CCM V K2 Final Report Feb 11 2009 - BIPM · CCM V K2 Final Report Feb 11 2009 .doc Page 9 of 36 No definitive cause has been determined for the situations reported by the first two

Final Report

CCM.V-K2 Comparison C. Patrick Maggi, David Trowbridge, M Thomas Zubler

Cannon Abstract This report describes the second CCM key comparison in capillary viscometry at nine National Metrology Institutes (NMIs), which was carried out between April and August 2006. Five NMIs, which do not maintain an independent viscosity scale, also took part in this comparison. One participant submitted changes to their originally submitted results for one liquid and requested that results be withdrawn for a second liquid. Six samples of Newtonian liquids with nominal kinematic viscosities of 80 mm²/s at -40°C, 20 mm²/s at -20°C, 5 mm²/s at 20°C, 1300 mm²/s at 20°C, 40 mm²/s at 100°C and 15 mm²/s at 150°C were used to determine the degrees of equivalence between the indi-vidual NMIs and the proposed key comparison reference values (KCRV). From the total number of 54 measurements carried out by all the participating NMIs, 7 measurements (13%) showed deviations from the proposed KCRVs greater than were covered by the measurement uncertainties. This compares to 18 deviations (24%) out of 74 total meas-urements made in the first key comparison.

Linkage to the first key comparison is found at two points - approximately 1300 mm2/s at 20ºC and 40 mm2/s at 100°C. For this key comparison, 13% of the measurements (3 out of 23) on these two points exceeded the proposed KCRVs by more than were covered by the respective measurement uncertainties.

For reference, the first CCM viscosity key comparison (CCM.V-K1) was conducted in 2002.

CCM V K2 Final Report Feb 11 2009 .doc Page 2 of 36

Table of Contents

1. INTRODUCTION ...........................................................................................3

2. LIST OF PARTICIPANTS..............................................................................4

3. VISCOSITY SCALES OF THE PARTICIPANTS...........................................6

4. LIQUID SAMPLES ........................................................................................6

5. ORGANIZATION OF THE COMPARISON ...................................................7

6. COMMENTS ON THE COMPARISON..........................................................7

7. RESULTS OF THE CCM.V-K2 COMPARISON ............................................9

8. REFERENCES ............................................................................................12

9. APPENDICES .............................................................................................13

Appendix A1 Summary of Degrees of Equivalence and Uncertainties, with Charts...................... 13

Appendix A2 Technical Protocol..................................................................................................... 32

Appendix A3 Original Timetable .................................................................................................... 36


1. Introduction

The organization of the second key comparison on viscosity was planned at the CCM Working Group on Viscosity meeting held April 26, 2005 at the BIPM in Sevres, France. Members agreed that all laboratories eligible under the rules of CIPM Mutual Recogni-tion Arrangement (CIPM MRA) could participate in the key comparison. NIST /Cannon Instrument (USA) agreed to be the pilot laboratory for the comparison, with the Physi-kalisch - Technische Bundesanstalt PTB (Germany) offering assistance as a working party. The goal of this second key comparison was to compare viscosity measurement results at temperatures below and above the range of the first key comparison (CCM.V-K1), spe-cifically -40ºC, -20ºC and 150ºC. In addition, measurements at 20°C and 100°C were included to provide linkage to the first key comparison. The proposed key comparison reference values (KCRV) were established from the results submitted by those laboratories maintaining an independent viscosity scale. Nine partici-pating NMI laboratories maintained an independent viscosity scale. Five additional par-ticipants took part in this comparison.

The organization of this key comparison followed the conventions of the first comparison where possible.


2. List of Participants

Dr. Salvatore LOREFICE

Instituto Nazionale di Ricerca Metrologica

Strada Delle Cacce 73

10135 Torino

INRiM Italy

Dr. Maria FERREIRA

Portugues da Qualidade Laborotorio Cental de Metrologia

Rua Antonio Giao 2,

2829-513 Caparica

IPQ * Portugal

Dr. Mohamed MEGHARFI

Laboratoire National de Metrologie et d’Essias

25 Avenue Albert Bartholome

75015 Paris

LNE France

Dr. Mostafa MEKAWY

Thermometry Lab National Institute for Standard

4 Tersa Street

E1Haram Giza

NIS * Egypt

Mr. Martijn VAN RIJN

NMI Van Swinden Laboratorium B.V., Section of Chemistry

PO Box 654, 2500 AR Delft

Thijsseweg 11, 2629 JA Delft

NMi The Netherlands

Dr. Yoshitaka FUJITA

National Metrology Institute of Japan(NMIJ), Fluid Properties Section, National Institute of Advanced Industrial Science and Technology

AIST Central 3,

1-1-1 Umezono Tsukuba, Ibaraki 305-8563

NMIJ Japan

Dr. Xuelin XU

National Institute of Metrology of P.R. China, Department of R&D and Planning (International Cooperation)

No. 18 Beisanhuandonglu,

Chaoyang District, Beijing, 100013

NIM China


Dr. Henning WOLF

Physikalisch-Technische Budnesanstalt, Braunschweig und Berlin

Bundesallee 100

38116 Braunschweig

PTB Germany

Dr. Natalia G. DOMOSTROEVA

19 Moskovsky Pr.

198 005 St. Petersburg

VNIIM Russia

Mr. Dalni MALTA

Instituto Nacional de Metrologia

Av. Nossa Senhora das Gracas 50

Predio 3

INMETRO * Brazil

Dr. Dusan TROCHTA

Slovak Institute of Metrology, Slovensky Metrologicky Ustav Centrum hmotnosti a tlaku, Centre of Mass and Pressure

Karloveska 63

SK-84255 Bratislava

SMU Slovakia

Dr. Dragos BOICIUC

Institutul National de Metrologie

Sos. Vitan-Barzesti 11, Sector 4

Bucuresti 042122

INM * Romania

Mr. Christian BUCHNER

Bundesamt fur Eich und Vermessungswesen (Federal Office of Metrology and Surveying), Masse und verwandte Groben(Mass and Realted Quantities)

Arltgasse 35

A1160 Wein

BEV * Austria

Mr. Thomas ZUBLER

Cannon Instrument Company, National Institute of Standards and Technology

2139 High Tech Rd.

State College, PA 16803

NIST/CANNON United States

* Laboratories not reporting an independent viscosity scale.


3. Viscosity Scales of the Participants

The first key comparison established the validity of the laboratory viscosity scales and their step up procedures from the generally accepted standard value of water (1.0034 mm²/s) [1]. Additional discussions about the viscosity scales of several participants can be found in the first key comparison [2]. The viscosity measurement uncertainty budgets for each participating laboratory are included in Appendix A3.

4. Liquid Samples

Cannon Instrument Company, as pilot laboratory, provided participating laboratories with samples of Newtonian standard liquids for measurement. Each 470 mL sample bottle was labelled as liquid A or liquid B and by the designated test temperature, for example ‘Liquid A -40’. Originally the protocol (Appendix A4) specified that both liquids were poly-alpha-olefins. However, upon pre-testing of the samples by Cannon, it was deter-mined that crystallization of the Liquid A could occur at temperatures above the target test temperature of –40°C. Therefore, the Liquid A was changed to a base stock mineral oil having an established history of use as a viscosity standard by Cannon from 1958 to the present.

