Smokeless powders are low explosives and are potentially found in cases involving firearms and improvised explosive devices. Apart from inorganic compound analysis, forensic determination of organic components of these materials appears as a promising alternative, especially the chromatographic techniques. This work describes the optimization of a solid-phase microextraction technique using an 85 μm polyacrylate fiber followed by gas chromatography-flame ionization detection for smokeless powder. A multivariate experimental design was performed to optimize extraction-influencing parameters. A 2(4) factorial first-order design revealed that sample temperature and extraction time were the major influencing parameters. Doehlert matrix design has subsequently selected 66°C and 21 min as the compromised conditions for the two predetermined parameters. This extraction technique has successfully detected the headspace compounds of smokeless powders from different ammunition types and allowed for their differentiation. The novel technique allows more rapid sample preparation for chromatographic detection of smokeless powders.
Gunshot residues, produced after shooting activity, have acquired their importance in analysis due to the notoriety of firearms-related crimes. In this study, solid-phase microextraction was performed to extract the headspace composition of spent cartridges using 85-μm polyacrylate fiber at 66°C for 21 min. Organic compounds, that is, naphthalene, 2,6-dinitrotoluene, 2,4-dinitrotoluene, diphenylamine, and dibutyl phthalate were detected and analyzed by gas chromatography-flame ionization detection technique. Evaluation of chromatograms for diphenylamine, dibutyl phthalate, and naphthalene indicates the period after a gunshot was discharged, whether it was 1 days, 2-4 days, <5 days, 10 days, 20 days, or more than 30 days ago. This study revealed the potential effects of environmental factors such as occasional wind blow and direct sunlight on the estimation of time after spent cartridges were discharged. In conclusion, we proposed reliable alternative in analyzing the headspace composition of spent cartridges in a simulated crime scene.
A modeling procedure that predicts trihalomethane (THM) formation from field sampling at the treatment plant and along its distribution system using Tampin district, Negeri Sembilan and Sabak Bernam district, Selangor as sources of data were studied and developed. Using Pearson method of correlation, the organic matter measured as TOC showed a positive correlation with formation of THM (r=0.380,P=0.0001 for Tampin and r=0.478,P=0.0001 for Sabak Bernam). Similar positive correlation was also obtained for pH in both districts with Tampin (r=0.362,P=0.0010) and Sabak Bernam (r=0.215,P=0.0010). Chlorine dosage was also found to have low correlation with formation of THM for the two districts with Tampin (r=0.233,P=0.0230) and Sabak Bernam (r=0.505,P=0.0001). Distance from treatment plant was found to have correlation with formation of THM for Tampin district with r=0.353 and P=0.0010. Other parameters such as turbidity, ammonia, temperature and residue chlorine were found to have no correlation with formation of THM. Linear and non-linear models were developed for these two districts. The results obtained were validated using three different sets of field data obtained from own source and district of Seremban (Pantai and Sg. Terip), Negeri Sembilan. Validation results indicated that there was significant difference in the predictive and determined values of THM when two sets of data from districts of Seremban were used with an exception of field data of Sg. Terip for non-linear model developed for district of Tampin. It was found that a non-linear model is slightly better than linear model in terms of percentage prediction errors. The models developed were site specific and the predictive capabilities in the distribution systems vary with different environmental conditions.