Science.gov

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

    PubMed

    Iablochkin, V D

    1999-01-01

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

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

    SciTech Connect

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

    1996-12-31

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

  4. Gas Chromatograph.

    DTIC Science & Technology

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

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

    NASA Astrophysics Data System (ADS)

    O'Hara, Dean; Singh, Hanwant B.

    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.

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

    NASA Technical Reports Server (NTRS)

    O'Hara, Dean; Singh, Hanwant B.

    1988-01-01

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

  7. 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.

  8. 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.

  9. Gas chromatograph injection system

    NASA Technical Reports Server (NTRS)

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

    1975-01-01

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

  10. 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.

  11. 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.

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

    SciTech Connect

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

    1998-01-01

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

  13. Rapid, automated gas chromatographic detection of organic compounds in ultra-pure water

    SciTech Connect

    MOWRY,CURTIS DALE; BLAIR,DIANNA S.; MORRISON,DENNIS J.; REBER,STEPHEN D.; RODACY,PHILIP J.

    2000-02-15

    An automated gas chromatography was used to analyze water samples contaminated with trace (parts-per-billion) concentrations of organic analytes. A custom interface introduced the liquid sample to the chromatography. This was followed by rapid chromatographic analysis. Characteristics of the analysis include response times less than one minute and automated data processing. Analytes were chosen based on their known presence in the recycle water streams of semiconductor manufacturers and their potential to reduce process yield. These include acetone, isopropanol, butyl acetate, ethyl benzene, p-xylene, methyl ethyl ketone and 2-ethoxy ethyl acetate. Detection limits below 20 ppb were demonstrated for all analytes and quantitative analysis with limited speciation was shown for multianalyte mixtures. Results are discussed with respect to the potential for on-line liquid process monitoring by this method.

  14. 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...

  15. 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...

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

    NASA Astrophysics Data System (ADS)

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

    2002-02-01

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

  17. 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.

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

    PubMed

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

    2006-01-01

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

  19. 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.

  20. 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.

  1. Gas chromatographic method for detection of urinary sucralose: application to the assessment of intestinal permeability.

    PubMed

    Farhadi, Ashkan; Keshavarzian, Ali; Holmes, Earle W; Fields, Jeremy; Zhang, Lei; Banan, Ali

    2003-01-25

    We developed a capillary column gas chromatography (CCGC) method for the measurement of urinary sucralose (S) and three other sugar probes including, sucrose, lactulose (L) and mannitol (M) for use in in vivo studies of intestinal permeability. We compared the capillary method with a packed column gas chromatography (PCGC) method. We also investigated a possible role for sucralose as a probe for the measurement of whole gut permeability. Sample preparation was rapid and simple. The above four sugars were detected precisely, without interference. We measured intestinal permeability using 5- and 24-h urine collections in 14 healthy volunteers. The metabolism of sugars was evaluated by incubating the intestinal bacteria with an iso-osmolar mixture of mannitol, lactulose and sucralose at 37 degrees C for 19 h. Sugar concentrations and the pH of the mixture were monitored. The use of the CCGC method improved the detection of sucralose as compared to PCGC. The average coefficient of variation decreased from 15% to 4%. It also increased the sensitivity of detection by 200-2000-fold. The GC assay was linear between sucralose concentrations of 0.2 and 40 g/l (r=1.000). Intestinal bacteria metabolized lactulose and acidified the media but did not metabolize sucralose or mannitol. The new method for the measurement of urinary sucralose permits the simultaneous quantitation of sucrose, mannitol and lactulose, and is rapid, simple, sensitive, accurate and reproducible. Because neither S nor M is metabolized by intestinal bacteria, and because only a tiny fraction of either sugar is absorbed, this pair of sugar probes appears to be available for absorption throughout the GI tract. Thus, the 24-h urinary concentrations of S and M, or the urinary S/M ratio following an oral dose of a sugar mixture, might be good markers for whole gut permeability.

  2. Gas chromatographic/mass spectrometric detection of narcotine, papaverine, and thebaine in seeds of Papaver somniferum.

    PubMed

    Paul, B D; Dreka, C; Knight, E S; Smith, M L

    1996-12-01

    In addition to codeine and morphine, three more compounds: narcotine (noscapine), papaverine, and thebaine were found in Indian and Netherlands poppy seeds (Papaver somniferum L). The compounds were detected by a GC/MS technique and the identities were confirmed by comparing retention times and ion ratios with the known references. The concentrations of codeine, morphine, thebaine, papaverine, and narcotine were 44, 167, 41, 67, and 230 micrograms/g in Indian poppy seeds, and were 1.8, 39, 1.0, 0.17, 0.84 micrograms/g in Netherlands poppy seeds, respectively. Because these compounds may be urinary products after poppy seed consumption, the lowest detectable concentrations of codeine, morphine, thebaine, papaverine, and narcotine in urine are of interest and were found to be 4, 4, 5, 0.4, and 4 ng/ml, respectively. The detection of urinary narcotine, papaverine, or thebaine may be utilized to differentiate poppy seed consumption from illicit codeine, morphine, or heroin use.

  3. 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.

  4. 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.

  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. 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)

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

    PubMed

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

    2001-03-09

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

  8. 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...

  9. 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...

  10. Equations for nickel-chromium wire heaters of column transfer lines in gas chromatographic-electroantennographic detection (GC-EAD).

    PubMed

    Byers, John A

    2004-05-30

    Heating of chromatographic columns, transfer lines, and other devices is often required in neuroscience research. For example, volatile compounds passing through a capillary column of a gas chromatograph (GC) can be split, with half exiting the instrument through a heated transfer line to an insect antenna or olfactory sensillum for electroantennographic detector (GC-EAD) recordings. The heated transfer line is used to prevent condensation of various chemicals in the capillary that would otherwise occur at room temperature. Construction of such a transfer line heater is described using (80/20%) nickel-chromium heating wire wrapped in a helical coil and powered by a 120/220 V ac rheostat. Algorithms were developed in a computer program to estimate the voltage at which a rheostat should be set to obtain the desired heater temperature for a specific coil. The coil attributes (radius, width, number of loops, or length of each loop) are input by the user, as well as AWG size of heating wire and desired heater temperature. The program calculates total length of wire in the helix, resistance of the wire, amperage used, and the voltage to set the rheostat. A discussion of semiochemical isolation methods using the GC-EAD and bioassays is presented.

  11. Determination of volatile organic compounds in ambient air with gas chromatograph-flame ionization and ion trap detection

    SciTech Connect

    Liu, S.; Carley, R.J.; Kang, J.; Chen, J.; Stuart, J.D.

    1994-12-31

    Two new techniques are utilized to integrate the following three equipments: an Entech 2000 automated air concentrator, a Hewlett Packard gas chromatograph (GC) with flame ionization detector (FID) and an ion trap mass spectrometer detector (ITD). This combined analytical system is used to determine low ppb level volatile organic compounds (VOC) in ambient air. The first technique is to configure the inlet system of the GC, so that the pressure regulated flow control system of the GC injection port is used to control the flow of both the desorb gas of the automated air concentrator and the carrier gas of the GC column. The injection port still can be used to inject gas and liquid samples directly. The second technique is to split the effluent of GC column at a 1:1 ratio to the ITD and the FID. In this way, both FID and ITD data can be obtained for each analysis. For ambient air non-methane hydrocarbons monitoring, the FID detector is widely used. Oxygen containing and halogenated organic compounds cannot be differentiated by FID detector and would be quantified as coeluting hydrocarbons. However, volatile organic compounds other than target hydrocarbons can be identified by ITD. This analytical system is very valuable research tool for non-methane hydrocarbons and urban air toxic monitoring. The performances of this developed system have been presented.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. Gas chromatographic determination of phosgene and dichloroacetylene in air1

    PubMed Central

    Jeltes, R.; Burghardt, E.; Breman, J.

    1971-01-01

    Jeltes, R., Burghardt, E., and Breman, J. (1971). Brit. J. industr. Med., 28, 96-99. Gas chromatographic determination of phosgene and dichloroacetylene in air. Phosgene and dichloroacetylene vapours may be present in the working environment near places where chlorinated hydrocarbons are used, including exposure chambers and the like in which people or animals are deliberately exposed to chlorinated hydrocarbons to investigate the effects of these substances. A gas liquid chromatographic method was developed for the determination of sub-Threshold Limit Value concentrations of phosgene and dichloroacetylene. Using electron capture detection, concentrations from 0·02 ppm of each compound could be determined. Images PMID:5543634

  18. High performance hand-held gas chromatograph

    SciTech Connect

    Yu, C M; Koo, J C

    2001-01-10

    Gas chromatography is a prominent technique for separating complex gases and then analyzing the relative quantities of the separate components. This analytical technique is popular with scientists in a wide range of applications, including environmental restoration for air and water pollution, and chemical and biological analysis. Today the analytical instrumentation community is to working towards moving the analysis away from the laboratory to the point of origin of the sample (''the field'') to achieve real-time data collection and lower analysis costs. The Microtechnology Center of Lawrence Livermore National Laboratory, has developed a hand-held, real-time detection gas chromatograph (GC) through Micro-Electro-Mechanical-System (MEMS) technology. The total weight of this GC is approximately 8 pounds, and it measures 8 inches by 5 inches by 3 inches. It consumes approximately 12 watts of electrical power and has a response time on the order of 2 minutes. The current detector is a glow discharge detector with a sensitivity of parts per billion. The average retention time is about 30 to 45 seconds. Under optimum conditions, the calculated effective plate number is 40,000. The separation column in the portable GC is fabricated completely on silicon wafers. Silicon is a good thermal conductor and provides rapid heating and cooling of the column. The operational temperature can be as high as 350 degrees Celsius. The GC system is capable of rapid column temperature ramping and cooling operations. These are especially important for organic and biological analyses in the GC applications.

  19. Mass Spectral Investigations on Toxins. 2. Simultaneous Detection and Quantification of Ultra-Trace Levels of Simple Trichothecenes in Environmental and Fermentation Samples by Gas Chromatographic/Negative Ion Chemical Ionization-Mass Spectrometric Techniques

    DTIC Science & Technology

    1987-01-01

    number) FIELD GROUP SUB-GRO Toxins Derivatization Gas chromatography 15 02 Trichothecenes Negative ion Mass spectrometry "N Mycotoxins Chemical ionization...method for simultnnnously detecting and quantifying several simple trichothecene mycotoxins and related molecules has been developed. The method...FERMENTATION SAMPLES BY GAS CHROMATOGRAPHIC/NEGATIVE ION CHEMICAL IONIZATION-MASS SPECTROMETRIC TECHNIQUES 1. IINTRODUCTION Trichothecene mycotoxins

  20. 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.

  1. Derivatization procedure for gas chromatographic determination of hydroxylamine

    SciTech Connect

    Pesselman, R.L.; Foral, M.J.; Langer, S.H.

    1987-04-15

    Hydroxylamine has been of special interest recently because of the possibilities of manufacturing it by using electrochemical methods in which ammonia might also be formed. Its general chemistry and applications have been described elsewhere. Presently, there are two gas chromatographic methods reported for the determination of hydroxylamine in aqueous media. The first involves reacting the hydroxylamine to form acetone oxime and subsequently injecting the aqueous solution directly into a gas chromatograph equipped with nitrogen and flame ionization detectors. The second involves oxidizing hydroxylamine to nitrous oxide and trapping the gas for determination in an electron capture equipped gas chromatograph. Limits of detection are in the micromolar range for the former and the nanomolar range for the latter. Here, an alternate gas chromatographic procedure for determining hydroxylamine as the acetone oxime is described. Neither direct aqueous injection nor elaborate instrumentation is required. Extraction of the oxime into an ether phase allows for concentrating the analyte ad facilitates the use of an internal standard. The limitations and inconveniences of direct aqueous injection are avoided included column degradation and filament burnout in mass spectrometry detectors.

  2. Simultaneous gas chromatographic determination of concentration and isotopic enrichment of fatty acids in human plasma using flame ionization and mass spectrometric detection.

    PubMed

    Ruiter, A F; Ackermans, M T; Endert, E

    2001-08-05

    Free fatty acids (FFAs) are important not only because they provide substrate for oxidation but also because they have the potential to regulate several metabolic and hormonal processes. Using stable isotope tracers, these processes can be studied. Here we present a gas chromatographic method to measure FFA concentrations and enrichments after extraction from plasma and subsequent derivatization in one analytical run, using both flame ionization and mass-selective detection. For concentration determinations intra-assay variation ranged from 1.5 to 4.9%, inter-assay variation ranged from 3 to 11%. Intra- and inter-assay variations of the enrichment determination of palmitic acid were 1.4 and 0.9%, respectively.

  3. A Small-Scale Low-Cost Gas Chromatograph

    ERIC Educational Resources Information Center

    Gros, Natasa; Vrtacnik, Margareta

    2005-01-01

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

  4. 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.

  5. 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

  6. Target urinary analytes for the gas chromatographic- mass spectrometric detection of procyclidine and benzhexol in drug abuse cases.

    PubMed

    El-Haj, Babiker; Al-Amri, Abdulkader; Ali, Heyam Saad

    2011-03-01

    The two antiparkinsonian drugs procyclidine and benzhexol are presently finding considerable favor for their euphoric hallucinogenic effects among drug abusers in some countries. In anticipation of their possible scheduling in national drug laws, gas chromatography-mass spectrometry (GC-MS) methods for their detection in urine will be required. However, because of uncertainty of the metabolic fate of the two drugs in humans, the urinary target analytes for GC-MS detection were not well defined. The problem was addressed in the present study in which it was found that mono-hydroxy metabolites, where hydroxylation took place at the cyclohexane ring in both drugs, could be endorsed as the major target analytes. The metabolites could only be detected as the mono- and/or di-trimethylsilyl (TMS) derivatives. The predominance of either derivative depended on the temperature and time of heating with the derivatizing reagent. Because of the basic properties of the hydroxy metabolites, analytic method optimization was needed for their detection in urine included extraction under basic pH conditions. Urine hydrolysis with β-glucuronidase did not have an effect on the recovery of the metabolites, but was usually performed in search for other drugs. Because of the relative abundance of ions, the electron impact mass spectra of the mono-TMS derivatives and the chemical ionization (CI) mass spectra of the mono- and di-TMS derivatives of the hydroxy metabolites of both drugs were found to be more structurally informative. The CI mass spectra of the di- TMS derivatives have the additive advantage of being potentially useful for quantitative analysis.

  7. A portable gas chromatograph with simultaneous detection by mass spectrometry and electroantennography for the highly sensitive in situ measurement of volatiles.

    PubMed

    Schott, Matthias; Wehrenfennig, Christoph; Gasch, Tina; Düring, Rolf-Alexander; Vilcinskas, Andreas

    2013-09-01

    Mating disruption is a sustainable method for the control of insect pests, involving the release of synthetic sex pheromones that disrupt the olfactory localization of females by males. However, the development and refinement of this strategy is hampered because current instruments lack the sensitivity to detect volatile organic chemicals in the field, and portable electroantennograms produce non-comparable relative units and distorted results in the presence of plant volatiles. To address the demand for more sensitive instruments that are suitable for the rapid in situ detection of airborne pheromones, we have developed a portable, automated needle trap device connected to a gas chromatograph, mass spectrometer, and electroantennographic detector (NTD-GC-MS/EAD) suitable for field applications. We tested the instrument by measuring the concentration of the sex pheromone (E,Z)-7,9-dodecadienyl acetate, which is used to disrupt the mating of the European grapevine moth Lobesia botrana (Lepidoptera: Tortricidae). Our data confirm that the instrument generates highly reproducible results and is highly sensitive, with a detection threshold of 3 ng/m(3) (E,Z)-7,9-dodecadienyl acetate in outside air.

  8. 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

  9. 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.

  10. 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.

  11. Designer drug 2,4,5-trimethoxyamphetamine (TMA-2): studies on its metabolism and toxicological detection in rat urine using gas chromatographic/mass spectrometric techniques.

    PubMed

    Ewald, Andreas H; Fritschi, Giselher; Maurer, Hans H

    2006-09-01

    Studies are described on the metabolism and the toxicological detection of the amphetamine-derived designer drug 2,4,5-trimethoxyamphetamine (TMA-2) in rat urine using gas chromatographic/mass spectrometric (GC/MS) techniques. The identified metabolites indicated that TMA-2 was metabolized by oxidative deamination to the corresponding ketone followed by reduction to the corresponding alcohol, O-demethylation followed by oxidative deamination, and finally O,O-bis-demethylation. All metabolites carrying hydroxy groups were found to be partly excreted in urine as glucuronides and/or sulfates. The authors' systematic toxicological analysis (STA) procedure using full-scan GC/MS after acid hydrolysis, liquid-liquid extraction, and microwave-assisted acetylation allowed the detection, in rat urine, of an intake of TMA-2 that corresponds to a common drug users' dose. Assuming similar metabolism, the described STA procedure in human urine should be suitable as proof of an intake of TMA-2. Copyright (c) 2006 John Wiley & Sons, Ltd.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. Synthesis and characterization of 4-hydroxy-2-nonenal derivatives for gas chromatographic analysis with electron capture detection (GC-ECD).

    PubMed

    Santaniello, Enzo; Repetto, Alessandro; Chiesa, Luca Maria; Biondi, Pier Antonio

    2007-01-01

    4-Hydroxy-2-nonenal (HNE) has been prepared from the corresponding dimethylacetal (HNE-DMA), in turn synthesized by a conventional approach with a few modifications of the experimental protocol and some improvements in the purification of the final product. In order to exploit the sensitivity of gas-chromatography with electron capture detector (GC-ECD) in the analysis of HNE derivatives, reaction of HNE with 2,4,6-trichlophenylhydrazine (TCPH) and 3,5-dichloro-phenylhydrazine (DCPH) was tested. Reaction with TCPH afforded a mixture of products, whereas with DCPH a single major product was formed that was prepared on a millimolar scale and purified. (1)H-NMR analysis established that the derivative of HNE with DCPH is HNE 3,6-dichloro-phenylhydrazone, that can be used as standard for GC-ECD analysis.

  17. Gas chromatographic/nitrogen-phosphorus detection method for determination of ethylene thiourea in finished drinking waters: collaborative study.

    PubMed

    Longbottom, J E; Edgell, K W; Erb, E J; Lopez-Avila, V

    1993-01-01

    A joint U.S. Environmental Protection Agency (USEPA)-AOAC interlaboratory method validation study was conducted on USEPA National Pesticide Survey (NPS) Method 6, "Determination of Ethylene Thiourea (ETU) in Finished Drinking Water by Gas Chromatography with a Nitrogen-Phosphorus Detector." The purpose of the study was to determine and compare the mean recoveries and precision for determination of ETU in reagent water and finished drinking waters. The study design was based on Youden's nonreplicate plan for collaborative tests of analytical methods. The waters were spiked with ETU at 6 concentrations levels, prepared as 3 Youden pairs. In the method, the test water is extracted by passing the sample through an absorbent matrix type tube. ETU is recovered from the tube with methylene chloride, the extract is solvent-exchanged to ethyl acetate, and an aliquot of each extract is analyzed by gas chromatography using a nitrogen-phosphorus detector. Twelve laboratories participated in the study. Data were analyzed using a USEPA computer program, which measured recovery and precision for ETU and compared the performance of the method between the 2 water types. Over the concentration range tested, the mean percent recoveries of ETU were 82-92% in reagent water and 85-98% in finished drinking water. The range of the between-laboratory relative standard deviations (RSDR) for the 6 concentrations was 5-24% in reagent water, but was only 4-9% in finished drinking water. The range of the within-laboratory relative standard deviations (RSDr) was 6-14% for reagent water and 6-10% for finished drinking water. Results for the 2 water matrixes showed no statistically significant differences.(ABSTRACT TRUNCATED AT 250 WORDS)

  18. Gas chromatographic determination of propylene glycol dinitrate in rodent skin.

    PubMed

    Godin, C S; Pollard, D L

    1992-01-01

    A gas chromatographic (GC) method was developed for the detection of propylene glycol dinitrate (PGDN) in rodent skin following extraction with ethyl acetate. Known quantities of PGDN contained in the torpedo fuel Otto Fuel II were added to homogenates of rat skin, which were subsequently extracted with two 10-mL portions of ethyl acetate. An aliquot of each extract was analyzed by GC with a flame ionization detector. With this method, concentrations ranging from 0.0042 to 11.2 mg/mL were determined by comparison with a standard curve. The extraction efficiencies ranged from 85.7% for the lowest concentration to 101% for the highest concentration.

  19. On-line gas chromatographic analysis of airborne particles

    SciTech Connect

    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.

  20. Continuous fraction collection of gas chromatographic separations with parallel mass spectrometric detection applied to cell-based bioactivity analysis.

    PubMed

    Jonker, Willem; Stöckl, Jan B; de Koning, Sjaak; Schaap, Jaap; Somsen, Govert W; Kool, Jeroen

    2017-06-01

    We describe the development and evaluation of a GC-MS fractionation platform that combines high-resolution fraction collection of full chromatograms with parallel MS detection. A y-split at the column divides the effluent towards the MS detector and towards an inverted y-piece where vaporized trap solvent is infused. The latter flow is directed outside the GC oven allowing subsequent condensation and stepwise collection of liquid fractions with trapped analytes on a 384-well plate. For study and optimization of the effluent split ratio, restriction capillaries of different lengths and diameters were evaluated. For a wide range of settings, local pressures were monitored during fractionation to assess the influence of MS vacuum and trap solvent infusion on the GC system stability. The platform performance was evaluated by GC-MS analysis and continuous fractionation of an n-alkane mixture followed by GC analysis of each fraction. Comparison of the on-line recorded and fraction-reconstructed chromatogram showed the GC separation is maintained during fractionation. Multiple fractionation cycles of the n-alkane sample on the same 384-well plate yielded a reconstructed chromatogram which was highly similar to that of a single analysis, demonstrating the high repeatability. The applicability of the GC-MS-fractionation platform for bioactivity screening was investigated by applying the AR-Ecoscreen reporter gene bioassay on fractions obtained after analysis of standard solutions and dust samples containing the anti-androgenic compounds vinclozolin and p,p'-DDE. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. 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

  2. Mars surface gas chromatograph mass spectrometer

    NASA Technical Reports Server (NTRS)

    Mahaffy, P.

    2000-01-01

    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.

  3. A capillary gas chromatographic assay with nitrogen phosphorus detection for the quantification of topiramate in human plasma, urine and whole blood.

    PubMed

    Riffitts, J M; Gisclon, L G; Stubbs, R J; Palmer, M E

    1999-03-01

    An accurate and robust method involving liquid liquid extraction and capillary gas chromatographic (GC) assay with nitrogen phosphorus detection (NPD) was developed and validated for the quantitative determination of topiramate [2,3:4,5-bis-O-(-1-methylethylidene)-beta-D-fructopyranose sulfamate], Topamax, an anticonvulsant drug, in human plasma, urine, and whole blood. The galactopyranose analog of topiramate was used as the internal standard. A DB-5, fused silica capillary column (J&W Scientific, Folsom, CA) was used, yielding typical retention times of 4.95 min for topiramate and 5.32 min for the internal standard in human plasma. The assay involved organic extraction with methyl t-butyl ether (MTBE) from base, a back extraction into acid and a second extraction in MTBE. The organic solvent was evaporated, and the residue was redissolved and injected for analysis. The standard curve was validated from 0.5 to 50 microg/ml(-1) for human plasma and whole blood, and from 1.0 to 50 microg/ml(-1) for urine. Peak area ratios of drug to internal standard were determined and used to construct a standard curve. The resulting chromatograms showed no endogenous interfering peaks with the respective blank human fluids. Chromatograms corresponding to topiramate and the internal standard produced sharp peaks that were well resolved. This assay showed precision and accuracy of < or = 5%. Two minor human metabolites of topiramate did not interfere with the assay. This assay was successfully applied to determine the pharmacokinetics of topiramate during the development of this drug.

  4. 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...

  5. 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)

  6. 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)

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

    PubMed

    Hoshika, Y; Iida, Y

    1977-04-11

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

  8. The gas-chromatographic analysis system in the JET active gas handling plant

    NASA Astrophysics Data System (ADS)

    Lässer, R.; Grieveson, B.; Hemmerich, J. L.; Stagg, R.; Dowhyluk, T.; Torr, K.; Massey, R.; Chambers, P.

    1993-09-01

    A gas chromatographic system for the analysis of gas species to be collected from the JET torus and to be processed in the JET active gas handling plant during the active operation phase with deuterium and tritium plasmas was designed and built by CFFTP under contract with JET. The gas-chromatograph consists of a compression/injection stage and of two parallel, analytical stages, one for the detection of helium, hydrogen, oxygen, nitrogen, methane, carbon monoxide, and the six hydrogen molecules by means of a thermal conductivity detector (TCD) and one for the detection of carbon monoxide, methane, carbon dioxide, and higher hydrocarbons by means of a flame ionization detector (FID). A flow proportional counting detector (FPCD) is placed in series to TCD and FID for the specific analysis of tritiated gas compounds. A detailed description of the system and of its performance will be given which was evaluated using several calibrated gas mixtures including test runs with tritiated species at JET. The gas species mentioned above can be detected in the concentration range from ppm levels to 100%. The estimated error is about 20% at very low concentrations and 1% at high concentrations. The required minimum detection limit for the TCD can be achieved by the injection of large samples and the use of large filament currents. In addition, neon or helium can be chosen as carrier gas. The use of Ne increases the sensitivity for hydrogen and allows the detection of He, whereas He carrier gas gives superior TCD results for all other gases. Due to the high sensitivity of the FPCDs ppb levels of tritiated gas species can be detected.

  9. Gas chromatographic determination of pentachlorophenol in gelatin.

    PubMed

    Borsetti, A P; Thurston, L S

    1984-01-01

    A method is described for the determination of pentachlorophenol (PCP) in gelatin. The method employs acid and heat to hydrolyze the gelatin matrix, a base partition and wash for separation and cleanup, and a reacidification and extraction with hexane for direct determination of PCP, without preparation of a derivative, using gas chromatography (GC) with a 1% SP- 124ODA liquid phase and a 63Ni electron capture detector. Recoveries averaged 106% for fortifications between 0.02 and 1.0 ppm. The limit of quantitation is 20 ppb. The limit of detection is 4-6 ppb. The method, which has undergone a successful intralaboratory trial, is simple and rapid, and requires only general laboratory reagents and equipment. GC of the acetate derivative of PCP is used for confirmation of identity.

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

    USGS Publications Warehouse

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

    1984-01-01

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

  11. 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.

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

    SciTech Connect

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

    1988-04-15

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

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

    PubMed

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

    2000-01-01

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

  14. 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. Copyright © 2011 John Wiley & Sons, Ltd.

  15. A gas chromatographic-mass spectrometric method using a PoraPLOT column for the detection of hydroperoxide lyase in Chlorella pyrenoidosa.

    PubMed

    Nuñez, A; Foglia, T A; Piazza, G J

    1998-05-01

    A gas chromatographic-mass spectrometric (GC-MS) method using a PoraPLOT Q column was developed for the analysis and identification of the volatile products produced by the action of hydroperoxide lyase (HPLS) upon 13-hydroperoxylinoleic or 13-hydroperoxylinolenic acids. The developed procedure required no derivatization, was not affected by the presence of water, did not require cryogenic conditions to be maintained during injection, and allowed for the quantitation of most products. An acetone powder preparation of Chlorella pyrenoidosa cells was triturated with borate buffer pH = 8.0, and the mixture centrifuged at 12,000 x g. The supernatant and pellet were assayed for HPLS activity by GC-MS analysis of the volatile products given by linoleic acid hydroperoxide. The data showed that the majority of HPLS activity resides in the pellet fraction, and that the primary volatile component was pentane, with smaller amounts of 2-(Z)-pentene and 1-pentene being produced. The fact that HPLS activity resides in the water-insoluble fraction of the acetone powder suggests that HPLS from Chlorella is a membrane-associated enzyme. This investigation also determined that a spectrophotometric assay using alcohol dehydrogenase for measuring HPLS activity was not specific, but measured enzymatic activity other than HPLS.

  16. Determination of plant stanols and plant sterols in phytosterol enriched foods with a gas chromatographic-flame ionization detection method: NMKL collaborative study.

    PubMed

    Laakso, Päivi H

    2014-01-01

    This collaborative study with nine participating laboratories was conducted to determine the total plant sterol and/or plant stanol contents in phytosterol fortified foods with a gas chromatographic method. Four practice and 12 test samples representing mainly commercially available foodstuffs were analyzed as known replicates. Twelve samples were enriched with phytosterols, whereas four samples contained only natural contents of phytosterols. The analytical procedure consisted of two alternative approaches: hot saponification method, and acid hydrolysis treatment prior to hot saponification. As a result, sterol/stanol compositions and contents in the samples were measured. The amounts of total plant sterols and total plant stanols varying from 0.005 to 8.04 g/100 g product were statistically evaluated after outliers were eliminated. The repeatability RSD (RSDr) varied from 1.34 to 17.13%. The reproducibility RSD (RSDR) ranged from 3.03 to 17.70%, with HorRat values ranging from 0.8 to 2.1. When only phytosterol enriched food test samples are considered, the RSDr ranged from 1.48 to 6.13%, the RSD, ranged from 3.03 to 7.74%, and HorRat values ranged from 0.8 to 2.1. Based on the results of this collaborative study, the study coordinator concludes the method is fit for its purpose.

  17. 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.

  18. 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.

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

    PubMed

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

    1985-02-08

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

  20. A gas chromatographic analysis of phosphine in biological material in a case of suicide.

    PubMed

    Musshoff, F; Preuss, J; Lignitz, E; Madea, B

    2008-05-20

    In a suicide committed using aluminium phosphide (AlP) the liberated toxic phosphine gas was detected in post-mortem specimens using a headspace gas chromatographic procedure with a nitrogen-phosphorous detector (HS-GC/NPD). At autopsy a direct sampling into airtight headspace vials for a later analysis is recommended. AlP has to be considered a potent pesticide and its use and availability should be restricted as much as possible.

  1. 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.

  2. 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.

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

    PubMed

    Regert, M; Langlois, J; Colinart, S

    2005-10-14

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

  4. 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.

  5. [Gas chromatographic analysis of cannabinoids on tandem columns].

    PubMed

    Petri, G; Nyiredy, S; Veszki, P; Oroszlán, P; Turiák, G

    1995-05-01

    A simple, isotherm packed column gas chromatographic method was developed for the quantitative determination of neutral cannabinoids using 4-androstene-3,17-dion as internal standard. In order to achieve the best resolution and to avoid the evaluation of the disturbing hydrocarbon peaks a method was developed using "tandem" column made of 3% OV-1 (90%) and 3% OV-17 (10%) stationary phases. The psychotropic cannabinoids delta 1-tetrahydrocannabinol (delta 1-THC) and delta 1(6)-tetrahydrocannabionol (delta 1(6)-THC), as well as, their main metabolites cannabidiol (CBD) and cannabichromene (CBC) were baseline separated except the cannabigerol (CBG) and cannabinol (CBN) pair, however for these compounds the separation was also satisfactory for the quantitative determinations. The Kováts retention indices were calculated for the most important cannabinoids and established the detection limits, respectively (20-50 ng range). The reproducibility was found excellent cv% = 1.06 for delta 1-THC and the analysis time was 55 minutes. The practical usefulness of the method was demonstrated by the comparative analyses on hashish- and fibre type hemps.

  6. Rapid high-performance liquid chromatographic determination with fluorescence detection of furosemide in human body fluids and its confirmation by gas chromatography-mass spectrometry.

    PubMed

    Saugy, M; Meuwly, P; Munafo, A; Rivier, L

    1991-04-05

    Furosemide (FD: Lasix) is a loop diuretic which strongly increases both urine flow and electrolyte urinary excretion. Healthy volunteers were administered 40 mg orally (dissolved in water) and concentrations of FD were determined in serum and urine for up to 6 h for eight subjects, who absorbed water at a rate of 400 ml/h. Quantification was performed by HPLC with fluorescence detection (excitation at 233 nm, emission at 389 nm) with a limit of detection of 5 ng/ml for a 300-microliters sample. The elution of FD was completed within 4 min using a gradient of acetonitrile concentration rising from 30 to 50% in 0.08 M phosphoric acid. The delay to the peak serum concentration ranged from 60 to 120 min. FD was still easily measurable in the sera from all subjects 6 h after administration. In urine, the excretion rates reached their maximum between 1 and 3 h. The total amount of FD excreted in the urine averaged 11.2 mg (range 7.6-14.0 mg), with a mean urine volume of 3024 ml (range 2620-3596 ml). Moreover, the urine density was lower than 1.010 (recommended as an upper limit in doping analysis to screen diuretics) only for 2 h. An additional volunteer was administered 40 mg of FD and his urine was collected over a longer period. FD was still detectable 48 h after intake. Gas chromatography-mass spectrometry with different types of ionization was used to confirm the occurrence of FD after permethylation of the extract. Negative-ion chemical ionization, with ammonia as reactant gas, was found to be the most sensitive method of detection.

  7. Determination of sulphur compounds in beer using headspace solid-phase microextraction and gas chromatographic analysis with pulsed flame photometric detection.

    PubMed

    Hill, P G; Smith, R M

    2000-03-03

    A simple and sensitive method for the analysis of volatile and semi-volatile sulphur compounds in beer at trace levels was developed using headspace solid-phase microextraction (SPME) and gas chromatography with pulsed flame photometric detection. Different SPME fibres were tested and a Carboxen-polydimethylsiloxane coated fibre was found to be the most appropriate. The adsorption and desorption conditions were optimised. The effect of ethanol concentration in the sample on the extraction of analytes was examined. A 60 m non-polar capillary column preceded by a 10 m length of a polar column was found to be capable of separating a wide range of C1-C6 sulphur compounds. The pulsed flame photometric detector enabled increased sensitivity to be obtained over previous methods, such as dynamic headspace followed by conventional flame photometric detection or sulphur chemiluminescent detection, with high sulphur selectivity. Two sulphur compounds, 2-methyl-1-butanethiol and 3-methylthiophene, were identified in beer for the first time.

  8. Gas chromatographic detection of some nitro explosive compounds in soil samples after solid-phase microextraction with carbon ceramic copper nanoparticle fibers.

    PubMed

    Farhadi, Khalil; Bochani, Shayesteh; Hatami, Mehdi; Molaei, Rahim; Pirkharrati, Hossein

    2014-07-01

    In this research, a new solid-phase microextraction fiber based on carbon ceramic composites with copper nanoparticles followed by gas chromatography with flame ionization detection was applied for the extraction and determination of some nitro explosive compounds in soil samples. The proposed method provides an overview of trends related to synthesis of solid-phase microextraction sorbents and their applications in preconcentration and determination of nitro explosives. The sorbents were prepared by mixing of copper nanoparticles with a ceramic composite produced by mixture of methyltrimethoxysilane, graphite, methanol, and hydrochloric acid. The prepared sorbents were coated on copper wires by dip-coating method. The prepared nanocomposites were evaluated statistically and provided better limits of detection than the pure carbon ceramic. The limit of detection of the proposed method was 0.6 μg/g with a linear response over the concentration range of 2-160 μg/g and square of correlation coefficient >0.992. The new proposed fiber has been demonstrated to be a suitable, inexpensive, and sensitive candidate for extraction of nitro explosive compounds in contaminated soil samples. The constructed fiber can be used more than 100 times without the need for surface generation. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Gas-chromatographic analysis of high-purity helium using a helium detector

    SciTech Connect

    Krylov, V.A.; Aleksandrov, S.D.; Krasotskii, S.G.; Chernyatin, A.K.; Shkrunina, T.V.

    1986-10-10

    The limits of gas-chromatographic detection of neon, hydrogen, argon, nitrogen, krypton, and methane in helium have been determined using a helium ionization detector under saturation current conditions. The detection limits are restricted by the gas permeability of the detector Teflon body and the injection system. The dependence of extraction of impurity gases by cryogenic adsorption enrichment on their contents and enrichment time has been examined. the relative detection limit can be lowered by preconcentration of 3 x 10/sup -5/% for neon and to 4 x 10/sup -7/ to 2 x 10/sup -8/% for other gases.

  10. Gas chromatographic method using electron-capture detection for the determination of musk xylene in human blood samples. Biological monitoring of the general population.

    PubMed

    Angerer, J; Käfferlein, H U

    1997-05-23

    Musk xylene (2,4,6-trinitro-1,3-dimethyl-5-tert.-butylbenzene, MX), a synthetic musk often used in different fragrances and soaps to substitute the natural musk, is a potential contaminant of humans. In this publication, a specific and sensitive detection method for the determination of musk xylene in human blood samples is described. The clean-up of the blood samples includes an extraction step followed by a solid-phase adsorption to separate MX from other plasma components. Separation and detection was carried out by capillary gas chromatography and an electron capture detector (GC-ECD). The results were verified using qualitative capillary gas chromatography and a mass selective detector with electron impact ionisation (GC-EI-MS). epsilon-Hexachlorocyclohexane (epsilon-HCH) is used as internal standard. The reliability of the GC-ECD method has been proved. The relative standard deviations of the within-series imprecision were 12.7% for samples with a concentration of 0.5 microg/l and 2.1% for samples with a concentration of 5.0 microg/l, whereas the relative standard deviations for the between-day imprecision were 14.9% (0.5 microg/l samples) and 3.4% (5.0 microg/l samples). The losses during sample treatment were between 10.1% and 17.8%. No interfering peaks were observed. The absolute detection limit was 0.1 microg/l plasma. A total of 72 human blood samples were analysed to determine the MX concentrations within the general population. In 66 of the 72 human blood samples, the MX concentrations ranged from 0.10 to 1.12 microg/l plasma for the described method. In six samples no MX was detected. The median concentration was 0.24+/-0.23 microg MX/l plasma. The 95 percentile was 0.79 microg/l. No correlation could be found between MX concentrations and smoking habit, broca index, age, sex as well as fish consumption habits. Nevertheless, the results demonstrate the exposure of the general population to MX.

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

    PubMed Central

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

    2010-01-01

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

  12. Determination of tetramethylenedisulfotetramine in human urine with gas chromatograph-flame thermionic detection coupling with direct immersed solid-phase micro-extraction.

