2.8% and less. The detection limit of this method ranges from 0.005 to 0.015 microg/mL equivalent level of 2-BAA in urine. PMID:17725869

  16. GAS CHROMATOGRAPHIC DETERMINATION OF AVIATION GASOLINE AND JP-4 JET FUEL IN SUBSURFACE CORE SAMPLES (JOURNAL VERSION)

    EPA Science Inventory

    A new gas chromatographic procedure for quantifying levels of aviation gasoline (avgas) and JP-4 jet fuel contamination in soils is described. The fuel is extracted from a small quantity of soil or subsurface material, typically about 6 g, using 3 mL of methylene chloride. The ex...

  17. EVALUATION OF THE BASIC GC/MS (GAS CHROMATOGRAPHIC/MASS SPECTROMETRIC) COMPUTER ANALYSIS TECHNIQUE FOR POLLUTANT ANALYSIS

    EPA Science Inventory

    The basic gas chromatographic/mass spectrometric/computer technique for the analysis of vapor-phase organic compounds collected on a solid sorbent was evaluated. Emphasis was placed on the assessment of performance and improvement in techniques in the following areas: (1) wide-bo...

  18. EVALUATION OF PHOTOVAC 10S50 PORTABLE PHOTOIONIZATION GAS CHROMATOGRAPH FOR ANALYSIS OF TOXIC ORGANIC POLLUTANTS IN AMBIENT AIR

    EPA Science Inventory

    The objective of the study was to evaluate the Photovac 10S50 portable photoionization gas chromatograph as a monitor for fourteen selected toxic organic vapors in ambient air. These included benzene, toluene, bromo- and chloro-benzene, o-xylene, and nine halo-methanes, ethanes, ...

  19. Inlet backflushing device for the improvement of comprehensive two dimensional gas chromatographic separations.

    PubMed

    Edwards, Matthew; Górecki, Tadeusz

    2015-07-10

    Comprehensive two-dimensional gas chromatography (GC×GC) is recognised as a powerful tool for the separation of complex mixtures of volatile and semi-volatile compounds. In the analysis of challenging samples containing highly concentrated, active analytes or those with complicated matrices, it is often the case that less than ideal chromatography is produced. GC×GC chromatograms of such samples typically contain broad, tailing analyte bands. This results in difficulties with quantitation and poor utilisation of the separation space. In this study we investigated the inlet and the modulator as the potential sources of these tailing bands. A simple inlet backflushing device was developed to isolate the inlet from the primary column after the injection, and a similar setup was used to isolate the modulator from the primary column. The device allowed us to divert carrier gas flow back through the inlet at a specified time after the injection, while allowing analytes to pass through the column for separation. Analytes retained within the inlet were prevented from entering the column, and were subsequently removed via the carrier gas split line. The study revealed that the inlet plays a significant role in the development of tailing chromatographic bands, while the modulator simply modulates the already elongated band. Inlet backflushing is a cheap, simple and effective tool that can be used to improve the chromatography of problematic GC×GC analyses of samples consisting of concentrated and active analytes, those derived from natural products and containing complicated matrices. PMID:26028511

  20. 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.

  1. COMPONENT LOSS DURING EVAPORATION-RECONSTITUTION OF ORGANIC ENVIRONMENTAL SAMPLES FOR GAS CHROMATOGRAPHIC ANALYSIS

    EPA Science Inventory

    Standard and sample solutions stored in borosilicate sample vials were allowed to evaporate to dryness at room temperature. The solutions were analyzed by gas chromatography-flame ionization detection before evaporation and after reconstitution to the original volume to determine...

  2. Gas-chromatographic analysis of Mars soil samples at Rocknest site with the SAM instrument onboard Curiosity

    NASA Astrophysics Data System (ADS)

    Cabane, Michel; Coll, Patrice; Szopa, Cyril; Coscia, David; Buch, Aranaud; Teinturier, Samuel; Navarro-gonzalez, Rafael; Gaboriaud, Alain; Mahaffy, Paul; MSL science Team

    2013-04-01

    Amongst the SAM suite of instruments [1], SAM-GC (Gas Chromatograph) is devoted to identify and quantify volatiles evolved from the thermal/chemical treatment of any soil sample collected by the Curiosity rover. The first soil samples analyzed with SAM were composed of sand collected at the Rocknest site. For their analysis, these samples were submitted to a pyrolysis at temperatures reaching about 900°C. For SAM-GC and GCMS analyses, different fractions of pyrolysates were collected at different temperature in the ambient-900°C range in order to discriminate potential different volatile fractions present in the solid sample. With the aim to search for potential organic molecules outgassed from the samples, a SAM-GC analytical channel composed of thermal-desorption injector and a MXT-CLP chromatographic column was used as it was designed for the separation of a wide range of volatile organic molecules. This channel is also equipped with a thermal conductivity detector (TCD) capable to detect the most abundant species (with abundances down to approximately 10-10 mol). It is thus complementary to the mass spectrometer detection for quantification of such species as this last instrument has not a linear response in this domain of high abundance, whereas it is significantly more sensitive than the TCD. The results obtained with this instrument for the analysis of Rocknest soil first show that the performances of SAM-GC are representative of those obtained during calibrations of the instrument in laboratory, as well as they are repeatable. Hence, the instrument performs nominally, making it the first GCMS running successfully on Mars since the Viking missions. Moreover, the complementarity of GC towards MS is also shown, either by allowing the quantification of the major species detected (as water), or by providing a chromatographic signal well resolved temporally which can be used to improve the QMS signal treatment. In the frame of research of organics, the SAM

  3. Gas chromatographic determination of the interconversion energy barrier for dialkyl 2,3-pentadienedioate enantiomers.

    PubMed

    Mydlová, J; Krupcík, J; Májek, P; Skacáni, I; Jakubík, T; Sandra, P; Armstrong, D W

    2007-05-25

    The enantiomers of dialkyl 2,3-pentadienedioate undergo interconversion during gas chromatographic separation on chiral stationary phases. In this paper the on-column apparent interconversion kinetic and thermodynamic activation data were determined for dimethyl, diethyl, propylbutyl and dibutyl 2,3-pentadienedioate enantiomers by gas chromatographic separation of the racemic mixtures on a capillary column containing a polydimethylsiloxane stationary phase coupled to 2,3-di-O-methyl-6-O-tertbutyldimethylsilyl-beta-cyclodextrin. A deconvolution method was used to determine the individual enantiomer peak areas and retention times that are needed to calculate the interconversion rate constants and the energy barriers. The apparent rate constants and interconversion energy barriers decrease slightly with an increase in the alkyl chain length of the dialkyl 2,3-pentadienedioate esters. The optimum conformation of the dialkyl 2,3-pentadienedioate molecules, their separation selectivity factors and apparent interconversion enthalpy and entropy data changes with the alkyl chain length. The dependence of the apparent interconversion energy barrier (deltaG(app)(a-->b), deltaG(app)(b-->a)) on temperature was used to determine the apparent activation enthalpy (deltaH(app)(a-->b), deltaH(app)(b-->a)) and apparent entropy (deltaS(app)(a-->b), deltaS(app)(a-->b)) (where a denotes the first and b second eluted enantiomer). The comparison of the activation enthalpy and entropy (deltaS(app)(a-->b), deltaS(app)(a-->b)) indicated that the interconversion of dialkyl 2,3-pentadienedioate enantiomers on the HP-5+Chiraldex B-DM column series is an entropy driven process at 160 degrees C. Data obtained for dimethyl 2,3-pentadienedioate enantiomers on the HP-5+Chiraldex B-DM column series at 120 degrees C (deltaG(app)(a-->b) = 123.3 and deltaG(app)(b-->a) = 124.4 kJ mol(-1)) corresponds (at the 95% confidence interval) with the value of deltaG(#) = 128+/-1 kJ mol(-1) found at this

  4. 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

  5. Airborne gas chromatograph for in situ measurements of long-lived species in the upper troposphere and lower stratosphere

    NASA Astrophysics Data System (ADS)

    Elkins, J. W.; Fahey, D. W.; Gilligan, J. M.; Dutton, G. S.; Baring, T. J.; Volk, C. M.; Dunn, R. E.; Myers, R. C.; Montzka, S. A.; Wamsley, P. R.; Hayden, A. H.; Butler, J. H.; Thompson, T. M.; Swanson, T. H.; Dlugokencky, E. J.; Novelli, P. C.; Hurst, D. F.; Lobert, J. M.; Ciciora, S. J.; McLaughlin, R. J.; Thompson, T. L.; Winkler, R. H.; Fraser, P. J.; Steele, L. P.; Lucarelli, M. P.

