A fat and convenient GC method has been developed for a compound (tris(2,3-dibromopropyl)phosphate) that poses a difficult analytical problem for both GC (thermal instability/low volatility) and LC (not amenable to commonly available, sensitive detectors) analysis. The method employed a short (10-meter), thin-film (0.53 micrometer), wide-bore (0.53 millimeter) column, a cool on-column inlet system, and a relatively fast flow rate. The conditions were successful in that elution times and column operating temperatures could be decreased to such an extent that the thermal lability of the compound was not prohibitive. The successful chromatography of Tris-BP on the short, thin-film column with both inlet systems illustrates the effect of film thickness and column length on thermally labile compounds. The integrity of the eluting peak was established by IR analysis. The type of application is important (assuming the approach is generally applicable to many low volatility, thermally labile compounds) because spectrometers (FT-IR and MS) coupled to GCs are almost commonplace. Chemical investigations that require spectroscopic analysis of eluents, such as hydrolysis product studies, can be enhanced greatly by technology that broadens the classes of compounds amenable to GC.