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1 Rapport BIPM-010/07 Bureau International des Poids et Mesures Upgrade of the BIPM Standard Reference Photometers for Ozone and the effect on the ongoing key comparison BIPM.QM-K1 y J. Viallon, P. Moussay, F. Idrees and R.I. Wielgosz BIPM Septemer 010 BIPM, Pavillon de Breteuil, F-931 Sèvres Cedex Rapport BIPM-010/07 01 Sep. 10 Page 1 of 16

2 Astract The NIST Standard Reference Photometer (SRP) maintained y the BIPM and used as the reference in the international key comparison BIPM.QM-K1 was upgraded in March 009. This followed the upgrade of almost all the other SRPs maintained y National Metrology Institutes or Designated Institutes which took part in this comparison. In order to ensure continuity etween the comparisons performed efore and after the upgrade, all degrees of equivalence etween participants and the (upgraded) common reference have een recalculated and are presented in this report. The result is a very small shift of the common reference towards the centre of the distriution of participants. The good agreement with all participants has een maintained. Contents: 1. INTRODUCTION BRIEF DESCRIPTION OF THE COMPARISONS METHOD BRIEF DESCRIPTION OF THE BIPM SRPS CALCULATION OF BIPM-SRP7 CORRECTION FACTORS RECALCULATION OF THE DEGREES OF EQUIVALENCE RECALCULATION OF THE LEAST-SQUARE REGRESSION PARAMETERS CONCLUSION REFERENCES Rapport BIPM-010/07 01 Sep. 10 Page of 16

3 1. Introduction The reference method for the measurement of ground level ozone concentration is ased on UV photometry, with the NIST SRP ozone reference standard acting as the primary standard for numerous national and international ozone monitoring networks. Several of these instruments are maintained y the BIPM, one of them eing the reference standard for international comparisons of national ozone standards which have een coordinated y the BIPM 1 since 003. After the first international comparisons, which were performed in , the BIPM and the NIST undertook a study of systematic iases in the NIST SRP [1], which highlighted two major iases in the instrument. Before starting any further international comparisons, the BIPM decided to modify its SRPs in order to correct for the oserved iases. One of the two iases, namely on the gas temperature evaluation, was removed with a physical modification of the instruments. For the second ias, arising from a limited knowledge of the light path length inside the instrument gas cells, a physical correction was not easy to achieve and a decision was made to numerically correct the path length of two SRPs (SRP7 and SRP8). A third BIPM instrument was physically modified and was used as internal reference to help monitor any drifts in the other SRPs. Since then, the NIST developed an upgrade kit to physically remove the oserved iases in the NIST SRPs, and started a series of upgrades of SRPs around the world []. The BIPM also performed some upgrades of other SRPs [3, 4]. National Metrology Institutes or Designated Institutes requested upgrades of their SRPs efore taking part in the key comparison BIPM.QM-K1 cycle 1 ( ) organized y the BIPM. The new comparison results clearly demonstrated that the measurement results of the common reference of the comparison, BIPM-SRP7 had slightly shifted from the mean of the group of upgraded SRPs. This shift was attriuted to a difference etween the numerical correction decided y the BIPM and the results of physical corrections introduced y the upgrade. These assumptions were confirmed y the more detailed study of the upgrade effect, which will e explained in a forthcoming paper. In view of the aove considerations, the BIPM, with the approval of the Gas Analysis Working Group of the CCQM, decided to undertake the upgrade of its two SRPs (7 and 8) after the completion of the first cycle of the key comparison BIPM.QM-K1 and efore starting the second cycle ( ). It was decided that all results from the first cycle of the key comparison would e recalculated to allow meaningful comparisons with following cycles. This report presents the results of the upgrade of BIPM-SRP7 and BIPM-SRP8 and the effect on the key comparison BIPM.QM-K1. More details of the upgrade procedure and its effect on a numer of SRPs in comparison with the study performed in 005 will e pulished separately. 1 Rapport BIPM-010/07 01 Sep. 10 Page 3 of 16