    A new instrument, the Airborne Chromatograph for Atmospheric Trace Species IV (ACATS-IV), for measuring long-lived species in the upper troposphere and lower stratosphere is described. Using an advanced approach to gas chromatography and electron capture detection, the instrument can detect low levels of CFC-11 (CCl3F), CFC-12 (CCl2F2), CFC-113 (CCl2F-CClF2), methyl chloroform (CH3CCl3), carbon tetrachloride (CCl4), nitrous oxide (N2O), sulfur hexafluoride (SF6), Halon-1211 (CBrClF2), hydrogen (H2), and methane (CH4) acquired in ambient samples every 180 or 360 s. The instrument operates fully-automated onboard the NASA ER-2 high-altitude aircraft on flights lasting up to 8 hours or more in duration. Recent measurements include 24 successful flights covering a broad latitude range (70°S-61°N) during the Airborne Southern Hemisphere Ozone Experiment/Measurements for Assessing the Effects of Stratospheric Aircraft (ASHOE/MAESA) campaign in 1994.

  6. Determination of thymol in human plasma by automated headspace solid-phase microextraction-gas chromatographic analysis.

    PubMed

    Kohlert, Claudia; Abel, Gudrun; Schmid, Eleonora; Veit, Markus

    2002-02-01

    A reliable and sensitive method was developed for determination of thymol in human plasma by automated headspace solid-phase microextraction (SPME). After enzymatic cleavage of thymol sulfate thymol was extracted by a 65 microm polydimethylsiloxane-divinylbenzene crimped fiber (Supelco) after addition of sodium chloride and phosphoric acid (85%). Desorption of the fiber was performed in the injection port of a gas chromatograph at 220 degrees C (HP 5890; 50 m x 0.2 mm I.D., 0.2 microm HP Innowax capillary column; flame ionization detection). Fibers were used repeatedly up to 40 analysis. The recovery was 5% after 35 min of extraction. The calibration curve was linear in the range of 8.1-203.5 ng ml(-1) with a limit of quantitation (LOQ) of 8.1 ng ml(-1). The within-day and between-day precision and accuracy were < or = 20% at the LOQ and <15% at higher concentrations according to international guidelines for validation of bioanalytical methods. After administration of a thymol-containing herbal extract only thymol sulfate, no free thymol, could be detected in human plasma, thus analysis of thymol was after enzymatic cleavage of thymol sulfate. It is concluded that the newly developed automated method can be used in clinical trials on bioavailability and pharmacokinetics of thymol-containing herbal medicinal products. PMID:11863281

  7. A general static-headspace gas chromatographic method for determination of residual benzene in oral liquid pharmaceutical products.

    PubMed

    Liu, Hui; Tang, Qinglin; Markovich, Robert J; Rustum, Abu M

    2011-01-25

    Sodium benzoate is used in oral liquid pharmaceutical products for its anti-microbial properties. The benzoate salts present in liquid pharmaceutical products can potentially generate residual levels of free benzene during manufacturing of the drug product and or during the shelf-life of the product under its storage conditions. To ensure the safety and quality of the pharmaceutical products (containing benzoate in the formulation), a selective and sensitive analytical method is required to monitor residual benzene in oral liquid pharmaceutical products. In this paper, we report the development and validation of a general static-headspace gas chromatographic (SH-GC) method to determine residual benzene in oral liquid pharmaceutical products. The liquid pharmaceutical drug product sample is dissolved in dimethylsulfoxide (DMSO) in a GC headspace vial. A DB-624 capillary column (30 m x 0.32 mm I.D. and 1.8 μm film thickness) was used under isothermal conditions with a flame ionization detection (FID). The benzene peak was well separated from all other volatile compounds that are present in the formulation of a number of liquid drug products. This method was successfully validated using a representative oral liquid pharmaceutical drug product. The limit of detection of the method for benzene is 0.5 ppm which met the 2 ppm limit of current ICH guideline for residual benzene in pharmaceutical products. PMID:20926217

  8. Gas chromatograph-based system for measuring the methane fraction of diesel-engine hydrocarbon emissions

    SciTech Connect

    Hoffman, J.S.; Geyer, S.M.; Lestz, S.S.; Black, F.M.

    1987-03-01

    An instrument has been developed (termed the methane analytical system) enabling diesel methane emissions to be quatified separately from total unburned hydrocarbon emissions. The instrument employed gas-chromatographic principles whereby a molecular-sieve column operating isothermally separated methane from the nonmethane hydrocarbons. Direct on-line sampling occurred via constant-volume sample loops. The effluent was monitored with a flame ionization detector. The instrument was fully calibrated (i.e., extremely linear response over a large concentration range) for use with diesel engines as part of an on-going alternative-fuels research program. Methane emissions from a light-duty, multi-cylinder, indirect-injected diesel engine fumigated with natural gas were measured on-line using the methane analytical system. Methane emissions were found to range from as low as 250 ppm to a high of nearly 2%. The nonmethane hydrocarbon emissions were determined by subtracting the methane level from the total unburned hydrocarbon level. In the event that the federal engine certification procedures are changed to be based on nonmethane hydrocarbon emissions, a methane analytical system such as the one described here would have great utility.

  9. 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.

  10. Evaluation of an automatic gas chromatographic system for the identification of bacterial infective agents

    PubMed Central

    Arcelloni, C.; Griffini, A.; Paroni, R.; Bonini, P. A.

    1989-01-01

    The potential clinical application of gas chromatography to microbial identifcation was evaluated. A completely automated system, the MIS (Microbial Identification System; Hewlett- Packard) can analyse and identify pure strains by comparison of their cellular fatty acids patterns (C9-C20) with the reference parameters stored in a library. Three hundred and sixty-seven strains were tested, comparing the gas chromatographic results with those obtained by the traditional microbiological methods in the bacteriology laboratory of our Institute. A standardized extractive procedure was followed to obtain the fatty acid methyl esters (FAMEs), but some modifications to the recommended procedure were introduced in the bacterial growth procedures: colonies harvested not only from the recommended growth media but also from selective media routinely used in the bacteriology laboratory were successfully examined. These modifications did not influence the results but improved the ease for the user; good agreement with the comparison method was observed as far as identifications of genus and species are concerned for 238 cases. The major advantages of this computerized system are a reduction in the time required to obtain the final results, the elimination of human errors by using the autosampler and a better inter-laboratory comparability of results owing to a higher degree of objectivity. On the other hand, the limited throughput of MIS (only 40 samples in 24 h) prevents its use in a large routine laboratory; this technology is appropriate in emergency cases, in taxonomic studies and as a confirmatory method. PMID:18924676

  11. Detection of gas leakage

    DOEpatents

    Thornberg, Steven M; Brown, Jason

    2015-02-17

    A method of detecting leaks and measuring volumes as well as a device, the Power-free Pump Module (PPM), provides a self-contained leak test and volume measurement apparatus that requires no external sources of electrical power during leak testing or volume measurement. The PPM is a portable, pneumatically-controlled instrument capable of generating a vacuum, calibrating volumes, and performing quantitative leak tests on a closed test system or device, all without the use of alternating current (AC) power. Capabilities include the ability is to provide a modest vacuum (less than 10 Torr) using a venturi pump, perform a pressure rise leak test, measure the gas's absolute pressure, and perform volume measurements. All operations are performed through a simple rotary control valve which controls pneumatically-operated manifold valves.

  12. Detection of gas leakage

    DOEpatents

    Thornberg, Steven; Brown, Jason

    2012-06-19

    A method of detecting leaks and measuring volumes as well as an apparatus, the Power-free Pump Module (PPM), that is a self-contained leak test and volume measurement apparatus that requires no external sources of electrical power during leak testing or volume measurement, where the invention is a portable, pneumatically-controlled instrument capable of generating a vacuum, calibrating volumes, and performing quantitative leak tests on a closed test system or device, all without the use of alternating current (AC) power. Capabilities include the ability is to provide a modest vacuum (less than 10 Torr), perform a pressure rise leak test, measure the gas's absolute pressure, and perform volume measurements. All operations are performed through a simple rotary control valve which controls pneumatically-operated manifold valves.

  13. Gas-Chromatographic analysis of Mars soil samples with the SAM instrument onboard Curiosity - the 180 first sols

    NASA Astrophysics Data System (ADS)

    Szopa, C.; Cabane, M.; Coll, P.; Coscia, D.; Buch, A.; Teinturier, S.; Navarro-Gonzalez, R.; Goutail, J.-P.; Montaron, C.; Rigal, J.-B.; Poinsignon, P.; Guerrini, V.; Clerc, M.-S.; Meftah, M.; Soldani, L.; Mettetal, F.; Jerôme, M.; Philippon, C.; Galic, A.; Sablairolles, J.; Triqueneaux, S.; Chazot, D.; Toffolo, B.; Rakoto, F. Y.; Gaboriaud, A.; Mahaffy, P.

