Derivatization of mixtures of bis(4-aminocyclohexyl)methane (PACM) and 2,2-bis(4-aminocyclohexyl)propane (PACP) with N,N-dimethylformamide dimethylacetal produces volatile and thermally stable N-dimethylaminomethylene derivatives which can be analyzed directly by gas chromatography without prior work-up. These derivatives yield well-resolved peaks on a Poly A-103 column. Analyses of the diamine mixtures give results with a standard deviation of less than 1 percent which are in good agreement with other standard methods.