SUMMARY: Gas‐liquid chromatographic methods are described for the identification of 87 components in distilled alcoholic liquors. Water‐free concentrates of ether‐pentane or Freon extracts of the distillates were injected into different column systems and the column effluent transported to a mass spectrometer. To our knowledge, 34 of the identified compounds have not been reported previously in whiskey.

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SUMMARY– A single‐pass gas‐liquid chromatography method is described for identifying compounds not reported previously in distilled alcoholic liquors. Water‐free concentrates of ether‐pentane extracts of the distillates were injected into a gas chromatographic column train and the column effluent transported to a mass spectrometer. Several hydrocarbons, and compounds apparently resulting from the reaction of acrolein with ethyl alcohol, were identified in the samples.

Components which have been identified in alcoholic beverages by this laboratory and by other workers are listed with the pertinent references.

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A single gas-liquid chromatographic column is described which will separate all the major fusel oil components rapidly and directly without prior concentration or extraction procedures. Quantitative data obtained using a 1:1 2% 1,2,6-hexanetrio 1:2% glycerol column compare favorably with those of the official AOAC colorimetric fusel oil method. Four additional components may be determined simultaneously and quantitatively.

Fifteen chemists participated in a collaborative study for the quantitative pas-liquid chromatographic determination of the individual fusel alcohols and ethyl acetate in whisky. Two levels of congeners represented by 4 coded samples of whisky were analyzed by using t h e proposed method, employing a glycerol-1,2,6-hexanetriol column, and the official AOAC method, 9.063-9.065. Since isobutyl and the atnyl alcohols comprise by far the greatest part of fusel oil, their determination is of major importance to the total fusel oil content . Statistical analyses show that the proposed method is superior to the AOAC method for the determination of these alcohols, whereas the official method is superior for the determination of ethyl acetate and n-propyl alcohol. In general, collaborators employing modern instrumentation preferred the proposed method over the AOAC method. The former method also separates and permits the quantitative measurement of active amyl and isoamyl alcohols. The proposed method has been adopted as official first action as an alternative to 9.063–9.065 for the determination of higher alcohols and ethyl acetate in whisky.