    2013-09-01

    Amongst the SAM suite of instruments [1], SAM-GC (Gas Chromatograph) is devoted to identify and quantify volatiles evolved from the thermal/chemical treatment of any soil sample collected by the Curiosity rover. The first soil samples analyzed with SAM were composed of sand collected at the Rocknest site, when the second site analyzed was a basin called "Yellowkive Bay". For their analysis, these samples were submitted to a pyrolysis at temperatures reaching about 900°C. For SAM-GC and GCMS analyses, different fractions of pyrolysates were collected at different temperature in the ambient-900°C range in order to discriminate potential different volatile fractions present in the solid sample. With the aim to search for potential organic molecules outgassed from the samples, a SAM-GC analytical channel composed of thermal-desorption injector and a MXT-CLP chromatographic column was used as it was designed for the separation of a wide range of volatile organic molecules. This channel is also equipped with a thermal conductivity detector (TCD) capable to detect the most abundant species (with abundances down to approximately 10-10 mol). It is thus complementary to the mass spectrometer detection for quantification of such species as this last instrument has not a linear response in this domain of high abundance, whereas it is significantly more sensitive than the TCD. The results obtained with this instrument first show that the performances of SAM-GC are representative of those obtained during calibrations of the instrument in laboratory, as well as they are repeatable. Hence, the instrument performs nominally, making it the first GCMS running successfully on Mars since the Viking missions. Moreover, the complementarity of GC towards MS is also shown, either by allowing the quantification ofthe major species detected (as water), or by providing a chromatographic signal well resolved temporally which can be used to improve the QMS signal treatment. In the frame of

  14. Liquid chromatographic analysis of glucosamine in commercial dietary supplements using indirect fluorescence detection.

    PubMed

    Shen, Xiaoxuan; Yang, Min; Tomellini, Sterling A

    2007-02-01

    A method of using indirect fluorescence detection is evaluated for the analysis of glucosamine in commercial dietary supplements following chromatographic separation. In this method, the eluting analyte, glucosamine, was detected by monitoring an increase in the fluorescence signal for L-tryptophan (L-Trp) or DL-5-methoxytryptophan (5-MTP) after glucosamine complexed with a copper(II) ion and released either L-Trp or 5-MTP from a copper(II) complex, which is introduced postcolumn. The fluorescence of L-Trp and 5-MTP are quenched when complexed with the copper(II) ion. The results obtained using indirect fluorescence detection are compared with the results obtained for precolumn derivatization with phenylisothiocyanate. Statistical analysis is performed to compare the results obtained for the two postcolumn interaction components, Cu(L-Trp)2 and Cu(5-MTP)2, as well as the results obtained using the indirect fluorescence detection method and a precolumn derivatization method. The indirect fluorescence detection method provided an alternative to precolumn derivatization for determining the concentration of glucosamine in commercial dietary supplements. The stability of the glucosamine-o-phthalaldehyde-3-mercaptopropionic acid derivative is also evaluated to investigate the applicability of the popular precolumn derivatization reagent, o-phthalaldehyde-3-mercaptopropionic acid, for this analysis. PMID:17425135

  15. Rayleigh light scattering detection of three α1-adrenoceptor antagonists coupled with high performance liquid chromatograph

    NASA Astrophysics Data System (ADS)

    Li, Ai Ping; Peng, Huanjun; Peng, Jing Dong; Zhou, Ming Qiong; Zhang, Jing

    2015-08-01

    Herein, a Rayleigh light-scattering (RLS) detection method combined with high performance liquid chromatograph (HPLC) without any post-column probe was developed for the separation and determination of three α1-adrenoceptor antagonists. The quantitative analysis is benefiting from RLS signal enhancement upon addition of methanol which induced molecular aggregation to form an hydrophobic interface between aggregates and water that produce a sort of superficial enhanced scattering effect. A good chromatographic separation among the compounds was achieved using a Gemini 5u C18 reversed phase column (250 mm × 4.6 mm; 4 μm) with a mobile phase consisting of methanol and ammonium acetate-formic acid buffer solution (25 mM; pH = 3.0) at the flow rate of 0.7 mL min-1. The RLS signal was monitored at λex = λem = 354 nm. A limit of detection (LOD) of 0.065-0.70 μg L-1 was reached and a linear range was found between peak height and concentration in the range of 0.75-15 μg L-1 for doxazosin mesylate (DOX), 0.075-3.0 μg L-1 for prazosin hydrochloride (PRH), and 0.25-5 μg L-1 for terazosin hydrochloride (TEH), with linear regression coefficients all above 0.999. Recoveries from spiked urine samples were 88.4-99.0% which is within acceptable limits. The proposed method is convenient, reliable and sensitive which has been used successfully in human urine samples.

  16. 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.

  17. Technical Note: Precise quantitative measurements of total dissolved inorganic carbon from small amounts of seawater using a gas chromatographic system

    NASA Astrophysics Data System (ADS)

    Hansen, T.; Gardeler, B.; Matthiessen, B.

    2013-10-01

    Total dissolved inorganic carbon (CT) is one of the most frequently measured parameters used to calculate the partial pressure of carbon dioxide in seawater. Its determination has become increasingly important because of the rising interest in the biological effects of ocean acidification. Coulometric and infrared detection methods are currently favored in order to precisely quantify CT. These methods however are not sufficiently validated for CT measurements of biological experiments manipulating seawater carbonate chemistry with an extended CT measurement range (~1250-2400 μmol kg-1) compared to natural open ocean seawater (~1950-2200 μmol kg-1). The requirement of total sample amounts between 0.1-1 L seawater in the coulometric- and infrared detection methods potentially exclude their use for experiments working with much smaller volumes. Additionally, precise CT analytics become difficult with high amounts of biomass (e.g., phytoplankton cultures) or even impossible in the presence of planktonic calcifiers without sample pre-filtration. Filtration however, can alter CT concentration through gas exchange induced by high pressure. Addressing these problems, we present precise quantification of CT using a small, basic and inexpensive gas chromatograph as a CT analyzer. Our technique is able to provide a repeatability of ±3.1 μmol kg-1, given by the pooled standard deviation over a CT range typically applied in acidification experiments. 200 μL of sample is required to perform the actual CT measurement. The total sample amount needed is 12 mL. Moreover, we show that sample filtration is applicable with only minor alteration of the CT. The method is simple, reliable and with low cumulative material costs. Hence, it is potentially attractive for all researchers experimentally manipulating the seawater carbonate system.

  18. Validation of a QuEChERS-based gas chromatographic method for analysis of pesticide residues in Cassia angustifolia (senna).

    PubMed

    Tripathy, Vandana; Saha, Ajoy; Patel, Dilipkumar J; Basak, B B; Shah, Paresh G; Kumar, Jitendra

    2016-08-01

    A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy-precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01-1.0 μg mL(-1) for OCs and OPs and 0.05-2.5 μg mL(-1) for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70-120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg(-1), and the LOQs were determined as 0.01-0.049 mg kg(-1). The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India. PMID:27153296

  19. Development of a harmonised method for the profiling of amphetamines: III. Development of the gas chromatographic method.

    PubMed

    Andersson, Kjell; Jalava, Kaisa; Lock, Eric; Finnon, Yvonne; Huizer, Henk; Kaa, Elisabet; Lopes, Alvaro; Poortman-van der Meer, Anneke; Cole, Michael D; Dahlén, Johan; Sippola, Erkki

    2007-06-14

    This study focused on gas chromatographic analysis of target compounds found in illicit amphetamine synthesised by the Leuckart reaction, reductive amination of benzyl methyl ketone, and the nitrostyrene route. The analytical method was investigated and optimised with respect to introduction of amphetamine samples into the gas chromatograph and separation and detection of the target substances. Sample introduction using split and splitless injection was tested at different injector temperatures, and their ability to transfer the target compounds to the GC column was evaluated using cold on column injection as a reference. Taking the results from both techniques into consideration a temperature of 250 degrees C was considered to be the best compromise. The most efficient separation was achieved with a DB-35MS capillary column (35% diphenyl 65% dimethyl silicone; 30 m x 0.25 mm, d(f) 0.25 microm) and an oven temperature program that started at 90 degrees C (1 min) and was increased by 8 degrees C/min to 300 degrees C (10 min). Reproducibility, repeatability, linearity, and limits of determination for the flame ionisation detector (FID), nitrogen phosphorous detector (NPD), and mass spectrometry (MS) in scan mode and selected ion monitoring (SIM) mode were evaluated. In addition, selectivity was studied applying FID and MS in both scan and SIM mode. It was found that reproducibility, repeatability, and limits of determination were similar for FID, NPD, and MS in scan mode. Moreover, the linearity was better when applying FID or NPD whereas the selectivity was better when utilising the MS. Finally, the introduction of target compounds to the GC column when applying injection volumes of 0.2 microl, 1 microl, 2 microl, and 4 microl with splitless injection respectively 1 microl with split injection (split ratio, 1:40) were compared. It was demonstrated that splitless injections of 1 microl, 2 microl, and 4 microl could be employed in the developed method, while split

  20. 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.

