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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

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

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.

Pengendapan Uranium pada Monasit Bangka sebagai Ammonium Diuranate (ADU) Menggunakan Gas NH3 Prassanti, Riesna; Fauzan, Ahmad Miftah; Putra, Aditya Widian; Pratama, Afiq Azfar; Dewita, Erlan; Hidayat, Rachmat Fauzi; Ani, Budi Yuli; Permana, Yoga
EKSPLORIUM Vol. 41 No. 1 (2020): MEI 2020
Publisher : BRIN Publishing

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.17146/eksplorium.2020.41.1.5879

Monazite, as a by-product of tin mining, contains rare earth elements (REE) and radioactive elements like uranium (U) and thorium (Th). The monazite processing Research and Development at the Center for Nuclear Mineral Technology-National Nuclear Energy Agency (PTBGN-BATAN) has succeeded in separating REE as a hydroxide compound with an 85% recovery. The radioactive elements U and Th are each obtained as a product in the form of concentrated compounds of ammonium diuranate (ADU)/(NH4)2U2O7 and thorium hydroxide (Th(OH)4). In previous studies, the separation of U as ADU in monazite was carried out by the precipitation process using NH4OH solution. In this research, U will be precipitated as an ADU using NH3 gas reagents to obtain precipitation optimum conditions. Precipitation feed in the form of (U, Th, REE) sulfate solution derived from the monazite processing using the alkali or base method, which includes decomposition using NaOH, partial dissolution using HCl, and total dissolution using H2SO4. The parameters studied include the effect of NH3 gas flow rate, process temperature, and contact time on U recovery. The results showed that on the static pH-7 condition, the optimum state of U precipitation using NH3 gas is at NH3 gas flow rate of 150 ml/minutes, processing temperature of 30oC, and 15 minutes contact time with precipitation recovery of U 100%, Th 99.97%, and REE 99.93%. These results indicate that U has been taken entirely but still mixed with other elements, which are Th and REE, so that further research is needed to obtain U with high purity on optimum pH condition.

Peningkatan Perolehan Uranium, Torium, dan Logam Tanah Jarang dalam Residu Pelarutan Parsial pada Pengolahan Monasit Fatihah, Novita Sari; Anggraini, Mutia; Pratama, Afiq Azfar; Widana, Kurnia Setiawan
EKSPLORIUM Vol. 42 No. 2 (2021): NOVEMBER 2021
Publisher : BRIN Publishing

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.17146/eksplorium.2021.42.2.6044

Monazite is a by-product of tin processing containing phosphate, rare earth elements, and radioactive elements such as uranium and thorium. These elements can be utilized optimally if separated from one another through processing. Monazite processing includes decomposition, partial dissolution, and precipitation processes. The separation of rare earth elements from radioactive elements in monazite is carried out through a partial dissolution process, but the separation is not optimal so that further processes are needed to increase the recovery of these elements. In this study, the process was carried out using two methods, namely total dissolution with hydrochloric acid (HCl) which aims to dissolve all elements in the precipitate and precipitation with ammonium hydroxide (NH4OH) which aims to separate radioactive elements and rare earth elements. Both methods were carried out under optimum process conditions with various variations in pH, temperature, and time. Based on observations, it was found that the optimum solubility of each element was 67.6% uranium, 15.3% thorium and 50.8% LTJ under the dissolving process conditions of pH 1, at 80°C for 2 hours. While in the deposition process, the precipitation recovery of each element is 57% uranium, 75.7% thorium, 4.8% rare earth metals at pH 6 conditions. Based on these data, it can be concluded that uranium, thorium, and rare earth elements can be dissolved at pH 1, at 80°C for 2 hours, and can be separated at pH 6 precipitation conditions.

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

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

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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