密闭消解-电感耦合等离子体原子发射光谱法测定铂钯精矿中铜金铂钯硒碲铋铱铑  

Determination of copper,gold,platinum,palladium,selenium,tellurium,bismuth,iridium and rhodium in platinum and palladium concentrate by inductively coupled plasma atomic emission spectrometry with sealed digestion

作　　者：刘芳美 赖秋祥 巫贞祥 衷水平[2] LIU Fangmei;LAI Qiuxiang;WU Zhenxiang;ZHONG Shuiping(FuJian Key Laboratory for Green Production of Copper and Comprehensive Utilization of Associated Resources,Zijin Copper Co.,Ltd.,Shanghang 364204,China;Zijin Mining Co.,Ltd.,Shanghang 364204,China)

机构地区：[1]紫金铜业有限公司,铜绿色生产及伴生资源综合利用福建省重点实验室,福建上杭364204 [2]紫金矿业集团股份有限公司,福建上杭364204

出　　处：《冶金分析》2021年第6期77-82,共6页Metallurgical Analysis

基　　金：国家质量基础的共性技术研究与应用(2019YFF0217100)。

摘　　要：准确测定铂钯精矿中铜、金、铂、钯、硒、碲、铋、铱、铑等元素含量,是从铂钯精矿中回收有价元素的重要理论支撑。一般采用重量法测定其中铂和钯,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定铜、金、硒、碲、铋,而铱、铑等多采用铅试金或锑试金预富集后再采用原子吸收光谱法逐一测定,存在分析速度慢、周期长、操作繁琐、检测成本高等问题,难以满足实际检测要求。为实现上述元素的准确、快速测定,实验通过密闭消解样品,建立了一次溶解样品后直接用ICP-AES测定铂钯精矿中铜、金、铂、钯、硒、碲、铋、铱、铑的方法。实验表明,在50 mL密闭消解罐中加入0.2 g样品,以王水(1+1)溶解,于160℃干燥箱中消解6 h,可将样品完全溶解;再选择合适的分析谱线消除谱线干扰,可实现ICP-AES对铂钯精矿中各元素的测定。在最优的实验条件下,各元素的校准曲线相关系数均大于0.999,方法检出限为0.0001%~0.0016%。实验方法用于测定实际铂钯精矿中铜、金、铂、钯、硒、碲、铋、铱、铑,结果的相对标准偏差(RSD,n=11)为0.33%~4.8%,加标回收率为96%~103%。The accurate determination of copper,gold,platinum,palladium,selenium,tellurium,bismuth,iridium and rhodium in platinum and palladium concentrates was an important theoretical support for the recovery of valuable metals from platinum and palladium concentrates.Platinum and palladium were commonly determined by the gravimetric method.The traditional determination method for copper,gold,selenium,tellurium and bismuth was inductively coupled plasma atomic emission spectrometry(ICP-AES),while the iridium and rhodium were determined one by one by atomic absorption spectrometry(AAS)after pre-enrichment by lead or antimony assay.However,it had many shortcomings such as slow analytical speed,long analytical period,complicated operation and high detection cost,which could not meet the actual detection requirements.In order to realize the accurate and rapid determination of above elements,the sample was digested in a sealed system,and then a direct determination method of copper,gold,platinum,palladium,selenium,tellurium,bismuth,iridium and rhodium in platinum and palladium concentrates was established by ICP-AES after a sample dissolution.The experimental results showed that 0.2 g of samples could be fully dissolved in 50 mL sealed digestion tank with aqua regia(1+1)as solvent,which was heated in drying oven at 160℃for 6 h.Then the spectral interference was eliminated by selecting proper spectral lines.Consequently,the determination of various elements in platinum and palladium concentrate by ICP-AES was realized.Under the optimal experimental conditions,the linear correlation coefficients of calibration curves of test elements were all higher than 0.999.The limits of detection of method were 0.0001%-0.0016%.The proposed method was applied to the determination of copper,gold,platinum,palladium,selenium,tellurium,bismuth,iridium and rhodium in platinum and palladium concentrate samples.The relative standard deviations(RSD,n=11)of the results were between 0.33% and 4.8%.The recoveries were between 96% and 103%.

关 键 词：密闭消解 铂钯精矿 电感耦合等离子体原子发射光谱法(ICP-AES) 铜 金 铂 钯 硒 碲 铋 铱 铑 

分 类 号：O657.31[理学—分析化学]