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

  • Duncan PirrieEmail author
  • Matthew R. Power
  • Gavyn K. Rollinson
  • Patricia E. J. Wiltshire
  • Julia Newberry
  • Holly E. Campbell

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 manufactured 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 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 instrumental 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.


Inorganic Component Crime Scene Forensic Investigation Mineralogical Data Accelerator Pedal 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.


Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.


  1. ASTM (2002). Standard guide for gunshot residue analysis by scanning electron microscopy/ energy dispersive spectroscopy. Annual Book of ASTM Standards 2002:528–530.Google Scholar
  2. Benvie B (2007). Mineralogical imaging of kimberlites using SEM-based techniques. Minerals Engineering 20:435–443.CrossRefGoogle Scholar
  3. Brown AG (2006). The use of forensic botany and geology in war crimes investigations in NE Bosnia. Forensic Science International 163:204–210.PubMedCrossRefGoogle Scholar
  4. Brown AG, Smith A and Elmhurst O (2002). The combined use of pollen and soil analyses in a search and subsequent murder investigation. Journal of Forensic Sciences 47:614–618.PubMedGoogle Scholar
  5. Brozek-Mucha Z and Jankowicz A (2001). Evaluation of the possibility of differentiation between various types of ammunition by means of GSR examination with SEM-EDX method. Forensic Science International 123:39–47.PubMedCrossRefGoogle Scholar
  6. Bull PA and Morgan RM (2006). Sediment fingerprints. Science and Justice 46:107–124.PubMedCrossRefGoogle Scholar
  7. Camm GS, Butcher AR, Pirrie D, Hughes PK and Glass HJ (2003). Secondary mineral phases associated with a historic arsenic calciner identified using automated scanning electron microscopy: a pilot study from Cornwall, UK. Minerals Engineering 16:1269–1277.CrossRefGoogle Scholar
  8. Dawson LA, Towers W, Mayes RW, Craig J, Väisänen RK and Waterhouse EC (2004). The use of plant hydrocarbon signatures in characterising soil organic matter. In: Forensic Geoscience: Principles, Techniques and Applications (Eds. K Pye and DJ Croft), pp 269–276. The Geological Society of London Special Publication 232, London.Google Scholar
  9. Goodall WR and Scales PJ (2007). An overview of the advantages and disadvantages of the determination of gold mineralogy by automated mineralogy. Minerals Engineering 20:506–517.CrossRefGoogle Scholar
  10. Knight RD, Klassen RA and Hunt P (2002). Mineralogy of fine-grained sediment by energy-dispersive spectrometry (EDS) image analysis — a methodology. Environmental Geology 42:32–40.CrossRefGoogle Scholar
  11. Lotter NO, Kowal DL, Tuzun MA, Whittaker PJ and Kormos L (2003). Sampling and flotation testing of Sudbury Basin drill core for process mineralogy modelling. Minerals Engineering 16:857–864.CrossRefGoogle Scholar
  12. Martin RS, Mather TA, Pyle DM, Power M, Allen AG, Aiuppa A, Horwell CJ and Ward CPJ (in press). Composition resolved size distributions of volcanic aerosols in the Mt Etna plumes. Journal of Geophysical Research.Google Scholar
  13. Marumo Y, Nagatsuka S and Oba Y (1986). Clay mineralogical analysis using the <0.05 mm fraction for forensic science investigation — its application to volcanic ash soils and yellow-brown forest soils. Journal of Forensic Sciences 31:92–105.Google Scholar
  14. McCrone WC (1992). Forensic soil examination. Microscope 40:109–121.Google Scholar
  15. McKinley J and Ruffell A (2007). Contemporaneous spatial sampling at scenes of crime: advantages and disadvantages. Forensic Science International 172:196–202.CrossRefGoogle Scholar
  16. McVicar MJ and Graves WJ (1997). The forensic comparison of soils by automated scanning electron microscopy. Journal of the Canadian Society of Forensic Scientists 30:241–261.Google Scholar
  17. Mildenhall DC, Wiltshire PEJ and Bryant VM (2006). Forensic palynology: why do it and how it works. Forensic Science International 163:163–172.PubMedCrossRefGoogle Scholar
  18. Morgan RM and Bull PA (2007). Forensic geoscience and crime detection. Minerva Medicolegale 127:73–89.Google Scholar
  19. Morgan RM, Wiltshire PEJ, Parker A and Bull PA (2006). The role of geoscience in wildlife crime detection. Forensic Science International 162:152–162.PubMedCrossRefGoogle Scholar