    PubMed

    Zeng, Dong; Chen, Bo; Yao, Shouzhuo; Ying, Jianying

    2006-06-02

    An analytical method for determination of tetramethylenedisulfotetramine (tetramine) in human urine by gas chromatography-flame thermionic detection (GC-FTD) coupling with a direct immersed solid-phase micro-extraction (DI-SPME) was developed. The enrichment effects of three fiber coatings of SPME for tetramine were compared. Results showed that the enrichment effect of polar 85 microm polyacrylate (PA) coating was better than that of apolar 100 and 7 microm polydimethylsiloxane (PDMS) coatings. Other experimental parameters, such as ionic strength, volume, temperature of sample solution and time for extraction, time and temperature for desorption, were also optimized. The correlation coefficient of the calibration curve was 0.9998 in the range of 0.082-41.0 ng/mL for tetramine. The limit of quantitation of tetramine in urine was 0.082 ng/mL. In this method, the sample pretreatment is simple and convenient. As a monitoring means, it has been successfully applied to detection of tetramine toxicosis in criminal cases, as well as clinical therapy of poisoned sufferer.

  13. Comparison of differential mobility spectrometry and mass spectrometry for gas chromatographic detection of ignitable liquids from fire debris using projected difference resolution.

    PubMed

    Lu, Yao; Chen, Ping; Harrington, Peter B

    2009-08-01

    The significance of forensic arson analysis accelerates the applications of new technologies in this area. Based on the previously reported application of differential mobility spectrometry (DMS) as a detection method for gas chromatography (GC) in arson analysis, the performances of DMS and mass spectrometry (MS) were compared using a novel chemometric tool, projected difference resolutions (PDRs). The PDR results show that one-way mass spectra data exhibit higher resolution than DMS data, while total ion chromatograms from GC-DMS show higher resolution than that from GC/MS for differentiating seven kinds of ignitable liquids. Combining the information from both chromatography and spectra, two-way data always have higher resolution than one-way data for these two detection methods, and GC/MS would exhibit better performance than GC-DMS according to the minimum resolution value. To verify the PDR results, a fuzzy rule-building expert system was applied for classifying these seven kinds of ignitable liquids from fire debris based on GC-DMS and GC/MS data, respectively. The prediction accuracies were consistent with PDR results, which proved that PDR is a powerful tool in comparing the performances of different analysis methods for pattern recognition.

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

    DTIC Science & Technology

    1981-12-01

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

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

    PubMed

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

    1995-01-01

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

  16. 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

  17. Gas chromatographic analysis of toxic edemagenic inhalation compounds

    SciTech Connect

    Shih, M.L.; Smith, J.R.; McMonagle, J.D. )

    1990-01-01

    Different megabore column and packed column phases were evaluated for their suitability in the gas chromatographic analysis of three toxic polyhalogenated compounds (phosgene, TFD, and PFIB). Adsorbent type stationary phases provide better retention and separation for the volatile fluorocarbons than do polar and nonpolar liquid phases. The reactivity of phosgene precludes the use of many phases having hydroxy, amino, or cyano functional groups. Silica gel is still the column of choice for phosgene. The use of gas sampling bags and gas-tight syringes can provide reliable quantitation of these compounds in air samples. TFD and PFIB exhibit different electron capture mechanisms and detector temperature dependency. The mechanisms are supported by the results of negative ion mass spectrometry.

  18. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

    PubMed

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  19. 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.

  20. 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

  1. 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

  2. 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

  3. Gas chromatographic characterization of vegetable oil deodorization distillate.

    PubMed

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

    2001-07-06

    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.

  4. 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.

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

    SciTech Connect

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

    1982-08-01

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

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

    PubMed

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

    2016-10-01

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

  7. 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.

  8. Gas chromatographic determination of oxalic acid in foods.

    PubMed

    Ohkawa, H

    1985-01-01

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

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

    PubMed

    Zygmunt, B; Namiesnik, J

    2001-08-01

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

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

    PubMed

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

    1981-01-01

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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. 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

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

    PubMed

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

    2014-03-01

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

  19. 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

  20. New designer drug alpha-pyrrolidinovalerophenone (PVP): studies on its metabolism and toxicological detection in rat urine using gas chromatographic/mass spectrometric techniques.

    PubMed

    Sauer, Christoph; Peters, Frank T; Haas, Claudia; Meyer, Markus R; Fritschi, Giselher; Maurer, Hans H

    2009-06-01

    The aim of the present study was to identify the metabolites of the new designer drug alpha-pyrrolidinovalerophenone (PVP) in rat urine using GC/MS techniques. Eleven metabolites of PVP could be identified suggesting the following metabolic steps: hydroxylation of the side chain followed by dehydrogenation to the corresponding ketone; hydroxylation of the 2''-position of the pyrrolidine ring followed by dehydrogenation to the corresponding lactam or followed by ring opening to the respective aliphatic aldehyde and further oxidation to the respective carboxylic acid; degradation of the pyrrolidine ring to the corresponding primary amine; and hydroxylation of the phenyl ring, most probably in the 4'-position. The authors' screening procedure for pyrrolidinophenones allowed the detection of PVP metabolites after application of a dose corresponding to a presumed user's dose. In addition, the involvement of nine different human cytochrome P450 (CYP) isoenzymes in the side chain hydroxylation of PVP was investigated and CYP 2B6, 2C19, 2D6, and 3A4 were found to catalyze this reaction.

  1. 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

  2. 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

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

    DTIC Science & Technology

    1985-08-01

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

  4. 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.

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

    NASA Technical Reports Server (NTRS)

    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.

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

    NASA Technical Reports Server (NTRS)

    Cannon, W. A.

    1972-01-01

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

  7. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-10-01

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

  9. 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.

  10. Liquid chromatographic determination of atropine in nerve gas antidotes and other dosage forms.

    PubMed

    Lehr, G J; Yuen, S M; Lawrence, G D

    1995-01-01

    A simple and specific liquid chromatographic method was developed for the determination of atropine in nerve gas antidotes and several other dosage forms. The method is also used simultaneously to quantitate phenol, an antimicrobial agent present in nerve gas antidotes, and to monitor the level of tropic acid, a principal degradation product of atropine. The system uses a Spherisorb CN column and a mobile phase of acetonitrile-0.05M sodium phosphate monobasic (10 + 90), pH 4.0. The detection wavelength is 220 nm. The method was validated by testing for accuracy, linearity, reproducibility and precision. In addition, the proposed method was applied to 8 commercial preparations of atropine, including injectables, ophthalmic solutions, and ointments, and was found to be satisfactory and free from interferences from preservatives, such as benzyl alcohol, methylparaben, benzalkonium chloride and chlorobutanol, that are present in these formulations.

  11. 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.

  12. 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.

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

    PubMed

    Albreht, Alen; Zupančič, Borut; Vovk, Irena

    2014-01-01

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

  14. Gas-chromatographic determination of aviation gasoline and JP-4 jet fuel in subsurface core samples (journal version)

    SciTech Connect

    Vandegrift, S.A.; Kampbell, D.H.

    1988-01-01

    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 extract is analyzed by wide-bore capillary-column gas chromatography with flame-ionization detection. Advantages of the method are a short analysis time of 20 minutes, the use of small amounts of solvent, detection limit in the low parts-per-million range, and determination of the type of fuel contamination (i.e. avgas or jet fuel) by the chromatographic pattern or fingerprint.

  15. Comprehensive headspace gas chromatographic analysis of denaturants in denatured ethanol.

    PubMed

    van Boxtel, Niels; Wolfs, Kris; Guillén Palacín, Marta; Van Schepdael, Ann; Adams, Erwin

    2017-08-09

    To discourage consumption, ethanol is often denatured using both volatile (e.g., methyl ethyl ketone and isopropanol) and nonvolatile (e.g., denatonium benzoate) chemical substances. As a result, the analysis of denatured ethanol samples is usually performed by multiple techniques such as gas chromatography for the volatile denaturants and liquid chromatography for the nonvolatile ones. However, the need for multiple techniques increases the cost of analysis and forms a severe obstruction for on-site product control. Using the full evaporation technique combined with gas chromatography and flame ionization detection, only one analytical methodology has to be used here to determine both volatile and nonvolatile denaturants in denatured ethanol. Denatonium benzoate is determined as benzyl chloride following an in-vial reaction. Compared to conventional techniques, the novel method performs equally well, but it is simpler to apply. At the same time, drawbacks of alternative methods are circumvented such as equilibration issues and alterations to the stationary phase when using liquid chromatography with ion pairing agents or matrix effects when applying static headspace gas chromatography. The developed method showed good linearity, repeatability, and recovery toward all analytes and was applied to the analysis of commercial denatured ethanol for disinfection and ethanol-based windscreen washer fluids. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Considerations on the temperature dependence of the gas-liquid chromatographic retention.

    PubMed

    González, Francisco Rex

    2002-01-04

    A discussion on the temperature dependence of the partition coefficient K is developed. This discussion embraces topics such as the limitations of conventional thermodynamic approaches followed in the chromatographic literature, qualitative theoretical notions arising from molecular thermodynamics and the experimental information that is accessible through modern capillary gas chromatography. It is shown that the heat capacity difference of solute transfer for flexible molecules has at least one maximum in the chromatographic range of temperature. As a consequence, a great amount of experimental data is required for a correct thermodynamic interpretation of the chromatographic retention.

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

    NASA Technical Reports Server (NTRS)

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

    1971-01-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1971-01-01

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

  19. 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

  20. 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.

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

    PubMed

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

    1999-01-01

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

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

    PubMed

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

    2007-07-09

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

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

    PubMed

    Meatherall, Robert; Palatnick, Wes

    2009-10-01

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

  4. Gas Chromatographic Analysis of Acidic Indole Auxins in Nicotiana1

    PubMed Central

    Bayer, Margret H.

    1969-01-01

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

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

    PubMed

    Héberger, Károly; Zenkevich, Igor G

    2010-04-23

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

  6. 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.

  7. 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.

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

    PubMed

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

    2001-11-30

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

  9. An inverse gas chromatographic methodology for studying gas-liquid mass transfer.

    PubMed

    Paloglou, A; Martakidis, K; Gavril, D

    2017-01-13

    A novel methodology of reversed flow inverse gas chromatography (RF-IGC) is presented. It permits the simultaneous determination of mass transfer coefficients across the gas liquid interface as well as the respective solubility parameters and thermodynamic functions of dissolution of gases into liquids. The standard deviation of the experimentally determined parameters is estimated for first time, which combined with the successful comparison of the values of the present parameters with other literature ones ascertain the reliability of the methodology. Another novelty of the present work is that the chromatographic sampling of the physicochemical phenomena is done without performing the usual flow reversals procedure. Vinyl chloride monomer's (VCM) interaction with various composition liquid foods: orange juice, milk and olive oil was used as model system. The present transfer rates are controlled by the gas film at lower temperatures, but at higher temperatures the resistances in both films tend to become equal. The found liquid diffusivity values express the total mass transfer from the gas phase into the liquid's bulk and they decrease with rising temperature, as the solubilities of gases in liquids do. Solubility, expressed by Henry's law constant and the mean values of interfacial thickness are of the same order of magnitude to literature ones. From the thermodynamic point of view, VCM dissolution in all liquids is accompanied by significant heat release and it is a slightly non-spontaneous process, near equilibrium, while the entropy change values are negative. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    SciTech Connect

    Mott, J.

    1995-12-31

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

  11. 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.

  12. 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.

  13. 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. Published by Elsevier B.V.

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

    PubMed

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

    2015-04-15

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

  15. 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

  16. 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

  17. 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

  18. 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

  19. [Gas chromatographic determination of N,N-asymmetric dimethylhydrazine in different environmental objects].

    PubMed

    Kuznetsova, L V; Egorova, G I; Mironov, A A

    2008-01-01

    The paper describes different guidelines used to develop a procedure for gas chromatographic determination of N,N-asymmetric dimethylhydrazine (NDMH) in various environmental objects in the area of a missile-dismantling base. The authors showed that the use of a capillary column with a 5-microm liquid phase layer on a Kristall-5000 chromatograph with a nitrogenous phosphoric detector (Russia) allowed development of a unified gas chromatographic procedure for determining NDMH in air, water, soil, biological material (urine), and plant cover (moss, couch-grass). The procedures differ in the way how to prepare samples and the analysis itself is based on conversion of NDMH to N,N-dimethylhydrazone-4-nitrobenzaldehyde, its liquid extraction from water, concentration of the extract via evaporation and assay by the internal standard test.

  20. 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)

  1. 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...

  2. 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...

  3. 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...

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

    PubMed

    Dong, Jinqiao; Liu, Yan; Cui, Yong

    2014-12-11

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

  5. 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...

  6. 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...

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

    PubMed

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

    2011-12-01

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

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

    PubMed

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

    2009-02-01

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

  9. 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.

  10. 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.

  11. 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.

  12. Gas chromatographic determination of hydroxyproline in urine hydrolysates.

    PubMed

    Makita, M; Yamamoto, S; Tsudaka, Y

    1978-09-01

    A simple and specific method for the determination of hydroxyproline in urine hydrolysates has been described. Hydroxyproline was converted into its N-isobutyloxycarbonyl methyl ester derivative without elaborate cleanup, which was analyzed by gas chromatography. Hydroxyproline was clearly separated from other urinary constituents on a 0.60% FFAP on dimethyldichlorosilane-treated Gas-Chrom P column. Kainic acid was used as the most convenient internal standard available. The relative standard deviations of peak height ratios were 1.15--2.51% at the 10--150 microgram levels. Percent recoveries of hydroxyproline added to urine hydrolysates ranged from 98.8 to 107.3%.

  13. A Gas-Liquid Chromatographic Examination of Stilbene Derivatives

    Treesearch

    Richard W. Hemingway; W. E. Hillis; K Burerton

    1970-01-01

    Trimethylsilyl ether derivatives of twenty hydroxystilbenes were separated by gas-liquid chromatography on Apiezon-L, OV-1, OV-17, and SE-54. Relative retention times were highly dependent upon the degree of hydroxylation and methoxylation, the positions of these groups and on cis-trans...

  14. 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.…

  15. 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.…

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

    PubMed

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

    2008-02-01

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

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

    SciTech Connect

    Chipman, D.W.; Takahashi, T.

    1992-12-01

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

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

    SciTech Connect

    Chipman, D.W.; Takahashi, T.

    1992-12-01

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

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

    SciTech Connect

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

    1980-11-01

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

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

    SciTech Connect

    Dix, K.D.

    1990-01-01

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

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

    DTIC Science & Technology

    2005-07-27

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

  2. 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.

  3. 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.

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

    PubMed

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

    2012-01-01

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

  5. A transportable turnkey gas chromatograph/ion trap detector for field analysis of environmental samples

    SciTech Connect

    Cisper, M.E.; Alarid, J.E.; Hemberger, P.H.; Vanderveer, E.P.

    1990-01-01

    We have developed two transportable gas chromatograph/ion trap detectors (GC/ITD) for the in-situ characterization of chemical waste sites. These instruments are based on a modular design and can be readily modified in the field for air, water, or soil sampling. A purge-and-trap GC is used for the separation of volatile organic compounds before their introduction to the ion trap for mass spectral analysis. A secondary, or daughter, microprocessor controls ancillary hardware by means of the ion trap software. Most analyses are accomplished in an automated 20-min procedure. The detection limit for trichloroethylene in water is in the low part-per-trillion range. The analysis of soil and water samples is demonstrated by using surrogate samples spiked with 24 volatile organic compounds. The first instrument has been used under field conditions for soil analysis at a chemical waste site. The second-generation instrument differs from the first in the extensive use of commercially available equipment. The second-generation instrument will be briefly described here and some preliminary comparisons will be made to the first instrument. 11 refs., 8 figs., 2 tabs.

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

    PubMed

    Faughnan, K T; Woodruff, M A

    1991-01-01

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

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

    PubMed

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

    1988-01-01

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

  8. 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.

  9. Micro-flame ionization detector with a novel structure for portable gas chromatograph.

    PubMed

    Wang, Jianwei; Wang, Hua; Duan, Chunfeng; Guan, Yafeng

    2010-08-15

    A micro-flame ionization detector (micro-FID) for portable gas chromatograph (GC) based on conventional mechanical fabrication techniques was developed and evaluated. Structure was redesigned and dimensions were optimized for best performance. Air is introduced from upper part of the detector, flowing downwards into the burning chamber along a narrow round gap between the collection electrode and the inner wall of the detector body, forming a uniform flow field around the burning jet. The lowest detection limit of the mu-FID was 5x10(-13)g/s for n-decane, with a linear response range of five orders of magnitude. The consumption of gases is only 10 ml/min for hydrogen, and 120 ml/min for air, that is about 1/3 of the gases required for conventional FIDs. A comparative study between the micro-FID and commercial FID was also performed that proved the advantages of the micro-FID. The micro-FID is simple in structure, low heating power, and low consumption of gases that not only decrease the cost of running, but also increase the portability of GC for filed applications. Copyright 2010 Elsevier B.V. All rights reserved.

  10. 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. W.; Sive, B. C.

    2010-12-01

    Hydrogen cyanide (HCN) is thought to be a unique, long lived atmospheric tracer for biomass burning emissions. Very few in-situ measurements of HCN have been made at Earth’s surface to date, yet they are critically needed to better evaluate the processes governing the distribution of HCN in the global atmosphere and to assess contributions of biomass burning to the composition and chemistry of ambient air. We developed a gas-chromatographic (GC) instrument with an aim to improve capabilities for measurement of 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. The instrument was deployed for a ~4 month period from January-June, 2010 at the AIRMAP atmospheric monitoring station Thompson Farm 2 (THF2) in rural Durham, New Hampshire, USA. A subset of the measurements will be presented with a detailed description of the instrument features and performance characteristics. The results demonstrate that the instrument is capable of making long term in-situ measurements of HCN in the lower atmosphere.

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

    PubMed

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

    2002-01-01

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

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

    PubMed

    Alves, Susana P; Bessa, Rui J B

    2009-06-26

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

  13. Gas-chromatographic screening of capsular polysaccharides of Neisseria meningitidis.

    PubMed

    Bryn, K; Frøholm, L O; Holten, E; Bøvre, K

    1983-06-01

    Thirteen systemic strains, i e strains isolated from systemic infections, and 77 carrier isolates of Neisseria meningitidis were serogrouped by agglutination and analyzed by gas chromatography (GC) of phenol extracts. For systemic strains the sugar patterns were in accordance with their group-specific capsular polysaccharides (CPS). Some carrier isolates revealed unexpected GC profiles. Upon immunological retesting with new sera, GC results were generally confirmed. Occasional isolates initially serogrouped as B or Y completely lacked neuraminic acid. Some non-groupable isolates were shown by ultracentrifugation and GC to have significant amounts of this sugar likely to originate from CPS of known composition or from unknown polysaccharides. One such originally non-groupable isolate showed a weak agglutination reaction specifically with group B antiserum when reexamined. Generally, carrier isolates had lower amounts of CPS than systemic strains of the same group. Five successive isolates from one carrier were first serogrouped as X, Z or non-groupable, but they had high amounts of galactosamine and 2-keto-3-deoxy octonate, sugars characterizing CPS of serogroup 29E. These isolates were confirmed by agglutination with recently available group 29E antiserum to be of this serogroup, which has not been reported before in Norway. Ultracentrifugation revealed the presence of unknown polysaccharides containing glucose, galactose or glucosamine, but further purification of these polymers is required to determine their composition and immunological importance.

  14. 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.

  15. 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.

  16. In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water.

    PubMed

    Varanusupakul, Pakorn; Vora-Adisak, Narongchai; Pulpoka, Bancha

    2007-08-13

    An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 degrees C for 60 min with 20% Na2SO4. The linear calibration curves were observed for the concentrations ranging from 1 to 300 microg L(-1) with the correlation coefficients (R2) being greater than 0.99. The method detection limits of most analytes were below 1 microg L(-1) except DCAA and MCAA that were 2 and 18 microg L(-1), respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water.

  17. Gas chromatographic analysis of dimethyltryptamine and beta-carboline alkaloids in ayahuasca, an Amazonian psychoactive plant beverage.

    PubMed

    Pires, Ana Paula Salum; De Oliveira, Carolina Dizioli Rodrigues; Moura, Sidnei; Dörr, Felipe Augusto; Silva, Wagner Abreu E; Yonamine, Mauricio

    2009-01-01

    Ayahuasca is obtained by infusing the pounded stems of Banisteriopsis caapi in combination with the leaves of Psychotria viridis. P. viridis is rich in the psychedelic indole N,N-dimethyltryptamine, whereas B. caapi contains substantial amounts of beta-carboline alkaloids, mainly harmine, harmaline and tetrahydroharmine, which are monoamine-oxidase inhibitors. Because of differences in composition in ayahuasca preparations, a method to measure their main active constituents is needed. To develop a gas chromatographic method for the simultaneous determination of dimethyltryptamine and the main beta-carbolines found in ayahuasca preparations. The alkaloids were extracted by means of solid phase extraction (C(18)) and detected by gas chromatography with nitrogen/phosphorous detector. The lower limit of quantification (LLOQ) was 0.02 mg/mL for all analytes. The calibration curves were linear over a concentration range of 0.02-4.0 mg/mL (r(2 )> 0.99). The method was also precise (RSD < 10%). A simple gas chromatographic method to determine the main alkaloids found in ayahuasca was developed and validated. The method can be useful to estimate administered doses in animals and humans for further pharmacological and toxicological investigations of ayahuasca. Copyright (c) 2009 John Wiley & Sons, Ltd.

  18. 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.

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

    NASA Technical Reports Server (NTRS)

    Brabbs, Theodore A.; Wey, Chowen Chou

    1996-01-01

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

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

    PubMed

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

    2001-05-11

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

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

    DTIC Science & Technology

    1986-11-01

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

  2. 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.

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

    NASA Technical Reports Server (NTRS)

    Niemann, Hasso B.

    2006-01-01

    The GCMS was part of the instrument complement on the Cassini-Huygens Probe to measure in situ the chemical composition of the atmosphere during the probe descent and coupled with the Aerosol Collector Pyrolyser (ACP) experiment by serving as detector for the pyrolization products to determine the composition of the aerosol particles. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns, a chemical scrubber and a hydrocarbon enrichment cell. The GCMS gas inlet was heated to prevent condensation, and to evaporate volatiles from the surface after impact. The GCMS collected data from an altitude of 146 km to ground impact. The Probe and the GCMS survived impact and collected data for 1 hour and 9 minutes on the surface. Mass spectra were collected during descent and on the ground over a range of m/z from 2 to 141. The major constituents of the lower atmosphere were confirmed to be NP and CH4. The methane mole fraction was uniform in the stratosphere. It increased below the tropopause, at about 32 km altitude, monotonically toward the surface, reaching a plateau at about 8 km at a level near saturation. After surface impact a steep increase of the methane signal was observed, suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. The measured mole fraction of Ar-40 is 4.3 x 10(exp-5) and of Ar-36 is 2.8 x 10(exp -7). The other primordial noble gases were below mole fraction. The isotope ratios of C-12/C-13 determined from methane measurements are 82.3 and of N-14/N-15 determined from molecular nitrogen are 183. The D/H isotope ratio determined from the H2 and HD measurements is 2.3 x l0(exp -4). Carbon dioxide, ethane, acetylene and cyanogen were detected evaporating from the surface in addition to methane.

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

    NASA Technical Reports Server (NTRS)

    Niemann, Hasso B.

    2006-01-01

    The GCMS was part of the instrument complement on the Cassini-Huygens Probe to measure in situ the chemical composition of the atmosphere during the probe descent and coupled with the Aerosol Collector Pyrolyser (ACP) experiment by serving as detector for the pyrolization products to determine the composition of the aerosol particles. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns, a chemical scrubber and a hydrocarbon enrichment cell. The GCMS gas inlet was heated to prevent condensation, and to evaporate volatiles from the surface after impact. The GCMS collected data from an altitude of 146 km to ground impact. The Probe and the GCMS survived impact and collected data for 1 hour and 9 minutes on the surface. Mass spectra were collected during descent and on the ground over a range of m/z from 2 to 141. The major constituents of the lower atmosphere were confirmed to be NP and CH4. The methane mole fraction was uniform in the stratosphere. It increased below the tropopause, at about 32 km altitude, monotonically toward the surface, reaching a plateau at about 8 km at a level near saturation. After surface impact a steep increase of the methane signal was observed, suggesting evaporation of surface condensed methane due to heating by the GCMS sample inlet heater. The measured mole fraction of Ar-40 is 4.3 x 10(exp-5) and of Ar-36 is 2.8 x 10(exp -7). The other primordial noble gases were below mole fraction. The isotope ratios of C-12/C-13 determined from methane measurements are 82.3 and of N-14/N-15 determined from molecular nitrogen are 183. The D/H isotope ratio determined from the H2 and HD measurements is 2.3 x l0(exp -4). Carbon dioxide, ethane, acetylene and cyanogen were detected evaporating from the surface in addition to methane.

  5. Gas chromatographic-mass spectrometric analysis of plasma oxybutynin using a deuterated internal standard.

    PubMed

    Patrick, K S; Markowitz, J S; Jarvi, E J; Straughn, A B; Meyer, M C

    1989-01-27

    A gas chromatographic-mass spectrometric method is described for the quantitative analysis of plasma oxybutynin. Deuterated oxybutynin served as the internal standard and its synthesis is described. Chromatographic separation on a methylsilicone capillary column avoided the thermal decomposition observed using a packed column. Electron-impact ionization and selected-ion monitoring of the alpha-cleavage fragments of drug and internal standard permitted quantitation of oxybutynin down to 0.25 ng/ml of plasma. At the 2 ng/ml level the accuracy and precision are 4 and 10%, respectively, and improved at higher drug concentrations. Application of the method to the pharmacokinetics of oral oxybutynin in man demonstrated rapid absorption and elimination of the drug.

  6. 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.

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

    PubMed

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

    2007-05-01

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

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

    PubMed

    Kolattukudy, P E; Dean, B B

    1974-07-01

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

  9. Gas chromatographic analysis of organic marker compounds in fine particulate matter using solid-phase microextraction.

    PubMed

    Lin, Lin; Lee, Milton L; Eatough, Delbert J

    2007-01-01

    A gas chromatographic method that uses solid-phase microextraction for analysis of organic marker compounds in fine particulate matter (PM2.5) is reported. The target marker compounds were selected for specificity toward emission from wood smoke, diesel or gasoline combustion, or meat cooking. Temperature-programmed volatilization analysis was used to characterize the thermal stabilities and volatile properties of the compounds of interest. The compounds were thermally evaporated from a quartz filter, sorbed to a solid phase microextraction (SPME) fiber, and thermally desorbed at 280 degrees C in a gas chromatograph injection port connected via a DB 1701 capillary separating column. Various experimental parameters (fiber type, time, and temperature of sorption) were optimized. It was found that high extraction yield could be achieved using a polyacrylate fiber for polar substances, such as levoglucosan, and a 7-microm polydimethylsiloxane (PDMS)-coated fiber for nonpolar compounds, such as hopanes and polyaromatic hydrocarbon. A compromise was made by selecting a carboxen/PDMS fiber, which can simultaneously extract all of the analytes of interest with moderate-to-high efficiency at 180 degrees C within a 30-min accumulation period. The optimized method was applied to the determination of levoglucosan in pine wood combustion emissions. The simplicity, rapidity, and selectivity of sample collection with a polymer-coated SPME coupled to capillary gas chromatography (GC) made this method potentially useful for atmospheric chemistry studies.

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

    PubMed

    Wu, C; Zeng, C

    1997-09-01

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

  11. 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.

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

    PubMed

    Takatsuki, K; Sakai, K

    1982-07-01

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

  13. 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

  14. Gas chromatographic/mass spectrometric analysis of morphine and codeine in human urine of poppy seed eaters.

    PubMed

    elSohly, H N; Stanford, D F; Jones, A B; elSohly, M A; Snyder, H; Pedersen, C

    1988-03-01

    In this study, poppy seeds were examined for a natural constituent that might serve as a maker for the seeds' ingestion as opposed to opiate abuse. Thebaine was selected as possible marker, since it was found to be a component of all poppy seeds examined and was not a natural component of different heroin samples. During the course of this investigation, a new extraction and cleanup procedure was developed for the gas chromatographic/nitrogen phosphorus detection (GC/NPD) and gas chromatographic/mass spectrometric (GC/MS) analysis of morphine and codeine in urine. A linear response, over a concentration range of 25 to 600 ng/mL, was obtained for codeine and morphine (r = 0.9982 and 0.9947, respectively). The minimum detectable level (LOD) and limit of quantitation (LOQ) for morphine were 10 and 30 ng/mL, respectively; whereas LOD and LOQ for codeine were 2 and 8 ng/mL, respectively. The coefficients of variance (CV, n = 6) for morphine and codeine analyses at the 100-ng/mL level were 13.3 and 4.6%, respectively. This procedure was used for the analysis of urine samples from five poppy seed eaters who each ingested 200 g of poppy seed cake. Results indicated that significant amounts of morphine and codeine are excreted in urine and that in all subjects, at least at one point in time, the apparent morphine concentration as determined by radioimmunoassay (RIA) analysis exceeded the cutoff value (300 ng/mL) established for screening. Thebaine was not detected in urine specimens collected following poppy seeds ingestion and thus could not be used as a marker.

  15. Capillary gas chromatographic assay of camphor and m-cresol in dermatological creams.

    PubMed

    Mirza, T; Tan, H S

    1998-09-01

    Camphor and m-cresol mixtures are used in antiseptic and anti-itching creams. No compendial method exists for these preparations. This paper reports a capillary gas chromatographic method using FID detection with 2,6-di-tert-butyl-4-methylphenol as internal standard on a 30 m x 0.32 mm Supelcowax -10 column (0.25 micron film) with helium as carrier gas. Ramped temperature programming was applied. The method allows simultaneous quantitation of camphor and m-cresol in the presence of o- and p-cresols, calamine and zinc oxide. Overall percent recoveries (+/- SD, n = 9) of camphor, o-, p- and m-cresol from spiked placebo creams, at a labeled amount of 10 (w/w)% were 96.9 +/- 0.6, 98.2 +/- 0.6, 99.2 +/- 0.5 and 101.0 +/- 0.9%, respectively, and at a labeled amount of 1% were 96.7 +/- 0.6, 97.8 +/- 0.9, 97.8 +/- 0.6, and 100.3 +/- 1.0%, respectively. The recovery studies were carried out at +/- 30% of the labeled amounts. Linear peak area or height ratios were obtained (r > 0.999) for camphor, o-, p- and m-cresol covering a concentration range of 10-200% of the labeled amount. Linearity (r > 0.999) was also obtained for m-cresol when the relative concentration of o- and p-cresol was varied from 5 to 100% of the m-cresol concentration. The resolution between the 'critical pair' of p- and m-cresol was > or = 1.1. The limit of quantitation was 23 pg for m-cresol and 9.3 pg for camphor using an injection split of 1:50. The repeatability (%RSD) for all compounds were < 2% for peak area and < 1.4% for peak height ratios. System suitability and robustness of the method were established. The method was successively applied to the assay of available commercial products and allows assay of camphor and the three cresol isomers.

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

    USDA-ARS?s Scientific Manuscript database

    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...

  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.

    2012-01-01

    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 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 capable of making long

  18. 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

  19. 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.

  20. Gas-liquid chromatographic determination of sulfamethazine in swine and cattle tissues.

    PubMed

    Manuel, A J; Steller, W A

    1981-07-01

    A gas-liquid chromatographic (GLC) method is described for determining sulfonamide residues in animal tissues, with specificity for 7 sulfonamides. Residues are extracted from tissues with acetone-chloroform, fatty substances are removed, and the sulfonamide residue is methylated with diazomethane in acetone-ether to render it amenable to determination by gas-liquid chromatography on an all-glass column suitable for direct on-column injection and a Ni electron-capture detector. Quantitation is achieved by external standardization. The method has a validated limit of sensitivity of 0.10 ppm with the corresponding control values for all tissues being less than 0.01 ppm. Satisfactory recoveries have been obtained for sulfamethazine in swine and cattle tissues. Specificity for sulfamethazine in the presence of sulfathiazole, sulfaquinoxaline, sulfadimethoxine, sulfabromomethazine, sulfaethoxypyridazine, and sulfachloropyrazine is attained by resolution of the respective methyl derivatives on the GLC column.

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

    PubMed

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

    1985-01-01

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

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

    PubMed Central

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

    1986-01-01

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

  3. Continuous Measurement of Multiple Gases Using Ball Surface Acoustic Wave Gas Chromatograph

    NASA Astrophysics Data System (ADS)

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

    2012-07-01

    Although portable gas chromatographs (GCs) have been developed for the monitoring of volatile organic compounds (VOCs) in working environments, they still need high power consumption for the heating column. Thus, we previously developed a portable surface acoustic wave (SAW) GC equipped with a ball SAW sensor and a micro-electromechanical-system column (ball SAW GC) and proved the usefulness of the forward flush (FF) method for realizing the fast analysis of multiple gases without a heater. However, its ability to measure ten kinds of VOCs at ppm order and automatic continuous measurement were not demonstrated. In this study, a ball SAW GC employing the FF method and equipped with a gas sampler for continuous injection was developed. Then, the performance of monitoring multiple gases in working environments was verified by measuring ten kinds of VOCs with maximum acceptable concentrations. Moreover, real-time monitoring of seven kinds of VOCs with a linear change in the response value to concentration changes was demonstrated.

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

    PubMed

    Berthou, F; Friovourt, M P

    1981-12-18

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

  5. 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.

  6. Modulation-induced error in comprehensive two-dimensional gas chromatographic separations.

    PubMed

    Harynuk, J J; Kwong, A H; Marriott, P J

    2008-07-18

    There is a fundamental difference between data collected in comprehensive two-dimensional gas chromatographic (GCxGC) separations and data collected by one-dimensional GC techniques (or heart-cut GC techniques). This difference can be ascribed to the fact that GCxGC generates multiple sub-peaks for each analyte, as opposed to other GC techniques that generate only a single chromatographic peak for each analyte. In order to calculate the total signal for the analyte, the most commonly used approach is to consider the cumulative area that results from the integration of each sub-peak. Alternately, the data may be considered using higher order techniques such as the generalized rank annihilation method (GRAM). Regardless of the approach, the potential errors are expected to be greater for trace analytes where the sub-peaks are close to the limit of detection (LOD). This error is also expected to be compounded with phase-induced error, a phenomenon foreign to the measurement of single peaks. Here these sources of error are investigated for the first time using both the traditional integration-based approach and GRAM analysis. The use of simulated data permits the sources of error to be controlled and independently evaluated in a manner not possible with real data. The results of this study show that the error introduced by the modulation process is at worst 1% for analyte signals with a base peak height of 10xLOD and either approach to quantitation is used. Errors due to phase shifting are shown to be of greater concern, especially for trace analytes with only one or two visible sub-peaks. In this case, the error could be as great as 6.4% for symmetrical peaks when a conventional integration approach is used. This is contrasted by GRAM which provides a much more precise result, at worst 1.8% and 0.6% when the modulation ratio (MR) is 1.5 or 3.0, respectively for symmetrical peaks. The data show that for analyses demanding high precision, a MR of 3 should be targeted as

  7. Solid-phase extraction with styrene-divinylbenzene sorbent for high-performance liquid or gas chromatographic determination of urinary chloro- and methylthiotriazines.

    PubMed

    Mendas, G; Drevenkar, V; Zupancic-Kralj, L

    2001-05-25

    A solid-phase extraction (SPE) procedure on a styrene-divinylbenzene (SDB-1 cartridge) for extraction and cleaning of the triazine herbicides atrazine, simazine, ametryn, and prometryn and atrazine monodealkylated metabolites from urine samples was developed and optimised for final high-performance liquid chromatographic (HPLC-UV diode array detection) and gas chromatographic (GC-electron-capture detection and GC-thermionic-sensitive detection) analyses. Interfering polar matrices were eliminated by rinsing SDB-1 with 1% acetonitrile in water or with pure water. Extraction recoveries were from 78 to 101% with an RSD of about 10% for all studied compounds. The extraction recovery for the didealkylated atrazine metabolite was significantly lower and this compound cannot be determined with these procedures. Sorbent matrix generated interferences, although not detected by the chromatographic system, lowered the response of nitrogen-phosphorus and electron-capture GC detectors for monodealkylated chlorotriazines when compared to standards prepared in n-hexane. HPLC and GC analysis with SPE (SDB-1) preconcentration showed excellent linearity over the concentration range tested, with detection limits in urine of 10 ng ml(-1) for the parent herbicides (HPLC and GC analysis) and 20 ng ml(-1) for monodealkylated chlorotriazines (HPLC analysis).

  8. 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

  9. 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

  10. Prediction of gas chromatographic retention indices based on Monte Carlo method.

    PubMed

    Veselinović, Aleksandar M; Velimorović, Dragan; Kaličanin, Biljana; Toropova, Alla; Toropov, Andrey; Veselinović, Jovana

    2017-06-01

    A new method for the prediction of retention indices using Monte Carlo method and based on local graph invariants and SMILES notation of studied compounds has been presented. Very satisfactory results were obtained with the proposed method, since robust model with good statistical quality was developed. The predictive potential of the applied approach was tested and the robustness of the model was proven with different methods. The best calculated QSPR model had following statistical parameters: r(2)=0.8097 for the training set and r(2)=0.9372 for the test set. Structural indicators defined responsible for the increases and decreases of gas chromatographic retention indices activity have been calculated. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    PubMed

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

    2013-08-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

  13. 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.

  14. Computerised gas chromatographic-mass spectrometric analysis of complex mixtures of alkyl porphyrins.

    PubMed

    Marriott, P J; Gill, J P; Evershed, R P; Hein, C S; Eglinton, G

    1984-01-01

    Computerised capillary gas chromatography-mass spectrometry (GC-MS) analysis of complex mixtures of alkyl porphyrins, as their bis-(trimethylsiloxy)silicon(IV) and bis(tert.-butyldimethylsiloxy)silicon(IV) derivatives, is described. The latter derivative is more suitable for routine GC-MS analysis. This computerised GC-MS approach, when applied to the alkyl porphyrins of two geological samples, a bitumen (Gilsonite, Eocene age, UT, U.S.A.) and a crude oil (Boscan, Cretaceous age, West Venezuela), has revealed the highly complex compositions of these fractions. Computer-aided data processing, using relative retention index (RRI) calculations, facilitated the classification of the chromatographic peaks according to structural type and membership of pseudo-homologous series. Computerised GC-MS is compared with, and contrasted to high-performance liquid chromatography as a means of petroporphyrin analysis.

