Abstract：The contents of micro elements in antimony ingot are main indexes to determine its quality. The current national standard method (GB/T 3253.X-2008/2009) has some shortcomings such as high operation difficulty and low efficiency, so it is of great significance to develop new determination method. In this paper, the sample was dissolved with aqua regia at low temperature. The hydrolysis of antimony was inhibited by adding hydrofluoric acid. Pb 220.353 nm, Fe 259.940 nm, Cu 324.754 nm, Cd 214.438 nm, As 193.759 nm, Se 196.090 nm, Bi 190.234 nm, Hg 194.227 nm and S 180.731 nm were selected as the analytical lines for Pb, Fe, Cu, Cd, As, Se, Bi, Hg and S, respectively. The influence of matrix effect was eliminated by drawing calibration curves with matrix matching method. Thus,a method for determination of 9 micro elements (Pb, Fe, Cu, Cd, As, Se, Bi, Hg and S) in antimony ingot was established by inductively coupled plasma emission spectrometry(ICP-AES). The linear correlation coefficients (r) of calibration curves of elements were greater than 0.999 5. The limits of detection of this method were 0.000 020%-0.000 21%, and the limits of quantification were 0.000 067%-0.000 70%. 9 micro elements in antimony ingot samples were determined according to the proposed method. The results were consistent with those obtained by national standard method (GB/T 3253.X-2008/2009), and the relative standard deviations (RSD, n=10) of determination results were between 1.3% and 9.4%.
[1] 丁学全,杨薛玲.对当前中国锑行业发展困境的思考[J].中国有色金属(China Nonferrous Metals),2016(1):28-29. [2] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 1599—2014 锑锭[S].北京:中国标准出版社,2014. [3] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 3253.X—2008/2009 锑及三氧化二锑化学分析方法[S].北京:中国标准出版社,2008/2009. [4] 张彦翠,方彦霞,齐白羽.电感耦合等离子体原子发射光谱法测定工业红矾钠中钙镁铝锰铁[J].冶金分析,2018,38(7):70-74. ZHANG Yancui, FANG Yanxia, QI Baiyu. Determination of calcium,magnesium,aluminum,manganese and iron in industrial sodium bichromate by inductively coupled plasma atomic emission spectrometry[J]. Metallurgical Analysis,2018,38(7):70-74. [5] 王志萍,孙洪涛,王巧.微波消解-电感耦合等离子体原子发射光谱法测定氧化铟锡靶材中11种痕量杂质元素[J].冶金分析,2018,38(5):60-65. WANG Zhiping,SUN Hongtao,WANG Qiao.Determination of eleven trace impurity elements in indium tin oxide target material by inductively coupled plasma atomic emission spectrometry after microwave digestion[J].Metallurgical Analysis,2018,38(5):60-65. [6] Zuma M C,Nomngongo P N,Mketo N.Simultaneous determination of REES in coal samples using the combination of microwave-assisted ashing and ultrasound-assisted extraction methods followed by ICP-OES analysis[J].Minerals,2021,11(10):1103. [7] Linderoth O,Johansson P.A method to determine binder content in small samples of cementitious material using hydrochloric acid and ICP-OES analysis[J].Materials Today Communications,2019,20:100538. [8] 刘芳美,甘聪,罗小兵,等.电感耦合等离子体发射光谱法同时测定文丘里泥中铜、铅、砷、锑、铋、碲、汞[J].化学分析计量,2023,32(1):61-64. LIU Fangmei,GAN Cong,LUO Xiaobing,et al.Determination of copper,lead,arsenic,antimony,bismuth,tellurium and mercury in venturi slime by inductively coupled plasma emission spectrometry[J].Chemical Analysis and Meterage,2023,32(1):61-64. [9] 卞大勇.电感耦合等离子体原子发射光谱法测定高含量碳化硅表面6种杂质成分[J].冶金分析,2018,38(5):72-77. BIAN Dayong.Determination of six impurity components on surface of high-content silicon carbide by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(5):72-77. [10] 易风兰.电感耦合等离子体原子发射光谱法测定锑锭中铅等多种杂质元素[J].金属材料与冶金工程,2012,40(3):52-54. YI Fenglan.Determination of impurity elements in antimony ingot by ICP-AES method[J].Metal Materials and Metallurgy Engineering,2012,40(3):52-54. [11] 冯先进,李培.锑锭中杂质元素的ICP-OES法测定方法研究[J].矿冶,2006(2):89-90,99. FENG Xianjn,LI Pei.Study on the determination of impurities in antimony ingot by ICP-OES[J].Mining and Metallurgy,2006(2):89-90,99. [12] Winge R k,Fassle V A,Peterson V J,et al.电感耦合等离子体发射光谱图册[M].Winge R K,钱国贤等,译.北京:中国光学学会光谱学会,1986.
