电感耦合等离子体发射光谱法测定硫化物矿中的汞
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摘要
建立电感耦合等离子体发射光谱法测定硫化物矿中汞的含量。采用王水密闭消解溶矿,汞的元素谱线为194.168 nm,功率为1.1 kW,等离子体气流量为15.0 L/min,辅助气流量为0.2 L/min,雾化气流量为0.8 L/min,溶液提升量为1.6 mL/min,轴向观测高度为15 mm,以电感耦合等离子体发射光谱法测定硫化物矿中汞。汞的质量浓度在0.05～20.0 mg/L范围内与光谱强度呈良好的线性关系,相关系数为0.999 9,方法检出限为1.25μg/g。测定结果的相对标准偏差小于5%(n=5),样品加标回收率为96%～106%。该方法操作简单快速,准确可靠,适用于硫化物矿中较高含量汞的测定。
A method for determination of mercury in sulphide ores by inductively coupled plasma emission spectrometry(ICP–OES) was established. Solution of ores by closed digestion with aqua regia. The elemental spectrum of mercury was 194.168 nm, the power was 1.1 kW, the plasma gas ?ow rate was 15.0 L/min, the auxiliary gas ?ow rate was 0.2 L/min, the atomization gas ?ow rate was 0.8 L/min, the solution lift rate was 1.6 mL/min, the axial observation height was 15 mm. The content of mercury in sulfide ore was determined by inductively coupled plasma emission spectrometry. The mass concentration of mercury in the range of 0.05–20.0 mg/L showed a good linear relationship with the spectral intensity, the correlation coef?cient was 0.999 9, and the detection limit was 1.25 μg/g. The relative standard deviations were less than 5%(n=5), and the recoveries were 96%–106%. The method is simple, rapid, accurate and reliable.It is suitable for the determination of higher mercury content in sul?de ores.
A method for determination of mercury in sulphide ores by inductively coupled plasma emission spectrometry(ICP–OES) was established. Solution of ores by closed digestion with aqua regia. The elemental spectrum of mercury was 194.168 nm, the power was 1.1 kW, the plasma gas ?ow rate was 15.0 L/min, the auxiliary gas ?ow rate was 0.2 L/min, the atomization gas ?ow rate was 0.8 L/min, the solution lift rate was 1.6 mL/min, the axial observation height was 15 mm. The content of mercury in sulfide ore was determined by inductively coupled plasma emission spectrometry. The mass concentration of mercury in the range of 0.05–20.0 mg/L showed a good linear relationship with the spectral intensity, the correlation coef?cient was 0.999 9, and the detection limit was 1.25 μg/g. The relative standard deviations were less than 5%(n=5), and the recoveries were 96%–106%. The method is simple, rapid, accurate and reliable.It is suitable for the determination of higher mercury content in sul?de ores.
引文
[1]岩石矿物分析编委会.岩石矿物分析(第三分册)[M].第4版.北京:地质出版社,2011:166-169.
[2]GB/T 8152.11-2006铅精矿化学分析方法汞量的测定原子荧光光谱法[S].
[3]陈焱,李勇,李长青.巯基棉分离富集-原子荧光光谱法测定重晶石中痕量汞[J].岩矿测试,2008,27(6):431-434.
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[6]钟勇,潘菲.氏管分离-冷原子荧光光谱法测定锌精矿中微量汞[J].岩矿测试,2001,20(2):145-146.
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[11]于永斌,何振辉,徐辉.王水消解/冷原子荧光法测定土壤中的微量汞[J].中国环境管理干部学院学报,2009,19(2):66-68.
[12]祝建国,毛振才.原子荧光光谱法快速测定锌精矿中汞/砷[J].地质实验室,1998,14(2):78-81.
[13]姜晓波,保春燕.水浴消解-原子荧光光度法测定土壤中的汞[J].工业安全与环保,2006,32(7):33-34.
[14]杨柳,刘新群,王进.氧化锌中铅镉汞的ICP-OES法测定[J].特种橡胶制品,2009,30(5):44-45.
[15]刘化玲,牛丽川,黄小亚,等.ICP-OES测定铅汞镉的参数优化[J].电视技术,2012,36(12):90-91.
[16]董敏茹.氢化物发生-ICP/AES测定石化废水中As、Pb、Hg[J].环境监测管理与技术,2004,16(4):33-34.
[2]GB/T 8152.11-2006铅精矿化学分析方法汞量的测定原子荧光光谱法[S].
[3]陈焱,李勇,李长青.巯基棉分离富集-原子荧光光谱法测定重晶石中痕量汞[J].岩矿测试,2008,27(6):431-434.
[4]梁镇宗,归俊,唐亲之,等.快速络合滴定法测定矿物中的汞[J].冶金分析,1988,8(6):46-47.
[5]余淑媛,陈向阳,冯均利,等.利用直接进样-冷原子吸收光谱法测定矿产品中的汞含量[J].冶金分析,2010,30(7):39-43.
[6]钟勇,潘菲.氏管分离-冷原子荧光光谱法测定锌精矿中微量汞[J].岩矿测试,2001,20(2):145-146.
[7]宋国玺.冷原子吸收法测定锌精矿中的汞[J].分析测试技术与仪器,2000,6(4):238-241.
[8]袁爱萍,唐艳霞,黄玉龙,等.氢化物-原子荧光法测定锑精矿中痕量砷、汞的研究[J].光谱学与光谱分析,2006,26(8):1 553-1 556.
[9]张善文.火焰原子吸收分光光度法测定汞精矿中高浓度汞[J].哈尔滨建筑工程学院学报,1983(3):93-96.
[10]张道礼,严少仪,魏伟,等.用冷蒸汽原子吸收光谱法测定铜精矿中的汞[J].光谱实验室,1993,10(5):52-56.
[11]于永斌,何振辉,徐辉.王水消解/冷原子荧光法测定土壤中的微量汞[J].中国环境管理干部学院学报,2009,19(2):66-68.
[12]祝建国,毛振才.原子荧光光谱法快速测定锌精矿中汞/砷[J].地质实验室,1998,14(2):78-81.
[13]姜晓波,保春燕.水浴消解-原子荧光光度法测定土壤中的汞[J].工业安全与环保,2006,32(7):33-34.
[14]杨柳,刘新群,王进.氧化锌中铅镉汞的ICP-OES法测定[J].特种橡胶制品,2009,30(5):44-45.
[15]刘化玲,牛丽川,黄小亚,等.ICP-OES测定铅汞镉的参数优化[J].电视技术,2012,36(12):90-91.
[16]董敏茹.氢化物发生-ICP/AES测定石化废水中As、Pb、Hg[J].环境监测管理与技术,2004,16(4):33-34.