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Books

Biber, K. & Luker, T. 2017, Evidence and the Archive: Ethics, Aesthetics and Emotion, Routledge.

Journal articles

Benson, N., Dos Santos, R.O., Griffiths, K., Cole, N., Doble, P., Roux, C. & Blanes, L. 2017, 'The development of a stabbing machine for forensic textile damage analysis.', Forensic Sci Int, vol. 273, pp. 132-139.
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This article describes the development of a horizontal stabbing machine with an interchangeable knife holder to simulate stab events. The machine consists of a motorised arm with a pneumatic system designed to deliver 60 unique stabbing positions. The mechanics were robust and the positioning system highly reproducible with standard deviations of less than 1.0mm in the x-axis and 2.3mm in the y-axis for a given stab position. The force of the instrument may be varied by the operator to a maximum of approximately 221N. The suitability of the instrument for simulating stab events was evaluated by measuring the severance length and textile damage from stab delivered from four different knives and nine penetrating angles.

Bishop, D.P., Blanes, L., Wilson, A.B., Wilbanks, T., Killeen, K., Grimm, R., Wenzel, R., Major, D., Macka, M., Clarke, D., Schmid, R., Cole, N. & Doble, P.A. 2017, 'Microfluidic high performance liquid chromatography-chip hyphenation to inductively coupled plasma-mass spectrometry', Journal of Chromatography A, vol. 149, pp. 64-69.
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© 2017 Elsevier B.V.The Agilent Chip Cube Interface is a microfluidic chip-based technology originally designed for nanospray molecular mass spectrometry in which the sample enrichment, nano-column, tubing, connectors and spray tip were integrated into a single biocompatible chip. Here we describe the hyphenation of the Chip Cube Interface to ICP-MS via modification of the standard HPLC chip design and a new total consumption nebuliser suitable for flow rates as low as 300nLmin-1. The potential of the instrument to eliminate common nanoLC - ICP-MS shortcomings such as leaks, blockages and band-broadening was demonstrated via analysis of cyanocobalamin in equine plasma. The method was linear over three orders of magnitude with an r2 of 0.9999, the peak area repeatability was 1.9% (n=7), and the detection limit was 14ngmL-1. This novel configuration of the Chip Cube Interface coupled to ICP-MS is a suitable platform for the analysis of biomolecules associated with trace metals and speciation applications.

Chadwick, S., Neskoski, M., Spindler, X., Lennard, C. & Roux, C. 2017, 'Effect of hand sanitizer on the performance of fingermark detection techniques.', Forensic Sci Int, vol. 273, pp. 153-160.
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Hand sanitizers have seen a rapid increase in popularity amongst the general population and this increased use has led to the belief that hand sanitizers may have an effect on subsequent fingermark detection. Based on this hypothesis, three alcoholic and two non-alcoholic hand sanitizers were evaluated to determine the effect they had on the detection of fingermarks deposited after their use. The following fingermark detection methods were applied: 1,2-indanedione-zinc, ninhydrin, physical developer (porous substrate); and cyanoacrylate, rhodamine 6G, magnetic powder (non-porous substrate). Comparison between hand sanitized fingermarks and non-hand sanitized fingermarks showed that the alcohol-based hand sanitizers did not result in any visible differences in fingermark quality. The non-alcoholic hand sanitizers, however, improved the quality of fingermarks developed with 1,2-indanedione-zinc and ninhydrin, and marginally improved those developed with magnetic powder. Different parameters, including time since hand sanitizer application prior to fingermark deposition and age of deposited mark, were tested to determine the longevity of increased development quality. The non-alcoholic hand sanitized marks showed no decrease in quality when aged for up to two weeks. The time since sanitizer application was determined to be an important factor that affected the quality of non-alcoholic hand sanitized fingermarks. It was hypothesized that the active ingredient in non-alcoholic hand sanitizers, benzalkonium chloride, is responsible for the increase in fingermark development quality observed with amino acid reagents, while the increased moisture content present on the ridges resulted in better powdered fingermarks.