  1. 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. PMID:24939086

  2. 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.

  3. Gas-chromatographic determination of 1,3-butadiene trimers in the atmosphere

    SciTech Connect

    Drugov, Yu.S.; Murav`eva, G.V.; Shlyakhov, A.F.

    1992-02-10

    In the catalytic polymerization of 1,3-butadiene during the manufacture of SKD-1 rubber (with titanium and aluminum compounds as catalysts) the toxic oligomers (1,3-butadiene trimers) t,t,t-1, 5,9-cyclododecatriene (I), t,t,c-1, 5,9-cyclododecatriene (II), n-2,4,6,10-dodecatetraene (III), n-1,3,6,10-dodecatertraine (IV), and others end up in the atmosphere and the manufacture of cyclododecane. In the content of the oligomers in the air used for drying the rubber was determined by passing it through active carbon and desorbing the trapped substances with water vapor. However, aspects of the concentration of the microimpurities during their determination in the atmosphere were not considered. The aim of the present work was to develop a gas-chromatographic procedure for the determination of small amounts of compounds in the atmosphere. The tentative safe level amounts to 0.008 mg/m{sup 3} for (I) and 0.01 mg/m{sup 3} for (II, III). In air these oligomers are present in the form of vapor and aerosols. 7 refs., 3 figs., 4 tabs.

  4. 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. PMID:23780497

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

    PubMed

    Zheng, Yunzhong; Qi, Meiling; Fu, Ruonong

    2016-07-01

    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. PMID:27266332

  6. Toward automated chromatographic fingerprinting: A non-alignment approach to gas chromatography mass spectrometry data.

    PubMed

    Vestner, Jochen; de Revel, Gilles; Krieger-Weber, Sibylle; Rauhut, Doris; du Toit, Maret; de Villiers, André

    2016-03-10

    In contrast to targeted analysis of volatile compounds, non-targeted approaches take information of known and unknown compounds into account, are inherently more comprehensive and give a more holistic representation of the sample composition. Although several non-targeted approaches have been developed, there's still a demand for automated data processing tools, especially for complex multi-way data such as chromatographic data obtained from multichannel detectors. This work was therefore aimed at developing a data processing procedure for gas chromatography mass spectrometry (GC-MS) data obtained from non-targeted analysis of volatile compounds. The developed approach uses basic matrix manipulation of segmented GC-MS chromatograms and PARAFAC multi-way modelling. The approach takes retention time shifts and peak shape deformations between samples into account and can be done with the freely available N-way toolbox for MATLAB. A demonstration of the new fingerprinting approach is presented using an artificial GC-MS data set and an experimental full-scan GC-MS data set obtained for a set of experimental wines. PMID:26893085

  7. Microwave-assisted phase-transfer catalysis for the rapid one-pot methylation and gas chromatographic determination of phenolics.

    PubMed

    Fiamegos, Yiannis C; Karatapanis, Andreas; Stalikas, Constantine D

    2010-01-29

    Microwave-assisted phase-transfer catalysis (PTC) is reported for the first time, for the one-step extraction-derivatization-preconcentration and gas chromatographic determination of twenty phenols and ten phenolic acids. The well established phase-transfer catalytic methylation is largely accelerated when heating is replaced with the "greener" microwave irradiation. The overall procedure was thoroughly optimized and the analytes were determined by GC/MS. The method presented adequate analytical characteristics being more sensitive in analyzing phenols than phenolic acids. The limits of detection without any additional preconcentration steps (e.g. solvent evaporation) were adequate and ranged from 0.4 to 15.8ng/mL while limits of quantitation were between 1.2 and 33.3ng/mL. The method was applied to the determination of phenols, in spiked environmental samples and phenolic acids in aqueous infusions of commercially available pharmaceutical dry plants. The recoveries of fortified composite lake water samples and Mentha spicata aqueous infusions ranged from 89.3% to 117.3% for phenols and 93.3% to 115.2% for phenolic acids. PMID:20022019

  8. Gas Flow Detection System

    NASA Technical Reports Server (NTRS)

    Moss, Thomas; Ihlefeld, Curtis; Slack, Barry

    2010-01-01

    This system provides a portable means to detect gas flow through a thin-walled tube without breaking into the tubing system. The flow detection system was specifically designed to detect flow through two parallel branches of a manifold with only one inlet and outlet, and is a means for verifying a space shuttle program requirement that saves time and reduces the risk of flight hardware damage compared to the current means of requirement verification. The prototype Purge Vent and Drain Window Cavity Conditioning System (PVD WCCS) Flow Detection System consists of a heater and a temperature-sensing thermistor attached to a piece of Velcro to be attached to each branch of a WCCS manifold for the duration of the requirement verification test. The heaters and thermistors are connected to a shielded cable and then to an electronics enclosure, which contains the power supplies, relays, and circuit board to provide power, signal conditioning, and control. The electronics enclosure is then connected to a commercial data acquisition box to provide analog to digital conversion as well as digital control. This data acquisition box is then connected to a commercial laptop running a custom application created using National Instruments LabVIEW. The operation of the PVD WCCS Flow Detection System consists of first attaching a heater/thermistor assembly to each of the two branches of one manifold while there is no flow through the manifold. Next, the software application running on the laptop is used to turn on the heaters and to monitor the manifold branch temperatures. When the system has reached thermal equilibrium, the software application s graphical user interface (GUI) will indicate that the branch temperatures are stable. The operator can then physically open the flow control valve to initiate the test flow of gaseous nitrogen (GN2) through the manifold. Next, the software user interface will be monitored for stable temperature indications when the system is again at

  9. 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

  10. Gas chromatographic techniques for the analysis of hydrocarbons in low-rank coal liquefaction products. Part II. Instrumental aspects

    SciTech Connect

    Raynie, D.E.; Farnum, S.A.; Potts, Y.R.

    1984-01-01

    Two long Continuous Processing Unit (CPU) runs were carried out to: (1) study the effect of two different start-up solvents on the composition of the recycle product; and (2) thoroughly characterize any change caused by the start-up solvent during the recycle process. Capillary gas chromatography has been chosen as the major analytical tool in these line-out studies of coal liquefaction products. Initial separations of distillate oils from CPU passes were carried out by the silical gel chromatographic method previously reported. The resulting hydrocarbon fractions were combined into four groups for gas chromatographic analysis. The four groups were chromatographed against the appropriate calibration mixture. Some components of the distillate oil were identified but not quantified due to insufficient amounts of some standards. Over 300 samples also necessitated the use of up to 30 components in a calibration standard. Resulting chromatograms showed near-ideal peak shapes. Peak areas were integrated, ratioed to the internal standard and compared to the appropriate calibration curve. Components were identified by comparing retention times and were confirmed by gas chromatography/mass spectroscopy. Parameters such as threshold, peak width, and baseline construction mode were adjusted for optimum sensitivity. For valid comparisons to be made conditions were carefully reproduced. Although chromatography is not often thought of as an exact science, chromatographic systems can be optimized for a given analytical situation. In this case, we have successfully used capillary gas chromatography for the automated identification and quantification of up to 30 species in a single coal liquefaction fraction. We have quantified 87 compounds in the distillate oil. This method may also serve as the basis for analysis of other complex samples.

  11. Ion-chromatographic determination of carbocisteine in pharmaceuticals based on non-suppressed conductimetric detection.

    PubMed

    Megoulas, Nikolaos C; Koupparis, Michael A

    2004-02-13

    A novel method for the determination of carbocisteine (S-CMC), a mucolytic and expectorant drug with an acidic amino acid structure, was developed and validated, using non-suppressed ion-chromatographic system with conductimetric detection, and anion or cation exchange columns. Among the various combinations of column type and eluent composition tested, a cation exchange column with a 0.25 mM tri-fluoroacetic acid (TFA) as eluent in isocratic mode at 1.2 ml/min gave the best results. S-CMC was very well separated from all common amino acids (resolution > 2.6). The retention time was 3.5 min and the asymmetry factor 1.1. A linear calibration curve from 17 to 400 microg/ml (r = 0.99994), with a detection limit of 0.14 microg (5.6 microg/ml-25 microl injection volume) and a precision of 1.5% R.S.D. (100 microg/ml, n = 3) was achieved. The proposed method was applied for the determination of S-CMC content in intensely colored commercial formulations (syrups). No interference from excipients was found and the only pretreatment step was the appropriate dilution with the mobile phase. Recovery from standard additions was ranged from 96.0 to 104.9% and precision (R.S.D., n = 3) 1.8-3.6%. PMID:14763743

  12. LIQUID AND GAS CHROMATOGRAPHIC ANALYSIS OF DIETHYL PHTHALATE IN WATER AND SEDIMENT

    EPA Science Inventory

    Diethyl phthalate was determined in water and sediment by high performance liquid chromatography (HPLC) and in water by gas-liquid chromatography with electron capture detection (GLC-ECD). Water samples were extracted with hexane, using a high-speed homogenizer-ultrasonic apparat...

