摘要
建立了王水溶矿-电感耦合等离子体发射光谱法测定砷矿石和锑矿石中主、次量元素砷、锑、硫及含量范围在100μg/g以上的铜、铅、锌等元素的方法。研究了放置时间、溶液酸度、氧化剂与络合剂对砷、锑、硫及其他元素测定的影响。不同王水浓度酸度对可同时测定的其他元素的影响不明显;当溶液酸度较小时,不能放置,应及时测定;如需放置,应在溶液定容前加入酒石酸防止水解。样品中砷、锑、硫的含量在0.74%～39.7%时,相对误差(RE)在-0.17%～7.74%,5次独立测定的相对标准偏差(RSD)均小于2%;含量在100～500μg/g以下的Sb,RE在-2.5%～4.79%,5次独立测定的RSD均小于2%。由于稀释倍数较大(DF=1000),不能准确测定含量在100μg/g以下的铜、铅、锌;含量在100μg/g以上的铜、铅、锌的RE在-10.3%～10.3%,5次独立测定的RSD基本小于5%。经标准物质验证获得满意结果。方法也可应用于砷、锑含量较高的硫化矿的测定。
The method for determining concentrations of As,Sb,S,and Cu,Pb,Zn which are above 100 μg/g,within arsenic ore and stibium ore by inductively coupled plasma-atomic emission spectrometry（ICP-AES）with aqua regia digestion is reported in this paper.The experimental conditions such as placement time,solution acidity,and the influence of oxidant and complexing agents on As,Sb,S and the other elements were studied.The relative error（RE） was determined to be between-0.17% and 7.74% with a RSD（n=5） of 2% if the concentrations of As,Sb,S in the samples were in the range of 0.74-39.7%.However,the RE was from-2.5% to 4.79% and RSD（n=5） was 2% if the Sb concentration is lower than 100-500 μg/g.The RE was determined to be between-10.3% and 10.3% with a RSD（n=5） of generally less than 5% if the Cu,Pb and Zn concentrations were more than 100 μg/g.No accurate data were obtained for Cu,Pb and Zn if the concentrations were lower than 100 μg/g,limited by the large dilution factor of 1 000.The accuracy and precision of the method were validated by reference materials.
出处
《岩矿测试》
CAS
CSCD
北大核心
2011年第2期190-194,共5页
Rock and Mineral Analysis
基金
国家地质实验测试中心基本科研业务费项目资助(2009CSJ04)
关键词
多元素测定
砷矿石
锑矿石
电感耦合等离子体发射光谱法
王水溶矿
multi-elements determination
arsenic ore
stibium ore
inductively coupled plasma-atomic emission spectrometry
aqua regia digestion