4 . Brief description of the comparisons method All comparisons reported here were performed y following the protocol of the key comparison BIPM.QM-K1, which can e downloaded from the BIPM wesite ( The results of one comparison etween a participant and the BIPM, as pulished in the Key Comparison Dataase maintained y the BIPM, is a set of two degrees of equivalence. They are calculated at two nominal ozone mole fractions among the twelve measured in each comparison, in the range 0 nmol/mol to 500 nmol/mol: 80 nmol/mol and 40 nmol/mol. Degrees of equivalence efore and after the upgrade of BIPM-SRP7 are presented in section 5 of this report. In addition, comparisons can e meaningfully descried y the two parameters of the linear regression performed etween the measurement results of the two instruments involved, taking into account standard measurement uncertainties. To this end, a piece of software called OzonE was used. This software, which is documented in a pulication [5], is an extension of the previously used software, B_Least, recommended y the ISO standard 6143:001 [6]. It includes the possiility of taking into account correlations etween measurements performed with the same instrument at different ozone mole fractions. In a direct comparison, a linear relationship etween the ozone mole fractions measured y SRPn and SRP7 is otained: x n a a x SRP 0 1 SRP7 (1) The associated uncertainties on the slope u(a 1 ) and the intercept u(a 0 ) are given y OzonE, as well as the covariance etween them and the usual statistical parameters to validate the fitting function. Parameters of the linear regression for all participants efore and after the upgrade of BIPM-SRP7 are presented in section 6 of this report. 3. Brief description of the BIPM SRPs 3.1. State of the BIPM SRPs efore the upgrade Compared to the original design descried in [7], SRP7, SRP8 and SRP31 were modified to deal with two iases revealed y the study conducted y the BIPM and the NIST [1]: - The three SRPs were equipped with a thermo-electric cooling device to remove excess heat from the lamp housing and to prevent heating of the cells. Together with a regular caliration of their temperature proe, this ensures the removal of the ias on the temperature measurement of the gas cell. - In SRP7 and SRP8 the optical path length was calculated as eing times the total length of the two cells within each instrument. Together with an increased uncertainty, this takes into account the ias on the optical path length. Rapport BIPM-010/07 01 Sep. 10 Page 4 of 16

5 - In SRP31 the gas cells have een physically modified to avoid multiple reflections of the light eam on the end windows. The BIPM workshop designed new cell ends, in which the windows make a 3 angle with the vertical. 3.. State of the BIPM SRPs after the upgrade The SRP upgrade kit was installed in BIPM-SRP7 and BIPM-SRP8. The upgrade kit consisted of two parts: - A new source lock was designed to minimize the gas temperature evaluation ias y etter thermal insulation of the UV source lamp (heated to a temperature of aout 60 C) from the rest of the optical ench, thus avoiding the temperature gradient oserved in the SRP when the original source lock was used. - A new set of asorption cells were installed. The new cells consisted of quartz tues closed at oth ends y optically sealed quartz windows. These windows were angled at 3 to the vertical plane to avoid multiple reflections along the light path. In addition, the thermo-cooling device designed at the BIPM was maintained in all three SRPs and was in-use during all comparisons Uncertainty udget of the BIPM-SRPs The uncertainty udget for the ozone mole fraction in dry air x measured y the instruments BIPM-SRP7, BIPM-SRP8 and BIPM-SRP31 in the nominal range 0 nmol/mol to 500 nmol/mol is given in Tale 1. The same uncertainty udget is applied to SRPs efore and after the upgrade. Tale 1: Uncertainty udget for the SRPs maintained y the BIPM Component (y) Optical Path L opt Pressure P Temperature T Ratio of intensities D Asorption Cross section Source Uncertainty u(y) Distriution Standard uncertainty Comined standard uncertainty u(y) Sensitivity coefficient x c i y Contriution to u(x) c i u( y) nmol/mol Measurement Rectangular cm Scale x Repeataility Normal 0.01 cm 0.5 cm Correction Lopt Rect 0.5 cm factor x Pressure gauge Rectangular 0.09 kpa Difference etween cells Rectangular kpa kpa x P x Temperature Rectangular 0.03 K x proe 0.07 K Temperature T Rectangular K gradient x Scaler Rectangular 8 10 resolution x Repeataility Triangular Dln( D) 0.8 Hearn value cm²/molecule cm²/molecule x x Rapport BIPM-010/07 01 Sep. 10 Page 5 of 16

