RI 5976 Determination Of Alcohols By Their Trimethylsilyl Ethers ? Summary

Direct mass spectrometric determination of alcohols in the presence of hydrocarbons has not been possible because of the similarity of hydrocarbon and alcohol mass spectra. Experiments have demonstrated that by converting the alcohols to their trimethylsilyl derivatives, characteristic mass spectra are obtained free of interference from hydrocarbon ion fragmentation. Hexa- methyldisilazane is the reagent selected for the conversion, An improved method of preparing the reagent is given, Mass spectrometric determination of alcohols as trimethylsilyl ethers now is not only possible without prior separation from other materials, but the range of the room-temperature mass spectrometer is also extended to include the C10 alcohol region. Water does not interfere because it is converted to hexamethyldisiloxane, which has its own distinctive mass spectral peak, Experience indicates that other compounds such as glycols, amines, and phenols probably could also be determined by mass spectrometry of their trimethylsilyl ethers. Studies on the similar detemination of phenols in coal oils have been started, When mass spectrometry is not available, gas-liquid chromatography of alcohols before and after their conversion to the trimethylsilyl derivatives probably could be performed. The preparation and properties of the trimethylsilyl derivatives of 23 alcohols, 2 glycols, 3 amines, and 1 mercaptan are detailed. INRODUCTION During investigations by the Bureau of Mines at the Pittsburgh Coal Research Center relative to the development of Fischer-Tropsch processes, complications were encountered in the mass spectrometric analysis of alcohols in hydrocarbon oils. The fragmentation peaks of the alcohols and the hydrocarbons were so similar that an accurate analysis was not possible, Since involved separation techniques are necessary to isolate alcohols from hydro-carbons for separate determinations, efforts were turned to the search for a