铅试金分离富集含银物料中铑的研究

Study on separation and enrichment of rhodium in silver-containing materials by lead fire assay

报道了一个改进的铅试金分离富集-ICP-AES测定含银物料中铑的方法。用钯粉或钯银粉混合物作灰吹保护剂,分别研究了钯与银的质量比、合粒中钯银与铑的质量比对分离富集含银物料中铑的影响。结果表明:当钯量:银量≥2:1时,铑在灰吹过程的损失可忽略;当钯银量:铑量≥40:1时合粒中铑在常压下可以完全溶解;当银量:钯量≥1:10时,合粒可以用HNO3(1+3)快速溶解。研究了钯量对电感耦合等离子体发射光谱法测定铑的影响。方法回收率98.2%～100.5%,对实际样品进行分析,测定值与推荐值一致,相对标准偏差小于4.0%(n=5)。

An improvement was made on the separation and enrichment of rhodium by lead fire assay with ICP- AES method. Using palladium powder or a mixture of palladium silver as protective reagent for cupellation, the effects of various testing factors, such as the mass ratio of palladium to silver and the mass ratio of palladium- silver to rhodium, have been studied in detail when rhodium was enriched. The results indicated that loss of rhodium could be ignored for cupellation process at Rh：Pd 1〉 2：1, rhodium of kernel could be completely dissolved at atmospheric pressure and Pd-Ag：Rh≥40：1, kernel of precious metals could be dissolved with HNO3 （1 ＋3） at Ag： Pd≥ 1：10. The effects of palladium on the determination of rhodium with inductively coupled plasma atomic emission spectrometry had been studied. The recoveries of silver in samples ranged from 98.2% to 100. 5%. Found values were consistent with recommended values, and the relative standard were less than 4. 0 % （ n = 5） in the real samples. derivations （RSDs）