Fatal respiration of liquefied petroleum gas.

We have found that an efficient method of providing evidence of lethal solvent abuse is to sample headspace above lung tissue and then perform cryogenically focused gas-liquid chromatography. In the case presented, the level of lethal agent in lung tissue was low, but the solvent was present in abundance in the pleural cavity. We conclude that the pleural cavity acts as an efficient trap for aspirated substances.     

Synthesis of 4-methyl-5-arylpyrimidines and 4-arylpyrimidines: route specific markers for the Leuckardt preparation of amphetamine, 4-methoxyamphetamine, and 4-methylthioamphetamine

General synthetic routes to 4-methyl-5-arylpyrimidines and 5-arylpyrimidines are described. 4-Benzylpyrimidine, 4-methyl-5-phenylpyrimidine, 4-(4-methoxybenzyl)pyrimidine, and 4-methyl-5-(4-methoxyphenyl)pyrimidine have been positively identified as route-specific by-products in the Leuckardt preparations of amphetamine and 4-methoxyamphetamine.Using headspace solid phase microextraction (SPME) 4-(4-methoxybenzyl)pyrimidine and 4-methyl-5-(4-methoxyphenyl)pyrimidine have been identified in illicit tablets containing 4-methoxyamphetamine. This is an indication that illicit laboratories use the Leuckardt method for the preparation of 4-methoxyamphetamine.Flatliner tablets containing 4-methylthioamphetamine have been screened for the presence of 4-(4-methylthiobenzyl)pyrimidine and 4-methyl-5-(4-methylthiophenyl)pyrimidine using both headspace and aqueous phase SPME. As these pyrimidines were not detected it would appear likely that illicit laboratories are not using the Leuckardt method for the preparation of 4-methylthioamphetamine.     

A rapid wire-based sampling method for DNA profiling

Abstract: This paper reports the results of a commission to develop a field deployable rapid short tandem repeat (STR)‐based DNA profiling system to enable discrimination between tissues derived from a small number of individuals. Speed was achieved by truncation of sample preparation and field deployability by use of an Agilent 2100 Bioanalyser^TM. Human blood and tissues were stabbed with heated stainless steel wire and the resulting sample dehydrated with isopropanol prior to direct addition to a PCR. Choice of a polymerase tolerant of tissue residues and cycles of amplification appropriate for the amount of template expected yielded useful profiles with a custom‐designed quintuplex primer set suitable for use with the Bioanalyser^TM. Samples stored on wires remained amplifiable for months, allowing their transportation unrefrigerated from remote locations to a laboratory for analysis using AmpFlSTR^® Profiler Plus^® without further processing. The field system meets the requirements for discrimination of samples from small sets and retains access to full STR profiling when required.     

Degradation in soil of precursors and by-products associated with the illicit manufacture of methylamphetamine: implications for clandestine drug laboratory investigation

Key precursors and by-products in the Leuckardt, Nagai and dissolving metal reductive syntheses of methylamphetamine undergo degradation in soil as a result of biotic and abiotic processes. Furthermore, methylamphetamine is a product of the degradation of 1-(1',4'-cyclohexadienyl)-2-methylaminopropane and N-formylmethylamphetamine. These findings have implications for the forensic assessment of buried residues recovered from clandestine laboratory sites because markers used to infer the synthetic methods used might be absent as a result of degradation and because methylamphetamine might be present in residues as a result of degradation rather than as a direct result of its manufacture in the laboratory.     

Styryl dye coated metal oxide powders for the detection of latent fingermarks on non-porous surfaces

Conventional fingermark powders rely on contrast induced by absorption/reflection (e.g. black powder) or luminescence in the visible region (e.g. Blitz Green(?)). In most cases, these powders provide sufficient contrast; however, in some circumstances surface characteristics can interfere with the visualisation of powdered fingermarks. Visualisation in the near infra-red (NIR) region, however, has been shown to eliminate interferences commonly encountered in the visible region. In this study, a mixture of rhodamine 6G and the NIR laser dye styryl 11 (STaR 11) was coated onto an aluminium oxide nanopowder and then mixed with silver magnetic powder to develop and visualise fingermarks in the NIR. When compared to Blitz Green(?), it was determined that the STaR 11 magnetic powder was better suited for marks deposited on textured surfaces and for older marks, whereas Blitz Green(?) performed better on smooth glossy surfaces. The ability of the STaR 11 mixed dye formulation to be visualised in both the visible and NIR regions also provides a significant advantage over conventional luminescent fingermark powders.     

