Speciation of Chromium in Alkaline Soil Extracts by an Ion-Pair Reversed Phase HPLC-ICP MS Method.

The aim of this work was to study by a hyphenated HPLC-ICP MS technique the chromium species released during alkaline extraction of various soils collected from a contaminated area of an old tannery. An ultrasound-assisted extraction procedure using 0.1 mol L Na₂CO₃ solution was developed for the release of chromium species from the soil. The chromium species in the soil extracts were separated on a C₈ column using EDTA and TBAH solution as a mobile phase. The use of an ICP-QQQ MS spectrometer in tandem mass configuration (MS/MS) combined with an octopole reaction system (ORS³) pressurized with helium allows one to eliminate spectral interferences during Cr determination in the soil extracts. The detection limit of the procedure was 0.08 µg L for Cr(III) and 0.09 µg L for Cr(VI) species. The trueness of the IP RP HPLC-ICP MS method was proved by an analysis of CRM 041 and CRM 060. The advantage of the proposed method is the analysis of soil extracts without their preliminary neutralization, which limits the losses of Cr(VI) due to the reduction process. The analysed soils mainly contained chromium in immobile forms (94.6⁻98.5% of the total Cr content). In all alkaline soil extracts mostly the Cr(VI) form was found, but in the extract of organic soils Cr(III) was also present. This arose from the reduction of Cr(VI) species by organic matter (humic acids) and Fe(II). The amount of formed Cr(III) species was dependent on the type of soil (content of organic matter, Mn and Fe) and its moistness. For the first time, the presence of neutral and non-polar chromium fractions in the soil extracts was also demonstrated. It was found that reliable speciation analysis results could be obtained for mineral soils.