NCJ Number
206378
Journal
Journal of Forensic Sciences Volume: 49 Issue: 3 Dated: May 2004 Pages: 523-528
Date Published
May 2004
Length
6 pages
Annotation
Some of the newer black powder substitutes that have been used in illicit pipe bombings throughout the United States are formulated with ascorbic acid; this research demonstrated the feasibility of identifying ascorbic acid and/or its degradation products in aged black powder substitutes by solvent extraction, TMS (trimethylsilyl) derivatization, and analysis by GC-MS.
Abstract
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