光谱法耦合增敏剂降低铜冶炼烟尘中微量铟检出限的研究  

Study on the Coupling of Spectral Method With Sensitizer to Reduce the Detection Limit of Trace Indium in Copper Smelting Dust

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作  者:屈伟 李子尚 李倩 张红致[1,2] QU Wei;LI Zi-shang;LI Qian;ZHANG Hong-zhi(GRINM Resources and Environment Tech.Co.,Ltd.,Beijing 101400,China;National Engineering Research Center for Environment-Friendly Metallurgy in Producing Premium Non-Ferrous Metals,Beijing 101400,China)

机构地区:[1]有研资源环境技术研究院(北京)有限公司,北京101400 [2]高品质有色金属绿色特种冶金国家工程研究中心,北京101400

出  处:《光谱学与光谱分析》2025年第5期1319-1324,共6页Spectroscopy and Spectral Analysis

基  金:国家重点研发计划项目(2022YFC3900800)资助。

摘  要:对于铜冶炼烟尘中微量铟的测定,标准方法采用火焰原子吸收光谱法,铟含量的测定范围为0.0200%~0.100%,无法实现铟含量低于0.0200%的测定。对于铟含量低于0.0200%的测定,参照国家标准《锌精矿化学分析方法》,但测试过程中需要用乙酸丁酯萃取微量的铟,再用盐酸溶液反萃,步骤繁琐、操作复杂、分析费时,不能快速配合选矿、冶金的科学研究。文章研究了在盐酸介质中,表面活性剂曲拉通X-100(OP)存在下,光谱法耦合增敏剂丙酮(Ac),降低了铜冶炼烟尘中微量铟的检出限。机理研究发现:在一定条件下,铟离子、丙酮和和曲拉通X-100形成三元配合物,对铟的原子吸收光谱产生协同增敏效应,改善了铟原子吸收光谱的强度,增加了其灵敏度。运用多元线性回归分析拟合出吸光度(A)与铟(In)、丙酮(Ac)和曲拉通X-100(OP)的浓度关系,运用多元线性回归分析求极值法,计算出三元配合物的摩尔比为1∶1∶2。此外,还研究了火焰原子吸收光谱法测定铟的特征光谱,丙酮和曲拉通X-100的加入量,酸种类的选择及加入量,乙炔流量,共存离子的影响等,并用萃取法进行对照实验,分析结果进行数理统计,得出结论:该研究具有良好的准确度和精密度,可用于铜冶炼烟尘中微量铟的分析检测;用试剂空白进行方法的检出限测定,在置信度为99%时,方法的检出限为0.0010%,比行业标准方法低20倍。For the determination of trace indium in copper smelting dust,the standard method adopts flame atomic absorption spectroscopy,and the determination range of indium content is 0.0200%~0.100%,which cannot achieve the determination of indium content below 0.0200%.To determine indium content below 0.0200%,reference is made to the national standard“Chemical Analysis Method for Zinc Concentrates”.However,during the testing process,trace amounts of indium need to be extracted with butyl acetate and back extracted with hydrochloric acid solution.The steps are cumbersome,the operation is complex,and the analysis is time-consuming,which cannot be quickly combined with scientific research in mineral processing and metallurgy.This article studies the coupling of spectroscopy with sensitizer acetone(Ac)in the presence of surfactant Triton X-100(OP)in a hydrochloric acid medium,which suppresses the interference of lead,zinc,copper,bismuth,and other elements and reduces the detection limit of trace indium in copper smelting dust.Mechanism studies have found that under certain conditions,indium ions,acetone,and Triton X-100 form ternary complexes,which synergistically enhance the atomic absorption spectra of indium,improve the intensity of indium atomic absorption spectra,and increase their sensitivity-using multiple linear regression analysis to fit the concentration relationship between absorbance(A)and indium(In),acetone(Ac).The P values of cIn,cAc and cOp in the fitting results are all less than 0.05,indicating that the three significantly impact absorbance.Using multiple linear regression analysis to find the extremum method,the molar ratio of the ternary complex was calculated to be 1∶1∶2.In addition,this article studied the spectral characteristics of indium determined by flame atomic absorption spectroscopy,the additional amount of acetone and Triton X-100,the selection and addition amount of acid types,acetylene flow rate,and the influence of coexisting ions.Comparative experiments were conducted using the extra

关 键 词:光谱法  三元配合物 检出限 协同增敏效应 

分 类 号:O657.3[理学—分析化学]

 

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