  13. A new method for total OH reactivity measurements using a fast Gas Chromatographic Photo-Ionization Detector (GC-PID)

    NASA Astrophysics Data System (ADS)

    Nölscher, A. C.; Sinha, V.; Bockisch, S.; Klüpfel, T.; Williams, J.

    2012-05-01

    The primary and most important oxidant in the atmosphere is the hydroxyl radical (OH). Currently OH sinks, particularly gas phase reactions, are poorly constrained. One way to characterize the overall sink of OH is to measure directly the ambient loss rate of OH, the total OH reactivity. To date direct measurements of total OH reactivity have been either performed using a Laser Induced Fluorescence (LIF) system ("pump-and-probe" or "flow reactor") or the Comparative Reactivity Method (CRM) with a Proton Transfer Reaction Mass Spectrometer (PTR-MS). Both techniques require large, complex and expensive detection systems. This study presents a feasibility assessment for CRM total OH reactivity measurements using a new detector, a Gas Chromatographic Photo-Ionization Detector (GC-PID). Such a system is smaller, more portable, less power consuming and less expensive than other total OH reactivity measurement techniques. Total OH reactivity is measured by the CRM using a competitive reaction between a reagent (here pyrrole) with OH alone and in the presence of atmospheric reactive molecules. The new CRM method for total OH reactivity has been tested with parallel measurements of the GC-PID and the previously validated PTR-MS as detector for the reagent pyrrole during laboratory experiments, plant chamber and boreal field studies. Excellent agreement of both detectors was found when the GC-PID was operated under optimum conditions. Time resolution (60-70 s), sensitivity (LOD 3-6 s-1) and overall uncertainty (25% in optimum conditions) for total OH reactivity were equivalent to PTR-MS based total OH reactivity measurements. One drawback of the GC-PID system was the steady loss of sensitivity and accuracy during intensive measurements lasting several weeks, and a possible toluene interference. Generally, the GC-PID system has been shown to produce closely comparable results to the PTR-MS and thus in suitable environments (e.g. forests) it presents a viably economical

  14. Total OH reactivity measurements using a new fast Gas Chromatographic Photo-Ionization Detector (GC-PID)

    NASA Astrophysics Data System (ADS)

    Nölscher, A. C.; Sinha, V.; Bockisch, S.; Klüpfel, T.; Williams, J.

    2012-12-01

    The primary and most important oxidant in the atmosphere is the hydroxyl radical (OH). Currently OH sinks, particularly gas phase reactions, are poorly constrained. One way to characterize the overall sink of OH is to measure directly the ambient loss rate of OH, the total OH reactivity. To date, direct measurements of total OH reactivity have been either performed using a Laser-Induced Fluorescence (LIF) system ("pump-and-probe" or "flow reactor") or the Comparative Reactivity Method (CRM) with a Proton-Transfer-Reaction Mass Spectrometer (PTR-MS). Both techniques require large, complex and expensive detection systems. This study presents a feasibility assessment for CRM total OH reactivity measurements using a new detector, a Gas Chromatographic Photoionization Detector (GC-PID). Such a system is smaller, more portable, less power consuming and less expensive than other total OH reactivity measurement techniques. Total OH reactivity is measured by the CRM using a competitive reaction between a reagent (here pyrrole) with OH alone and in the presence of atmospheric reactive molecules. The new CRM method for total OH reactivity has been tested with parallel measurements of the GC-PID and the previously validated PTR-MS as detector for the reagent pyrrole during laboratory experiments, plant chamber and boreal field studies. Excellent agreement of both detectors was found when the GC-PID was operated under optimum conditions. Time resolution (60-70 s), sensitivity (LOD 3-6 s-1) and overall uncertainty (25% in optimum conditions) for total OH reactivity were similar to PTR-MS based total OH reactivity measurements. One drawback of the GC-PID system was the steady loss of sensitivity and accuracy during intensive measurements lasting several weeks, and a possible toluene interference. Generally, the GC-PID system has been shown to produce closely comparable results to the PTR-MS and thus in suitable environments (e.g. forests) it presents a viably economical

  15. Matrix solid phase dispersion (MSPD) extraction and gas chromatographic screening of nine chlorinated pesticides in beef fat.

    PubMed

    Long, A R; Soliman, M M; Barker, S A

    1991-01-01

    A multiresidue technique is presented for the extraction and quantitative gas chromatographic screening of 9 insecticides (lindane, heptachlor, aldrin, heptachlor epoxide, p,p'-DDE, dieldrin, endrin, p,p'-TDE, and p,p'-DDT) as residues in beef fat. Beef fat was fortified by adding the 9 insecticides, plus dibutyl chlorendate as internal standard, to 0.5 g portions of beef fat and blending with 2 g C18 (octadecylsilyl)-derivatized silica. The C18/fat matrix blend was fashioned into a column by adding the blend to a 10 mL syringe barrel containing 2 g activated Florisil. The insecticides were then eluted from the column with 8 mL acetonitrile, and a 2 microL portion of the acetonitrile eluate was then directly analyzed by gas chromatography with electron capture detection. Unfortified blank controls were treated similarly. The acetonitrile eluate contained all of the pesticide analytes (31.25-500 ng/g) and was free of interfering co-extractants. Correlation coefficients for the 9 extracted pesticide standard curves (linear regression analysis, n = 5) ranged from 0.9969 (+/- 0.0021) to 0.9999 (+/- 0.0001). Average relative percentage recoveries (85 +/- 3.4% to 102 +/- 5.0%, n = 25 for each insecticide), inter-assay variability (6.0 +/- 1.0% to 14.0 +/- 6.7%, n = 25 for each insecticide), and intra-assay variability (2.5-5.1% n = 5 for each insecticide) indicated that the methodology is acceptable for the extraction, determination, and screening of these residues in beef fat. PMID:1874694

  16. Rapid gas chromatographic method for the determination of famoxadone, trifloxystrobin and fenhexamid residues in tomato, grape and wine samples.

    PubMed

    Likas, D T; Tsiropoulos, N G; Miliadis, G E

    2007-05-25

    Trifloxystrobin, fenhexamid and famoxadone belong to the generation of fungicides acting against a broad spectrum of fungi and widely used in Integrated Pest Management strategies in different agricultural crops but mainly in viticulture. In the present work, a gas chromatographic (GC) method for their determination was developed and validated on tomato, grape and wine matrices. The method was based on a simple one step liquid-liquid microextraction with cyclohexane/dichloromethane (9+1, v/v) and determination of fungicides by gas chromatography with nitrogen phosphorous (NP-) and electron capture (EC-) detection, and ion trap mass spectrometry (ITMS) for confirmation. The method was validated by recovery experiments, assessment of matrix effect and calculation of the associated uncertainty. Recoveries for GC-NPD and GC-ECD were found in the range of 81-102% with RSD <12%, while matrix-matched calibration solutions were imposed for quantification. LOQs ranged from 0.005 to 0.05 mg/kg and 0.01 to 0.10 mg/kg for the GC-ECD and GC-NPD, respectively, depending on the sensitivity of each compound with trifloxystrobin being the most sensitive. The expanded uncertainty, calculated for a sample concentration of 0.10 mg/kg, ranged from 4.8 to 13% for the GC-ECD and from 5.4 to 29% for the GC-NPD. The concentration levels for famoxadone residues found in tomato and grape samples from field experiments were clearly below the EU established MRL values, thus causing no problems in terms of food safety. PMID:16950327

  17. 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.

  18. Fission gas detection system

    DOEpatents

    Colburn, Richard P.

    1985-01-01

    A device for collecting fission gas released by a failed fuel rod which device uses a filter to pass coolant but which filter blocks fission gas bubbles which cannot pass through the filter due to the surface tension of the bubble.

  19. Statistical modelling of measurement errors in gas chromatographic analyses of blood alcohol content.

    PubMed

    Moroni, Rossana; Blomstedt, Paul; Wilhelm, Lars; Reinikainen, Tapani; Sippola, Erkki; Corander, Jukka

    2010-10-10

    Headspace gas chromatographic measurements of ethanol content in blood specimens from suspect drunk drivers are routinely carried out in forensic laboratories. In the widely established standard statistical framework, measurement errors in such data are represented by Gaussian distributions for the population of blood specimens at any given level of ethanol content. It is known that the variance of measurement errors increases as a function of the level of ethanol content and the standard statistical approach addresses this issue by replacing the unknown population variances by estimates derived from large sample using a linear regression model. Appropriate statistical analysis of the systematic and random components in the measurement errors is necessary in order to guarantee legally sound security corrections reported to the police authority. Here we address this issue by developing a novel statistical approach that takes into account any potential non-linearity in the relationship between the level of ethanol content and the variability of measurement errors. Our method is based on standard non-parametric kernel techniques for density estimation using a large database of laboratory measurements for blood specimens. Furthermore, we address also the issue of systematic errors in the measurement process by a statistical model that incorporates the sign of the error term in the security correction calculations. Analysis of a set of certified reference materials (CRMs) blood samples demonstrates the importance of explicitly handling the direction of the systematic errors in establishing the statistical uncertainty about the true level of ethanol content. Use of our statistical framework to aid quality control in the laboratory is also discussed. PMID:20494532

  20. 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.

