Speciation analysis of chromium in drinking water samples by ion-pair reversed-phase HPLC–ICP-MS: validation of the analytical method and evaluation of the uncertainty budget

Abstract

The approach presented in this article refers to the modification of a method for the detection and quantitative determination of chromium species in water by high-performance liquid chromatography inductively coupled plasma mass spectrometry. The main aim of this work was to establish a detailed validation of the analytical procedure and an estimation of the budget of measurement uncertainty which was helpful in recognizing the critical points of the presented method. As a result of the method validation experiment, the obtained limit of quantification, repeatability and intermediate precision were satisfied for the quantification Cr(III) and Cr(VI) in water matrices. The trueness of the method was verified via an estimation of the recovery of the spiked real samples. The recovery rate of both determined analytes was found to be between 93 and 115 %. Considering that the validation of the method and the evaluation of measurement uncertainty are crucial for quantitative analysis, the above-mentioned assessment of the uncertainty budget was performed in two different ways: a modelling approach and a single-laboratory validation approach. The measurement uncertainties of the results were found to be 4.4 and 7.8 % for Cr(III), 4.2 and 7.9 % for Cr(VI) using the classical concept and method validation data, respectively. This paper is the first publication to presenting all the steps needed to evaluate the measurement uncertainty for the speciation analysis of chromium species. In summary, the obtained results demonstrate that the method can be applied effectively for its intended use.

Atomic Spectrometry Update: review of advances in elemental speciation

“…98 The Cr species were extracted and separated from drinking water samples using RP ion pair HPLC. Two different approaches for estimating the uncertainties associated with an HPCL-ICP-MS measurement procedure, for Cr species present in drinking water, have been compared.…”

Development of a novel, fast, sensitive method for chromium speciation in wastewater based on an organic polymer as solid phase extraction material combined with HPLC–ICP-MS

“…For detection, inductively coupled plasma mass spectrometry (ICP-MS) is preferably used over the past decade due to the high sensitivity, rapidness and low detection limits. Hence, combining the advantages of these two techniques, HPLC-ICP-MS has been well used for the speciation of chromium in various samples [3][4][5][6][7][8][9]. However, direct determination of targets is extremely challenging for water samples which are complicated by the unknown matrices, in particular, the extremely low concentration of target analytes brings about huge toughness.…”

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

“…The inorganic arsenic species are highly toxic, with As(III) being the most toxic of arsenic species and a suspected human carcinogen, and with As(V) exhibiting relatively high toxicity [8,[25][26][27]. Chromium speciation is more complex, with Cr(III) being a necessary nutrient for humans, and with Cr(VI) reported as very mobile in the environment, carcinogenic and mutagenic [13,28,29].…”