6 Following this udget, the standard uncertainty associated with the ozone mole fraction measurement with the BIPM SRPs can e expressed as a numerical equation (numerical values expressed as nmol/mol): ux 3 ( ) (0.8) (.9 10 x) () 3.4. Covariance terms As explained previously, correlations etween the results of two measurements performed at two different ozone mole fractions with the BIPM maintained SRPs were taken into account in the software OzonE. More details on the covariance expression can e found in the protocol of the key comparison BIPM.QM-K1. The following expression was applied: ux (, x) x x u (3) i j i j where: u ( ) (4) u ( T) u ( P) u Lopt T P Lopt The value of u is given y the expression of the measurement uncertainty: u = or u = Calculation of BIPM-SRP7 correction factors All comparisons performed during the upgrade of SRP7 and SRP8 included SRP31 to monitor the changes in the measurement results. SRP31 was thus used as a transfer standard etween SRP7 efore the upgrade and SRP7 after the upgrade, in order to calculate correction factors for SRP7, as presented in this section. Considering the relationship etween SRP31 and SRP7 efore the upgrade of SRP7: xsrp31 a0 0 xsrp7 (5) Where the parameters of the linear equation take the following values: a 0 / u(a 0 ) / u(a 0, 0 ) / 0 u( 0 ) (nmol/mol) (nmol/mol) (nmol/mol) Rapport BIPM-010/07 01 Sep. 10 Page 6 of 16

7 And considering the relationship etween SRP31 and SRP7 after the upgrade of SRP7 (the prime notation is used to indicate measurement results of SRP7 after its upgrade): xsrp31 a1 1 x' SRP7 (6) Where the parameters of the linear equation take the following values: a 1 / u(a 1 ) / u(a 1, 1 ) / 1 u( 1 ) (nmol/mol) (nmol/mol) (nmol/mol) The relationship etween SRP7 after the upgrade and SRP7 efore the upgrade can e written: x' SRP7 a x SRP7 (7) Where the parameters of the linear equation take the following values: a / u(a ) / u(a, ) / u( ) (nmol/mol) (nmol/mol) (nmol/mol) The correction parameters a and are deduced from the equations: 0 (8) 1 a a a 0 1 (9) 1 And their uncertainty from: u ( 1) u0 1 0 ( ) u ( ) (10) 1 ua ( ) ua ( ) ua ( ) ( a a) u ( ) (11) u ( 1) u ( ) 1 u (, a) ( a0 a1) 0 a 4 (1) 1 1 Rapport BIPM-010/07 01 Sep. 10 Page 7 of 16

8 5. Recalculation of the degrees of equivalence 5.1. Definition In the key comparison BIPM.QM-K1, degrees of equivalence for the participant i were calculated at two particular values: 80 nmol/mol and 40 nmol/mol, according to the following equation: D x x (13) i i SRP7 where x i and x SRP7 are the measurement result of the participant i and of SRP7 at the nominal value x nom. Its associated standard uncertainty is: ud ( ) u u (14) i i SRP7 where u i and u SRP7 are the measurement uncertainties of the participant i and of SRP7 respectively. The correction factors a and deduced from the comparison etween SRP7 and SRP31 efore and after the upgrade are used to calculate a corrected reference value and associated uncertainty: x a x ' SRP7 SRP7 (15) ' SRP7 SRP7 SRP7 SRP7 ux ( ) ua ( ) ux ( ) u ( ) x x ua (, ) (16) In order to compute the corrected degrees of equivalence D i = x i x SRP7 and their associated uncertainties: ud ( ) u ux ( ) ' ' i i SRP7 (17) 5.. Particular case of the NMISA standard The comparison performed etween the NMISA and the BIPM is a particular case in BIPM.QM-K1, as the NMISA standard instrument was previously calirated y the BIPM, just efore performing the comparison. Therefore, measurement results of the NMISA and of the BIPM standards are correlated. Instead of equation 14, the uncertainty of the degree of equivalence D i for the NMISA is written, as explained in [8]: ud ( ) u u (18) i i SRP7 Rapport BIPM-010/07 01 Sep. 10 Page 8 of 16

9 Similarly, measurement results of the NMISA and of the BIPM standards after the upgrade are correlated. Instead of equation 17, the uncertainty of the degree of equivalence for NMISA is written: ud ( ) u ux ( ) ux ( ) ' ' ' i i SRP7 SRP7 (19) Where is the slope of the correction to e applied to SRP7 s measurement results, as defined in equation 8, and is the slope of the linear relationship etween the NMISA standard and SRP7: x x a x. i NMISA SRP Values The degrees of equivalence and their uncertainties calculated using the aove equations are reported in Tale and Tale 3 elow. Corresponding graphs of equivalence are displayed in Figure 1. The expanded uncertainties are calculated with a coverage factor k =. All participants in the first cycle of BIPM.QM-K1 have een included, except the VSL for which results were not ready at the time this report was written. New degrees of equivalence for the VSL will e pulished later. Tale : Degrees of equivalence of all participants in the key comparison BIPM.QM-K1 efore and after upgrade of the reference BIPM-SRP7, at the nominal ozone mole fraction 80 nmol/mol. La date x i u(x i ) x ref u(x ref ) x' ref u(x' ref ) D' i u(d' i ) U(D' i ) NIST Jan NIST Jan ISCIII Jun ISCIII Jun CHMI Sep INRIM Sep FMI Oct KRISS Oct UBA Nov VNIIM Nov VNIIM Nov NIM Mar LNE Apr NPL May METAS Jun NMISA Jul JRC Dec NPLI Mar Rapport BIPM-010/07 01 Sep. 10 Page 9 of 16

