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l^ST Technical Note 1450

CCT'K3: Key Comparison of Realizations

of ttie ITS'90 over ttie Range 83,8058 K to

933,473 K

B. W. Mangum, G. F. Strouse, and W. F. Guthrie

QC

100 ional Institute of Standards and Technology

.U5753 inology Administration, U.S. Department of Commerce

#1450

2002 c.x
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NIST Technical Note 1450

CCT-K3: Key Comparison of Realizations of tine ITS-90

over the Range 83.8058 K to 933.473 K

B. W. Mangum and G. F. Strouse

Process Measurements Division

Chemical Science and Technology Laboratory

W. F. Guthrie

Statistical Engineering Division

Information Technology Laboratory

National Institute of Standards and Technology

Gaithersburg, MD 20899-8360

February 2002

U.S. Department of Commerce

Donald L. Evans, Secretary

Technology Administration

Phillip J. Bond, Under Secretary of Commercefor Technology

National Institute of Standards and Technology

Arden L. Bement, Jr., Director
Certain commercial entities, equipment, or materials may be identified in this document in order to describe an

experimental procedure or concept adequately. Such identification is not intended to imply recommendation or endorsement by the National Institute of Standards and Technology, nor is it intended to imply that the entities,

materials, or equipment are necessarily the best available for the purpose.

National Institute of Standards U.S. Government Printing Office For Sale by the

and Technology Washington: 2002 Superintendent of Documents

Technical Note 1450 U.S. Government Printing Office

Natl. Inst. Stand. Technol. Stop SSOP, Washington, DC 20402-0001

Tech. Note 1 450 Phone: (202) 51 2-1 800

393 pages (February 2002) Fax: (202) 51 2-2250

CODEN: NTNOEF Internet: bookstore.gpo.gov
CCT-K3: Key Comparison of Realizations of the ITS-90 Over the Range

83.8058 K to 933.473 K

Prepared by

B. W. Mangum, G. F. Strouse and W. F. Guthrie

National Institute of Standards and Technology

Gaithersburg, MD

USA

Key Comparison 3

Coordinated by B. W. Mangum (NIST)

with

John Connolly (NML), Sub-coordinator for Asia/Pacific

and

Erich Tegeler (PTB), Sub-coordinator for part of Europe

CONTENTS

Abstract 1

1. INTRODUCTION 1 2. LABORATORIES PARTICIPATING IN KEY COMPARISON 3 1 3. DEVICES USED IN THE COMPARISON 2

3.1. SPRTs 2

3.2. Transfer Cells 4

3.2.1. Gallium Cells 4

3.2.2. Cadmium cells 5

3.2.3. Ancillary Components Accompanying the Cells and SPRTs 6

4. PARTICIPANTS' INSTRUMENTATION, FIXED-POINT CELLS, TECHNIQUES

AND OTHER DETAILS 7

5. RESULTS OF COMPARISONS 7

5.1. Immersion Results Provided by the Participants 7

5.2. Results of Measurements at Fixed Points 7

5.3. Data Analysis for Comparison of Fixed-Point-Cells 10

5.4. Results of Direct and Indirect Comparisons of Ga Cells 20

5.5. Results of Direct and Indirect Comparisons of Cd Cells 21

6. DISCUSSION 21

-in-
Tables

Table 1. Table 2. Table 3.

Table 4.

Table 5.

Table 6. Table?..

Table 8. Table 9. Table 10.

Table 11.

Table 12.

Table 13.

Table 14.

Table 15.

Table 16.

Table 17.

Table 18.

Table 19.

Table 20.

Table 21.

Table 22.

Table 23.

Table 24.

Table 25.

Table 26.

Table 27.

NIST direct comparison of the gallium cells 23

NIST direct comparison of the cadmium cells 24

Wvalues, their range and the uncertainty of measurements at the

fixed points:

(Hart Model 5681, s/n 1094) 26

(Hart Model 5681, s/n 1098) 27

Wvalues, their range and the uncertainty of measurements at the

fixed points:

(Rosemount Model 162 CE, s/n 4386) 28

(Hart Model 5681, s/n 1032) 29

(Isotech Model 0670, s/n 040) 30

Wvalues, their range and the uncertainty of measurements at the

Fixed points:

(Rosemount Model 162 CE, s/n 4385) 31

(Hart Model 5681, s/n 1030) 33

Differences in realization of ITS-90 between Lab X and BIPM 35

Differences in realization of ITS-90 between Lab X and BNM/INM 48

Differences in realization of rTS-90 between Lab X and EMGC 62

Differences in realization of ITS-90 between Lab X and KRISS 71

Differences in reahzation of ITS-90 between Lab X andMSL 81

Differences in realization of ITS-90 between Lab X and NIM 91

Differences in realization of ITS-90 between Lab X and NIST 101

Differences in reahzation of ITS-90 between Lab X and NML 107

Differences in realization of ITS-90 between Lab X and NPL 119

Differences in realization of ITS-90 between Lab X and NRC 133

Differences in realization of ITS-90 between Lab X and NRLM 142

Differences in realization of ITS-90 between Lab X and PTB 159

Differences in realization of ITS-90 between Lab X and SMU 178

Differences in realization of rrS-90 between Lab X and VNIIM 191

Differences in realization of ITS-90 between Lab X and VSL 202

Summary of differences of realizations and their uncertainties between

laboratories for Al 211

Summary of differences of realizations and their uncertainties between

laboratories for Zn 212

Summary of differences of realizations and their uncertainties between

laboratories for Cd 213

Summary of differences of realizations and their uncertainties between

laboratories forSn 214

Summary of differences of realizations and their uncertainties between

laboratories for In 215

Summary of differences of realizations and their uncertainties between

laboratories for Ga 216

Summary of differences of realizations and their uncertainties between

laboratories forHg 217

-IV-
Table 28. Summary of differences of realizations and their uncertainties between

laboratories for Ar 218

Table 29a. Direct and bilateral comparison results for the gallium melting point 219

Table 29b. Indirect and bilateral comparison results for the gallium melting point 219

Table 30a. Direct and bilateral comparison results for the cadmium freezing point 220

Table 30b. Indirect and bilateral comparison results for the cadmium freezing point 220

Figures

Figure 1. The resistance of SPRT 4385 (Rosemount 162 CE) at the triple point of water as obtained by the participants during the course of the comparison 221

Figure 2. The resistance of SPRT 1030 (Hart Model 568 1

) at the triple point of water as obtained by the participants during the course of the comparison 221

Figure 3. The resistance of SPRT 4386 (Rosemount 162 CE) at the triple point of water as obtained by the participants during the course of the comparison 222

Figure 4. The resistance of SPRT 1032 (Hart Model 5681) at the triple point of water as obtained by the participants during the course of the comparison 222

Figure 5. The resistance of SPRT 1094 (Hart Model 5681) at the triple point of water as obtained by the participants during the course of the comparison 223

Figure 6. The resistance of SPRT 1098 (Hart Model 5681) at the triple point of water

as obtained by the participants during the course of the comparison 223

Figure 7. The resistance of SPRT 040 (Isotech Model 0670) at the triple point of water as obtained by NML and NRLM during the course of the comparison 224

Figure 8. Range of W(A1) values, expressed in mK equivalents, by laboratory and SPRT 225

Figure 9. Range of W(Zn) values, expressed in mK equivalents, by laboratory and SPRT 225

Figure 10. Range of W(Cd) values, expressed in mK equivalents, by laboratory and SPRT 226

Figure 11. Range of W(Sn) values, expressed in mK equivalents, by laboratory and SPRT 226

Figure 12. Range of W(In) values, expressed in mK equivalents, by laboratory and SPRT 227

Figure 13. Range of W(Ga) values, expressed in mK equivalents, by laboratory and SPRT 227

Figure 14. Range of W(Hg) values, expressed in mK equivalents, by laboratory and SPRT 228

Figure 15. Range of W(Ar) values, expressed in mK equivalents, by laboratory and SPRT 228

Figure 16. Differences, with U (95 %), in ITS-90 realizations between laboratories at the Al

freezing point 229

Figure 17. Differences, with t/ (95 %), in ITS-90 realizations between laboratories at the Zn

freezing point 232

Figure 18. Differences, with U (95 %), in ITS-90 realizations between laboratories at the Cd

freezing point 235

Figure 19. Differences, with U (95 %), in ITS-90 realizations between laboratories at the Sn

freezing point 238

Figure 20. Differences, with U (95 %), in ITS-90 realizations between laboratories at the In freezing point 241

Figure 21. Differences, with U (95 %), in ITS-90 realizations between laboratories at the Ga

melting point 244

Figure 22. Differences, with U (95 %), in ITS-90 realizations between laboratories at the Hg

triple point 247

Figure 23. Differences, with U (95 %), in ITS-90 realizations between laboratories at the Ar

triple point 250

-V-
Figure 24. Direct, indirect and bilateral comparison results for the gallium melting point 253

Figure 25. Direct, indirect and bilateral comparison results for the cadmium freezing point 254

Appendices

Appendix I. Instructions Provided to Participants 255

Appendix II. Instrumentation and Experimental Details 260

Table II.l. Details of participants' instrumentation used in key comparison 3 261

Table n.2.1. Details of participant's Al cells and their respective furnaces, etc 263

Table 11.2.2. Details of participant's Zn cells and their respective furnaces, etc 266

Table n.2.3. Details of participant's Cd cells and their respective furnaces, etc 269

Table n.2.4. Details of participant's Sn cells and their respective furnaces, etc 272