Devièse, T., Ribechini, E., Castex, D., Stuart, B., Regert, M. & Colombini, M.P. 2017, 'A multi-analytical approach using FTIR, GC/MS and Py-GC/MS revealed early evidence of embalming practices in Roman catacombs', Microchemical Journal, vol. 133, pp. 49-59.
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© 2017 Elsevier B.V.During the second-third century, cremation was progressively abandoned for inhumation in the Roman Empire and was accompanied by new funeral practices. Recent archaeological excavations in the catacombs of Saints Peter and Marcellinus in Rome revealed thousands of formerly undiscovered skeletons of individuals plastered and methodically stacked in previously unknown and inaccessible rooms. By setting up and applying a multi-analytical approach to characterize chemically all amorphous materials surrounding the skeletons, we investigated this important cultural change regarding the treatment of death. Chemical characterization of the amorphous samples was achieved using FTIR spectroscopy and gas chromatography/mass spectrometry (Py-GC/MS and GC/MS) and by comparison with reference samples from known origin. This allowed for the unambiguous identification of precious and exotic resinous substances involved in the embalming process of the bodies. Amber, sandarac and frankincense, which were sourced from widespread locations, were used as part of the funerary treatment. This first evidence of such highly prized commodities in burial process provides us with new insight into funerary practices as well as commercial networks in the Roman Empire during the first centuries A.D.

Hare, D.J., Kysenius, K., Paul, B., Knauer, B., Hutchinson, R.W., O'Connor, C., Fryer, F., Hennessey, T.P., Bush, A.I., Crouch, P.J. & Doble, P.A. 2017, 'Imaging Metals in Brain Tissue by Laser Ablation - Inductively Coupled Plasma - Mass Spectrometry (LA-ICP-MS).', J Vis Exp, no. 119.
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Metals are found ubiquitously throughout an organism, with their biological role dictated by both their chemical reactivity and abundance within a specific anatomical region. Within the brain, metals have a highly compartmentalized distribution, depending on the primary function they play within the central nervous system. Imaging the spatial distribution of metals has provided unique insight into the biochemical architecture of the brain, allowing direct correlation between neuroanatomical regions and their known function with regard to metal-dependent processes. In addition, several age-related neurological disorders feature disrupted metal homeostasis, which is often confined to small regions of the brain that are otherwise difficult to analyze. Here, we describe a comprehensive method for quantitatively imaging metals in the mouse brain, using laser ablation - inductively coupled plasma - mass spectrometry (LA-ICP-MS) and specially designed image processing software. Focusing on iron, copper and zinc, which are three of the most abundant and disease-relevant metals within the brain, we describe the essential steps in sample preparation, analysis, quantitative measurements and image processing to produce maps of metal distribution within the low micrometer resolution range. This technique, applicable to any cut tissue section, is capable of demonstrating the highly variable distribution of metals within an organ or system, and can be used to identify changes in metal homeostasis and absolute levels within fine anatomical structures.

Heather, E., Bortz, A., Shimmon, R. & McDonagh, A.M. 2017, 'Organic impurity profiling of methylone and intermediate compounds synthesized from catechol.', Drug Test Anal, vol. 9, no. 3, pp. 436-445.
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This work examined the synthesis and organic impurity profile of methylone prepared from catechol. The primary aim of this work was to determine whether the synthetic pathway used to prepare 3,4-methylenedioxypropiophenone could be ascertained through analysis of the synthesized methylone. The secondary aim was the structural elucidation and origin determination of the organic impurities detected in methylone and the intermediate compounds. The organic impurities present in the reaction products were identified using GC-MS and NMR spectroscopy. Six organic impurities were detected in 1,3-benzodioxole and identified as the 1,3-benzodioxole dimer, 1,3-benzodioxole trimer, [1,3] dioxolo[4,5-b]oxanthrene, 4,4'-, 4,5'-, and 5,5'-methylenebis-1,3-benzodioxole. Six organic impurities were detected in 3,4-methylenedioxypropiophenone and identified as (2-hydroxyphenyl) propanoate, [2-(chloromethoxy) phenyl] propanoate, (2-propanoyloxyphenyl)propanoate, 5-[1-(1,3-benzodioxol-5-yl)prop-1-enyl]-1,3-benzodioxole, (5E)- and (5Z)-7-(1,3-benzodioxol-5-yl)-5-ethylidene-6-methyl-cyclopenta[f][1,3]benzodioxole). Exploratory synthetic experiments were also conducted to unambiguously identify the organic impurities detected in 3,4-methylenedioxypropiophenone. Two organic impurities were detected in 5-bromo-3,4-methylenedioxypropiophenone and identified as [2-(chloromethoxy)phenyl] propanoate and 3,4-methylenedioxypropiophenone. Five organic impurities were detected in methylone and identified as 3,4-methylenedioxypropiophenone, 1-(1,3-benzodioxol-5-yl)-N-methyl-propan-1-imine, 1-(1,3-benzodioxol-5-yl)-2-methylimino-propan-1-one, 1-(1,3-benzodioxol-5-yl)-N1,N2-dimethyl-propane-1,2-diimine and butylated hydroxytoluene. The origin of these organic impurities was also ascertained, providing valuable insight into the chemical profiles of methylone and the intermediate compounds. However, neither the catechol precursor nor the 1,3-benzodioxole intermediate could be identified based on the ...

