沉淀分离-氢化物发生原子荧光光谱法测定铜冶炼工业废水中砷  

Determination of arsenic in industrial wastewater of copper smelting by precipitation separation hydride generation atomic fluorescence spectrometry

作　　者：郭晶 冯媛 张倩 程思敏 刘艳 GUO Jing;FENG Yuan;ZHANG Qian;CHENG Simin;LIU Yan(Daye Nonferrous Design&Research Institute Co.,Ltd.,Huangshi 435000,China)

机构地区：[1]大冶有色设计研究院有限公司,湖北黄石435000

出　　处：《冶金分析》2023年第11期57-61,共5页Metallurgical Analysis

摘　　要：砷是一种剧毒物质,建立测定铜冶炼工业废水中砷的方法具有重要意义。铜冶炼工业废水中铜、铁、锌等盐分含量较高、基体复杂,采用HJ 694—2014中原子荧光光谱法测定时,会污染仪器管道、堵塞雾化器,同时存在记忆效应。本文以盐酸、硝酸将样品于80℃水浴中消解,用氢氧化镧共沉淀法对砷进行分离富集,以盐酸溶解沉淀,建立了沉淀分离-氢化物发生原子荧光光谱法(HG-AFS)测定铜冶炼废水中砷的方法,解决了仪器管道污染、雾化器堵塞和记忆效应等问题。实验表明,砷质量浓度在2.0~10.0μg/L范围内与其对应的荧光强度呈线性关系,相关系数为0.999 8,方法检出限为0.027μg/L。干扰试验表明,样品中的共存元素对测定无干扰。将实验方法应用于3个铜冶炼废水样品中砷含量的测定,并分别进行5次加标回收试验,测定结果的相对标准偏差(RSD,n=5)为2.0%~3.6%,回收率在97%~108%之间。按实验方法对铜冶炼废水样品中砷进行沉淀分离后测定,测得结果与标准HJ 694—2014基本一致。Arsenic is a highly toxic substance,and it is of great significance to establish a method for the determination of arsenic in industrial wastewater from copper smelting.The contents of salts such as copper,iron and zinc in industrial wastewater of copper smelting are high,and meanwhile,the matrix is complex.During the determination by atomic fluorescence spectrometry in HJ 694-2014,the sample will pollute the instrument pipeline and block the atomizer.Moreover,there is memory effect.In this study,the sample was digested with hydrochloric acid and nitric acid in water bath at 80℃.Arsenic in sample was separated and enriched by lanthanum hydroxide co-precipitation method.Then the precipitate was dissolved with hydrochloric acid.The method for the determination of arsenic in industrial wastewater of copper smelting by precipitation separation hydride generation atomic fluorescence spectrometry(HG-AFS)was established.The problems of instrument pipeline pollution,atomizer blocking and memory effect were solved.The results showed that the mass concentration of arsenic in range of 2.0-10.0μg/L had linear relationship with the corresponding fluorescence intensity.The correlation coefficient was 0.9998,and the limit of detection of method was 0.027μg/L.The interference tests showed that the coexisting elements in sample had no interference with the determination.The proposed method was applied for the determination of arsenic content in three wastewater samples from copper smelting.Moreover,the standard addition tests were conducted for five times.The relative standard deviations(RSD,n=5)of the measured results were 2.0%-3.6%,and the recoveries were 97%-108%.Arsenic in wastewater samples of copper smelting was determined after precipitation separation according to the experimental method,and the measured results were basically consistent with those obtained by standard HJ 694-2014.

关 键 词：沉淀 水浴消解 氢化物发生 原子荧光光谱法(HG-AFS) 砷 铜冶炼工业废水 

分 类 号：O657.31[理学—分析化学] TF03[理学—化学] TF811[冶金工程—冶金物理化学]