采用碱熔-碲共沉淀分离富集,用电感-耦合等离子体发射光谱法(ICP-AES)测定精细化工废催化剂不溶渣中的铂、钯、铑含量.系统考察了碱熔解和碲共沉淀富集分离的条件,研究了碲富集物中的主要元素和比例,确定了 ICP-AES 法测定铂、钯、铑的条件.结果表明,碱熔-共沉淀能够充分分离富集样品中的铂、钯、铑;测定催化剂不溶渣中653~3652 g/t铂、447~3804 g/t钯、539~6433 g/t铑时,相对标准偏差(RSD)、样品加标回收率分别为铂0.84%~1.78%、97.0%~99.4%,钯1.05%~ 1.82%、97.0%~100.6%,铑1.00%~2.12%、98.2%~100.4%.方法分析快速、易于掌握,已用于生产分析中.
With alkali fusion, tellurium co-precipitation separation, contents of Pt, Pd and Rh in insoluble slag of fine-chemical industry spent catalysts were determined by ICP-AES. The conditions of alkali fusion, tellurium co-precipitation separation, components of the enrichment, and ICP-AES determination condition were systemic investigated. Results indicated that Pt, Pd and Rh in the slag can be completely separated and enriched by fusion and co-precipitation. Contents of 653~3652 g/t Pt, 447~3804 g/t Pd, and 539~6433 g/t Rh in the slag were determined. The relative standard deviation (RSD), recoveries of standard addition were 0.84%~1.78%, 97.0%~99.4% for Pt, 1.05%~1.82%, 97.0%~100.6% for Pd, and 1.00%~2.12%, 98.2%~100.4% for Rh, respectively. The proposed method was rapid, easy to master and has beed applied to production analysis.
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