As part of a program to develop chemical tests which can be used to complement existing tests for mechanical properties, propellant ballistic performance, and explosive sensitivity, a detailed experimental procedure is presented for analysis of plastic‐bonded explosives (PBX's) by the coupled method of pyrolysis‐gas chromatography (PyGC). The method involves grinding the cooled PBX, pressing a controlled quantity on a pyrolysis wire, performing Curic‐Point pyrolysis, and detecting the products after separation by gas chromatography. PyGC results are presented to show the capability of the method to differentiate aged and unaged samples of PBX's and to differentiate stabilized and unstabilized PBX's based on RDX. Also included are results from several series of reproductibility studies, which suggest that the method may require only minor modifications before it can be implemented for regular screening of these complex formulations.