Bureau International des Poids et Mesures, Pavillon de Breteuil, Sèvres, France.
Anal Chem. 2012 Dec 4;84(23):10283-90. doi: 10.1021/ac3024153. Epub 2012 Nov 21.
The development and operation of a highly accurate primary gas facility for the dynamic production of mixtures of nitrogen dioxide (NO(2)) in nitrogen (N(2)) based on continuous weighing of a permeation tube and accurate impurity quantification and correction of the gas mixtures using Fourier transform infrared spectroscopy (FT-IR) is described. NO(2) gas mixtures in the range of 5 μmol mol(-1) to 15 μmol mol(-1) with a standard relative uncertainty of 0.4% can be produced with this facility. To achieve an uncertainty at this level, significant efforts were made to reduce, identify and quantify potential impurities present in the gas mixtures, such as nitric acid (HNO(3)). A complete uncertainty budget, based on the analysis of the performance of the facility, including the use of a FT-IR spectrometer and a nondispersive UV analyzer as analytical techniques, is presented in this work. The mixtures produced by this facility were validated and then selected to provide reference values for an international comparison of the Consultative Committee for Amount of Substance (CCQM), number CCQM-K74, (1) which was designed to evaluate the consistency of primary NO(2) gas standards from 17 National Metrology Institutes.
本文描述了一种基于连续称重渗透管和使用傅里叶变换红外光谱(FT-IR)准确量化和校正混合气体中杂质的方法,开发并运行了一种高精度的初级氮二氧化氮(NO(2))混合气体发生装置,用于动态生产氮气(N(2))中的 NO(2)混合气体。使用该设备可以产生浓度范围为 5 μmol mol(-1)至 15 μmol mol(-1)、标准相对不确定度为 0.4%的 NO(2)混合气体。为了达到这个不确定度水平,我们做了大量的工作来减少、识别和量化混合气体中存在的潜在杂质,如硝酸(HNO(3))。本文基于对该设备性能的分析,包括使用 FT-IR 光谱仪和非分散紫外分析仪作为分析技术,给出了一个完整的不确定度预算。该设备产生的混合物经过验证后被选中,为国际咨询委员会物质数量(CCQM),编号 CCQM-K74,(1)的国际比对提供参考值,该比对旨在评估来自 17 个国家计量研究所的初级 NO(2)气体标准的一致性。