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. Comparison of ultraviolet detection and charged aerosol detection methods for liquid-chromatographic determination of protoescigenin.

    PubMed

    Filip, Katarzyna; Grynkiewicz, Grzegorz; Gruza, Mariusz; Jatczak, Kamil; Zagrodzki, Bogdan

    2014-01-01

    Escin, a complex mixture of pentacyclic triterpene saponins obtained from horse chestnut seeds extract (HCSE; Aesculus hippocastanum L.), constitutes a traditional herbal active substance of preparations (drugs) used for a treatment of chronic venous insufficiency and capillary blood vessel leakage. A new approach to exploitation of pharmacological potential of this saponin complex has been recently proposed, in which the β-escin mixture is perceived as a source of a hitherto unavailable raw material, pentacyclic triterpene aglycone-protoescigenin. Although many liquid chromatography methods are described in the literature for saponins determination, analysis of protoescigenin is barely mentioned. In this work, a new ultra-high performance liquid chromatography (UHPLC) method developed for protoescigenin quantification has been described. CAD (charged aerosol detection), as a relatively new detection method based on aerosol charging, has been applied in this method as an alternative to ultraviolet (UV) detection. The influence of individual parameters on CAD response and sensitivity was studied. The detection was performed using CAD and UV (200 nm) simultaneously and the results were compared with reference to linearity, accuracy, precision and limit of detection. PMID:25745765

  6. Simultaneous derivatisation and preconcentration of parabens in food and other matrices by isobutyl chloroformate and dispersive liquid-liquid microextraction followed by gas chromatographic analysis.

    PubMed

    Jain, Rajeev; Mudiam, Mohana Krishna Reddy; Chauhan, Abhishek; Ch, Ratnasekhar; Murthy, R C; Khan, Haider A

    2013-11-01

    A simple, rapid and economical method has been proposed for the quantitative determination of parabens (methyl, ethyl, propyl and butyl paraben) in different samples (food, cosmetics and water) based on isobutyl chloroformate (IBCF) derivatisation and preconcentration using dispersive liquid-liquid microextraction in single step. Under optimum conditions, solid samples were extracted with ethanol (disperser solvent) and 200 μL of this extract along with 50 μL of chloroform (extraction solvent) and 10 μL of IBCF was rapidly injected into 2 mL of ultra-pure water containing 150 μL of pyridine to induce formation of a cloudy state. After centrifugation, 1 μL of the sedimented phase was analysed using gas chromatograph-flame ionisation detector (GC-FID) and the peaks were confirmed using gas chromatograph-positive chemical ionisation-mass spectrometer (GC-PCI-MS). Method was found to be linear over the range of 0.1-10 μg mL(-1) with square of correlation coefficient (R(2)) in the range of 0.9913-0.9992. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.029-0.102 μg mL(-1) and 0.095-0.336 μg mL(-1) with a signal to noise ratio of 3:1 and 10:1, respectively. PMID:23768377

  7. A pyrolysis/gas chromatographic method for the determination of hydrogen in solid samples.

    PubMed

    Carr, R H; Bustin, R; Gibson, E K

    1987-01-01

    A method is described for the determination of hydrogen in solid samples. The sample is heated under vacuum after which the evolved gases are separated by gas chromatography with a helium ionization detector. The system is calibrated by injecting known amounts of hydrogen, as determined manometrically. The method, which is rapid and reliable, was checked for a variety of lunar soils; the limit of detection is about 10 ng of hydrogen. PMID:11542122

  8. A pyrolysis/gas chromatographic method for the determination of hydrogen in solid samples

    NASA Technical Reports Server (NTRS)

    Carr, R. H.; Bustin, R.; Gibson, E. K.

    1987-01-01

    A method is described for the determination of hydrogen in solid samples. The sample is heated under vacuum after which the evolved gases are separated by gas chromatography with a helium ionization detector. The system is calibrated by injecting known amounts of hydrogen, as determined manometrically. The method, which is rapid and reliable, was checked for a variety of lunar soils; the limit of detection is about 10 ng of hydrogen.

  9. Flow system for optical activity detection of vegetable extracts employing molecular exclusion continuous chromatographic detection

    NASA Astrophysics Data System (ADS)

    Fajer, V.; Rodríguez, C.; Naranjo, S.; Mesa, G.; Mora, W.; Arista, E.; Cepero, T.; Fernández, H.

    2006-02-01

    The combination of molecular exclusion chromatography and laser polarimetric detection has turned into a carbohydrate separation and quantification system for plant fluids of industrial value, making it possible the evaluation of the quality of sugarcane juices, agave juices and many other plant extracts. Some previous papers described a system where liquid chromatography separation and polarimetric detection using a LASERPOL 101M polarimeter with He-Ne light source allowed the collection and quantification of discrete samples for analytical purposes. In this paper, the authors are introducing a new improved system which accomplishes polarimetric measurements in a continuous flux. Chromatograms of several carbohydrates standard solutions were obtained as useful references to study juice quality of several sugarcane varieties under different physiological conditions. Results by either discrete or continuous flux systems were compared in order to test the validation of the new system. An application of the system to the diagnostics of scalded foliar is described. A computer program allowing the output of the chromatograms to a display on line and the possibility of digital storing, maxima detections, zone integration, and some other possibilities make this system very competitive and self-convincing.

  10. Evaluation of a Gas Chromatograph-Differential Mobility Spectrometer for Potential Water Monitoring on the International Space Station

    NASA Technical Reports Server (NTRS)

    Wallace, William T.; Limero, Thomas F.; Gazda, Daniel B.; Macatangay, Ariel V.; Dwivedi, Prabha; Fernandez, Facundo M.

    2015-01-01

    Environmental monitoring for manned spaceflight has long depended on archival sampling, which was sufficient for short missions. However, the longer mission durations aboard the International Space Station (ISS) have shown that enhanced, real-time monitoring capabilities are necessary in order to protect both the crewmembers and the spacecraft systems. Over the past several years, a number of real-time environmental monitors have been deployed on the ISS. Currently, volatile organic compounds (VOCs) in the station air are monitored by the Air Quality Monitor (AQM), a small, lightweight gas chromatograph-differential mobility spectrometer. For water monitoring, real-time monitors are used for total organic carbon (TOC) and biocide analysis. No information on the actual makeup of the TOC is provided presently, however. An improvement to the current state of environmental monitoring could be realized by modifying a single instrument to analyze both air and water. As the AQM currently provides quantitative, compound-specific information for VOCs in air samples, this instrument provides a logical starting point to evaluate the feasibility of this approach. The major hurdle for this effort lies in the liberation of the target analytes from the water matrix. In this presentation, we will discuss our recent studies, in which an electro-thermal vaporization unit has been interfaced with the AQM to analyze target VOCs at the concentrations at which they are routinely detected in archival water samples from the ISS. We will compare the results of these studies with those obtained from the instrumentation routinely used to analyze archival water samples.

  11. Capillary column gas chromatographic determination of dicamba in water, including mass spectrometric confirmation.

    PubMed

    Jimenez, N C; Atallah, Y H; Bade, T R

    1989-01-01

    A sensitive method is described for determining dicamba at low micrograms/L levels in ground waters by capillary column gas chromatography with electron-capture detection (GC-EC); compound identity is confirmed by gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring. Dicamba residue is hydrolyzed in KOH to form the potassium salt. The sample is then extracted with ethyl ether which is discarded. The aqueous phase is acidified to pH less than 1 and extracted twice with ethyl ether. The combined ethyl ether extracts are concentrated, and the residue is methylated using diazomethane to form the corresponding dicamba ester. The derivatized sample is cleaned up on a deactivated silica gel column. The methylated dicamba is separated on an SE-30 capillary column and quantitated by electron-capture or mass spectrometric detection. Average recoveries (X +/- SD) for ground water samples fortified with 0.40 microgram/L of dicamba are 86 +/- 5% by GC-EC and 97 +/- 7% by GC-MS detections. The EDL (estimated detection limit) for this method is 0.1 microgram dicamba/L water (ppb). PMID:2808247

  12. Chromatographic analysis of amino and organic acids in physiological fluids to detect inborn errors of metabolism.

    PubMed

    Woontner, Michael; Goodman, Stephen I

    2006-11-01

    This unit describes methods for the preparation of samples for analysis of physiological amino acids and organic acids. Amino acids are analyzed by ion-exchange chromatography using an automated system. Organic acids are analyzed by gas-chromatography/mass spectrometry (GC-MS). Analysis of amino and organic acids is necessary to detect and monitor the treatment of many inborn errors of metabolism. PMID:18428392

  13. The Composition of Titan's Lower Atmosphere and Simple Surface Volatiles as Measured by the Cassini-Huygens Probe Gas Chromatograph Mass Spectrometer Experiment

    NASA Technical Reports Server (NTRS)

    Niemann, H. B.; Atreya, S. K.; Demick, J. E.; Gautier, D.; Haberman, J. A.; Harpold, D. N.; Kasprzak, W. T.; Lunine, J. I.; Owen, T. C.; Raulin, F.

