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Beside the usual reactants, the reaction medium of polymerization contains two inert compounds IMand IC, which act as internal standards of concentration corresponding, respectively, to the monomer M and the organometallic catalyst RMe. At given time intervals, small liquid samples are picked up and injected into a vaporization cell together with small amounts of water or alcohol. Then a part of the gaseous mixture is analyzed by gas chromatography. The consumption of the monomer and of the catalyst are obtained from the measurements of the ratios of the areas under the peaks M and IM, and RH and IC. Some results are given for the polymerizations of vinyl chloride with an organomagnesium catalyst and of isoprene with n-butyllithium.