Lee, R., Comber, B., Abraham, J., Wagner, M., Lennard, C., Spindler, X. & Roux, C. 2017, 'Supporting fingerprint identification assessments using a skin stretch model - A preliminary study.', Forensic Sci Int, vol. 272, pp. 41-49.
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To support fingerprint expert opinion, this research proposes an approach that combines subjective human analysis (as currently applied by fingerprint practitioners) with a statistical test of the result. This approach relies on the hypothesis that there are limits to the distortion caused by skin stretch. Such limits can be modelled by applying a multivariate normal probability density function to the distances and angle formed by a marked ridge characteristic and the two closest neighbouring minutiae. This study presents a model tested on 5 donors in total. The "expected range" of distortion in a within-source comparison using 10 minutiae was determined and compared to between-source comparisons. The expected range of log probability densities for within-source comparisons marked with 10 minutiae was determined to be from -33.4 to -60.0, with all between-source data falling outside this range, between -83 and -305. These results suggest that the proposed generated metric could be a powerful tool for the assessment of fingerprint expert opinion in operational casework.

Maitre, M., Kirkbride, K.P., Horder, M., Roux, C. & Beavis, A. 2017, 'Current perspectives in the interpretation of gunshot residues in forensic science: A review.', Forensic Sci Int, vol. 270, pp. 1-11.
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The traces produced when a firearm is discharged can provide important information in cases when questions regarding a possible association of the firearm with a person of interest (POI), time since discharge or shooting distance are raised. With advances in technology, the forensic challenges presented by these traces, known as gunshot residues (GSR), are moving from the analytical domain to the interpretation of the analytical results. Different interpretation frameworks are currently competing. Formal classification of particles, using standards such as that produced by ASTM, focusses only on evaluation of evidence at the sub-source level. Another approach, based on the application of Bayesian reasoning - namely the case-by-case approach - has been proposed that allows evaluation of evidence in regards to activity-related questions. This alternative approach allows an evaluation of the evidence that is more closely aligned to judicial and investigative aims. This paper critically presents the state of the art in regards to GSR interpretation in a holistic manner.

Michelot, H., Fu, S., Stuart, B., Shimmon, R., Raymond, T., Crandell, T. & Roux, C. 2017, 'Effect of drug precursors and chemicals relevant to clandestine laboratory investigation on plastic bags used for collection and storage.', Forensic Sci Int, vol. 273, pp. 106-112.
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In the area of clandestine laboratory investigations, plastic bags are used to collect and store evidence, such as solvents, precursors, and other compounds usually employed for the manufacturing of drugs (although liquids may be stored in glass containers within the bags first). In this study, three different types of plastic bags were provided by the NSW Police Force and investigated for their suitability for evidence collection: two different types of low-density polyethylene (LDPE) bags and one type of polyvinyl chloride (PVC) bag. Three different experiments were carried out: (1) storing relevant chemicals in the bags for up to three months; (2) exposing the bags including their content to accelerated conditions using a weatherometer, and (3) simulating an expected real case scenario. This study indicates that drugs and related chemicals stored in plastic bags may lead to a change in the composition of the chemical and an alteration or degradation of the plastic bag. All experiments led to the same conclusion: the polyvinyl chloride bags appeared to be the most affected. LDPE bags seem to be more appropriate for routine use, although it has been established they are not suitable for the collection of liquids (unless pre-packaged in, for instance, a glass container).

