Fast and Accurate Procedure for the Determination of Cr(VI) in Solid Samples by Isotope Dilution Mass Spectrometry

Abstract

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Quantification of Cr(VI) in soil samples from a contaminated area in northern Italy by isotope dilution mass spectrometry

“…The chromatographic separation of the Cr species was performed on a Dionex DX-120 LC System (Sunnyvale, CA, USA) with a Dionex Ion pack AS9-HC anion exchange column (PEEK, 4×250 mm×9 μm). The detection of the chromium species and iron (extracted together with chromium) was performed by ICP-MS using an Agilent 7500c quadrupole instrument (Agilent Technologies, Tokyo, Japan) equipped with an octopole collision cell and helium as the collision gas (Fabregat et al 2012). The determination of the total iron content (%) was performed by X-ray fluorescence spectrometry (Philips PW2404), and sample were prepared using a semiautomatic press (SPECEAC, Orpington, UK).…”

“…Measurement of isotope ratios by LC-ICP-MS Typical operating conditions and analytical characteristics of these determinations by LC-ICP-MS have been described elsewhere (Fabregat et al 2012). Integration of the chromatographic peaks was carried out using the commercial software supplied with the ICP-MS instrument.…”

“…The goal is to maximize extraction with a minimum rate of interconversion (EPA 2007). More recently, Fabregat et al (2012) demonstrated the advantages of the use of EDTA in the extraction phase to complex Cr(III) and prevent its potential oxidation to Cr(VI). In this study, Cr(III) was completely complexed by EDTA, and it was therefore not necessary to apply the double spike IDMS to correct for species interconversion.…”

“…In this work, we applied the extraction procedure developed by Fabregat et al (2012) to the analysis of a set of soil samples (SET1) from an area in the Lombardia region of northern Italy that is contaminated by the diffusion of Cr(VI) in groundwater. The extraction conditions previously optimized by Fabregat et al (2012) through the analysis of certified reference materials were modified here to minimize the extent of Cr(VI) reduction in the analysis of real samples (SET1).…”

“…The extraction conditions previously optimized by Fabregat et al (2012) through the analysis of certified reference materials were modified here to minimize the extent of Cr(VI) reduction in the analysis of real samples (SET1). Subsequently, milder extraction conditions were applied to a new set of soil samples (SET2) with a natural abundance of Cr(VI) coming from a wider area in the Lombardia region.…”