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敞口酸溶-电感耦合等离子体发射光谱法测定锑精矿中的砷 被引量:5

Determination of Arsenic in Antimony Concentrate by Open-mouth Acid Dissolution Inductively Coupled Plasma Atomic Emission Spectrometry
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摘要 锑精矿中的砷采用常规王水溶解不能有效的分解矿石中的硅酸盐组分导致分解不彻底,后续提取过程中锑的水解会对砷有一定的包裹造成砷测定结果偏低。本文采用氢氟酸-盐酸-硝酸-高氯酸混合体系敞口酸溶后加入酒石酸与锑络合抑制锑的水解消除锑沉淀对砷的包裹,在电感耦合等离子体发射光谱法分析过程中通过分析谱线的选择,对其中的砷进行准确测定,方法精密度(RSD,n=12)为0.99%~1.52%,回收率为97.8%~99.6%,方法检出限为1.01μg/g。本方法能快速有效溶解锑精矿并避免锑水解对砷的包裹,经国家一级标准物质GBW07175和GBW07176验证,所得结果与标准值一致,能够对锑矿石中含量范围在0.1~10%的砷进行快速准确测定。 The conventional aqua regia solution of arsenic in antimony concentrate can not effectively decompose the silicate component in the ore,resulting in incomplete decomposition.In the subsequent extraction process,the hydrolysis of antimony will package arsenic to a certain extent,resulting in low arsenic determination results.In this paper,the mixed system of hydrofluoric acid hydrochloric acid nitric acid perchloric acid was used to dissolve in open solution,then tartaric acid and antimony were added to inhibit the hydrolysis of antimony and eliminate the inclusion of arsenic by antimony precipitation.In the analysis process of inductively coupled plasma atomic emission spectrometry(ICP-AES),arsenic was accurately determined through the selection of analytical lines,and the method precision(RSD,n=12)was 0.99%~1.52%,and the recovery rate was 97.8%~99.6%,the detection limit was 1.01ug/g.This method can quickly and effectively dissolve antimony ore and avoid the inclusion of arsenic by antimony hydrolysis.The results are consistent with the standard values verified by the national first-class reference materials GBW07174 and GBW07175.It can quickly and accurately determine arsenic in antimony ore in the range of 0.1-10%.
作者 潘钢 雷勇 Pan Gang;Lei Yong(Institute of Multipurpose Utilization of Mineral Resources,CAGS,Chengdu,Sichuan,China)
出处 《矿产综合利用》 CAS 北大核心 2021年第4期201-205,共5页 Multipurpose Utilization of Mineral Resources
关键词 敞口酸溶 电感耦合等离子体发射光谱 锑精矿 Open acid dissolution ICP-AES Antimony concentrate Arsenic
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