Abstract：The content of antimony in silver concentrate should be detected to ensure the smooth transaction between the supplier and demander. The sample was dissolved with nitric acid-potassium chlorate-hydrofluoric acid-sulfuric acid system. The thiourea-ascorbic acid was used as the pre-reducing reagent and 10g/L potassium borohydride solution was used as the reducing reagent. A determination of antimony in silver concentrate by hydride generation atomic fluorescence spectrometry (HG-AFS) was realized in the medium of 10% (volume fraction) hydrochloric acid. The methods of sample dissolution as well as the interference and elimination of coexisting elements in samples were discussed in detail. The results showed that 0.2g of sample could be completely dissolved with 10.0mL of nitric acid, 0.50g of potassium chlorate, 5.0mL of hydrofluoric acid and 5.0mL of sulfuric acid (1+1). Except for arsenic, the interference of other coexisting elements with the determination of antimony could be ignored. Arsenic had positive interference with the determination of antimony, which could be eliminated by reducing the mass concentration of potassium borohydride solution to 10g/L. Under the selected experimental conditions, the mass concentration of antimony in the range of 5.00-100.0μg/L showed a linear relationship with its corresponding fluorescence intensity. The linear correlation coefficient was 0.9995. The detection limit of the method was 6×10-2 μg/L. The content of antimony in silver concentrate samples with the mass fraction of antimony from 0.01% to 0.50% was determined according to the experimental method. The found results were consistent with those obtained by inductively coupled plasma emission spectrometry (ICP-AES), and the relative standard deviations (RSDs, n=11) were between 1.0% and 2.3%. The recovery tests of two silver concentrate samples were conducted according to the experimental method. The spiked recoveries were between 95% and 105%
高云,宋召霞.硫化钠还原-硫酸铈滴定法测定含锑金精矿中锑[J].冶金分析,2017,37(3):39-43.GAO Yun,SONG Zhao-xia.Determination of antimony in gold concentrate containing antimony by cerium sulfate titrimetry with sodium sulfide reduction[J].Metallurgical Analysis,2017,37(3):39-43.
[3]
石文莹.硫酸铈滴定法测定湿法炼锑电解液中锑的含量[J].湖南有色金属,2017,33(3):76-77.SHI Wen-ying.Determination of antimony content in hydrometallurgical antimony electrolyte by cerium sulfate titration[J].Hunan Nonferrous Metals,2017,33(3):76-77.
[4]
姜淑娟,崔运成,吕明,等.锑矿中锑的测定[J].吉林师范大学学报:自然科学版,2004,25(2):95-96.JIANG Shu-juan,CUI Yun-cheng,LÜ Ming,et al.Determination of antimony in antimony deposit[J].Journal of Jilin Normal University:Natural Science Edition,2004,25(2):95-96.
[5]
王凯.孔雀绿分光光度法测定粗铟中锑[J].冶金分析,2004,24(2):66-67.WANG Kai.Spectrophotometric determination of antimony in crude indium with malachite green[J].Metallurgical Analysis,2004,24(2):66-67.
[6]
陈珍娥,马超,张海.分光光度计的改装及在锑测定中的应用[J].冶金分析,2017,37(5):77-81.CHEN Zhen-e,MA Chao,ZHANG Hai.Modification of spectrophotometer and its application in determination of antimony[J].Metallurgical Analysis,2017,37(5):77-81.
[7]
李报厚.石墨炉原子吸收法测定铜合金中微量锑[J].冶金分析,1986,6(3):29-32.LI Bao-hou.Determination of trace of antimony in the copper alloys by graphite furnace atomic absorption spectrometry[J].Metallurgical Analysis,1986,6(3):29-32.
[8]
刘慧明.原子吸收光谱法测定铜精矿中锑[J].铜业工程,2006(1):81-82.LIU Hui-ming.Determination of antimony in copper concentrates by atomic absorption spectrometry[J].Copper Engineering,2006(1):81-82.
魏雅娟,吴雪英,江荆,等.微波消解-电感耦合等离子体原子发射光谱法测定银精矿中铅锌铜砷锑铋镉[J].冶金分析,2018,38(5):51-57.WEI Ya-juan,WU Xue-ying,JIANG Jing,et al.Determination of Pb,Zn,Cu,Sb,Bi,Cd in silver concentrate by microwave digestion coupled with inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(5):51-57.
[11]
余灿辉,罗永锋,聂正才.ICP-MS测定无汞锌粉中砷、锑的量[J].中国有色冶金,2016,45(6):72-74.YU Can-hui,LUO Yong-feng,NIE Zheng-cai.ICP-MS determination of rsenic and antimony in mercury-free zinc powder[J].China Nonferrous Metallurgy,2016,45(6):72-74.
[12]
李岩.氢化物-原子荧光光谱法连续测定锌精矿中砷、锑、铋、锡[J].分析化学,2004,32(2):205-208.LI Yan.Sequential determination of As,Sb,Bi and Sn in zinc concentrates by hydride generation atomic fluorescence spectrometry in the presence of L-cysteine[J].Chinese Journal of Analytical Chemistry,2004,32(2):205-208.
[13]
孙伟.原子荧光光谱法快速测定化探样品中的微量砷、锑、铋、汞[J].光谱实验室,2001,18(4):513-516.SUN Wei.Rapid determination of arsenic,antimony,bismuth and mercury in geochemical sample by atomic fluorescence spectrometry[J].Chinese Journal of Spectroscopic Laboratory,2001,18(4):513-516.
[14]
祝建国,陈月源,张旺强,等.原子荧光光谱法快速测定锑矿石中的汞、铋、硒[J].化学分析计量,2010,19(4):63-65.ZHU Jian-guo,CHEN Yue-yuan,ZHANG Wang-qiang,et al.Rapid determination of mercury,bismuth,selenium in antimony ore by atomic fluorescence spectrometry[J].Chemical Analysis and Meterage,2010,19(4):63-65.
[15]
张效伟,张召香,宋琦,等.对喷式氢化物发生原子荧光光谱法同时测定烟叶中痕量砷和锑[J].分析化学,2006,34(10):1448-1450.ZHANG Xiao-wei,ZHANG Zhao-xiang,SONG Qi,et al.Simultaneous determination of trace As and Sb in tobacco samples by opposite spray hydride generation atomic fluorescence spectrometry[J].Chinese Journal of Analytical Chemistry,2006,34(10):1448-1450.
[16]
高丽娜,边疆.氢化物发生-原子荧光光谱法同时测定保健食品中砷和锑[J].中国卫生检验杂志(Chinese Journal of Health Laboratory Technology),2006,16(11):1333-1334.
[17]
赵振平,张怀成,冷家峰,等.王水消解蒸气发生-原子荧光光谱法测定土壤中的砷、锑和汞[J].中国环境监测,2004,20(1):44-46.ZHAO Zhen-ping,ZHANG Huai-cheng,LENG Jia-feng,et al.The method of VG-AFS with clearing by aqua regia to determine As,Sb and Hg in the soil[J].Environmental Monitoring in China,2004,20(1):44-46.
