Kenneth Pye Associates Ltd. - www.kpal.co.uk Kenneth Pye Associates Ltd.
 Scientific Research, Consultancy and Investigations

                     
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Chemical Analysis

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Major and Trace Element Analysis

A wide range of solid samples can be digested and analysed by inductively coupled plasma atomic emission spectrometry (ICP-AES) and ICP mass spectrometry (ICP-MS) to quantify the abundance of major, minor and trace elements.  Concentrations of up to 50 elements can be determined in small samples (>0.25 g). Where sample size is not limited, the composition can also be determined by x-ray fluorescence (XRF) analysis. Data can be processed to meet specific requirements using in-house proprietary software.  The data obtained can be compared with reference database information obtained from a wide range of environments and geographical coverage.

Examples using ICP data

    
Bivariate plots comparing: (left) Nd and Sm concentrations in a sample of boot mud and
control soil samples; (right) Ce/La ratio plotted against U/Th ratio for the same samples.

 

    
Spider diagrams comparing elemental concentrations (log scales) in mud taken from a suspect's boots
and control soil samples taken at a crime scene: (left) full suite of 49 elements, with the main differences
arrowed; (right) chondrite-normalized rare earth elements only.

 

    
Cumulative frequency plots comparing: (left) aluminium oxide concentration and (right) cerium/lanthanum
ratio in a database of nearly 2000 UK soil samples analysed by ICP.

 

Examples using XRF data


Locations of sediment samples collected from sand dune
sites in England and Wales.

 



Average SiO2 content in the 63-250 µm fraction of over 500 sediment samples collected
from dune sites in England and Wales: (top) east coast; and (bottom) west coast.

 


Plot of Al2O3/K2O ratio versus SiO2/Al2O3 ratio in the 63-250 µm fraction of over
500 dune sands from sites in England and Wales. The samples from Studland Bay,
Dorset (circled) are chemically clearly distinct.

 


Map showing the location of foredune crest sampling locations
along the coast of Denmark.

 

    
Frequency histograms of SiO2/Al2O3 ratio and Al2O3/Fe2O3 ratio for the 63-250 µm size
fractions of dune sand samples collected along the west coast of Denmark.

 


Cluster analysis dendrogram, obtained using Ward's method, for Danish
dune samples, based on concentration data for 29 elements determined by XRF.

 


Plots of the first two axes of a principal components analysis performed using
Ward's method, for Danish dune sand samples, based on concentration data
for 29 elements determined by XRF.

 


Stable Isotope Analysis

The 'light' elements hydrogen, carbon, nitrogen, oxygen and sulphur possess two or more stable isotopes which do not undergo radioactive decay. The isotopic ratios of these elements have been demonstrated to be useful indicators of many geological and biological processes. Ratios are determined either by continuous helium flow isotope ratio mass spectrometry (CF-IRMS) or combustion-gas chromatography isotope ratio mass spectrometry (C-GC-IRMS).

    

                                                       

Bivariate plots of δ13C against δ15N for: (left) the <150 mm, and (right) the >150 mm fractions of soil samples taken from one metre square
grids at two different locations in Berkshire, UK.

 


pH, Eh, Electrical Conductivity and Anion Analysis

Determination of pH, Eh and electrical conductivity (or total dissolved solids) can provide a useful indication of temporal and spatial variations in environmental conditions. Analyses can be performed in the field or laboratory using ion-selective electrodes. Anion determination by ion chromatography can also provide a rapid method of detecting variations in water and sediment character.


Variations in conductivity along approximately 40 km of the Bristol River Avon, UK.


Related Publications and Reports

Pye, K., Blott, S.J., Croft, D.J. and Witton, S.J. (2007). Discrimination between sediment and soil samples for forensic purposes using elemental data: An investigation of particle size effects. Forensic Science International 167, 30-42.
(click to view the abstract of this paper)

Pye, K., Blott, S.J., Croft, D.J. and Carter, J.F. (2006). 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.
(click to view the abstract of this paper)

Pye, K., Blott, S.J. and Wray, D.S. (2006). Elemental analysis of soil samples for forensic purposes by Inductively Coupled Plasma Spectrometry – precision considerations. Forensic Science International 160, 178-192.
(click to view the abstract of this paper)

Saye, S.E., Pye, K. and Clemmensen, L.B. (2006) Development of a cliff-top dune indicated by particle size and geochemical characteristics: Rubjerg Knude, Denmark. Sedimentology 53, 1-21.
(click to view the abstract of this paper)

Saye, S.E. and Pye, K. (2006). Variations in chemical composition and particle size of dune sediments along the west coast of Jutland, Denmark. Sedimentary Geology 183, 217-242.
(click to view the abstract of this paper)

Pye, K. and Blott, S.J. (2004). Comparison of soils and sediments using major and trace element data. In: Pye, K. and Croft, D. (Eds.) Forensic Geoscience - Principles, Techniques and Applications. Geological Society Special Publication No. 232, Geological Society Publishing House, Bath, pp. 183-196.
(click to view the abstract of this paper)

Saye, S.E. and Pye, K. (2004) Development of a coastal dune sediment database for England and Wales: forensic applications. In: Pye, K. and Croft, D. (Eds.) Forensic Geoscience - Principles, Techniques and Applications. Geological Society Special Publication No. 232, Geological Society Publishing House, Bath, pp. 75-96.
(click to view the abstract of this paper)

Croft, D.J. and Pye, K. (2004) Stable carbon and nitrogen isotope variations in soils: forensic applications. In: Pye, K. and Croft, D. (Eds.) Forensic Geoscience - Principles, Techniques and Applications. Geological Society Special Publication No. 232, Geological Society Publishing House, Bath, pp. 257-267.
(click to view the abstract of this paper)

Croft, D.J. and Pye, K. (2003) The potential use of continuous-flow isotope-ratio mass spectrometry as a tool in forensic soil analysis: a preliminary report. Rapid Communications in Mass Spectrometry 17, 2581-2584.
(click to view the abstract of this paper)



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Page last modified: November 04, 2008