Ascorbic acid gradually decomposes as the powder ages, making it difficult if not impossible for the forensic chemist to identify it by traditional bulk techniques. In the current study, various extraction and derivatization procedures were assessed in the course of developing the most effective method. The researchers found that extracting samples with a mixture of acetonitrile and N,O-bis(trimethylsilyl)acetamide (BSA) at room temperature without heating or ultrasonication allowed for the most sensitivity without further degrading any ascorbic acid present. Although solutions of derivitized ascorbic acid were found to be stable for periods of at least 24 hours, derivitized extracts of propellant samples did show continued degradation after standing for similar periods; therefore, GC-MS analysis was always performed immediately after sample extraction and derivatization. Thus, GC-MS analysis combined with BSA derivatization can provide an identification of aged and degraded samples of black powder substitutes that contain ascorbic acid, cooked sugars, or both. This method is particularly useful in cases when bulk methods fail. 6 figures and 9 references