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Automated SEM-EDS (QEMSCAN®) Mineral Analysis in Forensic Soil Investigations: Testing Instrumental Reproducibility

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Automated SEM-EDS (QEMSCAN®) Mineral Analysis in Forensic Soil Investigations: Testing Instrumental Reproducibility See discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/227276851 Automated SEM-EDS (QEMSCAN®) mineral analysis in forensic soil investigations: Testing instrumental reproducibility Chapter · January 2009 DOI: 10.1007/978-1-4020-9204-6_26 CITATIONS READS 24 583 6 authors, including: Duncan Pirrie Matthew Power 126 PUBLICATIONS 2,506 CITATIONS SGS Canada 54 PUBLICATIONS 631 CITATIONS SEE PROFILE SEE PROFILE Gavyn Rollinson Patricia E.J. Wiltshire University of Exeter University of Southampton 76 PUBLICATIONS 565 CITATIONS 46 PUBLICATIONS 754 CITATIONS SEE PROFILE SEE PROFILE Some of the authors of this publication are also working on these related projects: FAME (EU) View project Investigation into the applicability of Bayesian networks to palynological data. View project All content following this page was uploaded by Gavyn Rollinson on 24 October 2014. The user has requested enhancement of the downloaded file. Chapter 26 Automated SEM-EDS (QEMSCAN®) Mineral Analysis in Forensic Soil Investigations: Testing Instrumental Reproducibility Duncan Pirrie, Matthew R. Power, Gavyn K. Rollinson, Patricia E.J. Wiltshire, Julia Newberry and Holly E. Campbell Abstract The complex mix of organic and inorganic components present in urban and rural soils and sediments potentially enable them to provide highly distinctive trace evidence in both criminal and environmental forensic investigations. Organic components might include macroscopic or microscopic plants and animals, pollen, spores, marker molecules, etc. Inorganic components comprise naturally derived minerals, mineralloids and man-made materials which may also have been manu- factured from mineral components. Ideally, in any forensic investigation there is a need to gather as much data as possible from a sample but this will be constrained by a range of factors, commonly the most significant of which is sample size. Indeed, there are a very wide range of analytical approaches possible, and a range of parameters that can be measured in the examination of the inorganic components present in a soil or sediment. These may include bulk colour, particle size distribution, pH, bulk chemistry, mineralogy, mineral chemistry, isotope geochemistry, micropalaeontology D. Pirrie(*ü ) and H.E. Campbell1 Helford Geoscience LLP, Menallack Farm Treverva, Penryn, Cornwall TR10 9BP, UK [email protected] D. Pirrie and M.R. Power Intellection UK Ltd, North Wales Business Park Abergele LL22 8LJ, UK G.K. Rollinson Camborne School of Mines, University of Exeter Cornwall Campus, Penryn, Cornwall TR10 9EZ, UK P.E.J. Wiltshire Department of Geography and Environment, University of Aberdeen, Elphinstone Road Aberdeen AB24 3UF, UK J. Newberry Department of Natural and Social Sciences, University of Gloucestershire, Swindon Road, Cheltenham GL50 4AZ, UK K. Ritz et al. (eds.), Criminal and Environmental Soil Forensics 411 © Springer Science + Business Media B.V. 2009 412 D. Pirrie et al. and mineral surface texture, amongst a host of others. Whilst it would be prudent to utilise as many parameters as possible, the forensic significance of the resultant data should be carefully considered. In particular, many parameters that could be measured (such as particle size distribution, pH and colour) may be affected by the nature of the sample, and vary temporally, or in response to sample storage conditions and hence, provide misleading results. The inorganic components of soil and sediment are typically relatively inert and therefore, potentially, one of the more valuable parameters to measure. To this end, we have utilised an automated scanning electron microscope with linked energy dispersive X-ray spectrometers (QEMSCAN®) in numerous criminal forensic investigations. The sample measurement is operator independent and enables detailed characterisation of the mineralogy of even small samples. The reproducibility of automated SEM-EDS analysis using QEMSCAN was tested by the repeated analysis of the same samples using the same operating, measurement and processing parameters. The results show that instru- mental variability is significantly less than observed natural variability between samples. The observed instrumental variability is interpreted to be a function of the sub-sampling of a different sub-set of the overall assemblage of particles present in the samples analysed. Thus automated mineral analysis can be regarded as a robust, highly repeatable method in forensic soil examination. Introduction The analysis of particulate trace evidence which has been passively or actively transferred to an offender, or to a vehicle or an