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All Journal Eksplorium : Buletin Pusat Pengembangan Bahan Galian Nuklir Eksplorium : Buletin Pusat Pengembangan Bahan Galian Nuklir
Indryati, Suci
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Chemical Engineering, Chemistry & Bioengineering Earth & Planetary Sciences Energy Engineering Materials Science & Nanotechnology Social Sciences

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Analytical Method Validation of Thorium in Ore Sample Using UV-Vis Spectrophotometer Indryati, Suci; Hidayat, Amalia Ekaputri; Pratama, Afiq Azfar; Laksmana, Roza Indra; Widana, Kurnia Setiawan; Ramlan, Muhammad Alif; Purwanti, Tri; Prassanti, Riesna; Anggraini, Mutia; Rommy, Rommy
EKSPLORIUM Vol 44, No 2 (2023): November 2023
Publisher : Badan Riset dan Inovasi Nasional

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.55981/eksplorium.2023.6965

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.
Validation of The Gravimetry Method for Determining Rare Earth Elements Oxides Pratama, Afiq Azfar; Hidayat, Amalia Ekaputri; Rommy, Rommy; Indryati, Suci; Laksmana, Roza Indra; Trinopiawan, Kurnia; Purwanti, Tri; Widana, Kurnia Setiawan; Putra, Aditya Widian; Anggraini, Mutia; Nasrullah, Dzaki Hasan
EKSPLORIUM Vol 45, No 1 (2024): May 2024
Publisher : Badan Riset dan Inovasi Nasional

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.55981/eksplorium.2024.6972

Abstract

The demand for minerals to meet technological developments is increasing, including minerals that contain rare earth elements (REE). The levels of REE in solids can be determined using conventional analysis methods (gravimetry) and instruments. Even though the instrument method provides more accurate results with a small amount of analyte, the cost is higher compared to the gravimetric method, which requires more analyte and provides good results. Therefore, the gravimetric method is a solution for areas with limited instruments and budgets. The study aims to validate the gravimetric method for determining REE oxides levels, evaluate its precision and accuracy, and assess its feasibility of use. In this study, two methods were used for REE analysis: the ASTM E2941-14 method with sample weight modification and the addition of acid to increase REE oxides recovery and a precipitation method using oxalic acid. The validation stages include sample dissolution, precipitation, filtration, and ash-making. The research results show that the RSD value is 0.3154, which is smaller than 2/3 of Horwitz's CV, namely 4.1727, which means it meets the precision acceptance requirements of ISO/IEC 17025:2017. The REE oxides recovery value, which indicates accuracy, also increased to 97.74%. Therefore, the gravimetric method can be used as an alternative for determining REE oxides levels.
Validation of The Gravimetry Method for Determining Rare Earth Elements Oxides Pratama, Afiq Azfar; Hidayat, Amalia Ekaputri; Rommy; Indryati, Suci; Laksmana, Roza Indra; Trinopiawan, Kurnia; Purwanti, Tri; Widana, Kurnia Setiawan; Putra, Aditya Widian; Anggraini, Mutia; Nasrullah, Dzaki Hasan
EKSPLORIUM Vol. 45 No. 1 (2024): MAY 2024
Publisher : BRIN Publishing

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.55981/eksplorium.2024.6972

Abstract

The demand for minerals to meet technological developments is increasing, including minerals that contain rare earth elements (REE). The levels of REE in solids can be determined using conventional analysis methods (gravimetry) and instruments. Even though the instrument method provides more accurate results with a small amount of analyte, the cost is higher compared to the gravimetric method, which requires more analyte and provides good results. Therefore, the gravimetric method is a solution for areas with limited instruments and budgets. The study aims to validate the gravimetric method for determining REE oxides levels, evaluate its precision and accuracy, and assess its feasibility of use. In this study, two methods were used for REE analysis: the ASTM E2941-14 method with sample weight modification and the addition of acid to increase REE oxides recovery and a precipitation method using oxalic acid. The validation stages include sample dissolution, precipitation, filtration, and ash-making. The research results show that the RSD value is 0.3154, which is smaller than 2/3 of Horwitz's CV, namely 4.1727, which means it meets the precision acceptance requirements of ISO/IEC 17025:2017. The REE oxides recovery value, which indicates accuracy, also increased to 97.74%. Therefore, the gravimetric method can be used as an alternative for determining REE oxides levels.
Analytical Method Validation of Thorium in Ore Sample Using UV-Vis Spectrophotometer Indryati, Suci; Hidayat, Amalia Ekaputri; Pratama, Afiq Azfar; Laksamana, Roza Indra; Widana, Kurnia Setiawan; Ramlan, Muhammad Alif; Purwanti, Tri; Prassanti, Riesna; Anggraini, Mutia; Rommy, Rommy
EKSPLORIUM Vol. 44 No. 2 (2023): NOVEMBER 2023
Publisher : BRIN Publishing

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.55981/eksplorium.2023.6965

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.
Co-Authors Hidayat, Amalia Ekaputri Kurnia Setiawan Widana Kurnia Trinopiawan Laksamana, Roza Indra Laksmana, Roza Indra Mutia Anggraini Nasrullah, Dzaki Hasan Pratama, Afiq Azfar Purwanti, Tri Putra, Aditya Widian Ramlan, Muhammad Alif Riesna Prassanti Rommy Rommy, Rommy