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| 碱熔蒸馏分离-催化分光光度法测定超痕量锇、钌 |
| Determination of Ultra Trace Osmium and Ruthenium by Alkaline Fusion Distillation Separation-Catalytic Spectrophotometric Method |
| 投稿时间：2013-07-15 |
| DOI： |
| 中文关键词: 分析化学 蒸馏分离 催化分光光度法 超痕量 锇 钌 |
| 英文关键词: analytical chemistry distillation separation catalytic spectrophotometric method ultra trace osmium ruthenium |
| 基金项目:国土资源部公益性行业科研专项经费项目(201211081-03-34)。 |
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| 中文摘要: |
| 研制了新型的锇、钌混合氧化剂K2Cr2O7-NaBrO3和锇稀释剂As2O3-H2SO4，能够降低碱熔蒸馏分离-催化分光光度法测定锇、钌的全流程空白，提高了锇、钌催化As3+-Ce4+体系的灵敏度。在35℃时，通过延长反应时间，提高了方法的稳定性和降低方法的检测下线。使Os、Ru检出限(3σ)分别达到0.010 ng/g和0.012 ng/g。改进后的蒸馏装置使锇、钌蒸馏的安全性和工作效率极大提高。方法操作简便、效率高、成本低。测定国家铂族元素地球化学一级标准物质中的Os、Ru，相对误差(RE)为-18.0%~+4.40%，12次测定的相对标准偏差(RSD)均小于20.1%，满足地球化学调查样品分析质量要求。 |
| 英文摘要: |
| By developing a new type mixed oxidant of Os and Ru, K2Cr2O7-NaBrO3 anddiluentAs2O3-H2SO4 of Os, the full procedure blank in the determination of Ru and Os by alkali fusion distillation separation-catalytic spectro-photometric method was reduced, and the sensitivities of Os, Ru in As3+-Ce4+catalytic system were improved. The stability of the method was improved and the detection limit was reduced by prolonging the reaction time at 35℃. Detected limits (3σ) of Os and Ru were 0.010 ng/g and 0.012 ng/g, respectively. The results showed that the safety and efficiency of distillation were greatly improved by improve the distillation device. The method is simple operation, high efficiency and low cost. The method was applied to measure Os and Ru in National PGE geochemistry standard substance. The relative error (RE) was -18.0% ~ +4.40%, and the relative standard deviation (RSD) of 12-times results was less than 20.1%. The method could meet the analysis quality requirements of geochemical survey sample. |
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