4.0 Article

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

Journal

ACCREDITATION AND QUALITY ASSURANCE
Volume 18, Issue 5, Pages 391-401

Publisher

SPRINGER
DOI: 10.1007/s00769-013-1002-y

Keywords

Method validation; Measurement uncertainty; Speciation analysis; Chromium species; HPLC-ICP-MS

Funding

  1. Polish Ministry of Science and Higher Education [MNiSzW N N204 140439]

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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.

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