A rapid combustion technique in an oxygen atmosphere followed by a quantitative electrolysis of the initial quantity of water vapor produced is used for the microdetermination of carbon and hydrogen in organic compounds. The carbon dioxide also produced by combustion may be determined either by converting it to water vapor with subsequent electrolysis, or if need be, by quantitative gas chromatography. Both the carbon dioxide and water signals are integrated by inexpensive, low-inertia motors and the absolute amounts of carbon and hydrogen are obtained from respective calibration curves. The time required for a complete microanalysis is usually ten minutes or less, including the weighing of a 1 mg. sample. The absolute error of the method is approximately 0.5% for carbon and 0.1% for hydrogen for samples ranging from 0.5 to 1.5 mg.

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