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首页> 外文期刊>Mapan: Journal of Metrology Society of India >Development and Validation of Method with Evaluation of Measurement Uncertainty for the Speciation Analysis of Chromium by Ion Chromatography
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Development and Validation of Method with Evaluation of Measurement Uncertainty for the Speciation Analysis of Chromium by Ion Chromatography

机译：离子色谱法测定铬形态分析中测量不确定度评定方法的开发与验证

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摘要

In the present study a simple, sensitive and accurate method has been developed for the speciation analysis of chromium(III) and chromium(VI) in aqueous solution using ion chromatography separation followed by detection through a UV detector. Chromium(III) was detected as its pyridine-2,6-dicarboxylic acid (PDCA) complex at 365 nm by pre-derivatizing it with eluent containing PDCA. Chromium(VI) was detected by post column derivatization with diphenylcarbazide at 540 nm. This paper discusses in details about the method validation and established each parameter according to the IUPAC and EURACHEM approaches. Method is validated for linearity, accuracy, precision, limit of detection and limit of quantification as per the guide lines. The evaluation of expanded uncertainty in measurement of Cr(III) and Cr(VI) was done at 95 % confidence level (k = 2) according to EURACHEM GUM guide. The method can be applied to determine Cr(III) and Cr(VI) up to 2 mg/kg and 40 A mu g/kg respectively with associated measurement uncertainty value of about 5 %. The major contribution of uncertainty is due to recovery. The method described in the present study is sensitive, selective and capable of quantifying trace level of Cr(VI) and Cr(III).
机译：在本研究中，已开发出一种简单，灵敏且准确的方法，用于使用离子色谱分离然后通过UV检测器检测的水溶液中铬（III）和铬（VI）的形态分析。通过用含有PDCA的洗脱液对其进行预衍生化处理，检测到铬（III）在365 nm处为吡啶2,6-二羧酸（PDCA）络合物。通过二苯卡巴肼在540 nm柱后衍生检测铬（VI）。本文详细讨论了方法验证，并根据IUPAC和EURACHEM方法建立了每个参数。按照指导原则对方法的线性，准确性，精密度，检出限和定量限进行了验证。根据EURACHEM GUM指南，在95％置信度（k = 2）下完成了对Cr（III）和Cr（VI）测量的不确定性的扩展评估。该方法可用于测定分别高达2 mg / kg和40 Aμg / kg的Cr（III）和Cr（VI），相关的测量不确定度约为5％。不确定性的主要贡献是由于复苏。本研究中描述的方法灵敏，选择性强并且能够定量分析痕量Cr（VI）和Cr（III）。

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