辉光放电质谱(GD-MS)法测定高纯砷中16种杂质元素  

Determination of 16 Impurity Elements in High Purity Arsenic by Glow Discharge Mass Spectrometry

作　　者：邹琳 栾海光 王凌燕 徐萌琳 ZOU Lin;LUAN Haiguang;WANG Lingyan;XU Menglin(Kunming University of Science and Technology,Kunming,Yunnan 650093,China;Shandong Humon Smelting Co.,Ltd.,Yantai,Shandong 264100,China)

机构地区：[1]昆明理工大学,昆明650093 [2]山东恒邦冶炼股份有限公司,山东烟台264100

出　　处：《中国无机分析化学》2025年第4期576-581,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：山东省重大科技工程项目(2019TSLH0119)。

摘　　要：高新技术产业发展迅猛,半导体行业热度也越来越高,对于高纯砷的需求量相应不断增加,对于其纯度的要求也越来越高,尤其是在合成化合物半导体材料时。因此,对于高纯砷中杂质元素的检测也成为不容忽视的一部分。通过对制样方法、样品的处理方法、仪器的参数条件、积分时间的选择、优化数据处理以及如何避免污染等方面进行研究,建立了辉光放电质谱(GD-MS)法测定高纯砷中钠、镁、铝、钾、钙、铬、铁、镍等16种杂质元素的方法。通过对辉光放电质谱仪(GD-MS)测定杂质元素特点的研究,最终选择压片法进行样品制备;通过调节氩气流量、电流、电压、积分时间等使仪器达到最佳分析状态;通过建立相对灵敏度因子校正分析结果,并与电感耦合等离子体质谱仪的分析结果进行对比,结果均在误差范围之内。辉光放电质谱法操作便捷,结果准确可靠且精密度高。With the rapid development of high-tech industry and the increasing popularity of semiconductor industry,the demand for high-purity arsenic has surged,and the requirements for its purity are getting higher and higher,especially when synthesizing compound semiconductor materials.Therefore,the detection of impurity elements in high-purity arsenic has become a part that cannot be ignored.A method for the determination of 16 impurity elements in high-purity arsenic by glow discharge mass spectrometry(GD-MS)was established by studying sample preparation method,sample treatment method,instrument parameter conditions,selection of integration time,optimization of data processing and how to avoid pollution.By studying the characteristics of impurity elements determined by glow discharge mass spectrometer(GD-MS),the tabletting method was finally selected for sample preparation.By optimizing parameters such as argon flow,current,voltage and integration time,the instrument achieved the best analysis state.By establishing the relative sensitivity factor to correct the analysis results,and comparing with the analysis results of inductively coupled plasma mass spectrometer,all results fell within the error range.Glow discharge mass spectrometry is user-friendly,and the results are accurate and reliable with high precision.

关 键 词：辉光放电质谱仪 高纯砷 质谱干扰 相对灵敏度因子 

分 类 号：O657.63[理学—分析化学] TH843[理学—化学]