摘要
超高通量密闭微波消解法比干法灰化、湿法消解酸用量少、消解效率高,也比普通的微波消解法承压能力高,并且能同批次处理多达70个样品,大大提升了实验效率。而ICP-MS分析技术的检出限低、干扰少、精密度高,并且可以进行十几种微量元素的同时快速测定。将两种技术有机结合,建立了超高通量密闭微波消解-ICP-MS方法,对木质废弃物、秸秆、樟子松、红松、花生壳5种生物质燃料样品进行前处理,并测定各个样品中Cr、Mn、Co、Ni、Cu、Zn、As、Mo、Cd、Ba、Pb等11种微量元素含量。各元素的检出限为0.0007～0.2430μg/g,相对标准偏差基本低于5%,加标回收率为86.4%～113%。将超高通量密闭微波消解法与传统的电烘箱加热-高压密封罐消解法进行比较,结果表明,两种前处理方法测定的元素含量并无显著性差异,微波消解法比高压密封罐消解法操作简便、耗时短、消解效率高、酸用量少、对环境污染小且实验成本低,更适合大批量样品分析的前处理。微波消解法结合ICP-MS分析技术,可以对生物质燃料样品中的微量元素含量进行高效、快速、准确的分析。
Ultra-high throughout closed microwave digestion has higher digestion efficiency with less acid consumption than dry ashing and wet digestion,and also has higher loading capacity than the ordinary microwave digestion method.The method can digest up to 70 samples in a single batch,which greatly enhances the efficiency of the experiment.With low limit of detection,small interference and high precision,the ICP-MS technique can determine more than a dozen trace elements simultaneously.In this paper,the two techniques are combined as the ultra-high throughout closed microwave digestion-ICP-MS method to pretreat samples of five solid biofuels,including wood wastes,stalks,Scots pine（Pinus sylvestris L.）,Pinus koraiensis,and peanut shells,and determine the contents of eleven trace elements（Cr,Mn,Co,Ni,Cu,Zn,As,Mo,Cd,Ba,and Pb） in each sample.The detection limits for each element were in the range of 0.0007-0.2430μg/g and the relatively standard deviations were basically lower than 5%,with the standard recovery rates ranging between 86.4%and 113%.A comparison between traditional oven heating digestion under high pressure and ultra-high throughout closed microwave digestion shows that they have no significant difference in analysis results,only the microwave digestion method is easy to operate,more timesaving,and more efficient,uses less acid,has smaller environmental footprint,and requires lower experimental cost and is thus more suitable for pretreatment of bulk samples.The combination of ultra-high throughout closed microwave digestion and the ICP-MS technique allows researchers to determine the contents of trace elements in solid biofuels efficiently,rapidly and accurately.
出处
《中外能源》
CAS
2014年第5期28-35,共8页
Sino-Global Energy
基金
国家重大科学仪器设备开发专项项目"ICP痕量分析仪器的研制与应用"子课题--应用ICP痕量分析仪器检测地矿稀土
稀有
稀散元素的方法研究(编号:2011YQ140147)
基本科研业务费项目(编号:2002351300128)的资助
关键词
超高通量密闭微波消解
ICP-MS
生物质燃料
微量元素
前处理
检出限
相对标准偏差
ultra-high throughout closed microwave digestion
ICP-MS
solid biofuels
trace elements
pretreatment
limit of detection
relative standard deviation