10 Tale 3 : Degrees of equivalence of all participants in the key comparison BIPM.QM-K1 efore and after upgrade of the reference BIPM-SRP7, at the nominal ozone mole fraction 40 nmol/mol. La date x i u(x i ) x ref u(x ref ) x' ref u(x' ref ) D' i u(d' i ) U(D' i ) NIST Jan NIST Jan ISCIII Jun ISCIII Jun CHMI Sep INRIM Sep FMI Oct KRISS Oct UBA Nov VNIIM Nov VNIIM Nov NIM Mar LNE Apr NPL May METAS Jun NMISA Jul JRC Dec NPLI Mar Rapport BIPM-010/07 01 Sep. 10 Page 10 of 16

11 10 Di / (nmol/mol) 5 0 NIST ISCIII CHMI INRIM FMI KRISS UBA VNIIM NIM LNE NPL METAS NMISA JRC NPLI DoE after upgrade DoE efore upgrade (k = ) Nominal value 80 nmol/mol NIST ISCIII CHMI INRIM FMI UBA VNIIM NIM LNE NPL METAS NMISA JRC NPLI Di / (nmol/mol) DoE after upgrade KRISS DoE efore upgrade (k = ) Nominal value 40 nmol/mol Figure 1: Graphs of equivalence of all participants in the key comparison BIPM.QM-K1 efore and after upgrade of the reference BIPM-SRP7, at the nominal ozone mole fractions 80 nmol/mol and 40 nmol/mol Analysis The first important oservation is that the upgrade of BIPM-SRP7 did not change the good agreement etween all participants. All degrees of equivalence shifted only y a very small amount compared to the stated uncertainties. The average and the median values of the degrees of equivalence efore and after the upgrade are displayed in Tale 4: Tale 4: Average of the degrees of equivalence of all participants in BIPM.QM-K1 efore and after the upgrade of BIM-SRP7 efore after efore after nominal value / (nmol/mol) Average D i / (nmol/mol) median Rapport BIPM-010/07 01 Sep. 10 Page 11 of 16

12 Secondly, following the upgrade measurement, results from BIPM-SRP7 are indeed now closer to the centre of the distriution of participants measurement results in the key comparison BIPM.QM-K1. The uncertainties of all degrees of equivalence have slightly increased, due to the use of a transfer standard (SRP31) etween SRP7 efore and after the upgrade. The effect on the key comparison is however minor. 6. Recalculation of the least-square regression parameters As explained in section, the parameters of the linear regression etween two photometers measurement results also constitute meaningful characteristics of the agreement etween them. Therefore, those parameters which are always given for information in the key comparison BIPM.QM-K1 reports, were also recalculated, as well as their uncertainties, according to the following equation. Considering the relationship etween a photometer i and SRP7 efore the upgrade of SRP7: x a x (0) i SRP7 And the relationship etween a photometer i and SRP7 after the upgrade of SRP7: xi a' ' x' SRP7 (1) Where the parameters a and and their uncertainties are deduced from: a' a a () ' (3) a ( a) a 4 3 ua ( ') ua ( ) ua ( ) u ( ) u ( ) ua (, ) (4) u ( ) u ( ) u ( ') ' (5) Particular case of the NMISA comparison: As discussed previously, covariance terms etween the values associated with each instrument at the same nominal mole fraction should e calculated and taken into account Rapport BIPM-010/07 01 Sep. 10 Page 1 of 16

