电感耦合等离子体发射光谱(ICP-OES)法分析废钴钼催化剂中关键助剂元素钛含量

通过改变传统的灼烧再酸化处理催化剂的实验方法，采用硝酸-氢氟酸-高氯酸法将石化工业中常用的难溶废钴钼催化剂快速溶解并利用ICP-OES分析法准确测定样品中关键助剂元素钛，为钴钼催化剂后续工艺研究提供了一定的分析依据以及对钛金属元素的回收循环利用具有重要意义。实验优化了ICP-OES仪器最佳工作参数，确定了酸试剂体系及钛元素的分析谱线，对比了不同前处理方法的精密度。结果表明：相比于灼烧再酸化，直接采用硝酸-氢氟酸-高氯酸法溶解样品更为理想，这是由于在灼烧的过程中相当部分金属元素钴与Al2O3反应生成钴青（CoO·n Al2O3）使得回收率降低。在仪器最佳测定条件下校准曲线回归方程的线性相关系数为1，钛的相对标准偏差为0.54%，加标回收率在99%-101%之间。对同一样品与采用分光光度法分析和EDTA滴定法分析做对照实验，结果吻合，但本实验方法简便易操作且适合大批量的检测分析工作。

Determination of titanium as key promoter in waste cobalt-molybdenum catalyst by ICP-OES

The traditional method of experiment for treating catalyst by cauterization and reacidification was changed, nitric acid-hydrofluoric acid-perchloric acid method was used to rapidly dissolve the refractory waste cobalt-molybdenum catalyst in petrochemical industry and the key promoter elements Ti in samples were accurately determined by ICP-OES,this provide a certain analytical basis for follow-up process research of cobalt-molybdenum catalyst and has an important significance for the recovery and recycling of titanium.The best working parameters of ICP-OES instrument were optimized by experiment, the system of acid reagent and the analytical spectrum of titanium were determined, the precision of different pretreatment methods was compared. Results show that it is better to dissolve the sample directly by nitric acid-hydrofluoric acid-perchloric acid than cauterization and reacidification, this is due to the reaction of cobalt with Al2O3 to form cobalt blue (CoO·nAl2O3), which reduces the recovery of titanium. The linear correlation coefficient of titanium is 1 under optimum instrumental conditions for the regression equation of calibration curve,the relative standard deviations of titanium is 0.54%, and the recovery of standard addition is between 99% and 101% .The results are agreement with Spectrophotometer method and EDTA titrimetric method for same sample,but nitric acid-hydrofluoric acid-perchloric acid method is simple, convenient and suitable for large quantities of detection and analysis work.