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

    PubMed

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

    1988-01-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1995-01-01

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

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

    PubMed

    Legaz, M; Raisys, V A

    1976-02-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1995-01-01

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

  19. On-line overpressure thin-layer chromatographic separation and electrospray mass spectrometric detection of glycolipids.

    PubMed

    Chai, Wengang; Leteux, Christine; Lawson, Alexander M; Stoll, Mark S

    2003-01-01

    On-line thin-layer chromatographic separation and electrospray mass spectrometry (TLC/ESI-MS) has been accomplished by direct linking of a commercial overpressure TLC instrument, OPLC 50, and a Q-TOF mass spectrometer. Mass spectrometric detection sensitivity and chromatographic resolution achieved by this configuration were assessed using acidic glycolipids as examples. Under the optimized conditions, a sensitivity of 5 pmol of glycosphingolipid was readily demonstrated for TLC/ESI-MS and 20 pmol for TLC/ESI-MS/MS production scanning to derive the saccharide sequence and long chain base/fatty acid composition of the ceramide. Initial preconditioning of TLC plates is necessary to achieve high sensitivity detection by reducing chemical background noise. Plates can be used repeatedly (at least 10 times) for analysis, although this may result in a minor reduction in TLC resolution. Following solvent development, separated components on the TLC plates can be detected in the conventional way by nondestructive staining or UV absorption or fluorescence and can be stored for on-line TLC/ESI-MS analysis at a later stage without reduction in mass spectrometric detection sensitivity and chromatographic resolution. Aspects for further improvement of OPLC instrumentation include use of narrower TLC plate dimensions and refined design of the eluate exit system.

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

    PubMed

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

    2012-11-16

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

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

    NASA Astrophysics Data System (ADS)

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

    2017-03-01

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

  2. 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.

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

    PubMed

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

    2008-09-01

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

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

    PubMed

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

    2011-03-25

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

  5. A purge-and-trap capillary column gas chromatographic method for the measurement of halocarbons in water and air

    SciTech Connect

    Happell, J.D.; Wallace, D.W.R.; Wills, K.D.; Wilke, R.J.; Neill, C.C.

    1996-06-01

    This report describes an automated, accurate, precise and sensitive capillary column purge- and -trap method capable of quantifying CFC-12, CFC-11, CFC-113, CH{sub 3}CCL{sub 3}, and CCL{sub 4} during a single chromatographic analysis in either water or gas phase samples.

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

    DTIC Science & Technology

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

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

    PubMed

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

    2010-08-24

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

  8. Gas chromatographic-mass spectrometric method for the determination of the herbicides paraquat and diquat in plasma and urine samples.

    PubMed

    de Almeida, Rafael Menck; Yonamine, Mauricio

    2007-06-15

    In the present work, a method was developed and optimized aiming to determinate the herbicides paraquat (PQ) and diquat (DQ) in human plasma and urine samples. An initial procedure of chemical reduction of the analytes by adding NaBH4 directly in the buffered samples (pH 8.0) was performed. This procedure was necessary to convert the quaternary ammonium substances into more volatile compounds for gas chromatographic analysis. The reduction compounds were extracted with C18 cartridges (solid-phase extraction). Ethyl paraquat (EPQ) was used as internal standard (IS). Gas chromatography-mass spectrometry (GC-MS) was used to identify and quantify the analytes in selected ion monitoring (SIM) mode. The limits of detection were 0.05 mg/l for both PQ and DQ. By using the weighted least squares linear regression (1/x1/2 for plasma and 1/y for urine), the accuracy of the analytical method was improved at the lower end of the calibration curve (from 0.1 to 50 mg/l; r>0.98). This method can be readily utilized as an important tool to confirm the suspicion of PQ and/or DQ poisoning and evaluate the extent of the intoxication.

  9. A gas chromatographic method for the indirect determination of hydroxylamine in pharmaceutical preparations: conversion into nitrous oxide.

    PubMed

    Guzowski, J P; Golanoski, C; Montgomery, E R

    2003-12-04

    A simple, sensitive, and selective headspace gas-chromatographic method has been developed for measuring hydroxylamine (HA) in a variety of sample matrices including pharmaceutical formulations. This procedure relies on converting HA into nitrous oxide (N2O), which is a single-step reaction that is carried out directly in a heated headspace vial. The gaseous products are then analyzed by headspace capillary gas chromatography. Several detection strategies were evaluated and electron capture provided the best sensitivity (4 parts-per-billion (ppb)) while the mass selective and thermal conductivity values were higher (14 ppb and 1.4 parts-per-million (ppm), respectively). The method's linear dynamic range spans two to four decades with a run-to-run precision that was better than 5% R.S.D. (n=7). The reagent concentrations (oxidant, buffer) strongly impact the N2O signal and the greatest response was obtained for solutions that contained equimolar amounts of reactants. HA was efficiently (98%) recovered from a sample matrix that contained only the active pharmaceutical ingredient (API) but the recovery was lower (83%) when excipients were present.

  10. 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.

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

    PubMed

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

    2010-06-25

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

  12. Cucurbit[n]urils as a new class of stationary phases for gas chromatographic separations.

    PubMed

    Zhang, Pu; Qin, Shijia; Qi, Meiling; Fu, Ruonong

    2014-03-21

    Cucurbit[n]urils (CBs) possess unique structures and physicochemical properties as well as excellent thermal stability. These characteristics concur to make them good candidates for stationary phases in capillary gas chromatographic (GC) separations. Herein, CB7 and CB8 in neat (CB7, CB8) and binary (CB7-CB8) forms were investigated for this purpose. After they were statically coated onto fused silica capillary columns, the CB columns were evaluated in terms of chromatographic parameters, separation performance, thermal stability and column repeatability. The columns had efficiencies ranging from 1060 to 2200 plates per meter determined by n-dodecane at 100°C and exhibited nonpolar to weakly polar nature. These CBs columns showed good separation performance for a wide range of analytes such as n-alkanes, aromatic hydrocarbons, esters, aldehydes, ketones, alcohols and the Grob mixture, and exhibited nice peak shapes for analytes that are liable to peak-tailing in GC analysis. The results also proved the good column repeatability and thermal stability of the CB columns. No noticeable decreases in both retention times and resolution or appreciable baseline drift were observed after the columns were conditioned up to 250°C (CB8 and CB7-CB8 columns) or 280°C (CB7 column). This work demonstrates the promising future of CBs as a new class of GC stationary phase. To the best of our knowledge, this is the first report on using CB stationary phases in capillary GC separations. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. 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

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

    SciTech Connect

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

    1996-09-01

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

  15. 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.

  16. Gas chromatographic-mass spectrometric analysis of chemical volatiles in buffalo (Bubalus bubalis) urine.

    PubMed

    Barman, Purabi; Yadav, M C; Kumar, H; Meur, S K; Ghosh, S K

    2013-10-01

    Isolation of active fraction and characterization of chemosignals from urine have been attempted in several mammalian species in the recent years. The objective of this study was to identify the urinary volatiles across various reproductive stages of buffalo cow, namely, estrus, diestrus, and pregnancy, and in bull, by chemical extraction followed by gas chromatography-linked mass spectrometry (GC-MS). Urine samples were collected from six buffalo cows at two different phases of estrous cycle, namely, estrus and diestrus. Besides, urinary samples were collected from five pregnant buffalo cows (60-75 days after artificial insemination (AI)) and six adult bulls. Thin-layer chromatography was performed as a preliminary test for qualitative comparison of different compounds extracted by organic solvents. Identification of the urinary compounds was carried out in a gas chromatograph (Perkin Elmer, Autosystem XL) linked to a mass spectrometer (Turbomass). The results of GC-MS analysis indicated the presence of 21 compounds with varying molecular weights and retention time, which were further categorized as diestrus-specific, pregnancy-specific, and bull-specific urinary compounds. No compound, however, could be identified as estrus-specific. We concluded that qualitative differences do exist in estrus, diestrus, and pregnant buffalo cow urine and in bull urine, as evidenced by GC-MS. Copyright © 2013 Elsevier Inc. All rights reserved.

  17. Ethyl chloroformate as a derivatizing reagent for the gas chromatographic determination of isoniazid and hydrazine in pharmaceutical preparations.

    PubMed

    Khuhawar, Mohammad Yar; Zardari, Liaquat Ali

    2008-01-01

    Ethyl chloroformate was examined as a precolumn derivatizing reagent for the gas chromatographic (GC) determination of isoniazid (INH) and hydrazine (HZ). Phenylhydrazine (PHZ) was used as an internal standard. GC separation was carried out on an HP-5 column (30 m x 0.32 mm i.d.) with flame ionization detection. The elution was carried out at an initial column temperature of 150 degrees C for 1 min at a heating rate of 10 degrees C/min up to 250 degrees C, nitrogen flow rate of 4 ml/min and a split ratio of 10:1, v/v. The linear calibration ranges for INH and HZ were observed between 3.5-37.5 and 3.5-35 microg/ml with corresponding detection limits of 0.18 and 0.17 ng reaching the detector. The method was subsequently applied to the determination of INH and HZ in pharmaceutical preparations, achieving a relative standard deviation (RSD) of 3.8-5.8%. The recovery percentage of INH from isoniazid syrup was 98% with an RSD of 5.2%.

  18. 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

  19. Kinetics and mechanism of gas-phase thermolysis using headspace-gas chromatographic analysis.

    PubMed

    Cafferata, L F; Manzione, C J

    2001-02-01

    Headspace gas chromatography is employed in order to study the thermal decomposition reaction of gaseous di-tert-butyl peroxide (DTBP) in the 130 degrees C to 160 degrees C temperature range and in the presence of n-hexane as the internal standard and nitrogen as the carrier gas. The reaction exclusively yields acetone and ethane as products. First-order kinetics are observed, including when the surface-to-volume ratio (S/V) of the Pyrex 20-mL vial employed as the reactor is increased by packing it with silanized glass wool. However, a small increase in the rate constant values is observed at each temperature, which supports a heterogeneous surface process in DTBP decomposition. The rate constant's dependence on the homogeneous unimolecular decomposition reaction corresponds to the O-O bond rupture of the DTBP molecule in a stepwise three-stage mechanism. Thus, the relevant question of the participation of a surface catalytic effect in the DTBP gas-phase thermolysis can easily be assessed through the procedure described in this work. In general, this is advantageous for the rapid investigation of the reaction kinetics of volatile compounds at different temperatures.

  20. 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. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Gas chromatograph-surface acoustic wave for quick real-time assessment of blood/exhaled gas ratio of propofol in humans.

    PubMed

    Chen, X; Zhang, X L; Liu, L; Chen, Y; Piao, M Y; Zhang, F J; Wu, W D; Zhong, Y B; Sun, K; Zou, Y C; Zhang, X; Wang, D; Wang, P; Yan, M

    2014-11-01

    Although pilot studies have reported that exhaled propofol concentrations can reflect intraoperative plasma propofol concentrations in an individual, the blood/exhaled partial pressure ratio RBE varies between patients, and the relevant factors have not yet been clearly addressed. No efficient method has been reported for the quick evaluation of RBE and its association with inter-individual variables. We proposed a novel method that uses a surface acoustic wave (SAW) sensor combined with a fast gas chromatograph (GC) to simultaneously detect propofol concentrations in blood and exhaled gas in 28 patients who were receiving propofol i.v. A two-compartment pharmacokinetic (PK) model was established to simulate propofol concentrations in exhaled gas and blood after a bolus injection. Simulated propofol concentrations for exhaled gas and blood were used in a linear regression model to evaluate RBE. The fast GC-SAW system showed reliability and efficiency for simultaneous quantitative determination of propofol in blood (correlation coefficient R(2)=0.994, P<0.01) and exhaled gas (R(2)=0.991, P<0.01). The evaluation of RBE takes <50 min for a patient. The distribution of RBE in 28 patients showed inter-individual differences in RBE (median 1.27; inter-quartile range 1.07-1.59). Fast GC-SAW, which analyses samples in seconds, can perform both rapid monitoring of exhaled propofol concentrations and fast analysis of blood propofol concentrations. The proposed method allows early determination of the coefficient RBE in individuals. Further studies are required to quantify the distribution of RBE in a larger cohort and assess the effect of other potential factors. ChiCTR-ONC-13003291. © The Author 2014. Published by Oxford University Press on behalf of the British Journal of Anaesthesia. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  2. 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.

  3. 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

    2016-08-02

    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.

  4. 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.

  5. 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.

  6. 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.

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

    PubMed

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

    2015-12-04

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

  8. Gas Chromatographic Determination of Fatty Acids in Oils with Regard to the Assessment of Fire Hazard

    NASA Astrophysics Data System (ADS)

    Bartošová, Alica; Štefko, Tomáš

    2017-06-01

    The aim of the paper was to study and research the application of processing gas chromatographic method for the rapid and accurate determination of the composition of different types of oils, such as substances with the possibility of an adverse event spontaneous combustion or self-heating. Tendency to spontaneous combustion is chemically characterized mainly by the amount of unsaturated fatty acids, which have one or more double bonds in their molecule. Vegetable oils essentially consist of the following fatty acids: palmitic, stearic, oleic, linoleic, and linoleic. For the needs of assessment, the fire hazard must be known, in which the double bond is present, as well as their number in a molecule. As an analytical method, GCMS was used for determination of oils content. Three types of oil were used - rapeseed, sunflower, and coconut oil. Owing to the occurrence of linoleic acid C18:2 (49.8 wt.%) and oleic acid C18:1 (43.3 wt.%) with double bonds, sunflower oil is the most prone to self-heating. The coconut and rapeseed oils contain double bond FAME in lesser amount, and their propensity to self-heating is relatively low.

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

    PubMed

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

    1989-01-01

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

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

    PubMed

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

    2008-03-01

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

  11. Gas chromatographic method for analysis of 2,4-D in wheat: interlaboratory study.

    PubMed

    Smith, A E

    1984-01-01

    A procedure is described for the determination of 2,4-D (2,4-dichlorophenoxyacetic acid) in dried green plant material. Samples are first extracted with dilute sodium hydroxide, and then after acidification and solvent extraction, the residues are methylated using boron trifluoride-methanol reagent. The methyl ester of 2,4-D is cleaned up on a Florisil column and quantitated using a gas chromatograph equipped with an electron capture detector. Six laboratories made quadruplicate determinations on control, dried green wheat check samples, on 4 similar samples fortified at the 0.50 ppm level, and on 4 samples fortified at the 1.00 ppm level with 2,4-D. Based on the data from 5 laboratories, the plant fortifications of 0.50 and 1.00 ppm yielded average interlaboratory recoveries of 2,4-D of 83.3 and 88.2%, respectively. The procedure also has potential for the determination of 2,4-D in wheat straw and wheat grain.

  12. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    PubMed

    Zheng, Yunzhong; Qi, Meiling; Fu, Ruonong

    2016-07-08

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

  14. Graphitic carbon nitride nanofibers in seaweed-like architecture for gas chromatographic separations.

    PubMed

    Zheng, Yunzhong; Han, Qing; Qi, Meiling; Qu, Liangti

    2017-05-05

    Seaweed-like graphitic carbon nitride (g-C3N4) has a unique porous architecture composed of interlocking g-C3N4 nanofibers (NF-C3N4) with much higher surface area than bulk g-C3N4 and shows good potential in separation science. This work investigated the separation performance of NF-C3N4 as stationary phase for capillary gas chromatographic (GC) separations. The NF-C3N4 column exhibits weak polarity and high column efficiency of 4728 plates/m for n-dodecane. Importantly, it displays good separation performance for a wide range of analytes and shows different retention behaviors from the bulk g-C3N4 column and commercial HP-5MS column with 5% phenylpolysiloxane. Particularly, it shows high resolving capability for both aliphatic and aromatic isomers. In addition, NF-C3N4 column has high thermal stability up to 280°C and good separation repeatability with relative standard deviation (RSD) values in the range of 0.29-0.61% for intra-day, 0.56-1.1% for inter-day and 2.0-4.9% for between-column, respectively. Moreover, it was applied for the determination of isomer impurities in real samples, showing good potential in GC applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. 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. © Georg Thieme Verlag KG Stuttgart · New York.

  16. Exploring atmospheric photooxidation with a new Gas Chromatograph Time-of-Flight Chemical Ionization Mass Spectrometer (GC-ToF-CIMS)

    NASA Astrophysics Data System (ADS)

    Nölscher, A. C.; Allen, H. M.; Teng, A.; Crounse, J.; Wennberg, P. O.

    2015-12-01

    Atmospheric photooxidation is a fundamental process that effectively removes pollutants and greenhouse gases from the air we breathe. One way to explore these processes is to directly measure the stable intermediate oxidation products. Chemical Ionization Mass Spectrometry (CIMS) has proven to be a powerful tool to sensitively detect with high time resolution photooxidation products in the atmosphere such as hydroperoxides, acids, nitrates, and other oxygenated volatile organic compounds. Despite the potential to elucidate atmospheric photooxidation in detail, field observations of such compounds are sparse. Here we present the development of a new Gas Chromatograph Time-of-Flight Chemical Ionization Mass Spectrometer (GC-ToF-CIMS) for field deployment. Using low pressure gas chromatography and CF3O- ionization chemistry, the selective operation of a GC is combined with the sensitive, specific, and fast detection of a high-resolution ToF-CIMS. The combination of chromatographic separation and exact mass identification allows detecting isomer resolved photooxidation products. Direct measurements in the atmosphere of such isomer distributions are particularly interesting due to the broad range of their individual atmospheric lifetimes and impacts.

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

    PubMed

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

    1984-04-01

    Gas chromatography has found highly successful application in NASA's flight programs. Gas chromatographs have been flown to both Mars and Venus where detailed compositional measurements were made. These instruments were quite small and relatively sensitive when compared to commercially available instruments; however, they do not appear adequate for future missions currently being planned. The earlier flight GC's had incorporated thermistor bead thermal conductivity cells as the detector. This detector requires very precise temperature control and only provides about 1 ppm sensitivity. Temperature stabilization causes the detector to be quite heavy, i.e., about 200 g. Greater sensitivity will be required for measurements of trace components in extraterrestrial environments. Review of other detector types revealed the metastable ionization detector as a likely candidate because of its superior thermal stability and high sensitivity. The metastable detector, first described by Lovelock as an argon ionization detector, has been studied and somewhat modified by others. The commercial design by Hartmann and Dimick was used for comparison purposes in our work. In the past, three features of the metastable detector are prominent: it has part-per-billion sensitivity, contamination must be carefully controlled, and anomalous response is common. Since it is an ionization detector, however, temperature instabilities do not cause the major perturbations experienced by the thermal conductivity detectors. This paper describes a miniature metastable ionization detector featuring an unconventional electrode configuration, whose performance characteristics parallel those of traditional design, while its weight is quite small. The prototype has been used in our laboratories routinely for 2 years, and the concept will be incorporated into a flight GC for use in the Space Shuttle.

  18. 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. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  19. 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

  20. Gas chromatographic/mass spectrometric determination of lysergic acid diethylamide (LSD) in serum samples.

    PubMed

    Musshoff, F; Daldrup, T

    1997-08-04

    A sensitive method for the detection and quantification of lysergic acid diethylamide (LSD) in serum samples is described. After liquid-liquid extraction the trimethylsilyl derivative of LSD is detected by gas chromatography-mass spectrometry. Experiments with spiked samples resulted in a recovery of 76%, the coefficient of variation was 9.3%. Excellent linearity was obtained over the range 0.1-10 ng ml-1. Additionally experiments demonstrating the light sensitivity of LSD are presented together with casuistics.

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

    PubMed

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

    2011-08-01

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

  2. 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.

  3. Development of an Exhaled Breath Monitoring System with Semiconductive Gas Sensors, a Gas Condenser Unit, and Gas Chromatograph Columns.

    PubMed

    Itoh, Toshio; Miwa, Toshio; Tsuruta, Akihiro; Akamatsu, Takafumi; Izu, Noriya; Shin, Woosuck; Park, Jangchul; Hida, Toyoaki; Eda, Takeshi; Setoguchi, Yasuhiro

    2016-11-10

    Various volatile organic compounds (VOCs) in breath exhaled by patients with lung cancer, healthy controls, and patients with lung cancer who underwent surgery for resection of cancer were analyzed by gas condenser-equipped gas chromatography-mass spectrometry (GC/MS) for development of an exhaled breath monitoring prototype system involving metal oxide gas sensors, a gas condenser, and gas chromatography columns. The gas condenser-GC/MS analysis identified concentrations of 56 VOCs in the breath exhaled by the test population of 136 volunteers (107 patients with lung cancer and 29 controls), and selected four target VOCs, nonanal, acetoin, acetic acid, and propanoic acid, for use with the condenser, GC, and sensor-type prototype system. The prototype system analyzed exhaled breath samples from 101 volunteers (74 patients with lung cancer and 27 controls). The prototype system exhibited a level of performance similar to that of the gas condenser-GC/MS system for breath analysis.

  4. Development of an Exhaled Breath Monitoring System with Semiconductive Gas Sensors, a Gas Condenser Unit, and Gas Chromatograph Columns

    PubMed Central

    Itoh, Toshio; Miwa, Toshio; Tsuruta, Akihiro; Akamatsu, Takafumi; Izu, Noriya; Shin, Woosuck; Park, Jangchul; Hida, Toyoaki; Eda, Takeshi; Setoguchi, Yasuhiro

    2016-01-01

    Various volatile organic compounds (VOCs) in breath exhaled by patients with lung cancer, healthy controls, and patients with lung cancer who underwent surgery for resection of cancer were analyzed by gas condenser-equipped gas chromatography-mass spectrometry (GC/MS) for development of an exhaled breath monitoring prototype system involving metal oxide gas sensors, a gas condenser, and gas chromatography columns. The gas condenser-GC/MS analysis identified concentrations of 56 VOCs in the breath exhaled by the test population of 136 volunteers (107 patients with lung cancer and 29 controls), and selected four target VOCs, nonanal, acetoin, acetic acid, and propanoic acid, for use with the condenser, GC, and sensor-type prototype system. The prototype system analyzed exhaled breath samples from 101 volunteers (74 patients with lung cancer and 27 controls). The prototype system exhibited a level of performance similar to that of the gas condenser-GC/MS system for breath analysis. PMID:27834896

  5. Current Developments in Analyzing Food Volatiles by Multidimensional Gas Chromatographic Techniques.

    PubMed

    Cordero, Chiara; Schmarr, Hans-Georg; Reichenbach, Stephen E; Bicchi, Carlo

    2017-02-02

    This paper presents current developments and future perspectives on the spread of advanced analytical tasks in the field of food volatile analysis. The topics outlined comprise (a) recent advances on miniaturized sampling techniques; (b) the potential and challenges of multidimensional gas chromatography coupled with mass spectrometric detection for volatile identification and quantitation in samples with complex matrices;

  6. Optical fibre gas detections systems

    NASA Astrophysics Data System (ADS)

    Culshaw, Brian

    2016-05-01

    This tutorial review covers the principles of and prospects for fibre optic sensor technology in gas detection. Many of the potential benefits common to fibre sensor technology also apply in the context of gas sensing - notably long distance - many km - access to multiple remote measurement points; invariably intrinsic safety; access to numerous important gas species and often uniquely high levels of selectivity and/or sensitivity. Furthermore, the range of fibre sensor network architectures - single point, multiple point and distributed - enable unprecedented flexibility in system implementation. Additionally, competitive technologies and regulatory issues contribute to final application potential.

  7. Decomposition of GD on CeO2/Alumina Adsorbents in a Gas Chromatograph On-Column Injector Tube Reactor

    DTIC Science & Technology

    2006-10-01

    Perkin Elmer Auto M Gas Chromatograph and maintained at 30 0C. A Nicolet 800 Bench Spectrometer with a mercury - cadmium-telluride detector (11,700 to 600...and decomposition of liD by these groups occurs by an elimination mechanism and not substitution (hydrolysis). bThe adsorbents were rubbed across...were recorded between 4000 cm-1 and 600 cm1 as percent transmission versus wavenumber using a Nicolet 800 Bench Spectrometer equipped with a mercury

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

    PubMed

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

    2014-06-01

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

  9. Chromatographic behavior of selenoproteins in rat serum detected by inductively coupled plasma mass spectrometry.

    PubMed

    Anan, Yasumi; Hatakeyama, Yoshiko; Tokumoto, Maki; Ogra, Yasumitsu

    2013-01-01

    Two major selenoproteins are present in mammalian serum: extracellular glutathione peroxidase (eGPx) and selenoprotein P (Sel P). The chromatographic behaviors of the two serum selenoproteins were compared in four rodent species, and the selenoproteins in rat serum were identified by measuring enzyme activity and Western blotting. The selenoproteins in rat serum showed a specific chromatographic behavior. In particular, rat eGPx was eluted faster than eGPxs of the other rodent species, although the amino-acid sequences of the rodent species were identical. The elution profiles of Se in rat serum obtained by inductively coupled plasma tandem mass spectrometry (ICP-MS-MS) and ICP-MS were compared. The tandem quadrupoles and the O₂ reaction/collision gas completely removed severe interferences with the Se speciation originating from the plasma source and the biological sample matrix. ICP-MS-MS under the O₂ mass shift mode gave us more accurate abundance ratios of Se than ICP-MS.

  10. 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.

  11. Potential for aging female Aedes aegypti (Diptera: Culicidae) by gas chromatographic analysis of cuticular hydrocarbons, including a field evaluation.

    PubMed

    Desena, M L; Clark, J M; Edman, J D; Symington, S B; Scott, T W; Clark, G G; Peters, T M

    1999-11-01

    Gas chromatography with flame-ionization detection was used to measure the time-associated, quantitative changes in the cuticular hydrocarbons of female Aedes aegypti (L.). Cohorts of unstressed Ae. aegypti, Rockefeller strain, were reared and held at 3 constant temperatures (24, 28, and 30 degrees C). Five females from each cohort were taken at 33 degree-day (DD) intervals from 0 to 231 DD (using 17 degrees C as the threshold temperature). Quantitative changes over time of cuticular hydrocarbons associated with gas chromatographic peaks 1 and 5 were identified as having promise for age grading. The relative abundance of peak 1 (pentacosane) decreased linearly from 0 to 132 DD, whereas peak 5 (nonacosane) increased linearly over the same period. Suboptimal larval conditions (crowded and starved), which resulted in physiological stress (decreased size), had negligible effect on the relative abundance of pentacosane and nonacosane. Additionally, the rate of change in the relative abundance of pentacosane and nonacosane were the same for both a recently colonized Chachoengsao (Thailand) strain of Ae. aegypti compared with the long-colonized Rockefeller (Caribbean) strain over a 0-99 DD interval. Two linear regression models, one based on the relative abundance of pentacosane and the other on the logit transformation of these values, were developed for aging female Ae. aegypti. A blind study using laboratory-reared mosquitoes and a mark-release-recapture experiment using field mosquitoes validated these age-grading models and produced promising results for aging females up to 132 DD (19, 12, and 10 calendar days at 24, 28 and 30 degrees C, respectively). Therefore the regression models, based on the relative abundance of these 2 cuticular hydrocarbons, appeared to be a useful approach for age-grading Ae. aegypti up to at least 12 d of age regardless of environmental conditions (temperature and stress) and population history (origin and colonization time).

  12. [The rapid analysis of polychlorinated quaterphenyls in blood using different diameter capillary column with the high-resolution gas chromatograph high-resolution mass spectrometer].

    PubMed

    Yasutake, Daisuke; Ashizuka, Yuki; Hori, Tsuguhide; Kurokawa, Youichi; Kajiwara, Jumboku; Hirata, Teruaki; Ishiguro, Yasuhisa; Iida, Takao; Uchi, Hiroshi; Furue, Masutaka

    2011-04-01

    The polychlorinated quaterphenyl (PCQ) concentrations in blood are important discriminative parameters in yusho patient. In this study, a rapid analytical method for PCQ using different diameter capillary column (rapid-Rtx65TG) with high-resolution gas chromatograph high-resolution mass spectrometer (HRGC/HRMS) instead of the gas chromatograph electron capture detector (ECD/GC) was developed. Using different diameter capillary columns, the analysis time of the HRGC/HRMS was drastically shortened, and the detection sensitivity was improved. In the rapid-Rtx65TG column, a small-bore capillary column (length 1m, I.D. 0.1mm) was connected with the inlet side of the GC, and behind that column, a large-bore capillary column (length 15mm, I.D. 0.53mm) for octadecachloroquaterphenyl (ODCQ) analysis was connected. In the HRGC/HRMS measurement of ODCQ by the rapid-Rtx65TG column, the minimum limit of detection for the apparatus was 0.4 pg, and the minimum limit of determination for the blood was 0.008 ppb. On ECD/GC in the conventional method and HRGC/HRMS in this study, the PCQ concentration in blood including yusho patients and yusho suspected persons was almost equivalent.

  13. Ammonia Analysis by Gas Chromatograph/Infrared Detector (GC/IRD)

    NASA Technical Reports Server (NTRS)

    Scott, Joseph P.; Whitfield, Steve W.

    2003-01-01

    Methods are being developed at Marshall Space Flight Center's Toxicity Lab on a CG/IRD System that will be used to detect ammonia in low part per million (ppm) levels. These methods will allow analysis of gas samples by syringe injections. The GC is equipped with a unique cryogenic-cooled inlet system that will enable our lab to make large injections of a gas sample. Although the initial focus of the work will be analysis of ammonia, this instrument could identify other compounds on a molecular level. If proper methods can be developed, the IRD could work as a powerful addition to our offgassing capabilities.

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

    PubMed

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

    2012-08-21

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

  15. Relating gas chromatographic profiles to sensory measurements describing the end products of the Maillard reaction.

    PubMed

    Stanimirova, I; Boucon, C; Walczak, B

    2011-01-30

    Often in analytical practice, a set of samples is described by different types of measurements in the hope that a comprehensive characterisation of samples will provide a more complete picture and will help in determining the similarities among samples. The main focus is then on how to combine the information described by different measurement variables and how to analyse it simultaneously. In other words, the main goal is to find a common representation of samples that emphasises the individual and common properties of the different blocks of variables. Several methods can be adopted for the simultaneous analysis of multiblock data with a common object mode. These are: consensus principal component analysis (CPCA), SUM-PCA, multiple factor analysis (MFA) and structuration des tableaux à trois indices de la statistique (STATIS).In this article we present a comparison of the performances of these methods for data describing the chemistry and sensory profiles of the Maillard reaction products. The aroma compounds formed during the reaction of thermal heating between one or two selected amino acids and one or two reducing sugars have been analysed by head space gas chromatography and the intensity and nature of the odour of the resulting products has been evaluated according to selected descriptors by a panel of sensory experts.The results showed that using the information of the chromatographic and sensory data in conjunction enhanced the interpretability of the data. SUM-PCA and more specifically multiple factor analysis, MFA, allowed for a detailed study of the similarities of mixtures in terms of reaction products and sensory profiles. Copyright © 2010 Elsevier B.V. All rights reserved.

  16. Gas chromatographic and mass spectrometric investigations of organic residues from Roman glass unguentaria.

    PubMed

    Ribechini, Erika; Modugno, Francesca; Colombini, Maria Perla; Evershed, Richard P

    2008-03-07

    A combination of gas chromatographic (GC) and mass spectrometric (MS) techniques, including direct exposure-MS (DE-MS), high-temperature GC-MS (HTGC-MS) and GC-MS of neutral and acid fractions, was employed to study the composition and recognise origin of the organic materials used to manufacture balm residues surviving in a series of glass unguentaria recovered from excavations of a Roman villa (Villa B) in the ancient town of Oplontis (Naples, Italy). DE-MS provided comprehensive 'fingerprint' information on the solvent soluble components of the contents of the unguentaria, while GC-MS analyses provided detailed molecular compositions, highlighting the presence of a wide range of compound classes including mid- and long-chain fatty acids, long-chain hydroxy-acids, n-alkanols, alkandiols, n-alkanes, long-chain monoesters, phytosterols and diterpenoid acids. Characteristic biomarkers and their distributions indicate the presence of beeswax, Pinaceae resin and another wax, as the main organic constituents of all of the preparations examined. In particular, the occurrence of phytosterols and long-chain monoesters, in which the acyl moiety was not exclusively palmitic acid, suggested the presence of a second waxy-lipid constituent of plant origin. The results are consistent with beeswax being used in the preparation of the cosmetics preserved in the unguentaria, while the other lipids are most likely the residue of some as yet unidentified plant extract(s), possibly deriving from the cuticular waxes of flowers and/or leaves. The composition of the extracts are consistent with the ancient practices of maceration and/or "enfleurage", in which lipid-based materials, such as beeswax, animal fat or vegetables oils, were used to extract aromatic and fragrant substances from resin, flowers, spices and scented wood, in order to produce unguents and balms.

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

    PubMed

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

    2011-11-15

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

  18. 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.

  19. 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.

  20. 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

  1. Gas-chromatographic speciation of methylstannanes in the Chesapeake Bay using purge and trap sampling with a tin-selective detector

    SciTech Connect

    Jackson, J.A.A.; Blair, W.R.; Brinckman, F.E.; Iverson, W.P.

    1982-02-01

    A method was developed permitting detection and speciation of both volatile and nonvolatile organotin compounds in aqueous media. The method employed a commercial gas chromatograph (GC) with a flame photometric detector (FPD) optimized for tin-selective detection. A commercial automatic purge and trap sampler (P/T) employing a Tenax-GC filled trap concentrated the purged volatiles and species volatilized by hydridization with NaBH/sub 4/. The P/T-GC-FPD method was applied to detect varying amounts of methyltin compounds, including tetramethyltin and methyltin hydrides, in polluted sites in Baltimore Harbor. In vitro studies using GC-MS confirmed earlier reports of microbial methylation of inorganic Sn(IV) by a strain of Pseudomonas species isolated from the Chesapeake Bay. Consequently, biogenic origins are suspected for the methylstannanes (Me/sub n/SnH /sub 4-n/, n = 2,3) found in Chesapeake Bay.

  2. Improved gas chromatographic method for determination of daminozide by alkaline hydrolysis and 2-nitrobenzaldehyde derivatization and survey results of daminozide in agricultural products.

    PubMed

    Steinbrecher, K; Saxton, W L; Oehler, G A

    1990-01-01

    An improved method was developed for the quantitative determination of daminozide. This new method combines the alkaline hydrolysis and distillation steps of the PAM II method for daminozide with the derivatization, cleanup, and gas chromatographic determination steps of the Wright method for unsymmetrical dimethyl hydrazine (UDMH). The minimum detectable level is 0.05 ppm. Recoveries range from 85 to 110% when daminozide is added at 0.1 to 1.0 ppm, and are generally 40% at the 0.05 ppm level. A variety of domestic and imported products were analyzed by this improved method and daminozide was detected in 33 of the 98 samples analyzed. Levels detected ranged from a trace amount to 0.80 ppm. The identity of UDMH hydrazone was confirmed by mass spectrometry in many samples, thus confirming the presence of daminozide. Two samples containing daminozide were analyzed independently by a second laboratory and the findings were closely duplicated.

  3. Use of an acoustic wave device to detect target analytes during chromatographic separations

    SciTech Connect

    Tom-Moy, M.; Doherty, T.P.; Baer, R.L.

    1995-12-01

    Hewlett-Packard Laboratories has developed a proprietary acoustic wave device which permits the detection of specific analyte in a flowing system. By coupling specific chemistry to the surface of the device, the mass loading of the target analyte is detected as a shift in phase is measured in real time. In process monitoring, the analyte of interest is isolated by passing the sample through a series of chromatographic columns. Conventional HPLC systems monitor the protein peaks using UV-VIS. The peaks are collected and biochemical assays are performed to determine the specific peak of interest. We have configured our acoustic sensors to make specific chemical measurements without the use of labeled reagents or enzymes to generate a real time signal of specific analyte as it elutes from the column. The output signal can be integrated over time to yield a concentration. Such a detector has the potential to increase productivity in process chromatography in biopharmaceutical applications.

  4. Liquid chromatographic determination of amprolium in chicken tissues, using post-column reaction and fluorometric detection.

    PubMed

    Nagata, T; Saeki, M

    1986-01-01

    A method is presented for determination of amprolium residues in chicken muscles by a liquid chromatographic post-column reaction system. The drug is extracted from muscles with methanol, and the extract is concentrated to 3-4 mL. This aqueous solution is rinsed with n-hexane and cleaned up by alumina column chromatography. The drug is separated from the interferences on a LiChrosorb RP-8 column, reacted with ferricyanide in alkaline solution, and quantitated by fluorometric detection at 367 nm (excitation) and 470 nm (emission). Recoveries of amprolium added to chicken muscles at levels of 0.1 and 0.2 ppm were 74.9 and 80.9%, respectively. The detection limit was 1 ng for amprolium standard and 0.01 ppm in chicken muscles.

  5. The determination of the flour improver potassium bromate in bread by gas chromatographic and ICP-MS methods.

    PubMed

    Dennis, M J; Burrell, A; Mathieson, K; Willetts, P; Massey, R C

    1994-01-01

    The development and application of two methods for determining bromate in bread are described. A gas chromatographic (GC) method which relied on the formation of a volatile derivative of bromate gave a detection limit of 12 micrograms/kg. Duplicate analyses agreed well but recovery from breads spiked with bromate were low and averaged 30% for brown bread and 42% for white bread. Further studies indicated that this was caused by the derivatization reaction being suppressed by components of the sample and reagents used in their preparation. After taking both these factors into account, a recovery of 80% could be achieved. The GC method was used to carry out a survey of retail bread samples in 1989. Bromate was found in all six unwrapped breads analysed (median 35 micrograms/kg, range 17-317 micrograms/kg), whilst for 22 wrapped breads, seven were found to contain bromate (median < 12 micrograms/kg, range < 12-238 micrograms/kg). A second method of analysis employing inductively coupled plasma-mass spectrometry (ICP-MS) was developed which provided independent confirmation of the presence of bromate in these retail samples. The method gave a mean recovery of 71% from five spiked samples and a detection limit of 20 micrograms/kg. The GC and ICP-MS methods were compared by performing replicate analyses of a bread sample prepared with bromate-treated flour. Quantitative agreement between the two techniques was good. The precision of the ICP-MS technique (CV 12%) proved better than that found for the GC method (CV 18%). The Potassium Bromate (Prohibition as a Flour Improver) Regulation 1990 came into force on 1 April 1990 (Statutory Instrument 1990 Number 399).(ABSTRACT TRUNCATED AT 250 WORDS)

  6. 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.

