ICP-OES法分析钴钼催化剂中助剂锌含量的研究

Study on the determination of promoter zinc cotent in cobalt-molybdenum catalyst by ICP-OES

采用硝酸-氢氟酸-高氯酸将石化工业中常用的难溶废钴钼催化剂快速溶解并利用ICPOES分析法准确测定试样中关键助剂元素锌,考察了不同溶样方法、溶样酸的类别、仪器分析参数对精密度和加标回收率的影响。试验结果表明:相对于灼烧再酸化的溶样方法,直接采用硝酸-氢氟酸-高氯酸溶解试样效果更优,锌的相对标准偏差为2.02%,加标回收率为98%~102%。该分析方法简便易操作,适合大批量的检测分析工作,为石化工业水煤气变换反应中钴钼催化剂的后续工艺研究提供了参考,同时对金属锌的回收循环利用具有重要作用。

Nitric acid-hydrofluoric acid-perchloric acid is used to rapidly dissolve the cobalt-molybdenum catalyst commonly used in petrochemical industry and ICP-OES is used to accurately determine the key promoter element zinc in the sample.The effects of different sample dissolving methods,the types of sample dissolving acids and instrumental analysis parameters on the precision and standard addition recovery are investigated.The results show that compared with the method of cauterization and acidification,the effect of directly dissolving the sample with nitric acid-hydrofluoric acid-perchloric acid is better,the relative standard deviation of zinc is 2.02%,and the recovery rate is 98%-102%.The analytical method is simple and easy to operate,and suitable for large-scale detection and analysis.It provides a reference for the subsequent process research of cobalt-molybdenum catalyst in water gas shift reaction of petrochemical industry,and plays an important role in the recovery and recycling of metal zinc.