Determination of antimony in antimony ores from the beneficiation process in Yunnan by inductively coupled plasma atomic emission spectrometry
SUN Qiliang1,2,3, YAO Mingxing*1,2,3, ZHANG Hongli1,2,3, GUO Xiaorui1,2,3, NI Wenshan1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou 450006,China; 2. China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou 450006,China; 3. Key Laboratory for Polymetallic Ores' Evaluation and Utilization,MNR,Zhengzhou 450006,China
Abstract：Antimony plays an important role in modern industrial system. The rapid and accurate determination of antimony content in antimony ore has important guiding significance for the mining and beneficiation of antimony ores. Fluorite is the main associated ore of antimony ore in a mine in Yunnan Province. The existing mixed acid system containing hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid cannot completely decompose the samples. The process of alkali fusion treatment is long and a large amount of matrix is introduced, which cannot meet the requirements of accurate and rapid determination. The samples were decomposed with mixed acid of hydrofluoric acid and sulfuric acid followed by heating extraction with tartaric acid and hydrochloric acid mixed solution. The antimony in sample could be completely dissolved in the solution. The content of antimony was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) using Sb 206.833{463} nm as the analytical line. The results showed that the mass concentration of antimony in range of 5.0-80 μg/mL had a good linear relationship to the emission intensity. The linear correlation coefficient of calibration curve was r=0.999 8. The limit of detection of the method was 0.012 μg/mL. The contents of antimony in certified reference materials of antimony ore and actual antimony ores from the beneficiation process were determined according to the experimental method. The relative standard deviations (RSD, n=5) of the measured values were between 0.71% and 5.7%. The found results of certified reference materials were consistent with the certified values. The spiked recoveries of antimony for actual sample from the beneficiation process were between 97% and 102%, which could meet the requirements of the national geological and mineral industry standard DZ/T 0130-2006.
孙启亮, 姚明星, 张宏丽, 郭晓瑞, 倪文山. 电感耦合等离子体原子发射光谱法测定云南某矿山锑矿选矿流程样品中锑[J]. 冶金分析, 2022, 42(11): 55-61.
SUN Qiliang, YAO Mingxing, ZHANG Hongli, GUO Xiaorui, NI Wenshan. Determination of antimony in antimony ores from the beneficiation process in Yunnan by inductively coupled plasma atomic emission spectrometry. , 2022, 42(11): 55-61.
[1] 李中平.中国锑行业发展现状及高质量发展建议[J].中国国土资源经济,2021,34(3):17-20,68. LI Zhongping.Development status of antimony industry in china and suggestions for high-quality development[J].Resource Economy,2021,34(3):17-20,68. [2] 余晓,梁云生,毛禹平.极谱法和原子吸收光谱法快速分析矿石中的锑[J].中国无机分析化学,2014,4(4):21-23. YU Xiao,LIANG Yunsheng,MAO Yuping.Rapidanalysis of Sb in ore by polarographymethod and atomic absorption spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2014,4(4):21-23. [3] 刘志仓,郭国涛,王宏强,等.火焰原子吸收法测定矿石中锑元素的方法试验[J].中国金属通报,2018(4):198-200. LIU Zhicang,GUO Guotao,WANG Hongqiang,et al.Determination of antimony in ores by flame atomic absorption spectrometry[J].China Metal Bulletin,2018(4):198-200. [4] 黎香荣,唐梦奇,袁焕明,等.熔融制样-X射线荧光光谱法测定锑矿石中主次成分[J].