A modified lead–matrix separation procedure shown for lead isotope analysis in Trojan silver artefacts as an example

• Published in: Analytical and bioanalytical chemistry 2013-03, Vol.405 (9), p.2995-3000
• Main Authors: Vogl, Jochen, Paz, Boaz, Koenig, Maren, Pritzkow, Wolfgang
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Antiquities; Archaeology - history; Archaeology - methods; Artefacts; Bicarbonates - chemistry; Biochemistry; Characterization and Evaluation of Materials; Chemical properties; Chemistry; Chemistry and Materials Science; Chromatography; Chromatography - methods; Composition; Eluents; Food Science; History, Ancient; Identification and classification; Ionization; Isotopes; Isotopes - analysis; Isotopes - isolation & purification; Laboratory Medicine; Lead; Lead (metal); Lead - analysis; Lead - isolation & purification; Lead isotopes; Mass spectrometry; Mass Spectrometry - methods; Methods; Monitoring/Environmental Analysis; Precious metal products; Ratios; Recovery; Scientific imaging; Sensitivity and Specificity; Separation; Separation (Technology); Silver; Silver - analysis; Technical Note; Water analysis; Water sampling
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-012-6323-x

A modified Pb–matrix separation procedure using NH 4 HCO 3 solution as eluent has been developed and validated for determination of Pb isotope amount ratios by thermal ionization mass spectrometry. The procedure is based on chromatographic separation using the Pb·Spec resin and an in-house-prepared NH 4 HCO 3 solution serving as eluent. The advantages of this eluent are low Pb blanks (60 °C). Pb recovery is >95 % for water samples. For archaeological silver samples, however, the Pb recovery is reduced to approximately 50 %, but causes no bias in the determination of Pb isotope amount ratios. The validated procedure was used to determine lead isotope amount ratios in Trojan silver artefacts with expanded uncertainties ( k  = 2)