The pilot laboratory provided the following revised data for the samples:

Table 4-1: Standard Liquid Material Parameters

Standard

Temperature (°C)

Nominal kinematic viscosity (mm²/s)

Density (g/cm3)

Surface tension

(mN/m)

-40 80 0.9120 43.2

-20 20 0.8973 41.6 Liquid A (mineral oil)

20 5 0.8704 38.2

20 1300 0.8457 31.2

100 40 0.7985 28.4 Liquid B

(poly-alpha-olefin) 150 15 0.7691 26.7


5. Organization of the Comparison

Table 5-1: Chronology of Measurements

Date Who What

April 10, 2006 Pilot Labo-ratory

Shipment of the standard liquids, the data sheets, the timetable, and the technical report to the participants

April 20, 2006 All Partici-pants Start of the comparison measurements

May 3, 2006 All Partici-pants Receipt of the samples by the final participant

July 8, 2006 All Partici-pants Finishing of the comparison measurements

August 2, 2006 All Partici-pants Submission of the final results to the pilot laboratory

March 2007 Pilot Labo-ratory

Submission of Draft Report A, Revision 1 to the partici-pants

The original timetable is shown in Appendix A2.

6. Comments on the Comparison

The sample shipment date was delayed from the original timetable due to a change in material (see section 4) for one of the samples. The samples arrived at the participant’s laboratories between April 12th and May 3rd, 2006. Testing of the samples occurred dur-ing the period of May 8th through July 8th. The pilot laboratory received measurement results by July 31st, with final uncertainty information received on Aug 2nd. Not all par-ticipants chose to perform measurements at each temperature.

Following the compilation of the data for the draft A report, two participants were asked to verify their submitted results. One of the participants reviewed their data and estab-lished that no errors existed. VNIIM reviewed their data and submitted corrections to their reported data for ‘Liquid A–20C’. These corrections appeared to be for typographi-cal or transcription errors. VNIIM also requested that their submitted results for ‘Liquid A-40C’ be withdrawn. These results were withdrawn from the draft A report and noted in associated tables and charts.


Table 6-1: Participation Roster

Standard Liquid A Standard Liquid B Laboratory

-40°C -20°C 20°C 20°C 100°C 150°C

Cannon X X X X X X

INRiM X X X X

LNE X X X X X X NMi X X

NMIJ/AIST X X X X NIM X X

PTB X X X X X X SMU X X

VNIIM withdrawn X X X X

BEV X X X X X

INM X X X X X X INMETRO X X X

IPQ X X NIS X X

* Bold text denotes laboratory with independent viscosity scale The measurement report form was designed to follow the Guide to the Expression of Un-certainty in Measurement [3]. A table for the uncertainty budget was included with the measurement report form, for completion by each participating laboratory.

Several comments were submitted with certain test results: • PTB noted that when measuring liquid B, the first few measurements had con-

tinuously decreasing efflux times and thus used efflux times 6 through 10. The participant did not attribute this to temperature instability.

• NMi noted a problem when using three Ostwald viscometers (two for reporting and a third for validation). Successive efflux times for each filling were consis-tent. However, the average efflux times were significantly different between fill-ings (approximately 1% longer). This trend carried forward to a third filling (an additional 1% longer). This anomaly was observed only on sample Liquid B at 100°C. The participant did not attribute this to temperature instability or im-proper cleaning of the viscometers.

• SMU reported using only 1 filling of the Liquid B at 20°C because the bottle was broken and only one charge of the material could be saved. The sample was fil-tered for glass particulates prior to measurement.


No definitive cause has been determined for the situations reported by the first two of these three participants.

7. Results of the CCM.V-K2 Comparison

The measurement results are compiled in Table A1-1 through A1-6 in Appendix A1. In these tables, a bold font indicates data provided by the participants. Cells with a cross indicate the participant did not submit results for that liquid and temperature. The tem-perature corrected (normalized) kinematic viscosity result for each participant is listed in column V (mm2/s). The columns labeled Dxxx contain the degrees of equivalence of each measurement with the xxx central tendencies: mean, weighted mean, and weighted me-dian. The U(Dxxx) columns are the expanded uncertainty for the degrees of equivalence. Discrepant values [6] at the 5% level of significance are noted by red text in the columns with the heading: U(Dxxx) - |Dxxx|. A graphical representation of the Degree of Equiva-lence to the KCRV is displayed in the Figures A1-1 through A1-6. Degree of Equivalence between two laboratories is defined as the difference in results obtained by the two laboratories [expressed as Dij=Di-Dj,] and the expanded uncertainty of those values at a 95% confidence level [Uij=2(ui

2+uj2)1/2]. The results are given in Ta-

bles A1-1a through A1-6a. Tables A1-1 through A1-6 also list for each fluid and temperature the mean, weighted mean, and weighted median with their respective uncertainties (k=1) as ua and their re-spective relative expanded uncertainties (k=2) as Ur. Associated with each of these po-tential KCRV estimators is the difference between its value and the proposed KCRV value, with the uncertainty (k=2) of the difference as 2*((ua xxx)2 + (ua KCRV)2)½. [7]

A consistency check based on each of the three KCRV candidates was performed using a chi-squared test. [6] Data sets that failed the consistency check, Pr{χ2(υ) > χ2

obs} < 0.05 (υ is the degrees of freedom) are indicated in red text. If a data set failed the consistency check using the weighted mean, then the weighted median was proposed as the KCRV. The consistency check failed for the data sets of ‘Liquid A -20C’, ‘Liquid B 100C’, and ‘Liquid B 150C’. The KCRV values were derived from the results reported by those laboratories that main-tain an independent viscosity scale. A total of fourteen laboratories participated in this comparison. Nine of those participants have performed a calibration program of primary viscometers beginning with water at 20.00ºC (ISO 3666-1998) [1] and stepping up to higher viscosities in a dependent progression. This comparison included two different fluids and five test temperatures. While all labo-ratories reported results at 20°C, some laboratories did not report results for all five tem-peratures (see Table 6-1). The kinematic viscosity results reported by each participant are tabulated in Table A1-1 as V0 and the kinematic viscosity normalized to the target temperature is listed under the column heading, V. The expanded relative uncertainty listed in column Ur is for a 95% confidence interval. The expanded relative uncertainty was calculated by the pilot laboratory using the coverage factor (k, 95% CI) derived from the submitted combined uncertainty and effective degrees of freedom, for those partici-


pants providing that information. The coverage factor submitted by the participants did not always agree with the value calculated by the pilot laboratory. In these cases, the calculated value was reported. Attention should be drawn to the small number of data points available for the data sets of ‘Liquid A -40C’, ‘Liquid A -20C’, and ‘Liquid B 150C’. The mean and weighted mean values and their expanded uncertainties (k=2) were calcu-lated using standard Microsoft EXCEL functions. The weighted median values and their associated expanded uncertainties (k=2) were calculated following a Monte Carlo (MC) procedure [6] using statistical and matrix functions available in MathCAD. The ex-panded uncertainty (k=2) values for the participants without an independent scale were calculated for the differences from the mean and the weighted mean using equation 6 in the CCM.V-K1 Final Report [2]. The expanded uncertainty (k=2) values for the partici-pants without an independent scale were calculated for the differences from the weighted median using the determination of a 95% coverage interval following the procedure de-scribed by Cox in Appendix B of “The Evaluation of Key Comparison Data” [6]. The data analysis was expanded to include consideration of the robust mean [4]. The equations for the calculation of robust mean values and the associated uncertainties are available in the Royal Society of Chemistry paper [5]. Table 7-1 is a tabulation of re-ported viscosities, means, robust means, standard deviations, and coefficients of variation (CofV). A comparison of CofV values suggests a notable dispersion of viscosity values for ‘Liquid A-20C’ and ‘Liquid B100C’. The CofV values for these two samples are approximately an order of magnitude larger than the CofV values for the other data sets. Consequently, further statistical techniques were used to evaluate the data.

