【摘要】 提出了微波酸溶-电感耦合等离子体质谱法(ICP-MS)同时测定固体废物中17种元素的方法。取固体废物样品0.1~0.2g(称准至±0.1mg)加入硝酸-氢氟酸-盐酸-过氧化氢(4+1+1+1)混合液7mL,于175℃微波消解20min,将消解液于150℃蒸发至近干,加水溶解残渣并定容至50mL。取固体废物浸出液25.00mL,加入硝酸-盐酸(4+1)混合酸5mL,于165℃微波消解10min后,按上述手续处理后作为样液。用电感耦合等离子体质谱法测定上述两类样液中17种元素。各元素测定值的相对标准偏差(n=6)分别在4.5%~12%之间(固体样品)和0.4%~15%之间(浸出液样品);加标回收率分别在89.1%~116%和82.4%~113%之间。按所提出方法分析了一个CRM(TCLPlot#7044-52,ISS1),测定值与认定值一致。更多还原

【Abstract】 A method of determination of 17 elements in solid wastes was proposed by using microwave digestion coupled with ICP-MS.The sample of solid waste（0.1-0.2g,weighed to±0.1mg）was digested with7 mL of a mixture of HNO₃-HF-HCl-H₂O₂（4+1+1+1）at 175℃for 20 min in a microwave digester,the digested solution was evaporated to near dryness at 150 ℃ and the residue was taken up with water and made its volume to50 mL for use as sample solution.25.00 mL of the leachate were taken and digested with 5mL of a mixed acid of HNO3-HCl（4+1）at 165 ℃ for 10 min in a microwave digester,and then the digested solution was treated as described above to obtain the sample solution.17 elements in the sample solution were determined by ICP-MS.Values of RSDs（n=6）for the 17 elements were found in the ranges of 4.5%-12%（for the solid waste sample）and 0.4%-15%（for the solid waste leachate sample）,and values of recovery found by standard addition method were in the ranges of 89.1%-116% and 82.4%-113% respectively.A sample of CRM（TCLPlot#7044-52,ISS1）was analyzed by the proposed method,giving results in consistency with the certified values.更多还原