摘要
电子级氯气中痕量金属杂质检测过程存在氯气易挥发,毒性大,不易捕集等难点。研究提出了一种新型的金属杂质的捕集方法,通过构建参比、多级气体吸收、气液分离、金属离子反渗透和废气吸收等系统,利用高纯氮进行置换与吹扫,有效解决了金属杂质的捕集难点。采用电感耦合等离子质谱法(ICP-MS)对捕集后的金属离子进行检测,实现了21种痕量金属杂质的准确测定。结果表明,方法检出限为0.5~8.13 ng/L,各元素的相对标准偏差RSD为3.0%~6.6%,加标回收率为81%~106%。该方法具有捕集效率高、金属杂质干扰小、准确度及精密度高和重现性好的优点。其他腐蚀性电子级气体中痕量金属杂质的捕集与测定均可参照使用。
There are some difficulties in the detection of trace metal impurities in electronic grade chlorine gas,such as volatile chlorine gas,high toxicity and hard to trap.This thesis presents a novel collection approach by devising a series of precise systems,encompassing a reference system,multi-stage gas absorption system,gas-liquid separation system,metal reverse osmosis system,and waste gas absorption system,along with the utilization of high-purity nitrogen gas for flushing and purging.This effectively resolves the issue.The metal ions subsequently enriched are determined by inductively coupled plasma mass spectrometry(ICP-MS),which enables the accurate determination of 21 trace metal impurities in electronic-grade chlorine.The results shows that the detection limit of the method ranged from 0.5~8.13 ng/L,the relative standard deviation(RSD)of each element was within 3.0%~6.6%,and the recovery rate of standard samples was between 81%~106%.This method possesses the advantages of high trapping efficiency,low interference from metal impurities,high accuracy,high precision and good reproducibility.It can serve as a reference for the capture and determination of trace metal impurities in other corrosive electronic-grade gases.
作者
夏致远
侯建鑫
杨着
曾靖淞
刘悦
杨成
冯晨
曾远
万富强
贺兆波
XIA Zhiyuan;HOU Jianxin;YANG Zhuo;ZENG Jingsong;LIU Yue;YANG Cheng;FENG Chen;ZENG Yuan;WAN Fuqiang;HE Zhaobo(Hubei Sinophorus Electronic Materials Co.,Ltd.,Yichang 443711,China;Hubei Three Gorges Laboratory,Yichang 443711,China)
出处
《应用化工》
CSCD
北大核心
2024年第12期2919-2923,2929,共6页
Applied Chemical Industry
基金
湖北省自然科学基金项目(2024AFD140)。