  20. Morgan RM, Little M, Gibson A, Hicks L, Dunkerley S and Bull PA (in press). The preservation of quartz grain surface textures following vehicle fire and their use in forensic enquiry. Science and Justice.Google Scholar
  21. Pirrie D, Power MR, Rollinson G, Camm GS, Hughes SH, Butcher AR and Hughes P (2003). The spatial distribution and source of arsenic, copper, tin and zinc within the surface sediments of the Fal Estuary, Cornwall, UK. Sedimentology 50:579–595.CrossRefGoogle Scholar
  22. Pirrie D, Butcher AR, Power MR, Gottlieb P and Miller GL (2004). Rapid quantitative mineral and phase analysis using automated scanning electron microscopy (QEMSCAN®); potential applications in forensic geoscience. In: Forensic Geoscience: Principles, Techniques and Applications (Eds. K Pye and DJ Croft), pp 123–136. The Geological Society of London Special Publication 232, London.Google Scholar
  23. Pye K (2004). Forensic examination of sediments, soils, dusts and rocks using scanning electron microscopy and X-ray chemical microanalysis. In: Forensic Geoscience: Principles, Techniques and Applications (Eds. K Pye and DJ Croft), pp 103–122. The Geological Society of London Special Publication 232, London.Google Scholar
  24. Pye K and Croft DJ (2007). Forensic analysis of soil and sediment traces by scanning electron microscopy and energy-dispersive X-ray analysis: an experimental investigation. Forensic Science International 165:52–63.PubMedCrossRefGoogle Scholar
  25. Pye K, Blott SJ and Wray DS (2006a). Elemental analysis of soil samples for forensic purposes by inductively coupled plasma spectrometry — precision considerations. Forensic Science International 160:178–192.CrossRefGoogle Scholar
  26. Pye K, Blott SJ, Croft DJ and Carter JF (2006b). Forensic comparison of soil samples: Assessment of small-scale spatial variability in elemental composition, carbon and nitrogen isotope ratios, colour, and particle size distribution. Forensic Science International 163:59–80.CrossRefGoogle Scholar
  27. Rawlins BG, Kemp SJ, Hodgkinson EH, Riding JB, Vane CH, Poulton C and Freeborough K (2006). Potential and pitfalls in establishing the provenance of earth-related samples in forensic investigations. Journal of Forensic Sciences 51:832–845.PubMedCrossRefGoogle Scholar
  28. Reed SJB (2005). Electron Microprobe Analysis and Scanning Electron Microscopy in Geology. Cambridge University Press, Cambridge.Google Scholar
  29. Ruffell A and Wiltshire PEJ (2004). Conjunctive use of quantitative and qualitative X-ray diffraction analysis of soils and rocks for forensic analysis. Forensic Science International 145:13–23.PubMedGoogle Scholar
  30. Sugita R and Marumo Y (1996). Validity of colour examination for forensic soil identification. Forensic Science International 83:201–210.CrossRefGoogle Scholar
  31. Sugita R and Marumo Y (2001). Screening of soil evidence by a combination of simple techniques: validity of particle size distribution. Forensic Science International 122:155–158.PubMedCrossRefGoogle Scholar
  32. Wiltshire PEJ (2006). Consideration of some taphonomic variables of relevance to forensic palynological investigations in the United Kingdom. Forensic Science International 163:173–182.PubMedCrossRefGoogle Scholar
  33. Xiao Z and Laplante AR (2004). Characterizing and recovering the platinum group minerals - a review. Minerals Engineering 17:961–979.CrossRefGoogle Scholar
  34. Xie RK, Seip HM, Leinum JR, Winje T and Xiao JS (2005). Chemical characterization of individual particles (PM10) from ambient air in Guiyang City, China. Science of the Total Environment 343:261–272.PubMedCrossRefGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 2009

Authors and Affiliations

  • Duncan Pirrie
    • 1
    • 2
    Email author
  • Matthew R. Power
    • 2
  • Gavyn K. Rollinson
    • 3
  • Patricia E. J. Wiltshire
    • 4
  • Julia Newberry
    • 5
  • Holly E. Campbell
    • 1
  1. 1.Helford Geoscience LLPMenallack Farm TrevervaPenrynUK
  2. 2.Intellection UK Ltd.AbergeleUK
  3. 3.Camborne School of MinesUniversity of Exeter Cornwall CampusPenrynUK
  4. 4.Department of Geography and EnvironmentUniversity of AberdeenUK
  5. 5.Department of Natural and Social SciencesUniversity of GloucestershireUK

Personalised recommendations