    2010-01-01

    The Cassini-Huygens Probe Gas Chromatograph Mass Spectrometer (GCMS) determined the composition of the Titan atmosphere from 140km altitude to the surface. After landing, it returned composition data of gases evaporated from the surface. Height profiles of molecular nitrogen (N2), methane (CH4) and molecular hydrogen (H2) were determined. Traces were detected on the surface of evaporating methane, ethane (C2H6), acetylene (C2H2), cyanogen (C2N2) and carbon dioxide (CO2). The methane data showed evidence that methane precipitation occurred recently. The methane mole fraction was (1.48+/-0.09) x 10(exp -2) in the lower stratosphere (139.8 km to 75.5 km) and (5.65+/-0.18) x 10(exp -2) near the surface (6.7 km to the surface). The molecular hydrogen mole fraction was (1.01+/-0.16) x 10(exp -3) in the atmosphere and (9.90+/-0.17) x 10(exp -4) on the surface. Isotope ratios were 167.7+/-0.6 for N-14/N-15 in molecular nitrogen, 91.1+/-1.4 for C-12/C-13 in methane and (1.35+/-0.30) x 10(exp -4) for D/H in molecular hydrogen. The mole fractions of Ar-36 and radiogenic Ar-40 are (2.1+/-0.8) x 10(exp -7) and (3.39 +/-0.12) x 10(exp -5) respectively. Ne-22 has been tentatively identified at a mole fraction of (2.8+/-2.1) x 10(exp -7) Krypton and xenon were below the detection threshold of 1 x 10(exp -8) mole fraction. Science data were not retrieved from the gas chromatograph subsystem as the abundance of the organic trace gases in the atmosphere and on the ground did not reach the detection threshold. Results previously published from the GCMS experiment are superseded by this publication.

  14. 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. PMID:7756907

  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. Solid-state voltammetry and polymer electrolyte plasticization as a basis for an electrochemical gas chromatographic detector

    SciTech Connect

    Parcher, J.F.; Barbour, C.J.; Murray, R.W. )

    1989-03-15

    A new type of electrochemical gas chromatographic (ECGC) detector is described. The detector consists of a film of polymer electrolyte, PEO{sub 16}/LiCF{sub 3}SO{sub 3}, coating a microelectrode-based electrochemical cell and in contact with the effluent stream of a gas chromatograph. The PEO{sub 16}/LiCF{sub 3}SO{sub 3} polymer acts as an ionically conducting but physically rigid medium. Currents passed at the microelectrode/polymer interface depend on reactions of electroactive solutes dissolved in and diffusing through the polymer phase. These currents respond to the presence of sample components in the gas phase through their sorption into, and plasticization of, the PEO polymer phase. The polymer plasticization results in larger diffusion coefficients for the electroactive solutes and, consequently, larger microelectrode currents. Several forms of electrochemical potential control are examined as are the effects of chosen electroactive probe, probe concentration, polymer film thickness, and gaseous sample concentration and sorption. Faster detector responses are obtained with thin PEO{sub 16}/LiCF{sub 3}SO{sub 3} films and faster diffusing electroactive probes. The detector responds linearly to small quantities of sample but exponentially to large sample concentrations. The detector is unusual in that it is most sensitive to later-eluting components of a sample mixture; this effect results from the connection between the degree of sample component sorption or partition into the polymer electrolyte and the resulting degree of polymer plasticization and transport rate enhancement.

  17. 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.

  18. Gas chromatographic-mass spectrometric determination of ethyl carbamate in alcoholic beverages.

    PubMed

    Lau, B P; Weber, D; Page, B D

    1987-07-31

    A sensitive and specific method based on gas chromatography-mass spectrometry for the quantitative determination of ethyl carbamate in table wines, fortified wines (such as ports and sherries), distilled spirits, brandies and liqueurs has been developed. Three characteristic ions from ethyl carbamate [m/z 89 (molecular ion), 74 and 62] were monitored in the selected-ion monitoring (SIM) mode. The lowest detection limit (based on the response on the m/z 62 ion) was estimated to be 0.5 ng/g (ppb). Additional confirmation techniques, including high-resolution SIM, and methane or isobutane chemical ionization are described. PMID:3654867

  19. Quantitative liquid chromatographic determination of cefatrizine in serum and urine by fluorescence detection after post-column derivatization.

    PubMed

    Crombez, E; Van der Weken, G; Van den Bossche, W; De Moerloose, P

    1979-09-21

    A fast, specific and sensitive high-performance liquid chromatographic procedure for the determination of cefatrizine, an orally active cephalosporin, in serum and urine is proposed. The drug is determined by the internal standard method, using cephradine as the internal standard. The separation is carried out on a reversed-phase column, filled with octadecylsilane chemically bonded microparticles. The eluent is a mixture of acetonitrile with 0.025 M sodium phosphate buffer (pH 7). Quantitation is effected by fluorescence detection of the fluorophores formed after post-column derivatization with fluorescamine in a packed-bed reactor. The chromatographic conditions and the conditions for the post-column derivatization are discussed. The method has been applied to serum and urine samples, which were analysed after deproteinization with trichloroacetic acid and injection of the clear supernatant. The accuracy and reproducibility of the procedure were investigated by the determination of the cefatrizine content in spiked serum and urine samples. PMID:528641

  20. Determination of Milk Fat Adulteration with Vegetable Oils and Animal Fats by Gas Chromatographic Analysis.

    PubMed

    Kim, Jin-Man; Kim, Ha-Jung; Park, Jung-Min

    2015-09-01

    This study assessed the potential application of gas chromatography (GC) in detecting milk fat (MF) adulteration with vegetable oils and animal fats and of characterizing samples by fat source. One hundred percent pure MF was adulterated with different vegetable oils and animal fats at various concentrations (0%, 10%, 30%, 50%, 70%, and 90%). GC was used to obtain the fatty acid (FA) profiles, triacylglycerol (TG) contents, and cholesterol contents. The pure MF and the adulterated MF samples were discriminated based on the total concentrations of saturated FAs and on the 2 major FAs (oleic acid [C18:1n9c] and linoleic acid [C18:2n6c], TGs [C52 and C54], and cholesterol contents using statistical analysis to compared difference. These bio-markers enabled the detection of as low as 10% adulteration of non-MF into 100% pure MF. The study demonstrated the high potential of GC to rapidly detect MF adulteration with vegetable and animal fats, and discriminate among commercial butter and milk products according to the fat source. These data can be potentially useful in detecting foreign fats in these butter products. Furthermore, it is important to consider that several individual samples should be analyzed before coming to a conclusion about MF authenticity. PMID:26265530

  1. A validated method for gas chromatographic analysis of gamma-aminobutyric acid in tall fescue herbage.

    PubMed

    Kagan, Isabelle A; Coe, Brenda L; Smith, Lori L; Huo, Cheng-Jun; Dougherty, Charles T; Strickland, James R

    2008-07-23

    Gamma-aminobutyric acid (GABA) is an inhibitory neurotransmitter in animals that is also found in plants and has been associated with plant responses to stress. A simple and relatively rapid method of GABA separation and quantification was developed from a commercially available kit for serum amino acids (Phenomenex EZ:faast) and validated for tall fescue (Festuca arundinacea). Extraction in ethanol/water (80:20, v/v) at ambient temperature yielded detectable amounts of GABA. Clean separation from other amino acids in 28 min was achieved by gas chromatography (GC) with flame ionization detection (FID), using a 30 m, 5% phenyl/95% dimethylpolysiloxane column. The identity of the putative GABA peak was confirmed by GC with mass spectrometric (MS) detection. The relatively small effects of the sample matrix on GABA measurement were verified by demonstrating slope parallelism of GABA curves prepared in the presence and absence of fescue extracts. Limits of quantification and detection were 2.00 and 1.00 nmol/100 microL, respectively. Method recoveries at two different spike levels were 96.4 and 94.2%, with coefficients of variation of 7.3 and 7.2%, respectively. PMID:18558696

  2. Gas chromatographic-mass spectrometric determination of hydrophilic compounds in environmental water by solid-phase extraction with activated carbon fiber felt.

