Pd/C催化剂及其冶金废料分解和测定的研究

Research on Dissolution and Determination for Pd/C Catalyst and Its Metallurgy Waste

研究了Pd/C催化剂及其冶金废料分解和测定的问题。预先灼烧试样除去碳等杂质,再用焦硫酸钾熔解,溶解处理后分别以络合滴定法和分光光度法测定Pd。灼烧损失空白Pd/C加标回收率为99.4%-100.5%,证明试样预先灼烧未引起Pd的损失。结果表明：对于Pd含量高达xx%的样品,尽管试样组成复杂也应采用丁二肟沉淀分离滴定法进行测定;对于Pd含量〈5%的样品,无论试样组成简单或复杂均应采用操作简便的光度法。

The problem of decomposing Pd/C catalyst and its metallurgical waste materials, and determining of Pd content in them were discussed. These samples were ignited previously in order to remove carbon and other impurities, and then melted further by using potassium pyrosulfate. After that, the Pd content in them were determined by using complexometric titration and spectrophotometry, respectively. For the blank samples of Pd/C which had been ignited, the recovery of standard addition was between 99.4%-100.5%. It proved that palladium in these samples was not lost by igniting previously. The research results indicated that when these samples of Pd content above xx%, even if the composition of samples were complex, the method for determination of Pd should also select butanedione dioxime precipitation titration. But for samples of Pd content below 5%, regardless of the specimen composed of simple or complex by spectrophotometry and easy operation.