Table n.2.5. Details of participant's In cells and their respective furnaces, etc 275

Table II.2.6. Details of participant's Ga cells and their respective furnaces, baths, etc 278

Table 11.2.7. Details of participant's TPW cells and their respective baths, etc 281

Table n.2.8. Details of participant's Hg cells and their respective cryostats, baths, etc 284

Table n.2.9. Details of participant's Ar cells and their respective cryostats, etc 287

Table 11.3.1. Details of participant's techniques of realization of the freezing-point

temperature of A290

Table 11.3.2. Details of participant's techniques of realization of the freezing-point

temperature of Zn 296

Table 11.3.3. Details of participant's techniques of reahzation of the freezing-point

temperature of Cd 299

Table n.3.4. Details of participant's techniques of realization of the freezing-point

temperature of Sn 302

Table n.3.5. Details of participant's techniques of realization of the freezing-point

temperature of In 305

Table n.3.6. Details of participant's techniques of reahzation of the melting-point or triplepoint temperature of Ga 308

Table n.3.7. Details of participant's techniques of realization of the triple-point temperature

ofHzO 311

Table 11.3.8. Details of participant's techniques of realization of the triple-point temperature

ofHg 314

Table 11.3.9. Details of participant's techniques of realization of the triple-point temperature

of Ar 317

Appendix III. Immersion Curves 320

Figure IE. 1 Immersion curves for the various participants for Al 322

Figure 111.2 Immersion curves for the various participants for Zn 324

Figure in.3 Immersion curves for the various participants for Cd 326

Figure in.4 Immersion curves for the various participants for Sn 327

Figure in.5 Immersion curves for the various participants for In 329

-VI-
Figure III.6 Immersion curves for the various participants for Ga 331

Figure in.7 Immersion curves for the various participants for H2O 333

Figure in.8 Immersion curves for the various participants for Hg 334

Figure in.9 Immersion curves for the various participants for Ar 336

Appendix IV. Uncertainty Budgets 337

Table IV. 1(a). The uncertainty budget reported should include the following:

components of uncertainty budget for the triple point of water 338

Table IV. 1(b). The uncertainty budget reported should include the following:

components of uncertainty budget for W at the triple point/melting

point/freezing-point, as appropriate, of Ar, Hg, Ga, In, Sn, Cd, Zn

andAl 339

Table IV. 1(c). The uncertainty budget reported should include the following:

uncertainty budget for the comparison of fixed-point cells 340

Table IV.2. BIPM uncertainty budget for the gallium melting point and the triple

point of water, expressed in mK 341

Table IV.3(a). BNM-INM uncertainty budget for the fixed points other than the triple

point of water, expressed in mK 342

Table IV.3(b). BNM-INM uncertainty budget for the triple point of water, expressed

inmK 344

Table IV.4(a). IMGC uncertainty budget for the fixed points other than the triple point

of water, expressed in mK 345

Table rv.4(b). IMGC uncertainty budget for the triple point of water, expressed in mK 346

Table rv.5(a). KRISS uncertainty budget for the fixed points other than the triple point

of water, expressed in mK 347

Table IV.5(b). KRISS uncertainty budget for the triple point of water, expressed in mK 348

Table IV.6(a). MSL uncertainty budget for fixed points except the triple point of water,

expressed in mK 349

Table IV.6(b). MSL uncertainty budget for the triple point of water, expressed in mK 350

Table IV.7(a). NIM uncertainty budget for the fixed points other that the triple point of

water, expressed in mK 351

Table IV.7(b). NIM uncertainty budget for the triple point of water, expressed in mK 352

Table IV.8(a). NIST uncertainty budget for the fixed points other that the triple point of

water, expressed in mK 353

Table IV. 8(b). NIST uncertainty budget for the triple point of water cell, expressed in mK 354

Table IV.9. NML uncertainty budget for the fixed points, expressed in /xK 355

Table IV. 10. NPL uncertainty budget for the fixed points, expressed in mK 358

Table IV.U. NRC uncertainty budget for the fixed points, express in mK 359

Table IV. 12(a). NRLM uncertainty budget for fixed points except the triple point of

water, expressed in mK 360

Table IV.12(b). NRLM uncertainty budget for the triple point of water, expressed in mK 361

Table FV. 13(a). PTB uncertainty budget for the fixed points other than the triple point

of water, expressed in mK 362

Table IV.13(b). PTB uncertainty budget for the triple point of water, expressed in mK 363

-Vll-
Table FV. 14(a). SMU uncertainty budget for the fixed points other than the triple

point of water, expressed in mK 364

Table IV. 14(b). SMU uncertainty budget for the triple point of water, expressed in mK 365

Table IV. 15(a). VNIIM uncertainties for the fixed points, except the triple point of water,

expressed in mK 366

Table IV. 15(b). VNIIM uncertainties for the triple point of water, expressed in mK 367

Table IV. 16. VSL uncertainties {k= 1) for the fixed points, expressed in mK 368

Appendix V. Control Charts 369

Appendix VI. Additional Tables 372

Table VI. 1. Standard uncertainties for a single measurement (n = 1) for the fixed points

used for the various participants 372

Table VI.2. Standard uncertainties quantifying potential changes in SPRTs

that were used in KG 3. The associated degrees of freedom {DF)

are given also 375

Table VI.3. Actual coverage probabilities for expanded uncertainties with different

coverage factors and different degrees of freedom 376

Appendix VII. Comments by Participants on Key Comparison Reference Values 377

-vm-
Abstract

This is a report to the Comite Consultatif de Thermometrie (CCT) on Key Comparison 3, i.e., the

comparison of realizations of the ITS-90 over the range 83.8058 K to 933.473 K. The differences in

the reaHzations of the various fixed points in this range of the ITS-90 and the uncertainties of those

differences are given for the 15 standards laboratories participating in the comparison.

1. INTRODUCTION

This is a report to the Comite Consultatif de Thermometrie (CCT) on the key comparison of the

realizations of the ITS-90 over the temperature range from 83.8058 K (triple point of Ar) to 933.473 K (freezing point of Al). This comparison involved measurements in 15 standards

laboratories. Artifacts that were circulated among the participating laboratories were one, and in

some cases two, standard platinum resistance thermometers (SPRTs), a sealed gallium triple-point

cell, and a sealed cadmium freezing-point cell. With the exception of one rather unusually-long

SPRT that went from one of the sub-coordinating laboratories to one of the participating

laboratories, the SPRTs and the fixed-point cells were supplied by the National Institute of

Standards and Technology (NIST).

The coordinating laboratory for this comparison was NIST. There were two sub-coordinating

laboratories. National Measurement Laboratory (NML) of Australia for the Asia/Pacific area

participants and Physikahsch-Technische Bundesanstalt (PTB) of Germany for some of the

European participants.

The instructions to the participants are given in Appendix I.

2. LABORATORIES PARTICIPATING IN KEY COMPARISON 3

Coordinating laboratory - NIST

Sub-coordinating laboratories - NML and PTB

Laboratories performing comparisons directly with NIST

NML, PTB, NMiA^SL, NRC, IMGC

Laboratories performing comparisons directly with NML

MSL, NRLM, KRISS, NIM

Laboratories performing comparisons directly with PTB

VNIIM, BNM-INM, SMU, NPL

BEPM - special category, with measurements at Ga and H2O only

-1-
For the various laboratories, the persons involved in the comparisons were:

NIST B. W. Mangum, G. F. Strouse and W. F. Guthrie (statistician)

NML J. Connolly

PTB E. Tegeler, U. Noatsch, D. Heyer, B. Felhnuth and B. Thiele-Krivoj

MSL J. V. Nicholas (now deceased), D. R. White and T. D. Dransfield

NRLM K. Nara

KRISS K. S. Gam, K. H. Kang and Y.-G. Kim

NIM Y. Duan and Y. Qu

VNIEM A. I. Pokhodun, N. P. Moiseeva and A. G. Ivanova

BNM-INM E. Renaot, Y. Hermier and G. Bonnier

SMU S. Duris

NPL R.L. Rusby, J. Gray, F. J. M. Sutton and D. I. Head

BIPM R. Pello and M. Stock

NMiA^SL M. de Groot and J. Dubbeldam

NRC K. Hill

IMGC P. Marcarino

3. DEVICES USED IN THE COMPARISON

In preparation for the comparison, NIST constructed and evaluated the Ga and Cd fixed-point cells to be used by the participants of the comparison. In addition, NIST evaluated the SPRTs to be used

in the comparison.

It is well known that the temperature of the triple point of water, determined in cells prepared with

water from different sources and/or purified by different methods, has the potential of exhibiting

fairly large differences due to isotopic composition (as large as 0.25 mK). Since the isotopic

composition of Ga samples from widely different sources and of different purities is independent of

sample, a Ga cell was circulated among the participating laboratories to try to ascertain how closely

the triple-point/melting-point temperature of the various participants' Ga cells and the realizations

of their own Ga point agree and if Ga might be a better reference point than the triple point of water

for SPRT resistance ratios.

Since the Cd freezing-point temperature (321.069 °C) is a convenient value for it to be used as a check on the measurement process of calibrating SPRTs over the range from 83.8058 K to either

419.527 °C or 660.323 °C, and as a means of determining the non-uniqueness at that point, a NIST

Cd cell was circulated among the participating laboratories to try to ascertain how closely the

freezing-point temperatures of the various participants' Cd cells and their realizations of the Cd

point agree. Unfortunately, it was discovered that only seven participants had Cd fixed-point cells of their own.

