原子荧光光谱法测定硫化钠溶液中的砷  

Determination of Arsenic in Sodium Sulfide Solution by Atomic Fluorescence Spectrometry

作　　者：李伟[1] 李颖 赵有刚[1] 李玉昆 刘群 LI Wei;LI Ying;ZHAO Yougang;LI Yukun;LIU Qun(Jinchuan Group Co.,Ltd.Testing Center,Jinchang 737100,China)

机构地区：[1]金川集团股份有限公司检测中心,甘肃金昌737100

出　　处：《化工管理》2024年第23期57-61,共5页Chemical Management

摘　　要：砷元素作为镍电解系统溶液中重要的控制指标之一,其含量的高低影响镍板的品级率。通常在镍系统净化的除铜工序中加入大量硫化钠溶液作为沉淀剂,除去溶液中的铜,为避免硫化钠溶液引入过量的砷,需要对硫化钠溶液中砷含量进行分析。文章以碘单质为氧化剂,氧化硫化钠溶液中的二价硫离子,形成硫单质,过滤除去沉淀,建立了原子荧光法测定硫化钠溶液中砷的分析方法。文章进行了碘离子、碘单质、钠离子对砷测定的影响试验,确定了碘、盐酸、硫脲-抗坏血酸混合溶液的用量,以盐酸作载液、硼氢化钾作还原剂,采用原子荧光光谱法测定样品中砷含量。工作曲线线性范围在0~50μg/L时,相关系数可达到0.9995以上,相对标准偏差在6.55%~8.25%之间,加标回收率在85.0%~109.0%之间,满足分析要求。As one of the important control indexes in the solution of nickel electrolytic system,arsenic content affects the grade rate of nickel plate.A large amount of sodium sulfide solution is usually added in the copper removal process of nickel system purification as a precipitator to remove copper in the solution.In order to avoid excessive arsenic introduced into the sodium sulfide solution,arsenic content in the sodium sulfide solution needs to be analyzed.In this paper,an analytical method for the determination of arsenic in sodium sulfide solution by atomic fluorescence method has been established by using iodine as an oxidant to oxidize the divalent sulfur ion in sodium sulfide solution.In this paper,the effects of iodide,iodide and sodium ions on the determination of arsenic were tested,and the dosage of iodine,hydrochloric acid,thiourea-ascorbic acid mixed solution was determined.The content of arsenic in the sample was determined by atomic fluorescence spectrometry with hydrochloric acid as carrier and potassium borohydride as reducing agent.When the linear range of the working curve is 0~50μg/L,the correlation coefficient can reach above 0.9995,the relative standard deviation is 6.55%~8.25%,and the recoveries are 85.0%~109.0%,meeting the requirements of analysis.

关 键 词：原子荧光光谱法 硫化钠 砷 

分 类 号：O65[理学—分析化学]