CCQM-K137, Nitrogen Monoxide (NO) in nitrogen, 30 μmol mol^-1 and 70 μmol mol^-1 Final Report

The key comparison CCQM-K137 was aimed at evaluating the level of compatibility of laboratories' preparative capabilities for gravimetric nitrogen monoxide/nitrogen primary reference mixtures at mole fractions of 30 μmol mol-1 and 70 μmol mol-1 . The comparison was organised by the BIPM. It consisted in the simultaneous comparison of a suite of 2n primary gas standards, two standards to be prepared by each of the n participating laboratories at the nominal values of 30 μmol mol-1 and 70 μmol mol-1. Two independent analytical methods were used by the BIPM to analyse the amount fraction of nitrogen monoxide (NO) in nitrogen; UV spectrophotometry and chemiluminescence (CLD). The agreement between the results obtained with the two main techniques served to highlight possible issues in the preparation of the standards. During this comparison, standards prepared by two participants appeared to result in a larger bias between the analysers than observed for others. These observations were explained by the analysis of all standards by Fourier Transform Infrared Spectroscopy (FTIR) which identified the presence of a larger amounts of water vapour (H2O), nitrous oxide (N2O) and nitrogen dioxide (NO2) in these standards, which are the three main impurities which can appear in mixtures of NO in nitrogen. The above observations were used to underpin the selection of standards (at each nominal NO mole fraction) which can be considered as a consistent set, allowing the calculation of a calibration line by a Generalised Least-Square regression. Key Comparison Reference Values were then proposed for all participants as predicted values from the calibration lines. Interferences caused in the response of the CLD analyser by impurities (verified by FTIR measurements) led to only the results from the UV analyser being proposed for the KCRV and Degrees of Equivalence calculations. Good agreement was observed between all participants who could prepare their standards with minimum levels of impurities. The key comparison CCQM-K137 is considered to present an analytical challenge at both nominal mole fractions and therefore considered as a Specialised (Track C) comparison in the CCQM nomenclature.