Inductively coupled plasma‐mass spectrometry has revolutionized the field of multi‐elemental analysis because of its high sensitivity and speed of analysis. However, problems with polyatomic ion interferences during routine analysis can give rise to inaccuracies. We propose a method that systematically corrects for oxide and hydroxide interferences in routine analysis, for a wide range of materials. Oxide and hydroxide production for a specified element is calculated from measurements on each sample, as levels may depend on sample composition and may also vary with time. We show that oxide and hydroxide interferences can then be calculated for other elements, by reference to a set of oxide and hydroxide ratios measured on standard solutions. Validity of correction is controlled by internal tests involving two isotopes of one element with respect to experimental errors. The limits and validity of this approach are demonstrated with the analysis of selected reference materials.
A direct method for the determination of lead isotopic ratios by laser ablation‐inductively coupled plasma‐quadrupole mass spectrometry (LA‐ICP‐QMS) is presented. Samples of lake sediments were ground and pressed as pellets before being analysed. Mass bias was corrected by analysing an external calibration sample manufactured with pure silica doped with NIST SRM 981 solution. The efficiency of the mass bias correction was checked by comparing the ICP‐MS data with lead isotopic ratios determined by thermal ionisation mass spectrometry (TIMS). The average long term reproducibilities were 0.40%, 0.40%, 0.20% and 0.30% (RSD) respectively for the 206Pb/204Pb, 207Pb/204Pb, 206Pb/207Pb and 208Pb/206Pb ratios. The method was applied to the study of lake sediment samples, in order to determine the amount and origin of historical contamination by lead.
Revue d'archéométrie 34 | 2010 varia Mines d'argent du Montaigu (Hautes-Pyrénées, France) Une filière aquitaine de l'argent ? Étude isotopique du plomb Silver mines on the massif of Montaigu
The identification of gunshot residue (GSR) on wounds enables the differentiation of entry and exit wounds. Unfortunately, studies analyzing GSR on degraded bodies have been poorly documented, and no data exist regarding GSR detection after stagnant water immersion. The aim of this preliminary experimental study was to detect GSR on wounds altered in stagnant water, using scanning electron microscopy coupled with energy-dispersive X (SEM-EDX) and inductively coupled plasma mass spectrometry (ICP-MS). Shots were performed on sheep limbs with a 22LR at a distance of 20 cm. The limbs were then submerged in stagnant water and analyzed on days 0, 6, and 14. SEM-EDX was performed on previously dehydrated wounds. For ICP-MS analysis, the wounds were rubbed with a cotton swab that was then analyzed. In the SEM studies, a higher number of particles were detected in entry wounds compared to exit wounds under every set of experimental conditions. Unfortunately, SEM-EDX failed to detect GSR particles, even on day 0. ICP-MS enabled the detection of Pb, Sb, and Ba at every stage with higher quantities on entry than in exit. These elements remained detectable following limb immersion. ICP-MS enabled differentiate entry from exit wounds, even after immersion in stagnant water. Nevertheless, when manually swabbing the wounds, quantities of matter collected is highly variable. ICP-MS is a more suitable technique than SEM-EDX for GSR identification of wounds after decomposition in stagnant water; however, standardization is needed.
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