Table 7-1: Evaluation of Central Tendencies

-40°C -20°C 20°C 20°C 100°C 150°CCannon 78.952 20.796 4.6216 1367.8 41.534 13.672

INRiM 4.6215 1369.3 41.704 13.671LNE 78.932 20.762 4.6242 1371.1 41.607 13.699NMi 4.6221 42.576

NMIJ / AIST 78.981 4.6268 1368.7 41.610NIM 4.6254 1368.1PTB 78.962 20.784 4.6259 1368.0 41.602 13.726SMU 4.6327 1366.1

VNIIM 21.599 4.6272 1371.3 41.675Arithmetic Mean 78.957 20.985 4.6253 1368.8 41.758 13.692

StdDev 0.0207 0.4095 0.0035 1.7292 0.3647 0.0264Coeff. Of Variation 0.03% 1.95% 0.08% 0.13% 0.87% 0.19%

Robust Mean 78.957 20.815 4.6249 1368.8 41.642 13.692Robust StdDev 0.0234 0.0807 0.0031 1.9598 0.0864 0.0299

Coeff. Of Variation 0.03% 0.39% 0.07% 0.14% 0.21% 0.22%

Inde

pend

ent

Visc

osity

Sca

les

Robust Statistics - Ti CorrectedLiquid A Liquid B


The practice in the previous key comparison CCM.V-K1 [2], of using the En-criterion to quantify the compatibility between a measurement of an individual participant and the reference value, was repeated in this study. The results are tabulated in Table A1-7 in which the columns are arranged in sets of two for each liquid/temperature condition. The first of the two columns is |V-VKCRV|/VKCRV, the second is the result of the first column divided by √(ur

2i+u2

KCRV), which is the “normalized error”, En. Seven measurement val-ues did not fulfill the criteria that |En| ≤1 and are indicated by a yellow field.

Linkage to the first key comparison is found at two points - approximately 1300 mm2/s at 20ºC and 40 mm2/s at 100°C. For this key comparison, 13% of the measurements (3 out of 23) on these two points exceeded the KCRVs by a value corresponding to the measurement uncertainties submitted by those participants.

Table 7-4: Comparison to Past Key Comparison Results

Parameter CCM.V-K1 CCM.V-K2 Comments

Temperatures (°C) 20, 40, 100 -40, -20, 20, 100, 150

Linkage at 20 and 100

Number of Samples 5 6 PAO and mineral oil

Total Participants 18 (11 maintaining independent scale)

14 (9 maintaining independent scale)

Limited participa-tion at -40, -20, and 150°C

Total Measurements 74 54*

Measurement devia-tions greater than measurement uncer-tainty

18 7

Analyzed using the En-criterion as de-fined in CCM.V-K1

% Total Deviations 24% 15% *total does not include one withdrawn measurement.


8. References

1 ISO TR 3666: Viscosity of Water (1998) 2 CCM .V-K1 Intercomparison, Günther Klingenberg and Harro Bauer PTB

3 Guide to the Expression of Uncertainty in Measurement, corrected and re-printed 1995, International Organization of Standardization (Geneva, Switzer-land)

4 “Robust Statistics: A Method of Coping with Outliers” (AMC Technical Brief no. 6 Apr 2001, Analytical Methods Committee, Royal Society of Chemistry 2001)

5 “Robust Statistics-How Not to Reject Outliers”, Analytical Methods Commit-tee, Analyst, December 1989, 114

6 “The Evaluation of Key Comparison Data”, M. G. Cox, Metrologia, 2002, 39, 589-595

7 “Statistical Concepts in Metrology”, Harry H. Ku, in Precision Measurement and Calibration, NBS Special Publication 300 – vol. 1, 1969, page 315-39


9. Appendices

Appendix A1 Summary of Degrees of Equivalence and Uncertainties, with Charts

Table A1-1: Results of the CCM.V-K2 Comparison (Symbols defined within the text)

KCRV

Vo

/ mm2/sTemp.

/ °CV

/ mm2/sUr

[95% CI]

ua

[k=1] / mm2/s

Dmean

/ mm2/s

U(Dmean) [k=2]

/ mm2/s

U(Dmean) - |Dmean| / mm2/s

Dwtmean

/ mm2/s

U(Dwtmean) [k=2]

/ mm2/s

U(Dwtmean) - |Dwtmean| / mm2/s

Dmedian

/ mm2/s

U(Dmedian) [k=2]

/ mm2/s

U(Dmedian) - |Dmedian| / mm2/s

Cannon 78.952 -40.0000 78.952 0.00260 0.103 -0.005 0.165 0.160 -0.021 0.200 0.179 -0.009 0.185 0.176INRiMLNE 78.758 -39.9740 78.932 0.00257 0.101 -0.025 0.163 0.138 -0.041 0.196 0.155 -0.030 0.183 0.153NMiNMIJ / AIST 79.055 -40.0110 78.981 0.00073 0.029 0.025 0.088 0.064 0.009 0.034 0.025 0.020 0.082 0.062NIMPTB 78.970 -40.0012 78.962 0.00129 0.051 0.005 0.106 0.101 -0.011 0.091 0.080 0.001 0.102 0.101SMUVNIIM 78.690 -40.0200 withdrawn

BEVINM 78.480 -39.9920 78.533 0.00257 0.100 -0.424 0.215 -0.208 -0.440 0.207 -0.233 -0.428 0.175 -0.253INMETROIPQNISMean 78.957 0.0003 0.010 0.000 0.029 -0.016 0.052 -0.005 0.075Weighted Mean 78.973 0.0006 0.024 0.016 0.052 0.000 0.068 0.011 0.087Median (MC) 78.961 0.0009 0.036 0.005 0.075 -0.011 0.087 0.000 0.102

consistency check 0.8547 > 0.05 0.9533 > 0.05 0.9052 > 0.05

CCM.V-K2 Comparison - Liquid A at -40ºC

mean weighted mean median (Monte Carlo)

Inde

pend

ent S

cale


Table A1-1a: Results of the CCM.V-K2 Comparison Between Institutes

Lab j

Lab iD i U i D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij

Cannon -0.021 0.200 0.020 0.288 -0.029 0.213 -0.010 0.230 0.419 0.287LNE -0.041 0.196 -0.020 0.288 -0.050 0.210 -0.030 0.227 0.399 0.285NMIJ / AIST 0.009 0.034 0.029 0.213 0.050 0.210 0.019 0.118 0.448 0.209PTB -0.011 0.091 0.010 0.230 0.030 0.227 -0.019 0.118 0.429 0.226INM -0.440 0.207 -0.419 0.287 -0.399 0.285 -0.448 0.209 -0.429 0.226

/ mm2/s/ mm2/s / mm2/s / mm2/s / mm2/s

NMIJ / AIST PTB INM

CCM.V-K2 Comparison - Liquid A at -40ºC Degrees of Equivalence Between Institutes

LNE

/ mm2/s

Cannon



KCRV

Vo

/ mm2/sTemp.

/ °CV

/ mm2/s

Ur

[95% CI]

ua

[k=1] / mm2/s

Dmean

/ mm2/s

U(Dmean) [k=2]

/ mm2/s


Dwtmean

/ mm2/s

U(Dwtmean) [k=2]

/ mm2/s


Dmedian

/ mm2/s

U(Dmedian) [k=2]

/ mm2/s


Cannon 20.796 -20.0000 20.796 0.00260 0.027 -0.189 0.086 -0.103 0.013 0.052 0.038 0.005 0.033 0.028INRiMLNE 20.732 -19.9730 20.762 0.00175 0.018 -0.223 0.082 -0.142 -0.021 0.033 0.012 -0.030 0.038 0.008NMiNMIJ / AISTNIMPTB 20.784 -20.0000 20.784 0.00087 0.009 -0.201 0.079 -0.123 0.001 0.010 0.009 -0.008 0.026 0.018SMUVNIIM 21.610 -20.0100 21.599 0.01400 0.151 0.614 0.228 -0.386 0.816 0.302 -0.514 0.807 0.298 -0.509

