本文選題：電子級氮氣 + 純化　； 參考：《質(zhì)譜學報》2017年05期

【摘要】：采用大氣壓電離質(zhì)譜(APIMS)技術(shù)及標準添加法建立了一種電子級氮氣中超痕量雜質(zhì)的分析方法。以高效純化后氮氣中的5種雜質(zhì)(CO、CH_4、H_2、O_2和CO_2)作為檢測對象,以動態(tài)稀釋后的標準氣體作為參考進行回歸分析,標準氣體依據(jù)ISO 6142及ISO導則34規(guī)定的重量法在實驗室制備,同時采用蒙特卡洛(MCM)法及《不確定度表示指南》描述的GUM法對本方法的不確定度進行評定。結(jié)果表明:在0~1nmol/mol范圍內(nèi),5種雜質(zhì)的校準曲線呈現(xiàn)出良好的線性關(guān)系,線性相關(guān)系數(shù)R~2均大于0.998;方法的靈敏度高,檢出限可達幾至幾十pmol/mol水平,擴展不確定度為37%(k=2),通過與文獻中報道的數(shù)據(jù)相比,CH4和CO的檢出限分別改善了1個和2個數(shù)量級,H_2、O_2、CO_2則與文獻的報道值基本一致。本方法能夠滿足對相關(guān)電子氣體中雜質(zhì)的分析要求,并可為量值溯源提供參考依據(jù)。
[Abstract]:An analytical method for ultratrace impurities in electron-grade nitrogen was established by means of atmospheric pressure ionization mass spectrometry (APIMS) and standard addition method. Five kinds of impurities (COHCH4H2OV2 and COS2) in highly purified nitrogen gas were used as the detection objects, and the dynamically diluted standard gas was used as the reference for regression analysis. The standard gas was prepared in the laboratory according to the gravimetric method stipulated in ISO 6142 and ISO guideline 34. At the same time, the uncertainty of this method is evaluated by the Monte Carlo (MCM) method and the GUM method described in the Guide to the expression of uncertainty. The results show that the calibration curves of five impurities in the 0~1nmol/mol range show a good linear relationship, the linear correlation coefficient R ~ (2) is greater than 0.998, the sensitivity of the method is high, and the detection limit can reach several to dozens of pmol/mol levels. The extended uncertainty is 37% (KG 2). Compared with the reported data, the detection limits of CH4 and CO are improved by 1 and 2 orders of magnitude respectively. This method can meet the requirements of the analysis of impurities in the related electronic gases and can provide reference for traceability.
【作者單位】： 中國計量科學研究院;
【基金】：國家科技支撐計劃(2013BAK10B03) 國家自然科學基金(41275136)資助
【分類號】：O657.63

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本文編號：2087804