摘要
冰铜的成分比较复杂,若酸溶后直接利用电感耦合等离子体原子发射光谱法测定贵金属的含量,杂质元素含量过高,干扰较为严重,导致结果偏差较大。为了准确地测定冰铜样品中的金、银、钯的含量,首先用铅试金法在高温熔融状态下去除冰铜样品中的大部分杂质元素,将贵金属富集到铅扣中,然后将铅扣灰吹除铅后得到贵金属合粒,利用二次试金补正实验,用醋酸洗涤两次试金得到的合粒后称量质量,合粒经硝酸溶解后将金元素与其他元素分离,称量金粒质量,分金液中加入适量的盐酸溶液继续加热处理,然后采用电感耦合等离子体原子发射光谱(ICP-AES)法在选定的最佳仪器工作条件下测定分金液中的金、铅、铋、铜、钯的浓度,通过给定的公式计算得出冰铜样品中金、银、钯的含量。通过考察氧化铅用量、灰吹温度以及基体干扰对测定结果的影响,结果表明,当氧化铅加入量为200 g,灰吹温度为890℃时,实验效果最好,干扰实验表明,样品中银的含量高低均不会对Au、Pb、Bi、Cu和Pd的测定产生影响;银加标回收率在97.7%~100%,金的加标回收率在98.6%~102%,钯的加标回收率在98.0%~102%。方法操作简单,在测定冰铜样品中金、银、钯含量时均有很好的准确度和精密度,相对标准偏差(RSD)值均在1.1%~3.3%,可以满足实际检测的需求。
The composition of matte is relatively complex,if the content of noble metals is directly determined by inductively coupled plasma atomic emission spectrometry after acid dissolution,the content of impurity elements is too high,the interference is serious,leading to the large deviation of results.In this experiment,the lead assay method was first used to remove most of the impurity elements in the matte sample in a high-temperature molten state to enrich the precious metal into the lead buckle,and then the lead was removed from the lead buckle to obtain the precious metal particles after ash blowing.The results were corrected using second assay,the combined particles were dissolved in nitric acid to separate gold from other elements,and the mass of the gold particles was weighed,added an appropriate amount of hydrochloric acid solution to the gold separation solution and continued heating treatment,and then the concentrations of gold,lead,bismuth,copper,and palladium in the gold separation solution were measured by inductively coupled plasma atomic emission spectrometer under selected optimal instrument operating conditions.The contents of gold,silver,and palladium in the matte sample were calculated using the given formula.The effects of lead oxide dosage,ash blowing temperature and matrix interference on the determination results were discussed.When the amount of lead oxide added was 200 g and the ash blowing temperature was 890℃,the test results were the best.The interference test showed that the high or low content of silver in the sample would not affect the determination of Au,Pb,Bi,Cu,and Pd.The test results showed that the recovery of silver was 97.7%—100%,the recovery of gold was 98.6%—102%,and the recovery of palladium was 98.0%—102%.this method was easy to operate,and had good accuracy and precision the RSD values were between 1.1%and 3.3%,and could meet the needs of actual detection.
作者
刘秋波
李华昌
姜求韬
LIU Qiubo;LI Huachang;JIANG Qiutao(BGRIMM MTC Technology Co.,Ltd.,Beijing 102628,China)
出处
《中国无机分析化学》
CAS
北大核心
2023年第8期894-898,共5页
Chinese Journal of Inorganic Analytical Chemistry
基金
国家重点研发计划项目(2021YFC2903101)。