BEV 20.964 -20.0300 20.931 0.01200 0.126 -0.054 0.263 0.209 0.148 0.252 0.104 0.139 0.225 0.086INM 20.769 -20.0022 20.767 0.00224 0.023 -0.218 0.090 -0.128 -0.016 0.049 0.033 -0.025 0.047 0.022INMETROIPQNISMean 20.985 0.01950 0.205 0.000 0.579 0.202 0.410 0.193 0.410Weighted Mean 20.783 0.00075 0.008 -0.202 0.410 0.000 0.022 -0.009 0.030Median (MC) 20.791 0.00122 0.013 -0.193 0.410 0.009 0.030 0.000 0.036

consistency check 7.2E-152 < 0.05 9.99E-07 < 0.05 1.08E-06 < 0.05

Inde

pend

ent S

cale


CCM.V-K2 Comparison - Liquid A at -20ºC



Lab j

Lab iD i U i D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij

Cannon 0.005 0.033 0.034 0.065 0.012 0.057 -0.803 0.307 -0.135 0.257 0.029 0.071LNE -0.030 0.038 -0.034 0.065 -0.022 0.041 -0.837 0.305 -0.169 0.254 -0.005 0.059PTB -0.008 0.026 -0.012 0.057 0.022 0.041 -0.815 0.303 -0.147 0.252 0.017 0.050VNIIM 0.807 0.298 0.803 0.307 0.837 0.305 0.815 0.303 0.668 0.393 0.832 0.306BEV 0.139 0.225 0.135 0.257 0.169 0.254 0.147 0.252 -0.668 0.393 0.164 0.256INM -0.025 0.047 -0.029 0.071 0.005 0.059 -0.017 0.050 -0.832 0.306 -0.164 0.256

/ mm2/s / mm2/s

VNIIM BEVCannon LNE PTB

CCM.V-K2 Comparison - Liquid A at -20ºC Degrees of Equivalence Between Institutes

/ mm2/s / mm2/s/ mm2/s

INM

/ mm2/s / mm2/s



KCRV

Vo

/ mm2/sTemp.

/ °CV

/ mm2/s

Ur

[95% CI]

ua

[k=1] / mm2/s

Dmean

/ mm2/s

U(Dmean) [k=2]

/ mm2/s


Dwtmean

/ mm2/s

U(Dwtmean) [k=2]

/ mm2/s


Dmedian

/ mm2/s

U(Dmedian) [k=2]

/ mm2/s


Cannon 4.6216 20.0000 4.6216 0.00160 0.0037 -0.0037 0.0068 0.0032 -0.0043 0.0073 0.0030 -0.0037 0.0071 0.0034INRiM 4.6215 20.0001 4.6215 0.00092 0.0021 -0.0038 0.0043 0.0005 -0.0044 0.0041 -0.0003 -0.0037 0.0042 0.0005LNE 4.6242 20.0000 4.6242 0.00156 0.0036 -0.0011 0.0067 0.0056 -0.0017 0.0071 0.0054 -0.0011 0.0068 0.0058NMi 4.6221 20.0000 4.6221 0.00150 0.0035 -0.0032 0.0065 0.0033 -0.0038 0.0068 0.0030 -0.0032 0.0066 0.0035NMIJ / AIST 4.6277 19.9930 4.6268 0.00038 0.0009 0.0016 0.0026 0.0010 0.0009 0.0013 0.0003 0.0016 0.0026 0.0010NIM 4.6253 20.0010 4.6254 0.00108 0.0025 0.0001 0.0048 0.0046 -0.0005 0.0047 0.0043 0.0002 0.0048 0.0046PTB 4.6260 19.9995 4.6259 0.00053 0.0012 0.0007 0.0030 0.0024 0.0000 0.0022 0.0021 0.0007 0.0032 0.0025SMU 4.6327 20.0000 4.6327 0.00156 0.0037 0.0074 0.0068 -0.0007 0.0068 0.0072 0.0004 0.0074 0.0072 -0.0003VNIIM 4.6272 20.0000 4.6272 0.00200 0.0046 0.0019 0.0084 0.0065 0.0013 0.0092 0.0079 0.0019 0.0088 0.0068

BEV 4.6472 19.7630 4.6186 0.00300 0.0070 -0.0067 0.0141 0.0074 -0.0073 0.0140 0.0067 -0.0067 0.0132 0.0065INM 4.6251 20.0008 4.6252 0.00167 0.0038 -0.0001 0.0080 0.0079 -0.0007 0.0078 0.0071 -0.0001 0.0074 0.0073INMETRO 4.6230 20.0300 4.6266 0.00686 0.0162 0.0013 0.0324 0.0311 0.0007 0.0324 0.0317 0.0014 0.0317 0.0303IPQ 4.6208 20.0990 4.6327 0.00322 0.0074 0.0074 0.0149 0.0075 0.0068 0.0148 0.0080 0.0074 0.0140 0.0066NIS 4.5988 20.0000 4.5988 0.00660 0.0152 -0.0265 0.0304 0.0039 -0.0271 0.0304 0.0032 -0.0265 0.0300 0.0035

Mean 4.6253 0.00051 0.0012 0.0000 0.0033 -0.0006 0.0027 0.0000 0.0034Weighted Mean 4.6259 0.00026 0.0006 0.0006 0.0027 0.0000 0.0017 0.0006 0.0027Median (MC) 4.6253 0.00051 0.0012 0.0000 0.0034 -0.0006 0.0027 0.0000 0.0034


CCM.V-K2 Comparison - Liquid A at 20ºC

Inde

pend

ent S

cale




Lab j

Lab iD i U i D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij

Cannon -0.0043 0.0073 0.0001 0.0085 -0.0026 0.0103 -0.0005 0.0101 -0.0052 0.0076 -0.0038 0.0089 -0.0043 0.0078INRiM -0.0044 0.0041 -0.0001 0.0085 -0.0027 0.0084 -0.0006 0.0082 -0.0053 0.0046 -0.0039 0.0065 -0.0044 0.0050LNE -0.0017 0.0071 0.0026 0.0103 0.0027 0.0084 0.0021 0.0100 -0.0026 0.0074 -0.0012 0.0087 -0.0017 0.0076NMi -0.0038 0.0068 0.0005 0.0101 0.0006 0.0082 -0.0021 0.0100 -0.0047 0.0072 -0.0033 0.0085 -0.0038 0.0074NMIJ / AIST 0.0009 0.0013 0.0052 0.0076 0.0053 0.0046 0.0026 0.0074 0.0047 0.0072 0.0014 0.0052 0.0009 0.0031NIM -0.0005 0.0047 0.0038 0.0089 0.0039 0.0065 0.0012 0.0087 0.0033 0.0085 -0.0014 0.0052 -0.0005 0.0055PTB 0.0000 0.0022 0.0043 0.0078 0.0044 0.0050 0.0017 0.0076 0.0038 0.0074 -0.0009 0.0031 0.0005 0.0055SMU 0.0068 0.0072 0.0111 0.0104 0.0112 0.0085 0.0085 0.0103 0.0106 0.0101 0.0059 0.0075 0.0073 0.0088 0.0068 0.0077VNIIM 0.0013 0.0092 0.0056 0.0118 0.0057 0.0102 0.0030 0.0117 0.0051 0.0116 0.0004 0.0094 0.0018 0.0105 0.0013 0.0096BEV -0.0073 0.0140 -0.0030 0.0158 -0.0029 0.0146 -0.0056 0.0157 -0.0035 0.0156 -0.0083 0.0141 -0.0069 0.0148 -0.0074 0.0142INM -0.0007 0.0078 0.0036 0.0107 0.0037 0.0088 0.0010 0.0105 0.0031 0.0103 -0.0016 0.0079 -0.0002 0.0091 -0.0007 0.0081INMETRO 0.0007 0.0324 0.0050 0.0332 0.0051 0.0326 0.0024 0.0332 0.0045 0.0331 -0.0002 0.0324 0.0012 0.0327 0.0007 0.0325IPQ 0.0068 0.0148 0.0111 0.0165 0.0112 0.0154 0.0085 0.0164 0.0106 0.0163 0.0059 0.0149 0.0073 0.0156 0.0068 0.0150NIS -0.0271 0.0304 -0.0229 0.0312 -0.0228 0.0307 -0.0255 0.0312 -0.0233 0.0311 -0.0281 0.0304 -0.0267 0.0307 -0.0272 0.0305

