SIM SIM.M.D-K3. provide. SIM.M.M-K5 for. A set of. Institute LACOMET LATU INTI. Country Costa Rica Uruguay Argentina Chile México Canada Brazil

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FINAL REPORT SIM COMPARISON IN VOLUME OF WEIGHTS SIM.M.D-K3 Kornblit, F 1 ; Leiblich, J. 1 ; Becerra, L.O. ; Peña, L.M. ; Luján, L. ; Díaz,J.C. ; Centeno, L.M. ; Ramos, O 3 ; Rodríguez, S. 3 ; Santo, C. 4 ; Caceres, J. 4 ; García, F. 5 ; Leyton, F. 5 ; Claude J. 6 ; Loayza, V.M. 7 ; Cacais,F.A. 7 Abstract: This report summarizess the results of a comparison concerning the determination of volume of a set of four weights which nominal values are kg, 1 kg, g and. Seven NMIs within SIM have participated. The results reported are consistent with each other. Also, they can be used to evidencee degrees of equivalence with other RMOs results once linking results are available. 1. General Information The present comparison, named SIM.M.D-K3, was planned and carried out in orderr to evaluatee the degreee of equivalence in the calibration of high accuracy mass standards, and to provide evidence supporting CMCs claimed by the participants in determination of volume of mass standards. It is part of a more general project which comprisess three comparisons: SIM.M.M-K1 for mass calibration of nominal value 1 kg SIM.M.M-K5 for mass calibration of nominal values kg, g, 5 g, and mg SIM.M.D-K3 for volume determination of stainless steel weights of kg, 1 kg, g,. Data of the participant NMIs and Technical Contacts The following SIM institutes have participated in the comparison: Institute LACOMET LATU INMETRO Country Costa Rica Uruguay Argentina Chile México Canada Brazil Technical Contact( (s) Ramos, O; Rodríguez, S. Santo, C.; Cáceres, J. Kornblit, F; Leiblich, J. García, F.; Leyton, F. Becerra, L.O.; Peña, L.M.; Luján, L..; Díaz, J.C.; Centeno, L.M. Jacques, C. Loayza, V.M.; Cacais, F.A. (Argentina) 1 has acted as the pilot laboratory 3. General Considerations and Procedure A set of four stainless steel standards, made by Masstech and provided by was used for the comparison. The nominal values and identifications are shown in Table 1. 1, Instituto Nacional de Tecnología Industrial (Argentina), contact e-mail: ferk@inti.gob.ar;, Centro Nacional de Metrología (México); 3 LACOMET, Laboratorio Costarricense de Metrología; 4 LATU, Laboratorio Tecnológico del Uruguay (Uruguay); 5 (Chile); 6, National Research Council (Canada), INMETRO, Instituto Nacional de Metrologia, Qualidade e Tecnologia (Brazil) 1/7

Table 1. Data associated to the standard Nominal Serial mass value Number Identification kg 1 kg g 46114 577977194 The traveling standards were placed in individual wooden cases for transportation purposes, which was placed in a carrying transportation case, jointly with the standardss corresponding to the comparisonss SIM.M.M-K1 and SIM.M.M-K5. In all the cases, the transportation among laboratories was made by hand, by technical staff of the NMIs. A protocol was agreed previously to the comparison. In it, instructions to travel, initial inspection in each country, store, handling and acclimatization of the standards have been specified. Particularly, the following criteria were agreed: The hydrostatic method was employed to measure the volume of the standards Measurements were done after an appropriate acclimatization time The CIPM-7 formula [1] was applied by all the participants to determine the air density, in order to estimate air buoyancy effects. After the measurements, the travelling standards were cleaned in appropriate ways according to the transfer liquids employed in the calibrations. The volume thermal expansionn coefficient for all the traveling considered as equal to 4,8 x 1-5 ºC -1. standards was 4. Schedule The measurements followed the schedule shown in Table. Table. Measurement schedule N Institute / Country Dates of the measurementss 1 LACOMET / Costa Rica October 9 LATU / Uruguay January 1 3 / Argentina April 1 4 / Chile July 1 5 / Mexico June 11 6 /Canada February 11 7 INMETRO/Brazil January 1 /7

