摘要
在聚四氟乙烯内衬压力消解罐中,180℃的温度下,采用王水消解烘干的废钯炭催化剂样品,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定废钯炭催化剂中钯的方法.考察溶样方法、消解时间、消解温度和干扰离子对测定的影响.结果表明:废钯炭催化剂先做烘干处理,在180℃温度下消解6h,效果最佳;废钯炭催化剂中存在的Si、Al、Fe、Mg、Ca等元素对钯的测定无影响;钯浓度在0~250 mg/L范围内与强度呈线性关系,加标回收率为99.6%~100.5%,相对标准偏差小于1%.用实验方法与原子吸收光谱法测定同一个废钯炭催化剂样品,两者测定结果基本相符,方法适合废钯炭催化剂中钯的测定.
The dried waste palladium-carbon catalyst sample was digested with aqua regia in a pressure tank with polytetrafluoroethylene liner at 180℃. Then, the determination method of palladium in waste palladium-carbon catalyst by inductively coupled plasma atomic emission spectrometry (ICP- AES) was established. The effect of sample dissolution method, digestion time, digestion temperature and interference ions on the determination was investigated. The results showed that, the optimal effect could be achieved when the waste palladiumcarbon catalyst was firstly treated by drying followed by digestion at 180 ℃ for 6 h. The elements such as Si, A1, Fe, Mg and Ca in waste palladium- carbon catalyst had no influence on the determination of palladium. The intensity of palladium was linear to its concentration in range of 0-250 mg/L. The recoveries of standard addition were between 99.6% and 100.5%. The relative standard deviation (RSD) was less than 1%. One waste palladium- carbon catalyst sample was determined by this method and atomic absorption spectrometry, and the results were consistent. The proposed method was applicable for the determination of palladium in waste palladium-carbon catalyst.
出处
《冶金分析》
CAS
CSCD
北大核心
2014年第11期32-36,共5页
Metallurgical Analysis