D i U i D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij

Cannon -0.0043 0.0073 -0.0111 0.0104 -0.0056 0.0118 0.0030 0.0158 -0.0036 0.0107 -0.0050 0.0332 -0.0111 0.0165 0.0229 0.0312INRiM -0.0044 0.0041 -0.0112 0.0085 -0.0057 0.0102 0.0029 0.0146 -0.0037 0.0088 -0.0051 0.0326 -0.0112 0.0154 0.0228 0.0307LNE -0.0017 0.0071 -0.0085 0.0103 -0.0030 0.0117 0.0056 0.0157 -0.0010 0.0105 -0.0024 0.0332 -0.0085 0.0164 0.0255 0.0312NMi -0.0038 0.0068 -0.0106 0.0101 -0.0051 0.0116 0.0035 0.0156 -0.0031 0.0103 -0.0045 0.0331 -0.0106 0.0163 0.0233 0.0311NMIJ / AIST 0.0009 0.0013 -0.0059 0.0075 -0.0004 0.0094 0.0083 0.0141 0.0016 0.0079 0.0002 0.0324 -0.0059 0.0149 0.0281 0.0304NIM -0.0005 0.0047 -0.0073 0.0088 -0.0018 0.0105 0.0069 0.0148 0.0002 0.0091 -0.0012 0.0327 -0.0073 0.0156 0.0267 0.0307PTB 0.0000 0.0022 -0.0068 0.0077 -0.0013 0.0096 0.0074 0.0142 0.0007 0.0081 -0.0007 0.0325 -0.0068 0.0150 0.0272 0.0305SMU 0.0068 0.0072 0.0055 0.0118 0.0141 0.0157 0.0075 0.0106 0.0061 0.0332 0.0000 0.0165 0.0339 0.0312VNIIM 0.0013 0.0092 -0.0055 0.0118 0.0086 0.0167 0.0020 0.0120 0.0006 0.0337 -0.0055 0.0174 0.0285 0.0317BEV -0.0073 0.0140 -0.0141 0.0157 -0.0086 0.0167 -0.0066 0.0159 -0.0080 0.0352 -0.0141 0.0203 0.0198 0.0334INM -0.0007 0.0078 -0.0075 0.0106 -0.0020 0.0120 0.0066 0.0159 -0.0014 0.0333 -0.0075 0.0167 0.0264 0.0313INMETRO 0.0007 0.0324 -0.0061 0.0332 -0.0006 0.0337 0.0080 0.0352 0.0014 0.0333 -0.0061 0.0356 0.0279 0.0444IPQ 0.0068 0.0148 0.0000 0.0165 0.0055 0.0174 0.0141 0.0203 0.0075 0.0167 0.0061 0.0356 0.0339 0.0338NIS -0.0271 0.0304 -0.0339 0.0312 -0.0285 0.0317 -0.0198 0.0334 -0.0264 0.0313 -0.0279 0.0444 -0.0339 0.0338

CCM.V-K2 Comparison - Liquid A at 20ºC Degrees of Equivalence Between Institutes

/ mm2/s

INMETRO

/ mm2/s / mm2/s / mm2/s

Cannon PTB

/ mm2/s

NIS

/ mm2/s

/ mm2/s

/ mm2/s

/ mm2/s / mm2/s / mm2/s

SMU VNIIM BEV

INRiM LNE NMi

/ mm2/s

IPQ

/ mm2/s

INM

NMIJ / AIST NIM

/ mm2/s / mm2/s / mm2/s



KCRV

Vo

/ mm2/sTemp.

/ °CV

/ mm2/sUr

[95% CI]

ua

[k=1] / mm2/s

Dmean

/ mm2/s

U(Dmean) [k=2]

/ mm2/s


Dwtmean

/ mm2/s

U(Dwtmean) [k=2]

/ mm2/s


Dmedian

/ mm2/s

U(Dmedian) [k=2]

/ mm2/s


Cannon 1367.8 20.0000 1367.8 0.00380 2.6 -1.0 4.7 3.7 -1.0 5.1 4.2 -0.9 4.9 4.0INRiM 1369.3 20.0001 1369.3 0.00156 1.1 0.5 2.2 1.8 0.5 2.0 1.5 0.6 2.1 1.5LNE 1371.1 20.0000 1371.1 0.00373 2.6 2.3 4.6 2.3 2.4 5.1 2.7 2.4 4.9 2.5NMiNMIJ / AIST 1369.4 19.9930 1368.7 0.00089 0.6 -0.1 1.6 1.6 0.0 1.0 0.9 0.0 1.5 1.5NIM 1368.2 19.9990 1368.1 0.00200 1.3 -0.7 2.6 1.9 -0.6 2.5 1.9 -0.6 2.5 1.9PTB 1367.9 20.0010 1368.0 0.00119 0.8 -0.8 1.9 1.1 -0.7 1.4 0.7 -0.7 1.7 1.0SMU 1366.1 20.0000 1366.1 0.00334 2.3 -2.7 4.2 1.5 -2.6 4.5 1.9 -2.6 4.3 1.7VNIIM 1371.3 20.0000 1371.3 0.00200 1.4 2.5 2.7 0.2 2.5 2.6 0.1 2.5 2.7 0.2

BEV 1363.5 19.9722 1361.0 0.01000 6.8 -7.8 13.7 5.9 -7.7 13.7 5.9 -7.7 13.1 5.4INM 1368.0 20.0013 1368.1 0.00220 1.5 -0.7 3.3 2.6 -0.6 3.1 2.5 -0.6 2.9 2.3INMETRO 1368.0 20.0030 1368.3 0.00960 6.7 -0.5 13.5 12.9 -0.5 13.4 12.9 -0.5 13.1 12.6IPQ 1368.6 19.9990 1368.5 0.00495 3.4 -0.3 7.0 6.7 -0.2 6.9 6.6 -0.2 6.8 6.6NIS 1368.5 20.0000 1368.5 0.02370 16.2 -0.4 32.5 32.1 -0.3 32.4 32.1 -0.3 31.8 31.5

Mean 1368.8 0.00089 0.6 0.0 1.7 0.1 1.5 0.1 1.7Weighted Mean 1368.8 0.00057 0.4 -0.1 1.5 0.0 1.1 0.0 1.4Median (MC) 1368.7 0.00081 0.6 -0.1 1.7 0.0 1.4 0.0 1.6


Inde

pend

ent S

cale


CCM.V-K2 Comparison - Liquid B at 20ºC



Lab j


Cannon -1.0 5.1 -1.5 5.6 -3.3 7.3 -0.9 5.3 -0.3 5.8 -0.2 5.5INRiM 0.5 2.0 1.5 5.6 -1.8 5.6 0.6 2.5 1.2 3.4 1.3 2.7LNE 2.4 5.1 3.3 7.3 1.8 5.6 2.4 5.3 3.0 5.8 3.1 5.4NMIJ / AIST 0.0 1.0 0.9 5.3 -0.6 2.5 -2.4 5.3 0.6 2.9 0.7 2.1NIM -0.6 2.5 0.3 5.8 -1.2 3.4 -3.0 5.8 -0.6 2.9 0.1 3.1PTB -0.7 1.4 0.2 5.5 -1.3 2.7 -3.1 5.4 -0.7 2.1 -0.1 3.1SMU -2.6 4.5 -1.7 6.9 -3.2 5.1 -5.0 6.9 -2.6 4.8 -2.0 5.3 -1.9 4.9VNIIM 2.5 2.6 3.5 5.9 2.0 3.5 0.2 5.8 2.5 3.0 3.2 3.8 3.2 3.2BEV -7.7 13.7 -6.8 14.6 -8.3 13.8 -10.1 14.6 -7.7 13.7 -7.1 13.9 -7.0 13.7INM -0.6 3.1 0.3 6.0 -1.1 3.7 -3.0 5.9 -0.6 3.3 0.0 4.0 0.1 3.4INMETRO -0.5 13.4 0.5 14.4 -1.0 13.6 -2.8 14.4 -0.5 13.5 0.2 13.7 0.2 13.5IPQ -0.2 6.9 0.7 8.6 -0.8 7.2 -2.6 8.5 -0.2 7.0 0.4 7.3 0.5 7.0NIS -0.3 32.4 0.7 32.8 -0.8 32.5 -2.7 32.8 -0.3 32.5 0.3 32.5 0.4 32.5

