微波消解-等离子体发射光谱法测定含铜物料中9种组分

Inductively Coupled Plasma-Atomic Emission Spectrometric Determination of 9 Components in Materials Containing Copper with Microwave-assisted Digestion

含铜物料经盐酸-硝酸-氢氟酸混合酸在高压密闭容器中微波消解,电感耦合等离子体发射光谱法测定样品中的银、砷、铅、镉、锌、三氧化二铝、氧化钙、氧化镁、锰9种组分。对溶样试剂、微波消解条件、基体干扰进行了相关讨论。建立的溶样方法快速简单,矿样溶解完全;方法基体效应小,各待测元素之间没有明显干扰,待测元素回收率在93.3%～103.2%,方法测定下限在5～60μg/g,相对标准偏差(RSD,n=11)为0.5%～3.1%。使用建立的方法分析国家标准物质和实际样品,分析结果与标准值、其他常规方法测定值一致,在允许的误差范围内。与现行的分析方法相比,该法缩短了分析周期,适合大批量试样的分析,并已应用于实际的检验工作。

The materials containing copper were prepared by microwave assisted dissolution in a pressurized vessel with a mixture of HCl-HNO3-HF.Nine components in sample solution including silver,arsenic,lead,cadmium,zinc,alumina,calcium oxide,magnesium oxide and manganese are determined by inductively coupled plasma-atomic emission spectrometry（ICP-AES）.The sample could be quickly and completely dissolved.The effects of sample dissolving regents,microwave digestion conditions and matrix interference are discussed.The matrix effect of this method is small.There is no evident interference among testing elements.The recovery of this method is 93.3%-103.2%.The quantification lower limits of this method for nine components are 5-60 μg/g,and the relative standard deviation（n=11） are 0.5%-3.1%.The method is applied in the determination results of certified reference materials and actual sample and the results are in good agreement with the certified values and those obtained by other conventional methods.Compared with the currently used method,this method shortens the analysis period.The proposed method meets the requirement for commodity inspection and has been applied to routine inspection.