电感耦合等离子体发射光谱(ICP-OES)法测定废钴钼催化剂中关键助剂元素钛  

Determination of Titanium as Key Promoter in Waste Cobalt-Molybdenum Catalyst by ICP-OES

作　　者：石雪峰 王志坚 刘荣丽 张曼宁 陈燕群 SHI Xuefeng;WANG Zhijian;LIU Rongli;ZHANG Manning;CHEN Yanqun(Hunan Rare Earth Metal Materials Research Institute Co.,Ltd.,Changsha,Hunan 410126,China)

机构地区：[1]湖南稀土金属材料研究院有限责任公司,长沙410126

出　　处：《中国无机分析化学》2022年第4期115-120,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：湖南省稀土功能材料重点实验室资助项目(2017TP1031)。

摘　　要：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电感耦合等离子体发射光谱(ICP-OES)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,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-高氯酸法溶解样品时,测定结果更为理想,这是由于在灼烧的过程中相当部分金属元素钴与Al_(2)O_(3)反应生成钴青(CoO·n Al_(2)O_(3))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99.0%~101%。对同一样品与采用分光光度法和EDTA滴定法测定结果进行对照实验,结果吻合,方法简便易操作且适合大批量的检测分析工作。The traditional method of experiment for treating catalyst by cauterization and reacidification was changed,the mix acid method of nitric acid-hydrofluoric acid-perchloric acid 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 method provide a certain analytical basis for follow-up process research of cobalt-molybdenum catalyst and has 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 Al_(2)O_(3) to form cobalt blue(CoO·n Al_(2)O_(3)),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 99.0%—101%.The results are agreement with spectrophotometer method and EDTA titrimetric method for same sample,but the established nitric acid-hydrofluoric acid-perchloric acid method is simple,convenient and suitable for large quantities of detection and analysis work.

关 键 词：ICP-OES Co-Mo基催化剂 助催剂 钛 硝酸-氢氟酸-高氯酸法 

分 类 号：O657.31[理学—分析化学] TH744.11[理学—化学]