微波消解-电感耦合等离子体原子发射光谱法测定锌精矿中锑
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摘要
在锌的冶炼过程中,为了防止"烧板"现象,需要快速检测锌精矿中锑元素含量。采用硝酸、氢氟酸微波消解样品,消解结束后加入硫酸,用赶酸仪赶氢氟酸,选择Sb 217.582nm为分析谱线,采用基体匹配法绘制校准曲线消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定锌精矿中锑。锌质量浓度为0.05～200mg/L时与其发射强度呈线性关系,相关系数为0.999 6;方法检出限为0.003%(质量分数,下同),测定下限为0.01%。按照实验方法测定锌精矿样品中锑,结果的相对标准偏差(RSD,n=12)为1.7%;加标回收率为98%～99%。按照实验方法测定4个锌精矿样品中锑,测定结果与氢化物发生-原子荧光光谱法或硫酸铈滴定法的测定结果一致。
In the process of zinc smelting,the content of antimony in zinc concentrate should be rapidly detected in order to prevent the "burning plate"phenomenon.The sample was treated with nitric acid and hydrofluoric acid by microwave digestion.Sulfuric acid was added after digestion to remove hydrofluoric acid with the acid catcher.Sb 217.582 nm was selected as the analytical line.The influence of matrix effect was eliminated by preparing calibration curve with matrix matching method.The content of antimony in zinc concentrate was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The mass concentration of antimony in range of 0.05-200 mg/L was linear to its corresponding emission intensity with correlation coefficient of 0.999 6.The detection limit of method was 0.003%(mass fraction,the same below)and the low limit of determination was 0.01%.The content of antimony in zinc concentrate sample was determined according to the experimental method.The relative standard deviation(RSD,n=12)of the determination results was 1.7%.The spiked recoveries were between 98% and 99%.The proposed method was applied for determination of antimony in four zinc concentrate samples,and the found results were consistent with those obtained by hydride generation-atomic fluorescence spectrometry(HG-AFS)or cerium sulfate titration.
In the process of zinc smelting,the content of antimony in zinc concentrate should be rapidly detected in order to prevent the "burning plate"phenomenon.The sample was treated with nitric acid and hydrofluoric acid by microwave digestion.Sulfuric acid was added after digestion to remove hydrofluoric acid with the acid catcher.Sb 217.582 nm was selected as the analytical line.The influence of matrix effect was eliminated by preparing calibration curve with matrix matching method.The content of antimony in zinc concentrate was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The mass concentration of antimony in range of 0.05-200 mg/L was linear to its corresponding emission intensity with correlation coefficient of 0.999 6.The detection limit of method was 0.003%(mass fraction,the same below)and the low limit of determination was 0.01%.The content of antimony in zinc concentrate sample was determined according to the experimental method.The relative standard deviation(RSD,n=12)of the determination results was 1.7%.The spiked recoveries were between 98% and 99%.The proposed method was applied for determination of antimony in four zinc concentrate samples,and the found results were consistent with those obtained by hydride generation-atomic fluorescence spectrometry(HG-AFS)or cerium sulfate titration.
引文
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[3]岩石矿物编委会.岩石矿物分析:第3分册[M].4版.北京:地质出版社,2011:134-151.
[4]王淑梅,赵迎.火焰原子吸收光谱法测定辉锑矿中锑[J].分析试验室,2001,20(1):95-96.WANG Shu-mei,ZHAO Ying.Determination of Sb in antimonite by flame atomic absorption spectrophotometry[J].Chinese Journal of Analysis Laboratory,2001,20(1):95-96.
[5]范凡,温宏利,屈文俊,等.王水溶样-等离子体质谱法同时测定地质样品中砷锑铋银镉铟[J].岩矿测试,2009,28(4):333-336,341.FAN Fan,WEN Hong-li,QU Wen-jun,et al.Determination of arsenic,antimony,bismuth,silver,cadmium and indium in geological samples by inductively coupled plasma-mass spectrometry with aqua regia sample digestion[J].Rock and Mineral Analysis,2009,28(4):333-336,341.
[6]葛晶晶,刘洁.电感耦合等离子体质谱法测定高纯锌中7种痕量元素[J].冶金分析,2016,36(9):37-41.GE Jing-jing,LIU Jie.Determination of seven trace elements in high purity zinc by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2016,36(9):37-41.
[7]陈殿耿,李华昌,孙龄高,等.氢化物发生-原子荧光光谱法测定高纯锌中砷、锑、铋[J].分析试验室,2006,25(8):38-41.CHEN Dian-geng,LI Hua-chang,SUN Ling-gao,et al.Determination of arsenic,antimony and bismuth in high purity zinc by hydride generation-atomic fluorescence spectrometry[J].Chinese Journal of Analysis Laboratory,2006,25(8):38-41.
[8]何飞顶,李华昌,袁玉霞.氢化物发生-原子荧光光谱法同时测定红土镍矿中砷锑铋[J].冶金分析,2011,31(4):44-47.HE Fei-xiang,LI Hua-chang,YUAN Yu-xia.Determination of arsenic,antimony and bismulth in laterite nickel ore by hydride generation-atomic fluorescence spectrometry[J].Metallurgical Analysis,2011,31(4):44-47.
[9]冯宝艳.ICP-AES测定铜精矿中As,Sb,Bi,Ca,Mg,Pb,Co,Zn和Ni[J].分析试验室(Chinese Journal of Analysis Laboratory),2008,27(Z1):67-68.
[10]马新荣,马生凤,王蕾,等.王水溶矿-等离子体光谱法测定砷矿石和锑矿石中砷锑硫铜铅锌[J].岩矿测试,2011,30(2):190-194.MA Xin-rong,MA Sheng-feng,WANG Lei,et al.Determination of As,Sb,S,Cu,Pb,Zn in arsenic ore and stibium ore by inductively coupled plasma-atomic emission spectrometry with aqua regia digestion[J].Rock and Mineral Analysis,2011,30(2):190-194.
[11]李景文.电感耦合等离子体发射光谱法测定铅锑合金中锑砷铋锡锌铁[J].岩矿测试,2010,29(2):185-186.LI Jing-wen.Determination of Sb,As,Bi,Sn,Zn and Fe in lead-antimony alloy by inductively coupled plasma-atomic emission spectrometry[J].Rock and Mineral A-nalysis,2010,29(2):185-186.