Study on multielemental speciation analysis of Cr(VI), As(III) and As(V) in water by advanced hyphenated technique HPLC/ICP-DRC-MS. Fast and reliable procedures.

Analytical procedures for multielemental speciation analysis of arsenite - As(III), arsenate - As(V) and hexavalent chromium - Cr(VI) in water using high performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC/ICP-DRC-MS) hyphenated technique have been developed. A dynamic reaction cell (DRC) for spectral interferences elimination has been involved in the experiment. Application of oxygen and ammonia as reaction gases in the DRC under various conditions has been verified. Optimization of the following chromatographic conditions: mobile phase composition, concentration of particular components, mobile phase pH and flow rate, injection volume and column temperature, has been conducted. Species separation has been carried out on anion-exchange chromatographic column using isocratic elution with: 22 mM (NH4)2HPO4, 25 mM NH4NO3 (for procedure A) and 22 mM (NH4)2HPO4, 65 mM NH4NO3 (for procedure B) as mobile phases. Detection limits (LD) for procedure A were 0.16 µg L(-1), 0.090 µg L(-1), 0.073 µg L(-1), and for procedure B were 0.14 µg L(-1), 0.062 µg L(-1), 0.15 µg L(-1) for As(III), As(V) and Cr(VI), respectively. Linearity was tested at two concentration ranges of: (0.5-10.0) µg L(-1) for procedure A and (5-50) µg L(-1) for procedure B, and showed correlation coefficients for each of the analytes to be above 0.999. Repeatability values obtained for spiked real water samples were in the range of (4.2-7.6)% and (2.0-2.4)% for procedure A and B respectively. Accuracy was calculated based on the analysis of spiked real water samples at three concentration levels. Obtained recoveries were from 94% to 102%.