微波消解-氢化物发生原子荧光光谱法测定锌渣中硒  

Determination of selenium in zinc slag by hydride generation atomic fluorescence spectrometry with microwave digestion

作　　者：魏军 胡艳巧 刘爱琴 李丹 刘俊妙 陈超 WEI Jun;HU Yanqiao;LIU Aiqin;LI Dan;LIU Junmiao;CHEN Chao(Hebei Research Center for Geoanalysis,Baoding 071052,China)

机构地区：[1]河北省地质实验测试中心,河北保定071052

出　　处：《冶金分析》2023年第12期67-72,共6页Metallurgical Analysis

基　　金：河北省地质勘查局项目(454-0601-YBN-DONH)。

摘　　要：锌渣中硒的准确测定对其回收利用有重要意义。采用HNO3-HClO4-HF-H2SO4体系微波消解样品,将样品溶液于电热板上蒸至剩余2~3 mL后用王水(1+1)浸提,建立了氢化物发生原子荧光光谱法(HG-AFS)对锌渣中硒测定的方法。实验表明,硒质量浓度在2~16μg/L范围内与其对应的荧光强度呈良好的线性关系,相关系数为0.999 7,方法检出限为0.01μg/g,定量限为0.03μg/g。对大量锌渣样品中共存元素的含量进行统计分析,发现锌渣中主要成分有铁、锌、铅、铝,干扰试验表明,这些共存元素对测定的干扰可忽略。按照实验方法对3个不同硒含量的锌渣样品进行精密度和加标回收试验,硒测定结果的相对标准偏差(RSD,n=12)为1.2%~2.0%,加标回收率为93%~101%。对硒质量分数为2.35~100μg/g的锌渣样品中硒进行测定,测定结果与碱熔-HG-AFS结果基本一致。The accurate determination of selenium in zinc slag is of great significance for its recycle.The sample was treated with HNO3-HClO4-HF-H2SO4 system by microwave digestion.Then the sample solution was steamed on the electric heating plate until the volume remained 2-3 mL followed by extraction with aqua regia.Consequently,a method for determination of selenium in zinc slag was established by hydride generation atomic fluorescence spectrometry(HG-AFS).The results showed that the mass concentration of selenium in range of 2-16μg/L had a good linear relationship with its corresponding fluorescence intensity.The correlation coefficient was 0.9997.The limit of detection of the method was 0.01μg/g,and limit of quantification was 0.03μg/g.The statistical analysis of coexisting elements contents in a large number of zinc slag samples was conducted.It was found that the main components in zinc slag were iron,zinc,lead,and aluminum.The interference tests indicated that the coexisting elements in samples had no interference with the determination.Three zinc slag samples with different contents of selenium were used for tests of precision and recovery according to the proposed method.The relative standard deviations(RSD,n=12)of the determination results were between 1.2%and 2.0%,and the recoveries were between 93%and 101%.The content of selenium in zinc slag samples with mass fraction of 2.35-100μg/g was determined,and the results were basically consistent with those obtained by HG-AFS with alkali fusion.

关 键 词：固体废物 锌渣 硒 微波消解 氢化物发生原子荧光光谱法(HG-AFS) 

分 类 号：O657.31[理学—分析化学] X705[理学—化学]