Analytical Method Validation of Thorium in Ore Sample Using UV-Vis Spectrophotometer

Suci Indryati, Amalia Ekaputri Hidayat, Afiq Azfar Pratama, Roza Indra Laksmana, K. Widana, Muhammad Alif Ramlan, Tri Purwanti, R. Prassanti, M. Anggraini, Rommy Rommy
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Abstract

Monazite contains several rare earth elements (REE) along with radioactive elements, i.e., thorium (Th) and uranium (U). Thorium content in monazite is several times higher than uranium. Monazite contains around 12% thorium oxide, but the thorium content in this mineral varies depending on location. To determine the thorium content in monazite, an appropriate and validated analytical method is needed so that the reliability of the test results can be trusted. Apart from that, method validation is one of the clauses in SNI ISO/IEC 17025:2017 that must be fulfilled by the laboratory to be certified and produce reliable data. This research aims to validate analytical methods for non-standard and modified methods that are likely to be used outside the scope. In this research, the method used to digest and analyze thorium in mineral samples refers to the ASTM E2941-14 method with several modifications. Therefore, the analysis method needs to be validated. Validation of the analytical method is carried out by testing several parameters such as linearity and working range tests, accuracy, precision (repeatability), Limit of Detection (LOD), and Limit of Quantitation (LOQ). The results of linearity, accuracy, and repeatability tests that meet the acceptance requirements can be used as a method of validation evaluation. The results of the method validation parameter test met the acceptance requirements, with the linearity test showing a coefficient of determination (R2) of 0.997, the accuracy test showing % a recovery value of 106.22%, and the precision (repeatability) test showing %RSD of 3.76% with LOD value is 0.650 mg/L, and LOQ is 0.724 mg/L. Based on the results of these parameter tests, the method for analyzing thorium in mineral samples was validated.
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使用紫外可见分光光度计验证矿石样品中钍的分析方法
独居石含有几种稀土元素(REE)以及放射性元素,即钍(Th)和铀(U)。独居石中的钍含量是铀的数倍。独居石含有约 12% 的氧化钍,但这种矿物中的钍含量因地点而异。要确定独居石中的钍含量,必须采用适当且经过验证的分析方法,这样才能确保检测结果的可靠性。此外,方法验证是 SNI ISO/IEC 17025:2017 的条款之一,实验室必须满足该条款才能获得认证并生成可靠的数据。本研究旨在验证可能在范围外使用的非标准和修改过的分析方法。在本研究中,用于消化和分析矿物样品中钍的方法参照了 ASTM E2941-14 方法,并进行了若干修改。因此,需要对分析方法进行验证。分析方法的验证是通过测试几个参数来进行的,如线性和工作范围测试、准确度、精确度(重复性)、检测限(LOD)和定量限(LOQ)。符合验收要求的线性、准确度和重复性测试结果可用作验证评估方法。方法验证参数测试的结果符合验收要求,线性测试的确定系数(R2)为 0.997,准确度测试的回收率为 106.22%,精密度(重复性)测试的 RSD 为 3.76%,LOD 值为 0.650 mg/L,LOQ 为 0.724 mg/L。根据这些参数测试的结果,对矿物样品中钍的分析方法进行了验证。
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