3.1. SPRTs

After the SPRTs had been selected for use in the comparison and had been aimealed at 675 °C until

their resistance at the triple point of water (TPW) was repeatable to < 0.2 mK, they underwent three

complete calibrations. For these calibrations, all of the defining fixed points throughout the range
from 83.8058 K to 933.473 K were used. During each of the three caHbration cycles, the SPRTs

were cahbrated also at the Cd freezing point. For the three calibrations, the range of values of W

{[W= R{Tpp)/R{273.l6 K)], where R{Ty:p) is the resistance of the SPRT at a fixed-point temperature

Tfp and i?(273.16 K) is its resistance at the TPW}, was no greater than the equivalent of 0.35 mK at any of the fixed points. The range of values of i?(273.16 K) over the three calibrations was no

greater than 0.68 mK.

Figures 1 through 6 show the resistances of the various SPRTs at the TPW obtained during their

annealing and calibrations at the fixed points, as measured at NIST before and after the other

participants of the comparison, and also as reported by the participants. The first set of NIST values

in each figure shows the variations among the values obtained during calibration of the SPRT after

the SPRT had been annealed. The last set of NIST values in each figure includes all measurements

of the SPRT at the TPW after the SPRT was received from the last participant. Upon receipt of the

SPRT from the last participant, the SPRT resistance was measured at the TPW once, and in some

cases several times, before annealing. These results (obtained before annealing) are shown in the

figures as open symbols and are not considered in the range of values given for the SPRT that were

obtained during calibration. All values reported by the participants are indicated in the figures and

those obtained during annealing are indicated by open symbols. The effects of annealing on the

resistance of the SPRTs are obvious. Similar to Figures 1 through 6, Figure 7 shows results for the

SPRT that was measured only at NML and NRLM.

It is well known that the Pt wire of SPRT elements undergoes oxidation at temperatures below

about 420 °C and breakdown of the oxide layer at temperatures above about 420 °C. The process is reversible and the breakdown occurs fairly rapidly at temperatures of 450 °C and above. Thus,

compared to the value of i?(273.16 K) obtained soon after annealing and just before measurements

at the Al freezing point and/or the Zn freezing point, the value of i?(273.16 K) obtained immediately

following measurements at either of these points is normally about the same, or it is slightly smaller

(0.1 mK to 0.2 mK). If the SPRT had been at room temperature for a number of hours since being

exposed to heat treatment at 450 °C or higher before measurement at the TPW, then the TPW value

obtained after measurements at the Al or Zn freezing point will be slightly smaller. Also, it is normal to observe some slight increases in the i?(273.16 K) following measurements at Cd, Sn, In and even Ga, compared to the value obtained before measurements at either of these points. Thus,

during a calibration starting at the Al freezing point in which the SPRT is at, or near, the fixed-point

temperature for about 1.5 h, one should expect the i?(273.16K) measured immediately after

measurements of the SPRT at the freezing points of Cd, Sn and In to increase, and maybe even

increase a bit after the Ga melting point. As stated above, these rather small reversible changes in

i?(273.16 K) during the calibration of an SPRT are to be expected and, in our opinion, should not be

classified as instabilities. Such reversible changes that occur during calibration, however, should

not be greater than a total of about 0.5 mK to 0.7 mK. Changes greater than these are likely due to the other causes. If mechanical strains are somehow introduced during the measurement process,

annealing at about 675 °C should remove all but the most severe and the i<I(273.16 K) should retum

to a value approximately the same as that observed before the sfrains were introduced. In

calibrations of SPRTs, it is very important that measurements at the triple point of water are made

on the same oxidation state of the SPRT as that existing at the preceding temperature of interest. If an SPRT is unstable, due to mechanical problems with the Pt sensing element or its support, say, it is our opinion that the instability likely will be observed during measurements in any laboratory.
Referring to Figures 1 through 6, one can see that the ranges of values obtained for a given SPRT

during its cahbrations at some laboratories, after annealing, were somewhat smaller than those

obtained in the other laboratories. The reason for the difference in behavior is not likely to be

instability of the SPRTs, as we define the term. Consequently, the cause must be related in some

way to the techniques used by the participants, including those used by NIST.

The value of the realized ohm may be slightly different in the different laboratories so the absolute

value of i?(273 . 1 6 K) will reflect that difference.

3.2. Transfer Cells

3.2.1. Gallium Cells

The NIST reference cell, designated cell Ga 94-3 and against which the Ga transfer cells were

compared, contains 99.999 995% pure Ga.

The Ga transfer cells that were used in the comparison contained Ga of 99.999 99+% purity. The Ga

was contained in a Teflon crucible of the usual NIST design. The Teflon crucible contained a Teflon

cap through which the thermometer re-entrant well assembly was inserted. The crucible was located

in a borosilicate glass holder. For the first cells constructed for this comparison, this holder also

contained a borosilicate glass re-entrant thermometer well, as an integral part. This crucible

container was evacuated before being sealed. Thus, the Ga transfer cells that were a part of the

comparison were Ga triple-point cells.

The Ga cell that was initially sent to NML for circulation among the laboratories of its participants

did not survive shipment to NML. Its re-entrant well tube was broken at its junction with the outer

glass envelope. After several unsuccessful attempts at repairs, a cell plus enclosure that included a one-piece Nylon cap and re-entrant well was designed at NIST. This cap assembly was attached to the outer glass envelope of the cell by a clamp, with an 0-ring seal between the cap and the glass

envelope that was suitable for maintaining a vacuum in the cell. A valve attached to the cap

permitted evacuation of the cell. Later in the comparison, it was discovered that during air shipment

of the cells a small amoimt of air would leak into the cells. Presumably, that was caused by

contraction of the Nylon cap and the O-ring due to the low temperatures in the cargo bay of the

airplanes transporting the cells. Such contraction would loosen the cap sufficiently to let air leak

slowly past the O-ring seal. Although the leaks were not large enough for the cells to come to atmospheric pressure during the flights, the effects were detectable in the triple-point temperatures

of the cells. Once this problem of leaks developing during transportation of the cells was detected,

the cell could be easily returned to its initial condition by the participating laboratory simply by

evacuating the cell upon its receipt from the airline.

The Ga cell with a one-piece glass re-entrant well tube and outer envelope that was initially sent to PTB for circulation among the laboratories of its participants survived the transportation to, and

measurements at, PTB, VNIIM and BNM/INM but was broken during measurements at SMU.

NIST then provided a new Ga cell of the new Nylon cap design described above for the completion

of measurements at PTB, NPL, BIPM and the final measurements at PTB.
The Ga cell that was circulated among NIST, NMiA^SL, NRC and IMGC was of the Nylon cap

design. The cell was hand-carried during ground transportation to and from NRC so no problem of

the cell admitting air into its vacuum space was encountered before the NRC measurements, or after

their measurements and the cell's transportation back to NIST. A change in the cell's fixed-point

temperature was detected at IMGC, however, upon direct comparison measurements of the cell with

the IMGC cell, and again at NIST upon the cell's return to NIST and direct comparison

measurements with the reference cell at NIST. Consequently, in both cases the cell was evacuated

to ensure that the triple-point temperature would be obtained. Since the results of comparisons of

the NIST cell with the NMiA^SL cell were not reported to NIST until some months after the cells

and SPRTs used in the comparison had been returned to NIST, it is not known to what extent there

might have been leakage into the cell during its shipment to NMiA/'SL. Upon the return of the cell

from NMiA^SL, however, direct comparison of the cell with the NIST reference cell, before the

transfer cell was evacuated, indicated that the 'triple-point' temperature of the transfer cell was

0.07 mK colder than that of the NIST reference cell. This indicates that air had leaked into the cell

but it is unknown as to how much of the change occurred before measurements at NMiA^SL. After

evacuation of the cell, its triple-point temperature agreed with that of the NIST reference cell to within 0.01 mK.

With the exception of cell Ga 961, which contained a glass re-entrant well tube and that was broken

during measurements at SMU, the triple-point temperatures of the Ga transfer cells were directly

compared with the NIST reference cell before and after measurements on them by the participants.

As indicated above, after the cells were returned to NIST, preliminary direct-comparison

measurements were made on them to get an indication of any loss of vacuum and then they were

evacuated. The direct comparisons of the newly-evacuated transfer cells showed that their triplepoint temperatures were within 0.01 mK of that of our reference cell. Thus, the triple-point

temperatures of the cells at the completion of the comparisons were unchanged from their original

values. This indicates that the fransfer cells had not become contaminated during the key

comparison, although air had leaked into the cells during airplane transportation. The results of the

direct comparisons at NIST before and after the comparisons by the other participants are given in

Table 1.

3.2.2. Cadmium Cells

The Cd cells that were used in the comparison contained 99.999 99% pure Cd. The new NIST

laboratory reference cell (designated Cd 96-3) contains 99.999 99% pure Cd also and was one of

five cells constructed at the same time (all of the same lot) before the key comparison began. Four

of those five cells were the cells circulated among participants in the key comparison. The cells

sent to the participants were sealed under a pressure of one standard atmosphere of argon gas (at the

Cd freezing-point temperature). Those cells were directly compared at NIST with a cell containing

99.9999% pure Cd before measurements on them by the participants. Upon their return from the

participants, the cells were directly compared with our new Cd reference cell (Cd 96-3). The W

values of the cells, obtained following measurements by the participants, were found to be

unchanged from those before measurements by the participants to within the repeatability of

measurements at NIST, i.e., to within 0.03 mK {k = 2). The results of the comparison measurements

at NIST on the Cd transfer cells relative to the NIST 99.9999%) pure Cd cell and relative to our new

Cd reference cell (Cd 96-3) are given in Table 2.

