基体分离-电感耦合等离子体原子发射光谱(ICP-AES)法测定精铋中10种杂质元素  

Determination of Ten Impurity Elements in Refined Bismuth by Inductively Coupled Plasma Atomic Emission Spectrometry with Separating Matrix

作　　者：孔会民 董更福 王景凤 岳萍 KONG Huimin;DONG Gengfu;WANG Jingfeng;YUE Ping(Technology Development of Western Mining Group Co.,Ltd.,Xining,Qinghai 810000,China)

机构地区：[1]西部矿业科技发展有限公司,西宁810000

出　　处：《中国无机分析化学》2021年第3期71-74,共4页Chinese Journal of Inorganic Analytical Chemistry

基　　金：青海省重大科技专项(2018-GX-A7)。

摘　　要：采用电感耦合等离子体原子发射光谱(ICP-AES)法测定精铋中Cd、Co、Cu、Fe、Mg、Mn、Ni、Pb、Ti、Zn等十种杂质元素,样品用优级纯硝酸溶解,往60℃左右的溶液中,滴加氨水(1+1),控制pH值在3.0~4.0。考察了温度、酸度、沉降时间对铋的去除率和对检测结果的影响。根据分析线的选择原则,结合待测元素的检测范围,选择无干扰、峰形对称、灵敏度适中的谱线作为分析线(Cd 228.802 nm、Co 237.862 nm、Cu 324.754 nm、Fe 259.940 nm、Mg 279.553 nm、Mn 257.610 nm、Ni 231.604 nm、Pb 182.205 nm、Ti 323.452 nm、Zn 213.856 nm)。各元素的质量浓度在一定范围内与其发射强度呈线性,校准工作曲线的线性相关系数均大于0.9997,各元素检出限为0.002~0.253μg/g。按照实验方法测定精铋实际样品,结果的相对标准偏差(RSD,n=9)为2.5%~9.8%,加标回收率为95.1%~102%,满足检测要求。Ten impurity elements(Cd,Co,Cu,Fe,Mg,Mn,Ni,Pb,Ti,Zn)in fine bismuth were determined by inductively coupled plasma emission spectrometry.The sample was dissolved in pure high-grade nitric acid.Ammonia water(1+1)was added to the solution at about 60℃,and the pH value was controlled at 3.0~4.0.The effects of temperature,acidity and settling time on the removal rate and the test results were investigated.According to the selection principle of the analysis line and the detection range of the element to be tested,the spectral line with no interference,symmetrical peak shape and moderate sensitivity was selected as the analysis line(Cd 228.802 nm,Co 237.862 nm,Cu 324.754 nm,Fe 259.940 nm,Mg 279.553 nm,Mn 257.610 nm,Ni 231.604 nm,Pb 182.205 nm,Ti 323.452 nm and Zn 213.856 nm)The mass concentration of each element is linear with its emission intensity within a certain range,and the linear correlation coefficient of the calibration curve is all greater than 0.9997.The detection limit of each element of the method is 0.002—0.253μg/g.The relative standard deviation(RSD,n=9)is 2.5%—9.8%,and the standard recovery is 95.1%—102%.The method meets test requirements.

关 键 词：基体分离 电感耦合等离子体原子发射光谱法(ICP-AES) 镉 钴 铜 铁 镁 锰 镍 铅 钛 锌 

分 类 号：O657.31[理学—分析化学] TH744.11[理学—化学]