Performance and optimization of a combustion interface for isotope ratio monitoring gas chromatography/mass spectrometry. 1995

D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
Departments of Chemistry and Geological Sciences, Indiana University, Bloomington 47405, USA.

Conditions and systems for on-line combustion of effluents from capillary gas chromatographic columns and for removal of water vapor from product streams were tested. Organic carbon in gas chromatographic peaks 15 s wide and containing up to 30 nanomoles of carbon was quantitatively converted to CO2 by tubular combustion reactors, 200 x 0.5 mm, packed with CuO or NiO. No auxiliary source of O2 was required because oxygen was supplied by metal oxides. Spontaneous degradation of CuO limited the life of CuO reactors at T > 850 degrees C. Since NiO does not spontaneously degrade, its use might be favored, but Ni-bound carbon phases form and lead to inaccurate isotopic results at T < 1050 degrees C if gas-phase O2 is not added. For all compounds tested except CH4, equivalent isotopic results are provided by CuO at 850 degrees C, NiO + O2 (gas-phase mole fraction, 10(-3)) at 1050 degrees C and NiO at 1150 degrees C. The combustion interface did not contribute additional analytical uncertainty, thus observed standard deviations of 13C/12C ratios were within a factor of 2 of shot-noise limits. For combustion and isotopic analyses of CH4, in which quantitative combustion required T approximately 950 degrees C, NiO-based systems are preferred, and precision is approximately 2 times lower than that observed for other analytes. Water must be removed from the gas stream transmitted to the mass spectrometer or else protonation of CO2 will lead to inaccuracy in isotopic analyses. Although thresholds for this effect vary between mass spectrometers, differential permeation of H2O through Nafion tubing was effective in both cases tested, but the required length of the Nafion membrane was 4 times greater for the more sensitive mass spectrometer.

UI MeSH Term Description Entries
D008401 Gas Chromatography-Mass Spectrometry A microanalytical technique combining mass spectrometry and gas chromatography for the qualitative as well as quantitative determinations of compounds. Chromatography, Gas-Liquid-Mass Spectrometry,Chromatography, Gas-Mass Spectrometry,GCMS,Spectrometry, Mass-Gas Chromatography,Spectrum Analysis, Mass-Gas Chromatography,Gas-Liquid Chromatography-Mass Spectrometry,Mass Spectrometry-Gas Chromatography,Chromatography, Gas Liquid Mass Spectrometry,Chromatography, Gas Mass Spectrometry,Chromatography, Mass Spectrometry-Gas,Chromatography-Mass Spectrometry, Gas,Chromatography-Mass Spectrometry, Gas-Liquid,Gas Chromatography Mass Spectrometry,Gas Liquid Chromatography Mass Spectrometry,Mass Spectrometry Gas Chromatography,Spectrometries, Mass-Gas Chromatography,Spectrometry, Gas Chromatography-Mass,Spectrometry, Gas-Liquid Chromatography-Mass,Spectrometry, Mass Gas Chromatography,Spectrometry-Gas Chromatography, Mass,Spectrum Analysis, Mass Gas Chromatography
D008697 Methane The simplest saturated hydrocarbon. It is a colorless, flammable gas, slightly soluble in water. It is one of the chief constituents of natural gas and is formed in the decomposition of organic matter. (Grant & Hackh's Chemical Dictionary, 5th ed)
D009532 Nickel A trace element with the atomic symbol Ni, atomic number 28, and atomic weight 58.69. It is a cofactor of the enzyme UREASE.
D010100 Oxygen An element with atomic symbol O, atomic number 8, and atomic weight [15.99903; 15.99977]. It is the most abundant element on earth and essential for respiration. Dioxygen,Oxygen-16,Oxygen 16
D011407 Propane A three carbon alkane with the formula H3CCH2CH3.
D002244 Carbon A nonmetallic element with atomic symbol C, atomic number 6, and atomic weight [12.0096; 12.0116]. It may occur as several different allotropes including DIAMOND; CHARCOAL; and GRAPHITE; and as SOOT from incompletely burned fuel. Carbon-12,Vitreous Carbon,Carbon 12,Carbon, Vitreous
D002245 Carbon Dioxide A colorless, odorless gas that can be formed by the body and is necessary for the respiration cycle of plants and animals. Carbonic Anhydride,Anhydride, Carbonic,Dioxide, Carbon
D002247 Carbon Isotopes Stable carbon atoms that have the same atomic number as the element carbon but differ in atomic weight. C-13 is a stable carbon isotope. Carbon Isotope,Isotope, Carbon,Isotopes, Carbon
D002623 Chemistry Techniques, Analytical Methodologies used for the isolation, identification, detection, and quantitation of chemical substances. Analytical Chemistry Techniques,Analytical Chemistry Methods,Analytical Chemistry Method,Analytical Chemistry Technique,Chemistry Method, Analytical,Chemistry Methods, Analytical,Chemistry Technique, Analytical,Method, Analytical Chemistry,Methods, Analytical Chemistry,Technique, Analytical Chemistry,Techniques, Analytical Chemistry
D003300 Copper A heavy metal trace element with the atomic symbol Cu, atomic number 29, and atomic weight 63.55. Copper-63,Copper 63

Related Publications

D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
August 2007, Analytical chemistry,
D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
January 2007, Rapid communications in mass spectrometry : RCM,
D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
November 2008, Analytical chemistry,
D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
December 2012, Drug testing and analysis,
D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
March 2009, Steroids,
D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
November 2021, Journal of chromatography. A,
D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
January 1994, Organic geochemistry,
D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
October 2012, Rapid communications in mass spectrometry : RCM,
D A Merritt, and K H Freeman, and M P Ricci, and S A Studley, and J M Hayes
July 1999, Rapid communications in mass spectrometry : RCM,
Copied contents to your clipboard!