The evaluation results of the metrological performance of a dilution and a permeation standard for generating SI-traceable calibration gas mixtures of NO, SO2 and NO2 for ambient air measurements are presented. The composition of the in situ produced reference gas mixtures is calculated from the instantaneous values of the input quantities of the generating standards. In a measurement comparison, the calibration and measurement capabilities of five laboratories were evaluated for the three analytes at limiting amount of substance fractions in ambient air between 20 and 150 nmol mol−1. For the upper generated reference values the target relative uncertainties of ⩽2% (for NO and SO2) and ⩽3% (for NO2) for evaluating the laboratory results were fulfilled in 12 out of 13 cases. For the analytical results seven out of nine laboratories met the criteria for the upper values for NO and NO2, for SO2 it was one out of four. From the negative degrees of equivalence of all NO2 comparison results it was supposed that the permeation rate of NO2 through the FEP polymer membrane of the permeator was different in air and N2. Subsequent precision permeation measurements with various carrier gases revealed that the permeation rate of NO2 was ≈0.8% lower in synthetic air compared to N2. With the corrected NO2 reference values for air the degrees of equivalence of the laboratory results were improved and closer to be symmetrically distributed.
Abstract. The European Directive (2008/50/EC) sets up, among other things, the limit values i.e. the maximum allowed concentrations at given time average in the air, for specified pollutants. Calibration of the measurement instruments needs to be performed at regular time intervals. In the framework of an European Joint Research Programme (JRP) named Metrology for Chemical Pollutants in Air (MACPoll) one task aims to provide harmonized dilution methods for air pollutant gases at low concentration for calibration and quality control purposes. The study focuses on the reactive gases nitrogen dioxide and sulphur dioxide at concentration levels corresponding to the limit values given in the European Directive (2008/50/EC). Nitrogen oxide (NO) is studied as well as NO2 because both of them are measured simultaneously for NOx. This work consists in improving the dilution methods for generating calibration standards for SO2, NO, NO2 at limit values and to validate them by an interlaboratory comparison.
This supplementary comparison (EURAMET.QM-S8) concerns the purity analysis of nitrogen as used in reference gas mixture preparation. This project was carried out without adding impurities to the gas used for this comparison, and is therefore more representative to evaluate the analysis of carbon monoxide, carbon dioxide, methane, oxygen, argon and water impurities in high-purity nitrogen. The analysis of the amount-of-substance fraction water was optional.Two 50 litre high purity nitrogen cylinders were purchased from a well-qualified supplier of specialty gases. The listed components were expected to be present in the pure nitrogen at the target levels as a result of the purification of the nitrogen. From the start of this comparison it was clear that the comparison may not lead to reference values for the constituents analysed.The results indicate that analyses of high purity gases are often limited by the limits of detection of analytical equipment used. The reports of the participating laboratories also indicate that there is no agreed method of determination of the uncertainty on a detection limit value. The results provide useful information on the performance of participants. For all analysed components there is reasonable agreement in results for LNE, VSL, METAS and NPL. For BAM only the argon result is in agreement.Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.The final report has been peer-reviewed and approved for publication by EURAMET, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
As part of the on-going key comparison BIPM.QM-K1, a comparison has been performed between the ozone national standard of the Laboratoire National de métrologie et d'Essais (LNE) and the common reference standard of the key comparison, maintained by the Bureau International des Poids et Mesures (BIPM). The instruments have been compared over a nominal ozone mole fraction range of 0 nmol/mol to 500 nmol/mol.Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA).
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