碘量法测定碲化铜中铜的方法改进  

The improvement of determination method of copper in Copper Telluride

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作  者:刘芳美 LIU Fang-mei(Zijin Copper Co.,Ltd,Shanghang 364204 China;FuJian Key Laboratory for Green Production of Copper and Comprehensive Utilization of Associated Resources,Shanghang 364204 China)

机构地区:[1]紫金铜业有限公司,福建上杭364204 [2]福建省铜绿色生产及伴生资源综合利用重点实验室,福建上杭364204

出  处:《世界有色金属》2023年第20期119-121,共3页World Nonferrous Metals

摘  要:使用行业标准方法YS/T 1329.2—2019碘量法测定碲化铜中铜时,采用氢溴酸除去试样中硒、砷等干扰元素,溶样过程操作繁琐,耗时长,易发生溅跳而造成无效结果,且检测效率低,因此不适用于冶炼企业大批量样品同时快速分析检测。实验称取2.0g试样,使用盐酸、硝酸溶解,溴除去试样中硒、砷等杂质元素后定容至100mL容量瓶,分取10.00mL试液加纯水至约30mL后加热溶解盐类后测定试样中铜含量,从而对YS/T 1329.2—2019碘量法测定碲化铜中铜的方法进行了改进。按照实验方法测定碲化铜试样中铜,测定结果的相对标准偏差(RSD,n=7)在0.13%~0.21%之间,加标回收率在98.20%~101.8%之间,精密度和准确度分别满足《化学分析方法验证确认和内部资料控制要求(GB/T32465-2015)和合格评定化学分析方法确认和验证指南》(GB/T27417-2017)要求。各试样测定结果与行业标准方法YS/T 1329.2—2019结果一致,且两种方法间不存在显著性差异,可用于冶炼企业大批量快速分析检测碲化铜中铜量。The hydrobromic acid is used to remove selenium,arsenicand other interfering elements in the sample when in the detection copper in copper telluride by the industry standard method YS/T 1329.2-2019.The sample dissolution process is tedious,time-consuming,and easy to splash,which will cause invalid results and reduce the detection efficiency.So,it is not suitable for rapid analysis and detection of a large number of samples in smelting enterprises at the same time.In the experiment,the 2.0g sample was dissolved with hydrochloric acid and nitric acid.And the selenium,arsenic and other impurities in the sample were removed by bromine.Then the volume was fixed to a 100mL volumetric flask.The 10.00mL test solution was used to determine the content of copper in the sample.Thus,the proposed method could improve the YS/T 1329.2-2019 method for the determination of copper in copper telluride.The content of copper in copper telluride sample was determined according to the experimental method.The relative standard deviation(RSD,n=7)of the determination results were between 0.13%and 0.21%.And the recovery were in the range of 98.20%to 101.8%.The precision and accuracy of the proposed method meet《Requirements for verification&validation of detection methods and internal quality control on chemical analysis》(GB/T32465-2015)and《Comformity assessment-Guidance on validation and verification of chemical analytical methods》(GB/T27417-2017),respectively.The found results of each sample were consistent with those obtained by industrial standard method YS/T 1329.2-2019.There was no significant difference between the two methods.It could be used for rapid analysis and determination of copper in copper telluride in large quantities in smelting enterprises.

关 键 词:碲化铜 碘量法  改进 

分 类 号:TF811[冶金工程—有色金属冶金]

 

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