Functional Group Analysis by Gas Chromatography. IV. Pyrolytic Reaction of Carboxylic Acids in Sulfur Vapor

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This paper deals with a quantitative gas chromatographic analysis of the product evolved by the pyrolytic reaction between carboxylic acid and sulfur vapor. About 10 mg of carboxylic acid was mixed with 2–3 g sulfur and made to react at 1000–1100°C for 10min. The gaseous product was taken in a gas sampler and subjected to gas chromatography. Carbon dioxide was produced from the carboxyl group, carbon disulfide from carbon, hydrogen sulfide from hydrogen and nitrogen molecule from nitrogen. The peak area ratios of carbon disulfide and hydrogen sulfide to carbon dioxide were found in the gas chromatogram with glycine as a standard substance, and the other carboxylic acids were analyzed on the basis of the relation between the peak area ratio and the chemical composition of glycine. Aliphatic and aromatic carboxylic acids gave satisfactory resuls by this method, but not pyridine carboxylic acid. Weighing a definite amount of sample is not needed in this method. Information concerning the chemical composition as well as the functional group of a carboxylic acid can be obtained.
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