质谱学报2017，Vol.38Issue(5)：574-583,10.DOI:10.7538/zpxb.2016.0166
电子级氮气中超痕量杂质的质谱分析方法及测量不确定度评估
Determination of Ultra-Trace Impurities in Electronic Grade Nitrogen by Mass Spectrometry with Evaluation of Measurement Uncertainty
摘要
Abstract
A determination method for the ultra-trace impurities in electronic grade nitrogen was developed by using atmospheric pressure ionization mass spectrometry (APIMS) with standard addition method.5 impurities (CO,CH4,H2,O2,CO2) in high purity nitrogen were detected after purifying via a high-efficiency purifier.The standard gas used for calibrating APIMS was gravimetrically prepared in the lab according to the rules in ISO 6142 & ISO Guide 34,and it was added into the ionization source with different concentrations by dynamic dilution,then the fitting curve was built based on the data from different dilution points.Furtherly,the measurement uncertainty was evaluated through the method described in Guide to the expression of uncertainty in measurement (GUM) and Monte Carlo Method (MCM).The results show that all the 5 impurities have good linearity (R2＞0.998) in the dynamic range of 0-1 nmol/mol,and the high sensitivity is achieved,the detection limits (LOD) reached to the low level of several to tens of pmol/mol with the expanded uncertainty of 37％ (k=2).By compared with the previously reported data in the articles,the LOD values of magnitude for CH4 and CO are improved 1 and 2 orders,and the LOD values for other three impurities H2,O2,CO2 are the same levels as the reported data.It indicates that the method can be used for the relevant electronic gases for ultra-trace analysis with the traceability supporting.关键词
电子级氮气/纯化/超痕量杂质/大气压电离质谱(APIMS)/不确定度Key words
electronic grade nitrogen/purification/ultra-trace impurity/atmospheric pressure ionization mass spectrometry(APIMS)/measurement uncertainty分类
化学化工引用本文复制引用
张体强,胡树国,吴海,韩桥..电子级氮气中超痕量杂质的质谱分析方法及测量不确定度评估[J].质谱学报,2017,38(5):574-583,10.基金项目
国家科技支撑计划(2013BAK10B03) （2013BAK10B03）
国家自然科学基金(41275136)资助 （41275136）
