双向观测-电感耦合等离子体发射光谱法测定湿法炼锌浸出液中的多种元素  

Bidirectional observation-inductively coupled plasma emission spectrometry method for determination of various elements in leaching solution of zinc hydrometallurgy

作　　者：龙兴杰 闵娇 刘传仕 魏巍 阳俊成 Long Xingjie;Min Jiao;Liu Chuanshi;Wei Wei;Yang Junchengn(Yun-Tin Wenshan Zinc Indium Smelting Co.,Ltd.,Wenshan,Yunnan 663700,China)

机构地区：[1]云锡文山锌铟冶炼有限公司,文山663700

出　　处：《分析仪器》2024年第2期20-27,共8页Analytical Instrumentation

摘　　要：湿法炼锌浸出液中Zn、In、Fe、Cu、Cd、Mg、Co、Mn、As、Si、Sb、Ge元素的含量多采用滴定法、分光光度法、火焰原子吸收法、原子荧光法、示波极谱法等经典分析方法来测定,一般较难实现多元素同时分析,且存在分析流程长、操作繁琐、检测结果时效性差的弊端。本实验建立了样品不经预处理,在3%(V/V)的硝酸介质中,在仅仅只绘制两条校准曲线的情况下,充分利用双向观测-电感耦合等离子体发射光谱法(ICP-OES)径向观测线性范围宽、基体效应小的特点来测定湿法炼锌浸出液中浓度水平在0.50g/L~150g/L的Zn、Fe、Mg、Mn、Cu;利用该法轴向观测灵敏度高、检出限低的特点来测定湿法炼锌浸出液中浓度小于0.50g/L的In、Fe、Cu、Cd、Co、As、Si、Sb、Ge。该方法操作简单,分析结果时效性强,各元素的测定结果与滴定法、分光光度法、火焰原子吸收法、原子荧光法、示波极谱法测得值相符,该法各元素的检出限在0.0009μg/mL~0.079μg/mL之间,相对标准偏差在0.30%~1.81%之间,加标回收率均在90.0%~107.0%之间,能较好的应用于湿法炼锌浸出液中主元素及杂质元素的测定。The content of Zn,In,Fe,Cu,Cd,Mg,Co,Mn,As,Si,Sb,Ge elements in the leaching solution of zinc hydrometallurgy is often determined using classic analysis methods such as titration,spectrophotometry,flame atomic absorption,atomic fluorescence,and oscillopolarography.It is generally difficult to achieve simultaneous analysis of multiple elements,and there are drawbacks such as long analysis process,cumbersome operation,and poor timeliness of detection results.A method is established for the determination of Zn,Fe,Mg,Mn,Cu in zinc hydrometallurgy leaching solution at concentrations ranging from 0.50g/L to 150g/L without pre-treatment of the sample in a 3%(V/V)nitric acid medium,using only two calibration curves and fully utilizing the characteristics of wide linear range and small matrix effect of bidirectional observation inductively coupled plasma emission spectroscopy(ICP-OES)radial observation.Using the characteristics of high axial observation sensitivity and low detection limit of this method to determine In,Fe,Cu,Cd,Co,As,Si,Sb,Ge with a concentration less than 0.50g/L in the zinc leaching solution of hydrometallurgy.The determination results of each element are consistent with the values measured by titration,spectrophotometry,flame atomic absorption spectrometry,atomic fluorescence spectrometry,and oscillopolarography.The detection limit of each element in this method is between 0.0009g/mL and 0.079g/mL,the relative standard deviation is between 0.30%and 1.81%,and the recovery rate of the added standard is between 90.0%and 107.0%.This method is simple to operate and has strong timeliness in the analysis results.

关 键 词：双向观测 电感耦合等离子体发射光谱 湿法炼锌 浸出液 

分 类 号：O657.31[理学—分析化学] TF813[理学—化学]