Pasin, D., Cawley, A., Bidny, S. & Fu, S. 2017, 'Characterization of hallucinogenic phenethylamines using high-resolution mass spectrometry for non-targeted screening purposes.', Drug Test Anal.
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Hallucinogenic phenethylamines such as 2,5-dimethoxyphenethylamines (2C-X) and their N-(2-methoxybenzyl) derivatives (25X-NBOMe) have seen an increase in novel analogues in recent years. These rapidly changing analogues make it difficult for laboratories to rely on traditional targeted screening methods to detect unknown new psychoactive substances (NPS). In this study, twelve 2C-X, six 2,5-dimethoxyamphetamines (DOX), and fourteen 25X-NBOMe derivatives, including two deuterated derivatives (2C-B-d6 and 25I-NBOMe-d9 ), were analyzed using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS). Collision-induced dissociation (CID) experiments were performed using collision energies set at 10, 20, and 40 eV. For 2C-X and DOX derivatives, common losses were observed including neutral and radical losses such as NH3 (17.0265 Da), •CH6 N (32.0500 Da), C2 H7 N (45.0578 Da) and C2 H9 N (47.0735 Da). 2C-X derivatives displayed common product ions at m/z 164.0837 ([C10 H12 O2 ](+•) ), 149.0603 ([C9 H9 O2 ](+) ), and 134.0732 ([C9 H10 O](+•) ) while DOX derivatives had common product ions at m/z 178.0994 ([C11 H14 O2 ](+•) ), 163.0754 ([C10 H11 O2 ](+) ), 147.0804 ([C10 H11 O](+) ), and 135.0810 ([C9 H11 O](+) ). 25X-NBOMe had characteristic product ions at m/z 121.0654 ([C8 H9 O](+) ) and 91.0548 ([C7 H7 ](+) ) with minor common losses corresponding to 2-methylanisole (C8 H10 O, 122.0732 Da), 2-methoxybenzylamine (C8 H11 NO, 137.0847 Da), and •C9 H14 NO (152.1074 Da). Novel analogues of the selected classes can be detected by applying neutral loss filters (NLFs) and extracting the common product ions. Copyright © 2017 John Wiley & Sons, Ltd.

Portbury, S.D., Hare, D.J., Sgambelloni, C.J., Bishop, D.P., Finkelstein, D.I., Doble, P.A. & Adlard, P.A. 2017, 'Age modulates the injury-induced metallomic profile in the brain.', Metallomics, vol. 9, no. 4, pp. 402-410.
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The biological transition metals iron (Fe), copper (Cu) and zinc (Zn) are thought to contribute to the neuronal pathologies that occur following traumatic brain injury (TBI), and indeed our previously published work in young (3 month-old) mice clearly demonstrates a significant spatiotemporal modulation of metals following TBI. Of note, however, is the literature observation that there is both an apparent detrimental effect of aging on TBI outcomes and an alteration in metals and their various transporters with normal advancing age. Therefore, to determine whether there was an interaction between aging, metals and TBI, we have utilised laser ablation-inductively coupled plasma-mass spectrometry to examine the spatial and temporal distribution of Fe, Zn and Cu following an acute controlled cortical impact brain injury in aged (24 months) rodents. The relative abundance of metals in corresponding regions within the ipsilateral and contralateral hemispheres as well as the hippocampus was assessed. Substantial region and time point specific alterations in Fe, Zn and Cu were identified immediately and up to 28 days post-TBI. The data from this follow-up study has also been compared to our previous data from young animals, and aged mice exhibit an appreciably enhanced and persistent elevation of all metals in every region surveyed, with individual metal disparities at various time points observed post-injury. This may potentially contribute to the acceleration in the onset of cognitive decline and neurological disease that has been observed in the aged population following head trauma.

Stuart, B.H. & Thomas, P.S. 2017, 'Pigment characterisation in Australian rock art: A review of modern instrumental methods of analysis', Heritage Science, vol. 5, no. 1.
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© 2017 The Author(s).The many thousands of Aboriginal rock art sites extending across Australia represent an important cultural record. The styles and materials used to produce such art are of great interest to archaeologists and those concerned with the protection of these significant works. Through an analysis of the mineral pigments utilised in Australian rock art, insight into the age of paintings and practices employed by artists can be gained. In recent years, there has been an expansion in the use of modern analytical techniques to investigate rock art pigments and this paper provides a review of the application of such techniques to Australian sites. The types of archaeological information that may be extracted via chemical analysis of specimens collected from or at rock art sites across the country are discussed. A review of the applicability of the techniques used for elemental analysis and structural characterisation of rock art pigments is provided and how future technological developments will influence the discipline is investigated.

Su, D., McDonagh, A., Qiao, S.-.Z. & Wang, G. 2017, 'High-Capacity Aqueous Potassium-Ion Batteries for Large-Scale Energy Storage.', Adv Mater, vol. 29, no. 1.
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A potassium iron (II) hexacyanoferrate nanocube cathode material is reported, which operates with an aqueous electrolyte to deliver exceptionally high capacities (up to 120 mA h g(-1) ). The cathode material exhibits excellent structural integrity, leading to fast kinetics and highly reversible properties. All of the battery materials are safe, inexpensive, and provide superior high-rate, long-cycle-life electrochemical performance.