冶金分析,2014,34(7):38-42. LI Xiangrong,TANG Mengqi,YUAN Huanming,et al.Determination of major and minor components in antimony ore by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2014,34(7):38-42. [5] 郑向明,吴雪英,魏雅娟,等.氢化物发生-原子荧光光谱法测定银精矿中锑[J].冶金分析,2019,39(6):49-53. ZHENG Xiangming,WU Xueying,WEI Yajuan,et al.Determination of antimony in silver concentrate by hydride generation atomic fluorescence spectrometry[J].Metallurgical Analysis,2019,39(6):49-53. [6] 魏轶,窦向丽,巨力佩,等.四酸溶解-电感耦合等离子体发射光谱法测定金锑矿和锑矿石中的锑[J].岩矿测试,2013,32(5):715-718. WEI Yi,DOU Xiangli,JU Lipei,et al.Determination of antimony in gold-antimony ore and antimony ore by inductively coupled plasma-atomic emission spectrometry with four acids dissolution[J].Rock and Mineral Analysis,2013,32(5):715-718. [7] 郑智慷,曾江萍,王家松,等.常压密闭微波消解-电感耦合等离子体发射光谱法测定锑矿石中的锑[J].岩矿测试,2020,39(2):208-215. ZHENG Zhikang,ZENG Jiangping,WANG Jiasong,et al.Determination of antimony in antimony ores by inductively coupled plasma-optical emission spectrometry with microwave digestion[J].Rock and Mineral Analysis,2020,39(2):208-215. [8] 李皓,张尼,马熠罡.碱熔样电感耦合等离子体发射光谱法测定锑矿石中锑[J].化学分析计量,2016,25(2):69-71. LI Hao,ZHANG Ni,MA Yigang.Determination of antimony in antimony ore by inductively coupled plasma emission spectrometry combined with alkali fusion pretreatment[J].Chemical Analysis and Meterage,2016,25(2):69-71. [9] 任志海,牟思名,程功,等.王水密闭溶矿-电感耦合等离子体原子发射光谱法测定锑矿石中的锑[J].中国无机分析化学,2014,4(1):53-55. REN Zhihai,MOU Siming,CHENG Gong,et al.Determination of Sb in stadium ore by inductively coupled plasma-atomic emission spectrometry with closed digestion usingaguaregia[J].Chinese Journal of Inorganic Analytical Chemistry,2014,4(1):53-55. [10] 陈丽珠,曹胜.电感耦合等离子体发射光谱(ICP-OES)法测定矿石中锑[J].中国无机分析化学,2017,7(4):60-63. CHEN Lizhu,CAO Sheng.Determination of antimony in ores by inductively coupled plasma-optical emission spectrometry(ICP-OES)[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(4):60-63. [11] 杨惠玲,夏辉,杜天军,等.电感耦合等离子体发射光谱法同时测定锡矿石中锡钨钼铜铅锌[J].岩矿测试,2013,32(6):887-892. YANG Huiling,XIA Hui,DU Tianjun,et al.Simultaneous determination of Sn,W,Mo,Cu,Pb and Zn in Tin ores by inductively coupled plasma-atomic emission spectrometry[J].Rock and Mineral Analysis,2013,32(6):887-892. [12] 严慧,王干珍,汤行,等.电感耦合等离子体原子发射光谱法同时测定锑矿石中14种元素的含量[J].理化检验(化学分册),2017,53(1):34-38. YAN Hui,WANG Ganzhen,TANG Xing,et al.Simultaneous determination of 14 elements in antimony ores by inductively coupled plasma-atomic emission spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2017,53(1):34-38. [13] 薛宁.电感耦合等离子体原子发射光谱法测定萤石中11种元素[J].冶金分析,2021,41(3):62-67. XUE Ning.Determination of eleven elements in fluorite by inductively coupled plasma atomic emissions spectrometry[J].Metallurgical Analysis,2021,41(3):62-67. [14] 《岩石矿物分析》编委会.岩石矿物分析:第三分册[M].4版.北京:地质出版社,2011,134-151. [15] 熊英,董亚妮,裴若会,等.电感耦合等离子体发射光谱法应用于锑矿石化学物相分析[J].岩矿测试,2019,38(5):497-502. XIONG Ying,DONG Yani,PEI Ruohui,et al.Determination of antimony content in antimony ores by inductively coupled plasma-optical emission spectrometry[J].Rock and Mineral Analysis,2019,38(5):497-502. [16] 潘钢,雷勇.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[J].矿产综合利用,2021(4):201-205. PAN Gang,LEI Yong.Determination of arsenic in antimony concentrate by open-mouth acid dissolution inductively coupled plasma atomic emissions spectrometry[J].Multipurpose Utilization of Mineral Resources,2021(4):201-205.
