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NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur. For the publisher's version, please access the DOI link below./ Pour consulter la version de l'éditeur, utilisez le lien DOI ci-dessous.http://doi.org/10.1039/a909296jJournal of Analytical Atomic Spectrometry, 15, 2, pp. 143-149, 2000 A novel introduction system for hydride generation-inductively coupled plasma mass spectrometry: determination of selenium in biological materials A novel, robust hydride generation system compatible with sample introduction with inductively coupled plasma mass spectrometry is described and applied to the determination of Se in biological tissues. A short reaction time (60 ms) and a rapid separation of the reaction products is obtained by mixing the acidi®ed sample and the sodium borohydride reductant solution at the tip of a cross-¯ow nebuliser. A modi®ed Scott spray chamber serves as a gas±liquid separator, providing 30 s wash-in and wash-out times. Analytical results generated by external calibration and isotope dilution methodologies agree well with the certi®ed values for Se in certi®ed biological reference materials DORM-2 and DOLT-2. Detection limits for Se and other hydride forming elements, i.e., As, Sn and Sb, are below 10 ng l 21 with typical precision of 2% RSD at the 10 ng ml 21 level. Volatile species o...
Sixteen soil and sedimentary geological reference materials were analysed for As and the heavy metals Cd, Co, Cr, Cu, Ni, Pb and Zn by inductively coupled plasma-atomic emission spectrometry (ICP-AES) and inductively coupled plasma-mass spectrometry (ICP-MS) in combination with total and partial dissolution of the samples. It can be demonstrated that none of the modern ICP methods is completely free from analytical problems. This applies in particular when the concentrations are close to the detection limits (e.g. in ICP-AES) and is mainly due to the wide variation in the bulk composition of soils resulting in complex matrix effects (e.g. in ICP-MS). In order to determine the extent of soil pollution by heavy metals, both partial and total dissolution have to be performed prior to analysis.
The suitability of laser ablation ICP-MS for minor and trace analysis of archaeological iron finds, produced by a direct reduction process in a 'bloomery' furnace, is reported. The analysis of elemental impurities in the iron can provide useful archaeometallurgical information on the production process and the provenance of the iron. Since, even after refinement, the iron resulting from this process may contain many inclusions (slag, charcoal, holes, etc.), a method should be used with sufficient spatial resolution to preclude the inclusions from the analysis. The ablation parameters are selected such that ablation craters of approx. 100 microm in diameter are obtained. The method is validated with low alloy steel and cast iron standard reference materials and by a comparative analysis with electron probe microanalysis (EPMA). The precision is limited mainly by the homogeneity of the iron, rather than by instrumental reproducibility. The advantages and drawbacks of the method are briefly compared with EPMA. Preliminary results from the analysis of archaeological iron samples from excavations at Develier-Courtetelle (Canton Jura, CH), Neftenbach (Canton Zurich, CH), Wartau (Canton St Gallen, CH) and Mont Chemin (Canton Valais, CH) are given.
Careful tracing of evidence at the site of a crime must be performed before suspects can be convicted of a crime or homicide. Fingerprints and ballistic control samples are important evidence. A common method used to examine lead bullets is comparison of physical properties such as weight, dimensions, shape, and distinctive markings. However ballistic investigations, for example comparison of characteristic scratches and marks left on fired bullets, do not always give sufficient information. Ballistic abrasion patterns can change for a variety of reasons, e.g. deformation or mechanical strain. Sometimes only particles remain in a victim's body. In such cases trace-element composition and lead-isotope ratios can be compared with those of controls. Elemental composition of particles and deformed bullets have been compared with the elemental fingerprints and isotope ratios of potential bullet types found on suspects. The applicability of the method was studied for two different cases. Data interpretation and several limitations of the technique are also discussed in this paper.
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