13 when performing the regression. Unfortunately, this feature is not availale in the software OzonE. As the least-square results are given in comparison reports for information only, the NMISA parameters were calculated without these covariances Values The new parameters and their uncertainties, calculated using the aove equations, are reported in Tale 5. The corresponding graphs are displayed in Figure. The expanded uncertainties are calculated with a coverage factor k =. Tale 5 : New parameters of the linear regression etween each participant standard and the common reference standard SRP7 after its upgrade. La date ' u(') a' u(a') NIST Jan NIST Jan ISCIII Jun ISCIII Jun CHMI Sep INRIM Sep FMI Oct KRISS Oct UBA Nov VNIIM Nov VNIIM Nov NIM Mar LNE Apr NPL May METAS Jun NMISA Jul JRC Dec NPLI Mar Rapport BIPM-010/07 01 Sep. 10 Page 13 of 16

14 NIST ISCIII CHMI INRIM FMI UBA VNIIM NIM LNE NPL METAS NMISA JRC NPLI slope KRISS after upgrade efore upgrade 1 NIST ISCIII CHMI INRIM FMI KRISS UBA VNIIM NIM LNE NPL METAS NMISA JRC NPLI intercept after upgrade efore upgrade Figure : Parameters of the linear regression etween each participant standard and the common reference standard SRP7 for all participants in the key comparison BIPM.QM-K1 efore and after upgrade of the reference BIPM-SRP Analysis As with the degrees of equivalence, the first important oservation is that the upgrade of BIPM-SRP7 did not change the good agreement with all participants. All slopes have shifted y a very small amount compared to their stated uncertainties. The average and the median of the degrees of equivalence efore and after the upgrade are given in Tale 6: Rapport BIPM-010/07 01 Sep. 10 Page 14 of 16

15 Tale 6: Average and median of the regression parameters of all participants in BIPM.QM-K1 efore and after the upgrade of BIM-SRP7 efore after efore after Slope Intercept / (nmol/mol) Average Median It appears that the measurement results from BIPM-SRP7 are now closer to the centre of the distriution of participants measurement results in the key comparison BIPM.QM-K1. 7. Conclusion The NIST SRP, maintained y the BIPM and used as the reference in the international key comparison BIPM.QM-K1, underwent an upgrade in March 009. This followed the upgrade of almost all the other SRPs maintained y National Metrology Institutes or Designated Institutes. In order to ensure the continuity etween comparisons performed efore and after the upgrade, all degrees of equivalence etween participants and the (upgraded) common reference have een recalculated. As expected, the effect of the upgrade on comparison results was a minor shift of the common reference BIPM-SRP7 towards the centre of the distriution of results. This was expected, ased on the origin of the remaining difference etween BIPM-SRP7 and other upgraded SRPs, which was a numerical correction of the ias on the light path length compared to a physical correction, as will e explained in a forthcoming pulication on SRP upgrades. 8. References [1] Viallon J., Moussay P., Norris J.E., Guenther F.R. and Wielgosz R.I., 006, A study of systematic iases and measurement uncertainties in ozone mole fraction measurements with the NIST Standard Reference Photometer. Metrologia [] Norris J.E., Viallon J., Moussay P., Guenther F.R. and Wielgosz R.I., 008, Results of Temperature Gradient and Path-length Bias Modifications to NIST Ozone Reference Standards. In: Air & Waste Management 101st Annual Conference, (Portland, Oregon) [3] Viallon J., Moussay P., Wielgosz R., Walden J. and Kuronen P., 009, Final report, on-going key comparison BIPM.QM-K1: Ozone at amient level, comparison with FMI, 007. Metrologia [4] Viallon J., Moussay P., Wielgosz R.I., Quincey P. and Sweeney B., 009, Final report, on-going key comparison BIPM.QM-K1: Ozone at amient level, comparison with NPL, 008. Metrologia [5] Bremser W., Viallon J. and Wielgosz R.I., 007, Influence of correlation on the assessment of measurement result compatiility over a dynamic range. Metrologia [6] ISO : 001 Gas analysis - Determination of the composition of caliration gas mixtures - Comparison methods (International Organization for Standardization) [7] Paur R.J., Bass A.M., Norris J.E. and Buckley T.J., 003, Standard Reference Photometer for the Assay of Ozone in caliration Atmospheres. NISTIR 6963 (NIST) Rapport BIPM-010/07 01 Sep. 10 Page 15 of 16

16 [8] Viallon J., Botha A., Wielgosz R.I. and Moussay P., 010, Final report on the ongoing key comparison BIPM.QM-K1: Ozone at amient level, comparison with NMISA, 008. Metrologia Rapport BIPM-010/07 01 Sep. 10 Page 16 of 16

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