辉光放电质谱应用和定量分析
Application and Quantitative Analysis of Glow Discharge Mass Spectrometry
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摘要: 辉光放电质谱(GDMS)是利用辉光放电源作为离子源的一种无机质谱方法。GDMS采用固体进样,样品准备过程简单、分析速度快、基体效应小、线性范围宽,是痕量分析的一种重要分析手段,在国外已经成为高纯金属和半导体分析的行业标准方法。GDMS可以进行深度分析,选择合适的放电条件,可以在样品表面获得平底坑,深度分辨率可以满足对微米量级的层状样品进行测量。目前商业化的GDMS都是直流放电源,这些仪器需要用第二阴极法或混合法才能对非导电材料进行测量,从而限制了GDMS在非导体材料分析方面的应用。GDMS放电源和单接收方式并不能满足同位素丰度精确测量的要求,在精确度要求不高的情况下,GDMS在固体样品同位素丰度的快速测量方面还是有一定的应用价值。文章总结了近几年国内外GDMS在各领域的应用进展和定量分析技术发展方向。GDMS已经成为一种高纯导电材料分析的重要方法;在深度分析、非导电材料分析、固体同位素丰度快速测量中有一定的应用前景。在定量测量方面,由于受到基体、测量条件等影响因素较多,缺乏合适的基体匹配的标准物质用于校正,GDMS主要停留在定性和半定量分析阶段。目前,国外已有关于GDMS定量分析的报道,采用掺杂的方法合成校正样品,利用一系列校正样品获得的标准曲线实现定量分析,这种方法过程较为复杂,但可以获得较好的定量分析结果,是一种不错的校正方法。Abstract: Glow Discharge Mass Spectrometry (GDMS) is a kind of solid mass spectrometry using a glow discharge ion source. In recent years, it has become the industry standard method for the analysis of trace elements in metals and semiconductors, because of its simple sample preparation process, rapid, insignificant matrix effect and wide dynamic range. GDMS can be used in the profile study of depth. By optimizing the sputtering conditions and source geometry, a crater with a flat bottom can be achieved and depth resolution is good enough to profile multi-layer samples in the order of micrometers. Commercial GDMS, with direct current sources can analyse nonconductive materials with a second cathode or mixed with a conducting host. It makes the sample preparation process more complex and limits the applications of GDMS. GDMS is not stable enough to carry out highly accurate and precise isotope ratio measurements. However, it is still a rapid analysis technique for a preliminary study. The development of applications and quantitative analysis in all research fields in recent years have been summarized here. GDMS was developed as an important analysis method for high purity conduction materials. Moreover, it has some degree of application prospect for depth profiling studies, non conduction materials analysis and solid isotope composition abundance determination. Since the limitations of matrix effect and determination conditions and lack of certified reference materials, GDMS is still a quantitative and semiquantitative analysis method. Some papers on quantitative analysis were reported in oversea journals by using a work curve obtained with a series of synthetic calibration samples. The method is complex, but it can provide quantitative results.
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Keywords:
- glow /
- discharge /
- mass /
- spectrometry
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