Elemental analysis of soil samples for forensic purposes by inductively coupled plasma spectrometry - precision considerations

Major and trace elemental composition provides a powerful basis for forensic comparison of soils, sediments and rocks. However, it is important that the potential 'errors' associated with the procedures are fully understood and quantified, and that standard protocols are applied for sample preparation and analysis. This paper describes such a standard procedure and reports results both for instrumental measurement precision (repeatability) and overall 'method' precision (reproducibility). Results obtained both for certified reference materials and example soils show that the instrumental measurement precision (defined by the coefficient of variation, CV) for most elements is better than 2-3%. When different solutions were prepared from the same sample powder, and from different sub-sample powders prepared from the same parent sample, the CV increased to c. 5-6% for many elements. The largest variation was found in results for certified reference materials generated from 23 instrument runs over an 18 month period (mean CV=c. 11%). Some elements were more variable than others. W was found to be the most variable and the elements V, Cr, Co, Cu, Ni and Pb also showed higher than average variability. SiO2, CaO, Al2O3 and Fe2O3, Rb, Sr, La, Ce, Nd and Sm generally showed lower than average variability, and therefore provided the most reliable basis for inter-sample comparison. It is recommended that, whenever possible, samples relating to the same investigation should be analysed in the same sample run, or at least sequential runs.

An integrated study (geochemistry, stable oxygen and carbon isotopes, nannofossils, planktonic foraminifera, inoceramid bivalves, ammonites and crinoids) of the Waxahachie Dam Spillway section, north Texas: a possible boundary stratotype for the base of the Campanian Stage

The spillway of Lake Waxahachie, Ellis County (Texas), exposes a > 17 m section of the Hutchins Member of the Austin Chalk Group, un-conformably overlain by Taylor Clay. The Austin sequence was regarded as a potential Global Stratotype Section for the base of the Campanian Stage at the 1995 Brussels meeting on Cretaceous Stage boundaries, with the last occurrence of the crinoid Marsupites testudinarius (von Schlotheim, 1820) as the potential boundary marker. An integrated study of the geochemistry, stable carbon and oxgen isotopes, nannofossils, planktonic foraminifera, inoceramid bivalves, ammonites and crinoids of this section place the last occurrence of M. testudinarius in a matrix of eighteen ancillary biostratigraphic markers, while the boundary can also be recognised on the basis of a delta C-13 excursion that can, in principle, be detected globally in marine sediments. A new forma of the crinoid Marsupites testudinarius is introduced. The Waxahachie section fulfils sufficient geological criteria as to be an excellent candidate GSSP for the base of the Campanian Stage, if problems of ownership and access to the section can be resolved.