影响辉光放电发射光谱分析准确性的因素探讨  

Discussion on influence factors for analysis accuracy of glow discharge optical emission spectrometry

作　　者：张毅[1] 何晓蕾[1] 缪乐德[1] 于永波 ZHANG Yi;HE Xiaolei;MIAO Lede;YU Yongbo(Central Research Institute,Baoshan Iron&Steel Co.,Ltd.,Shanghai 201999,China)

机构地区：[1]宝山钢铁股份有限公司中央研究院,上海201999

出　　处：《冶金分析》2021年第12期50-57,共8页Metallurgical Analysis

摘　　要：基于辉光放电发射光谱分析定量原理讨论了影响其分析结果准确性的几个因素:深度剖析中,浓度的定量取决于经溅射率校正的校准曲线是否能够覆盖所有元素的浓度值,必要时需要拓展校准曲线;深度的定量准确性则依赖于加权平均法密度与实际密度间的一致性,相差较大时,可以通过软件或硬件进行修正;样品中存在有机物质时,辉光放电等离子体中的分子谱带对其他元素谱线强度形成干扰,导致分析结果中出现"伪峰"或定量分析结果出现较大偏差,需要根据样品的工艺实际对分析结果进行甄别;比较深度剖析与其他分析技术的定量结果,应考虑镀层均匀性和取样量差异的影响;成分分析的重复性和再现性能够满足金属固体样品快速分析的要求,最新国家标准中的精密度结果令人满意;元素痕量分析时,需要关注谱线发射强度是否大幅降低,长时间溅射低熔点金属或有机物样品少量物质沉积于透镜处是原因之一。Several factors influencing the analysis accuracy of glow discharge optical emission spectrometry(GDOES) are discussed based on its quantitative analysis principle.In depth profile analysis, the quantification of concentration depends on whether the calibration curves corrected by the sputtering rate could cover the concentration ranges of all elements or not. The calibration curves should be extended to meet the analysis requirements if necessary. The accuracy of quantitative analysis of depth depends on the consistency between the density calculated by the weighted average method and the actual density. If the difference is large, it could be corrected by software or hardware. When there are organic substances in the sample, the molecular band in the glow discharge plasma will interfere with the emission intensity of other elements, leading to "false peek" in analytical results or large deviations in the quantitative results. Therefore, the analysis results should be identified according to the actual process of the sample. During the comparison between the quantitative depth profile analysis by GDOES with other analytical techniques, the influence of coating uniformity and sampling amount difference should be considered. The repeatability and reproducibility of bulk analysis could meet the requirements of rapid analysis of metal solid samples, and the precision results in the latest national standard experiment has been proved to be satisfactory. In the analysis of trace elements, it is necessary to pay more attention to whether the emission intensity of the element is greatly reduced. One of the reasons is that long time sputtering of low melting-point metals or organic samples will lead to the deposition of few substances onto the lens.

关 键 词：辉光放电发射光谱(GDOES) 深度剖析 成分分析 准确性 

分 类 号：O657.31[理学—分析化学]