Abstract

Trace concentrations of Cd, Cu, Pb and Zn in four different sediment fractions extracted in sequence were determined by isotope dilution inductively coupled mass spectrometry (IDICPMS). The metals from each fraction were extracted following the sequential extraction procedure recommended by the Bureau Commun de Référence (BCR) of the Commission of the European Communities. As an alternative to external calibration, the elements were quantified by spiking the extracted solutions with 112Cd, 63Cu, 208Pb and 66Zn and application of isotope dilution. The proposed approach was applied to a sample collected from a lake and two standard reference materials, NIST2704 river sediment from the National Institute of Standards & Technology and the BCR-277 estuarine sediment. Detection limits, for each extracted solution, varied from 0.31 to 0.53 mug L¹ for Cd, 0.92 to 2.9 mug L¹ for Cu, 0.22 to 1.1 mug L¹ for Pb and 1.3 to 7.6 mug L¹ for Zn. The sum of the metals concentration in the different fractions was compatible with 95% confidence level found amounts obtained with complete digestion of the samples and with the certified values of the standard reference materials.

Highlights

  • Since total concentration does not yield information on mobility, origin or bioavailability of metallic elements, metals in sediments have to be associated with the different fractions present

  • Repeated determinations of Ca, Mg, Fe and Ti in five sediment sub-samples by inductively coupled plasma-mass spectrometry (ICP-MS) present less than 5% variability, confirming the homogeneous distribution of these elements

  • The sample matrices produced by the application of the Bureau Commun de Référence (BCR) protocol were different from that of the standard solution used

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Summary

Introduction

Since total concentration does not yield information on mobility, origin or bioavailability of metallic elements, metals in sediments have to be associated with the different fractions present. For soils and sediments the term speciation refers to the process of identification and quantification of metals in phases, such as carbonates, J. Soc. procedure for inter-laboratory comparison.[10,11,12] This protocol emphasizes the extraction of metals using acetic acid for exchangeable and soluble compounds, hydroxylamine chloride for Mn and Fe oxides, hydrogen peroxide plus ammonium acetate for those bound to organic matter and sulphides, and aqua regia plus perchloric acid for the mineral fractions

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