Tam, R., Heather, E., Shimmon, R., Lam, B. & McDonagh, A.M. 2017, 'Synthesis and organic impurity profiling of 4-methoxymethamphetamine hydrochloride and its precursors.', Forensic Sci Int, vol. 272, pp. 184-189.
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4-Methoxymethamphetamine (PMMA) was synthesised from star anise and from 4-methoxytoluene and the organic impurity profiles examined. These two starting materials are unrestricted chemicals in many jurisdictions and contain the requisite functional groups and are thus well suited for clandestine manufacturers. trans-Anethole was extracted from star anise and oxidised to 4-methoxyphenyl-2-propanone (PMP2P). 4-Methoxytoluene was oxidised to anisaldehyde, converted to 4-methoxyphenyl-2-nitropropene, and then reduced to PMP2P. The PMP2P obtained by both methods was then converted to PMMA via the Leuckart reaction. 4-Methoxymethamphetamine hydrochloride (PMMA·HCl) was synthesised from PMMA using hydrogen chloride gas. Both of the examined synthetic methods were found to be feasible routes into PMMA·HCl. The products of each step were analysed by gas chromatography-mass spectrometry (GC-MS) and proton nuclear magnetic resonance spectroscopy ((1)H NMR). Impurities were examined in an attempt to identify route specific compounds, which may provide valuable information about the synthetic pathway and precursors.

Taudte, R.V., Roux, C. & Beavis, A. 2017, 'Stability of smokeless powder compounds on collection devices.', Forensic Sci Int, vol. 270, pp. 55-60.
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The current trend towards the implementation of organic gunshot residue (OGSR) analysis into gunshot residue (GSR) investigation protocols typically involves the sequential analysis of inorganic and organic GSR. However, to allow for the consecutive analysis of inorganic and organic GSR, specimens will often be stored for different lengths of time which may result in compounds of interest degrading. In order to optimise storage conditions, it is important to consider compound degradation on collection devices during storage. This study investigated the degradation over time of compounds potentially present in smokeless powders and OGSR on two collection devices, alcohol swabs and GSR stubs. Over a period of 63 days, the highest degree of degradation was found in the first four days. Interestingly, energetic compounds were generally found to be more stable than smokeless powder additives such as stabilisers including diphenylamine and ethyl centralite, which might be problematic considering that these compounds are common targets for OGSR. The findings can provide valuable information to operational forensic laboratories to optimise their storage durations.

Wei, Z., Niu, Q., Zhang, F., Xiao, K., Liu, L., Wang, Y., Jia, J., Cao, J., Fu, S. & Yun, K. 2017, 'The effect of sodium fluoride, formaldehyde, and storage temperature on the stability of methamidophos in post-mortem blood and liver.', Int J Legal Med, vol. 131, no. 3, pp. 667-675.
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Poisoning by organophosphorus insecticides such as methamidophos makes up a significant portion of forensic identification cases in China. Stability of methamidophos during specimen storage remains largely unknown. This study aimed to examine the long-term stability of methamidophos in postmortem specimens. Three experimental dogs after oral administration of methamidophos were sacrificed, and blood and liver specimens were collected and stored at various conditions. Gas chromatography-mass spectrometry (GC/MS) was used to measure the methamidophos concentrations after 0, 4, 7, 12, 16, 60, and 180 days of storage. The results showed that methamidophos was not stable and followed first-order degradation kinetics at all storage conditions investigated. The degradation half-life in blood was 12.2, 16.9, 11.0, and 1.0 days when the samples were stored at room temperature (RT, 20 °C), 4 °C, -20 °C, and at RT with 1 % sodium fluoride (NaF), respectively. The degradation half-life in liver was 4.1, 9.8, 17.8, and 2.0 days when the samples were stored at RT, 4 °C, -20 °C, and at RT with liver fixed in 10 % formaldehyde solution, respectively. These findings are significant in guiding sample storage and data interpretation. Specimens containing methamidophos should be stored at -20 °C and analyzed as early as possible. Addition of NaF in blood and fixation of liver in formaldehyde should be avoided due to the accelerated degradation of methamidophos under these conditions. The preliminary study suggests that it might be possible to calculate methamidophos concentration at the time of death based on its first-order degradation kinetic under specific storage conditions.