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机构地区:[1]苏州科技学院化学与生物工程学院,江苏苏州215011 [2]吉林大学地球科学学院,吉林长春130061 [3]吉林工程技术师范学院信息工程学院,吉林长春130052
出 处:《分析测试学报》2009年第1期105-108,共4页Journal of Instrumental Analysis
基 金:国家重点基础研究发展计划973项目课题(2006CB701403-03)
摘 要:利用微波消解法处理植物灰分样品,讨论了混合酸组成、混酸配比、固液比和微波消解时间对样品制备结果的影响。优选微波消解方案:微波压力(MPa)0.5、1.0、1.5、2.0,消解时间(min)4、3、3、10的微波程序,混合酸体系HNO3-HCl-HF-HClO4(体积比为6:2:1:1)。在此条件下,进行了方法准确度实验和测量结果重复性实验,该方法经植物国家标准物质(GBW07603)验证,微量元素测试结果的相对误差为1.06%~5.60%,相对标准偏差为0.87%~5.25%;稀土元素测试结果的相对误差为1.82%~10.2%,相对标准偏差为2.14%~8.00%。应用电感耦合等离子体质谱法(ICP-MS)同时测定植物灰分中21种微量元素和15种稀土元素。结果表明,微波消解法处理植物灰分样品,具有快速、简便、节省试剂、消解完全等特点,测定结果的准确度和精密度令人满意。A microwave-assisted extraction technique coupled to ICP- MS method was developed for determination of trace and rare elements. Effects of the constitutes and ratios of mixed acid system, proportion between solid and liquid, as well as digestion time of microwave on the sample preparation were discussed. The optimal conditions were using the following program : microwave powers are 0. 5, 1.0, 1.5, 2.0 MPa, microwave digested time are 4, 3, 3, l0 min, the mixed acid system is HNO3 - HC1 - HF - HC104 with volume ratio of 6 : 2 : 1 : 1. Under the optimal conditions, the method was used for simultaneously determination of 21 trace and 15 rare earth elements in national standard matter( GBW07603 ). The results showed that relative error and RSD of trace elements were range of 1.06% - 5.60% and 0. 87% - 5.25% , respectively, and that of rare earth elements were 1.82%- 10.2% and 2. 14% - 8.00% , respectively. The method showed better accuracy and preci- sion, and was applied in the determination of trace and rare earth elements in real sample with satis- factory results.
关 键 词:电感耦合等离子体质谱 微波消解 植物灰分 微量元素 稀土元素
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