D i U i D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij

Cannon -1.0 5.1 1.7 6.9 -3.5 5.9 6.8 14.6 -0.3 6.0 -0.5 14.4 -0.7 8.6 -0.7 32.8INRiM 0.5 2.0 3.2 5.1 -2.0 3.5 8.3 13.8 1.1 3.7 1.0 13.6 0.8 7.2 0.8 32.5LNE 2.4 5.1 5.0 6.9 -0.2 5.8 10.1 14.6 3.0 5.9 2.8 14.4 2.6 8.5 2.7 32.8NMIJ / AIST 0.0 1.0 2.6 4.8 -2.5 3.0 7.7 13.7 0.6 3.3 0.5 13.5 0.2 7.0 0.3 32.5NIM -0.6 2.5 2.0 5.3 -3.2 3.8 7.1 13.9 0.0 4.0 -0.2 13.7 -0.4 7.3 -0.3 32.5PTB -0.7 1.4 1.9 4.9 -3.2 3.2 7.0 13.7 -0.1 3.4 -0.2 13.5 -0.5 7.0 -0.4 32.5SMU -2.6 4.5 -5.1 5.4 5.1 14.4 -2.0 5.5 -2.1 14.2 -2.4 8.2 -2.3 32.8VNIIM 2.5 2.6 5.1 5.4 10.2 13.9 3.1 4.1 3.0 13.7 2.8 7.4 2.8 32.5BEV -7.7 13.7 -5.1 14.4 -10.2 13.9 -7.1 14.0 -7.2 19.1 -7.5 15.3 -7.4 35.2INM -0.6 3.1 2.0 5.5 -3.1 4.1 7.1 14.0 -0.1 13.7 -0.4 7.5 -0.3 32.6INMETRO -0.5 13.4 2.1 14.2 -3.0 13.7 7.2 19.1 0.1 13.7 -0.2 15.1 -0.2 35.1IPQ -0.2 6.9 2.4 8.2 -2.8 7.4 7.5 15.3 0.4 7.5 0.2 15.1 0.1 33.1NIS -0.3 32.4 2.3 32.8 -2.8 32.5 7.4 35.2 0.3 32.6 0.2 35.1 -0.1 33.1

PTB

/ mm2/s

IPQ

/ mm2/s/ mm2/s

INM INMETRO NIS

/ mm2/s

SMU VNIIM BEV

/ mm2/s / mm2/s / mm2/s / mm2/s

CCM.V-K2 Comparison - Liquid B at 20ºC Degrees of Equivalence Between Institutes

/ mm2/s

Cannon INRiM LNE NMIJ / AIST NIM

/ mm2/s

/ mm2/s / mm2/s / mm2/s / mm2/s/ mm2/s



KCRV

Vo

/ mm2/sTemp.

/ °CV

/ mm2/s

Ur

[95% CI]

ua

[k=1] / mm2/s

Dmean

/ mm2/s

U(Dmean) [k=2]

/ mm2/s


Dwtmean

/ mm2/s

U(Dwtmean) [k=2]

/ mm2/s


Dmedian

/ mm2/s

U(Dmedian) [k=2]

/ mm2/s


Cannon 41.534 100.000 41.534 0.00260 0.054 -0.224 0.136 -0.088 -0.078 0.106 0.028 -0.088 0.101 0.013INRiM 41.704 100.000 41.704 0.00183 0.039 -0.054 0.120 0.066 0.092 0.074 -0.017 0.082 0.078 -0.003LNE 41.605 100.002 41.607 0.00239 0.050 -0.151 0.131 -0.020 -0.005 0.097 0.092 -0.015 0.089 0.074NMi 42.576 100.000 42.576 0.01563 0.299 0.818 0.515 -0.303 0.964 0.597 -0.367 0.954 0.588 -0.366NMIJ / AIST 41.580 100.026 41.610 0.00069 0.015 -0.148 0.104 -0.045 -0.002 0.021 0.018 -0.012 0.051 0.039NIMPTB 41.602 100.000 41.602 0.00083 0.017 -0.157 0.105 -0.052 -0.011 0.028 0.018 -0.021 0.050 0.030SMUVNIIM 41.675 100.000 41.675 0.00800 0.167 -0.083 0.299 0.216 0.063 0.333 0.270 0.053 0.317 0.264

BEV 43.752 100.006 43.759 0.02400 0.525 2.001 1.055 -0.946 2.147 1.050 -1.097 2.137 1.021 -1.116INM 41.504 100.002 41.506 0.00200 0.042 -0.252 0.131 -0.121 -0.106 0.086 -0.021 -0.116 0.085 -0.031INMETRO 41.600 100.051 41.659 0.01000 0.212 -0.099 0.436 0.337 0.047 0.425 0.378 0.037 0.397 0.360IPQNISMean 41.758 0.00660 0.138 0.000 0.390 0.146 0.276 0.136 0.279Weighted Mean 41.612 0.00049 0.010 -0.146 0.276 0.000 0.029 -0.010 0.050Median (MC) 41.622 0.00111 0.023 -0.136 0.279 0.010 0.050 0.000 0.065



Inde

pend

ent S

cale




Lab j

Lab iD i U i D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij

Cannon -0.088 0.101 -0.170 0.133 -0.073 0.147 -1.042 0.607 -0.076 0.112INRiM 0.082 0.078 0.170 0.133 0.097 0.126 -0.872 0.602 0.094 0.082LNE -0.015 0.089 0.073 0.147 -0.097 0.126 -0.968 0.606 -0.003 0.104NMi 0.954 0.588 1.042 0.607 0.872 0.602 0.968 0.606 0.966 0.598NMIJ / AIST -0.012 0.051 0.076 0.112 -0.094 0.082 0.003 0.104 -0.966 0.598PTB -0.021 0.050 0.068 0.114 -0.102 0.085 -0.006 0.105 -0.974 0.598 -0.008 0.045VNIIM 0.053 0.317 0.141 0.350 -0.029 0.342 0.068 0.348 -0.901 0.684 0.065 0.335BEV 2.137 1.021 2.225 1.056 2.055 1.053 2.152 1.055 1.183 1.208 2.149 1.050INM -0.116 0.085 -0.028 0.136 -0.198 0.113 -0.101 0.129 -1.070 0.603 -0.104 0.088INMETRO 0.037 0.397 0.125 0.438 -0.045 0.431 0.051 0.436 -0.917 0.733 0.049 0.425

D i U i D ij U ij D ij U ij D ij U ij D ij U ij D ij U ij

Cannon -0.088 0.101 -0.068 -0.141 0.350 -2.225 1.056 0.028 0.136 -0.125 0.438INRiM 0.082 0.078 0.102 0.085 0.029 0.342 -2.055 1.053 0.198 0.113 0.045 0.431LNE -0.015 0.089 0.006 0.105 -0.068 0.348 -2.152 1.055 0.101 0.129 -0.051 0.436NMi 0.954 0.588 0.974 0.598 0.901 0.684 -1.183 1.208 1.070 0.603 0.917 0.733NMIJ / AIST -0.012 0.051 0.008 0.045 -0.065 0.335 -2.149 1.050 0.104 0.088 -0.049 0.425PTB -0.021 0.050 -0.073 0.335 -2.158 1.051 0.095 0.090 -0.057 0.426VNIIM 0.053 0.317 0.073 0.335 -2.084 1.102 0.169 0.344 0.016 0.540BEV 2.137 1.021 2.158 1.051 2.084 1.102 2.253 1.053 2.101 1.133INM -0.116 0.085 -0.095 0.090 -0.169 0.344 -2.253 1.053 -0.153 0.432INMETRO 0.037 0.397 0.057 0.426 -0.016 0.540 -2.101 1.133 0.153 0.432


Cannon INRiM LNE NMi NMIJ / AIST

/ mm2/s / mm2/s / mm2/s / mm2/s / mm2/s/ mm2/s

INM INMETRO

/ mm2/s / mm2/s / mm2/s / mm2/s / mm2/s / mm2/s

PTB VNIIM BEV



KCRV

Vo

/ mm2/sTemp.