  7. Fuzzy C-means clustering for chromatographic fingerprints analysis: A gas chromatography-mass spectrometry case study.

    PubMed

    Parastar, Hadi; Bazrafshan, Alisina

    2016-03-18

    Fuzzy C-means clustering (FCM) is proposed as a promising method for the clustering of chromatographic fingerprints of complex samples, such as essential oils. As an example, secondary metabolites of 14 citrus leaves samples are extracted and analyzed by gas chromatography-mass spectrometry (GC-MS). The obtained chromatographic fingerprints are divided to desired number of chromatographic regions. Owing to the fact that chromatographic problems, such as elution time shift and peak overlap can significantly affect the clustering results, therefore, each chromatographic region is analyzed using multivariate curve resolution-alternating least squares (MCR-ALS) to address these problems. Then, the resolved elution profiles are used to make a new data matrix based on peak areas of pure components to cluster by FCM. The FCM clustering parameters (i.e., fuzziness coefficient and number of cluster) are optimized by two different methods of partial least squares (PLS) as a conventional method and minimization of FCM objective function as our new idea. The results showed that minimization of FCM objective function is an easier and better way to optimize FCM clustering parameters. Then, the optimized FCM clustering algorithm is used to cluster samples and variables to figure out the similarities and dissimilarities among samples and to find discriminant secondary metabolites in each cluster (chemotype). Finally, the FCM clustering results are compared with those of principal component analysis (PCA), hierarchical cluster analysis (HCA) and Kohonon maps. The results confirmed the outperformance of FCM over the frequently used clustering algorithms. Copyright © 2016 Elsevier B.V. All rights reserved.

  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. Simultaneous gas chromatographic determination of dibutyltin and tributyltin compounds in biological and sediment samples

    SciTech Connect

    Tsuda, T.; Nakanishi, H.; Morita, T.; Takebayashi, J.

    1986-11-01

    A method is described for the simultaneous determination of nanogram amounts of dibutyltin and tributyltin compounds in biological and sediment samples. These compounds are converted to the corresponding chlorides with HCl, extracted with ethyl acetate-hexane (3 + 2) for biological samples and with hexane for sediment samples, and hydrogenated with sodium borohydride. The corresponding hydrides, Bu2SnH2 and Bu3SnH, are detected by electron-capture gas chromatography after cleanup by silica gel column chromatography. Detection limits are 1.0-2.0 and 0.5-1.0 ng/g, respectively, for biological and sediment samples.

  10. Determination of triazine and chloroacetanilide herbicides in soils by microwave-assisted extraction (MAE) coupled to gas chromatographic analysis with either GC-NPD or GC-MS.

    PubMed

    Vryzas, Zisis; Papadopoulou-Mourkidou, Euphemia

    2002-08-28

    A simple and rapid method based on microwave-assisted extraction (MAE) coupled to gas chromatographic analysis was developed for the analysis of triazine (atrazine, cyanazine, metribuzine, simazine and deethylatrazine, and deisopropylatrazine) and chloroacetanilide (acetochlor, alachlor, and metolachlor) herbicide residues in soils. Soil samples are processed by MAE for 5 min at 80 degrees C in the presence of acetonitrile (20 mL/sample). Mean recovery values of most solutes are >80% in the 10 to 500 microg/kg fortification range with respective RSDs (relative standard deviations) < 20%. The limits of quantification (LOQ) and limits of detection (LOD) are 10 and 1 to 5 microg/kg, respectively. The method was validated with two types of soils containing 1.5 and 3.0% organic matter content, respectively; no statistically significant differences were found between solute recovery values from the two types of soils. The solute mean recovery values from freshly spiked (24 h aging) and spiked samples stored refrigerated for one week before processed were also not statistically different. Residue levels determined in field weathered soils were higher when soils were processed by MAE than with a comparison method based on flask-shaking of soil suspensions overnight. Extracts were analyzed by a gas chromatographic system equipped either with a thermionic (GC-NPD) or a mass spectrometric detector (GC-MS).

  11. 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.

  12. Rapid differentiation of the major causative agents of bacterial meningitis by use of frequency-pulsed electron capture gas-liquid chromatograph: analysis of acids.

    PubMed

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

    1980-01-01

    The major causative agents of bacterial meningitis, Haemophilus influenzae serogroup B, Neisseria meningitidis serogroups B and C, Klebsiella pneumoniae, Streptococcus pneumoniae, and two types of Escherichia coli, were cultured in a modified chemically defined Catlin medium and in a commercial version of the unmodified Catlin medium. The spent media were extracted under acidic conditions, and electron-capturing derivatives were prepared by derivatization with trichloroethanol or haptafluorobutyric anhydride. The derivatives were analyzed on a gas chromatograph equipped with a frequency-pulsed electron capture detector and a PEP-2 computer. The data obtained from the study show that these organisms can be easily distinguished from each other on the basis of metabolic products detected in either type of medium. Three different metabolic groups were detected within two serogroups of N. meningitidis. The methods are practical, and the new technique should offer clinical laboratories and hospitals a better method for rapid identification of this important group of pathogens.

  13. A low thermal mass fast gas chromatograph and its implementation in fast gas chromatography mass spectrometry with supersonic molecular beams.

    PubMed

    Fialkov, Alexander B; Moragn, Mati; Amirav, Aviv

    2011-12-30

    A new type of low thermal mass (LTM) fast gas chromatograph (GC) was designed and operated in combination with gas chromatography mass spectrometry (GC-MS) with supersonic molecular beams (SMB), including GC-MS-MS with SMB, thereby providing a novel combination with unique capabilities. The LTM fast GC is based on a short capillary column inserted inside a stainless steel tube that is resistively heated. It is located and mounted outside the standard GC oven on its available top detector port, while the capillary column is connected as usual to the standard GC injector and supersonic molecular beam interface transfer line. This new type of fast GC-MS with SMB enables less than 1 min full range temperature programming and cooling down analysis cycle time. The operation of the fast GC-MS with SMB was explored and 1 min full analysis cycle time of a mixture of 16 hydrocarbons in the C(10)H(22) up to C(44)H(90) range was achieved. The use of 35 mL/min high column flow rate enabled the elution of C(44)H(90) in less than 45 s while the SMB interface enabled splitless acceptance of this high flow rate and the provision of dominant molecular ions. A novel compound 9-benzylazidanthracene was analyzed for its purity and a synthetic chemistry process was monitored for the optimization of the chemical reaction yield. Biodiesel was analyzed in jet fuel (by both GC-MS and GC-MS-MS) in under 1 min as 5 ppm fatty acid methyl esters. Authentic iprodion and cypermethrin pesticides were analyzed in grapes extract in both full scan mode and fast GC-MS-MS mode in under 1 min cycle time and explosive mixture including TATP, TNT and RDX was analyzed in under 1 min combined with exhibiting dominant molecular ion for TATP. Fast GC-MS with SMB is based on trading GC separation for speed of analysis while enhancing the separation power of the MS via the enhancement of the molecular ion in the electron ionization of cold molecules in the SMB. This paper further discusses several features of

  14. Liquid chromatographic determination of amprolium in poultry feed and premixes using postcolumn chemistry with fluorometric detection.

    PubMed

    Vanderslice, J T; Huang, M H

    1987-01-01

    Two extraction and liquid chromatographic procedures are presented which separate amprolium from compounds in poultry feed or premixes that could interfere with its fluorometric determination. The procedures are based on earlier work on the determination of thiamine in food samples. Amprolium is extracted from feed with a hexane-aqueous sulfosalicylic acid mix, separated on a C18 column, and detected fluorometrically after postcolumn derivatization. For premixes, water extraction is used. Values for the amprolium content of poultry feed obtained with these procedures are in good agreement with those obtained with AOAC official methods. It is suggested that these methods with suitable modifications may be of use for routine analysis of amprolium in feeds. The overall methods are rapid and appear to give reasonable results.

  15. 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.

  16. 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.

  17. Chromatographic separation and detection of target analytes from complex samples using inkjet printed SERS substrates.

    PubMed

    Yu, Wei W; White, Ian M

    2013-07-07

    In principle, surface enhanced Raman spectroscopy (SERS) is thought to provide unique identification of a target analyte, even in complex samples or in the presence of multiple analytes. In practice, however, this is not always true for real-world samples due to various forms of interference. In this report, we build upon our previous work on inkjet-printed SERS substrates by using paper and polymer membranes to integrate sample cleanup and analyte separation with SERS detection. Inkjet-printed paper SERS substrates provide a highly sensitive chemical detection platform of unprecedented cost and simplicity. In addition, paper inherently provides unique capabilities, such as capillary-actuated fluid transport and selective molecular retention. Utilizing these properties, we demonstrate two-dimensional chromatographic separation and SERS detection on inkjet-printed paper SERS substrates. Then, we leverage the separation properties of paper and polymer membranes for real applications that feature complex sample matrices, including the detection of down to 5 ppm melamine in infant formula, as well as the quantification of nanograms of heroin in samples contaminated with a highly fluorescent background. The results presented here demonstrate that inkjet-printed paper SERS devices not only provide advantages in terms of sensitivity and cost, but the paper provides inherently integrated sample cleanup capabilities that are not available in traditional SERS substrates and microfluidic SERS devices. These unique capabilities of paper SERS devices enable the identification of targeted analytes even in complex real-world samples.

  18. High-performance liquid chromatographic assay for mitoxantrone in plasma using electrochemical detection.

    PubMed

    Choi, K E; Sinkule, J A; Han, D S; McGrath, S C; Daly, K M; Larson, R A

    1987-09-04

    A sensitive and specific high-performance liquid chromatographic (HPLC) assay was developed for the quantitation of mitoxantrone in plasma using electrochemical detection. Bisantrene was chosen as the internal standard. A reversed-phase, 10-microns muBondapak C18 analytical column (30 cm X 3.9 mm) with an isocratic mobile phase of 28% acetonitrile in 80 mM sodium formate buffer (pH 3.0) was used. The eluent was monitored by both electrochemical detection at an applied potential of +0.75 V vs. Ag/AgCl and visible absorbance at 660 nm. Only electrochemical detection was able to quantitate the internal standard and provided ten times higher sensitivity than visible absorbance for mitoxantrone with a detection limit as low as 0.1 ng/ml. Calibration curves in the range 0.1-1000 ng/ml showed good linearity (r = 0.998) and precision (coefficient of variation less than 10%). This HPLC method utilized a reproducible and inexpensive liquid-liquid extraction procedure. Using methylene chloride, the extraction efficacy of mitoxantrone from plasma was 85.3% with a coefficient of variation less than 2.1%. This new assay was then applied to measure mitoxantrone concentrations in plasma obtained from two leukemic patients receiving 12 mg/m2 mitoxantrone as a 1-h infusion.

  19. 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.

  20. 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.

  1. Gas chromatographic-mass spectrometric determination of macrolide antibiotics in beef and pork using single ion monitoring.

    PubMed

    Takatsuki, K; Ushizawa, I; Shoji, T

    1987-03-27

    A gas chromatographic-mass spectrometric (GC-MS) method using single ion monitoring (SIM) is described for the determination of residual macrolide antibiotics, oleandomycin, kitasamycin, spiramycin and tylosin, in beef and pork. For GC-MS determination, oleandomycin is acid hydrolysed to desoleandomycin and acetylated, in the same way as erythromycin. However, for elution from a GC column, the carbon-carbon double bonds in the antibiotics must be hydrogenated to single bonds before acid hydrolysis. Kitasamycin and spiramycin are therefore converted into hydroforocidine acetate and tylosin into hydro-O-mycaminosyl tylonolide acetate, which are determined by GC-MS with SIM.

  2. Multiresidue method for the gas chromatographic determination of pesticides in honey after solid-phase extraction cleanup.

    PubMed

    Jansson, C

    2000-01-01

    A new multiresidue method is described for the determination of pesticides in honey. The method involves dissolution of the honey in a methanol-water mixture, followed by solid-phase extraction cleanup and gas chromatographic determination. Twenty-six pesticides used on flowering field crops, on flowering fruit and vegetables, or as acaricides to control Varroa jacobsoni in beehives are determined by the method. Recoveries from honey, spiked at 0.02-1.6 mg/kg, ranged from 85 to 127% with a relative standard deviation (RSD) of 2-16%, except for the RSD of 27% for captan at 0.05 mg/kg.

  3. 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.

  4. 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.

  5. Control of propranolol intake by direct chromatographic detection of alpha-naphthoxylactic acid in urine.

    PubMed

    Ruiz-Angel, M J; Fernández-López, P; Murillo-Pulgarín, J A; García-Alvarez-Coque, M C

    2002-02-15

    A rapid chromatographic procedure with a C18 column, a mobile phase of 0.15 M sodium dodecyl sulfate (SDS)-10% (v/v) 1-propanol at pH 3 (0.01 M phosphate buffer), and fluorimetric detection, is reported for the control of propranolol (PPL) intake in urine samples, which are injected directly without any other treatment than filtration. The peak of PPL was only observed in samples taken a few hours after ingestion of the drug due to its extensive conjugation and metabolisation. The detection of several unconjugated PPL metabolites was therefore considered: desisopropylpropranolol (DIP), propranolol glycol (PPG), alpha-naphthoxylactic acid (NLT) and alpha-naphthoxyacetic acid (NAC). NLT showed the best characteristics: it eluted at a much shorter retention time than PPL, its concentration in urine samples was greater and it did not present any interference from endogeneous compounds in urine, common drugs or drugs administered in combination with PPL. The limit of quantification, measured as the concentration of analyte providing a relative standard deviation of 20%, was 24 ng/ml, and the day-to-day imprecision was below 4% for concentrations above 200 ng/ml. The procedure allows the routine control of PPL at therapeutic urine levels. Urinary excretion studies showed that the detection of NLT is possible at least up to 20-30 h after oral administration.

  6. 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.

  7. Validated gas chromatographic-negative ion chemical ionization mass spectrometric method for delta(9)-tetrahydrocannabinol in sweat patches.

    PubMed

    Saito, Takeshi; Wtsadik, Abraham; Scheidweiler, Karl B; Fortner, Neil; Takeichi, Sanae; Huestis, Marilyn A

    2004-11-01

    A sensitive gas chromatography-negative ion chemical ionization mass spectrometry (GC/MS-NICI) method was developed and validated for the measurement of Delta(9)-tetrahydrocannabinol (THC) in human sweat patches. THC-d(0) and THC-d(3) were added to worn blank sweat patches (PharmChek; PharmChem Incorporated) and extracted with 3 mL of methanol-0.2 mol/L sodium acetate buffer (pH 5.0, 3:1 by volume) on a reciprocating shaker at ambient temperature for 30 min. Extracted solution (2 mL) was diluted with 8 mL of 0.1 mol/L sodium acetate buffer (pH 4.5) and extracted by use of solid-phase extraction columns (CleanScreen; United Chemical Technologies). Dried extracts were derivatized with trifluoroacetic acid and analyzed with an Agilent 6890 gas chromatograph interfaced with an Agilent 5973 mass selective detector operated in NICI-selected ion-monitoring mode. The lower limits of detection and quantification for THC in human sweat were 0.2 and 0.4 ng/patch, respectively. The calibration curve was linear from 0.4 to 10 ng/patch (R(2) >0.995). Overall recovery of THC from blank worn patches to which 0.6, 4.0, and 8.0 ng of THC had been added was 44-46%. Assay imprecision, expressed as CV, was <10% for 0.6, 4.0, and 8.0 ng/patch quality-control samples. Twenty-one potential interfering compounds (50 ng/patch) added to low quality-control samples (0.6 ng/patch) did not influence THC quantification. This GC/MS-NICI assay for THC in human sweat provides adequate sensitivity and performance characteristics for analyzing THC in sweat patches and meets the requirements of the proposed Substance Abuse and Mental Health Administration's guidelines for sweat testing.

  8. Hybrid preconcentrator/focuser module for determinations of explosive marker compounds with a micro-scale gas chromatograph.

    PubMed

    Serrano, Gustavo; Sukaew, Thitiporn; Zellers, Edward T

    2013-03-01

    This article describes the development and characterization of a partially selective preconcentrator/focuser (PCF) module for a field-portable micro-scale gas chromatograph (μGC) designed to rapidly determine trace levels of two vapor-phase markers of the explosive trinitrotoluene (TNT): 2,3-dimethyl-2,3-dinitrobutane (DMNB) and 2,4-dinitrotoluene (2,4-DNT). The PCF module has three primary components. The first is a high-volume sampler, comprising a resistively-heated 6-cm long stainless steel tube packed with tandem beds of the graphitized carbons Carbopack B (C-B, 30 mg) and Carbopack Y (C-Y, 15 mg), which traps the markers but permits more volatile interferences to pass through largely unretained. The second component is a microfocuser (μF), comprising a 4.2×9.8 mm Si chip containing a deep-reactive-ion-etched (DRIE) cavity packed with 2mg of C-B, a Pyrex cap, integrated heaters, and etched fluidic channels. The third component is a commercial polymer-membrane filter used as a pre-trap to remove particles and adsorbed low volatility interferences. Markers captured in the sampler are thermally desorbed and transferred to the μF, and then thermally desorbed/injected from the μF into a downstream separation (micro)column and detected. Scrubbed ambient air is used as carrier gas. The adsorbent capacities, baseline temperatures, sampling and desorption flow rates, and heating profiles were optimized for each PCF module component while minimizing the analysis time. An overall transfer efficiency of 86% was achieved at marker concentrations of ~0.2-2.6 ppb. In the final configuration the PCF module requires just 60s to collect a 1-L sample (3 L/min), focus (40 mL/min), and inject the markers (3 mL/min), producing half-maximum injection peak widths of ~2 and 5 s, and preconcentration factors of 4500 and 1800, for DMNB and 2,4-DNT, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. 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.

  10. Classification of gasoline by octane number and light gas condensate fractions by origin with using dielectric or gas-chromatographic data and chemometrics tools.

    PubMed

    Rudnev, Vasiliy A; Boichenko, Alexander P; Karnozhytskiy, Pavel V

    2011-05-15

    The approach for classification of gasoline by octane number and light gas condensate fractions by origin with using dielectric permeability data has been proposed and compared with classification of same samples on the basis of gas-chromatographic data. The precision of dielectric permeability measurements was investigated by using ANOVA. The relative standard deviation of dielectric permeability was in the range from 0.3 to 0.5% for the range of dielectric permeability from 1.8 to 4.4. The application of exploratory chemometrics tools (cluster analysis and principal component analysis) allow to explicitly differentiate the gasoline and light gas condensate fractions into groups of samples related to specific octane number or origin. The neural networks allow to perfectly classifying the gasoline and light gas condensate fractions.

  11. Paper-based chromatographic chemiluminescence chip for the detection of dichlorvos in vegetables.

    PubMed

    Liu, Wei; Kou, Juan; Xing, Huizhong; Li, Baoxin

    2014-02-15

    Paper chromatography was a big breakthrough in the early of 20th century but it is rarely used due to the long separation time and the diffusion on the sample spots. In this work, for the first time, a paper-based chemiluminescence (CL) analytical device combined with paper chromatography was developed for the determination of dichlorvos (DDV) in vegetables without complicated sample pretreatment. The paper chromatography separation procedure can be accomplished in 12 min on a paper support (0.8 × 7.0 cm(2)) by using 5 µL sample spotted on it. After sample developing, the detection area (0.8 × 1.0 cm(2)) was cut and inserted between two layers of water-impermeable single-sided adhesive tapes. The paper-based chip was made by attaching the middle layer of paper onto the bottom layer. Then it was covered by another tape layer, which was patterned by the cutting method to form a square hole (0.8 × 1.0 cm(2)) in it. 10 μL mixed solution of luminol and H2O2 was dropped on the detection area to produce CL. A linear relationship was obtained between the CL intensity and the concentrations of DDV in the range between 10.0 ng mL(-1) and 1.0 μg mL(-1)and the detection limit was 3.6 ng mL(-1). Water-soluble metal ions and vitamins can be developed at different spatial locations relative to DDV, eliminating interference with DDV during detection. The paper-based chromatographic chip can be successfully used for the determination of DDV without complicated sample preparation in vegetables. This study should, therefore, be suitable for rapid and sensitive detection of trace levels of organophosphate pesticides in environmental and food samples.

  12. Gas chromatographic determination of polycyclic aromatic hydrocarbons in water and smoked rice samples after solid-phase microextraction using multiwalled carbon nanotube loaded hollow fiber.

    PubMed

    Matin, Amir Abbas; Biparva, Pourya; Gheshlaghi, Mohammad

    2014-12-29

    A novel solid-phase microextraction fiber was prepared based on multiwalled carbon nanotubes (MWCNTs) loaded on hollow fiber membrane pores. Stainless steel wire was used as unbreakable support. The major advantages of the proposed fiber are its (a) high reproducibility due to the uniform structure of the hollow fiber membranes, (b) high extraction capacity related to the porous structure of the hollow fiber and outstanding adsorptive characteristics of MWCNTs. The proposed fiber was applied for the microextraction of five representative polycyclic aromatic hydrocarbons (PAHs) from aqueous media (river and hubble-bubble water) and smoked rice samples followed by gas chromatographic determination. Analytical merits of the method, including high correlation coefficients [(0.9963-0.9992) and (0.9982-0.9999)] and low detection limits [(9.0-13.0ngL(-1)) and (40.0-150.0ngkg(-1))] for water and rice samples, respectively, made the proposed method suitable for the ultra-trace determination of PAHs.

  13. Development of Packed Column for Surface Acoustic Wave Gas Chromatograph Using Anodically Bonded Silicon-Glass Structure with a Compression Jacket

    NASA Astrophysics Data System (ADS)

    Yamamoto, Yutaro; Akao, Shingo; Sakuma, Masanori; Kobari, Kentaro; Noguchi, Kazuhiro; Nakaso, Noritaka; Tsuji, Toshihiro; Yamanaka, Kazushi

    2009-07-01

    Gas or liquid chromatographs (GC/LCs) are frequently used for multiple-compound sensing, but they are too large and heavy to be portable. To provide a handy GC/LC, many groups have proposed micro GC/LCs in which large columns are replaced by small micro-electro-mechanical-system (MEMS) columns. However, because of the high packing pressure, a packed MEMS column using an anodically bonded structure has not been realized so far. In this study, we realized such a MEMS column for the first time by introducing a compression jacket to reduce the tensile stress at the silicon-glass boundary. Consequently we succeeded in the separation and detection of lower hydrocarbons using a ball surface acoustic wave sensor.

  14. Measurement of dissolved H2, O2, and CO2 in groundwater using passive samplers for gas chromatographic analyses.

    PubMed

    Spalding, B P; Watson, D B

    2006-12-15

    A simple in-situ passive dissolved gas groundwater sampler, comprised of a short length of silicone tubing attached to a gastight or other syringe, was adapted and tested for in-situ collection of equilibrium gas samples. Sampler retrieval after several days of immersion in groundwater allowed the direct injection of the sample onto a gas chromatograph (GC), simplifying field collection and sample handling over the commonly used "bubble stripping" method for H2 analyses. A GC was modified by sequencing a thermal conductivity (TC) detector followed by a reductive gas (RG) detector so that linear calibration of H2 over the range 0.2-200,000 ppmv was attained using a 0.5-mL gas sample; inclusion of the TC detector allowed the simultaneous quantification of other fixed gases (O2, CO2, He, and Ne) to which the RG detector was not responsive. Uptake kinetics for H2 and He indicated that the passive sampler reached equilibrium within 12 h of immersion in water. Field testing of these passive samplers revealed unusually large equilibrium gas-phase H2 concentrations in groundwater, ranging from 0.1 to 13.9%, by volume, in 11 monitoring wells surrounding four former radiological wastewater disposal ponds at the Y-12 plant in Oak Ridge, Tennessee.

  15. 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

    2015-09-09

    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.

  16. Gas chromatographic-mass spectrometric determination of plasma saturated fatty acids using pentafluorophenyldimethylsilyl derivatization.

    PubMed

    Yang, Y J; Choi, M H; Paik, M J; Yoon, H R; Chung, B C

    2000-05-26

    An improved method for the detection of 11 saturated fatty acids (SFAs) including C12:0-C26:0 (even numbers only), C17:0, C19:0 and C23:0 in human plasma by gas chromatography-mass spectrometry (GC-MS) with a stable isotope internal standard as d3-stearic acid is described. This procedure was based on acidic treatment, liquid-liquid extraction, and chemical derivatization prior to instrumental analysis. Eleven pentafluorophenyldimethylsilyl-SFA derivatives were well separated without any interfering peaks in plasma samples. The characteristic ions at M-15, constituting the base peaks in the electron impact mass spectra for 11 SFAs, permitted their sensitive detection by GC-MS in the selected ion monitoring (SIM) mode. The SIM responses were linear with correlation coefficients varying from 0.993 to 0.999 in the concentration range of 0.05 to approximately 50 microg/ml for the 11 SFAs. The detection limits for SIM of the SFAs varied in the range of 0.05 to approximately 10.0 pg. When applied to the plasma samples of normal subjects and patients with X-linked adenoleukodystrophy, which is one of the hereditary peroxisomal disorders, the present method enabled us to determine the SFAs with good sensitivity and good overall precision and accuracy within the concentration ranges of 0.14 to approximately 82.35 micromol/l.

  17. 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%.

  18. 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.

  19. 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.

  20. 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.

  1. Gas chromatographic-mass spectrometric determination of adipate-based polymeric plasticizers in foods.

    PubMed

    Castle, L; Mercer, A J; Gilbert, J

    1988-01-01

    A method for the quantitative determination of adipate-based polymeric plasticizers in foods is described. The procedure involves extraction from the food and transmethylation of the polymeric plasticizer to form dimethyladipate (DMA). The derivative is cleaned up by size-exclusion chromatography and determined by capillary gas chromatography-mass spectrometry with selected ion monitoring. The use of a deuterated internal standard at the extraction stage enables quantitation by stable isotope dilution. A detection limit of 0.1 mg/kg of the polymeric plasticizer in foods and a relative standard deviation of 4% have been achieved routinely. The method has been applied successfully to the analysis of cheese, sandwiches, meat, biscuits, and cake that have been in contact with polymeric plasticized poly(vinyl chloride) films.

  2. Thermal desorption-Gas chromatographic methodology for the determination of residual solvents in mesoporous silica.

    PubMed

    Asfaw, Adissu Alemayehu; Wolfs, Kris; Schepdael, Ann Van; Adams, Erwin

    2017-06-02

    In this work, thermal desorption-gas chromatography-flame ionization detection (TD-GC-FID) was adapted to enable the determination of residual solvents (RS) in mesoporous silica (MPSi). MPSi is often utilized in various pharmaceutical formulations or drug delivery systems and the accurate determination of RS is an important part of pharmaceutical quality control. Seven commonly used solvents (methanol, ethanol, acetone, isopropanol, dichloromethane, tetrahydrofuran and hexafluoroisopropanol) were evaluated in combination with 3 types of MPSi having pore sizes of 2-3, 15 and 25nm. Validation results showed general recovery values >98% and good linearity over the concentration ranges studied. The limits of detection (LOD) and limits of quantification (LOQ) for the different solvents ranged from 0.03 to 0.08μg and from 0.1 to 0.2μg per tube, respectively. Verification of the accuracy of the TD method was investigated by using an alternative method based on complete dissolution of MPSi in hydrofluoric acid (HF) followed by full evaporation headspace-GC (HS-GC). The results obtained from both procedures were not statistically different (p>0.05) when applied to actual experimental drug samples consisting of itraconazole loaded on MPSi. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. 33 CFR 127.1203 - Gas detection.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 33 Navigation and Navigable Waters 2 2010-07-01 2010-07-01 false Gas detection. 127.1203 Section 127.1203 Navigation and Navigable Waters COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED... Waterfront Facilities Handling Liquefied Hazardous Gas Equipment § 127.1203 Gas detection. (a) Each...

  4. 33 CFR 127.1203 - Gas detection.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 33 Navigation and Navigable Waters 2 2012-07-01 2012-07-01 false Gas detection. 127.1203 Section 127.1203 Navigation and Navigable Waters COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED... Waterfront Facilities Handling Liquefied Hazardous Gas Equipment § 127.1203 Gas detection. (a) Each...

  5. 33 CFR 127.1203 - Gas detection.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 33 Navigation and Navigable Waters 2 2011-07-01 2011-07-01 false Gas detection. 127.1203 Section 127.1203 Navigation and Navigable Waters COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED... Waterfront Facilities Handling Liquefied Hazardous Gas Equipment § 127.1203 Gas detection. (a) Each...

  6. 33 CFR 127.1203 - Gas detection.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 33 Navigation and Navigable Waters 2 2013-07-01 2013-07-01 false Gas detection. 127.1203 Section 127.1203 Navigation and Navigable Waters COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED... Waterfront Facilities Handling Liquefied Hazardous Gas Equipment § 127.1203 Gas detection. (a) Each...

  7. 33 CFR 127.1203 - Gas detection.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 33 Navigation and Navigable Waters 2 2014-07-01 2014-07-01 false Gas detection. 127.1203 Section 127.1203 Navigation and Navigable Waters COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED... Waterfront Facilities Handling Liquefied Hazardous Gas Equipment § 127.1203 Gas detection. (a) Each...

  8. Gas chromatographic metabolic profiling: a sensitive tool for functional microbial ecology.

    PubMed

    Coucheney, Elsa; Daniell, Tim J; Chenu, Claire; Nunan, Naoise

    2008-12-01

    Microbial metabolomics, which consists of a non-targeted analysis of the metabolites released from ('exometabolome') or existing in ('endometabolome') a cell has mostly been used to study the metabolism of particular microbes. Metabolomes also represent a picture of microbial activity and we suggest that the exometabolome may also contain pertinent information for studying microbial interaction networks. Gas chromatography coupled to mass spectrometry is the most commonly used technique in metabolomics studies. It allows a wide range of metabolites to be detected but requires the derivatisation of compounds prior to detection. This type of non-targeted analysis can introduce biases to the detection and quantification of the different metabolites, particularly at the extraction and derivatisation steps. The aims of this study, therefore, were to quantify the sources of variability and to test the sensitivity of the GC metabolic profiling approach to small environmental changes such as shifts in temperature. The temperature sensitivity of metabolic profiles was compared with that of catabolic profiles obtained using Biolog microplates. Analytical variability was compared with biological variability by incubating bacterial strains isolated from soil with fructose at 20 degrees C and by replicating each step of the protocol (incubation, extraction and derivatisation). For both the endo- and the exometabolome, more than 70% of the total variability was of biological origin and principal components analysis clearly separated the strains along the first ordination axis. The endometabolome distinguished bacterial strains at the species level only, whereas separation was evident at the species and group level with the exometabolome. Temperature had a significant but differential effect on the metabolite production of the bacterial strains whilst their catabolic profiles remained relatively unaffected. The exometabolome was more sensitive to temperature shifts than the

  9. Ion chromatographic determination of perchlorate in foods by on-line enrichment and suppressed conductivity detection.

    PubMed

    Niemann, Richard A; Krynitsky, Alexander J; Nortrup, David A

    2006-02-22

    Systemic uptake of perchlorate anion, a rocket fuel component and potential thyroid function disruptor, by leafy vegetables and other crops grown in contaminated waters is a public health concern. A column-switching anion-exchange chromatographic method with suppressed conductivity detection, described in this paper, achieved a 3-6 microg/kg method limit of quantitation in analysis of the wet weight edible portion of cantaloupe, carrots, lettuce, and spinach samples with field-incurred perchlorate. A test portion was blended with dilute nitric acid, and the extract was filtered under vacuum. A portion of the measured filtrate was acidified to pH approximately 2 by addition of cation-exchange resin, 4 mL was passed through a graphitized carbon cleanup column, and an aliquot of a collected fraction was pushed through a short precolumn for anion extraction, enrichment, and injection onto the analytical column. Statistical comparison with determination by tandem mass spectrometry-ion chromatography analysis of untreated filtrate revealed that the difference between means was not significant at the 95% confidence level (P value > or = 0.12) for crops tested. In addition, the method was applied to cooked vegetables processed as baby food.

  10. Chromatographic tandam mass spectrometric detection of papaverine and its major metabolites in rat urine

    NASA Astrophysics Data System (ADS)

    Peng, Zhihong; Song, Wei; Han, Fengmei; Chen, Huaixia; Zhu, Mingming; Chen, Yong

    2007-10-01

    A rapid, sensitive and specific liquid chromatographic-electrospray ionization (ESI) tandem ion trap mass spectrometric method has been developed for identification of papaverine and its metabolites in rat urine. Six healthy rats were administrated a single dose (100 mg/kg) of papaverine by oral gavage. The urine were sampled for 0-24 h and purified by using a C18 solid-phase extraction cartridge, then the purified urine samples were separated on a reversed-phase C18 column using methanol/2 mmol/L ammonium acetate (70:30, v/v, adjusted to pH 3.5 with formic acid) as mobile phase and detected by an on-line MS detector. Identification and structural elucidation of the metabolites were performed by comparing their changes in molecular mass ([Delta]m) and full scan MSn spectra with those of the parent drug. The results indicated that there were 14 metabolites in rat urine, such as de-methoxyl, hydroxyl, glucuronide and sulfate conjugated metabolites and so on. All these metabolites were reported for the first time.

  11. 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.

  12. Development of a switchable multidimensional/comprehensive two-dimensional gas chromatographic analytical system.

    PubMed

    Maikhunthod, Bussayarat; Morrison, Paul D; Small, Darryl M; Marriott, Philip J

    2010-02-26

    In this study, a new system for analysis using a dual comprehensive two-dimensional gas chromatography/targeted multidimensional gas chromatography (switchable GC x GC/targeted MDGC) analysis was developed. The configuration of this system not only permits the independent operation of GC, GC x GC and targeted MDGC analyses in separate analyses, but also allows the mode to be switched from GC x GC to targeted MDGC any number of times through a single analysis. By incorporating a Deans switch microfluidics transfer module prior to a cryotrapping device, the flow stream from the first dimension column can be directed to either one of two second dimension columns in a classical heart-cutting operation. Both second columns pass through the cryotrap to allow solute bands to be focused and then rapidly remobilized to the respective second columns. A short second column enables GC x GC operation, whilst a longer column is used for targeted MDGC. Validation of the system was performed using a standard mixture of compounds relevant to essential oil analysis, and then using compounds present at different abundances in lavender essential oil. Reproducibility of retention times and peak area responses demonstrated that there was negligible variation in the system over the course of multiple heart-cuts, and proved the reliable operation of the system. An application of the system to lavender oil, as a more complex sample, was carried out to affirm system feasibility, and demonstrate the ability of the system to target multiple components in the oil. The system was proposed to be useful for study of aroma-impact compounds where GC x GC can be incorporated with MDGC to permit precise identification of aroma-active compounds, where heart-cut multidimensional GC-olfactometry detection (MDGC-O) is a more appropriate technology for odour assessment.

  13. Modified ion source triple quadrupole mass spectrometer gas chromatograph for polycyclic aromatic hydrocarbon analyses

    PubMed Central

    Anderson, Kim A.; Szelewski, Michael J.; Wilson, Glenn; Quimby, Bruce D.; Hoffman, Peter D.

    2015-01-01

    We describe modified gas chromatography electron-impact/triple-quadrupole mass spectrometry (GC–EI/MS/MS) utilizing a newly developed hydrogen-injected self-cleaning ion source and modified 9 mm extractor lens. This instrument, with optimized parameters, achieves quantitative separation of 62 polycyclic aromatic hydrocarbons (PAHs). Existing methods historically limited rigorous identification and quantification to a small subset, such as the 16 PAHs the US EPA has defined as priority pollutants. Without the critical source and extractor lens modifications, the off-the-shelf GC–EI/MS/MS system was unsuitable for complex PAH analysis. Separations were enhanced by increased gas flow, a complex GC temperature profile incorporating multiple isothermal periods, specific ramp rates, and a PAH-optimized column. Typical determinations with our refined GC–EI/MS/MS have a large linear range of 1–10,000 pg μl−1 and detection limits of <2 pg μl−1. Included in the 62 PAHs, multiple-reaction-monitoring (MRM) mode enabled GC-EI/MS/MS identification and quantitation of several constituents of the MW 302 PAHs isomers. Using calibration standards, values determined were within 5% of true values over many months. Standard curve r2 values were typically >0.998, exceptional for compounds which are archetypally difficult. With this method benzo[a]fluorene, benzo[b]fluorene, benzo[c]fluorene were fully separated as was benzo[b]fluoranthene, benzo[k]fluoranthene, and benzo[j]fluoranthene. Chrysene and triphenylene, were sufficiently separated to allow accurate quantitation. Mean limits of detection (LODs) across all PAHs were 1.02 ± 0.84 pg μl−1 with indeno[1,2,3-c,d] pyrene having the lowest LOD at 0.26 pg μl−1 and only two analytes above 2.0 pg μl−1; acenaphthalene (2.33 pg μl−1) and dibenzo[a,e]pyrene (6.44 pg μl−1). PMID:26454790

  14. Modified ion source triple quadrupole mass spectrometer gas chromatograph for polycyclic aromatic hydrocarbon analyses.

