Determination of bismuth in silver concentrate by hydridegeneration atomic fluorescence spectrometry
LIU Xiao-yan1, LUO Jiang-bo*2
1.Daye Non-Ferrous Design & Inspection Institute Co., Ltd., Huangshi 435000, China; 2.Product Quality Supervision and Inspection Institute, Huangshi 435000, China
Abstract：During the trade of silver concentrate between supply and requisitioning parties as well as the determination of production technology process, the content of related elements such as bismuth plays an important role. The sample dissolution method in standard YS/T 445.11-2001 was modified. The potassium chlorate-nitric acid-sulfuric acid-aqua regia system was replaced by potassium chlorate-nitric acid-hydrofluoric acid-sulfuric acid-hydrochloric acid system to dissolve the sample. The determination of bismuth in silver concentrate by hydride generation atomic fluorescence spectrometry was realized using thiourea-ascorbic acid as pre-reduction reagent, potassium borohydride as reducing agent, and 5% (volume fraction) hydrochloric acid as determination medium. Under the selected experimental conditions, the mass concentration of bismuth in range of 20.0-200.0ng/mL had linear relationship with the spectral intensity. The correlation coefficient was 0.9994. The interference tests were conducted according to the maximum content of major coexisting elements in silver concentrate. The results showed that the interferences could be ignored. The detection limit was 2×10-5 μg/mL. The silver concentrate sample (the mass fraction of bismuth was in range of 0.010%-0.50%) was determined, and the found results were basically consistent with those obtained by flame atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry. The relative standard deviations (RSD, n=9) were between 1.9% and 10.6%. The recoveries were between 99% and 102%.
魏雅娟,吴雪英,江荆,等.火焰原子吸收光谱法(AAS)测定银精矿中铋元素的含量[J].山东工业技术,2018(7):225-226.WEI Ya-juan,WU Xue-ying,JIANG Jing,et al.Determination of bismuth content in silver concentrates by the flame atomic absorption spectrophotometry method (AAS)[J].Shandong Industrial Technology,2018(7):225-226.
[3]
蒯丽君.Na2EDTA滴定法测定锡阳极泥中的铋量[J].中国无机分析化学,2016,6(3):81-86.KUAI Li-jun.Determination of bismuth in tin anode slime by Na2EDTA titrimetric method[J].Chinese Journal of Inorganic Analytical Chemistry,2016,6(3):81-86.
[4]
于兆水,李淑娟,张勤.氢化物发生-原子荧光光谱法测定地球化学样品中痕量铋[J].岩矿测试,2005,24(3):217-220.YU Zhao-shui,LI Shu-juan,ZHANG Qin.Determination of trace bismuth in geological samples by hydride generation-atomic fluorescence spectrometry[J].Rock and Mineral Analysis,2005,24(3):217-220.
[5]
王婕.氢化物发生-原子荧光光谱法同时测定土壤和沉积物中的汞和铋[J].现代盐化工,2014(4):22-24.WANG Jie.The determination of mercury and bismuthby in soll and sediment by the hydride-atomic fluorescence method[J].Modern Salt and Chemical Industry,2014(4):22-24.
[6]
王明海.氢化物发生-原子荧光光谱法测定钢铁及合金中痕量砷和铋[J].冶金分析,2006,26(5):33-36.WANG Ming-hai.Determination of trace arsenic and bismuth content in iron,steel and alloys by hydride generation-atomic fluorescence spectrometric method[J].Metallurgical Analysis,2006,26(5):33-36.
[7]
董海龙,李华昌,孙龄高.氢化物发生-原子荧光光谱法测定高纯锌中痕量铋[J].理化检验:化学分册,2008,44(2):175-177.DONG Hai-long,LI Hua-chang,SUN Ling-gao.Determination of trace amount of bismuth in high purity zinc by hydride generation-atomic fluorescence spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2008,44(2):175-177.
[8]
叶海辉,周聪,赵敏,等.氢化物发生-原子荧光光谱法同时测定食品中砷锑铋硒[J].安徽农业科学,2012,40(12):7434-7435.YE Hai-hui,ZHOU Cong,ZHAO Min,et al.Determination of As,Sb,Bi and Se in food by hydride generation-atomic fluorescence spectrometry (HG-AFS)[J].Journal of Anhui Agricultural Sciences,2012,40(12):7434-7435.
[9]
王向东.氢化物发生-原子荧光光谱法测定水中微量元素[J].云南环境科学,2001,20(4):56-57.WANG Xiang-dong.Determination trace element in water by hydroxide produced atomic fluorescence spectrometry[J].Yunnan Environmental Sciences,2001,20(4):56-57.
陈永欣,黎香荣,魏雅娟,等.氢氧化铁和氢氧化镧共沉淀分离电感耦合等离子体原子发射光谱法测定铜精矿中铅砷锑铋[J].冶金分析,2009,29(5):41-44.CHEN Yong-xin,LI Xiang-rong,WEI Ya-juan,et al.Determination of lead, arsenic, stibium and bismuth in copper concentrates with ironic hydroxide and lanthanum hydroxide co-precipitation and inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2009,29(5):41-44.
