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采用过氧化钠高温熔解样品,3.0~4.5mol/L盐酸介质中二氯化锡还原、碲共沉淀富集铂、钯,选择Pt 265.945nm、Pd 340.458nm作为分析谱线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定石油化工废催化剂不溶渣中铂、钯的方法。样品中铂的质量浓度在2~27μg/mL、钯的质量浓度在0.7~20μg/mL范围内,校准曲线线性方程分别为I_(Pt)=3 624×ρ_(Pt)-180.4和I_(Pd)=9 869×ρPd-220.9,线性相关系数R2均为0.999 98。方法中铂、钯的检出限分别为0.017μg/mL和0.004 2μg/mL。测定石油化工废催化剂不溶渣样品中109~1 342g/t铂和37~977g/t钯,结果的相对标准偏差(RSD,n=5~11)分别为1.1%~1.9%和1.1%~3.6%,测定结果与火试金富集-电感耦合等离子体原子发射光谱法的测定结果一致,铂、钯的回收率分别为99%~100%和100%。
The sample was dissolved with high temperature sodium peroxide, and the tin dichloride was reduced with 3.0 ~ 4.5mol / L hydrochloric acid. The platinum and palladium were enriched with tellurium coprecipitation. The analytical spectra of Pt265.945nm and Pd340.458nm were selected as the analytical line, and the inductively coupled plasma Determination of platinum and palladium in insoluble residue of petrochemical waste catalyst by ICP-AES. The concentration of platinum in the sample ranged from 2μg / mL to 27μg / mL and the concentration of palladium in the range of 0.7μg / mL to 20μg / mL. The linear calibration equations were Pt = 3 624 × Pt - 180.4 and Pd ) = 9 869 × ρPd-220.9, the linear correlation coefficient R2 is 0.999 98. The detection limits of platinum and palladium in the method were 0.017μg / mL and 0.0042μg / mL, respectively. The relative standard deviations (RSD, n = 5-11) of 109 ~ 1 342g / t platinum and 37 ~ 977g / t palladium in the petrochemical waste catalyst-free slag samples were 1.1% ~ 1.9% and 1.1% ~ 3.6% %. The results are in good agreement with the results of FAAS-ICP-AES. The recoveries of platinum and palladium are 99% -100% and 100%, respectively.