摘要
采用均匀设计与正交设计联用,优化电感耦合等离子发射光谱法测定铅锌矿石中锌、铜、砷、铁含量的微波消解样品条件.在微波功率为800 W的条件下,以测定结果的回收率和相对标准偏差为指标,对试样量、盐酸和硝酸体积比、微波消解时间、微波消解最高温度4个因素进行均匀设计,并在此基础上选取因素水平范围进行正交试验,优选最佳微波消解条件:称样质量为0.2 g,盐酸和硝酸体积比为3:1,微波消解时间为45 min,微波消解最高温度为175℃.在该消解条件下进行实验,方法回收率为95.2%~98.6%,测定结果的相对标准偏差为0.10%~0.16%(n=6).对该实验条件参数进行稳健性试验,结果表明该方法稳定可行.该方法准确、可靠,可用于矿石中锌、铜、砷、铁含量的测定.
The conditions of microwave digestion pretreatment for determination of zinc,copper,arsenic and iron in lead –zinc ore by inductively coupled plasma emission spectrometry were optimized by using combination of uniform design and orthogonal design. Under the condition of the microwave power of 800 W,recovery and relative standard deviation of the determination results were used as index,uniform design was carried out for four factors of the sample quantity,the volume ratio of hydrochloric acid–nitric acid,the time of microwave digestion,and the highest temperature of microwave digestion,then the horizontal range of factors was selected for orthogonal test. The optimum conditions for microwave digestion: the mass of the sample was 0.2 g,the volume ratio of hydrochloric acid–nitric acid was 3∶1,the time of microwave digestion was 45 min,and the highest temperature of microwave digestion was 175 ℃. The experimental design under this condition shows that the recovery of the method was 95.2%–98.6%,and the relative standard deviation of determination results was 0.10%–0.16%(n=6). The robustness test of the experimental parameters was carried out,the experimental results showed that the method was stable and feasible. The method is accurate and reliable,and can be used to determine the contents of zinc,copper,arsenic and iron in lead –zinc ore.
作者
洪颖
吴桐彬
王金陵
朱园园
张跃
唐晨
HONG Ying;WU Tongbin;WANG Jinling;ZHU Yuanyuan;ZHANG Yue;TANG Chen(Technology Center of Nanjing Inspection and Quarantine, Nanjing 210046, China;Jiangsu Yangzi Inspection Certification Co., Ltd., Nanjing 210046, China)
出处
《化学分析计量》
CAS
2019年第5期99-103,共5页
Chemical Analysis And Meterage
关键词
微波消解
正交设计
均匀设计
稳健性试验
铅锌矿石
microwave digestion
uniform design
orthogonal design
robustness test
lead-zinc ore
作者简介
通讯作者:王金陵,理学学士,从事有毒有害物质检测,E-mail:wjl3651667@sina.com.