object linked to an offender, has been widely used in the detection of serious crime. For example, trace evidence might include tissue, hair or body fluids from the victim or fibres from a victim’s clothing or some other surface. In other cases, trace evidence might include particulate materials present in the environment, either derived from natural biological or geological origins, or man-made materials or mineral products that are also present in the environment. To test an association or otherwise, between a suspect and a place or a victim, consideration of the overall assemblage of particles present can provide a much more distinctive pattern, than an elusive search for so-called rare or distinctive particles. In particular, it can be very compelling in criminal forensics if two populations or assemblages of particles from unrelated classes of trace evidence co-occur in samples from, for example, a crime scene and a possible offender’s footwear. Soil is a valuable type of trace evidence in that it is largely composed of two broadly unrelated groups of particulate trace evidence – the organic and the inorganic components. Soils will contain organic components such as macroscopic and micro- scopic plant remains, commonly the most useful of which are pollen and spores. Organic components in soil samples might also include micro-organisms such as 26 Instrumental Variability in Automated SEM-EDS Mineralogy 413 diatoms, or biological marker molecules. The soil sample will also contain an inorganic component which will be dominantly composed of naturally occurring mineral grains derived from the underlying bedrock geology and its weathering products, along with minerals from overlying superficial deposits. Additionally, even in rural environments, there may be introduced inorganic components, including both naturally occurring minerals and mineral products and also other man-made materials. Although there is an interrelationship between the organic (biological) and the inorganic (geological) particles present, they can largely be viewed as discrete classes of trace evidence. Consequently, if the same populations of both organic and inorganic particulates co-occur in control samples from a crime scene and from samples related to a suspect, then the presence of these two classes of trace evidence together can strengthen any evidential link (e.g. Brown et al. 2002). There is a wide range of different physical, chemical, mineralogical and biological parameters which can be measured in a soil sample. In both research articles and forensic casework, physical, chemical and mineralogical approaches used to test the similarity, or otherwise, of different soil samples have included: particle size distribution, sand grain surface morphology, bulk soil colour, pH, conductivity, bulk major, minor and trace element geochemistry, individual grain chemistry, bulk mineralogy, individual grain mineralogy and stable isotope geochemistry (e.g. Brown 2006; Brown et al. 2002; Marumo et al. 1986; McCrone 1992; McVicar and Graves 1997; Morgan et al. 2006; Pirrie et al. 2004; Pye 2004; Pye and Croft 2007; Pye et al. 2006a, b; Rawlins et al. 2006; Ruffell and Wiltshire 2004; Sugita and Marumo 1996, 2001). Biological approaches have included the examination of soil palynology, microbiology, such as mycology, diatoms, micro-palaeontology (Mildenhall et al. 2006; Wiltshire 2006), and the examination of organic marker molecules (Dawson et al. 2004). In the UK there is no agreement on the best protocols or methodologies for the forensic examination of soil samples. The evidential value of many of these approaches can be challenged both scientifically and in court, and the resultant data might lead to erroneous false positive or false negative conclusions as to the similarity or otherwise between two soil samples (c.f. Morgan and Bull 2007). For example, it is clear through forensic casework experience that different fabrics coming into contact with the same soil surface will pick up and retain different particle sizes. The relationships between grain size and mineralogy of the soil, and other indirect parameters which are controlled by the soil mineralogy, such as the bulk soil geochemistry, will affect such phenomena. Consequently, the direct, uncritical comparison of the bulk chemistry of the soil and the particles recovered from clothing would potentially give a false negative correlation. Of the currently available methodologies for the examination of soil samples, an integrated soil mineralogy and soil palynology approach has been shown to provide the best discriminatory ability and has also proven to be the best approach when examining the provenance of an unknown soil sample (e.g. Brown 2006; Brown et al. 2002; Rawlins et al. 2006). Although soil mineralogy is acknowledged as an appropriate and important discriminant, there are a number of methods
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