/ °CV

/ mm2/s

Ur

[95% CI]

ua

[k=1] / mm2/s

Dmean

/ mm2/s

U(Dmean) [k=2]

/ mm2/s


Dwtmean

/ mm2/s

U(Dwtmean) [k=2]

/ mm2/s


Dmedian

/ mm2/s

U(Dmedian) [k=2]

/ mm2/s


Cannon 13.672 150.000 13.672 0.00260 0.018 -0.020 0.028 0.008 -0.032 0.034 0.002 -0.018 0.028 0.011INRiM 13.670 150.003 13.671 0.00164 0.011 -0.021 0.020 -0.001 -0.033 0.020 -0.013 -0.019 0.022 0.003LNE 13.699 150.002 13.699 0.00157 0.011 0.007 0.020 0.012 -0.004 0.019 0.015 0.010 0.017 0.007NMiNMIJ / AISTNIMPTB 13.727 149.998 13.726 0.00110 0.008 0.034 0.016 -0.018 0.023 0.011 -0.012 0.037 0.022 -0.015SMUVNIIMBEV 14.330 150.614 14.458 0.00600 0.043 0.766 0.087 -0.679 0.754 0.087 -0.667 0.768 0.075 -0.693INM 13.705 150.002 13.705 0.00144 0.010 0.013 0.023 0.010 0.002 0.022 0.020 0.016 0.025 0.009INMETROIPQNISMean 13.692 0.00192 0.013 0.000 0.037 -0.012 0.028 0.003 0.031Weighted Mean 13.704 0.00076 0.005 0.012 0.028 0.000 0.015 0.014 0.019Median (MC) 13.690 0.00117 0.008 -0.003 0.031 -0.014 0.019 0.000 0.023



Inde

pend

ent S

cale




Lab j


Cannon -0.018 0.028 0.001 0.042 -0.027 0.042 -0.054 0.039 -0.786 0.093 -0.033 0.041INRiM -0.019 0.022 -0.001 0.042 -0.029 0.031 -0.056 0.027 -0.787 0.089 -0.035 0.030LNE 0.010 0.017 0.027 0.042 0.029 0.031 -0.027 0.026 -0.758 0.089 -0.006 0.029PTB 0.037 0.022 0.054 0.039 0.056 0.027 0.027 0.026 -0.731 0.087 0.021 0.025BEV 0.768 0.075 0.786 0.093 0.787 0.089 0.758 0.089 0.731 0.087 0.752 0.088INM 0.016 0.025 0.033 0.041 0.035 0.030 0.006 0.029 -0.021 0.025 -0.752 0.088

/ mm2/s

Cannon INRiM LNE PTB BEV

/ mm2/s / mm2/s / mm2/s / mm2/s


INM

/ mm2/s / mm2/s


Table A1-7: Calculated Values of Normalized Error

|V-VKCRV|/ prev. col. / |V-VKCRV|/ prev. col. / |V-VKCRV|/ prev. col. / |V-VKCRV|/ prev. col. / |V-VKCRV|/ prev. col. / |V-VKCRV|/ prev. col. /VKCRV (ur

2+u2KCRV)½ VKCRV (ur





2+u2KCRV)½

Cannon 2.6E-04 0.0980 2.2E-04 0.0760 9.3E-04 0.5728 7.0E-04 0.1817 2.1E-03 0.7494 1.3E-03 0.4487INRiM 9.5E-04 0.9947 3.9E-04 0.2350 2.0E-03 0.9183 1.4E-03 0.6862LNE 5.2E-04 0.1973 1.4E-03 0.6704 3.7E-04 0.2325 1.7E-03 0.4552 3.6E-04 0.1353 7.2E-04 0.3677NMi 8.2E-04 0.5380 0.0000 2.3E-02 1.4622NMIJ / AIST 1.1E-04 0.1148 2.0E-04 0.4378 1.9E-05 0.0183 2.9E-04 0.2244NIM 1.0E-04 0.0929 4.7E-04 0.2271PTB 1.4E-04 0.0954 3.8E-04 0.2557 6.9E-06 0.0117 5.3E-04 0.4021 4.9E-04 0.3567 2.7E-03 1.6690SMU 1.5E-03 0.9281 1.9E-03 0.5688VNIIM 3.9E-02 2.7603 2.8E-04 0.1395 1.8E-03 0.8831 1.3E-03 0.1573

BEV 6.7E-03 0.5536 1.6E-03 0.5231 5.6E-03 0.5620 5.1E-02 2.1372 5.6E-02 9.2547INM 5.6E-03 2.1082 1.2E-03 0.4696 1.5E-04 0.0897 4.4E-04 0.1954 2.8E-03 1.2183 1.2E-03 0.6249INMETRO 1.5E-04 0.0223 3.5E-04 0.0369 8.8E-04 0.0876IPQ 1.5E-03 0.4552 1.8E-04 0.0356NIS 5.9E-03 0.8885 2.2E-04 0.0093

Liquid B 150CLiquid A -40C Liquid A -20C Liquid A 20C Liquid B 20CCCM.V-K2 Comparison - Calculated Values of Normalized Error, En

Liquid B 100C


Figure A1-1: Liquid A -40C Degrees of Equivalence

-1.0

-0.8

-0.6

-0.4

-0.2

0.0

0.2

0.4

0.6

0.8

1.0

V - V

KC

RV /

mm

2 /s

wei

ghte

d m

ean

with IVS -0.021 -0.041 0.009 -0.011

w/o IVS -0.440

uh 0.068 0.068 0.068 0.068 0.068 0.068 0.068 0.068 0.068 0.068 0.068 0.068 0.068 0.068

ul -0.068 -0.068 -0.068 -0.068 -0.068 -0.068 -0.068 -0.068 -0.068 -0.068 -0.068 -0.068 -0.068 -0.068

