铑-高碘酸钾-固绿FCF体系催化动力学光度法测定痕量铑

doi:10.13228/j.issn.1000-7571.2014.09.013

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摘要在氢氧化钾介质中,于沸水浴加热13 min,痕量铑对高碘酸钾氧化固绿FCF(FG)的褪色反应有催化作用,依此建立了催化动力学光度法测定痕量铑的新方法。探讨了该催化反应的最佳反应条件并测定了动力学参数。结果表明,铑的浓度在1～12 ng/mL范围内与催化反应和非催化反应的吸光度差(ΔA)呈良好的线性关系,相关系数r=0.998 9,方法的检出限为9.52×10^-11 g/mL。测得表观速率常数为6.97×10^-3/s,表观活化能为71.08 kJ/mol。方法用于铑炭和铂铑催化剂中铑的测定,测定值与氯化亚锡光度法基本一致,相对标准偏差(RSD,n= 6)为2.4%～3.6%,加标回收率为99%～102%。

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	宋学省

关键词 ：铑, 高碘酸钾, 氢氧化钾, 催化动力学光度法, 固绿FCF

Abstract：In potassium hydroxide, trace rhodium (Ⅲ) could catalyze fading reaction of periodate potassium oxidizing fast green FCF(FG) in boiling bath for 13 min, based on which a novel method for catalytic kinetic spectrophotometric determination of trace rhodium was established. The optimal conditions of catalytic reaction and the kinetics parameters were discussed. It was found that, the concentration of rhodium showed a good linear relationship with the absorbance difference (ΔA) of the catalytic and non-catalytic reaction within the range of 1-12 ng/mL, and the correlation coefficient (r) was 0.998 9. The detection limit was 9.52×10^-11 g/mL. The apparent rate constant was 6.97×10^-3/s and the apparent activation energy was 71.08 kJ/mol. The method has been applied to determine rhodium in catalysts of rhodium-carbon and platinum-rhodium. The results were basically consistent with those obtained by stannous chloride spectrophotometry. The relative standard deviation (RSD, n=6) was 2.4%-3.6%, and the standard addition recovery was 99%-102%.

Key words： rhodium periodate potassium potassium hydroxide catalytic kinetic spectrophotometry fast green FCF

收稿日期: 2014-03-09

ZTFLH:

O657.32

基金资助:山东省青年奖励基金(2011BSA13013)

作者简介: 宋学省(1969-),男,副教授,学士,主要从事光谱分析研究;E-mail:songxuesheng@lytu.edu.cn

引用本文:

宋学省. 铑-高碘酸钾-固绿FCF体系催化动力学光度法测定痕量铑[J]. 冶金分析, 2014, 34(9): 66-69. SONG Xue-sheng. Catalytic kinetic spectrophotometric determination of trace rhodium with rhodium-potassium periodate-fast green FCF system. , 2014, 34(9): 66-69.

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