New developments in SPME Part 2: Analysis of ammonium nitrate-based explosives

Solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS) is a simple, reliable technique for the recovery and analysis of many organic explosives. However, this technique is impractical for the analysis of ammonium nitrate-type explosives due to the extreme polarity, low molecular weight, and high volatility of the amine moiety. This article describes an initial investigation of a derivatization process utilizing alkylchloroformates that converts ammonium nitrate and methylammonium nitrate into a form suitable for recovery by SPME and analysis by GC-MS.     

Microbial degradation of illicit drugs,their precursors,and manufacturing by-products: implications for clandestine drug laboratory investigation and environmental assessment

Chemicals associated with clandestine drug laboratories are often disposed of covertly into soil, sewerage systems, or public waste management facilities. There are two significant issues relating to such dumps of materials; they might contain valuable evidence as to drug manufacture, and they might be a source of pollution. This study presents initial findings in relation to the impact microorganisms from environmental sources have upon drugs, their precursors, and manufacturing by-products. The aim of this study was to identify which chemicals associated with clandestine drug laboratories persist in the environment in order to allow forensic drug chemists to link discarded residues with the method of manufacture, and to allow the environmental impact of clandestine drug laboratories to be assessed accurately. When exposed to soil microorganisms, phenyl-2-propanone (P2P) was rapidly metabolized into mixtures of 1-phenyl-2-propanol, 1-phenyl-1,2-propanedione, 1-hydroxy-1-phenyl-2-propanone, 2-hydroxy-1-phenyl-1-propanone, and the two diastereoisomers of 1-phenyl-1,2-propanediol. On the other hand, when exposed under the same conditions, methylamphetamine sulphate (MAS) remained virtually unchanged. Implications relating to evidence gathering for forensic purposes and to environmental assessment of clandestine drug laboratories are discussed.     

Characterisation of 0.22 caliber rimfire gunshot residues by time-of-flight secondary ion mass spectrometry (TOF-SIMS): a preliminary study

The application of time-of-flight secondary ion mass spectrometry (TOF-SIMS) for the characterisation of gunshot residue (GSR) from 0.22 caliber rimfire ammunition is reported. Results obtained by TOF-SIMS were compared with conventional scanning electron microscopy (SEM) studies. As could be expected, TOF-SIMS exhibited greater elemental sensitivity than SEM equipped with energy dispersive X-ray detection (SEM-EDX), and was also capable of detecting fragments characteristic of inorganic compounds. This preliminary study indicates that TOF-SIMS offers substantial potential for forensic GSR examinations as a complementary technique to SEM-EDX. In addition TOF-SIMS is applicable to the analysis of individual particles in the typical size range encountered in GSR casework.     

Glass-containing gunshot residue particles: a new type of highly characteristic particle?

In 0.22 caliber rimfire ammunition, the primer often contains lead or lead and barium compounds. As residues from these primers do not contain lead, barium, and antimony, they cannot be uniquely classified as gunshot residue (GSR) under ASTM designation E 1588-95. In many types of 0.22 caliber rimfire ammunition, the cartridge contains a primer sensitized with glass. In this paper we describe a previously unreported type of GSR particle consisting of glass fused with other primer components. As there appear to be few potential environmental or occupational sources of particles composed of lead and barium compounds fused to glass, particularly borosilicate glass, these particles may have high evidential value. Scanning electron microscopy with energy dispersive X-ray detection (SEM-EDX) and time-of-flight secondary ion mass spectrometry (TOF-SIMS) were evaluated for the characterization of glass-containing GSR particles. The occurrence of glass-containing GSR particles was established in the residue from various brands of 0.22 caliber ammunition, and several sub-types were identified.