-5-
Four Cd cells were damaged during the comparison. After measurements had been completed at VNIIM and the cell returned to PTB, it was discovered that a small amount of Cd metal was located

between the graphite crucible and the glass enclosure. The cell was returned to NIST where it was

opened, the ingot of Cd metal removed from the crucible and placed in another (new) graphite

crucible, the cell reassembled and then compared to our reference cell. The freezing-point

temperature of the repaired cell was unchanged (to within our measurement repeatability) from the

value of the original cell. In the meantime, a spare cell had been sent to PTB. That second cell

survived measurements without incident at PTB, SMU, PTB, NPL and PTB. At the time of the

comparison, BNM-INM did not have a Cd cell and made no measurements on the NIST Cd cell. During final shipment of the cell from PTB to NIST, however, rough handling by the shipper broke

the very bottom part of the cell's glass enclosure, but did no damage to the crucible. The crucible of

Cd was removed from the broken cell and placed in a new glass enclosure. The cell was then

compared with the NIST reference cell. To within the NIST measurement repeatability (0.03 mK

for k = 2), the freezing-point temperature of the sample was unchanged from its value obtained

before its shipment to PTB. This repaired cell was then sent to NRC and later to IMGC. During

return shipment of the cell from IMGC, just as in the case of the cell shipped from PTB, rough

handling by the shipper broke the very bottom part of the cell's glass enclosure, but did no damage

to the crucible. The crucible of Cd was removed from the broken cell and placed in a new glass

enclosure. The cell was then compared with the NIST reference cell. To within our measurement

repeatability (0.03 mK for k = 2), the freezing-point temperature of the sample was unchanged from

its value obtained before its shipment to IMGC.

Upon return of the Cd cell from NMiA^SL, its condition was very similar to that of the cell returned

from VNIIM, as described above. That is to say, there was Cd metal between the graphite crucible

and the glass enclosure. The cell was repaired and then compared with the NIST reference cell. To

within our repeatability (0.03 mK for k = 2), the freezing-point temperature of the sample was

unchanged from its value obtained before shipment of the cell to NMiA^SL.

3.2.3. Ancillary Components Accompanying the Cells and SPRTs

For the convenience of each set of participants in obtaining good thermal contact of the Rosemount

SPRT accompanying a Ga fransfer cell with the liquid-solid interface of the Ga sample, an Al

bushing was provided by NIST for use when the participants were making measurements with that

SPRT in that Ga transfer cell. Similarly, an Al bushing to be used in a Cd fransfer cell with the

accompanying Rosemount SPRT was provided by NIST for each set of participants to use when

they were making measurements with the Rosemount SPRTs in that Cd fransfer cell. Additionally, a special heater and thermistor were provided with the Ga fransfer cell for use in preparing the inner

liquid-solid interface in that cell. Bushings for the participants' cells were not provided since the

diameters of the re-enfrant thermometer wells of the participants' cells were unknown to NIST staff. Furthermore, it was expected that the participants normally use such bushings and would provide

their own special-size bushings for thefr particular Ar, Hg, H2O, Ga, In, Sn, Cd, Zn and Al cells. Also, it was expected that a light mineral oil would be used in the re-enfrant thermometer well of a Ga cell to improve the thermal contact of the SPRT with the irmer liquid-solid interface of the

metal.
4. PARTICIPANTS' INSTRUMENTATION, FIXED-POINT CELLS, TECHNIQUES AND

OTHER DETAILS

The details of the participants instrumentation, their fixed-point cells, their samples, their fiimaces

and/or baths, their techniques for preparing freezes or melts, and other relevant information are given in Appendix 11.

5. RESULTS OF COMPARISONS

5.1. Immersion Results Provided by the Participants

Although special bushings for use with a Rosemount SPRT to improve thermal contact in the Ga

and Cd transfer cells were provided by NIST for each set of participants to use when they were making measurements with the Rosemount SPRTs in those cells, reports from the participants

indicate that many of them did not use the bushings. Reports from the participants indicate also that

many of them did not use the special heater with a thermistor thermometer provided by NIST with

the Ga fransfer cell for the convenience of the participant in preparing the inner liquid-solid

interface in that, or their own, cell. Furthermore, some participants did not use a liquid in the

thermometer well of the Ga cells to improve thermal contact between the SPRT and the liquid-solid

interface of the Ga. The alternative (non-protocol) techniques used by some of the participants may

very well have contributed to errors and increased uncertainties in their measurements. In fact, it is rather likely that some of the participants did not prepare an inner liquid/solid interface in the Ga

cell. This latter situation can lead to improper immersion and, consequently, poor-quality results.

The immersion curves provided by the participants for SPRTs in their fixed-point cells are presented in Fig. III.l through Fig. III.9 in Appendix III. Not all participants provided immersion

data, although they were requested to do so in the instructions to the participants (see Appendix I). Those not providing immersion curves were: BIPM, BNM-INM, MSL (except of NIST Cd) and

NMi/VSL. Information provided by BNM-INM and BIPM on immersion in their cells are given in

Appendix HI.

5.2. Results of Measurements at Fixed-Points

Although the comparison was designed to cover the range from 83.8058 K to 933.473 K, not all of

the participants had the capability to make comparisons over the entire range. The list of W values

in Tables 3, 4 and 5 specify the fixed points used by a given participant. In these tables we also list the mean Revalues and their uncertainties. The uncertainties listed are combined uncertainties with a coverage factor of ^ = 1 and are expressed as the temperature equivalent. The uncertainties are given as reported by the participants for each SPRT, or SPRTs, circulated among the given set of

participants but adjusted for the number of W values obtained from different freezes (or melts, as appropriate) at each fixed point (see Section 5.3). When a participant sent the results to NIST in

elecfronic form, the values of W (not rounded to eight decimal places) in the elecfronic file were

used in calculating the mean value given in the tables for a given fixed point. As a result, the mean

values given in the tables may differ by about 0.01 mK from the values of the mean as calculated

directly from the listed W values. The range of W values for each of the fixed points obtained by

each of the participants is given also in the tables in equivalent temperature. These ranges of W

-7-
values for participants and SPRTs are shown in Figures 8 through 15 for Al, Zn, Cd, Sn, In, Ga, Hg

and Ar, respectively. The uncertainty budgets, as reported by the participants and that lead to the

expanded uncertainty values in the results, are given in Appendix IV.

In Table 6 through 20 we give the mean W values, their combined uncertainties, Uc ik=l), the

degrees of freedom (DF), and the differences and their uncertainties between the mean W values,

expressed as the equivalent temperatures, from the realizations by each of the participants and those

of the other 14 participants. The uncertainties were calculated as described in Section 5.3. Except

for the case of NRLM, measurements were made by NIST on each of the SPRTs circulated among

the participants. The fiimace-cell arrangement at NRLM precluded their use of the NIST SPRT sent

to them; their system requires an exceptionally long SPRT. Fortunately, NML was able to obtain an SPRT that met NRLM's requirements. NIST did not make measurements on that SPRT.

Consequently, the uncertainties in the differences between NRLM and the participants other than

NML may be larger than would otherwise be the case since the results of an additional intermediate

laboratory is involved in computing those differences.

The pair-wise temperature differences and their associated uncertainties given in Tables 6 through

20 and shown in Figures 1 6 through 23 were calculated for the various laboratories by two paths.

Those paths are indicated by the terms 'direct' and 'inclusive' and yield results that are indicated in

the tables and figures by the same terms. In some cases, the paths are identical.

The 'direct' differences are the temperature differences between the realizations of a pair of

laboratories that were obtained using the shortest available path linking those laboratories. In some

cases, this means that the laboratories are compared using measurements made on the same SPRT

or SPRTs. Where necessary, however, NIST or NML serves as an intermediary, linking the

measurements of the two laboratories.

In some cases, of course, direct differences may not use all of the data reported by one or the other

of the laboratories of the pair or of the intermediate laboratory (if any). This situation often arises in cases in which both laboratories of the pair made measurements on one SPRT but in which one or both members also made measurements on another SPRT not measured by the other laboratory.

Examples of this case are provided by the temperature differences between SMU and BNM-INM,

VNIIM and NPL, SMU and VNIIM, VNIIM and BNM-INM, and NPL and BNM-INM. hi other

cases, however, as can be seen from Tables 6 through 20, the direct differences do use all of the

reported data of the two laboratories of the pair. For example, differences such as those between

SMU and NPL use all of the date reported by both laboratories.

The 'inclusive' differences are those in which all of the data obtained by the pair of laboratories

involved are used in the calculations of their pair-wise temperature differences and their associated

uncertainties. In inclusive differences, whether or not there is a direct linkage between the

laboratories, NIST and possibly also NML may be used as intermediaries so that the temperature

differences can be computed using all relevant data. NIST was selected as the intermediate

laboratory for these differences because, overall, that results in a minimum number of intermediate

laboratories in the pair-wise differences. If NML and PTB had been included as intermediate

laboratories, the pair-wise differences would have been somewhat different but the uncertainties

would have been only slightly different.
When pair-wise temperature differences obtained from calculations using the direct and inclusive

paths are different, then one or the other path may provide the better precision. Because the direct

differences use measurements only from the shortest path between the laboratories, they will tend to provide more precise estimates of the temperature differences when the uncertainties of the

intermediate laboratories (when needed) are large relative to the uncertainties of the pair of

laboratories. Due to the increased averaging of results across different SPRTs, inclusive differences

will tend to be more precise in cases in which the intermediate laboratories have relatively low

uncertainty.

