电感耦合等离子体发射光谱法测定铅锌矿中15个主次量元素

Simultaneous Determination of 15 Elements in Lead-Zinc Ore by Inductively Coupled Plasma-Atomic Emission Spectrometry

铅锌矿多元素同时测定中,样品预处理过程受多种不同因素的影响,单因素试验往往无法同时为多因素实验提供合理的优化方案。本文采用盐酸-硝酸溶矿,考察了样品预处理过程中混合酸配比、混合酸体积、消解时间及消解温度对消解效果的影响,利用正交试验设计及极差分析确定了最优消解条件：盐酸-硝酸混合酸配比3∶1,混合酸体积10 m L,消解时间120 min,消解温度90℃,用电感耦合等离子体发射光谱法同时测定铅锌矿中15个主次量元素（铅锌铜锰砷银铋镉钴镍镓铟钼锗锑）的含量。在最优条件下,用富铅锌矿石国家标准物质（GBW 07165）进行试验,大多数元素的精密度（RSD,n=12）和准确度小于5%,方法检出限为0.0019~0.048μg/g。基于铅锌矿主要是以硫化物形式存在,采用一系列硫化物国家标准物质验证方法的准确度及可行性,检测结果基本都在标准值的误差范围内。应用该方法分析湖南某矿区中大批量铅锌矿样品,标样质量统计合格率为100%,密码质量统计合格率大于97%。

The process of sample preparation is affected by many different factors in multi-element determination for lead-zinc ore.However,single-factor experiment design cannot provide a reasonable solution for the simultaneous optimization of multiple-factor experiments.In this study,minerals were dissolved by hydrochloric acid-nitric acid.The effect of digestion conditions was studied.Ratio and volume of the mixed acids as well as time and temperature of the digestion were optimized by orthogonal test and range analysis.The conditions of digestion were optimized as：ratio and volume of the mixed acids at 3 ∶ 1 and 10 m L,respectively,time and temperature of the digestion of 120 min and 90℃,respectively.The contents of 15 major and trace elements（Pb,Zn,Cu,Mn,As,Ag,Bi,Cd,Co,Ni,Ga,In,Mo,Ge and Sb） were determined simultaneously by Inductively Coupled Plasma Atomic Emission Spectrometry（ICP-AES）.Under optimal conditions,the method was verified by certified national reference material GBW 07165.The results show that the precision（RSD,n = 12） and accuracy are less than 5% for most elements,and the detection limit is 0.0019- 0.048 μg / g.In addition,as the lead-zinc ore usually exits in the form of sulfide,the accuracy and feasibility of the method can be verified by a series of national standard sulfide materials.The results were consistent with the certified values within uncertainties.After using the proposed method to analyze large quantities of lead-zinc ore samples collected from Hunan,the qualification rates for standard samples and blind samples are 100% and 97%,respectively.This method optimizes the experimental conditions,and solves the complex problem of sample pretreatment.The method has many advantages,including low consumption of reagents,green environment and simultaneous determination of multi-elements,which indicates that it is an accurate and practical method to simultaneously determine the content of lead and zinc.