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DOI: 10.1039/A804444I (Paper) Reference Section for: J. Anal. At. Spectrom., 1998, 13, 1245-1248

Decomposition of marine sediments for quantitative recovery of chromium and inductively coupled plasma mass spectrometric analysis

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L. Yang, J. W. H. Lam, R. E. Sturgeon and J. W. McLaren

Abstract

A method is described for the determination of total chromium in National Research Council of Canada Certified Reference Material (CRM) sediments HISS-1, PACS-2 and BCSS-1 using inductively coupled plasma mass spectrometry (ICP-MS). Complete solubilization of Cr was achieved with closed vessel microwave digestion using a mixture of HNO3 and HF followed by an open beaker reflux with HClO4 and H2SO4 for 8-12 h at 290[thin space (1/6-em)]°C. Subsequent quantification by quadrupole ICP-MS required complete removal of residual HClO4 and H2SO4 in order to eliminate polyatomic ion interferences on 52Cr and 53Cr from 35ClOH, 34S18O and 37ClO, respectively; this was achieved by baking the residue at 335[thin space (1/6-em)]°C. Values of 30.0±3.4, 95.6±1.0 and 123±2 μg g–1 were obtained for HISS-1, PACS-2 and BCSS-1, respectively, in agreement with their respective certified values of 30.0±6.8, 91.8±5.8 and 123±14 μg g–1. The detection limit (3σ), based on a 0.25 g sample and a 250 ml final volume, was 0.4 μg g–1. The methodology is suitable for the determination of other trace elements of interest in these sediments.

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