Comparison of direct and inclusive differences also can provide further insight into the differences

between laboratories. Direct differences can provide temperature differences as observed for a

single SPRT. This can be useful as a check for interactions between particular thermometers and a laboratory's measurement procedures. Two laboratories may agree closely with one another when

the results are averaged across different thermometers because one or both may have results that are systematically higher for some thermometers and systematically lower for others. Of course, this

type of interaction between thermometers and measurement procedures can be detected only when

one laboratory is compared with another using at least two SPRTs. This is observable in some of

the pairs of direct and inclusive comparisons in this study. Significant interactions between

thermometers and laboratories could arise from a variety of causes. Some possible causes include

thermometer instability, inadequate immersion, particular measurement methods, measurement

equipment, laboratory conditions, etc. hi any specific case, however, the actual cause of an

interaction can really only be determined by study of the underlying physics of the problem and

fiirther experimentation, the logical follow-ups to a key comparison.

As can be seen in Tables 4 and 5 for NML, PTB, BNM-INM, SMU, NPL and BIPM, comparison

measurements were made in each of those laboratories with at least two SPRTs that were also used

in measurements at NIST. As can further be seen from the data presented in those tables, the

pertinent pair-wise differences in realizations in those laboratories, as obtained with the different

SPRTs, sometimes differ from one another . Since the participants sent the results of their

measurements on both SPRTs to NIST, we used the averages of the differences obtained with the

different SPRTs in all subsequent calculations of pair-wise differences.

The pair-wise differences, and then uncertainties, between laboratories given in Tables 6 through 20

are siramiarized for each of the fixed points Al, Zn, Cd, Sn, hi, Ga, Hg and Ar in Tables 21 through

28, respectively. The differences obtained with the different SPRTs are apparent in the bilateral

differences given in these tables for the cases where the 'direct" and 'inclusive', as described above,

are different.

Plots of the differences between the W values of any one of the various participants and all of the

other participants for each of the fixed points Al, Zn, Cd, Sn, hi, Ga, Hg and Ar are given in Figures

16 through 23. The uncertainty bars represent the expanded uncertainty interval that should capture

the true temperature difference between any two laboratories with approximately 95% confidence

(or more in a few cases, as described in the Section 5.3). The values of the differences are expressed as the equivalent temperature differences.

-9-
5.3 Data Analysis for Comparison of Fixed-Point Cells

This section describes the procedures used in the analysis of the data for key comparison 3 of the

realizations of the ITS-90. As previously described, each laboratory participating in the key

comparison provided resistance ratios, denoted W, measured in their own fixed-point cells with

transfer thermometers provided by NIST (by NML in the case of NRLM) for some or all of the

eight fixed points included in the comparison, i.e., for Al, Zn, Cd, Sn, In, Ga, Hg, and Ar. Some

participants measured each fixed point in only a single freeze or melt, while others used multiple

freezes or melts at each point. Similarly, some participants used only one fransfer thermometer

while others made measurements with two fransfer thermometers. Uncertainties, computed from

the comparison data directly, or based on additional measurements with the fixed-point cells and a check thermometer, were also provided by each participant (see Appendix IV).

Differences of mean resistance ratios for each fixed point were computed from the W values for a given fransfer SPRT for every pair of laboratories making measurements with that SPRT and then

converted into the equivalent temperature differences using values of dWr/dT where Wt is the

relevant ITS-90 reference fimction. For each pafr of laboratories using a common fransfer

thermometer, the temperature differences between the laboratories were computed directly. If a pair

of laboratories each made measurements with a particular pair of fransfer thermometers, then

temperature differences were computed for each thermometer and the differences were averaged to obtain the overall difference between those laboratories.

In cases where two laboratories did not make measurements on the same fransfer thermometer, the

differences were computed through the coordinating laboratory (NIST). The only exception to this

was for comparisons with NRLM. For additional information on the temperature differences

computed, see Section 5.2.

The information provided as part of the uncertainty of the measurements at each fixed point by each

participant included the repeatability, or standard uncertainty, of a single resistance ratio for

multiple freezes or melts, denoted ^a, the number of freezes or melts reported for computation of

mean temperature differences, denoted n, the degrees of freedom associated with ^a, denoted DFa,

and the standard uncertainties for any other sources of variation affecting the measurements. Some

of the sources of uncertainty typically included, in addition to the resistance-ratio repeatabihty, were

impurities in fixed-point cell composition, hydrostatic-head errors, SPRT self-heating errors, etc. The specific sources of uncertainty and associated uncertainty values can be found for each

laboratory in Appendix IV. The combined uncertainty due to sources of variability other than

resistance ratio repeatability were combined by root-sum-of-squares and are denoted by Sb

Generally, uncertainties were given in terms of temperature rather than in terms of W. Whenever

uncertainty values were given in terms of AW, the values were converted into the equivalent

temperatures using the values of dWr/dT. All uncertainties given in this section are reported in

terms of temperature and are given in mK.

Typically, the resistance-ratio repeatability, 5'a, was obtained using Type A methods of evaluating

uncertainty, thus giving rise to the notation being used. In some cases, the 5'a was obtained from

data of control charts for check thermometers, such as those given for NIST, as an example, in

-10-
Appendix V. In other cases, where control-chart data or degrees of freedom were not available, ^a

was computed from the PT values reported for the key comparison. If a laboratory reported Sa as the

standard uncertainty of the mean of some number of measurements, Sa was converted to the

standard uncertainty for a single freeze or melt using information provided by the laboratory

describing their computation and reporting of Sa- It was occasionally the case that at one, or a few,

of the fixed points, a participant evaluated resistance-ratio repeatability using Type B methods;

these too are included in ^a despite the suggestion that Sa is an uncertainty term evaluated purely by

Type A methods.

The other sources of uncertainty, summarized in the term ^b, were generally obtained using Type B

methods. These sources of uncertainty are taken to be components of uncertainty that affect a set of

measurements made with a specific fixed-point cell in a specific measurement system in the same

way. That is, the effects of these sources of variability do not vary in any practical sense from

freeze to freeze. As for ^a, the amount of uncertainty associated with a particular uncertainty source included in Sb was occasionally evaluated by Type A methods but is still summarized in Sb- All sources of uncertainty included in ^b were confirmed to be reported in terms of standard uncertainty

before being summarized as the combined uncertainty .Sb- In some cases, degrees of freedom were

expHcitly given for each source of uncertainty included in 5*3. When this was done, the degrees of

freedom associated with Sb were obtained by using the Welch-Satterthwaite formula as described in

the ISO Guide to the Expression of Uncertainty in Measurement (1993, pp 61-65). If the degrees of

freedom were not given explicitly for a particular component included in 5'b, then that component of

^b was assumed to have an infinite number of degrees of freedom. The degrees of freedom

associated with Sb are denoted by DFb.

As mentioned in the previous section, uncertainties are reported in Tables 3, 4, and 5 for the mean

resistance ratio, W , obtained by each laboratory for each fransfer thermometer. These values

typically differ from the summary values reported by each laboratory (and given in Appendix IV)

because the laboratories were not required to summarize their uncertainties for each thermometer in a standardized format. Therefore, when the uncertainties were summarized for inclusion in Tables 3,

4, and 5, they were all converted, as necessary, to a common format. In the format used in Tables 3,

4, and 5, the combined standard uncertainty of W for each thermometer is related to the final

uncertainties calculated for the temperature differences between laboratories given in Tables 6

through 20. The relationship between the components of uncertainty reported by the laboratories

and the combined standard uncertainty of W,Uc(W ), expressed in mK, is given by

V n We give some numerical examples to clarify the computations described in the paragraph above.

First, consider the uncertainty for Al as measured with SPRT 4385 by NIST. The ff values and

Mc( W) for this fixed-point are shown in Table 5 and the uncertainties reported by NIST are given in

Table IV. 8(a). NIST made four measurements of W{A[) with SPRT 4385 and reported values of

^a = 0.28 and 5b = 0.16. Inserting these into eq. (1) yields

-11-
78^

M„=,,.^l±^ + 0.16- =0.21. (2) i

NIST's reported combined standard uncertainty in Table IV. 8(a) does not take into account the

number of fF values measured with SPRT 4385 in this comparison and is given as Uc = 0.32. For

SPRT 1030, also shown in Table 5, NIST made five measurements. During the course of the

comparison, however, NIST was informed by PTB that SPRT 1030 was involved in some unknown

incident just before measurements at SMU and that the subsequent measurements should reflect

this. This led to the division of the data into sets denoted by 1030A and 1030B. These data were

treated as coming from two SPRTs. NIST made three measurements using SPRT 1030A and the

value of Wc( ^) was computed to be

w =,p?^ + 0.16' =0.23. (3)

For SPRT 1030B, Uc{W) = 0.25 because « = 2.

One of the interesting features in the estimation of uncertainties for the temperature differences in

this comparison arises from the fact that the degrees of freedom and the number of measurements

used to compute the mean resistance ratio are not necessarily directly related. In most applications

the same data used to estimate a mean quantity are also used to estimate the uncertainty. In this

comparison, however, because check thermometers can be used to estimate the resistance-ratio

repeatability of a measurement system and fixed-point cell, the degrees of freedom can be much

greater than the number of measurements used in any particular comparison. For example, for SPRT

4385 NIST has Az = 4 at the Al fixed-point but has DFa = (130 - 1) = 129, as shown in Tables 5 and

IV.8(a).

