电感耦合等离子体原子发射光谱法测定催化裂化烟气硫转移剂中铈含量

DETERMINATION OF CERIUM IN SULFUR TRANSFER ADDITIVE FOR FCC FLUE GAS BY ICP-AES

选择盐酸作为消解液并利用微波消解法处理催化裂化烟气硫转移剂样品,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定催化裂化硫转移剂中铈(Ce)含量的方法。考察了消解液种类、配比以及消解温度对消解效果的影响,优化了微波消解程序,具体分析了ICP-AES分析过程中的元素间干扰,确定了方法的精密度和准确性。结果表明:采用12 mL质量分数为36%~38%的盐酸可使0.05 g硫转移剂样品完全消解,ICP-AES分析样品溶液中铈含量的方法检出限为0.01 mg/L,标准曲线线性范围为0.01~10 mg/L,线性相关系数为0.99995,测定结果相对标准偏差(测定6次)小于4%,方法加标回收率在93.1%~101.0%之间。

The sulfur transfer additive for FCC flue gas was treated by microwave-assisted digestion using hydrochloric acid and the content of cerium in the additive was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The kinds and compositions of digestion solution and the digestion temperature were investigated to optimize the microwave-assisted digestion procedure.The interelement interference in ICP-AES analysis was analyzed to determine the precision and accuracy of the method.The results showed that 0.05 g sulfur transfer additive was completely digested by 12 mL hydrochloric acid with a mass concentration of 36%—38%under the optimal digestion conditions.After sample digested,the content of cerium was determined by ICP-AES.The detection limit of ICP-AES method for analyzing the content of cerium in sample solution was 0.01 mg/L,the linear range of standard curve was 0.01 mg/L with a linear correlation coefficient of 0.99995;the relative standard deviation(6 times)was less than 4%,and the method recovery was between 93.1%and 101.0%.