Cannon INRiM LNE NMi NMIJ / AIST NIM PTB SMU VNIIM BEV INM INMETRO IPQ NIS

withdrawn


Figure A1-2: Liquid A -20C Degrees of Equivalence

-1

-0.8

-0.6

-0.4

-0.2

0

0.2

0.4

0.6

0.8

1

V - V

KC

RV /

mm

2 /s

med

ian

with IVS 0.005 -0.030 -0.008 0.807

w/o IVS 0.139 -0.025

uh 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272 0.035826272

"ul" -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272 -0.035826272



Figure A1-3: Liquid A 20C Degrees of Equivalence

-0.06

-0.05

-0.04

-0.03

-0.02

-0.01

0.00

0.01

0.02

0.03

0.04

0.05

0.06

V - V

KC

RV

/ m

m2 /s

wei

ghte

d m

ean

with IVS -0.0043 -0.0044 -0.0017 -0.0038 0.0009 -0.0005 0.0000 0.0068 0.0013

w/o IVS -0.0073 -0.0007 0.0007 0.0068 -0.0271

uh 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752 0.001729752

"ul" -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752 -0.001729752



Figure A1-4: Liquid B 20C Degrees of Equivalence

-10

-8

-6

-4

-2

0

2

4

6

8

10

V - V

KC

RV

/ m

m2 /s

wei

ghte

d m

ean

with IVS -1.0 0.5 2.4 0.0 -0.6 -0.7 -2.6 2.5

w/o IVS -7.7 -0.6 -0.5 -0.2 -0.3

uh 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008 1.10395008

ul -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008 -1.10395008




-3.0

-2.5

-2.0

-1.5

-1.0

-0.5

0.0

0.5

1.0

1.5

2.0

2.5

3.0

V - V

KC

RV /

mm

2 /s

med

ian

with IVS -0.088 0.082 -0.015 0.954 -0.012 -0.021 0.053

w/o IVS 2.137 -0.116 0.037

uh 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995 0.065050995

ul -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995 -0.065050995




-0.20

-0.15

-0.10

-0.05

0.00

0.05

0.10

0.15

0.20

V - V

KC

RV /

mm

2 /s

med

ian

with IVS -0.018 -0.019 0.010 0.037

w/o IVS 0.768 0.016

uh 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956 0.022700956

ul -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956 -0.022700956



Appendix A2 Technical Protocol

Technical Protocol for the CCM Key Comparison of the Viscosity

CCM.V–K2 Pilot Laboratory: NIST / Cannon Instrument (J. Whetstone, G. Strouse / P.

Maggi, D. Trowbridge, T. Zubler) Working Party: Physikalisch–Technische Bundesanstalt (H. Bauer)

Outline of the CCM key comparison of the viscosity This key comparison, CCM.V-K2, has been undertaken by the CCM Working Group on Viscosity to compare the viscosity determinations of participating labo-ratories. The four objectives are:

• Compare viscosity measurements at temperatures outside of the range of the first key comparison.

• Compare viscosity measurements made at -40ºC and at -20ºC using a stan-dard fluid designated as Liquid A.

• Compare viscosity measurements made at 150ºC using a standard fluid des-ignated as Liquid B.

• Compare results from this key comparison to results from the previous key comparison using viscosity measurements made at 20ºC and at 100ºC involv-ing both Liquid A and Liquid B.

Certain participants have performed a calibration program of primary viscometers beginning with water at 20.00ºC (ISO 3666-1998) [1] and stepping up to higher viscosities in a dependent progression. Results from these participants will con-tribute to the reference value obtained from this comparison. The non-contributing participants will be providing viscosities determined from viscometers calibrated by other metrology institutes. (A list of the addresses of the contribut-ing and non-contributing participants will be established later, coordinated by Dr. Davis.) The results of this comparison will be of interest for the entries concerning vis-cosity in the Calibration and Measurement Capability (CMC) tables.

Purpose of this document The purpose of this document is to provide the participating laboratories with in-structions for the handling of the liquid samples and to report on the measure-ment results and the measuring procedure. It is important that all instructions given in this document be followed. This will ensure that the measurement data are obtained under comparable conditions and are presented in the same format. Any deviation from the instructions has to be reported to the pilot laboratory.


Liquid samples The measurements are to be carried out on samples of two standard liquids pro-vided by NIST/Cannon as the pilot laboratory. Both samples are poly-α-olefines, not labelled as dangerous goods. Standard liquid A,

• approximate kinematic viscosity at -40°C / -20°C / 20°C: 150 mm²/s / 35 mm²/s / 7 mm²/s

• density: to be specified

• surface tension: to be specified Standard liquid B,

• approximate kinematic viscosity at 20°C / 100°C / 150°C: 1300 mm²/s / 40 mm²/s / 15 mm²/s

• density: to be specified

• surface tension: to be specified For both standard liquids, the long term stability of the kinematic viscosity is bet-ter than 0.1% over 6 month. Exposure to bright light and high temperatures should be avoided. The sealed glass bottles should not be opened before the measurements are started. The oils may be heated to 70°C to facilitate filling of the viscometers.

Format for reporting the measurement results The information is to be given for each liquid. Please use:

• Report_ Form_1_A_-40°C for liquid sample A, -400°C

• Report_ Form_1_A_-20°C for liquid sample A, -20°C

• Report_ Form_1_A_20°C for liquid sample A, 20°C

• Report_Form_1_ B_20°C for liquid sample B, 20°C

• Report_ Form _1_B_100°C for liquid sample B, 100°C

• Report_Form_1_ B_150°C for liquid sample B, 150°C


Uncertainty of measurement All of the report forms (1A -40°C, 1A -20°C, 1A 20°C, 1B 20°C, 1B 100°C, 1B 150°C ) give a list of main components of the uncertainty budget. Please add any additional component occurring in your measurements. Do not include a term for a potential long-term drift of the viscosity. The uncertainty of the viscosity is to be given as one standard uncertainty and in addition as expanded uncertainty U95 for a confidence level of 95%. This is ob-tained by combining the individual standard uncertainties obtained from Type A and Type B evaluations. The uncertainty evaluation should include a list of all influence quantities, their values and standard uncertainties, together with their degrees of freedom. The combined standard uncertainty, as well as the effective degrees of freedom νeff of the combined standard uncertainty uc and the t-factor t95(νeff) taken from the t-distribution for a 95% confidence level must be stated. The expanded uncertainty is given as U95 = t95(veff) · uc . The uncertainties are to be calculated and reported according to ISO "Guide to the Expression of Uncer-tainty in Measurement" [2].

Details of viscosity measurement Give the mathematical model equations for calculating the viscosity of the liquid

samples. (Example: SKEcal

cttCgg )( −=ν In this equation, ν is the kine-

matic viscosity in mm²/s, g is the acceleration of free fall at the point of meas-

urement in m²/s, calg is the acceleration of free fall at the point of calibration,

C is the viscometer constant in mm²/s², t is the flow time in s, KEt the kinetic

energy correction in s, and Sc the surface tension correction factor.) Describe how the standard uncertainties of the individual influence quantities of Report Form 1 in the uncertainty of the viscosity were estimated. It is important to know in what way the participants calibrated the viscometers used in this comparison. Concerning the additional participants, it is important to know the source of the calibration certificate. Please give references to publications concerning your viscosity scale. If possi-ble, send a copy of the publication to the Pilot Laboratory.

Deadline The reports are to be sent to the Pilot laboratory as soon as possible and four weeks after the measurements are completed at the latest. A result is not con-sidered complete if no associated uncertainty supported by a complete uncer-tainty budget is given. The results are confidential until all the participants have completed their measurements and all the results have been received (or until the deadline for receipt of the results is over).


[1] ISO TR 3666: Viscosity of water 1998 [2] Guide to the expression of Uncertainty in Measurement, corrected and

reprinted 1995, International Organization of Standardization (Geneva, Switzerland)


Appendix A3 Original Timetable

Starting date: March 15st, 2006

Timetable:

March 15th, 2006 (pilot laboratory): Mailing of the standard liquids, the data sheets, the timetable, and the technical report

to the participants

April 20th, 2006 (all participants): Start of the comparison measurements

May 25th, 2006 (all participants): Finishing of the comparison measurements

June 26th, 2006 (all participants): Submission of the results to the pilot laboratory

Aug 1st, 2006 (pilot laboratory): Submission draft report A to the participants

October 20th, 2006 (BIPM): Submission of draft B

In the case of unexpected delay at a participant institute it is possible, that these data can-not be taken into account.

Documents

CCM V K2 Final Report Feb 11 2009 - BIPM · CCM V K2 Final Report Feb 11 2009 .doc Page 9 of 36 No definitive cause has been determined for the situations reported by the first two