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。
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.
参考文献
| [1] | Date A R;Davis A E;Cheung Y Y .The potential of fire assay and inductively coupled plasma source mass spectrometry for the determination of platinum group elements in geological materials[J].ANALYST,1987,112(09):1217-1222. |
| [2] | Parry S J;Asif M;Sinclair I W .Radiochemical fire-assay for determination of the platinum-group elements[J].Journal of Radioanalytical and Nuclear Chemistry,1988,123(02):593-606. |
| [3] | 孙亚莉,管希云,杜安道.锍试金富集贵金属元素Ⅰ.等离子体质谱法测定地质样品中痕量铂族元素[J].岩矿测试,1997(01):12. |
| [4] | 何红蓼,吕彩芬,周肇茹,史世云,李冰.锍镍试金-等离子体质谱法测定地球化学勘探样品中的铂族元素和金Ⅰ.分析流程的简化[J].岩矿测试,2001(03):191-194. |
| [5] | 吕彩芬,何红蓼,周肇茹,支辛辛,李冰,张勤.锍镍试金-等离子体质谱法测定地球化学勘探样品中的铂族元素和金Ⅱ.分析流程空白的降低[J].岩矿测试,2002(01):7-11. |
| [6] | 李祖碧,曹秋娥,王加林,徐其亨.高碘酸盐氧化亚甲蓝动力学光度法测定痕量锇[J].分析化学,2000(03):361-341. |
| [7] | 张庆合;赵中一;金继红 等.催化褪色光度法测定痕量锇-邻硝基苯基荧光酮-锇-H2O2体系[J].理化检验:化学分册,1994,30(06):335-336. |
| [8] | 唐宁莉,唐建洪.催化光度法测定痕量锇[J].岩矿测试,1996(04):283. |
| [9] | 蒋治良.超痕量钌的催化光度分析-KIO4-罗丹明B新体系[J].化学通报,1992(01):38-40. |
| [10] | 周之荣,张丽珍,王群,章淑媛,张圆玲,苏志文.过氧化氢氧化邻硝基苯基荧光酮褪色反应动力学光度法测定痕量钌[J].冶金分析,2008(12):66-69. |
| [11] | 董守安.现代贵金属分析[M].北京:化学工业出版社,2007 |
| [12] | 郭漾光 .催化比色测定矿石中的锇和钌[J].贵金属,1981,2(02):22-28. |
| [13] | 王琳.炭质页岩及矿化炭质页岩中锇钌的测定[J].黄金,2004(06):50-52. |
| [14] | 王琳,来新泽,吴建政,王烨,孙红林.地球化学勘探样品中超痕量锇、钌分析方法研究[J].贵金属,2004(03):49-53. |
| [15] | GB/T 17418.5-2010.地球化学样品中贵金属分析方法第5部分:钌量和锇量蒸馏分离-催化分光光度法[S].北京:中国标准出版社,2011. |
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