    PubMed

    Anderson, Kim A; Szelewski, Michael J; Wilson, Glenn; Quimby, Bruce D; Hoffman, Peter D

    2015-11-06

    We describe modified gas chromatography electron-impact/triple-quadrupole mass spectrometry (GC-EI/MS/MS) utilizing a newly developed hydrogen-injected self-cleaning ion source and modified 9mm extractor lens. This instrument, with optimized parameters, achieves quantitative separation of 62 polycyclic aromatic hydrocarbons (PAHs). Existing methods historically limited rigorous identification and quantification to a small subset, such as the 16 PAHs the US EPA has defined as priority pollutants. Without the critical source and extractor lens modifications, the off-the-shelf GC-EI/MS/MS system was unsuitable for complex PAH analysis. Separations were enhanced by increased gas flow, a complex GC temperature profile incorporating multiple isothermal periods, specific ramp rates, and a PAH-optimized column. Typical determinations with our refined GC-EI/MS/MS have a large linear range of 1-10,000pgμl(-1) and detection limits of <2pgμl(-1). Included in the 62 PAHs, multiple-reaction-monitoring (MRM) mode enabled GC-EI/MS/MS identification and quantitation of several constituents of the MW 302 PAH isomers. Using calibration standards, values determined were within 5% of true values over many months. Standard curve r(2) values were typically >0.998, exceptional for compounds which are archetypally difficult. With this method benzo[a]fluorene, benzo[b]fluorene, benzo[c]fluorene were fully separated as was benzo[b]fluoranthene, benzo[k]fluoranthene, and benzo[j]fluoranthene. Chrysene and triphenylene, were sufficiently separated to allow accurate quantitation. Mean limits of detection (LODs) across all PAHs were 1.02±0.84pgμl(-1) with indeno[1,2,3-c,d] pyrene having the lowest LOD at 0.26pgμl(-1) and only two analytes above 2.0pgμl(-1); acenaphthalene (2.33pgμl(-1)) and dibenzo[a,e]pyrene (6.44pgμl(-1)). Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Evaluation of poly(90% biscyanopropyl/10% cyanopropylphenyl siloxane) capillary columns for the gas chromatographic quantification of trans fatty acids in non-hydrogenated vegetable oils.

    PubMed

    Delmonte, Pierluigi

    2016-08-19

    Current gas chromatographic (GC) methods for the analysis of fatty acids (FA) were optimized primarily for the quantification of the trans 18:1 FAs (18:1 tFAs) produced during the partial hydrogenation of fats and oils. Recent regulatory action regarding the application of partial hydrogenation in the processing of edible fats and oils may reshape the FA composition of these products. The higher content in 18:3 tFAs compared to 18:1 tFAs of most refined non-hydrogenated vegetable oils (RNHVO), and the challenge in their quantification applying current methods, suggest the need for new methodologies. This manuscript describes a simple GC method for the analysis of FAs in RNHVOs utilizing a 100m (0.25mm I.D.) capillary column coated with poly(90% biscyanopropyl/10% cyanopropylphenyl siloxane) (90% BCS). The optimization of the chromatographic conditions and the detection of co-eluting compounds were carried out by applying comprehensive two dimensional gas chromatography with online reduction (GC-OR×GC). Results showed that 90% BCS capillary columns operated at the elution temperature of 162°C provide the separation of the 18:1, 18:2 and 18:3 tFAs, contained in RNHVOs, from other components. A minor constituent of Canola oil, 16:3n-3, partially co-eluted with trans-18:1 FAMEs. This simple GC method showed the ability to measure trans-fat in RNHVOs at the level of 0.5g/100g, providing comparable quantitative results to the more complex GC×GC methodology.

  16. Prototype of the gas chromatograph-mass spectrometer to investigate volatile species in the lunar soil for the Luna-Resurs mission

    NASA Astrophysics Data System (ADS)

    Hofer, L.; Wurz, P.; Buch, A.; Cabane, M.; Coll, P.; Coscia, D.; Gerasimov, M.; Lasi, D.; Sapgir, A.; Szopa, C.; Tulej, M.

    2015-06-01

    In preparation for the Russian Luna-Resurs mission we combined our compact time-of-flight mass spectrometer (TOF-MS) with a chemical pre-separation of the species by gas chromatography (GC). Coupled measurements with both instruments were successfully performed with the prototype of the mass spectrometer and a flight-like gas chromatograph. The system was tested with two test gas mixtures, a mixture of hydrocarbons and a mixture of noble gases. Due to its capability to record mass spectra over the full mass range at once with high sensitivity and a dynamic range of up to 106 within 1 s, the TOF-MS system is a valuable extension of the GC analytical system. Based on the measurements with calibration gases performed with the combined GC-MS prototype and under assumption of mean characteristics for the Moon's regolith, the detection limit for volatile species in a soil sample is estimated to 2·10-10 by mass for hydrocarbons and 2·10-9 by mass for noble gases.

  17. Capillary gas chromatographic determination of prometryn and its degradation products in parsley.

    PubMed

    Bardalaye, P C; Wheeler, W B

    1985-01-01

    Residue analysis of the herbicide prometryn (2,4-bis(isopropylamino)-6-methylthio-1,3,5-triazine) is widely known, but an analytical method for determining its metabolities or degradation products in addition to the parent chemical has not yet been reported in the literature. The procedure reported here is for the extraction and determination of prometryn and 2 metabolites, 2-amino-4-isopropylamino-6-methyl-thio-1,3,5-triazine and 2,4-diamino-6-methylthio-1,3,5-triazine, in parsley. Crops were extracted with 2-propanol followed by concentration of the extract and partitioning with a minimum amount of hexane in the presence of a large excess of water to remove most of the green pigment. The aqueous phase was divided into 2 equal halves: (A) One-half portion was partitioned with dichloromethane in the presence of saturated sodium chloride solution, the dichloromethane phase was separated, and the aqueous phase was discarded. The organic solvent was evaporated, and the contents were reconstituted in petroleum ether before prometryn analysis. (B) The other half was made slightly alkaline with ammonium hydroxide solution and was partitioned with ethyl acetate in the presence of saturated sodium chloride solution. The ethyl acetate phase was concentrated, centrifuged to remove any turbidity, and analyzed for the 2 metabolities above. Fused silica capillary gas chromatography (GC) with nitrogen-phosphorus (N-P) detection was used for quantitation. The limit of detection was 0.05 mg/kg for all the compounds examined. Recoveries from fortified parsley samples ranged from 59 to 73% at fortification levels of 0.05 to 1.0 mg/kg.

  18. Detection of Gas Slugs in Heat Pipes

    NASA Technical Reports Server (NTRS)

    Jones, J. A.

    1985-01-01

    Temperature sensing system detects presence of gas slugs in heat pipes. System designed for operation between zero and 70 degrees C and detects noncondensable pockets of gas that result from decomposition of ammonia cooling fluid. Slugs 1 in. (25mm) in length detected.

  19. 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.

  20. 46 CFR 154.1345 - Gas detection.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 46 Shipping 5 2013-10-01 2013-10-01 false Gas detection. 154.1345 Section 154.1345 Shipping COAST... § 154.1345 Gas detection. (a) Each vessel carrying a cargo that is designated with an “I” or “I and T” in Table 4 must have: (1) A fixed flammable gas detection system that meets § 154.1350; and (2) Two...

  1. 46 CFR 154.1345 - Gas detection.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 46 Shipping 5 2011-10-01 2011-10-01 false Gas detection. 154.1345 Section 154.1345 Shipping COAST... § 154.1345 Gas detection. (a) Each vessel carrying a cargo that is designated with an “I” or “I and T” in Table 4 must have: (1) A fixed flammable gas detection system that meets § 154.1350; and (2) Two...

  2. 46 CFR 154.1345 - Gas detection.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 46 Shipping 5 2014-10-01 2014-10-01 false Gas detection. 154.1345 Section 154.1345 Shipping COAST... § 154.1345 Gas detection. (a) Each vessel carrying a cargo that is designated with an “I” or “I and T” in Table 4 must have: (1) A fixed flammable gas detection system that meets § 154.1350; and (2) Two...

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

    PubMed

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

    2015-07-24

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

  4. Ambient Atmospheric Hydrocarbon Content as Determined by Gas Chromatographic Techniques from Rural Tidewater Virginia in Late Spring 1974

    NASA Technical Reports Server (NTRS)

    Copeland, G. E.; Davis, R.; Maroulis, P.; Bandy, A. R.; Denyszyn, R.; Kindle, E. C.

    1975-01-01

    In an attempt to ascertain the naturally generated hydrocarbon contribution to the air quality of the Hampton Roads region of Tidewater Virginia, a series of 27 air samples was obtained in two rural locations during late spring of 1974. These samples were analyzed for their hydrocarbon content (carbon number range C5 to C10) using gas chromatographic techniques. The thirty different hydrocarbon species were identified and monitored in the experiment. Preliminary analysis of the data indicates an average concentration of 397 parts per billion by weight (carbon) for the total non-methane hydrocarbon loading for C5 to C10 during the experiment. This value exceeds the National Primary Air Quality Standards as set by the Environmental Protection Agency.

  5. Analysis of sulfur-organic compounds in jet fuel by chromatographic sniffing and gas chromatography with atomic emission detector

    SciTech Connect

    Skoog, P.A.

    1995-04-01

    When the Swedish Air Force changed fuel from Jet B to Jet A-1 during 1991-1992, a working environmental problem was reported from the military air force bases. The symptoms were unpleasant odor, headache and indisposition. This problem arose from some batches of the new fuel, Jet A-1. In order to investigate the compounds in the fuel which gave rise to this problem a chromatographic sniffing technique (sensory analysis) was used. The identification of the compounds from the sniffing analysis was done with a atomic emission detector for gas chromatography. The problem stemmed from relatively volatile sulfur-organic compounds. An interesting question is if these compounds also are strongly involved in the fuel system deposit formation. This presentation shows this new analysis technique and the complex pattern of sulfur-organic compounds related to fuels from different refinery processes.

  6. Detection and identification of bacteria by gas chromatography.

    PubMed

    Henis, Y; Gould, J R; Alexander, M

    1966-07-01

    Ether extracts of cultures of 29 strains representing 6 species of Bacillus, and of individual strains of Escherichia coli, Aerobacter aerogenes, and Pseudomonas aeruginosa were examined in a gas chromatograph by use of flame ionization and electron capture detectors. Among the products detected were compounds with the chromatographic characteristics of acetic, propionic, and butyric acids, ethyl alcohol, diacetyl, acetoin, and 2,3-butanediol. The differences in peak areas of the various products formed by the bacteria were determined statistically for the chromatograms obtained with the two detectors, and the peaks were arranged in order of decreasing areas to yield a signature for each bacterial strain. Different signatures were obtained for the various genera and species and for strains of the same species. B. licheniformis, B. subtilis, and A. aerogenes formed significant quantities of a number of volatile compounds, and qualitative and quantitative differences between strains were noted. The electron capture detector was particularly sensitive to diacetyl and acetoin as well as to unknown compounds. By use of this detector, the presence of 5 pg of diacetyl and 20 pg of acetoin could be demonstrated. The quantity of acetoin detected in B. subtilis and B. licheniformis cultures was present in as little as 6.3 x 10(-3) muliters of medium.

  7. In-line gas chromatographic apparatus for measuring the hydrophobic micropore volume (HMV) and contaminant transformation in mineral micropores.

    PubMed

    Cheng, Hefa; Reinhard, Martin

    2010-07-15

    Desorption of hydrophobic organic compounds from micropores is characteristically slow compared to surface adsorption and partitioning. The slow-desorbing mass of a hydrophobic probe molecule can be used to calculate the hydrophobic micropore volume (HMV) of microporous solids. A gas chromatographic apparatus is described that allows characterization of the sorbed mass with respect to the desorption rate. The method is demonstrated using a dealuminated zeolite and an aquifer sand as the model and reference sorbents, respectively, and trichloroethylene (TCE) as the probe molecule. A glass column packed with the microporous sorbent is coupled directly to a gas chromatograph that is equipped with flame ionization and electron capture detectors. Sorption and desorption of TCE on the sorbent was measured by sampling the influent and effluent of the column using a combination of switching and injection valves. For geosorbents, the HMV is quantified based on Gurvitsch's rule from the mass of TCE desorbed at a rate that is characteristic for micropores. Instrumental requirements, design considerations, hardware details, detector calibration, performance, and data analysis are discussed along with applications. The method is novel and complements traditional vacuum gravimetric and piezometric techniques, which quantify the total pore volume under vacuum conditions. The HMV is more relevant than the total micropore volume for predicting the fate and transport of organic contaminants in the subsurface. Sorption in hydrophobic micropores strongly impacts the mobility of organic contaminants, and their chemical and biological transformations. The apparatus can serve as a tool for characterizing microporous solids and investigating contaminant-solid interactions. 2010 Elsevier B.V. All rights reserved.

  8. Integration of gas chromatographs into the Federal Highway Administration/Environmental Protection Agency near road MSAT study in Las Vegas, NV

    EPA Science Inventory

    This paper documents the technical evaluation of a semi-continuous gas chromatograph (GC) for the measurement of benzene and 1,33butadiene in the near road environment. This paper will also consider the some of the non-technical implications associated with the operation of a GC ...

  9. Evaluation of a gas chromatograph with a novel surface acoustic wave detector (SAW GC) for screening of volatile organic compounds in Hanford waste tank samples

    SciTech Connect

    Lockrem, L.L.

    1998-01-12

    A novel instrument, a gas chromatograph with a Surface Acoustic Wave Detector (SAW GC), was evaluated for the screening of organic compounds in Hanford tank headspace vapors. Calibration data were developed for the most common organic compounds, and the accuracy and precision were measured with a certified standard. The instrument was tested with headspace samples collected from seven Hanford waste tanks.

  10. Integration of gas chromatographs into the Federal Highway Administration/Environmental Protection Agency near road MSAT study in Las Vegas, NV

    EPA Science Inventory

    This paper documents the technical evaluation of a semi-continuous gas chromatograph (GC) for the measurement of benzene and 1,33butadiene in the near road environment. This paper will also consider the some of the non-technical implications associated with the operation of a GC ...

  11. Gas chromatography with diode array detection in series with flame ionisation detection.

    PubMed

    Gras, Ronda; Luong, Jim; Shellie, Robert A

    2017-06-02

    We introduce a gas chromatography detection approach that uses diode array detection operated in series with flame ionisation detection and demonstrate the utility of the detection approach for determination of volatile organic compounds. Diode array detection brings ultraviolet - visible spectroscopy (over a range of 190-640nm) onto the capillary gas chromatography time-scale, where average peak widths of analytes are on the order of 3-5s. The non-destructive nature of the diode array detector affords serially-coupled flame ionisation detection. This arrangement delivers near-simultaneous selective and universal detection without incurring additional analytical time, and without recourse to column flow splitting. The hyphenated technique is shown to be effective for chromatographic applications spanning an equivalent volatility range from C1 to C7n-paraffin hydrocarbons. The approach introduced herein provides increased sensitivity and selectivity for classes of compounds amenable to electronic spectroscopy such as alkenes, dienes, sulfurs, and aromatic compounds. The approach is demonstrated for direct measurement of carbon disulfide in work place atmospheres with a detection limit of 93pg on column and for the direct measurement of 1,3-butadiene in hydrocarbon matrices and ambient air with a detection of 73pg on column, each in less than 5min. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. A water extraction, static headspace sampling, gas chromatographic method to determine MTBE in heating oil and diesel fuel.

    PubMed

    Cummins, T M; Robbins, G A; Henebry, B J; Goad, C R; Gilbert, E J; Miller, M E; Stuart, J D

    2001-03-15

    A method was developed to determine the fuel/water partition coefficient (KMTBE) of methyl tert-butyl ether (MTBE) and then used to determine low parts per million concentrations of MTBE in samples of heating oil and diesel fuel. A special capillary column designed for the separation of MTBE and to prevent coelution and a gas chromatograph equipped with a photoionization detector (PID) were used. MTBE was partitioned from fuel samples into water during an equilibration step. The water samples were then analyzed for MTBE using static headspace sampling followed by GC/PID. A mathematical relationship was derived that allowed a KMTBE value to be calculated by utilizing the fuel/water volume ratios and the corresponding PID signal. KMTBE values were found to range linearly from 3.8 to 10.9 over a temperature range of 5-40 degrees C. This analysis method gave a MDL of 0.7 ppm MTBE in the fuel and a relative average accuracy of +/-15% by comparison with an independent laboratory using purge and trap GC/ MS analysis. MTBE was found in home heating oil in residential tanks and in diesel fuel at service stations throughout the state of Connecticut. The levels of MTBE were found to vary significantly with time. Heating oil and diesel fuel from terminals were also found to contain MTBE. This research suggests thatthe reported widespread contamination of groundwater with MTBE may also be due to heating oil and diesel fuel releases to the environment. used extensively for the past 20 years as a gasoline additive (up to 15 wt %) to reduce automobile carbon monoxide and hydrocarbon emissions. The fact that MTBE is highly soluble in water (approximately 5 wt %) (3) and chemically inert when compared to other fuel constituents causes it to be often detected at high concentrations in groundwater in the vicinity of gasoline spills. The EPA has reported that low levels of MTBE in drinking water (above 40 microg/L) may cause unpleasant taste and odors and has designated MTBE as a

  13. Aging and analytical performances evolution of a gas chromatographic system at Mars

    NASA Astrophysics Data System (ADS)

    Bonnet, J.-Y.; Szopa, C.; Millan, M.; Coscia, D.; Cabane, M.; Belmahdi, I.; Buch, A.; Dequaire, T.; Coll, P.; Teinturier, S.; Mahaffy, P.

    2015-10-01

    Health data from the gas chromatography (GC) module onboard the SAM instrument [1] will be presented to assess the analytical performances evolution of a GC device in Martian environment through 3 years.

  14. Gas Chromatographic Determination of Methyl Salicylate in Rubbing Alcohol: An Experiment Employing Standard Addition.

    ERIC Educational Resources Information Center

    Van Atta, Robert E.; Van Atta, R. Lewis

    1980-01-01

    Provides a gas chromatography experiment that exercises the quantitative technique of standard addition to the analysis for a minor component, methyl salicylate, in a commercial product, "wintergreen rubbing alcohol." (CS)

  15. Gas Chromatographic Determination of Methyl Salicylate in Rubbing Alcohol: An Experiment Employing Standard Addition.

    ERIC Educational Resources Information Center

    Van Atta, Robert E.; Van Atta, R. Lewis

    1980-01-01

    Provides a gas chromatography experiment that exercises the quantitative technique of standard addition to the analysis for a minor component, methyl salicylate, in a commercial product, "wintergreen rubbing alcohol." (CS)

  16. Development and validation of a stability-indicating gas chromatographic method for quality control of residual solvents in blonanserin: a novel atypical antipsychotic agent.

    PubMed

    Peng, Ming; Liu, Jin; Lu, Dan; Yang, Yong-Jian

    2012-09-01

    Blonanserin is a novel atypical antipsychotic agent for the treatment of schizophrenia. Ethyl alcohol, isopropyl alcohol and toluene are utilized in the synthesis route of this bulk drug. A new validated gas chromatographic (GC) method for the simultaneous determination of residual solvents in blonanserin is described in this paper. Blonanserin was dissolved in N, N-dimethylformamide to make a sample solution that was directly injected into a DB-624 column. A postrun oven temperature at 240°C for approximately 2 h after the analysis cycle was performed to wash out blonanserin residue in the GC column. Quantitation was performed by external standard analyses and the validation was carried out according to International Conference on Harmonization validation guidelines Q2A and Q2B. The method was shown to be specific (no interference in the blank solution), linear (correlation coefficients ≥0.99998, n = 10), accurate (average recoveries between 94.1 and 101.7%), precise (intra-day and inter-day precision ≤2.6%), sensitive (limit of detection ≤0.2 ng, and limit of quantitation ≤0.7 ng), robust (small variations of carrier gas flow, initial oven temperature, temperature ramping rate, injector and detector temperatures did not significantly affect the system suitability test parameters and peak areas) and stable (reference standard and sample solutions were stable over 48 h). This extensively validated method is ready to be used for the quality control of blonanserin.

  17. Quantification of Biogenic and Anthropogenic Hydrocarbons using a Commercial Gas Chromatograph - Ion Trap Mass Spectrometer at a Ground Site near Fort McKay, AB

    NASA Astrophysics Data System (ADS)

    Tokarek, T. W.; Osthoff, H. D.

    2014-12-01

    The extraction of fossil fuels from the Alberta oil sands has been the focus of considerable attention due to its association with sizeable emissions of a variety of atmospheric pollutants, the magnitude and impacts of which are currently poorly constrained by observations. In order to more reliably estimate the magnitude and impact of these emissions, an intensive air quality measurement campaign, called "Fort McMurray Oil Sands Strategic Investigation of Local Sources" (FOSSILS), was conducted in the summer of 2013 as part of the Alberta-Canada joint oil sands monitoring program (JOSM) to identify and quantify emissions and their transformations from the Alberta oil sands. The challenge is that the region is surrounded by boreal forest, which provides a substantial background of biogenic hydrocarbons during summer. In this presentation, measurements of volatile organic compounds (VOCs) at the AMS13 ground site near Fort McKay, Alberta, from Aug 17 to Sept 6, 2013 using a commercial Griffin 450 gas chromatograph equipped with ion trap mass spectrometric detection and Tenax preconcentration are described. The combination of retention information and electron impact mass spectral data allowed unambiguous identification and quantification of the major biogenic monoterpenes, e.g., α and β-pinene, limonene, camphene, and 3Δ-carene, and of many anthropogenically derived hydrocarbons. Mixing ratios of biogenic hydrocarbons varied with time of day, temperature, and solar radiation, with maxima typically occurring at night, rationalized by nocturnal mixing heights and low mixing ratios of the nocturnal oxidants ozone (O3) and the nitrate radical (NO3). In contrast, mixing ratios of anthropogenic VOCs, e.g., benzene, toluene, ethyl benzene, and o-, p-, and m-xylene (BTEX), strongly depended on meteorological conditions, i.e., local wind direction. During episodes with high BTEX abundance, many additional high molecular weight hydrocarbons were observed which were not

  18. Use of a modified Tenax GC column packing for the direct gas chromatographic analysis of phenols in water at the ppm level.

    PubMed

    Bartle, K D; Elstub, J; Novotny, M; Robinson, R J

    1977-05-21

    Dilute solutions of phenols in water at the ppm level may be analysed gas chromatographically by direct injection onto a column with a packing similar to that used in the Viking 1975 spacecraft: Tenax GC (2,6-diphenyl-p-phenylene oxide polymer) modified with polymetaphenyl ether liquid phase to eradicate irreversible adsorption. Symmetrical peaks were observed for injections of less than 1 ng of phenol and some of its alkylated derivatives. Chromatographic properties of modified Tenax GC columns are reported along with their application to the analysis of some industrial effluents with previous work-up.

  19. On-line gas chromatographic analysis of Fischer-Tropsch synthesis products formed in a supercritical reaction medium

    SciTech Connect

    Snavely, K.; Subramaniam, B.

    1997-10-01

    C{sub 1}-C{sub 30} products from Fischer-Tropsch synthesis, conducted in a supercritical n-hexane medium over an Fe catalyst in a fixed-bed reactor, are analyzed using on-line gas chromatography. A Hewlett-Packard 5890 Series II gas chromatograph (GC) is modified to minimize the effects of condensation of the on-line sample in the transfer lines. The GC is configured with a Supelco Petrocol DH capillary column connected to a flame ionization detector (FID) and two 1.83 m {times} 3.18 mm stainless steel columns placed in series, packed with 80/100 mesh HayeSep D, connected to a thermal conductivity detector (TCD). It is shown that pressure and temperature affect the elution order of oxygenates relative to hydrocarbons in the nonpolar capillary column. This phenomenon is exploited for obtaining improved resolution; several distinct methods produce similar elution orders. Ar, added to the syngas feed, is used to calculate syngas conversion. All compounds eluting before hexane (C{sub 1}-C{sub 5}, other than 2-methylpropene/1-butene and propanal/propanone) and nearly all the major peaks eluting after hexane are resolved in the capillary column. H{sub 2}, Ar, CO, CH{sub 4}, CO{sub 2}, and H{sub 2}O are resolved in the packed columns. The method provides excellent quantitative measurement of component mole fractions that are within the range of calibration.

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

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.

    1986-01-01

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

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

    PubMed

    Fleet, B; Risby, T H

    1969-07-01

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

  2. Gas Chromatographic Verification of a Mathematical Model: Product Distribution Following Methanolysis Reactions.

    ERIC Educational Resources Information Center

    Lam, R. B.; And Others

    1983-01-01

    Investigated application of binomial statistics to equilibrium distribution of ester systems by employing gas chromatography to verify the mathematical model used. Discusses model development and experimental techniques, indicating the model enables a straightforward extension to symmetrical polyfunctional esters and presents a mathematical basis…

  3. Theory and use of the pseudophase model in gas-liquid chromatographic enantiomeric separations.

    PubMed

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

    2006-01-01

    The theory and use of the "three-phase" model in enantioselective gas-liquid chromatography utilizing a methylated cyclodextrin/polysiloxane stationary phase is presented for the first time. Equations are derived that account for all three partition equilibria in the system, including partitioning between the gas mobile phase and both stationary-phase components and the analyte equilibrium between the polysiloxane and cyclodextrin pseudophase. The separation of the retention contributions from the achiral and chiral parts of the stationary phase can be easily accomplished. Also, it allows the direct examination of the two contributions to enantioselctivity, i.e., that which occurs completely in the liquid stationary phase versus the direct transfer of the chiral analyte in the gas phase to the dissolved chiral selector. Six compounds were studied to verify the model: 1-phenylethanol, alpha-ionone, 3-methyl-1-indanone, o-(chloromethyl)phenyl sulfoxide, o-(bromomethyl)phenyl sulfoxide, and ethyl p-tolylsulfonate. Generally, the cyclodextrin component of the stationary phase contributes to retention more than the bulk liquid polysiloxane. This may be an important requirement for effective GC chiral stationary phases. In addition, the roles of enthalpy and entropy toward enantiorecognition by this stationary phase were examined. While enantiomeric differences in both enthalpy and entropy provide chiral discrimination, the contribution of entropy appears to be more significant in this regard. The three-phase model may be applied to any gas-liquid chromatography stationary phase involving a pseudophase.

  4. Gas Chromatographic Verification of a Mathematical Model: Product Distribution Following Methanolysis Reactions.

    ERIC Educational Resources Information Center

    Lam, R. B.; And Others

    1983-01-01

    Investigated application of binomial statistics to equilibrium distribution of ester systems by employing gas chromatography to verify the mathematical model used. Discusses model development and experimental techniques, indicating the model enables a straightforward extension to symmetrical polyfunctional esters and presents a mathematical basis…

  5. Detection and quantification of affinity ligand leaching and specific antibody fragment concentration within chromatographic fractions using surface plasmon resonance.

    PubMed

    Thillaivinayagalingam, Pranavan; Newcombe, Anthony R; O'Donovan, Kieran; Francis, Richard; Keshavarz-Moore, Eli

    2007-12-01

    Rapid analyses of chromatographic steps within a biopharmaceutical manufacturing process are often desirable to evaluate column performance, provide mass balance data and to permit accurate calculations of yields and recoveries. Using SPR (surface plasmon resonance) biosensor (Biacore) technology, we have developed a sandwich immunoassay to quantify polyclonal anti-digoxin Fab fragments used for the production of the FDA (Food and Drug Administration)-approved biotherapeutic DigiFab. The results show that specific Fab may be quantified in all affinity process streams and accurate yield and mass balance data calculated. Control experiments using sheep Fab and Fc indicate that the assay is specific to DigiFab. The quantification of potential leached ligand within chromatographic fractions may also be technically challenging, particularly when low-molecular-mass ligands are covalently coupled with an affinity absorbent. Typical methods to assess ligand leakage such as DDMA (digoxin-dicarboxymethoxylamine; digoxin analogue) often involve the use of labelled ligands and relatively complex and labour-intensive analytical techniques. Using the same analytical methodologies, an assay to detect leached or eluted ligand off the column was developed. The results indicate minimal levels of leached ligand in all chromatographic fractions, with total levels of leached DDMA calculated to be 1.52 microg. This is less than 0.01% of the total amount of DDMA coupled with the laboratory-scale affinity column. The SPR methods described in the present study may be applicable for the rapid in-process analysis of specific polyclonal Fab fragments (within a polyclonal mixture) and to rapidly assess leakage of small molecule ligands covalently attached to chromatographic supports.

  6. System and method for detecting gas

    DOEpatents

    Chow, Oscar Ken; Moulthrop, Lawrence Clinton; Dreier, Ken Wayne; Miller, Jacob Andrew

    2010-03-16

    A system to detect a presence of a specific gas in a mixture of gaseous byproducts comprising moisture vapor is disclosed. The system includes an electrochemical cell, a transport to deliver the mixture of gaseous byproducts from the electrochemical cell, a gas sensor in fluid communication with the transport, the sensor responsive to a presence of the specific gas to generate a signal corresponding to a concentration of the specific gas, and a membrane to prevent transmission of liquid moisture, the membrane disposed between the transport and the gas sensor.

  7. A technique for rapid source apportionment applied to ambient organic aerosol measurements from a thermal desorption aerosol gas chromatograph (TAG)

    NASA Astrophysics Data System (ADS)

    Zhang, Yaping; Williams, Brent J.; Goldstein, Allen H.; Docherty, Kenneth S.; Jimenez, Jose L.

    2016-11-01

    We present a rapid method for apportioning the sources of atmospheric organic aerosol composition measured by gas chromatography-mass spectrometry methods. Here, we specifically apply this new analysis method to data acquired on a thermal desorption aerosol gas chromatograph (TAG) system. Gas chromatograms are divided by retention time into evenly spaced bins, within which the mass spectra are summed. A previous chromatogram binning method was introduced for the purpose of chromatogram structure deconvolution (e.g., major compound classes) (Zhang et al., 2014). Here we extend the method development for the specific purpose of determining aerosol samples' sources. Chromatogram bins are arranged into an input data matrix for positive matrix factorization (PMF), where the sample number is the row dimension and the mass-spectra-resolved eluting time intervals (bins) are the column dimension. Then two-dimensional PMF can effectively do three-dimensional factorization on the three-dimensional TAG mass spectra data. The retention time shift of the chromatogram is corrected by applying the median values of the different peaks' shifts. Bin width affects chemical resolution but does not affect PMF retrieval of the sources' time variations for low-factor solutions. A bin width smaller than the maximum retention shift among all samples requires retention time shift correction. A six-factor PMF comparison among aerosol mass spectrometry (AMS), TAG binning, and conventional TAG compound integration methods shows that the TAG binning method performs similarly to the integration method. However, the new binning method incorporates the entirety of the data set and requires significantly less pre-processing of the data than conventional single compound identification and integration. In addition, while a fraction of the most oxygenated aerosol does not elute through an underivatized TAG analysis, the TAG binning method does have the ability to achieve molecular level resolution on

  8. A technique for rapid source apportionment applied to ambient organic aerosol measurements from a thermal desorption aerosol gas chromatograph (TAG)

    SciTech Connect

    Zhang, Yaping; Williams, Brent J.; Goldstein, Allen H.; Docherty, Kenneth S.; Jimenez, Jose L.

    2016-11-25

    Here, we present a rapid method for apportioning the sources of atmospheric organic aerosol composition measured by gas chromatography–mass spectrometry methods. Here, we specifically apply this new analysis method to data acquired on a thermal desorption aerosol gas chromatograph (TAG) system. Gas chromatograms are divided by retention time into evenly spaced bins, within which the mass spectra are summed. A previous chromatogram binning method was introduced for the purpose of chromatogram structure deconvolution (e.g., major compound classes) (Zhang et al., 2014). Here we extend the method development for the specific purpose of determining aerosol samples' sources. Chromatogram bins are arranged into an input data matrix for positive matrix factorization (PMF), where the sample number is the row dimension and the mass-spectra-resolved eluting time intervals (bins) are the column dimension. Then two-dimensional PMF can effectively do three-dimensional factorization on the three-dimensional TAG mass spectra data. The retention time shift of the chromatogram is corrected by applying the median values of the different peaks' shifts. Bin width affects chemical resolution but does not affect PMF retrieval of the sources' time variations for low-factor solutions. A bin width smaller than the maximum retention shift among all samples requires retention time shift correction. A six-factor PMF comparison among aerosol mass spectrometry (AMS), TAG binning, and conventional TAG compound integration methods shows that the TAG binning method performs similarly to the integration method. However, the new binning method incorporates the entirety of the data set and requires significantly less pre-processing of the data than conventional single compound identification and integration. In addition, while a fraction of the most oxygenated aerosol does not elute through an underivatized TAG analysis, the TAG binning method does have the ability to achieve molecular level

  9. A technique for rapid source apportionment applied to ambient organic aerosol measurements from a thermal desorption aerosol gas chromatograph (TAG)

    DOE PAGES

    Zhang, Yaping; Williams, Brent J.; Goldstein, Allen H.; ...

    2016-11-25

    Here, we present a rapid method for apportioning the sources of atmospheric organic aerosol composition measured by gas chromatography–mass spectrometry methods. Here, we specifically apply this new analysis method to data acquired on a thermal desorption aerosol gas chromatograph (TAG) system. Gas chromatograms are divided by retention time into evenly spaced bins, within which the mass spectra are summed. A previous chromatogram binning method was introduced for the purpose of chromatogram structure deconvolution (e.g., major compound classes) (Zhang et al., 2014). Here we extend the method development for the specific purpose of determining aerosol samples' sources. Chromatogram bins are arrangedmore » into an input data matrix for positive matrix factorization (PMF), where the sample number is the row dimension and the mass-spectra-resolved eluting time intervals (bins) are the column dimension. Then two-dimensional PMF can effectively do three-dimensional factorization on the three-dimensional TAG mass spectra data. The retention time shift of the chromatogram is corrected by applying the median values of the different peaks' shifts. Bin width affects chemical resolution but does not affect PMF retrieval of the sources' time variations for low-factor solutions. A bin width smaller than the maximum retention shift among all samples requires retention time shift correction. A six-factor PMF comparison among aerosol mass spectrometry (AMS), TAG binning, and conventional TAG compound integration methods shows that the TAG binning method performs similarly to the integration method. However, the new binning method incorporates the entirety of the data set and requires significantly less pre-processing of the data than conventional single compound identification and integration. In addition, while a fraction of the most oxygenated aerosol does not elute through an underivatized TAG analysis, the TAG binning method does have the ability to achieve molecular level

  10. Determination of partition coefficients of refrigerants by gas liquid chromatographic headspace analysis.

    PubMed

    Abraham, Michael H; Gil-Lostes, Javier; Corr, Stuart; Acree, William E

    2012-11-23

    Gas-water partition coefficients, K(w), and gas-solvent partition coefficients, K(s), have been determined for chlorodifluoromethane and for 1,1,1,3,3,3-hexafluoropropane by headspace analysis, using a very simple experimental procedure. These partition coefficients then yield water-solvent partition coefficients, P(s). Where comparisons can be made there is excellent agreement with literature values for K(w) and P(s). The obtained values of K(s) and P(s) can be used to obtain physicochemical properties, or descriptors, for the refrigerants. Combination of these descriptors with previous equations we have developed enables partition coefficients to be obtained for a host of systems. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Gas-liquid chromatographic measurement of lignocaine in small samples of canine myocardium after enzymatic digestion.

    PubMed Central

    Holt, D W; Loizou, M; Wyse, R K

    1979-01-01

    A method is described whereby lignocaine can be measured in small samples of canine myocardium. A proteolytic enzyme is used to digest the tissue, and the drug, together with an internal standard, is subsequently extracted into an organic solvent and measured by gas-liquid chromatography. The method is reproducible using tissue samples as small as 50 mg and appears to be suitable for the measurement of a number of drugs in small samples of tissue. PMID:429588

  12. On-line gas chromatographic studies of rutherfordium (Element 104), hahnium (Element 105), and homologs

    SciTech Connect

    Kadkhodayan, B.

    1993-05-01

    Gas-phase isothermal chromatogaphy is a method by which volatile compounds of different chemical elements can be separated according to their volatilities. The technique, coupled with theoretical modeling of the processes occurring in the chromatogaphy column, provides accurate determination of thermodynamic properties (e.g., adsorption enthalpies) for compounds of elements, such as the transactinides, which can only be produced on an atom-at-a-time basis. In addition, the chemical selectivity of the isothermal chromatogaphy technique provides the decontamination from interfering activities necessary for the determination of the nuclear decay properties of isotopes of the transactinide elements. Volatility measurements were performed on chloride species of Rf and its group 4 homologs, Zr and Hf, as well as Ha and its group 5 homologs, Nb and Ta. Adsorption enthalpies were calculated for all species using a Monte Carlo code simulation based on a microscopic model for gas thermochromatography in open columns with laminar flow of the carrier gas. Preliminary results are presented for Zr- and Nb-bromides.

  13. A small, portable gas chromatograph-quadrupole mass spectrometer for on-site analysis

    SciTech Connect

    Andresen, B.; Coutts, G.; Alcaraz, A.; Bushman, J.; Cornish, J.

    1994-04-01

    Gas chromatography-mass spectrometry (GC-MS) is the analytical tool of choice for the exact identification of unknown organic chemicals in environmental samples. Capillary gas chromatography, combined with the specific identification capabilities of mass spectrometry, allows the rapid and complete characterization of individual compounds in complex mixtures. As the technology has developed, many manufacturers have offered bench-top MS systems that provide a variety of analytical capabilities. Many instruments have been promoted as ``detectors for gas chromatography.`` More recently, manufacturers have offered integrated packages that can be transported to the field to provide analytical capabilities previously available only in the laboratory. The demonstrated field utility of these field-transportable units has triggered an interest in smaller, lighter weight, and more portable instruments. However, the current weight (>100 lb), large size, and laboratory-based power consumption requirements of these units is viewed as a liability by some potential field instrument users. Over the past several years, the interest in field-deployable instruments has resulted in research and development into smaller GC-MS systems designed with limited applications. While the development of these instruments is certainly worthwhile, a reliable and robust GC-MS instrument that clearly addresses the field-deployable needs for all environmental sampling and analysis would have considerable utility. We have developed portable instruments with analytical performance characteristics similar to those obtained with bench-top instruments. The current instrument, developed at LLNL and described here, was originally designed for use by on-site inspection teams supporting the Chemical Weapons Convention (CWC). The portability and expanded capabilities of this integrated instrument now make it a useful tool for environmental monitoring and on-site analysis studies.

