Analytical Methods In Mass Spectrometry

THE PURPOSE of this investigation was to develop methods for analyzing coal derivatives and products from the Fischer-Tropsch synthesis. As part of this investigation it was necessary to study the mass spectral characteristics of many classes of compounds. The mass spectra of alcohols, the trimethylsilyl ether derivatives of alcohols, acetal-type compounds, ketones, esters, and naphthenes were correlated with structure, and analytical methods were formulated. A method was devised to determine the ratio of branched to normal hydrocarbons up to CIS in the Fischer-Tropsch product. Low-ionizing-voltage mass spectrometry was combined with type-analyses to analyze tar acids and neutral oils from coal. The necessary sensitivity correlations at low-ionizing voltage were developed, particularly for phenolic compounds. Special analytical techniques were developed for the mass spectral analyses of specific compounds and compound types including (1) oxides of nitrogen, (2) hydrogen sulfide, (3) isomers of butenes and pentenes, and (4) hydrogen deuteride. An investigation was made of the effects of various hydrocarbons and oxygenated compounds on tungsten filaments in the mass spectrometer. The operating characteristics of rhenium filaments under similar conditions were studied. Several improved sample handling techniques were developed, including an automatic manometer and a self-filling micropipet. Studies were made of anomalous and negative peaks in the mass spectra of certain gases.