In addition to the uncertainties reported by each laboratory for the data they collected for this key

comparison, uncertainties for possible changes in each fransfer thermometer over the course of the

comparison were also computed and included for each temperature difference. This component of

uncertainty was computed in response to discussion at the thermometry working meeting held at NIST in January 2000. Because they affect only differences in measurements made with the

transfer thermometers over time, these SPRT uncertainty components are included only in the

uncertainties of the temperature differences between laboratories, and not in the uncertainties of the

measurements made in a single laboratory.

These additional uncertainties were computed by first computing the difference in W observed at NIST (or at NML for SPRT 040) at each fixed point, using data taken before each thermometer was

sent out to the sub-coordinating laboratories and after its return. If there were no evidence of

change in the before and after PF values for the thermometer use at a particular fixed point, based on

a t test, the additional uncertainty component for that fixed point was set to zero. If the t test indicated that a change was likely to have occurred, the absolute difference between the before and

after Wvalues was converted to a Type B uncertainty based on a uniform distribution by dividing

the half-width of the interval defined by the before and after travel difference by V3 . The degrees

-12-
of freedom for this uncertainty were approximated using the methods described in Appendix E

(equation G.3) of the ISO Guide to the Expression of Uncertainty in Measurement.

The formula for the t-test used to determine whether or not a change in the SPRT had occurred is

(J^ After -fTBefore) ±t{Q.915,DFJS^ + (4)

aw^ / ai

where

dW^/dT ^in^^^ «B^f^^,

fFBefore is the mcan resistance ratio measured at NIST before the thermometer traveled to the subcoordinating laboratory,

frAfter is the mean resistance ratio measured at NIST after the thermometer returned from the subcoordinating laboratory,

t (0.975, DFj^) is the 95% expansion factor from the t distribution for a two-sided interval and the

degrees of freedom of NIST's freeze-to-freeze repeatability, iS'a,

^Before ^^ thc uumber of measurements made at NIST before the thermometer traveled, and

"After is ^^^ number of measurements made at NIST after the thermometer traveled.

As a numerical example to make the equations above easier to follow, if one inserts the numbers for

SPRT 1098A for the Al fixed-point into eq. (4), it yields the following confidence interval:

(3.375747625-3.375746950) ^ (,573524,(0.28),! , i

0.000003205 Vl 3

(5)

which simplifies to 0.21 mOK.± 0.64 mK.

Since the expanded uncertainty (0.64 mK) is larger in absolute value than the observed difference

(0.21 mK) between the temperatures measured before and after the thermometer traveled, we

conclude that nothing happened that affected the thermometer during fravel.

Whenever the confidence interval for the difference in SPRT response before and after the SPRT

fraveled indicated that a significant change occurred during fravel, then an uncertainty term for the

difference was calculated as shown below, according to formula (6) from the ISO Guide to the

Expression of Uncertainty in Measurement (page 13 in the 1993 edition).

"sPRT

P^After —W-QtioK

iSidWJdiT)

(6)

-13-
The degrees of freedom for this uncertainty were obtained by using formula G.3 from the ISO

Guide to the Expression of Uncertainty in Measurement, substituting an estimate of the standard

deviation of the absolute value of the difference of two normal random variables and the absolute

temperature difference into the general terms given in the equation listed in the ISO Guide to the

Expression of Uncertainty in Measurement. This is equivalent to the use of Msprt and its uncertainty

in the formula since the scaling factor, 2V3 , cancels out of formula G.3. The formula for the

estimate of the variance of the absolute difference of two normal random variables, which is not

intuitively easy to understand, was obtained from the Handbook ofthe Normal Distribution by Patel

and Read (1982, pp 33-34) and works out to be

WAn.r-WBefore dWjdT

(WAner-WBefore) dWjdf

+sl

f 1 +

1

V

'^ After '^Before J

„ rry— -(fFAfter -fFBefore)" Sf^-sjziTr exp • is'^imjdTY

(J)

{WAfier-WBeioxe)

f

dWidT

1-20

\ \2

(fF After -fFBefore)

V s^{mjdT) Jj)

where Mis the cumulative distribution function of the standard normal distribution.

This complicated formula gives numerical answers for the degrees of freedom that are only slightly

different than those that would be obtained by approximating the variance of the absolute

temperature difference by

^After-^Before dWJdT ~'^A

( 1 1 +

^After '^Before )

(8)

All of the results given in this report are based on the more complicated, theoretically correct

formula, however, because the approximation slightly under-estimates the degrees of freedom.

Using an under-estimate of the degrees of freedom could have a high cost in terms of total

uncertainty if the degrees of freedom computed with formula G.3 are small (i.e. three or less) and

MspRT is large relative to the other uncertainty components.

In the two cases in which the shipment of the transfer thermometers easily allowed, or necessitated,

the treatment of each SPRT as two effectively-different thermometers, the estimation of the

uncertainty for potential thermometer changes was computed separately for each effectivelydifferent thermometer, if possible. Accordingly, SPRTs 1098A and 1098B have different

uncertainties for potential thermometer changes during use. There were no intermediate

measurements at NIST for SPRTs 1030A and 1030B, however, so the uncertainties for them are based on before and after measurements that include the change in SPRT 1030 leading to its

-14-
treatment as two separate thermometers. As a result, the uncertainties given for SPRTs 1030A and

1030B are conservative estimates of MsprtThe uncertainties quantifying potential changes in the transfer thermometers with use, and their

associated degrees of freedom, are given in Table VI.2 in Appendix VI.

Focusing now on the computation of the temperature differences between laboratories and their

uncertainties, derivation of the appropriate combined standard uncertainty from the formulas used to compute the temperature differences between laboratories yields the following results:

For a direct comparison between two laboratories using a single transfer thermometer

which then leads to the uncertainty formula,

'Labi '^hzbl

hi the formula for the uncertainty of a direct comparison between laboratories with a single transfer

thermometer, multiple freezes reduce the uncertainty in resistance-ratio repeatability, but not the

uncertainty firom the sources that are summarized in .Sb. This is because all of the resistance ratios are affected by those sources of uncertainty in exactly the same, unknown way. The term dPT/dr

does not appear in the uncertainty formula because the conversion to temperature units is implicit in

the definition of 5a and S^.

For a direct comparison between two laboratories using two transfer thermometers

— (J^Labl.SPRTl — J^ Lab2, SPRT 1 ) H ()^Labl,SPRT2 — i^ Ub2, SPRT 2 ) AT =2. 2 ,Y\\ ^-'Labl-Lab2 j tt7 / j t-

' ^ ^

dW^ /aT

which yields the uncertainty formula,

"c(A^Ubl-Lab2) =

rr2 rr2 ^2 rt2 2 2 ('[2)

^^"1

I Al31,;^ ^2 ^ '^Aubi

I "^Al^mI ^2 ^ ^SPRTl , ^SPRT2 ^ ^ 4n An ^'^'" An An

^

^''Labl.SPRTl ^"Lab2,SPRTl ^"Labl,SPRT2 ^"Lab2,SPRT2

Lab2

hi this uncertainty formula, as in the immediately preceding one, the averaging of data from

multiple freezes reduces the amount of uncertainty arising from sources of random imcertainty. The

averaging of temperature differences measured with different thermometers also reduces the amount

15-
of random uncertainty from potential changes in the SPRT over time but does not affect the amount

of uncertainty from the sources summarized in Sb, which often tend to dominate the total

uncertainty. Averaging the results from two thermometers for laboratories 1 and 2 is the source of

the number 4 in the denominators of the Sa and Msprt terms.

For an indirect comparison of the temperature difference between two laboratories, with the

exceptions noted above for NRLM,

'^-'Labl-Lab2 ~ V^"' Labl-NIST ~ '^-'Laba-NISl) ' y'-^)

which leads to the uncertainty

"c(ArL,bl-Lab2) = V"c (^^Ubl-NIST ) + "c ( ArNisT-Ub2 ) " ^^B^,, (14)

Li this uncertainty formula, the variances of the temperature differences between each laboratory

and NIST are first combined and then adjusted so that the term ^b, which affects all of the

measurements made using the NIST measurement system and fixed-point cells in the same, but

unknown, way is not included in the imcertainty. This term can, and in fact should, be eliminated

from this uncertainty because the effects from the sources of uncertainty in the NIST measurements

included in 5'b,^,3^ cancel out in the indirect comparison computations.

The equations above for typical indirect comparisons could be used to describe the indirect

comparisons between NRLM and the other laboratories whose measurements were coordinated by

NML by substituting NML for NIST in the subscripts. For indirect comparisons between NRLM

and laboratories whose measurements were coordinated by PTB or NIST, the temperature

difference is computed by

^-'Ubl-NRLM ~ V^-'ubl-NIST ~ ^-' NML-NIST ~

'^-'nRLM-NMl) V-'--^-'

which leads to the uncertainty

"c ( A^ubl-NRLM ) = V"c (^^Labl-NIST ) + K ( ^^"nisT-NML ) + "c ( A^Wl-NRLM ) " ^-^b^^^ - 25^^ (16)

For all of the different types of temperature differences and uncertainties described above, expanded

uncertainties were then computed by algebraically expanding the uncertainty estimates given above

into independent terms, collecting the terms and finding the effective degrees of freedom for the

uncertainty using the Welch-Satterthwaite formula (as cited above). The coverage factor, k, was

taken to be the 97.5% percentile of the Student's t distribution with the effective degrees of freedom

resulting from the Welch-Satterthwaite calculations. This yields an expanded uncertainty interval

that should capture the true temperature difference between any two laboratories with

approximately 95% confidence.

