微波消解-电感耦合等离子体原子发射光谱法测定锌精矿中锑  

Determination of antimony in zinc concentrate by inductively coupled plasma atomic emission spectrometry with microwave digestion

作　　者：李海[1] LI Hai(Hebei Mining Bureau Fifth Brigade Tangshan Experimental Test Institute, Tangshan 063000, China)

机构地区：[1]河北省地矿局第五地质大队唐山实验测试所

出　　处：《冶金分析》2019年第6期29-33,共5页Metallurgical Analysis

摘　　要：在锌的冶炼过程中,为了防止“烧板”现象,需要快速检测锌精矿中锑元素含量。采用硝酸、氢氟酸微波消解样品,消解结束后加入硫酸,用赶酸仪赶氢氟酸,选择Sb217.582nm为分析谱线,采用基体匹配法绘制校准曲线消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定锌精矿中锑。锌质量浓度为0.05~200mg/L时与其发射强度呈线性关系,相关系数为0.9996;方法检出限为0.003%(质量分数,下同),测定下限为0.01%。按照实验方法测定锌精矿样品中锑,结果的相对标准偏差(RSD,n=12)为1.7%;加标回收率为98%~99%。按照实验方法测定4个锌精矿样品中锑,测定结果与氢化物发生-原子荧光光谱法或硫酸铈滴定法的测定结果一致。In the process of zinc smelting, the content of antimony in zinc concentrate should be rapidly detected in order to prevent the “burning plate” phenomenon.The sample was treated with nitric acid and hydrofluoric acid by microwave digestion. Sulfuric acid was added after digestion to remove hydrofluoric acid with the acid catcher. Sb 217.582 nm was selected as the analytical line. The influence of matrix effect was eliminated by preparing calibration curve with matrix matching method. The content of antimony in zinc concentrate was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The mass concentration of antimony in range of 0.05-200 mg/L was linear to its corresponding emission intensity with correlation coefficient of 0.999 6. The detection limit of method was 0.003%(mass fraction, the same below) and the low limit of determination was 0.01%. The content of antimony in zinc concentrate sample was determined according to the experimental method. The relative standard deviation (RSD, n =12) of the determination results was 1.7%. The spiked recoveries were between 98% and 99%. The proposed method was applied for determination of antimony in four zinc concentrate samples, and the found results were consistent with those obtained by hydride generation-atomic fluorescence spectrometry (HG-AFS) or cerium sulfate titration.

关 键 词：微波消解 电感耦合等离子体原子发射光谱法(ICP-AES) 锌精矿 锑 

分 类 号：O657.31[理学—分析化学]