摘要: |
运用电感耦合等离子体发射光谱法(Inductively Coupled Plasma-Optical Emission Spectrometry,ICP-OES) 比较研究了干法灰化、湿法消解和微波消解3 种前处理方法对海带样品中 Se、Fe、Mn、Zn、Ca、Mg、P、As、Cd、Cr、Cu 和 Pb 12 种元素含量测定的影响。结果表明, 不同前处理方法对微量元素的测定结果会产生不同程度的影响。干法灰化对易挥发元素 As 等带来明显的负误差; 湿法消解由于加入的消解液量大, 对低含量的微量元素常带来较大的试剂空白; 微波消解法相对于其他两种前处理方法适于样品的快速消解, 具有操作简便、试剂用量少、操作误差小等优点, 检测结果具备较高的准确度、精密度和回收率, 对海带样品微波消解 ICP-OES 检测的相对标准偏差为0.29%~2.63%, 加标回收率为 87.3%~103.6%。微波消解是海带等海洋生物样品中微量元素测定较理想的前处理方法。 |
关键词: 微波消解 干法灰化 湿法消解 比较 电感耦合等离子体发射光谱法 |
DOI:10.11759/hykx20130818001 |
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Comparison of three pretreatment methods for the determination of 12 elements in Thallus laminariae by ICP-OES |
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Abstract: |
Three sample pretreatment methods, including dry ashing, wet and microwave digestion, had been compared in determination of 12 elements (Se, Fe, Mn, Zn, Ca, Mg, P, As, Cd, Cr, Cu and Pb) in Thallus laminariae by inductively coupled with plasma-optical emission spectrometry (ICP-OES). The results indicated that different digestion methods had some influences on the results of the determined elements. Dry ashing had obvious negative deviation on the volatile elements, such as As. Because adding more digestion reagents, wet digestion had larger reagent blank for low content trace elements. Compared to dry ashing and wet digestion, microwave digestion was a rapid and efficient method for sample decomposition, offering more significant advantages, such as more convenient, less acid consuming and good precision, accuracy and recovery rate. The relative standard deviations of determination for trace elements by ICP-OES after microwave digestion were between 0.29%~2.63% and the recovery rates were in the range of 87.3%~103.6%. Microwave digestion was proved to be suitable for pretreating T. laminariae as well as other marine biological samples. |
Key words: microwave digestion dry ashing wet digestion comparison ICP-OES |