亚钛还原钒酸铵微量滴定法测定矿石中微量铀方法的改进

徐卫东; 孙 荣; 朱霞萍; 刘平辉

亚钛还原钒酸铵微量滴定法测定矿石中微量铀方法的改进

1.
东华理工大学放射性地质与勘探技术国防重点学科实验室, 江西抚州 344000
2.
东华理工大学放射性地质与勘探技术国防重点学科实验室, 江西抚州 344000
3.
东华理工大学放射性地质与勘探技术国防重点学科实验室, 江西抚州 344000
4.
东华理工大学放射性地质与勘探技术国防重点学科实验室, 江西抚州 344000

基金项目:

基金资助: 江西省教育厅重点科技项目资助——相山铀矿开采区稻谷中天然放射性核素铀、钍含量研究(GJJ09023)

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出版历程
- 收稿日期: 2009-12-06
- 修回日期: 2010-02-03

Determination of Micro-amount of Uranium in Ore by Microtitration with Reduction of Ammonium Vanadate by Titanous Chloride

1.
Key Laboratory of Radioactive Geology and Exploration Technology Fundamental Science for National Defense, East China Institute of Technology, Fuzhou 344000, China
2.
Key Laboratory of Radioactive Geology and Exploration Technology Fundamental Science for National Defense, East China Institute of Technology, Fuzhou 344000, China
3.
Key Laboratory of Radioactive Geology and Exploration Technology Fundamental Science for National Defense, East China Institute of Technology, Fuzhou 344000, China
4.
Key Laboratory of Radioactive Geology and Exploration Technology Fundamental Science for National Defense, East China Institute of Technology, Fuzhou 344000, China

摘要

摘要: 根据亚钛还原钒酸铵滴定法的测定原理,对样品溶样、过滤洗涤、还原氧化、滴定等操作方法做了改进。磷酸-盐酸-过氧化氢混合酸低温溶解样品,离心分离过滤,亚钛还原UO²⁺₂,过量亚钛用次溴酸钠氧化,尿素亚硝酸钠混合液进一步氧化未被次溴酸钠氧化的微量低价杂质。在小体积(10 mL)范围内,用低浓度钒酸铵标准溶液进行滴定操作测定微量铀,滴定终点清晰,相对标准偏差(RSD,n＝5)为0.05%~0.07%,方法测定下限为0.001%,适于矿石和矿渣中0.001%~0.01%铀的测定。方法简便、快速,能满足生产和科研的需要。
- 亚钛 /
- 钒酸铵 /
- 滴定法 /
- 微量铀 /
- 矿石
Abstract: Based on the titrimetry with reduction of ammonium vanadate by titanous chloride for the determination of micro-amount of uranium, some operation procedures in sample digestion, filtration and washing, reduction-oxidation and titration were improved. Samples were digested with H₃PO₄-HCl-H₂O₂ at low temperature. After centrifugation, filtering, reduction of UO²⁺₂ with Ti³⁺, oxidization of excessive Ti³⁺ by NaBrO₃ and further oxidization of trace impurities with low valence by urea-NaNO₃, uranium in the sample solution in a small volume (10 mL) was titrated with ammonium vanadate. The end point of the titration was very clear. Detection limit of the method for uranium was 0.001% and precision was 0.05%~ 0.07%RSD. The method provides the advantages of simple operation, high efficiency and is suitable for the determination of 0.001%~0.01% uranium in ore and slag samples.
- titanous /
- chloride /
- ammonium /
- vanadate /
- titrimetry