  14. Gas chromatographic-mass spectrometric analysis of creosotes extracted from wooden sleepers installed in playgrounds

    SciTech Connect

    Rotard, W.; Mailahn, W.

    1987-01-01

    In order to evaluate their hygienic risk, wood samples from sleepers (railroad cross ties) impregnated with coal tar creosote were taken from playgrounds and investigated for hazardous compounds. The samples were extracted with ether, and acid-base-neutral separations were made on the creosote extracts. Water-soluble compounds were also isolated. All the fractions were investigated by capillary gas chromatography-mass spectrometry. Besides phenols in the acidic fractions and N-heterocyclic polynuclear aromatic hydrocarbons (PAH) in the basic fractions, high amounts of neutral PAH and also, in several samples high levels of carcinogenic and cocarcinogenic PAH were determined.

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

    SciTech Connect

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

    1987-04-01

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

  16. Simultaneous determination of CFC-11, CFC-12 and CFC-113 in seawater samples using a purge and trap gas-chromatographic system.

    PubMed

    Massolo, Serena; Rivaro, Paola; Frache, Roberto

    2009-12-15

    We have optimized the analytical parameters of a homemade instrument for the simultaneous measurement of the chlorofluorocarbons CCl(2)F(2) (CFC-12), CCl(3)F (CFC-11) and C(2)Cl(3)F(3) (CFC-113) in seawater. Seawater samples are flame sealed into 60 ml glass ampoules avoiding any contact with the atmosphere and stored in cold, dark condition until analysis. In the laboratory, after cracking the ampoule in an enclosed chamber filled with ultra-pure nitrogen, the seawater sample is transferred to a stripping chamber, where ultra-pure nitrogen is used to purge the dissolved CFCs from the seawater. The extracted gases are then cryogenically trapped, subsequently the trap is isolated and heated and the CFCs are transferred by a carrier gas stream into a precolumn and then are separated on a gaschromatographic packed column. To separate adequately CFC-12 from N(2)O, during the early part of the chromatographic run, the gas stream passes through a molecular sieve, which is then isolated and backflushed. The CFCs are detected on an electron capture detector ((63)Ni ECD). After a careful choice of the experimental conditions, the performances of the system were evaluated. The detection limits for seawater samples are: 0.0081 pmol kg(-1) for CFC-12, 0.0073 pmol kg(-1) for CFC-11 and 0.0043 pmol kg(-1) for CFC-113. The reproducibility of replicate samples lies within 5% for the three CFCs. The system has been successfully employed for CFC measurements in seawater samples collected in the Ross Sea (Antarctica) in the framework of the Italian Antarctic research project.

  17. MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission: results and performance

    NASA Astrophysics Data System (ADS)

    Buch, A.; Pinnick, V. T.; Szopa, C.; Grand, N.; Humeau, O.; van Amerom, F. H.; Danell, R.; Freissinet, C.; Brinckerhoff, W.; Gonnsen, Z.; Mahaffy, P. R.; Coll, P.; Raulin, F.; Goesmann, F.

    2015-10-01

    The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquiring samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular and chiral) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis/chemical derivatization gas chromatography (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide information on elemental and molecular makeup, polarity, chirality and isotopic patterns of analyte species. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatographymass spectrometry (GC-MS) mode of operation.

  18. Method for detecting gas turbine engine flashback

    SciTech Connect

    Singh, Kapil Kumar; Varatharajan, Balachandar; Kraemer, Gilbert Otto; Yilmaz, Ertan; Lacy, Benjamin Paul

    2012-09-04

    A method for monitoring and controlling a gas turbine, comprises predicting frequencies of combustion dynamics in a combustor using operating conditions of a gas turbine, receiving a signal from a sensor that is indicative of combustion dynamics in the combustor, and detecting a flashback if a frequency of the received signal does not correspond to the predicted frequencies.

  19. Gas chromatographic fingerprinting of crude oil from Idu-Ekpeye oil spillage site in Niger-delta, Nigeria.

    PubMed

    Udoetok, Inimfon A; Osuji, Leo C

    2008-06-01

    Samples were collected from an oil polluted site in Niger-delta, Nigeria. Gas chromatographic analyses carried out on the samples revealed an abundance of n-alkanes within the n-C8-n-C23 region. The pristane/phytane ratio of 5.70 obtained for the samples depicted a plant/terrestrial source input and a possible oxic depositional environment. The n-C17/pristane and n-C18/phytane ratios of 2.80 and 2.77, respectively, suggested that the spilled oil was only slightly weathered, as corroborated by the presence of peaks in the aromatic hydrocarbon fingerprints. The polycyclic aromatic hydrocarbon (PAH) fractions showed that the hydrocarbon fractions might have undergone combustion and/or that there was bush burning at the site prior to the oil spill incidence. This is supported by the abundance of high-molecular-weight PAHs which are pyrogenic in nature. High molecular weight PAHs are products of the combustion of petroleum or its products. The phenanthrene/anthracene ratio of 0.95, fluorathene/pyrene ratio of 2.23 and the summation operator (other three to six ringed PAHs)/ summation operator (five alkylated PAHs) ratio far greater than unity (4.10) also affirm this. On the other hand, the benzo (a) anthracene to chrysene ratio of 0.24 confirms the petrogenic origin of the spilled oil because chrysene which is highly abundant is a fossil PAH.

  20. Integration and Ruggedization of a Commercially Available Gas Chromatograph and Mass Spectrometer (GCMS) for the Resource Prospector Mission (RPM)

    NASA Technical Reports Server (NTRS)

    Loftin, Kathleen; Griffin, Timothy; Captain, Janine

    2013-01-01

    The Resource Prospector is a mission to prospect for lunar volatiles (primarily water) at one of the two lunar poles, as well as demonstrate In-Situ Resource Utilization (ISRU) on the Moon. The Resource Prospector consists of a lander, a rover, and a rover-borne scientific payload. The Regolith and Environment Science and Oxygen & Lunar Volatile Extraction (RESOLVE) payload, will be able to (1) locate near subsurface volatiles, (2) excavate and analyze samples of the volatile-bearing regolith, and (3) demonstrate the form, extractability and usefulness of the materials. The gas chromatograph mass spectrometer (GCMS) is the primary instrument in the RESOLVE instrumentation suite responsible for identification and quantification of the volatiles evolved from the lunar regolith. Specifically, this instrument must have: a low mass, a low power consumption, be able to perform fast analyses of samples ranging from less than one to greater than ninety nine percent water by mass, be autonomously controlled by the payload's software and avionics platform, and be able to operate in the harsh lunar environment. The RPM's short mission duration is the primary driver of the requirement for a very fast analysis time currently base lined at less than 2 minutes per sample. This presentation will discuss the requirements levied upon the GCMS design, lessons learned from a preliminary field demonstration deployment, the current design, and the path forward.

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

    PubMed

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

    2015-09-11

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

  2. Gas chromatographic determination of phosphate-based flame retardants in styrene-based polymers from waste electrical and electronic equipment.

    PubMed

    Roth, Thomas; Urpi Bertran, Raquel; Pöhlein, Manfred; Wolf, Marion; van Eldik, Rudi

    2012-11-02

    Two methods for the determination of phosphate-based flame retardants (PFRs) and similar organophosphates (OPs) were developed. Two gas chromatographic systems were applied, one equipped with a quadrupole mass spectrometer (GC/MS), the other with a specific phosphorus-nitrogen detector (GC/PND). A procedure of ultrasonic supported extraction and precipitation (USSE) was applied and verified using in-house produced reference materials. Twelve polymer parts of electrical and electronic devices, and eight polymer references were analysed for their PFR contents. The results show that the methods are capable of identifying PFRs in concentration ranges from 3 μg L(-1) (tricresyl phosphate, TCP) to 12 μg L(-1) (cresyl diphenyl phosphate, CDP) on GC/PND and from 110 μg L(-1) (triphenyl phosphine oxide, TPPO) to 3250 μg L(-1) (tris(ethylhexyl) phosphate, TEHP) on GC/MS in reference solutions. LODs in polymer extracts range from 180 μg g(-1) (triphenyl phosphate, TPP) to 670 μg g(-1) (bisphenol-A-bis(diphenyl phosphate), BDP) on GC/PND and from 75 μg g(-1) (TPPO) to 780 μg g(-1) (BDP) on GC/MS. The overall procedure time for one sample was less than 45 min (GC/MS) and less than 65 min (GC/PND). Copyright © 2012. Published by Elsevier B.V.

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

    SciTech Connect

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

    2006-10-01

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

  4. Development of a miniaturized diffusive sampler for true breathing-zone sampling and thermal desorption gas chromatographic analysis.

    PubMed

    Lindahl, Roger; Levin, Jan-Olof; Sundgren, Margit

    2009-07-01

    Exposure measurements should be performed as close as possible to the nose and mouth for a more correct assessment of exposure. User-friendly sampling equipment, with a minimum of handling before, during and after measurement, should not affect ordinary work. In diffusive (passive) sampling, no extra equipment as sampling pumps is needed, making the measurements more acceptable to the user. The diffusive samplers are normally attached on a shoulder, on a breast-pocket or on the lapel. There are, however, difficulties if true breathing-zone sampling is to be performed, since available diffusive samplers normally cannot be arranged close to the nose/mouth. The purpose of this work was to study the performance of a miniaturized tube type diffusive sampler attached to a headset for true breathing-zone sampling. The basis for this miniaturization was the Perkin Elmer ATD tube. Both the size of the tube and the amount of adsorbent was decreased for the miniaturized sampler. A special tube holder to be used with a headset was designed for the mini tube. The mini tube is thermally desorbed inside a standard PE tube. The new sampler was evaluated for the determination of styrene, both in laboratory experiments and in field measurements. As reference method, diffusive sampling with standard Perkin Elmer tubes, thermal desorption and gas chromatographic (GC) analysis was used. The sampling rate was determined to 0.356 mL min(-1) (CV 9.6%) and was not significantly affected by concentration, sampling time or relative humidity.

  5. [Correlation between octanol-air partition coefficients and retention parameters of polychlorinated biphenyls on gas chromatographic columns].

    PubMed

    Zhang, Qing; Zhao, Hongxia; Chen, Jiping; Liang, Xinmiao

    2005-09-01

    Octanol-air partition coefficient (Koa) is a key descriptor for describing the partitioning of organic pollutants, especially persistent organic pollutants (POPs), between air and environmental organic phases. Thus it is necessary to determine or predict the Koa values of these compounds. A novel method was introduced to describe the quantitive relationship between the octanol-air partition coefficients and gas chromatographic (GC) retention parameters A, B values of polychlorinated diphenyls (PCBs) which are typical persistent organic pollutants. By the correlation analysis between GC retention parameters A, B values of PCBs on DB-1, DB-5 and DB-1701 columns, and their octanol-air partition coefficients, a good linear relationship was found. The stepwise multiple linear regression was used to derive binary equations with the correlation coefficients greater than 0.99, and the standard deviations are less than 0.11. In addition, based on the 153 experimental A, B values and 56 predicted A, B values, the Koa values of the remaining 190 PCBs were predicted.

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

    PubMed

    Pensabene, J W; Fiddler, W

    1994-01-01

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

  7. Inverse gas chromatographic method for measurement of interactions between soy protein isolate and selected flavor compounds under controlled relative humidity.

    PubMed

    Zhou, Qiaoxuan; Cadwallader, Keith R

    2004-10-06

    An inverse gas chromatographic (IGC) method was developed to study the binding interactions between selected volatile flavor compounds and soy protein isolate (SPI) under controlled relative humidity (RH). Three volatile probes (hexane, 1-hexanol, and hexanal) at very low levels were used to evaluate and validate system performance. On the basis of the thermodynamic data and the isotherms measured at 0% RH, 1-hexanol and hexanal had higher binding affinities than hexane, which could be attributed to hydrogen-bonding interactions with SPI. At 30% RH, 1-hexanol and hexanal were retained less than at 0% RH, indicating possible competition for binding sites on the SPI surface between water and volatile probe molecules. Results showed that the thermodynamic data determined were comparable to the available literature values. Use of IGC allowed for the rapid and precise generation of sorption isotherms. Repeatability between replicate injections and reproducibility across columns were very good. IGC is a potentially high-throughput method for the sensitive, precise, and accurate measurement of flavor-ingredient interactions in low-moisture food systems.

  8. Gas chromatographic-mass spectrometric determination of isotopic enrichment of 6-15NH2 in adenine nucleotides.

    PubMed

    Lewis, S; Yudkoff, M

    1985-03-01

    A gas chromatographic-mass spectrometric method for the determination of isotopic abundance in [6-15NH2]adenine nucleotides is described. The method involves formation of the di-t-butyldimethylsilyl (TBDMS) derivative of adenine following isolation of the nucleotide fraction with solid-phase ion-exchange chromatography and subsequent acid hydrolysis of nucleotides to free base. Mass spectra for both adenine-diTBDMS and [6-15NH2]adenine-diTBDMS were obtained to identify those ions containing the 6-NH2 moiety. The base peak (m/z 306) was formed by loss of C4H9 (57) and constitutes approximately one-third of the total ion current. Using selected ion monitoring of the m/z 306/m/z 307 ratio, levels of isotopic abundance of 1.0-50.0 mol% excess could be measured reproducibly with the injection of 10-20 pmol of the adenine-diTBDMS derivative obtained from isolated rat hepatocytes. Confirmation that measured isotopic abundance was referable to labeling of the 6-15NH2 group was obtained by oxidation of adenine to hypoxanthine and determination of enrichment in the hypoxanthine-diTBDMS derivative. The method was used to study the formation of [6-15NH2]adenine nucleotides during the incubation of isolated rat hepatocytes with [15N]alanine. A level of approximately 6.0 mol% excess was observed at 60 min incubation.

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

    SciTech Connect

    Kang, L.; Armstrong, D.W.

    1994-12-31

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

  10. Field screening of volatile and semi-volatile organic pollutants using a heated, portable micro gas chromatograph

    SciTech Connect

    Bruns, M.W.; Gonzalez, D.L.

    1995-12-31

    A heated, portable silicon micromachined gas chromatograph was designed, developed and recently utilized in the characterization of volatile and some semi-volatile organic compound distribution in soil at a site in the Midwest. The use of this system in the field allowed for the rapid, on-site characterization and field screening of gasoline range VOCs and semi-volatiles (e.g., benzene, toluene, ethylebenzene, and xylene; and naphthalene) and chlorinated hydrocarbon solvents in soil and assisted in the geological mapping of environmental hot spots. The sample inlet and introduction system of the micro GC is heatable to 110 C to further extend the application range of the micro GC to samples with high moisture content, high concentration of condensable vapors, and semi-volatile compounds. Data will be presented on the use of the heated system in the characterization of the site with details provided regarding the advantages of individual compound characterization, sampling for screening purposes, and environmental screening in the field (to locate hot spots) and in mobile laboratories (to prevent overloading of GC/MS systems).

  11. Radioimmunological screening and gas chromatographic determination of morphine and related narcotic analgesics in post mortem blood.

    PubMed

    Cimbura, G; Koves, E

    1981-01-01

    A sensitive, reproducible, and relatively specific procedure is presented for the screening, identification, and quantitation of morphine, hydromorphone, codeine, oxycodone, and hydrocodone in autopsy blood. The drugs are isolated from whole blood by adsorption on an XAD-2 resin slurry and subsequent elution with an organic solvent mixture. Part of the resin extract is screened for morphine and related cross-reacting compounds by a commercially available radioimmunoassay (RIA) and the remainder of the same extract is analyzed by gas chromatography using a nitrogen/phosphorus detector (GC/NP). The procedure has been used frequently in forensic toxicological casework. Since toxic blood concentrations of hydrocodone have not been well documented, the results of toxicological examination of two fatalities involving this drug are presented.

  12. Liquid chromatographic analysis of a formulated ester from a gas-turbine engine test

    NASA Technical Reports Server (NTRS)

    Jones, W. R., Jr.; Morales, W.

    1983-01-01

    Size exclusion chromatography (SEC) utilizing mu-Bondagel and mu-Styragel columns with a tetrahydrofuran mobile phase was used to determine the chemical degradation of lubricant samples from a gas-turbine engine test. A MIL-L-27502 candidate, ester-based lubricant was run in a J57-29 engine at a bulk oil temperature of 216 C. In general, the analyses indicated a progressive loss of primary ester, additive depletion, and formation of higher molecular weight material. An oil sample taken at the conclusion of the test showed a reversal of this trend because of large additions of new oil. The high-molecular-weight product from the degraded ester absorbed strongly in the ultraviolet region at 254 nanometers. This would indicate the presence of chromophoric groups. An analysis of a similar ester lubricant from a separate high-temperature bearing test yielded qualitatively similar results.

  13. Gas chromatographic study of degradation phenomena concerning building and cultural heritage materials.

    PubMed

    Metaxa, E; Agelakopoulou, T; Bassiotis, I; Karagianni, Ch; Roubani-Kalantzopoulou, F

    2009-05-30

    Air pollution influences all aspects of social and economical life nowadays. In order to investigate the impact of air pollution on materials of works of art, the method of Reversed Flow-Inverse Gas Chromatography has been selected. The presence of various atmospheric pollutants is studied on marbles, oxides--building materials and samples of authentic statues from the Greek Archaeological Museums of Kavala and of Philippi. The method leads to the determination of several physicochemical quantities and the characterization of the heterogeneous surfaces of these solids. Moreover, the influence of a second pollutant (synergistic effect) is examined. The structure, the properties and the behavior of the materials are examined by X-Ray Diffraction, Scanning Electron Microscopy and Raman Spectroscopy. Therefore, the precise measurement of the above mentioned quantities form the scientific basis for elucidation of the mechanism of the whole phenomenon of the degradation, thus providing a scientific platform to conservation procedures.

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

    USGS Publications Warehouse

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

    1978-01-01

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

  15. Inverse gas chromatographic study of the oxidation stability of lubricating base oils via solubility parameter calculations.

    PubMed

    Moustafa, Nagy Emam; Eissa, Elham Ahmed

    2007-11-01

    The Flory-Huggins interaction parameter (chi1, 2(infinity)) and solubility parameter (delta2) and its hydrogen bonding sensing component (delta(h)) were determined using inverse gas chromatography (IGC). These parameters were successfully used in the probes of chemical changes that occur during the oxidation of naphthenic and paraffinic base oils in a GC column. Changes in chi1, 2(infinity) values reflect the different types of intermolecular interactions (dispersive, polar, hydrogen bonding) of the given lubricating base oil during oxidation. The obtained results showed that delta(h) component of solubility parameter is the most important parameter for probing the oxidative-chemical changes during the oxidation of given lubricating oils.

  16. Liquid chromatographic analysis of a formulated ester from a gas-turbine engine test

    NASA Technical Reports Server (NTRS)

    Jones, W. R., Jr.; Morales, W.

    1983-01-01

    Size exclusion chromatography (SEC) utilizing mu-Bondagel and mu-Styragel columns with a tetrahydrofuran mobile phase was used to determine the chemical degradation of lubricant samples from a gas-turbine engine test. A MIL-L-27502 candidate, ester-based lubricant was run in a J57-29 engine at a bulk oil temperature of 216 C. In general, the analyses indicated a progressive loss of primary ester, additive depletion, and formation of higher molecular weight material. An oil sample taken at the conclusion of the test showed a reversal of this trend because of large additions of new oil. The high-molecular-weight product from the degraded ester absorbed strongly in the ultraviolet region at 254 nanometers. This would indicate the presence of chromophoric groups. An analysis of a similar ester lubricant from a separate high-temperature bearing test yielded qualitatively similar results.

  17. Gas chromatographic-mass spectrometric method for polycyclic aromatic hydrocarbon analysis in plant biota.

    PubMed

    Meudec, A; Dussauze, J; Jourdin, M; Deslandes, E; Poupart, N

    2006-03-10

    Using gas chromatography-mass spectrometry, a new method was developed for the identification and the quantification of polycyclic aromatic hydrocarbons (PAHs) in plants. This method was particularly optimised for PAH analyses in marine plants such as the halophytic species, Salicornia fragilis Ball et Tutin. The saponification of samples and their clean up by Florisil solid-phase extraction succeeded in eliminating pigments and natural compounds, which may interfere with GC-MS analysis. Moreover, a good recovery of the PAHs studied was obtained with percentages ranging from 88 to 116%. Application to the determination of PAH in a wide range of coastal halophytic plants is presented and validated the efficiency, the accuracy and the reproducibility of this method.

  18. Multidimensional gas chromatographic determination of paraffins, olefins and aromatics in naphthas.

    PubMed

    Lo Coco, Filippo; Gasparini, Gianni; Lanuzza, Francesco; Stani, Gianluca; Adami, Gianpiero

    2006-01-01

    In order to cope with the increasing demand for gasoline and the need to reduce environmental impact for sustainable development, refineries have installed refining technology by introducing cracking, reforming, isomerization and alkylation. The standard EN 228: 2004 outlines the specification that gasoline, deriving from the blend of several fractions, must have for use in modem piston engines. Naphtha is one of the products from distilling crude oil that can be used as starting material in the reforming process whose derivatives, which are a fraction of gasoline, depend on the composition of the naphtha. Knowledge of the naphtha composition thus enables to provide the final composition of the products of reforming, the efficiency of the plant and also provides information about the crude oil used. In this paper some naphtha samples were analysed by multidimensional gas chromatography. This technique allows in a single analysis a good separation of the hydrocarbon types and within each hydrocarbon type a good carbon number separation.

  19. Gas chromatographic study of the volatile products from co-pyrolysis of coal and polyethylene wastes.

    PubMed

    Domínguez, A; Blanco, C G; Barriocanal, C; Alvarez, R; Díez, M A

    2001-05-18

    The aim of this study was to determine the volatile products distribution of co-processing of coal with two plastic wastes, low-density polyethylene from agriculture greenhouses and high-density polyethylene from domestic uses, in order to explain the observed decrease in coal fluidity caused by polyethylene waste addition. Polymeric materials, although they are not volatile themselves, may be analysed by gas chromatography through the use of pyrolysis experiments. In this way, a series of pyrolysis tests were performed at 400 and 500 degrees C in a Gray-King oven with each of the two plastic wastes, one high-volatile bituminous coal and blends made up of coal and plastic waste (9:1, w/w, ratio). The pyrolysis temperatures, 400 and 500 degrees C, were selected on the basis of the beginning and the end of the coal plastic stage. The organic products evolved from the oven were collected, dissolved in pyridine and analysed by capillary gas chromatography using a flame ionization detector. The analysis of the primary tars indicated that the amount of n-alkanes is always higher than that of n-alkenes and the formation of the alkenes is favoured by increasing the pyrolysis temperature. However, this effect may be influenced by the size of the hydrocarbon. Thus, the fraction C17-C31 showed a higher increase of n-alkenes/n-alkanes ratio than other fractions. On the other hand, the difference between the experimental and estimated values from tars produced from single components was positive for n-alkanes and n-alkenes, indicating that co-pyrolysis of the two materials enhanced the chemical reactivity during pyrolysis and produced a higher conversion than that from individual components.

  20. Analysis of ketone bodies in exhaled breath and blood of ten healthy Japanese at OGTT using a portable gas chromatograph.

    PubMed

    Tanda, Naoko; Hinokio, Yoshinori; Washio, Jumpei; Takahashi, Nobuhiro; Koseki, Takeyoshi

    2014-11-24

    Ketone bodies including acetone are disease biomarkers for diabetes that sometimes causes severe ketoacidosis. The present study was undertaken to clarify the significance of exhaled acetone and plasma ketone bodies at bedside in a clinical setting. The oral glucose tolerance test (OGTT) was performed in 10 healthy Japanese volunteers (five females and five males). Exhaled breath acetone and volatile sulfide compounds (VSCs) in mouth air were measured simultaneously with blood sampling during the OGTT using a portable gas chromatograph equipped with an In2O3 thick-film type gas sensor and a VSC monitor. Acetone, β-hydroxybutyrate (β-OHB) and acetoacetate (AcAc) in blood plasma as well as glucose and insulin were examined. Oral conditions were examined based on the Community Periodontal Index (CPI) by one dentist. In addition, the same type of analysis was applied to two uncontrolled type 2 diabetes mellitus patients hospitalized at Tohoku University Hospital. Exhaled acetone was measured at the same time as blood withdrawal in the morning before breakfast and at night before bed at the beginning, the middle, and the end of hospitalization. All volunteers showed normal OGTT patterns with no ketonuria and periodontitis; however, there were significant correlations between breath acetone and plasma β-ΟΗΒ and between breath acetone and plasma AcAc under fasting conditions. Breath acetone of the type 2 diabetes mellitus patients showed positive correlations with plasma glucose when the level of plasma glucose tended to decrease during hospitalization. In spite of a very limited number of cases, our results support the idea that exhaled breath acetone may be related to plasma β-OHB and AcAc, which reflect glucose metabolism in the body.

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

    PubMed

    Hammann, Simon; Vetter, Walter

    2015-12-15

    Steryl esters are high molecular weight compounds (600-700g/mol) regularly present as a minor lipid class in animal and plant lipids. Different sterol backbones (e.g., cholesterol, β-sitosterol and brassicasterol) which can be esterified with various fatty acids can result in highly complex steryl ester patterns in food samples. The gas chromatographic (GC) analysis of intact steryl esters is challenging, since high elution temperatures are required for their elution. On nonpolar GC phases, steryl esters with fatty acids with differing degree of unsaturation (e.g., oleate and linoleate) cannot be separated and there are only few polar columns available with sufficient temperature stability. In this study, we used gas chromatography with mass spectrometry (GC/MS) and analyzed intact steryl esters on a commercial room temperature ionic liquid (RTIL) column which was shortened to a length of 12m. The column separated the steryl esters both by total carbon number and by degree of unsaturation of the fatty acid. For instance, cholesteryl esters with stearic acid (18:0), oleic acid (18:1n-9), linoleic acid (18:2n-6) and α-linolenic acid (18:3n-3) could be resolved (R≥1.3) from each other. By analysis of synthesized standard substances, the elution orders for different steryl backbones and different fatty acids on a given sterol backbone could be determined. Analysis of spreads and plant oils allowed to determine retention times for 37 steryl esters, although a few co-elutions were observed. The ionic liquid column proved to be well-suited for the analysis of intact steryl esters. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    PubMed

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

    2016-09-02

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

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

    PubMed Central

    Jones, Thomas M.; Albersheim, Peter

    1972-01-01

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

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

    PubMed

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

    2014-08-08

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

  5. Gas chromatographic determination of carbonyl compounds in biological and oil samples by headspace single-drop microextraction with in-drop derivatisation.

    PubMed

    Fiamegos, Yiannis C; Stalikas, Constantine D

    2008-02-25

    A suitable method for the gas chromatographic determination of 10 characteristic carbonyls in biological and oil samples based on the in-drop formation of hydrazones by using 2,4,6-trichlorophenylhydrazine (TCPH), has been developed. The derivatisation-extraction procedure was optimized separately for aqueous and oil samples with respect to the appropriate organic drop solvent, drop volume, in-drop TCPH concentration, sample stirring rate, temperature during single-drop microextraction (SDME), reaction time and headspace-to-sample volume ratio. The optimization showed differentiation of optimum values between the studied matrices. The limits of detection were found to range from 0.001 to 0.003microgmL(-1) for the aqueous biological samples and from 0.06 to 0.20microgmL(-1) for the oil samples. The limits of quantification were in the range of 0.003-0.010microgmL(-1) and 0.020-0.059microgmL(-1) for aqueous and oil samples, respectively. The overall relative standard deviations of the within-day repeatability and between-day reproducibility were <4.4% and <8.2% for the aqueous biological samples and <3.9% and <7.4% for the oxidized oil samples.

  6. [Analysis of pesticides including chlorine in welsh onions and mushrooms using gas chromatograph with an atomic emission detector (GC-AED)].

    PubMed

    Tateishi, Yukinari; Takano, Ichiro; Kobayashi, Maki; Tamura, Yasuhiro; Tomizawa, Sanae; Sakai, Naoko; Kamijo, Kyoko; Nagayama, Toshihiro; Kamata, Kunihiro

    2004-12-01

    An analytical method for the determination of 32 kinds of pesticide residues in onions, Welsh onions and mushrooms using gas chromatograph with an atomic emission detector (GC-AED) was developed. The pesticides were extracted with acetone-n-hexane (2:3) mixture. The crude extract was partitioned between 5% sodium chloride and ethyl acetate-n-hexane (1:4) mixture. The extract was passed through a Florisil mini-column for cleanup with 10 mL of acetone-n-hexane (1:9) mixture. Although the sensitivity of GC-AED was inferior to that of GC-ECD, GC-AED has a superior element-selectivity. Therefore pesticide residues in foods could be analyzed more exactly by using GC-AED. Thirty-two pesticides including chlorine in onion, Welsh onion and shiitake mushroom were detected without interference. Recoveries of these pesticides from samples determined by GC-AED were 64-114%, except for a few pesticides.

  7. Round-robin evaluation of a solid-phase microextraction-gas chromatographic method for reliable determination of trace level ethylene oxide in sterilized medical devices.

    PubMed

    Harper, Thomas; Cushinotto, Lisa; Blaszko, Nancy; Arinaga, Julie; Davis, Frank; Cummins, Calvin; DiCicco, Michael

    2008-02-01

    Medical devices that are sterilized with ethylene oxide (EtO) retain small quantities of EtO residuals, which may cause negative systemic and local irritating effects, and must be accurately quantified to ensure non-toxicity. The goal of this round-robin study is to investigate the capability of a novel solid-phase microextraction-gas chromatographic (SPME-GC) method for trace-level EtO residuals analysis: three independent laboratories conducted a guided experiment using this SPME-GC method, in assessing method performance, ruggedness and the feasibility of SPME fibers. These were satisfactory across the independent laboratories, at the 0.05-5.00 ppm EtO range. This method was then successfully applied to analyze EtO residuals in several sterilized/aerated medical devices of various polymeric composition, reliably detecting and quantifying the trace levels of EtO residuals present ( approximately 0.05 ppm EtO). SPME is a feasible alternative for quantifying trace-level EtO residuals in sterilized medical devices, thereby lowering the limit of quantification (LOQ) by as much as two to three orders of magnitude over the current GC methodology of direct liquid injection.

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

    PubMed

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

    2000-03-01

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

  9. Development and evaluation of gas and liquid chromatographic methods for the analysis of fatty amines.

    PubMed

    Breitbach, Zachary S; Weatherly, Choyce A; Woods, Ross M; Xu, Chengdong; Vale, Glenda; Berthod, Alain; Armstrong, Daniel W

    2014-03-01

    In contrast to the plethora of publications on the separation of fatty acids, analogous studies involving fatty amines are scarce. A recently introduced ionic-liquid-based capillary column for GC was used to separate trifluoroacetylated fatty amines focusing on the analysis of a commercial sample. Using the ionic liquid column (isothermal mode at 200 °C) it was possible to separate linear primary fatty amines from C12 to C22 chain length in less 25 min with MS identification. The log of the amine retention factors are linearly related to the alkyl chain length with a methylene selectivity of 0.117 kcal/mol for the saturated amines and 0.128 kcal/mol for the mono-unsaturated amines. The sp2 selectivity for unsaturated fatty amines also could be calculated as 0.107 kcal/mol for the ionic liquid column. The commercial sample was quantified by GC with flame ionization detection (FID). An LC method also was developed with a reversed phase gradient separation using acetonitrile/formate buffer mobile phases and ESI-MS detection. Native amines could be detected and identified by their single ion monitoring chromatograms even when partial coelution was observed. The analysis of the commercial sample returned results coherent with those obtained by GC-FID and with the manufacturer's data.

  10. [The gas chromatographic determination of sulfur- and oxygen-containing organic compounds released into the air of cellulose sulfate works].

    PubMed

    Taranenko, N A; Dorogova, V B

    1992-01-01

    The article presents data on the design of sensitive, selective, useful in group analysis method to detect dimethylsulphide, dimethyldisulphide, acetic, propionic, butyric and valeric acids, methyl alcohol and phenol by means of gas chromatography in the air of cellulose sulphate production working zone. The methods were tested in examining the work conditions in Bratsk found-lavage shops.

  11. Multiresidue chromatographic method for the determination of macrolide residues in muscle by high-performance liquid chromatography with UV detection.

    PubMed

    Juhel-Gaugain, M; Anger, B; Laurentie, M

    1999-01-01

    A high-performance liquid chromatographic (HPLC) method for the simultaneous determination of tilmicosin, tylosin, spiramycin, and its major metabolite neospiramycin was developed that is suitable for porcine, bovine, and poultry muscles. Macrolide residues were extracted from muscle with acetonitrile, fat was removed by liquid-liquid extraction with isooctane, and the extract was then cleaned on Bond Elut C18 cartridges. The HPLC separation was performed on an Inertsil ODS3 C18 column (150 x 4 mm) with 0.05% trifluoroacetic acid-acetonitrile in a gradient mode. Two different chromatographic gradients were used for tilmicosin-tylosin and spiramycin-neospiramycin, and the detection wavelengths were 287 and 232 nm, respectively. The method was validated from 1/2 the maximum residue limit (MRL) to 4 times the MRL with pork muscle samples. Mean recoveries were 60, 63.5, 51, and 42% for tilmicosin, tylosin, spiramycin, and neospiramycin, respectively. The detection limits are 15 micrograms/kg for tilmicosin and tylosin, 30 micrograms/kg for spiramycin, and 25 micrograms/kg for neospiramycin. Linearity, precision, and accuracy of the method were also tested.

  12. Gas-liquid chromatographic determination of total cholesterol in multicomponent foods.

    PubMed

    Punwar, J K

    1975-07-01

    A method is described for the determination of total cholesterol in multicomponent foods and also other products such as nonfat dry milk, dried whole egg solids, and certain candy bars. The lipid is extracted from the sample by a mixed solvent and saponified. The unsaponifiable fraction which contains the cholesterol and other sterols is extracted with benzene. An aliquot is evaporated to dryness and the residue is dissolved in dimethylformamide. The sterols are derivatized to form trimethylsilyl (TMS) ethers. The TMS-cholesterol derivative is quantitatively determined by gas-liquid chromatography, using 5alpha-cholestane as an internal standard. Nine laboratories participated in a collaborative study of the determination of total cholesterol in deviled ham sandwich spread, vegetable beef stew, corned beef hash, frozen chicken pot pie, pizza pepperoni, fish sticks, breaded shrimp, chocolate-covered candy bars, dried whole egg solids, and nonfat dry milk and the results are reported here. The coefficient of variation ranged from 5.64 to 23.2%, with an average coefficient of variation of 14.8%.

  13. Gas chromatographic analysis of histamine in mahi-mahi (Coryphaena hippurus).

    PubMed

    Antoine, Francis R; Wei, Cheng-I; Otwell, W Steve; Sims, Charlie A; Littell, Ramon C; Hogle, Amanda D; Marshall, Maurice R

    2002-08-14

    Several authors have studied histamine using gas chromatography (GC) as a tool for quantitation, but the methods used were not always suitable depending on the kind of food. Problems frequently cited include incomplete histamine elution from the columns and peak tailing. Histamine is of interest because it is the factor common to all cases of scombroid poisoning, it has physiological and biological activity, and it is a chemical indicator of fish quality. In this study a modified GC method was used to quantify histamine in mahi-mahi (Coryphaena hippurus). Mean recovery was 67% for the GC method, compared with 90% for the AOAC fluorometric method. There was a 0.96 correlation of the GC histamine values with those of the AOAC fluorometric method. A temperature program, splitless/split injection, and analyte cleanup were essential for GC properties. Histamine retention time was 8.2 min. The method allowed peak height to be used for quantitation and simultaneous analysis of cadaverine and putrescine.

  14. Gas chromatographic isolation of individual compounds from complex matrices for radiocarbon dating

    SciTech Connect

    Eglinton, T.I.; Aluwihare, L.I.; McNichol, A.P.; Bauer, J.E.; Druffel, E.R.M.

    1996-03-01

    This paper describes the application of a novel, practical approach for isolation of individual compounds from complex organic matrices for natural abundance radiocarbon measurement. This is achieved through the use of automated pereparative capillary gas chromatography (PCGC) to separate and recover sufficient quantities of individual target compounds for {sup 14}C analysis by accelerator mass spectrometry (AMS). We developed and tested this approach using a suite of samples (plant lipids, petroleums) whose ages spanned the {sup 14}C time scale and which contained a variety of compound types (fatty acids, sterols, hydrocarbons). Comparison of individual compound and bulk radiocarbon signatures for the isotopically homogeneous samples studied revealed that {Delta}{sup 14}C values generally agreed well ({+-}10%). Background contamination was assessed at each stage of the isolation procedure, and incomplete solvent removal prior to combustion was the only significant source of additional carbon. Isotope fractionation was addressed through compound-specific stable carbon isotopic analyses. Fractionation of isotopes during isolation of individual compounds was minimal (<5% for {delta}{sup 13}C), provided the entire peak was collected during PCGC. Trapping of partially coeluting peaks did cause errors, and these results highlight the importance of conducting stable carbon isotopic measurements of each trapped compound in concert with AMS for reliable radiocarbon measurements. 29 refs., 9 figs., 2 tabs.

  15. Gas chromatographic retention index as a basis for predicting evaporation rates of complex mixtures.

    PubMed

    Mcllroy, John W; Jones, A Daniel; McGuffin, Victoria L

    2014-12-10

    Models that predict the fate of petroleum fuels in the environment are often required for effective remediation of fuel-contaminated sites. In this research, an environmental fuel spill was simulated by means of a diesel/water microcosm, in which the temporal changes in composition were assessed during evaporation by gas chromatography-mass spectrometry (GC-MS). First-order kinetic rate constants were calculated for 51 selected compounds and utilized to develop predictive models for evaporation rate constants, using GC retention indices on a nonpolar stationary phase. Models were initially developed to predict rates of evaporation of compounds from individual classes (normal alkane, branched alkane, alkyl benzene, and polycyclic hydrocarbon) and then expanded to include all compounds (comprehensive model). Using the comprehensive model, the rate constants were predicted with a mean absolute percent error (MAPE) of 10%, whereas the class-specific models resulted in less error (4-8%). These models were employed to predict the fraction remaining of the total fuel (6% error) as well as the fraction remaining of individual compounds (13% MAPE). Accurate models such as these will facilitate remediation of environmental releases of petroleum products. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. π-Extended triptycene-based material for capillary gas chromatographic separations.