    PubMed

    Kawata, K; Ibaraki, T; Tanabe, A; Yagoh, H; Shinoda, A; Suzuki, H; Yasuhara, A

    2001-03-01

    Simple gas chromatographic-mass spectrometric determination of hydrophilic organic compounds in environmental water was developed. A cartridge containing activated carbon fiber felt was made by way of trial and was evaluated for solid-phase extraction of the compounds in water. The hydrophilic compounds investigated were acrylamide, N,N-dimethylacetamide, N,N-dimethylformamide, 1,4-dioxane, furfural, furfuryl alcohol, N-nitrosodiethylamine and N-nitrosodimethylamine. Overall recoveries were good (80-100%) from groundwater and river water. The relative standard deviations ranged from 4.5 to 16% for the target compounds. The minimum detectable concentrations were 0.02 to 0.03 microg/l. This method was successfully applied to several river water samples. PMID:11269598

  3. Advances in the gas chromatographic determination of persistent organic pollutants in the aquatic environment.

    PubMed

    van Leeuwen, S P J; de Boer, J

    2008-04-01

    Environmental chemists have been challenged for over 30 years to analyse complex mixtures of halogenated organic pollutants like polychlorinated biphenyls (PCBs), polychlorinated alkanes (PCAs), polybrominated diphenyl ethers (PBDEs) and polychlorinated dibenzo-p-dioxins and polychlorinated furans (PCDD/Fs). Gas chromatography (GC) often proved to be the method of choice because of its high resolution. The recent developments in the field of comprehensive two-dimensional GC (GCxGC) show that this technique can provide much more information than conventional (single-column) GC. Large volume injection (e.g. by programmed temperature vaporiser, or on-column injection) can be employed for the injection of tens of microliters of sample extract, in that way substantially improving the detection limits. Electron-capture detection (ECD) is a sensitive detection method but unambiguous identification is not possible and misidentification easily occurs. Mass spectrometric (MS) detection substantially improves the identification and the better the resolution (as with MS/MS, time-of-flight (TOF) MS and high-resolution (HR)MS), the lower the chances of misidentification are. Unfortunately, this comes only with substantially higher investments and maintenance costs. Co-extracted lipids, sulphur and other interferences can disturb the GC separation and detection leading to unreliable results. Extraction, and more so, sample clean-up and fractionation, are crucial steps prior to the GC analysis of these pollutants. Recent developments in sample extraction and clean-up show that selective pressurised liquid extraction (PLE) is an effective and efficient extraction and clean-up technique that enables processing of multiple samples in less than 1h. Quality assurance tools such as interlaboratory studies and reference materials are very well established for PCDD/Fs and PCBs but the improvement of that infrastructure is needed for brominated flame retardants, PCAs and toxaphene. PMID

  4. Optimisation of a gas chromatographic method for trace gaseous impurities in nitrogen trifluoride by column sequence reversal.

    PubMed

    de Coning, Johannes Petrus; Swinley, John McNeil

    2008-02-01

    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 mg/L levels included dioxygen (O2), dinitrogen (N2), carbon dioxide (CO2), carbon monoxide (CO), sulfur hexafluoride (SF6), methane (CH4) and nitrous oxide (N2O). Carbon tetrafluoride (CF4) is also present in the product at levels of 20-400mg/L and had to be analysed as well. This paper compares the use of a custom-built dual-channel gas chromatograph utilising single column back flush switching on one channel for the determination of O2, N2, CH4 and CO with column sequence reversal on a second channel for the determination of CO2, N2O, SF6 and CF4 to a similar system using a combination of dual-column back flush and heart-cut configurations. Pulsed discharge helium ionisation detectors were used on both channels in both configurations. PMID:18155712

  5. 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. PMID:10763233

  6. Characterization of Atypical Off-Flavor Compounds in Natural Cork Stoppers by Multidimensional Gas Chromatographic Techniques.

    PubMed

    Slabizki, Petra; Fischer, Claus; Legrum, Charlotte; Schmarr, Hans-Georg

    2015-09-01

    Natural cork stoppers with sensory deviations other than the typical cork taint were subgrouped according to their sensory descriptions and compared with unaffected control cork stoppers. The assessment of purge and trap extracts obtained from corresponding cork soaks was performed by heart-cut multidimensional gas chromatography-olfactometry (MDGC-O). The identification of compounds responsible for atypical cork taint detected in MDGC-O was further supported with additional multidimensional GC analysis in combination with mass spectrometric detection. Geosmin and 2-methylisoborneol were mainly found in cork stoppers described as moldy and cellarlike; 3-isopropyl-2-methoxypyrazine and 3-isobutyl-2-methoxypyrazine were found in cork stoppers described with green attributes. Across all cork subgroups, the impact compound for typical cork taint, 2,4,6-trichloroanisole (TCA), was present and is therefore a good marker for cork taint in general. Another potent aroma compound, 3,5-dimethyl-2-methoxypyrazine (MDMP), was also detected in each subgroup, obviously playing an important role with regard to the atypical cork taint. Sensory deviations possibly affecting the wine could be generated by MDMP and its presence should thus be monitored in routine quality control. PMID:26257078

  7. A gas chromatograph system for semi-continuous greenhouse gas measurements at Puy de Dôme station, Central France

    NASA Astrophysics Data System (ADS)

    Lopez, M.; Schmidt, M.; Ramonet, M.; Bonne, J.-L.; Colomb, A.; Kazan, V.; Laj, P.; Pichon, J.-M.

    2015-03-01

    Three years of greenhouse gases measurements, obtained using a gas chromatograph (GC) system located at the Puy de Dôme station at 1465 m a.s.l. in Central France are presented. The GC system was installed in 2010 at Puy de Dôme and was designed for automatic and accurate semi-continuous measurements of atmospheric carbon dioxide, methane, nitrous oxide and sulfur hexafluoride mole fractions. We present in detail the instrumental set up and the calibration strategy, which together allow the GC to reach repeatabilities of 0.1 μmol mol-1, 1.2, 0.3 nmol mol-1 and 0.06 pmol mol-1 for CO2, CH4, N2O and SF6, respectively. Comparisons of the atmospheric time series with those obtained using other instruments shown that the GC system meets the World Meteorological Organization recommendations. The analysis of the three-year atmospheric time series revealed how the planetary boundary layer height drives the mole fractions observed at a mountain site such as Puy de Dôme where air masses alternate between the planetary boundary layer and the free troposphere. Accurate long-lived greenhouse gases measurements collocated with 222Rn measurements as an atmospheric tracer, allowed us to determine the CO2, CH4 and N2O emissions in the catchment area of the station. The derived CO2 surface flux revealed a clear seasonal cycle with net uptake by plant assimilation in the spring and net emission caused by the biosphere and burning of fossil fuel during the remainder of the year. We calculated a mean annual CO2 flux of 1150 t(CO2) km-2. The derived CH4 and N2O emissions in the station catchment area were 5.6 t(CH4) km-2 yr-1 and 1.5 t(N2O) km-2 yr-1, respectively. Our derived annual CH4 flux is in agreement with the national French inventory, whereas our derived N2O flux is five times larger than the same inventory.

  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. Selection of adsorption traps for in situ gas chromatographic analysis of polar regolith volatiles on board of the Luna-Resource lander

    NASA Astrophysics Data System (ADS)

    Aseev, Sergey; Gerasimov, Mikhail; Zaitsev, Maxim

    Investigation of volatile species in the polar regions of the Moon is an important task for better understanding of its evolution and for further exploration, in particular, to provide resources for future permanent stations. Gas chromatographic complex of Space Research Institute of the Russian Academy of Science is focused on measurements of volatile compounds composition, supposedly existing in the polar regions of the Moon in the area of Luna-Resource probe landing (2017). Also, this devise can be used on the Mars in the area of ExoMars landing mission (2018). One of the features of this gas analytical system is the use of adsorption traps, which can retain volatile compounds continuously coming into the gas chromatograph as a result of pyrolysis of the regolith sample and shortly release them for injection into chromatographic system for analysis. To improve sensitivity and analytical properties of the gas chromatograph, it’s necessary to provide concentrated injection of all the volatile components, which were released during pyrolysis of the regolith sample. It takes ~15 minutes to complete this pyrolysis operation. Such permanent gases as noble gases and N2, Ar, CO on the left hand have low dynamic viscosity, which cause their short retention time in adsorption traps, but on the right hand - these gases are released from the soil sample close to the end of the heating cycle. Summarizing these principles, we can say that 5 minutes of trapping for specified gases is efficient enough for their accumulation with consequent heating of adsorption trap up to 150°C to produce concentrated injection of all these compounds to the analytical columns of gas chromatography system. In the most of space missions (Viking, Phoenix, MSL, Rosetta), which use gas chromatography as the main method for in situ chemical analysis of volatiles, chromatography columns are usually mounted in parallel scheme. It is well known that water has a negative influence on analytical

  10. 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.