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Quality Assurance for In Situ Uranium Concentration Measurements of Aqueous Samples from Mineral Processing Studies Using a Portable XRF Analyser in Compliance with ISO/IEC 17025 Requirements
Geostandards and Geoanalytical Research ( IF 3.8 ) Pub Date : 2021-05-04 , DOI: 10.1111/ggr.12384
Ahmad Abukashabeh 1, 2 , Rachael Abu‐Halimeh 3
Affiliation  

The method developed in this article aims to control the quality of uranium leaching and processing measurements at the Jordan Atomic Energy Commission, through the instant determination of uranium in aqueous samples without chemical preparation using portable X-Ray Fluorescence (pXRF) analysis. Acidic and alkaline samples were analysed via pXRF then compared with results from ICP-MS/ICP-AES. The pXRF method validation, in view of ISO/IEC 17025:2017 requirements, was applied to real samples and simulated uranium ore solutions from single uranium and two other certified reference materials. The slopes acquired from correlations between pXRF results and reference values were 1.026, 1.021 and 0.9664, respectively, with correlation coefficients (r2) approaching 1.0. Precision calculations showed values < 5% RSD for samples having uranium contents > 10 mg l−1, while this value was ±10% at 5 mg l−1. The detection and quantification limits were determined as 2.5 and 7.7 mg l−1, respectively. Relative expanded uncertainty was found to equal 12.5% with a coverage factor k = 2 at the quantification limit. Finally, a paired t-test and linear regression combining the pXRF results and reference values obtained by ICP-MS and ICP-AES demonstrated no significant difference at the 95% confidence level. This work eventually led to the laboratory’s ISO/IEC 17025:2017 accreditation for this method.

中文翻译:

使用符合 ISO/IEC 17025 要求的便携式 XRF 分析仪对来自矿物加工研究的水性样品进行原位铀浓度测量的质量保证

本文开发的方法旨在通过使用便携式 X 射线荧光 (pXRF) 分析法在没有化学制备的情况下即时测定水性样品中的铀,从而控制约旦原子能委员会的铀浸出和处理测量的质量。通过 pXRF 分析酸性和碱性样品,然后与 ICP-MS/ICP-AES 的结果进行比较。根据 ISO/IEC 17025:2017 要求,将 pXRF 方法验证应用于来自单一铀和其他两种认证参考材料的真实样品和模拟铀矿石溶液。从 pXRF 结果与参考值之间的相关性中获得的斜率分别为 1.026、1.021 和 0.9664,相关系数 ( r 2) 接近 1.0。精密度计算显示,对于铀含量 > 10 mg l -1 的样品,值 < 5% RSD ,而该值在 5 mg l -1 时为 ±10% 。检测限和定量限分别确定为 2.5 和 7.7 mg l -1。发现相对扩展不确定度等于 12.5%,覆盖因子k  = 2 在定量限。最后,结合 pXRF 结果和 ICP-MS 和 ICP-AES 获得的参考值的配对t检验和线性回归表明,在 95% 的置信水平上没有显着差异。这项工作最终导致实验室对该方法的 ISO/IEC 17025:2017 认证。
更新日期:2021-05-04
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