建立了微波和湿法两种消解方式的不同条件下土壤/沉积物中V、Cr、Co、Ni、Cu、Zn、Se、As、Sr、Mn、Pb、Cd、Ba和Fe共14种金属元素的ICP-MS准确测定方法.比较了微波消解不同称样量及湿法不同消解体系、温度对不同金属元素的消解效果.以103Rh和195Pt作为ICP-MS测定时的内标元素,针对不同测定元素选择合适的监测质量数及碰撞/反应模式.结果表明,微波消解称样量为0.10 g、消解体系为硝酸-盐酸-氢氟酸时,除Mn、Sr、Ba、Fe等半金属外大部分金属元素消解效果良好;湿法消解采用硝酸-盐酸-高氯酸-氢氟酸(5∶1∶1∶5)体系、消解最高温度为180℃时消解效果最佳,14种金属元素测定结果均在标准值范围内,但需防止少数易挥发元素如As、Se、Pb等在蒸酸过程中挥发损失.分别采用上述两种消解体系对湖底沉积物和两种国际比对土壤样品进行了前处理,并以ICP-MS进行了准确测定,14种金属元素的RSD均在0.10％-3.32％范围之间,国际比对中As、Cd、Pb、Mn的测定结果与初步公布结果一致.该方法重复性好、准确度高,适用于常规土壤/沉积物样品的准确测定.
A method for the accurate determination of V,Cr,Co,Ni,Cu,Zn,Se,As,Sr,Mn,Pb,Cd,Ba and Fe in soil/sediment samples by ICP-MS with different digestion conditions of microwave and wet digestion was established.Factors such as sample mass in microwave digestion,different system of mixed acids and temperature of wet digestion were optimized.103Rh and 195Pt were used as internal standards in ICP-MS analysis.Appropriate monitoring isotopes,collision or reaction mode were selected according to different elements.The results showed that when HNO3-HCl-HF was used in microwave digestion and the sample mass was 0.10 g,most of metal elements were completely decomposed except for semi-metals such as Mn,Sr,Ba and Fe.For the wet digestion,all the 14 metal elements were consistent with the certified values when HNO3-HCl-HClO4-HF (5∶ 1∶ 5∶ 1) were used at 180 ℃.Lake sediments and two soil samples for BIPM international comparison were digested by the two methods and determined by ICP-MS.Results indicate that the RSD for the 14 elements were from 0.10％ to 3.32％.The results of As,Cd,Pb,Mn in the two international comparison samples were consistent with the preliminary results reported by the comparison coordinating institute.This method is simple and convenient with good repeatability and accuracy,and it is applicable for a wide range of similar matrix samples.
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