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研究了硫镍试金法应用于失效汽车催化剂中铂、钯、铑富集的方法,探讨了小型硫镍试金应用于前处理失效汽车催化剂类样品的试金配方,结合正交试验法和控制变量法考察了熔炼温度、熔炼时间、硅酸度、捕集剂镍粉量、硫镍质量比例、助熔剂用量和助熔剂配比对样品前处理效果的影响。最佳试金配方为:熔炼温度为1 050℃;熔炼时间为30 min;硅酸度K=3.5;0.88g镍;m(Ni)∶m(S)=0.9∶1;4g助熔剂(m(Na2CO3)∶m(Na2B4O7)=1∶2)。以硫镍试金-碲共沉淀-电感耦合等离子体原子发射光谱法(ICP-AES)测定失效汽车催化剂中的铂、钯、铑,方法中铂、钯、铑的检出限分别为0.008 9、0.005 1、0.002 4μg/mL。按照实验方法对样品RM-1、RM-2、RM-3(企业内部质控样)和标准样品GYBW-CHJ-1中铂、钯、铑进行测定,结果的相对标准偏差(n=6)在0.14%~2.7%之间,测定值均与参考值/认定值相吻合。
The method of sulfur and nickel gold assay was applied to the enrichment of platinum, palladium and rhodium in deactivated car catalysts. The application of small sulfur and nickel gold assay to pretreatment of failed car catalyst samples was discussed. The orthogonal test method and The influence of melting temperature, smelting time, silicic acid, the amount of nickel powder collector, the mass ratio of sulfur and nickel, flux dosage and flux ratio on the sample pretreatment effect were investigated by the control variable method. The best test gold formula is: melting temperature is 1 050 ℃; melting time is 30 min; silicic acid degree K = 3.5; 0.88g nickel; m (Ni): m Na2CO3): m (Na2B4O7) = 1: 2). The detection limits of platinum, palladium and rhodium in platinum, palladium and rhodium were determined by sulfur-nickel test-tellurium coprecipitation-inductively coupled plasma atomic emission spectrometry (ICP-AES), respectively. The detection limits were 0.008 9 , 0.005 1,0.002 4 μg / mL. The relative standard deviations (n = 6) of the results were determined experimentally for platinum, palladium and rhodium in samples RM-1, RM-2, RM-3 (internal quality control sample) and standard sample GYBW-CHJ- Between 0.14% and 2.7%, the measured values are consistent with the reference value / certified value.