5. Summary of the reported results The results sent by the participants, expressed as the volumes V (referred to ºC), and their associated standard uncertainty u V, are shown in table 3. kg 3 V / cm u V / cm 3 LACOMET LATU INMETRO RV 54.6744 54.663 54.6655 54.668 54.6644 54.6566 54.668 54.665.4.5.4.4.4.9.5. Table 3. Data sent by the participants 1 kg g V / cm 3 u V / cm 3 V / cm 3 u V / cm 3 V / cm 3 u V / cm 17.43.1 4.857 4. 8.16 1 3 17.4 9 17.4 4 17.37 17.37 4 17.39 91 17.38 4 17.39 86 1... 16.1 4. 16 4.857 5 4.853 4.854 4.853 94 4.854 1 4.853 7 4.854 1. 1. 1. 5. 66. 4. 5. 4.15 63.15 99.16.15 83.15 89.16.15 89. 8.. 3. 8.. 6. 6. Liquids employed in the hydrostatic weighing The laboratories employed different liquids to perform the hydrostatic weighing and different ways to determine their density. Some laboratories used pure water and calculated its density by the Tanaka s formula []. In the other cases the measurementss of the liquids density are traceable to liquid or solid density standards. The buoyant liquids employed, their estimated density values referred to C and the corresponding standard uncertainties u are summarized in table 4, as well as the methods and traceability sources to determine. Table 4. Buoyant liquids employed and methods and traceability sources used to measuree their density NMI Buoyant liquid / kg m -3 u / kg m -3 Method / Traceability source Bidistilled and LACOMET deionized water 998.191 3.31 4 Hydrostatic weighing / Tanaka formula [] LATU Distilled water Distilled water 997.581 16 998.78 7. 43.8 4 Hydrostatic weighing / Tanaka formula [] Hydrostatic weighing / Tanaka formula [] Hydrostatic Weighing / Silicon Ciclohexane 778.6 6.1 5 crystal traceable to PTB Hydrostatic weighing / Zerodur sphere, Pentadecane 768.638. traceable to PTB Hydrostatic weighing / Tanaka formula [] ( kg) water 998.. with isotopic correction Comparison with a silicon cylinder / FC-4 1 878.685 (1kg, g, ) Tanaka formula [] with isotopic correction Hydrostatic Weighing / Silicon sphere, INMETRO ( kg) n-dodecane 748.86. 5 traceable to NMIJ Comparison with the volume of an E INMETRO (1 kg) FC-4 1 88.94.4 1 stainless steel weight measured at INMETRO ( g, ) FC-4 1 88.94.4 Subdivision Method / INMETRO 3/7

7. Dataa consistency and computation of reference values and degrees of equivalence In order to check the consistency of the results, tests were applied. For the different standards, the obs statistics as defined in [3] were calculated. The following values were obtained: Nominal value obs kg.5 1 kg 5.7 g 4.8 1.6 The corresponding critical value for = 6 degrees of freedom and significant level.5 is 1.6 (the same for all the standards). Therefore, in all the cases obs. So, all the dataa can be considered consistent and the assumptions to employ the so-called Procedure A in [3] are considered valid. Strictly speaking, not all of them are fully satisfied. INMETRO has employed a solid standard calibrated at as traceability source for 1 kg, 5 g and (seee table 4). Then, the results providedd by both NMIs are linked to a common standardd (a s zerodur sphere). So, a positive correlation exists between them and the Condition of Use in [3] may be considered breached. However, the uncertainty associated to that common standard is an order smaller than the uncertainties declared by both NMIs in the comparison. Then, the effect produced by that correlation is considered negligible. Then, the weighted averages were calculated and established as the reference values of the comparison (RV). They are shown in the last row of table 3 with their associated uncertainties. For each participant and standard, degrees of equivalence D and normalized errors E n were calculated according to (1). They are shown in tables 5A and 5B. D V RV; U D u V u ; RV E n D U D (1) where V and u V are the results reported by the participant. Bilateral differences between pairs of participants and bilateral normalized errors can be calculated according to: Dij Dij xi x j Eij () u u i j 4/7

Table 5A. Degrees of equivalence kg 3 D / cm U D / cm 3 LACOMET LATU INMETRO.9 -. -.1 -.9.8.8.6.7.6.17.9 D / cm 3.1 - -.. 5 -.1 5 1 kg g U D / cm 3 D / cm 3 U D / cm 3 D / cm 3 U D / cm.4 3.16..6 6.6 4. 4 -. 3. 6.6 -.1 1.. 1. 4.4. 1. 1. 1. 6.4.. 1 3 -. 1. 6. 6.. 1.. 1. 8 -. 4. 1. 3.1 Table 5B. Values of En kg 1 kg g LACOMET LATU INMETRO.1 -.3..3 -.1 -.5.3.1.5.1 -.7 -.6.8 -.5..8 -.6 -.1 -.1.4 -.4. -.5.3. -.1..3 8. Link to CCM key comparisons CCM comparisons in density of solids are not available yet. However, there is a planned one, named CCM.D-K3 (see [4]). Once it is complete, the current comparison could be linked to it for nominal values common to both them. 9. Plots. The results indicated in table 4. A are plotted in figures 1,, 3, and 4. In those plots, the dotted pink lines represent the expanded uncertainty U RV associated to RV. In some of them, both lines are too closed to be distinguished for the scale chosen. Figure 1. Plot of the measured results for the kg standard 1 SIM.M.MK5 kg weight 5-5 -1 LACOMET LATU INMETRO 5/7

Figure. Plot of the measured results for the 1 kg standard 5 SIM.M.MK5 1 kg weight 5-5 -5 LACOMET LATU INMETRO Figure 3. Plot of the measured results for the g standard SIM.M.MK5 g weight 1-1 - LACOMET LATU INMETR RO Figure 4. Plot of the measured results for the standard SIM.M.MK5 weight 8 4-4 -8 LACOMET LATU INMETRO 6/7

9. References 1. Picard A.. Davis R.S.. Gläser M.. Fujii K.. Revised formula for the density of moist air (CIPM-7). Metrologia 45 (8). 149-155. Tanaka. M; Girard. G.; Davis. R.; Peuto. A.; Bignell. N.; Recommended table for the density of water between C and 4 C based on recent experimental reports; Metrologia 38 (1). 31-39. 3. Cox. M.G.. The evaluation of key comparison data. Metrologia 39 () 589-595 4. http://kcdb.bipm.org/appendixb/kcdb_apb_search_result.asp?search=1& &met_idy=6& bra idy=3&cmt_idy=1&ett_idy_org=16&epo_idy=&cou_cod= 7/7