The analysis of metallic sodium heretofore has been made by the titrimetric method, employing its solution oxidized by alcohol. In using this method unsatisfactory results have been obtained, which are due to the presence of NaOH as an impurity. Therefore a more accurate method to determine the amount of hydrogen produced by the oxidation of sodium with alcohol has been carried out. In this method, the presence of NaOH or Na2CO3 in the metal does not cause any error. Since the gas analysis requires careful caution for the measurents of the gas volume which is sensitve for the change of temperature and pressure, the necessary apparatus and reagent have been investigated. The method can be operated simply in a short time with better accuracy than the titrimetric method. A table for correction of the volume of gas is presented in order to make a rapid calculation. The standerd deviation of measurements was 0. 009 % and it showed higher accuracy than the titrimetric method.