本文已被:浏览 2865次 下载 585次
投稿时间:2013-05-08 修订日期:2013-06-20
投稿时间:2013-05-08 修订日期:2013-06-20
中文摘要: 建立了微波消解-石墨炉原子吸收光谱法(GF-AAS)测定纳米二氧化钛中痕量杂质元素砷的分析方法。采用由一定浓度和比例的氢氟酸、硝酸组成的混合试剂,结合应用高压密闭微波加热技术快速完全消解纳米二氧化钛样品,方法优选了最佳微波加热控制程序,不仅解决了二氧化钛难消解和待测元素砷高温消解过程中易挥发损失等难点,而且检测溶液酸度低,避免对GF-AAS石墨管的侵蚀。并且,通过基体效应影响实验,优化选择了石墨管类型、石墨炉升温原子化控制程序以及原子吸收光谱仪检测参数,消除热稳定性强的二氧化钛基体对测定易挥发痕量元素砷的影响。方法检出限为0.02 μg/L,回收率为93.0%~106.0%,相对标准偏差9.4%,与ICP-MS检测方法结果对照一致。
Abstract:An analysis method for the determination of trace impurity element arsenic in the nano-titanium dioxide by microwave digestion - graphite furnace atomic absorption spectrometry (GF-AAS) was established. A mixture digestion reagent which consist of a certain concentration and proportion of hydrofluoric acid and nitric acid were used in the sample digestion experiments. The nano-titanium dioxide samples were quickly and completely digested by high pressure microwave heating technology. The microwave heating control program were optimized. The new method not only solves the problem of difficult digestion of titanium dioxide and the loss of the analyte arsenic due to its evaporation during the high temperature digestion process, but also avoids the erosion of GF-AAS graphite tube due to the low acidity of the test solution. Furthermore, the type of graphite tube, graphite furnace atomization procedures and atomic absorption spectrometer detection parameters have been optimized through the matrix effect testing experiments, and thus the influence of the thermally stable titanium dioxide matrix on the determination of volatile trace element arsenic was eliminated. The detection limit the method is 0.02 μg/L. The recovery rate is in the range of 93.0% to 106.0%. The RSD is less than 9.4%. The results are consistent with those by ICP-MS method.
文章编号: 中图分类号: 文献标志码:
基金项目:
作者 | 单位 |
黄木辉 | 四川攀枝花公安局,四川 攀枝花 617000 |
Author Name | Affiliation |
HUANG Muhui | Sichuan Panzhihua Police Department, Panzhihua , Sichuan 617000, china |
引用文本:
黄木辉.微波消解-石墨炉原子吸收光谱法测定纳米二氧化钛中痕量砷[J].中国无机分析化学,2013,3(4):41-44.
HUANG Muhui.Microwave Digestion-Graphite Furnace Atomic Absorption Spectrometry Determination of Trace Arsenic in Nano-Titanium Dioxide[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(4):41-44.
黄木辉.微波消解-石墨炉原子吸收光谱法测定纳米二氧化钛中痕量砷[J].中国无机分析化学,2013,3(4):41-44.
HUANG Muhui.Microwave Digestion-Graphite Furnace Atomic Absorption Spectrometry Determination of Trace Arsenic in Nano-Titanium Dioxide[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(4):41-44.