Using the effective degrees of freedom in the uncertainty calculations is important because the

degrees of freedom account for the uncertainty in the uncertainty estimates, which can be

-16-
appreciable in some cases. Because there was not an agreed upon number of measurements to be

made by each participant in the comparison, there were sometimes wide variations in the number of

measurements used to compute mean resistance ratios and uncertainties. Table VI.3 of Appendix

VI shows the actual coverage probabilities obtained when ^ = 2 is used to compute expanded

uncertainties and the data have different numbers of degrees of freedom. Expanded uncertainties

based on A: = 2 are often assumed to have confidence close to the nominal 95% level obtained when

the degrees of freedom are large. As the numbers in Table VI.3 show, however, for low degrees of

freedom the confidence level attained can be quite different from 95%. Analogous confidence

levels are given also for combined uncertainties computed with k= I. The combined uncertainties are subject also to the same variations in attained coverage when the degrees of freedom are low to moderate rather than obtaining the nominal coverage 68.3% generally associated with /c=l.

Therefore, using standard uncertainties does not save us from accounting for the degrees of freedom

used in each comparison.

As Table VI.3 shows, some of the expanded uncertainties in this comparison could be as low as 80% confidence intervals while others would be 95% intervals (or shghtly higher) if a uniform

expansion factor of k=2 was used instead of taking the degrees of freedom associated with each

particular comparison into account. The values of k needed to obtain 95% coverage, listed in the

right-hand column of the table, show the nonlinearity in the relationship between expansion factors

and degrees of freedom for 95%) confidence intervals.

The differences between nominal and actual coverage values for both the k=l and Jc=2 intervals

comes from the uncertainty in the uncertainty estimates themselves. Without having a fairly large

amount of data to compute uncertainty estimates, they are subject to relatively large amounts of

random error. Each uncertainty estimate is an unbiased estimate of the true uncertainty but will

fluctuate a lot from one set of measurements to the next when based on few measurements. The

amount of uncertainty in the uncertainty estimates is quantified by the degrees of freedom. High

degrees of freedom indicate uncertainty estimates that are well known, or have small uncertainty,

while low degrees of freedom indicate uncertainty estimates that are poorly known, or have large

uncertainty.

Unfortunately, in a few cases the results obtained by computing the expanded uncertainties using

the procedure described above were subject to paradoxical behavior relative to physical intuition.

Due to the nature of statistical confidence intervals based on quantities distributed according to a Student's t distribution, it is possible for the expanded uncertainty from a direct comparison

between two laboratories, say Lab 1 and NIST, to be larger than the expanded uncertainty of an

indirect comparison between Lab 1 and Lab 2 that includes the direct comparison between the

laboratories Lab 1 and NIST and Lab 2 and NIST. Confidence intervals computed using the WelchSatterthwaite formula to approximate the degrees of freedom of the uncertainty are prone to this in

particular, although not exclusively. This is considered by some, including some of the authors of

this report, to be a limitation of these formulae. For example, the expanded uncertainty for a comparison between a laboratory, denoted Lab 1, and NIST of the form

dfF, /dT

-17-
can be larger than the expanded uncertainty for a comparison of Lab 1 with another laboratory, Lab

2, in which the comparison is made through NIST and is of the form

It is important to note that this effect occurs only with expanded uncertainties. The standard

uncertainties are ordered as physical intuition suggests they should be and are not affected by this

phenomenon. This is because the confidence levels of these intervals with k=\ are not being held at fixed confidence levels that are specified in the analysis methods.

Surprisingly, the counter-intuitive phenomenon described in the previous two paragraphs is not a

defect of statistical theory, although it seems so at first glance. This phenomenon occurs because of

the effective "averaging out" or "balancing" of errors in the uncertainty estimates when multiple

uncertainty estimates are combined. As the uncertainty of the aggregate uncertainty estimate drops,

its degrees of freedom increase and the associated value of k needed to maintain 95% confidence

also drops. In fact, when the degrees of freedom start at the low end of the scale, the coverage

factor drops extremely quickly, sometimes faster than the uncertainty estimate itself increases. As

the drop in the coverage factor occurs, however, the desired confidence level is maintained.

In any case, because of the situation described above, the majority of the authors of this report

favored an altemative approach to the computation of expanded uncertainties. This altemative

approach is used for all of the results given in this report and is described next.

In the altemative approach to the computation of expanded uncertainties that was chosen,

the first two steps in the computation are essentially the same as the ISO method, the standard

uncertainty for each type of comparison described above was algebraically expanded into

independent terms in each uncertainty and the terms were collected. Then the effective degrees of

freedom for all of the terms associated with each laboratory were computed using the WelchSatterthwaite formula. Expanded uncertainties were computed for each laboratory's contribution to the total uncertainty using a coverage factor from the t distribution and the effective degrees of

freedom. The effective degrees of freedom and coverage factor for each laboratory's uncertainty

are given by the formulas

r^2 \2

s

+s.B Labi DF =^^ ^

(19)

and

'^Lab ~ ^0.975, DFi_^^

• \'^^)

Coverage factors for the uncertainty attributed to the use of each SPRT (denoted A:sprt) were also

computed as shown in Eq. (20) using the effective degrees of freedom foimd in Table VI.2 in

-18-
Appendix VI. Finally, these expanded uncertainties were combined by root-sum-of-squares to obtain the final expanded uncertainty.

For a direct comparison of the temperature at two laboratories of the type

Ar,Labl-Lab2 dW/dT (21)

in which each laboratory used the same transfer thermometer, this results in the following expanded

uncertainty

UiAT,Labl-Lab2 ) = JkLabi V

^Labl +sl

^ rc2

+ ^Lab2 V ^Lab2 +sl J - 2 (22)

For an indirect comparison of the temperature at two laboratories of the type

^-'Labl-Lab2 ~ (^-'Ubl-NIST ^-'ub2-NIST-' (23)

in which each laboratory used a different transfer thermometer, this results in the following

expanded uncertainty

U(AT,Labl-Labl ) =

'Labi ^'^Labl + s: + kNIST

\^ ^NIST,

+

'NIST- + kUb2

2/ \^ ^Lab2 + sl J 2 2 ] 2 2

(24)

Note that in eq. (24), the coverage factor for NIST is based only on the random portion of the

uncertainty, ^a, because that is the only portion of the uncertainty that affects the temperature

difference in the cases in which NIST serves as an intermediary.

The expanded uncertainties for all of the other types of comparisons between laboratories described

above were obtained analogously.

While the alternate method for computing expanded uncertainties used here is not in line with the

methods described in the ISO Guide to the Expression of Uncertainty in Measurement, it always

results in larger expanded uncertainty intervals than the ISO methods and is therefore more

conservative than the procedures outlined there. When the degrees of freedom associated with each

of the components of uncertainty in u^ are large, the alternative method will be only slightly

conservative. When the degrees of freedom for one or more of the uncertainty components in u^ are low, however, it can become exfremely conservative. Of course one of the primary advantages

suggesting use of this alternate method is the fact that both the standard uncertainties and expanded

uncertainties will be ordered according to physical intuition.

-19-
The results of the data analysis are given in the Tables 6 through 28 and Figures 16 through 23. The

3sults reported include mean resistance ratios for each laboratory for each thermometer used in a

particular comparison, the standard uncertainty of the mean resistance ratio (given in terms of

temperature), and the effective degrees of freedom of the mean resistance ratio. The estimated

temperature differences between the laboratories and the standard and expanded uncertainties of the

temperature differences are given also. Please note that the description of the data analysis given

above provides the general procedures followed for each comparison. In some cases, the data for a

particular comparison had to be handled slightly differently than the general case described above.

5.4. Results of Direct and Indirect Comparisons of Ga Cells

As stated in Section 3, a Ga transfer cell was included among the devices sent to each participant to ascertain how closely the temperatures of all the participating laboratories' Ga cells agreed among

themselves, as determined by "direct" or, in some cases, by "indirect" comparisons with the transfer

cell. The results are presented in Tables 29a and 29b, respectively, and displayed in graphical form

in Figure 24. These temperature differences obtained by direct or indirect comparisons of the cells

may be compared with the bilateral temperature differences, also given in Tables 29a and 29b,

obtained from the realizations of the Ga melting point as indicated by the calibrations of the

circulating SPRTs.

The data analysis for the direct and indirect comparisons of the Ga cells was handled similarly to the

analysis of the ITS-90 realizations. For the direct comparisons, those in which the two cells were

measured simultaneously in nearly identical fiimaces, paired differences of the Wvalues, converted

to terms of temperature, were averaged to determine the differences between the cells. The paired

differences were used also to determine the repeatability of the measurements since the paired

results should be less variable than non-paired results. The other sources of uncertainty included in

the direct comparisons included hydrostatic head effects, SPRT self-heating effects, immersion

effects, and effects arising from the choice of plateau values. All other sources of uncertainty

reported by the participants will not affect the direct comparisons because each will affect the

results in the same way and will therefore cancel.

