CAJ | 학술논문

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%，满足地球化学调查杨品分析质量要求。
연제료신형적철、조혼합양화제K2Cr2O7-NaBrO3화철희석제As2O3-H2SO4，능구강저감용증류분리-최화분광광도법측정철、조적전류정공백，제고료철、조최화 As3+-Ce4+체계적령민도。재35℃시，통과연장반응시간，제고료방법적은정성화강저방법적검측하선。사Os、Ru검출한(3σ)분별체도0.010 ng/g화0.012 ng/g。개진후적증류장치사철、조증류적안전성화공작효솔겁대제고。방법조작간편、효솔고、성본저。측정국가박족원소지구화학일급표준물질중적 Os、Ru，상대오차(RE)위-18.0%~+4.40%，12차측정적상대표준편차(RSD)균소우20.1%，만족지구화학조사양품분석질량요구。
By developing a new type mixed oxidant of Os and Ru, K2Cr2O7-NaBrO3 and diluent As2O3-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.