电感耦合等离子体发射光谱法(ICP-AES)测定冶炼副产品硫酸镍中砷、锌、钴
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摘要
冶炼副产品硫酸镍组成成分复杂,准确分析杂质元素As、Zn、Co含量对设计硫酸镍提纯工艺有重要意义。采用硝酸-盐酸-氢氟酸-高氯酸体系对样品进行前处理,优化仪器工作条件,建立了电感耦合等离子体发射光谱法(ICP-AES)测定冶炼副产品硫酸镍中As、Zn、Co的方法。本实验分别以As 189.042nm,Zn 206.200nm,Co 228.616nm为分析谱线。实验结果表明:待测溶液中20g/L硫酸镍基体及1g/L Cu、20mg/L Cd、Cr、Fe、Sb、Ca、Mg、Al、Mn、Sn、Bi等共存杂质元素对As、Zn、Co的测定结果基本无影响。As、Zn、Co的标准曲线线性相关系数均在0.9999以上,方法检出限为0.0021～0.026mg/L,方法定量限为0.0063～0.078mg/L。采用实验方法测定冶炼副产品硫酸镍实际样品中As、Zn、Co,所得结果的相对标准偏差(RSD,n=11)介于1.51%～2.77%之间,加标回收率在89.6%～108.4%之间。
The smelting by-product nickel sulfates are complicated in composition,so it is important to accurate analysis of the content of arsenic,zinc and cobalt for designing the purification process of nickel sulfate.The sample was pretreated by nitric acid-hydrochloric acid-hydrofluoric acid-perchloric acid system,and the working conditions of the instrument were optimized.A method for the determination of arsenic,zinc and cobalt in smelting by-product nickel sulfate by inductively coupled plasma-atomic emission spectrometry(ICP-AES)was established.In this experiment,As 189.042 nm,Zn 206.200 nm and Co 228.616 nm were used as analytical lines.The experimental results showed that the influence of 20 g/L nickel sulfate matrix,1 g/L copper and 20 mg/L cadmium,chromium,iron,antimony,calcium,magnesium,aluminum,manganese,tin,bismuth and other coexisting impurity elements coexisting impurity elements had little effect on the determination results of arsenic,zinc and cobalt.The linear correlation coefficients of standard curves of arsenic,zinc and cobalt were above 0.9999.The detection limit of the method was from 0.0021 mg/L to 0.026 mg/L,and the quantitative limit of the method was from 0.0063 mg/L to 0.078 mg/L.The arsenic,zinc and cobalt in the actual sample of nickel sulfate,a by-product of smelting,were determined by experimental method.The relative standard deviation(RSD,n=11)of the results were from 1.51%to 2.77%,and the recoveries were between 89.6%and 108.4%.
The smelting by-product nickel sulfates are complicated in composition,so it is important to accurate analysis of the content of arsenic,zinc and cobalt for designing the purification process of nickel sulfate.The sample was pretreated by nitric acid-hydrochloric acid-hydrofluoric acid-perchloric acid system,and the working conditions of the instrument were optimized.A method for the determination of arsenic,zinc and cobalt in smelting by-product nickel sulfate by inductively coupled plasma-atomic emission spectrometry(ICP-AES)was established.In this experiment,As 189.042 nm,Zn 206.200 nm and Co 228.616 nm were used as analytical lines.The experimental results showed that the influence of 20 g/L nickel sulfate matrix,1 g/L copper and 20 mg/L cadmium,chromium,iron,antimony,calcium,magnesium,aluminum,manganese,tin,bismuth and other coexisting impurity elements coexisting impurity elements had little effect on the determination results of arsenic,zinc and cobalt.The linear correlation coefficients of standard curves of arsenic,zinc and cobalt were above 0.9999.The detection limit of the method was from 0.0021 mg/L to 0.026 mg/L,and the quantitative limit of the method was from 0.0063 mg/L to 0.078 mg/L.The arsenic,zinc and cobalt in the actual sample of nickel sulfate,a by-product of smelting,were determined by experimental method.The relative standard deviation(RSD,n=11)of the results were from 1.51%to 2.77%,and the recoveries were between 89.6%and 108.4%.
引文
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[8]马荣锴,冯吉福,袁江涛.电感偶合等离子体发射光谱法(ICP-OES)测定卡林型金矿冶金样品中的金[J].矿产与地质,2017,31(1):194-198.
[9]成勇,敬守斌.电感耦合等离子体原子发射光谱法测定钒铝合金中15种杂质元素[J].理化检验-化学分册,2013,49(1):44-47.
[10]杨晓艳,杜钰娉.ICP-AES测定水稻不同部位12种元素的含量[J].光谱实验室,2011,28(4):1963-1965.
[11]龚昌合.ICP-AES测定工业硫酸镍中的12种元素[J].光谱实验室,2013,30(4):2016-2019.
[12]全国认证认可标准化技术委员会实验室认可分技术委员会(SAT/TC 261/SC 1).合格评定化学分析方法确认和验证指南:GB/T 27417-2017[S].北京:中国标准出版社,2017.
[13]潘霞,何静,王夏阳,等.铜电解脱铜后液除Ni并制取粗硫酸镍[J].矿冶工程,2016,36(6):79-83.
[2]陈松.用金川氧化钴系统萃余液制备电池工业用精制硫酸镍的研究[D].长沙:中南工业大学,1999:1-5.
[3]李伟.铜冶炼过程产粗硫酸镍精制及电池级硫酸镍制备研究[D].长沙:中南大学,2014:3-4.
[4]李伟,吴展,郭学益.粗硫酸镍溶液净化除杂试验研究[J].湿法冶金,2015,34(1):72-75.
[5]吴展,陈志友,侯琼英,等.从粗硫酸镍溶液中净化分离铁砷试验研究[J].湿法冶金,2013,32(2):122-124.
[6]全国化学标准化技术委员会无机化工分会.工业硫酸镍:HG/T2824-2009[S].北京:化学工业出版社,2010.
[7]姚佳,王莉丽,刘连利,等.ICP-OES法测定锦州某铁合金厂附近水、土壤、玉米中重金属含量[J].渤海大学学报(自然科学版),2007,28(3):230-234.
[8]马荣锴,冯吉福,袁江涛.电感偶合等离子体发射光谱法(ICP-OES)测定卡林型金矿冶金样品中的金[J].矿产与地质,2017,31(1):194-198.
[9]成勇,敬守斌.电感耦合等离子体原子发射光谱法测定钒铝合金中15种杂质元素[J].理化检验-化学分册,2013,49(1):44-47.
[10]杨晓艳,杜钰娉.ICP-AES测定水稻不同部位12种元素的含量[J].光谱实验室,2011,28(4):1963-1965.
[11]龚昌合.ICP-AES测定工业硫酸镍中的12种元素[J].光谱实验室,2013,30(4):2016-2019.
[12]全国认证认可标准化技术委员会实验室认可分技术委员会(SAT/TC 261/SC 1).合格评定化学分析方法确认和验证指南:GB/T 27417-2017[S].北京:中国标准出版社,2017.
[13]潘霞,何静,王夏阳,等.铜电解脱铜后液除Ni并制取粗硫酸镍[J].矿冶工程,2016,36(6):79-83.