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研究了地质样品(含微量铀岩石)在分解和分离过程中保持铀原始价态稳定不变的最佳条件。建立了在高浓度保护剂存在下,用浓HF(40±5)℃分解样品,使样品中铀(Ⅵ)全部溶出,并立即生成稳定的UO_2F_2络合物;铀(Ⅳ)在载体载带下迅速定量沉淀。用抽滤法快速分离。从HF溶样到沉淀分离全过程在2min内完成。分离后的铀(Ⅳ)和铀(Ⅵ)视含量多少分别选用激光荧光法或容量法测定。方法检出限为0.7μg/g,RSD为10.5％,铀测定范围2×10~(-6)～10~(-1)g/g。测定了100多个地质样品(砂岩、花岗岩)中铀含量及其价态比,其结果的准确性和精密度均满足铀矿地质科研的需要。
The optimal conditions for keeping the original uranium valence unchanged during the decomposition and separation of geological samples (including trace uranium rocks) were studied. In the presence of a high concentration of protective agent, the sample was decomposed with concentrated HF (40 ± 5) ℃ to dissolve all the uranium (Ⅵ) in the sample and produce a stable UO_2F_2 complex. Uranium (Ⅳ) Rapid quantitative precipitation. Fast filtration with suction filtration. The whole process of sample digestion from HF to sedimentation is completed within 2 min. After separation of uranium (Ⅳ) and uranium (Ⅵ) depending on the amount of content were selected by laser fluorescence or volumetric method. The detection limit of the method was 0.7μg / g, the RSD was 10.5% and the determination range of uranium was 2 × 10 -6 ~ 10 -1 g / g. The uranium content and valence ratio in more than 100 geological samples (sandstone and granite) were determined. The accuracy and precision of the results meet the needs of uranium geological research.