    PubMed

    Yang, Yinhui; Wang, Qinsi; Qi, Meiling; Huang, Xuebin

    2017-10-02

    Triptycene-based materials feature favorable physicochemical properties and unique molecular recognition ability that offer good potential as stationary phases for capillary gas chromatography (GC). Herein, we report the investigation of utilizing a π-extended triptycene material (denoted as TQPP) for GC separations. As a result, the TQPP capillary column exhibited high column efficiency of 4030 plates m(-1) and high-resolution performance for a wide range of analytes, especially structural and positional isomers. Interestingly, the TQPP stationary phase showed unique shape selectivity for alkanes isomers and preferential retention for analytes with halogen atoms and H-bonding nature mainly through their halogen-bonding and H-bonding interactions. In addition, the TQPP column had good repeatability and reproducibility with the RSD values of 0.02-0.34% for run-to-run, 0.09-0.80% for day-to-day and 1.4-5.2% for column-to-column, respectively, and favorable thermal stability up to 280 °C. This work demonstrates the promising future of triptycene-based materials as a new class of stationary phases for GC separations. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Calix[4]pyrroles: highly selective stationary phases for gas chromatographic separations.

    PubMed

    Fan, Jing; Wang, Zhenzhong; Li, Qian; Qi, Meiling; Shao, Shijun; Fu, Ruonong

    2014-10-03

    Calix[4]pyrroles offer a great potential as stationary phases for gas chromatography (GC) due to their unique structures and physicochemical properties. Herein we present the first report of using two calix[4]pyrroles, namely meso-tetra-cyclohexylcalix[4]pyrrole (THCP) and meso-octamethylcalix[4]pyrrole (OMCP). These stationary phases were statically coated onto capillary columns and investigated in terms of column efficiency, polarity, separation performance, thermal stability and repeatability. The columns achieved column efficiencies of 2200-3000plates/m and exhibited nonpolar nature with an average polarity of 67 for THCP and 64 for OMCP, respectively. THCP stationary phase shows high selectivity for analytes of different polarity and exhibits nice peak shapes, especially for aldehydes, alcohols and anilines that are prone to severe peak tailing in GC analysis. Interestingly, THCP stationary phase possesses superior resolving ability for aniline and benzenediol positional isomers while OMCP shows preferential selectivity for nonpolar analytes such as hexane isomers. Moreover, calix[4]pyrrole columns also have good thermal stability up to 260°C and repeatability with a relative standard deviation (RSD%) of less than 0.10% for run-to-run and less than 5.2% for column-to-column. This work demonstrates the unique separation performance of calix[4]pyrroles and their promising future as a new class of GC stationary phases. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Detection of adulterated Ginkgo biloba supplements using chromatographic and spectral fingerprints.

    PubMed

    Harnly, James M; Luthria, Devanand; Chen, Pei

    2012-01-01

    The fingerprints of 18 commercially available Ginkgo biloba supplements, 12 samples of raw G. biloba leaves, and three G. biloba standard reference materials from the National Institute of Standards and Technology were acquired directly (no chromatography) by UV spectrometry and after separation using HPLC with a diode array detector. The fingerprints consisted of the UV spectral images, the chromatographic images, and the areas of the 21 most prominent chromatographic peaks. Data were analyzed by principal component analysis and one-class soft independent modeling of class analogy (SIMCA). It was determined that three of the commercial products were adulterated with rutin, four with quercetin, and one with an unidentified flavonol glycoside. One-class SIMCA of the authentic products allowed the adulterated products to be easily distinguished using Q-residuals. Authentic supplements and raw leaf materials were easily distinguished. The finely powdered samples were also analyzed by near-IR (NIR) spectrometry. The authentic and adulterated products could not be distinguished by NIR spectrometry because of the excipients.

  19. Needle concentrator for gas chromatographic determination of BTEX in aqueous samples.

    PubMed

    Kubinec, Róbert; Berezkin, Victor G; Górová, Renáta; Addová, Gabriela; Mracnová, Helena; Soják, Ladislav

    2004-02-05

    A simple method of solventless extraction of volatile organic compounds (BTEX) from aqueous samples was developed and validated. A new arrangement of the full volume inside needle capillary adsorption trap (INCAT) device with Porapak Q as a sorbent material and wet alumina as a source of desorptive water vapour flow in a closed analytical system is presented. The analytical characteristics of developed device and of compared purge-and-trap (PTI) device for BTEX compounds are similar; the limits of detection as well as quantification are lower than 1 microg l(-1).

  20. Capillary gas chromatographic analysis of nerve agents using large volume injections.

    PubMed

    Degenhardt-Langelaan, C E; Kientz, C E

    1996-02-02

    The use of large volume injections has been studied for the verification of intact organophosphorus chemical warfare agents in water samples. As the use of ethyl acetate caused severe detection problems new potential solvents were evaluated. With the developed procedure, the nerve agents sarin, tabun, soman, DFP and VX can be determined in freshly prepared water samples at ppt levels. Except for the nerve agent tabun all other agents added to the water samples were still present after 8 days at 20-60% levels, if the pH of the water sample is adjusted to ca. 5 shortly after sampling and adjusted to pH 7 for analysis.

  1. Gas chromatographic/mass spectrometric and microbiological analyses on irradiated chicken

    NASA Astrophysics Data System (ADS)

    Parlato, A.; Calderaro, E.; Bartolotta, A.; D'Oca, M. C.; Giuffrida, S. A.; Brai, M.; Tranchina, L.; Agozzino, P.; Avellone, G.; Ferrugia, M.; Di Noto, A. M.; Caracappa, S.

    2007-08-01

    Ionizing radiation is widely used as treatment technique for food preservation. It involves among others reduction of microbial contamination, disinfestations, sprout inhibition and extension of shelf life of food. However, the commercialization of irradiated food requires the availability of reliable methods to identify irradiated foodstuffs. In this paper, we present results on the application to irradiated chicken of this method, based on the detection, in muscle and skin samples, of the peaks of ions 98 Da and 112 Da, in a ratio approximately 4:1, typical of radiation induced 2-dodecylcyclobutanones (2-DCB). Aim of the work was also to study the time stability of the measured parameters in samples irradiated at 3 and 5 kGy, and to verify the efficacy of the treatment from a microbiological point of view. Our results show that, one month after irradiation at 3 kGy, the method is suitable using the skin but not the muscle, while the measured parameters are detectable in both samples irradiated at 5 kGy. The microbial population was substantially reduced even at 3 kGy.

  2. Gas chromatographic analysis of infant formulas for total fatty acids, including trans fatty acids.

    PubMed

    Satchithanandam, Subramaniam; Fritsche, Jan; Rader, Jeanne I

    2002-01-01

    Twelve powdered and 13 liquid infant formulas were analyzed by using an extension of AOAC Official Method 996.01 for fat analysis in cereal products. Samples were hydrolyzed with 8 N HCl and extracted with ethyl and petroleum ethers. Fatty acid methyl esters were prepared by refluxing the mixed ether extracts with methanolic sodium hydroxide in the presence of 14% boron trifluoride in methanol. The extracts were analyzed by gas chromatography. In powdered formulas, saturated fatty acid (SFA) content (mean +/- SD; n = 12) was 41.05 +/- 3.94%, monounsaturated fatty acid (MUFA) content was 36.97 +/- 3.38%, polyunsaturated fatty acid (PUFA) content was 20.07 +/- 3.08%, and total trans fatty acid content was 1.30 +/- 1.27%. In liquid formulas, SFA content (mean +/- SD; n = 13) was 42.29 +/- 2.98%, MUFA content was 36.05 +/- 2.47%, PUFA content was 20.65 +/- 2.40%, and total trans fatty acid content was 0.88 +/- 0.54%. Total fat content in powdered formulas ranged from 4.4 to 5.5 g/100 kcal and linoleic acid content ranged from 868 to 1166 mg/100 kcal. In liquid formulas, total fat content ranged from 4.1 to 5.1 g/100 kcal and linoleic acid content ranged from 820 to 1100 mg/100 kcal. There were no significant differences between powdered and liquid infant formulas in concentrations of total fat, SFA, MUFA, PUFA, or trans fatty acids.

  3. A practical methodology to measure unbiased gas chromatographic retention factor vs. temperature relationships.

    PubMed

    Peng, Baijie; Kuo, Mei-Yi; Yang, Panhia; Hewitt, Joshua T; Boswell, Paul G

    2014-12-29

    Compound identification continues to be a major challenge. Gas chromatography-mass spectrometry (GC-MS) is a primary tool used for this purpose, but the GC retention information it provides is underutilized because existing retention databases are experimentally restrictive and unreliable. A methodology called "retention projection" has the potential to overcome these limitations, but it requires the retention factor (k) vs. T relationship of a compound to calculate its retention time. Direct methods of measuring k vs. T relationships from a series of isothermal runs are tedious and time-consuming. Instead, a series of temperature programs can be used to quickly measure the k vs. T relationships, but they are generally not as accurate when measured this way because they are strongly biased by non-ideal behavior of the GC system in each of the runs. In this work, we overcome that problem by using the retention times of 25 n-alkanes to back-calculate the effective temperature profile and hold-up time vs. T profiles produced in each of the six temperature programs. When the profiles were measured this way and taken into account, the k vs. T relationships measured from each of two different GC-MS instruments were nearly as accurate as the ones measured isothermally, showing less than two-fold more error. Furthermore, temperature-programmed retention times calculated in five other laboratories from the new k vs. T relationships had the same distribution of error as when they were calculated from k vs. T relationships measured isothermally. Free software was developed to make the methodology easy to use. The new methodology potentially provides a relatively fast and easy way to measure unbiased k vs. T relationships. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. A Practical Methodology to Measure Unbiased Gas Chromatographic Retention Factor vs. Temperature Relationships

    PubMed Central

    Peng, Baijie; Kuo, Mei-Yi; Yang, Panhia; Hewitt, Joshua T.; Boswell, Paul G.

    2014-01-01

    Compound identification continues to be a major challenge. Gas chromatography-mass spectrometry (GC-MS) is a primary tool used for this purpose, but the GC retention information it provides is underutilized because existing retention databases are experimentally restrictive and unreliable. A methodology called “retention projection” has the potential to overcome these limitations, but it requires the retention factor (k) vs. T relationship of a compound to calculate its retention time. Direct methods of measuring k vs. T relationships from a series of isothermal runs are tedious and time-consuming. Instead, a series of temperature programs can be used to quickly measure the k vs. T relationships, but they are generally not as accurate when measured this way because they are strongly biased by non-ideal behavior of the GC system in each of the runs. In this work, we overcome that problem by using the retention times of 25 n-alkanes to back-calculate the effective temperature profile and hold-up time vs. T profiles produced in each of six temperature programs. When the profiles were measured this way and taken into account, the k vs. T relationships measured from each of two different GC-MS instruments were nearly as accurate as the ones measured isothermally, showing less than 2-fold more error. Furthermore, temperature-programmed retention times calculated in five other labs from the new k vs. T relationships had the same distribution of error as when they were calculated from k vs. T relationships measured isothermally. Free software was developed to make the methodology easy to use. The new methodology potentially provides a relatively fast and easy way to measure unbiased k vs. T relationships. PMID:25496658

  5. Cross-column prediction of gas-chromatographic retention of polybrominated diphenyl ethers.

    PubMed

    D'Archivio, Angelo Antonio; Giannitto, Andrea; Maggi, Maria Anna

    2013-07-12

    In this paper, we predict the retention of polybrominated diphenyl ethers (PBDEs) in capillary gas-chromatography (GC) within a useful range of separation conditions. In a first stage of this study, quantitative structure-retention relationships (QSRRs) of PBDEs in six stationary phases with different polarity are established. The single-column QSRR models are generated using the retention data of 126 PBDE congeners by multilinear regression (MLR) coupled to genetic algorithm variable selection applied to a large set of theoretical molecular descriptors of different classes. A quite accurate fitting of experimental retentions is obtained for each of the six GC columns adopting five molecular descriptors. In a further step of this work six molecular descriptors were extracted within the set of molecular descriptors (17 variables) involved in the various single-column QSRRs. The selected molecular descriptors are combined with observed retentions of ten representative PBDEs, adopted as descriptors of the GC system. These quantities are considered as the independent variables of a multiple-column retention model able to simultaneously relate GC retention to PBDE molecular structure and kind of column. The quantitative structure/column-retention relationship is established using a multi-layer artificial neural network (ANN) as regression tool. To optimise the ANN model, a validation set is generated by selecting two out of the six calibration columns. Splitting of columns between training and validation sets, as well as selection of PBDE congeners to be used as column descriptors, is performed with the help of a principal component analysis on the retention data. Cross-column predictive performance of the final model is tested on a large external set consisting of retention data of 180 PBDEs collected in four separation conditions different from those considered in model calibration (different columns and/or temperature program). Copyright © 2013 Elsevier B.V. All

  6. Characterization of low-temperature cofired ceramic tiles as platforms for gas chromatographic separations.

    PubMed

    Darko, Ernest; Thurbide, Kevin B; Gerhardt, Geoff C; Michienzi, Joseph

    2013-06-04

    A gas chromatography (GC) column is fabricated within a low-temperature cofired ceramic (LTCC) tile, and its analytical properties are characterized. By using a dual-spiral design, a 100 μm wide square channel up to 15 m in length is produced within an 11 cm × 5.5 cm LTCC tile. The channel is dynamically coated with an OV-101 stationary phase that is cross-linked with dicumyl peroxide. While the uncoated LTCC tiles were able to separate a mixture of n-alkanes, the peak shapes were broad (base width of ~2 min) and tailing. In contrast to this, the coated LTCC tiles produced sharp (base width of ~8-10 s), symmetrical, well-resolved peaks for the same analytes. By using a 7.5 m long channel, about 15,000 plates were obtained for a dodecane test analyte. Further, the coated LTCC tiles were found to produce plate heights that were about 3-fold smaller than those obtained from a conventional capillary GC column of similar length, dimension, and coating operated under the same conditions. As a result, test analyte separations were slightly improved in the LTCC tiles, and their overall performance fared well. In terms of temperature programming, it was found that a series of n-alkanes separated on the LTCC tile provided a cumulative peak capacity of around 54 peaks when using C₈ to C₁₃ as analyte markers. Results indicate that LTCC tiles provide a viable and useful alternative platform for performing good quality GC separations.

  7. Detection of hydrogen chloride gas in air

    NASA Technical Reports Server (NTRS)

    Gregory, G. L.

    1978-01-01

    Launch vehicle effluent (LVE) monitoring is part of NASA's overall tropospheric and stratospheric environmental program. Following nine techniques are evaluated and developed in report: bubbler method, pH measurements, indicator tubes, microcoulometers, modified condensation nuclei counter, dual-isotope absorption, gas-filter correlation, chemiluminescent nitric oxide detection, chemiluminescent luminol-oxidation detection.

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

    PubMed

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

    2015-04-03

    The analysis of complex mixtures of permanent gases consisting of low molecular weight hydrocarbons, inert gases, and toxic species plays an increasingly important role in today's economy. A new gas chromatography detector based on vacuum ultraviolet (VUV) spectroscopy (GC-VUV), which simultaneously collects full scan (115-240 nm) VUV and UV absorption of eluting analytes, was applied to analyze mixtures of permanent gases. Sample mixtures ranged from off-gassing of decomposing Li-ion and Li-metal batteries to natural gas samples and water samples taken from private wells in close proximity to unconventional natural gas extraction. Gas chromatography separations were performed with a porous layer open tubular column. Components such as C1-C5 linear and branched hydrocarbons, water, oxygen, and nitrogen were separated and detected in natural gas and the headspace of natural gas-contaminated water samples. Of interest for the transport of lithium batteries were the detection of flammable and toxic gases, such as methane, ethylene, chloromethane, dimethyl ether, 1,3-butadiene, CS2, and methylproprionate, among others. Featured is the capability for deconvolution of co-eluting signals from different analytes. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    PubMed

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

    2016-04-29

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

  10. [Diol column as stationary phase for high performance liquid chromatographic analysis of carbohydrates in drinks with evaporative light scattering detection].

    PubMed

    Wei, Y; Guo, L; Ding, M Y

    2001-11-01

    A high performance liquid chromatographic method with a diol column and evaporative light scattering detector (ELSD) was established for the direct analysis of fructose, glucose, sucrose, maltose and raffinose in mixture. A separation column (Lichrospher 100 Diol, 250 mm x 4.0 mm i.d., 5 microns, Hewlett-Packard, USA) and a guard column (Zorbax Rx-SIL, 12.5 mm x 4.6 mm i.d., 5 microns) were used. The mobile phase was a mixture of dichloromethane-methanol (3.2:1, volume ratio). Regression equations revealed linear relationship (correlation coefficients: 0.995-0.999) between the mass of carbohydrates injected and the peak area of carbohydrates detected by ELSD. The detection limits of ELSD (S/N = 3) were about 0.20 microgram for all carbohydrates. This system could be used for the routine analysis of simple carbohydrates in some common drinks on market.

  11. Gas sensitive materials for gas detection and methods of making

    DOEpatents

    Trakhtenberg, Leonid Israilevich; Gerasimov, Genrikh Nikolaevich; Gromov, Vladimir Fedorovich; Rozenberg, Valeriya Isaakovna

    2014-07-15

    A gas sensitive material comprising SnO.sub.2 nanocrystals doped with In.sub.2O.sub.3 and an oxide of a platinum group metal, and a method of making the same. The platinum group metal is preferably Pd, but also may include Pt, Ru, Ir, and combinations thereof. The SnO.sub.2 nanocrystals have a specific surface of 7 or greater, preferably about 20 m2/g, and a mean particle size of between about 10 nm and about 100 nm, preferably about 40 nm. A gas detection device made from the gas sensitive material deposited on a substrate, the gas sensitive material configured as a part of a current measuring circuit in communication with a heat source.

  12. Gas sensitive materials for gas detection and method of making

    DOEpatents

    Trakhtenberg, Leonid Israilevich; Gerasimov, Genrikh Nikolaevich; Gromov, Vladimir Fedorovich; Rozenberg, Valeriya Isaakovna

    2012-12-25

    A gas sensitive material comprising SnO2 nanocrystals doped with In2O3 and an oxide of a platinum group metal, and a method of making the same. The platinum group metal is preferably Pd, but also may include Pt, Ru, Ir, and combinations thereof. The SnO2 nanocrystals have a specific surface of 7 or greater, preferably about 20 m2/g, and a mean particle size of between about 10 nm and about 100 nm, preferably about 40 nm. A gas detection device made from the gas sensitive material deposited on a substrate, the gas sensitive material configured as a part of a current measuring circuit in communication with a heat source.

  13. Gas chromatographic evaluation of pesticide residue contents in nectarines after non-toxic washing treatments.

    PubMed

    Pugliese, P; Moltó, J C; Damiani, P; Marín, R; Cossignani, L; Mañes, J

    2004-10-01

    Washing with aqueous solutions of citric acid, ethanol, glycerol, hydrogen peroxide, potassium permanganate, sodium metabisulfite, sodium laurylsulfate (SLS), sodium hypochlorite, and urea is evaluated for pesticide residue reduction in nectarines and compared with simple tap water washing. Residues of pesticides commonly utilized in nectarines (chlorpyrifos, fenarimol, iprodione, malathion, methidathion, myclobutanil, parathion and pirimicarb) are extracted with ethyl acetate and anhydrous sodium sulfate, extract is concentred and analyzed by GC with nitrogen-phosphorus detection. The formation of possible toxic by-products (chlorpyrifos oxon, malaoxon, methidaoxon and paraoxon methyl) is studied by GC-MS. No toxic by-products are identified in the extracts of the washed samples for the washing-time and concentrations studied, but high levels of sodium hypochlorite, hydrogen peroxide and potassium permanganate form oxons from the organophosphorus pesticides. Ethanol, glycerol and SLS solutions removed near the 50% of the pesticide residues. The other solutions were not more effective than tap water washing. The amount of pesticide removed by washings is related to its water solubility and octanol-water partition coefficient.

  14. Comprehensive two-dimensional gas chromatographic analysis of commercial lemon-flavored beverages.

    PubMed

    Komura, Hajime

    2006-10-01

    Fresh lemon juice and lemon-flavored beverages were analyzed by using comprehensive 2-D GC (GC x GC) with flame-ionization detection, with a nonpolar-polar column combination. A low-alcohol, ready-to-drink (RTD) beverage was also analyzed as fresh, and after deterioration for 12 days at 50 degrees C. Identification of some of the components in the 2-D plots was performed by comparison of peak positions of authentic standards and comparison with 1-D GC. However, without the aid of GC x GC-mass spectral data, only 24 components were identified; a large number of components remained unassigned. In some soft drinks obtained in the market, components indicative of deterioration, such as p-methylacetophenone and p-cymen-8-ol were already present in the products. In contrast, even upon heat challenge, a low-alcohol RTD beverage did not generate deterioration products of citral, such as p-methylacetophenone and the intermediates, p-menth-2-ene-1,8-diols. This was apparently related to the fact that the original formulation contained only a minute amount of the citral ingredient.

  15. Gas chromatographic method for assessing the dermal exposure of greenhouse applicators to dimethoate and malathion.

    PubMed

    Castro Cano, M L; Martínez Vidal, J L; Egea González, F J; Martínez Galera, M

    2001-08-01

    An analytical method is developed to determine potential and actual dermal exposure to dimethoate and malathion for agricultural workers using whole body dosimetry. The methodology described includes three different aspects: the validation of the analytical method incorporating a matrix effect for establishing performance parameters such as recovery rates (between 92% and 103% for both pesticides), limits of detection and quantitation, and precision of measurements (RSD < 10%); a field sampling strategy developing a procedure for collecting samples and carrying out field spikes and field blanks in order to ensure the stability of samples during transport, storage, and analysis; and finally, a quality control procedure for ensuring that data are under statistical control. The method is applied to evaluate the potential and actual dermal exposure as well as its distribution for a pesticide applicator and the applicator's assistant after a greenhouse application. Operator exposure levels of approximately 68 mL/h, and 25 mL/h in the case of the assistant, are found. The body areas most exposed are the lower body and hands.

  16. Miniaturized molecularly imprinted polymer extraction method for the gas chromatographic analysis of flavonoids.

    PubMed

    Nolvachai, Yada; Kulsing, Chadin; Boysen, Reinhard I; Hearn, Milton T W; Marriott, Philip J

    2014-04-01

    In this study, the use of monolithic molecularly imprinted polymers in a micropipette tip format allowing the simple and fast extraction of flavonoids from standard solutions and a black tea sample is demonstrated. The imprinted polymer employed quercetin, methacrylic acid or 4-vinylpyridine, and ethylene glycol dimethacrylate as template, functional monomer, and cross-linker, respectively. Surface morphologies of the quercetin-imprinted polymers and the corresponding nonimprinted polymers were characterized by SEM. Extraction of flavonoid standards was performed to evaluate the selectivity and recovery with these imprinted and nonimprinted polymers. Flavonoid compositions in aliquots eluted from the tips were identified using fast GC with flame ionization detection. Maximum specific capacities of 0.2, 5.7, and 16.0 mg/g for catechin, morin, and quercetin, respectively, were obtained with the imprinted polymer prepared with methacrylic acid, with the corresponding recoveries of 99.8, 98.8, and 95.4%, respectively. Efficient extraction by the quercetin-imprinted polymer of epicatechin, catechin, and quercetin from an apple-flavored black tea sample was achieved, with GC-MS employed for compound identification for both the tea and extracted samples.

  17. A minicomputer-automated array spectrometer for liquid-chromatographic detection of metabolites.

    PubMed

    Dessy, R E; Reynolds, W D; Nunn, W G; Titus, C A; Moler, G F

    1976-09-01

    A third-generation multiwavelength array spectrometer was developed as a detector for the high-resolution liquid-chromatographic characterization of metabolites. Components include a PDP-8/e minicomputer, matched pair of linear photodiode arrays, holographically-ruled gratings, fiber optics, flow cells, and high intensity xenon light source. The wavelength range is 256 nm differential with 1-nm resolution and can be adjusted from 200 to 800 nm. The system is capable of storing 20 spectra per second (200-456 nm) in a dual-beam mode. Special features include minicomputer-driven signal enhancement via integration as a function of signal strength. The display output includes presentation of the total absorption chromatogram vs. elution time in both real and post-run time as well as selectable single absorption band vs. elution time (post-run time). Application of this dedicated system is illustrated by the separation and charcterization of the metabolites of a carcinogen, 4-ethylsulfonyl-1 napthalenesulfonamide.

  18. Gas chromatographic/mass spectrometric analysis of polar components in weathered' gasoline/water matrix as an aid in identifying gasoline

    SciTech Connect

    Kanai, H.; Yazawa, L.; Maka, J. ); Inouye, V. ); Goo, R. ); Chun, C. )

    1991-01-01

    Gasoline contamination is often found in streams and in urban storm drainage systems. These samples are usually found as weathered' gasoline/water matrix. The identification of weathered' gasoline solely through gas chromatographic fingerprints' of hydrocarbon portion is difficult. The polar components of three different weathered' gasoline/water samples were analyzed by gas chromatography/mass spectrometry and compared to similar components of the same three gasolines by this technique. This study shows that large portions of gasoline additives are partitioned into the aqueous phase, and this information can be used as an aid in identifying a weathered' gasoline sample.

  19. Evaluation of two adsorbents for diffusive sampling and thermal desorption-gas chromatographic analysis of monoterpenes in air.

    PubMed

    Sunesson, A L; Sundgren, M; Levin, J O; Eriksson, K; Carlson, R

    1999-02-01

    Tube type samplers with two different adsorbents, Chromosorb 106 and Tenax TA, were evaluated by laboratory experiments and field tests for simultaneous diffusive sampling of alpha-pinene, beta-pinene and delta 3-carene and subsequent thermal desorption-gas chromatographic analysis. No statistically significant effects of exposure time, concentrations of monoterpenes or relative humidity were found for samplers with Chromosorb 106 when running a factorial design, with the exception of the adsorption of delta 3-carene, for which some weak effects were noted. Samplers with Tenax TA were affected by the sampling time as well as the concentration for all terpenes, with a strong interaction effect between these two factors. The terpenes showed good storage stability on both adsorbents. No effect of back-diffusion was noted when using Chromosorb 106, while Tenax TA showed some back-diffusion effects. The uptake rates, in ml min-1, for the terpenes on Chromosorb 106 were 0.36 for alpha-pinene, 0.36 for beta-pinene and 0.40 for delta 3-carene. The corresponding average values on Tenax TA were 0.30 for alpha-pinene, 0.32 for beta-pinene and 0.38 for delta 3-carene. The field validation proved that diffusive sampling on Chromosorb 106 agreed well with pumped sampling on charcoal for stationary samples, while the personal samples indicated a discrepancy of 25% between Chromosorb 106 and charcoal samples. Tenax TA generally gave lower results than Chromosorb 106 in all field samples. Samplers packed with Chromosorb 106 could be used to monitor terpene levels in workplaces such as sawmills. The major advantages with this method are the sampling procedure, which is simple to perform compared to other techniques, the easily automated analysis procedure and the possibility to reuse the samplers.

  20. Gas chromatographic-olfactometric aroma profile and quantitative analysis of volatile carbonyls of grilled beef from different finishing feed systems.

    PubMed

    Resconi, Virginia Celia; del Mar Campo, María; Montossi, Fabio; Ferreira, Vicente; Sañudo, Carlos; Escudero, Ana

    2012-06-01

    In this study, the important odor impact volatiles generated in the meat of grilled beef loin muscle were characterized. Animals were finished in 4 different diet systems: T₁, pasture (a mixture of Medicago sativa, Trifolium repens, and Festuca arundinacea); T₂, pasture supplemented with cracked corn grain (offered at 0.6% live weight, LW); T₃, pasture supplemented with cracked corn grain (offered at 1.2% LW); and T₄, concentrate (pellets with 85% corn and 12.8% sunflower, on a dry-matter basis) plus alfalfa hay (both ad libitum). Aroma compounds were assessed by dynamic headspace-solid phase extraction (DHS-SPE) and gas chromatographic-olfactometric (GC-O) analysis. Most odorants were carbonyl compounds, some of them reaching high GC-O scores, especially 1-octen-3-one, (E)-2-octenal, methional, and hexanal. A specific quantitative analysis of ketones and aldehydes was conducted through their derivatization with o-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine hydrochloride directly on the headspace trap and analyzed by GC-MS, with the purpose of studying the effect of finishing diet systems. From the 23 carbonyl compounds quantified, 2 were especially affected by the diet system; methional was higher in the treatment based on concentrates, whereas (E,E)-2,4-heptadienal was higher in the treatment based only in pastures. The results are discussed considering previous published productive and quality traits. The knowledge of how production factors, such as animal feeding, can affect the flavor of meat is of significant interest toward in achieving a high-quality and differentiated product. The development of more specific and efficient methodologies is necessary to analyze meat aroma compounds, which would be used as routine analysis, that is for product authentication. In the future, the use of this analysis would allow producing and designing specific foods according to different markets. © 2012 Institute of Food Technologists®

  1. Gas phase chemical detection with an integrated chemical analysis system

    SciTech Connect

    CASALNUOVO,STEPHEN A.; FRYE-MASON,GREGORY CHARLES; KOTTENSTETTE,RICHARD; HELLER,EDWIN J.; MATZKE,CAROLYN M.; LEWIS,PATRICK R.; MANGINELL,RONALD P.; BACA,ALBERT G.; HIETALA,VINCENT M.

    2000-04-12

    Microfabrication technology has been applied to the development of a miniature, multi-channel gas phase chemical laboratory that provides fast response, small size, and enhanced versatility and chemical discrimination. Each analysis channel includes a sample preconcentrator followed by a gas chromatographic separator and a chemically selective surface acoustic wave detector array to achieve high sensitivity and selectivity. The performance of the components, individually and collectively, is described.

  2. Semiconducting polymers for gas detection

    NASA Technical Reports Server (NTRS)

    Byrd, N. R.; Sheratte, M. B.

    1975-01-01

    Conjugated polyenes, and polyesters containing phthalocyanine in their backbone, were synthesized. These polymers were characterized by chemical analysis, thermogravimetric analysis, spectral analysis, and X-ray diffraction studies for crystallinity, as well as for their film-forming capability and gas/polymer interactions. Most of the polymers were relatively insensitive to water vapor up to 50 percent relative humidity, but the polyester/phthalocyanine (iron) polymer was relatively insensitive up to 100 percent RH. On the other hand, poly(p-dimethylaminophenylacetylene) was too conductive at 100 percent RH. Of the gases tested, the only ones that gave any evidence of interacting with the polymers were SO2, NOx, HCN and NH3. Poly(imidazole)/thiophene responded to each of these gases at all relative humidities, while the other polymers gave varying response, depending upon the RH. Thus, since most of these gases were electron-accepting, the electron-donating character of poly(imidazole)/thiophene substantiates the concept of electronegativity being the operating principle for interaction effects. Of the six polymers prepared, poly(imidazole)/thiophene first showed a very good response to smoldering cotton, but it later became nonresponsive; presumably due to oxidation effects.

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

    USGS Publications Warehouse

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

    1981-01-01

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

  4. Comparing different gas chromatographic methods for the quantification of bisphenol A (BPA) trace levels in paper and cardboard products from the market.

    PubMed

    Jurek, A; Leitner, E

    2015-01-01

    Bisphenol A (BPA; 4,4'-(propane-2,2-diyl)diphenol), a suspected endocrine disruptor with weak estrogenic activity, is used in a variety of consumer products, including paper and cardboard products used as food contact materials. The present study compared four different gas chromatographic methods for the analysis of BPA in paper and cardboard food packages. Eighteen different food packages were extracted and BPA was determined using two different derivatisation reactions--trimethylsilylation with N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and halide alkylation with pentafluorobenzoyl chloride (PFBOCl)--and four different separation and detection techniques. The BSTFA derivatives were quantified with (1) GC-MS in single-ion monitoring (SIM) mode with electron ionisation (EI-GC-MS) and (2) GC-MS/MS in multiple reaction monitoring (MRM) mode using electron ionisation (EI-GC-MS/MS); while the PFBOCl derivatives were quantified with (3) GC-MS using electron ionisation (EI-GC-MS) as well as (4) GC-MS with negative chemical ionisation (NCI-GC-MS). All developed methods showed good linearity (R(2) > 0.9938), precision (CV < 4.5% for reproducibility; CV < 2.2% for repeatability) and sensitivity, with limits of detection (LODs) between 0.02 µg kg(-1) for the pentafluorobenzoyl derivatives measured with the NCI-GC-MS method and 6 µg kg(-1) for the pentafluorobenzoyl derivatives determined with EI-GC-MS. Levels of BPA in the samples were in agreement for all methods, ranging from values below the limit of quantitation (LOQ) to 11.9 mg kg(-1) paper. In a last step, the maximum potential migration into food products was calculated for all tested paper and cardboard samples, assuming a 'worst case' scenario of 100% migration.

  5. Application of microwave-assisted desorption/headspace solid-phase microextraction as pretreatment step in the gas chromatographic determination of 1-naphthylamine in silica gel adsorbent.

    PubMed

    Yan, Cheing-Tong; Jen, Jen-Fon; Shih, Tung-Sheng

    2007-03-30

    Pretreatment of silica gel sample containing 1-naphthylamine by microwave-assisted desorption (MAD) coupled to in situ headspace solid phase microextraction (HS-SPME) has been investigated as a possible alternative to conventional methods prior to gas chromatographic (GC) analysis. The 1-naphthylamine desorbs from silica gel to headspace under microwave irradiation, and directly absorbs onto a SPME fiber located in a controlled-temperature headspace area. After being collected on the SPME fiber, and desorbed in the GC injection port, 1-naphthylamine is analyzed by GC-FID. Parameters that influence the extraction efficiency of the MAD/HS-SPME, such as the extraction media and its pH, the microwave irradiation power and irradiation time as well as desorption conditions of the GC injector, have been investigated. Experimental results indicate that the extraction of a 150mg silica gel sample by using 0.8ml of 1.0M NaOH solution and a PDMS/DVB fiber under high-powered irradiation (477W) for 5min maximizes the extraction efficiency. Desorption of 1-naphthylamine from the SPME fiber in GC injector is optimal at 250 degrees C held for 3min. The detection limit of method is 8.30ng. The detected quantity of 1-naphthylamine obtained by the proposed method is 33.3 times of that obtained by the conventional solvent extraction method for the silica gel sample containing 100ng of 1-naphthylamine. It provides a simple, fast, sensitive and organic-solvent-free pretreatment procedure prior to the analysis of 1-naphthylamine collected on a silica gel adsorbent.

  6. Gibbs energy additivity approaches to QSRR in generating gas chromatographic retention time for identification of fatty acid methyl ester.

    PubMed

    Pojjanapornpun, Siriluck; Aryusuk, Kornkanok; Lilitchan, Supathra; Krisnangkura, Kanit

    2017-02-06

    The Gibbs energy additivity method was used to correlate the retention time (t R) of common fatty acid methyl esters (FAMEs) to their chemical structures. The t R of 20 standard FAMEs eluted from three capillary columns of different polarities (ZB-WAXplus, BPX70, and SLB-IL111) under both isothermal gas chromatography and temperature-programmed gas chromatography (TPGC) conditions were accurately predicted. Also, the predicted t R of FAMEs prepared from flowering pak choi seed oil obtained by multistep TPGC with the BPX70 column were within 1.0% of the experimental t R. The predicted t R or mathematical t R (t R(math)) values could possibly be used as references in identification of common FAMEs. Hence, FAMEs prepared from horse mussel and fish oil capsules were chromatographed on the BPX70 and ZB-WAXplus columns in single-step and multistep TPGC. Identification was done by comparison of t R with the t R of standard FAMEs and with t R(math). Both showed correct identifications. The proposed model has six numeric constants. Five of six could be directly transferred to other columns of the same stationary phase. The first numeric constant (a), which contained the column phase ratio, could also be transferred with the adjustment of the column phase ratio to the actual phase ratio of the transferred column. Additionally, the numeric constants could be transferred across laboratories, with similar correction of the first numeric constant. The TPGC t R predicted with the transferred column constants were in good agreement with the reported experimental t R of FAMEs. Moreover, hexane was used in place of the conventional t M marker in the calculation. Hence, the experimental methods were much simplified and practically feasible. The proposed method for using t R(math) as the references would provide an alternative to the uses of real FAMEs as the references. It is simple and rapid and with good accuracy compared with the use of experimental t R as references.

  7. Rule-based expert system for evaluating the quality of long-term, in-situ, gas chromatographic measurements of atmospheric methane. Technical memo

    SciTech Connect

    Masarie, K.A.; Steele, L.P.; Lang, P.M.

    1991-11-01

    Methane is an important trace constituent of the earth's atmosphere because it is active both chemically and radiatively. The absorption of infrared radiation by atmospheric methane, and the rapid increase in the global atmospheric burden of methane over the past century combine to raise concerns that continued increases may contribute to global warming and climate change within the next century. The use of a rule-based expert system to assess the integrity of in situ gas chromatographic methane measurements made at the NOAA/CMDL Point Barrow, Alaska and Mauna Loa, Hawaii observatories is presented. The expert system flags ambient samples analyzed during chromatograph system instability and excludes them from further scientific analysis. The development and implementation of the expert system are described in detail. A comparison between data sets flagged by a human expert and by the expert system shows that the expert system can successfully reproduce the efforts of a human when evaluating gas chromatograph system stability. Advantages and limitations of the use of an expert system for the task are also discussed.

  8. Air Monitoring for Hazardous Gas Detection

    NASA Technical Reports Server (NTRS)

    Arkin, C. Richard; Griffin, Timothy P.; Adams, Frederick W.; Naylor, Guy; Haskell, William; Floyd, David; Curley, Charles; Follistein, Duke W.

    2004-01-01

    The Hazardous Gas Detection Lab (HGDL) at Kennedy Space Center is involved in the design and development of instrumentation that can detect and quantify various hazardous gases. Traditionally these systems are designed for leak detection of the cryogenic gases used for the propulsion of the Shuttle and other vehicles. Mass spectrometers are the basis of these systems, which provide excellent quantitation, sensitivity, selectivity, response times and detection limits. A Table lists common gases monitored for aerospace applications. The first five gases, hydrogen, helium, nitrogen, oxygen, and argon are historically the focus of the HGDL.

