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《化学分析计量》 2019年增刊
DOI:10.3969/j.issn.1008-6145.2019.z1.006
气相色谱法测定空气中痕量三氟化氮
尹强,陈玲,许俊斌,贾相锐,叶丽芳,毛沅文,周阳,黄彦捷,周瑾艳
广东省计量科学研究院,广州 510000 
Determination of trace nitrogen trifluoride in air by gas chromatography
YIN Qiang, CHEN Ling, XU Junbin, JIA Xiangrui, YE Lifang, MAO Yuanwen, ZHOU Yang, HUANG Yanjie, ZHOU Jinyan
Guangdong Institute of Metrology, Guangzhou 510000, China 
摘要:建立了测定空气中痕量三氟化氮的气相色谱分析方法。采用专属性实验验证杂质含量对待测组分测量值的影响。利用红外光谱和质谱法对市售三氟化氮气体进行定性检验,采用重量法配制一系列准确浓度的标准气体,在100~1 000 μmol/mol 的浓度范围内建立非线性校正曲线,利用线性乘幂法将非线性曲线转化为线性曲线,简化了拟合曲线的不确定度计算过程,平行样品测定结果的相对标准偏差为0.20%~0.62%(n=5),配制样品测定结果相对误差的绝对值小于2%,空气加标样品三氟化氮的平均回收率为96.5%~101%。 
Abstract:A gas chromatography method to determine trace nitrogen trifluoride in air was established. The specific property experiment was used to verify that the impurity did not affect the measured value of the measured component. The nitrogen trifluoride was qualitative analysis by infrared spectroscopy and mass spectrometry, a series of gas reference materials with accurate concentration were prepared by gravimetric method. The calibration curves were established in the concentration range of 100-1 000 μmol/mol. The linear power method was used to transform the nonlinear curves into linear curves. The calculation formula of uncertainty of the fitting curve was given. The relative standard deviation of the parallel sample detectcion datas was 0.20%-0.62%(n=5), the absolute values of the relative deviation of the mixture samples were less than 2%, and the average standard addition recoveries of the air samle were 96.5%-101%.  
关键词:三氟化氮;气相色谱;校正曲线;不确定度 
Keywords:nitrogen trifluoride; gas chromatograthy; fitting curve; uncertainty 
基金:广东省科技计划项目(2016A040403072,2017A040405034) 
本文引用格式:
尹强,陈玲,许俊斌,等. 气相色谱法测定空气中痕量三氟化氮[J]. 化学分析计量,2019,28(Z1):28-31.
YIN Q,CHEN L,XU J B,et al. Determination of trace nitrogen trifluoride in air by gas chromatography[J]. Chemical analysis and meterage,2019,28(Z1):28-31. 

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