Cordeiro Fernando, Robouch Piotr, de la Calle Maria Beatriz, Emteborg Håkan, Charoud-Got Jean, Schmitz Franz
European Commission, Directorate General Joint Research Centre, Institute for Reference Materials and Measurements, B-2440 Geel, Belgium.
J AOAC Int. 2011 Sep-Oct;94(5):1592-600. doi: 10.5740/jaoacint.10-404.
A collaborative study, International Evaluation Measurement Programme-25a, was conducted in accordance with international protocols to determine the performance characteristics of an analytical method for the determination of dissolved bromate in drinking water. The method should fulfill the analytical requirements of Council Directive 98/83/EC (referred to in this work as the Drinking Water Directive; DWD). The new draft standard method under investigation is based on ion chromatography followed by post-column reaction and UV detection. The collaborating laboratories used the Draft International Organization for Standardization (ISO)/Draft International Standard (DIS) 11206 document. The existing standard method (ISO 15061:2001) is based on ion chromatography using suppressed conductivity detection, in which a preconcentration step may be required for the determination of bromate concentrations as low as 3 to 5 microg/L. The new method includes a dilution step that reduces the matrix effects, thus allowing the determination of bromate concentrations down to 0.5 microg/L. Furthermore, the method aims to minimize any potential interference of chlorite ions. The collaborative study investigated different types of drinking water, such as soft, hard, and mineral water. Other types of water, such as raw water (untreated), swimming pool water, a blank (named river water), and a bromate standard solution, were included as test samples. All test matrixes except the swimming pool water were spiked with high-purity potassium bromate to obtain bromate concentrations ranging from 1.67 to 10.0 microg/L. Swimming pool water was not spiked, as this water was incurred with bromate. Test samples were dispatched to 17 laboratories from nine different countries. Sixteen participants reported results. The repeatability RSD (RSD(r)) ranged from 1.2 to 4.1%, while the reproducibility RSD (RSDR) ranged from 2.3 to 5.9%. These precision characteristics compare favorably with those of ISO 15601. A thorough comparison of the performance characteristics is presented in this report. All method performance characteristics obtained in the frame of this collaborative study indicate that the draft ISO/DIS 11206 standard method meets the requirements set down by the DWD. It can, therefore, be considered to fit its intended analytical purpose.
一项名为“国际评估测量计划 - 25a”的合作研究按照国际协议开展,以确定一种测定饮用水中溶解溴酸盐的分析方法的性能特征。该方法应满足欧盟理事会指令98/83/EC(在本工作中称为《饮用水指令》;DWD)的分析要求。正在研究的新的标准方法草案基于离子色谱法,随后进行柱后反应和紫外检测。参与合作的实验室使用了国际标准化组织(ISO)草案/国际标准草案(DIS)11206文件。现有的标准方法(ISO 15061:2001)基于使用抑制电导检测的离子色谱法,对于低至3至5微克/升的溴酸盐浓度测定,可能需要一个预浓缩步骤。新方法包括一个稀释步骤,可减少基质效应,从而能够测定低至0.5微克/升的溴酸盐浓度。此外,该方法旨在尽量减少亚氯酸根离子的任何潜在干扰。合作研究调查了不同类型的饮用水,如软水、硬水和矿泉水。其他类型的水,如生水(未处理的)、游泳池水、空白水样(称为河水)和溴酸盐标准溶液,也作为测试样品。除游泳池水外,所有测试基质都加入了高纯度溴酸钾,以使溴酸盐浓度范围为1.67至10.0微克/升。游泳池水未添加,因为该水样中已含有溴酸盐。测试样品被分发给来自九个不同国家的17个实验室。16名参与者报告了结果。重复性相对标准偏差(RSD(r))范围为1.2%至4.1%,而再现性相对标准偏差(RSDR)范围为2.3%至5.9%。这些精密度特征与ISO 15601的特征相比具有优势。本报告对性能特征进行了全面比较。在这项合作研究框架内获得的所有方法性能特征表明,ISO/DIS 11206标准方法草案符合DWD规定的要求。因此,可以认为它适合其预期的分析目的。