  9. Infrared hyperspectral imaging sensor for gas detection

    NASA Astrophysics Data System (ADS)

    Hinnrichs, Michele

    2000-11-01

    A small light weight man portable imaging spectrometer has many applications; gas leak detection, flare analysis, threat warning, chemical agent detection, just to name a few. With support from the US Air Force and Navy, Pacific Advanced Technology has developed a small man portable hyperspectral imaging sensor with an embedded DSP processor for real time processing that is capable of remotely imaging various targets such as gas plums, flames and camouflaged targets. Based upon their spectral signature the species and concentration of gases can be determined. This system has been field tested at numerous places including White Mountain, CA, Edwards AFB, and Vandenberg AFB. Recently evaluation of the system for gas detection has been performed. This paper presents these results. The system uses a conventional infrared camera fitted with a diffractive optic that images as well as disperses the incident radiation to form spectral images that are collected in band sequential mode. Because the diffractive optic performs both imaging and spectral filtering, the lens system consists of only a single element that is small, light weight and robust, thus allowing man portability. The number of spectral bands are programmable such that only those bands of interest need to be collected. The system is entirely passive, therefore, easily used in a covert operation. Currently Pacific Advanced Technology is working on the next generation of this camera system that will have both an embedded processor as well as an embedded digital signal processor in a small hand held camera configuration. This will allow the implementation of signal and image processing algorithms for gas detection and identification in real time. This paper presents field test data on gas detection and identification as well as discuss the signal and image processing used to enhance the gas visibility. Flow rates as low as 0.01 cubic feet per minute have been imaged with this system.

  10. High-pressure/high-temperature gas-solubility study in hydrogen-phenanthrene and methane-phenanthrene systems using static and chromatographic techniques

    SciTech Connect

    Malone, P.V.

    1987-01-01

    The design and discovery of sources for alternative energy such as coal liquefaction has become of major importance over the past two decades. One of the major problems in such design in the lack of available data, particularly, for gas solubility in polycyclic aromatics at high temperature and pressure. Static and gas-liquid partition chromatographic methods were used for the study of hydrogen-phenanthrene and methane-phenanthrene systems. The static data for these two binaries were taken along 398.2, 423.2, 448.2, and 473.2 K isotherms up to 25.23 MPa. Gas-liquid partition chromatography was used to study the infinite dilution behavior of methane, ethane, propane, n-butane, and carbon dioxide in the hydrogen-phenanthrene system as well as hydrogen, ethane, n-butane, and carbon dioxide in the methane-phenanthrene binary. The principle objective was to examine the role of the elution gas. Temperatures were along the same isotherms as the static data and up to 20.77 MPa. With the exception of carbon dioxide, Henry's constants were calculated for all systems. Expressions for the heat of solution as a function of pressure were derived for both binary and chromatographic data. Estimates of delta H/sub i/sup sol/ at high pressure were presented.

  11. Detection of gas atoms with carbon nanotubes

    PubMed Central

    Arash, B.; Wang, Q.

    2013-01-01

    Owning to their unparalleled sensitivity resolution, nanomechanical resonators have excellent capabilities in design of nano-sensors for gas detection. The current challenge is to develop new designs of the resonators for differentiating distinct gas atoms with a recognizably high sensitivity. In this work, the characteristics of impulse wave propagation in carbon nanotube-based sensors are investigated using molecular dynamics simulations to provide a new method for detection of noble gases. A sensitivity index based on wave velocity shifts in a single-walled carbon nanotube, induced by surrounding gas atoms, is defined to explore the efficiency of the nano-sensor. The simulation results indicate that the nano-sensor is able to differentiate distinct noble gases at the same environmental temperature and pressure. The inertia and the strengthening effects by the gases on wave characteristics of carbon nanotubes are particularly discussed, and a continuum mechanics shell model is developed to interpret the effects.

  12. Method for measuring changes in the atmospheric O2/N2 ratio by a gas chromatograph equipped with a thermal conductivity detector

    NASA Astrophysics Data System (ADS)

    Tohjima, Yasunori

    2000-06-01

    We present a method for measuring changes in the atmospheric O2/N2 ratio based on data from a gas chromatograph (GC) equipped with a thermal conductivity detector (TCD). In this method, O2 and N2 in an air sample are separated on a column filled with molecular sieve 5A with H2 carrier gas. Since the separated O2 includes Ar, which has a retention time similar to that of O2, the (O2+Ar)/N2 ratio is actually measured. The change in the measured (O2+Ar)/N2 ratio can be easily converted to that in the O2/N2 ratio with a very small error based on the fact that the atmospheric Ar/N2 ratio is almost constant. The improvements to achieve the high-precision measurement include stabilization of the pressure at the GC column head and at the outlets of the TCD and the sample loop. Additionally, the precision is improved statistically by repeating alternate analyses of sample and a reference gas. The standard deviation of the replicate cycles of reference and sample analyses is about 18 per meg (corresponding to 3.8 parts per million (ppm) O2 in air). This means that the standard error is about 7 per meg (1.5 ppm O2 in air) for seven cycles of alternate analyses, which takes about 70 min. The response of this method is likely to have a 2% nonlinearity. Ambient air samples are collected under pressure in glass flasks equipped with two stopcocks sealed by Viton O-rings at both ends. Pressure depletion in the flask during the O2/N2 measurement does not cause any detectable change in the O2/N2 ratio, but the O2/N2 ratio in the flask was found to gradually decrease during the storage period. We also present preliminary results from air samples collected at Hateruma Island (latitude 24°03'N, longitude 123°49') from July 1997 through March 1999. The observed O2/N2 ratios clearly show a seasonal variation, increasing in spring and summer and decreasing in autumn and winter.

  13. Good odorant practices ensure safer operations. [Natural gas odorant detection methods

    SciTech Connect

    Oudman, P. )

    1993-12-01

    Regulations in Canada and the US require that combustible gas used as a fuel be odorized at such a level that a concentration in air of one-fifth the lower explosive limit the gas can be readily detected and recognized by a person with a normal sense of smell. These regulations do not specify how the odorant level should be determined. However, since the requirement is related to smell, the level should be determined by an olfactory method. There are two odorant monitoring methods commonly used by gas companies, the olfactory (odorometer) and the instrumentation (gas chromatograph) methods. The instrument method provides only quantitative results, which somehow must be related to an olfactory response. This paper discusses these methods.

  14. Automated Hydrogen Gas Leak Detection System

    NASA Technical Reports Server (NTRS)

    1995-01-01

    The Gencorp Aerojet Automated Hydrogen Gas Leak Detection System was developed through the cooperation of industry, academia, and the Government. Although the original purpose of the system was to detect leaks in the main engine of the space shuttle while on the launch pad, it also has significant commercial potential in applications for which there are no existing commercial systems. With high sensitivity, the system can detect hydrogen leaks at low concentrations in inert environments. The sensors are integrated with hardware and software to form a complete system. Several of these systems have already been purchased for use on the Ford Motor Company assembly line for natural gas vehicles. This system to detect trace hydrogen gas leaks from pressurized systems consists of a microprocessor-based control unit that operates a network of sensors. The sensors can be deployed around pipes, connectors, flanges, and tanks of pressurized systems where leaks may occur. The control unit monitors the sensors and provides the operator with a visual representation of the magnitude and locations of the leak as a function of time. The system can be customized to fit the user's needs; for example, it can monitor and display the condition of the flanges and fittings associated with the tank of a natural gas vehicle.

  15. Gas chromatographic/tandem mass spectrometric identification and quantitation of metabolic 4-acetyltoluene-2,4-diamine from the F344 rat.

    PubMed

    Bartels, M J; Timchalk, C; Smith, F A

    1993-03-01

    2,4-Toluenediamine (TDA) and 2,4-toluenediisocyanate (TDI) are metabolized in the Fischer 344 rat to monoacetyl-2,4-toluenediamine (Ac-TDA) and diacetyl-2,4-toluenediamine (Ac2-TDA). A gas chromatographic/tandem mass spectrometric (GC/MS/MS) method was developed to characterize the structure of the Ac-TDA metabolite (2-acetyl versus 4-acetyl), as a D3-diacetyl-TDA derivative. This method was also shown to be useful in the measurement of urinary levels of TDA, Ac-TDA and Ac2-TDA. Urine samples (1.0 g) were adjusted to pH 6.5-7.0, fortified with the internal standard D9-Ac2-TDA (D3-ring + D3-acetyl x 2) and extracted with ethyl acetate (2 x 2 ml). The extract residues were then derivatized with D6-acetic anhydride and analyzed via electron impact GC/MS/MS. MS/MS analysis of the D3-Ac2-TDA derivative of the two Ac-TDA isomers yielded different daughter ion spectra from the common parent ion (m/z 209). Analysis of urine samples from rats administered TDA (p.o., i.v.) and TDI (p.o., inhalation) indicated that all of the metabolic Ac-TDA from these test materials was the 4-acetyl-TDA isomer. Subsequent GC/MS analysis of the heptafluorobutyric acid (HFBA) derivative of this metabolite confirmed the MS/MS results. Selected ion monitoring of the M-acetyl daughter ions from the derivatized TDA, Ac-TDA and Ac2-TDA was shown to be a useful technique for quantitation of urinary levels of these compounds, with a detection limit of 35 ng g-1 urine for TDA and 10 ng g-1 urine for Ac-TDA and Ac2-TDA.

  16. Performance characteristics of an automated gas chromatograph-ion trap mass spectrometer system used for the 1995 Southern Oxidants Study field investigation in Nashville, Tennessee

    NASA Astrophysics Data System (ADS)

    Daughtrey, E. Hunter; Adams, Jeffrey R.; Oliver, Karen D.; Kronmiller, Keith G.; McClenny, William A.

    1998-09-01

    A trailer-deployed automated gas chromatograph-mass spectrometer (autoGC-MS) system capable of making continuous hourly measurements was used to determine volatile organic compounds (VOCs) in ambient air at New Hendersonville, Tennessee, and Research Triangle Park, North Carolina, in 1995. The system configuration, including the autoGC-MS, trailer and transfer line, siting, and sampling plan and schedule, is described. The autoGC-MS system employs a pair of matched sorbent traps to allow simultaneous sampling and desorption. Desorption is followed by Stirling engine cryofocusing and subsequent GC separation and mass spectral identification and quantification. Quality control measurements described include evaluating precision and accuracy of replicate analyses of independently supplied audit and round-robin canisters and determining the completeness of the data sets taken in Tennessee. Data quality objectives for precision (±10%) and accuracy (±20%) of 10- to 20-ppbv audit canisters and a completeness of >75% data capture were met. Quality assurance measures used in reviewing the data set include retention time stability, calibration checks, frequency distribution checks, and checks of the mass spectra. Special procedures and tests were used to minimize sorbent trap artifacts, to verify the quality of a standard prepared in our laboratory, and to prove the integrity of the insulated, heated transfer line. A rigorous determination of total system blank concentration levels using humidified scientific air spiked with ozone allowed estimation of method detection limits, ranging from 0.01 to 1.0 ppb C, for most of the 100 target compounds, which were a composite list of the target compounds for the Photochemical Assessment Monitoring Station network, those for Environmental Protection Agency method TO-14, and selected oxygenated VOCs.

  17. Polymer-coated micro-optofluidic ring resonator detector for a comprehensive two-dimensional gas chromatographic microsystem: μGC ×μGC-μOFRR.

    PubMed

    Collin, William R; Scholten, Kee W; Fan, Xudong; Paul, Dibyadeep; Kurabayashi, Katsuo; Zellers, Edward T

    2016-01-07

    We describe first results from a micro-analytical subsystem that integrates a detector comprising a polymer-coated micro-optofluidic ring resonator (μOFRR) chip with a microfabricated separation module capable of performing thermally modulated comprehensive two-dimensional gas chromatographic separations (μGC ×μGC) of volatile organic compound (VOC) mixtures. The 2 × 2 cm μOFRR chip consists of a hollow, contoured SiO(x) cylinder (250 μm i.d.; 1.2 μm wall thickness) grown from a Si substrate, and integrated optical and fluidic interconnection features. By coupling to a 1550 nm tunable laser and photodetector via an optical fiber taper, whispering gallery mode (WGM) resonances were generated within the μOFRR wall, and shifts in the WGM wavelength caused by transient sorption of eluting vapors into the PDMS film lining the μOFRR cylinder were monitored. Isothermal separations of a simple alkane mixture using a PDMS coated 1st-dimension ((1)D) μcolumn and an OV-215-coated 2nd-dimension ((2)D) μcolumn confirmed that efficient μGC ×μGC-μOFRR analyses could be performed and that responses were dominated by film-swelling. Subsequent tests with more diverse VOC mixtures demonstrated that the modulated peak width and the VOC sensitivity were inversely proportional to the vapor pressure of the analyte. Modulated peaks as narrow as 120 ms and limits of detection in the low-ng range were achieved. Structured contour plots generated with the μOFRR and a reference FID were comparable.

  18. Gas chromatographic/mass spectrometric determination of 3-methoxy-1,2-propanediol and cyclic diglycerols, by-products of technical glycerol, in wine: interlaboratory study.

    PubMed

    Fauhl, Carsten; Wittkowski, Reiner; Lofthouse, Janice; Hird, Simon; Brereton, Paul; Versini, Giuseppe; Lees, Michele; Guillou, Claude

    2004-01-01

    The aim of the present study was to provide the official wine control authorities with an internationally validated method for the determination of 3-methoxy-1,2-propanediol (3-MPD) and cyclic diglycerols (CycDs)-both of which are recognized as impurities of technical glycerol-in different types of wine. Because glycerol gives a sweet flavor to wine and contributes to its full-body taste, an economic incentive is to add glycerol to a wine to mask its poor quality. Furthermore, it is known that glycerol, depending on whether it is produced from triglycerides or petrochemicals, may contain considerable amounts of 3-MPD in the first case or CycDs in the second. However, because these compounds are not natural wine components, it is possible to detect glycerol added to wine illegally by determining the above-mentioned by-products. To this end, one of the published methods was adopted, modified, and tested in a collaborative study. The method is based on gas chromatographic/mass spectrometric analysis of diethyl ether extracts after salting out with potassium carbonate. The interlaboratory study for the determination of 3-MPD and CycDs in wine was performed in 11 laboratories in 4 countries. Wine samples were prepared and sent to participants as 5 blind duplicate test materials and 1 single test material. The concentrations covered ranges of 0.1-0.8 mg/L for 3-MPD and 0.5-1.5 mg/L for CycDs. The precision of the method was within the range predicted by the Horwitz equation. HORRAT values obtained for 3-MPD ranged from 0.8 to 1.7, and those obtained for CycDs ranged from 0.9 to 1.3. Average recoveries were 104 and 109%, respectively.

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

    PubMed

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

    2017-03-07

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

  20. Field gas chromatograph analyses of gases from a glowing dome at Merapi volcano, Java, Indonesia, 1977, 1978, 1979

    NASA Astrophysics Data System (ADS)

    Le Guern, F.; Gerlach, T. M.; Nohl, A.

    1982-12-01

    A new field gas chromatograph (FGC) and conventional evacuated bottle (EB) techniques have been used to study high temperature (> 600°C) volcanic gases from Merapi Volcano, Indonesia during 1977, 1978, and 1979. The FGC design allows analysis of H 2O, CO 2, SO 2, H 2S, H 2, COS, CH 4, CO, N 2, Ar, and O 2 in a manner that prevents loss of sulfur and water by condensation, inhibits corrosion from reactions of gases with lead-in tubes, and minimizes atmospheric contamination. The FGC analyses are highly superior to the EB data especially with respect to prevention of sulfur loss from reaction of SO 2 and H 2S. In addition to providing much improved H 2S data, the FGC system minimizes oxidation of H 2 and CO from contaminating atmospheric O 2 because of the elimination of a lengthy time interval between collection and analysis. Thermodynamic calculations indicated small errors for H 2 and CH 4 in the 1978 analyses provided by the proto-type FGC device. A later model FGC provided excellent analyses that were shown by thermodynamic calculations to be nearly equilibrium mixtures, requiring only minor corrections. The Merapi gases are H 2O-rich (88-95%) containing small amounts of CO 2 (3.5 to 7.5%), SO 2 (0.3 to 1.2%), and H 2S (0.3 to 1.2%). They resemble "excess volatiles" (Rubey,1955) except for too high a sulfur content. Thermodynamic calculations based on the analyses indicate that the gases were once at temperatures of at least 915°C with O 2 fugacities near quartz -magnetite-fayalite and that they have not been significantly diluted by disequilibrium admixture of meteoric water below these temperatures. This conclusion takes on special importance because stable isotope studies (Allard, 1980, 1982) of Merapi gases have shown that the water is meteoric and that much of the carbon and sulfur could be from sedimentary sources. The Merapi gases, therefore, may be "magmatic" even though they are not "juvenile" but recycled crustal volatiles.

  1. Gas chromatographic vapor pressure determination of atmospherically relevant oxidation products of β-caryophyllene and α-pinene

    NASA Astrophysics Data System (ADS)

    Hartonen, Kari; Parshintsev, Jevgeni; Vilja, Vesa-Pekka; Tiala, Heidi; Knuuti, Sinivuokko; Lai, Ching Kwan; Riekkola, Marja-Liisa

    2013-12-01

    Vapor pressures (subcooled liquid, pliquid) of atmospherically relevant oxidation products of β-caryophyllene (β-caryophyllene aldehyde 0.18 ± 0.03 Pa and β-nocaryophyllene aldehyde 0.17 ± 0.03 Pa), and α-pinene (pinonaldehyde 16.8 ± 0.20 Pa, cis-pinic acid 0.12 ± 0.06 Pa, and cis-pinonic acid 0.99 ± 0.19 Pa) at 298 K were obtained by gas chromatography with flame ionization detection (FID) and mass spectrometric (MS) detection. The effects of stationary phase polarity and column film thickness on the vapor pressure values were investigated. Increase in stationary phase polarity provided smaller values, while increase in film thickness gave slightly higher values. Values for vapor pressure were at least two orders of magnitude lower when obtained by a method utilizing vaporization enthalpy (determined by gas chromatography-mass spectrometry) than by retention index method. Finally, the results were compared with values calculated by group contribution theory. For the β-caryophyllene oxidation products, the values measured by gas chromatography were slightly lower than those obtained by theoretical calculations. The opposite trend was observed for the α-pinene oxidation products. The methods based on gas chromatography are concluded to be highly useful for the determination of vapor pressures of semi-volatile compounds. Except for the most polar pinic and pinonic acids, differences between vapor pressure values obtained by GC-FID and GC-MS were small. Since GC-MS provides structural information simultaneously, the use of GC-MS is recommended.

  2. Parabens determination in cosmetic and personal care products exploiting a multi-syringe chromatographic (MSC) system and chemiluminescent detection.

    PubMed

    Rodas, Melisa; Portugal, Lindomar A; Avivar, Jessica; Estela, José Manuel; Cerdà, Víctor

    2015-10-01

    Parabens are widely used in dairy products, such as in cosmetics and personal care products. Thus, in this work a multi-syringe chromatographic (MSC) system is proposed for the first time for the determination of four parabens: methylparaben (MP), ethylparaben (EP), propylparaben (PP) and butylparaben (BP) in cosmetics and personal care products, as a simpler, practical, and low cost alternative to HPLC methods. Separation was achieved using a 5mm-long precolumn of reversed phase C18 and multi-isocratic separation, i.e. using two consecutive mobile phases, 12:88 acetonitrile:water and 28:72 acetonitrile:water. The use of a multi-syringe buret allowed the easy implementation of chemiluminescent (CL) detection after separation. The chemiluminescent detection is based on the reduction of Ce(IV) by p-hydroxybenzoic acid, product of the acid hydrolysis of parabens, to excite rhodamine 6G (Rho 6G) and measure the resulting light emission. Multivariate designs combined with the concepts of multiple response treatments and desirability functions have been employed to simultaneously optimize and evaluate the responses. The optimized method has proved to be sensitive and precise, obtaining limits of detection between 20 and 40 µg L(-1) and RSD <4.9% in all cases. The method was satisfactorily applied to cosmetics and personal care products, obtaining no significant differences at a confidence level of 95% comparing with the HPLC reference method. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Enhancement of fluorescence detection in chromatographic methods by computer analysis of second order data. Progress report, August 1, 1990--October 1, 1993

    SciTech Connect

    Rutan, S.C.

    1993-12-31

    Two types of experiments were studied during the course of this project. The first was liquid chromatographic separation of polyaromatic hydrocarbons (PAHs) followed by detection with full-spectrum fluorescence spectroscopy using anintensified diode array detector. Methods such as generalized rank annihilation and adaptive Kalman filtering were developed and evaluated. The second was the use of a thin-layer chromatographic or planar electrophoretic separation of analytes (amino acids or enzymes). The analytes are then reacted with a reagent or enzyme substrate; the reaction is followed by fluorescence intensity vs time and migration distance, and kinetic analysis is used to quantify the component species.

  4. Minimum detectable gas concentration performance evaluation method for gas leak infrared imaging detection systems.

    PubMed

    Zhang, Xu; Jin, Weiqi; Li, Jiakun; Wang, Xia; Li, Shuo

    2017-04-01

    Thermal imaging technology is an effective means of detecting hazardous gas leaks. Much attention has been paid to evaluation of the performance of gas leak infrared imaging detection systems due to several potential applications. The minimum resolvable temperature difference (MRTD) and the minimum detectable temperature difference (MDTD) are commonly used as the main indicators of thermal imaging system performance. This paper establishes a minimum detectable gas concentration (MDGC) performance evaluation model based on the definition and derivation of MDTD. We proposed the direct calculation and equivalent calculation method of MDGC based on the MDTD measurement system. We build an experimental MDGC measurement system, which indicates the MDGC model can describe the detection performance of a thermal imaging system to typical gases. The direct calculation, equivalent calculation, and direct measurement results are consistent. The MDGC and the minimum resolvable gas concentration (MRGC) model can effectively describe the performance of "detection" and "spatial detail resolution" of thermal imaging systems to gas leak, respectively, and constitute the main performance indicators of gas leak detection systems.

  5. Gas-chromatographic studies of the sorption thermodynamics of adamantanes on a carbon adsorbent modified with polyethylene glycol with β-cyclodextrin additives

    NASA Astrophysics Data System (ADS)

    Yashkin, S. N.; Ageeva, Yu. A.

    2013-11-01

    The thermodynamic characteristics of sorption of adamantane and its derivatives on a mixed stationary phase consisting of a graphite-like solid substrate, polyethylene glycol, and β-cyclodextrin (βCD) were determined by gas chromatography. The introduction of β-CD additives to a polar polymer matrix was shown to considerably decrease the chromatographic retention of the sorbates, which is evidence of the macrocyclic effect. The presence of β-CD molecules was found to increase the selective properties of the mixed sorbent with respect to the structural isomers of adamantanes.

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

    PubMed

    Rogosa, M; Love, L L

    1968-02-01

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

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

    PubMed Central

    Rogosa, M.; Love, L. L.

    1968-01-01

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

  8. A quantitative gas-liquid chromatographic method for the estimation of hecogenin and tigogenin in the leaves, juice and sapogenin concentrates of Agave sisalana.

    PubMed

    Cripps, A L; Blunden, G

    1978-05-01

    A gas-liquid chromatographic method has been devised for the routine estimation of the hecogenin [3beta-hydroxy-(25R)-5beta-spirostan-12-one] and tigogenin [ (25R)-5beta-spirostan-3beta-ol] contents of Agave sisalana leaf and juice samples and of the crude sapogenin concentrates known as "coffee grounds". Because of partial degradation of the sapogenins in the GLC system it was found necessary to acetylate the compounds prior to their estimation. In East African samples the tigogenin proportion of the total sapogenin content is usually about 10%. At this level, the 95% inverse tolerance limits on predicted tigogenin weights are approximately +/- 7%.

  9. Determination of fluoxetine and norfluoxetine in plasma by gas chromatography with electron-capture detection

    SciTech Connect

    Nash, J.F.; Bopp, R.J.; Carmichael, R.H.; Farid, K.Z.; Lemberger, L.

    1982-10-01

    This gas-chromatographic method for assay of fluoxetine and norfluoxetine in human plasma involves extraction of the drugs and use of a /sup 63/Ni electron-capture detector. The linear range of detection is 25 to 800 micrograms/L for each drug. Overall precision (CV) in the concentration range of 10 to 100 micrograms/L for both drugs was approximately 10%. Accuracy (relative error) in the same concentration range was approximately +10%. None of the commonly prescribed antidepressants or tranquilizers that we tested interfere with the assay.

  10. Immuno-Chromatographic Wicking Assay for the Rapid Detection of Chikungunya Viral Antigens in Mosquitoes (Diptera: Culicidae).

    PubMed

    Hinson, Juanita M; Davé, Sonia; McMenamy, Scott S; Davé, Kirti; Turell, Michael J

    2015-07-01

    The outbreak of disease caused by chikungunya virus (CHIKV) in 2006 and the recent spread of this virus to the Americas in 2013 indicate the potential for this virus to spread and cause significant disease. However, there are currently no accurate and reliable field-usable, diagnostic methods to provide critical, real-time information for early detection of CHIKV within the vector populations in order to implement appropriate vector control and personal protective measures. In this article, we report the ability of an immuno-chromatographic assay developed by VecTOR Test Systems Inc. to detect CHIKV in a pool of female Aedes mosquitoes containing a single CHIKV-infected mosquito. The CHIKV dipstick assay was simple to use, did not require a cold chain, and provided clear results within 1 h. It was highly specific and did not cross-react with samples spiked with a variety of other alpha, bunya, and flaviviruses. The CHIKV assay can provide real-time critical information on the presence of CHIKV in mosquitoes to public health personnel. Results from this assay will allow a rapid threat assessment and the focusing of vector control measures in high-risk areas.

  11. Detection of arecoline by simple high-performance thin-layer chromatographic method in Indian nontobacco pan masala

    PubMed Central

    Adhikari, Anjan; Hazra, Alok Kumar; Sur, Tapas Kumar

    2015-01-01

    Chewing the habit of blended pan masala containing areca nut with or without tobacco is a common practice in the Indian subcontinent. Arecoline, a pyridine alkaloid presence in areca nut alarmed for oral carcinogenesis and strictly prohibited in the western world. However, in India using blended pan masala is very popular among young and old individuals. In this context, we aimed to detect arecoline in Indian blended nontobacco pan masala sold in Kolkata using a simple densitometric high-performance thin-layer chromatographic (HPTLC) method and for alarming their use in common people. Eleven popularly Indian blended nontobacco pan masala were collected from the territory of Kolkata and isolated arecoline, following solvent extraction method derived for pyridine alkaloid. The quantitative analysis of arecoline was measured using automated software-based HPTLC instruments and validated the method according to International Conference on Harmonization guidelines. Arecoline was detected in all 11 blended nontobacco pan masala samples in a range of minimum 130 to maximum 415 μg/g dry samples. Arecoline is hazardous carcinogenic compound, so the use of Indian blended nontobacco pan masala should be restricted. Further, the method was found suitable for routine quantitative analysis of arecoline in areca nut containing substances. PMID:26605162

  12. Cleaning validation 2: development and validation of an ion chromatographic method for the detection of traces of CIP-100 detergent.

    PubMed

    Resto, Wilfredo; Hernández, Darimar; Rey, Rosamil; Colón, Héctor; Zayas, José

    2007-05-09

    A cleaning validation method, ion chromatographic method with conductivity detection was developed and validated for the determination of traces of a clean-in-place (CIP) detergent. It was shown to be linear with a squared correlation coefficient (r(2)) of 0.9999 and average recoveries of 71.4% (area response factor) from stainless steel surfaces and 101% from cotton. The repeatability was found to be 2.17% and an intermediate precision of 1.88% across the range. The method was also shown to be sensitive with a detection limit (DL) of 0.13 ppm and a quantitation limit (QL) of 0.39 ppm for EDTA, which translates to less than 1 microL of CIP diluted in 100mL of diluent in both cases. The EDTA signal was well resolved from typical ions encountered in water samples or any other interference presented from swabs and surfaces. The method could be applied to cleaning validation samples. The validated method could be included as a suitable one for rapid and reliable cleaning validation program.

  13. Detection of arecoline by simple high-performance thin-layer chromatographic method in Indian nontobacco pan masala.

    PubMed

    Adhikari, Anjan; Hazra, Alok Kumar; Sur, Tapas Kumar

    2015-01-01

    Chewing the habit of blended pan masala containing areca nut with or without tobacco is a common practice in the Indian subcontinent. Arecoline, a pyridine alkaloid presence in areca nut alarmed for oral carcinogenesis and strictly prohibited in the western world. However, in India using blended pan masala is very popular among young and old individuals. In this context, we aimed to detect arecoline in Indian blended nontobacco pan masala sold in Kolkata using a simple densitometric high-performance thin-layer chromatographic (HPTLC) method and for alarming their use in common people. Eleven popularly Indian blended nontobacco pan masala were collected from the territory of Kolkata and isolated arecoline, following solvent extraction method derived for pyridine alkaloid. The quantitative analysis of arecoline was measured using automated software-based HPTLC instruments and validated the method according to International Conference on Harmonization guidelines. Arecoline was detected in all 11 blended nontobacco pan masala samples in a range of minimum 130 to maximum 415 μg/g dry samples. Arecoline is hazardous carcinogenic compound, so the use of Indian blended nontobacco pan masala should be restricted. Further, the method was found suitable for routine quantitative analysis of arecoline in areca nut containing substances.

  14. Heterodyne method for high specificity gas detection.

    NASA Technical Reports Server (NTRS)

    Dimeff, J.; Donaldson, R. W.; Gunter, W. D., Jr.; Jaynes, D. N.; Margozzi, A. P.; Deboo, G. J.; Mcclatchie, E. A.; Williams, K. G.

    1971-01-01

    This paper describes a new technique for measuring trace quantities of gases. The technique involves the use of a reference cell (containing a known amount of the gas being sought) and a sample cell (containing an unknown amount of the same gas) wherein the gas densities are modulated. Light passing through the two cells in sequence is modulated in intensity at the vibrational-rotational lines characteristic of the absorption spectrum for the gas of interest. Since the absorption process is nonlinear, modulating the two absorption cells at two different frequencies gives rise to a heterodyning effect, which in turn introduces sum and difference frequencies in the detected signal. Measuring the ratio of the difference frequency signal for example, to the signal introduced by the reference cell provides a normalized measure of the amount of the gas in the sample cell. The readings produced are thereby independent of source intensity, window transparency, and detector sensitivity. Experimental evaluation of the technique suggests that it should be applicable to a wide range of gases, that it should be able to reject spurious signals due to unwanted gases, and that it should be sensitive to concentrations of the order of 10 to the minus 8th power when used with a sample cell of only 20 cm length.

  15. Chromatographic detection of nitroaromatic and nitramine compounds by electrochemical reduction combined with photoluminescence following electron transfer.

    PubMed

    Woltman, S J; Even, W R; Sahlin, E; Weber, S G

    2000-10-15

    The oxidizing agent tris(bipyridyl)ruthenium(III), or Ru-(bpy)(3)3+, is used as a postcolumn reagent for the detection of nitroaromatic and nitramine explosive compounds. After separation, the explosives are reduced electrochemically to oxidizable products such as hydroxlamines and nitrosamines, and these products react readily with Ru-(bpy)(3)3+ and Ru(bpy)(3)2+. The photoluminescence from the latter is used for detection. A porous carbon electrode was used for on-line analyte reduction following chromatography. Another porous carbon electrode was used to generate the nonluminescent Ru(bpy)(3)3+ from Ru(bpy)(3)3+ on-line at high efficiency. The two streams were combined, and the Ru(bpy)(3)2+ produced by oxidation of the reduced analytes was detected by laser illumination and light detection. Reductive hydrodynamic voltammograms of nitrobenzene, 2,4,6-trinitrotoluene, and hexahydro-1,3,5-trinitro-1,3,5-triazine indicated that a potential of - 1500 mV vs Ag/AgCl was sufficient to achieve a maximum signal from the reduced analytes. HPLC with a water/acetonitrile gradient on a C-18 reversed-phase column was then used to determine these three compounds plus the four additional examples, 1,3,5,7-tetrazocine, 2,4-dinitrotoluene; 2,6-dinitrotoluene, and 4-nitrotoluene. For both hydrodynamic voltammetry and HPLC detection, the photoluminescence following electron-transfer signal was calibrated using the one-electron standards ferrocene and ferrocenecarboxylic acid. Detection limits were in the low-nanomolar range for 20-microL injections of nonpreconcentrated nitro compounds.

  16. Analysis of Biologic Samples for Morphine and Morphine-Related Compounds by Gas Chromatographic-Mass Spectrometric Methods

    DTIC Science & Technology

    1976-04-01

    chromatographic methods are used for prelimi- nary purification of the sample when this effect is present. A second difficulty when drug studies are...Investigations were carried out of hydrolysis conditions, extraction and purification methods, procedures for derivative formation, mass spectral...One ml of acetic anhydride was added and the mixture was allowed to stand for 24 hours. Ice and water were added, and the product was extracted with

  17. Gas chromatographic-mass spectrometric characterisation of amiton and the recovery of amiton from concrete, paint, rubber and soil matrices.

    PubMed

    Borrett, Veronica T; Gan, Tiang-Hong; Lakeland, Barry R; Leslie, D Ralph; Mathews, Robert J; Mattsson, Eric R; Riddell, Stuart; Tantaro, Vince

    2003-06-27

    Amiton [O,O-diethyl S-[2-(diethylamino)ethyl] phosphorothiolate], is an organophosphorus chemical included in Schedule 2 of the Chemical Weapons Convention (CWC). Verification provisions under the CWC rely on the existence of a database of analytical information for scheduled chemicals and related compounds. Little analytical information is available for amiton. In this study, gas chromatography-mass spectrometry (GC-MS) characterisation of amiton and its typical impurities (including by-products and degradation products), supported by selective GC detection and 31P NMR data, was undertaken. Twenty-one compounds, including a by-product unique to amiton from an industrial source, were identified. Involatile degradation products of amiton were derivatised to enable their identification by GC-MS. The recovery of amiton from matrices that may be expected in an inspection scenario (i.e. concrete, paint, rubber and soil) was also examined. Paint and concrete matrices were the most useful matrices for the detection of amiton, and its by-products and degradation products. Amiton was readily detected in these matrices after 28 days.

  18. Sequential determination of triglycerides and free fatty acids in biological fluids by use of a continuous pretreatment module coupled to a gas chromatograph.

    PubMed

    Cárdenas, M S; Ballesteros, E; Gallego, M; Valcárcel, M

    1994-11-01

    A continuous system coupled to a gas-liquid chromatograph was used for the sequential determination of triglycerides and free fatty acids in serum and urine. The module provides compositional information and hence more detailed information on lipid metabolism changes in patients suffering metabolic disorders. Lipids in biological samples are manually extracted in methanol-n-hexane and introduced into the flow system; free fatty acids are then separated by retention on an ion-exchange resin and triglycerides (not retained) are transesterified with acetyl chloride in methanol. The resulting methyl esters are continuously injected into the gas chromatograph and determined by using a flame ionization detector. In a second step, retained free fatty acids are eluted and derivatized (also with acetyl chloride in methanol) and subsequently determined similarly as the triglycerides. The proposed method was applied to the determination of triglycerides in a lipid control serum; free fatty acids were determined in a human pool serum by the proposed method and compared with the volumetric method used in clinical practice. The results obtained in both instances showed good agreement between the results provided for triglycerides and free fatty acids. The proposed method was also applied to urine samples; a parallel recovery study was also made in order to assess the performance of the method.

  19. Determination of hexanal as an oxidative marker in vegetable oils using an automated dynamic headspace sampler coupled to a gas chromatograph/mass spectrometer.

    PubMed

    Ha, Jaeho; Seo, Dong-Won; Chen, Xi; Hwang, Jin-Bong; Shim, You-Shin

    2011-01-01

    An automated dynamic headspace sampler coupled to a gas chromatograph/mass spectrometer was evaluated as an oxidative marker to determine hexanal content in vegetable oils. For the effective analysis, a cooled injection system (CIS) was used to focus and to introduce the hexanal desorbed from the Tenax TA. The temperature of the CIS was maintained at -60 °C for 12 min before desorbing the hexanal. Hexanal was separated on a capillary column (DB-5, 0.25 mm × 60 m, 0.25 µm in film thickness) from 50 to 230 °C, followed by mass spectrometer-selected ion monitoring analysis at m/z 56. The instrumental response to hexanal was highly linear from 10 ng mL(-1) to 1 µg mL(-1) (r(2) = 0.9999). The relative standard deviation (RSD) of intra- and inter-day repeatability was acceptable, with values of less than 3.88 and 4.25%, respectively. The LOD and LOQ of hexanal were determined by gas chromatograph/mass spectrometer-selected ion monitoring to be 3.3 and 9.8 ng mL(-1), respectively. The acid value, peroxide value and fatty acid composition revealed a good correlation with the hexanal concentration.

  20. Sensitive Detection of Botulinum Neurotoxin Types C and D with an Immunoaffinity Chromatographic Column Test

    PubMed Central

    Gessler, Frank; Hampe, Katrin; Böhnel, Helge

    2005-01-01

    A sensitive and specific immunoassay for the simultaneous detection of Clostridium botulinum type C (BoNT/C) and type D neurotoxin was developed. Goat anti-mouse immunoglobulin G was bound to polyethylene disks in a small disposable column used for this assay. The sample was preincubated together with monoclonal antibodies specific for the heavy chain of BoNT/C and D and affinity-purified, biotinylated polyclonal antibodies against these neurotoxins. This complex was captured on the assay disk. Streptavidin-poly-horseradish peroxidase was used as a conjugate, and a precipitating substrate allowed the direct semiquantitative readout of the assay, if necessary. For a more accurate quantitative detection, the substrate can be eluted and measured in a photometer. Depending on the preincubation time, a sensitivity of 1 mouse lethal dose ml−1 was achieved in culture supernatants. PMID:16332765