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《化学分析计量》 2020年第01期
DOI:10.3969/j.issn.1008-6145.2020.01.004
硫酸分离-火试金重量法测定碲化铜中的金和银
李先和,万双
(阳谷祥光铜业有限公司,山东聊城 252327) 
Determination of gold and silver in copper telluride by sulfuric acid separation-fire assay gravimetric method
LI Xianhe, WAN Shuang
(Shandong Yanggu Xiangguang Copper Co., Ltd., Liaocheng 252327, China) 
摘要:建立了用硫酸分离-火试金重量法测定碲化铜中的金和银含量的方法。用硫酸溶解碲化铜样品,过滤, 除去铜和碲,得到含金、银的沉淀物,沉淀物经灰化、配料、高温熔融制得铅扣。将铅扣灰吹,得到金银合粒,用硝酸溶 解分离金,用重量法测定金含量。用金银合粒的质量扣除金粒的质量和分金液、洗液中杂质的质量即为银含量。采 用灰皿、残渣熔融法补正,或用含碲、铜物料做基体加入纯金、纯银同试样方法测定,根据金、银的回收率加以补正,从 而得到试样中的碲含量。实验结果表明,浓硫酸的加入量为30 mL,残余量应不少于15 mL。火试金中硅酸度为1 左 右,试样进炉温度以900℃为宜。该方法金、银测定结果的相对标准偏差分别为0.33%~1.97%,0.28%~1.27%(n=9)。 金的回收率为98.5%~100.2%,银的回收率为95.5%~101.4%。该法满足生产控制检测和贸易结算的要求。 
Abstract:A method was established to determine gold and silver in copper telluride by sulfuric acid separation-fire assay gravimetry. Copper telluride sample was dissolved with sulfuric acid, after being filted, copper and tellurium was removed to get the precipitate, which was ashed, mixed, and melted at high temperature to obtain lead button. Ash was removed from the lead button by blowing to obtain gold and silver particles which were divided into gold by nitric acid, and the gold content was determined by gravimetric method. The mass of the gold particles and the amount of impurities in the gold separating liquid and washing liquid were reduced by using the mass of the composite particles to obtain the silver amount. The method of ash pan and residue melting method were adopted to correct the detection results, or tellurium and copper-containing materials were used as the matrix together with pure gold and pure silver, which was determined by the same method as the sample, and the detection result was corrected according to the recovery rate of gold and silver. The experimental results showed that the proper addition amount of concentrated sulfuric acid was 30 mL, and the residual amount should be not less than 15 mL. The silicic acid degree in fire test gold was about 1, and the appropriate temperature for the sample to enter the furnace was 900℃. The relative standard deviation of gold and silver was 0.33%-1.97% and 0.28%-1.27% (n=9), respectively. The recovery rate of gold was 98.5%-100.2%, and that of silver was 95.5%-101.4%. The method fully meets the requirements of production control and trade settlement. 
关键词:硫酸分离;火试金重量法;碲化铜;金;银 
Keywords:sulfuric acid separation; fire assay gold gravimetry; copper telluride; gold; silver 
基金:中华人民共和国有色金属行业标准起草项目(2016–0230T–YS) 
本文引用格式:
李先和,万双. 硫酸分离- 火试金重量法测定碲化铜中的金和银[J]. 化学分析计量,2020,29(1):13-17.
LI X H,WAN S. Determination of gold and silver in copper telluride by sulfuric acid separation-fire assay gravimetric method[J]. Chemical analysis and meterage,2020,29(1):13-17. 

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