Gas chromatograph-mass spectrometer with dual electron impact/high pressure ion source

1976 ◽  
Vol 48 (12) ◽  
pp. 1829-1832 ◽  
Author(s):  
Ragnar. Ryhage
2016 ◽  
Vol 2016 ◽  
pp. 1-9
Author(s):  
Yury I. Lyakhovetsky ◽  
Elena A. Shilova ◽  
Alexandra P. Pleshkova ◽  
Alexander I. Belokon ◽  
Sergey O. Yakushin ◽  
...  

C60was shown to react with organosilanes Me4Si, Ph2SiH2, Ph2MeSiH, Ph4Si, andα-naphthylphenylmethylsilane in the electron ionization ion source of a mass spectrometer with the transfer of the corresponding organic radicals (Me, Ph, andα-naphthyl) from the silanes to the fullerene. The reactions were accompanied by hydrogen addition to some products and hydrogen loss from them. C70reacted with Me4Si analogously. A reaction mechanism involving homolytic dissociation of the silanes under electron impact to the corresponding organic radicals, which react further with C60at the surface of the ionization chamber of the mass spectrometer to give the respective adducts, was offered. A mechanistic study of the reaction of C60with Me4Si supported it. No silicon containing derivatives of the fullerenes were found. C60reacted with Ph4Si in solution under UV irradiation in a similar fashion furnishing phenyl derivatives of the fullerene. These results provide an additional support to the hypothesis formulated earlier thatthe homolytic reactive mass spectrometry of fullerenes (the reactions of fullerenes with other species in the ionization chambers of mass spectrometers and their mass spectral monitoring)can predict the reactivity of them toward the same reagents in solution to a significant extent.


1981 ◽  
Vol 59 (15) ◽  
pp. 2412-2416 ◽  
Author(s):  
John A. Stone ◽  
Margaret S. Lin ◽  
Jeffrey Varah

The reactivity of the dimethylchloronium ion with a series of aromatic hydrocarbons has been studied in a high pressure mass spectrometer ion source using the technique of reactant ion monitoring. Benzene is unreactive but all others, from toluene to mesitylene, react by CH3+ transfer to yield σ-bonded complexes. The relative rate of reaction increases with increasing exothermicity in line with current theories of nucleophilic displacement reactions.


1985 ◽  
Vol 31 (5) ◽  
pp. 741-746 ◽  
Author(s):  
D G Deutsch ◽  
R J Bergert

Abstract We evaluated the Hewlett-Packard 5995B benchtop capillary gas chromatograph-mass spectrometer (GC-MS) for its ability to identify drugs commonly detected and (or) measured in the clinical toxicology laboratory. Initial experiments indicated that the instrument as originally configured, with an isolation valve between the gas chromatograph and mass spectrometer, was unsatisfactory for the identification of hypnotics-sedatives. However, with the capillary inserted directly into the ion source, we could detect 10 ng of these drugs on a total-ion chromatogram. The software programs cause the instrument to be highly automated. In terms of ease of operation and speed it was found suitable for use in a routine clinical laboratory. Chromatography of urine extracts on the capillary gas chromatograph-mass spectrometer yielded excellent resolution of parent compounds and metabolites (e.g., diphenhydramine together with approximately four metabolites and propoxyphene with four metabolites). However, the manufacturer's computer program used to evaluate the quality of the match between the experimental mass spectra and the 375 drug reference spectra was only moderately successful in identifying unknown compounds. The ability of this capillary GC-MS to identify most compounds with a high degree of confidence will be increased by enlarging the library to include more drugs and metabolites and by using a more reliable computerized matching program.


1987 ◽  
Vol 65 (12) ◽  
pp. 2849-2854 ◽  
Author(s):  
Anastasia C. M. Wojtyniak ◽  
Xiaoping Li ◽  
John A. Stone

The association equilibrium [Formula: see text] has been studied in a high pressure mass spectrometer ion source using tetramethylsilane/methane mixtures. Measurement of the equilibrium constant over a range of temperatures yields ΔH0 = −22.3 ± 0.4 kcal mol−1 and ΔS0 = −35.2 ± 0.9 cal mol−1 K−1. Collision-assisted dissociation experiments suggest that the methyl groups retain their integrity in (CH3)7Si2+. Mixed ions such as (CH3)7SiGe+ and (CH3)7GeSn+ were not observed in mixtures of (CH3)4X and (CH3)4Y(X ≠ Y = Si, Ge, Sn). Instead CH3− transfer equilibrium reactions were observed viz. [Formula: see text] (ΔH0 = −10.2 ± 1.2 kcal mol−1, ΔS0 = −3.7 ± 2.4 cal K−1 mol−1) and [Formula: see text], ΔS0 = −0.9 ± 1.6 cal K−1 mol−1. These are in excellent agreement with some published differences in appearance potentials for (CH3)3X+ from (CH3)4X (X = Si, Ge, Sn).


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