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    微波消解-电感耦合等离子体原子发射光谱法测定催干剂中金属元素含量

    ICP-AES Determination of Metal Elements in Various Driers with Microwave Assisted Sample Digestion

    • 摘要: 应用电感耦合等离子体原子发射光谱法(ICP-AES)测定了不同种类催干剂中9种金属元素,即钴、锰、铅、钙、锌、钒、锆、镧和铈.样品置于聚四氟乙烯溶样罐中加入浓硝酸及高氯酸,盖紧罐盖后按预设程序分两步进行微波加热,加压消解,所得溶液稀释至一定体积供ICP-AES分析.对上述元素的谱线中选择合适的谱线作分析线,达到了9元素的同时测定.同混合标准溶液制备各元素的工作曲线,其线性范围均在100.0 mg·L-1以内.以一催干剂样品为基体,用标准加入法作回收试验,测得回收率在93.8%~109.9%之间,测定值的相对标准偏差(n=6)在0.11%~1.56%之间.不同来源的5个催干剂样品的分析结果表明所测得的金属元素的类别和含量显著差异.试验还证实所提出的方法具有操作快速、简单、方便,适合应用于日常分析工作.

       

      Abstract: Nine metal elements,i.e.,Co,Mn,Pb,Ca,Zn,V,Zr,La and Ce,in various driers were determined by ICP-AES.The drier sample was digested with conc.HNO3 and HClO4 in a closed PTFE vessel under pressure and heated by microwave in 2 steps.The solution obtained was diluted to a definite volume and used for ICP-AES analysis.Simultaneous determination of the 9 elements was achieved by choosing appropriate analytical spectral lines.Standard working curves were prepared by using mixed standard solution,giving ranges of linearity between values within 100.0 mg·L-1 for all these elements.On the base of a drier sample,test for recovery was made by addition of standard solution,and the values of recovery found were in the range of 93.8%-109.9%,with values of RSD′s (n=6) ranged from 0.11% to 1.56%.As shown by the results of analysis of 5 driers from various sources,kinds and contents of metal elements found were quite different.It was also proved that the proposed method is rapid,convenient and easy in operation and is feasible for routine analysis.

       

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