A continuous flow method of determining the quantitative isotopic composition of hydrogen comprised in a compound is disclosed, together with apparatus for carrying out the method. The method involves introducing the sample to be analysed into a flow of carrier gas which does not contain hydrogen, the carrier gas then being arranged to flow through a heated catalytic reactor which contain a chromium-based catalyst. The sample is pyrolysed in the catalytic reactor so as to form molecular hydrogen which is then analysed mass-spectrometrically. Preferably a gas chromatrograph is disposed before the catalytic reactor so that one or more components or a mixture may be separately analysed.