As a powerful tool for the analysis of high pure metal and semiconductor, glow discharge mass spectrometry (GDMS) has been extended applied in China. The primary theory and application of GDMS were simply introduced and the instrumental conditions, measurement repeatability and series certified reference materials with different metallic matrix were researched in detail. The measured repeatabilities of analysis results were in the range of 1% -5% for the impurities which the con-tents were about 1 mg/kg. The series of certified reference materials of steel, copper, including SRM1761a, SRM1762a, SRM1763a, SRM1764a, SRM1765, SRM1766, SRM1767, SRM1767, SRM1112 -SRMC1117 and SRM1256b purchased from National Institute of Standards and technology (NIST) of USA, were investigated and the results were compared. It was found that the same correction factors could be used in the measurement of impurities with similar matrix in a wide range of contents under the same measurement conditions. The correlation coefficients of series results were more than 0. 999. It was found that there were obvious matrix effects in the measurements of samples with different matrixes. The routine instrumental values of some relative sensitivity factors ( RSFs) , especially for the elements of lighter mass number, were not suitable for the quantitative analysis, but it is enough for the semi-quantitative analysis because the differences were no more than double of the RSFs. The result indicated that the correction of RSFs was the key technique for the measurement traceability through the research of the quantitative analysis by GDMS spectrometry.%辉光放电质谱(GDMS)作为高纯金属和半导体材料分析的强有力工具在国内已得到了大量应用,该文简要介绍了GDMS的基本原理和国内外应用现状,对仪器测量条件的选择、测量重复性进行了详细研究,对于含量在1 mg/kg左右的杂质,测量的重复性将产生约1％～5％的不确定度；对不同金属基体的系列标准物质进行对比研究,发现对于基体相同的样品,杂质元素在较宽的浓度范围内可以使用同样的校正系数进行校正,大部分元素的线性相关系数达到0.999以上,但对于不同基体的样品,测量中仍存在明显的基体效应,一些元素,尤其是轻质量数元素的相对灵敏度因子(RSF)设定值存在较大的偏差,并不适合定量分析,但绝大部分不超过2倍误差,可以满足半定量分析的要求.通过对GDMS定量分析中关键因素的研究,认为相对灵敏度因子的校正是GDMS测量结果可溯源性的关键.
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