For indirect comparisons, those in which the cells were compared sequentially in the same furnace

rather than simultaneously, the mean Wvalues were computed for each cell and then the difference

of the means, expressed in terms of temperature, was used to determine the difference between the

cells. When more than one thermometer was used, the results were averaged to get the best possible

estimate of the difference between the cells. The sources of uncertainty included when assessing

the variability of these mean temperature differences included all sources reported by the

laboratories except for effects due to impurities in the cells. For the indirect comparisons, the values

of measurement repeatability reported by the participants were used, rather than the values

computed from the comparison data. This was done because the participant-reported-measurementrepeatability values were often based on more degrees of freedom and over a wider range of

environmental conditions than the repeatability estimates from the comparison data alone.

For both types of comparisons, the number of freezes used to compute the mean differences in the

cells was used in the uncertainty calculations. Also, as in the comparison of the ITS-90 reahzations,

-20-
expanded uncertainties for the differences between fixed-point cells were obtained for each

laboratory's contribution to the comparison and then those expanded uncertainties were combined

by root-sum-of-squares. The same method for obtaining expanded uncertainties as described in

Section 5.3 applies to the analysis when used for direct or indirect comparison of fixed-point cells.

5.5. Results of Direct and Indirect Comparisons of Cd Cells

A Cd transfer cell was included also among the devices sent to each participant to ascertain how

closely the temperatures of all the participating laboratories' Cd cells agreed among themselves, as determined by "direct" or, in some cases, by "indirect" comparisons with the transfer cell. The

results are presented in Table 30a and Table 30b, respectively, and displayed in graphical form in

Figure 25. These temperature differences obtained by direct or indirect comparisons of the cells

may be compared with the bilateral temperature differences, also given in Tables 30a and 30b,

obtained from the realizations of the Cd freezing point as indicated by the calibrations of the

circulating SPRTs.

The data analysis methods used for the comparison of Cd fixed point cells is exactly analogous to the methods used for comparison of Ga cells. For a description of the methods used please refer to the discussion in Section 5.4.

6. DISCUSSION

The best method to compare the temperatures of fixed-point cells is by a direct, i.e., simultaneous,

comparison of the cells, with the cells located in nearly identical furnaces and with measurements

made on the samples at the same liquid/solid ratio. This method eliminates most systematic errors.

The best method for comparison of laboratories is to compare not only the temperatures of fixedpoint cells by a direct comparison, but also to compare realizations of those fixed points through the

calibrations of one or more SPRTs at those points in the respective laboratories, since the latter includes most systematic errors present in the measurements made in each of the laboratories. This,

however, is not a practical method for key comparisons because of the amount of time and the cost

that would be involved.

Considering the points made above, the types of comparisons utilized in this CCT key comparison

appear to be a good compromise, hi fact, it is believed that key comparison 3 represents the best

global comparison to date of realizations of the ITS-90 over the temperature range of the

comparison.

It was expected that the agreement among the laboratories of the Ga fixed-point temperature would

be to within 0.02 mK to 0.05 mK, and certainly no worse than 0.05 mK. As can be seen from the

results of the direct and indirect comparisons presented in Table 29a and Table 29b, respectively,

however, the results are disappointing and obviously did not meet expectations. It is surprising that

the results are in such poor agreement.

-21-
It appears that some, or most, of those participants not using bushings with the Rosemount transfer

SPRTs may not have waited a sufficient length of time for the SPRTs to come into equihbrium with

the inner Hquid/soHd interface of the sample. If that were the case, then the measured fF values may

not accurately reflect the true values for the respective fixed points.

The participants were asked to provide immersion curves, determined from data obtained at two

measuring currents at each SPRT position in the cell (and obtained during insertion of the SPRTs

into the cell) in order to determine the values at zero power dissipation. Some participants did not

obtain immersion curves for some or all of the fixed points and some used only one current for the

measurements. Consequently, those participants obtained comparison data that may have been

obtained when the SPRT was not in equilibrium with the liquid-solid interface of the sample (and

perhaps would have been influenced by variations of several kelvins in the temperature of the

furnace), or when it was not clear if an inner hquid-sohd interface had been formed along the full length of the sample. If the measurement techniques led to either of these conditions, then erroneous values of varying magnitude would have been obtained.

The Cd freezing-point temperature is a good secondary fixed point that can be used as a check point

to evaluate the quality of calibrations of SPRTs from °C through either 419.527 °C, 660.323 °C or 961.78 °C. As can be seen from the results of the direct and indirect comparisons, presented in

Table 30a and Table 30b, respectively, and from the differences of those with those from

reaHzations also presented in Table 30a and Table 30b, the agreement of the temperatures of the

participants' cells was rather poor. Unfortunately, it was discovered that only seven participants

had Cd fixed-point cells of their own so we decided not to address the non-uniqueness issue in the

report since so many of the participants had little or no experience in using the Cd cell and

consequently had no estimate of the uncertainty in the realization of its freezing point.

It was decided that key comparison reference values would not be given for this report. The NIST

correspondence given in Appendix VII states the course of action on which the participants of key

comparison 3 agreed. A tabulation of votes by the participants for and against key comparison

reference values is given in Appendix VII. Additionally, the comments from the participating

laboratories concerning key comparison reference values for this comparison are given also in

Appendix VU. Although a minority of participants (5) thought that key comparison reference values

should be used, they withdrew their objections in order for the report to be completed.

-22-
Table 1. NIST direct comparison of the gallium cells.

Ga961 Ga94-3

before PTB W(Ga) PF(Ga) Ar,mK

1 1.118 137 63 1.118 137 67 -0.01,

2 1.118 137 62 1.118 137 65 -O.OOg

3 1.118 137 64 1.118 137 67 -O.OO7

after repair

4 1.118 137 63 1.118 137 65 -O.OOs

5 1.118 137 62 1.118 137 67 -0.01,

6 1.118 137 63 1.118 137 66 -O.OO7

after PTB

7 1.118 137 63 1.118 137 66 -O.OOg

8 1.118 137 62 1.118 137 66 -O.Olo

9 1.118 137 64 1.118 137 66 -0.006

Ga962 Ga94-3

before NML WiGa) W(Ga) A7',mK

1 1.118 137 59 1.118 137 65 -O.Olfi 2 1.118 137 56 1.118 137 66 -0.024

3 1.118 137 60 1.118 137 66 -O.OI4

after NML

4 1.118 137 57 1.118 137 66 -0.023

5 1.118 137 56 1.118 137 64 -0.02o

6 1.118 137 58 1.118 137 67 -0.02,

Ga965 Ga94-3

. before VSL W(Ga) W(Ga) Ar,mK

• 1 1.118 137 63 1.118 137 68 -O.OI2

2 1.118 137 64 1.118 137 67 -O.OO9

3 1.118 137 61 1.118 137 67 -O.OI5

after VSL

4 1.118 137 66 1.118 137 70 -0.01,

5 1.118 137 65 1.118 137 66 -0.00,

6 1.118 137 65 1.118 137 68 -O.OO7

after NRC

7 1.118 137 63 1.118 137 67 -O.Olo

8 1.118 137 63 1.118 137 67 -O.OI2

9 1.118 137 62 1.118 137 67 -O.OI3

after IMGC

10 1.118 137 66 1.118 137 67 -0.00,

11 1.118 137 68 1.118 137 66 O.OO4

12 1.118 137 66 1.118 137 68 -0.006

-23-
Table 2. NIST direct comparison of the cadmium cells.

Cd 96-1 Cd 78-2

beft)re PTB fF(Cd) ^(Cd) Ar,mK

12

3

after repair

2.218 819 92

2.218 819 83

2.218 820 03

Cd 96-1

2.218 818 42

2.218 818 57

2.218 818 63

Cd 96-3

0.42

0.35 0.39

4

56

after NRC

2.218 819 79

2.218 819 70

2.218 819 90

Cd96-1

2.218 819 90

2.218 819 88

2.218 820 02

Cd 96-3

-0.03 -0.04

-0.03

7

89

after IMGC

2.218 819 58

2.218 819 64

2.218 819 62

Cd 96-1

2.218 819 72

2.218 819 76

2.218 819 94

Cd 96-3

-0.03

-0.03 -0.08

10

1112

2.218 819 66

2.218 819 53

2.218 819 75

Cd 96-2

2.218 819 79

2.218 819 62

2.218 819 75

Cd 78-2

-0.03 -0.02 0.00

before NML ^(Cd) W{Cd) Ar,mK

12

3

after NML

2.218 819 79

2.218 819 70

2.218 819 90

Cd 96-2

2.218 818 54

2.218 818 36

2.218 818 65

Cd 96-3

0.32 0.34

0.32

4

56

2.218 819 59

2.218 819 68

2.218 819 30

2.218 819 73

2.218 819 95

2.218 819 45

-0.03 -0.07

-0.04

Cd 96-3 Cd 78-2

WiCd) WjCd) Ar, mK

2.218 819 49 2.218 817 99 0.38 2.218 819 65 2.218 818 07 0.40

2.218 819 88 2.218 818 31 0.40

-24-
Table 2. cont'd. NIST direct comparison of the cadmium cells.

Cd 96-4 Cd 78-2

before PTB W(Cd) ^(Cd) Ar,mK

12

3

after PTB

2.218 819 81 2.218 820 07

2.218 819 69

Cd 96-4

2.218 818 58

2.218 818 70

2.218 818 39

Cd 96-3

0.31 0.35

0.33

4

56

2.218 818 67

2.218 818 77

2.218 818 95

Cd 96-5

2.218 818 63

2.218 818 83

2.218 819 04

Cd 78-2

0.01 -0.02 -0.02

before VSL W(Cd) W(Cd) Ar. mK

12

3

2.218 819 69

2.218 820 04

2.218 819 86

Cd 96-5

2.218 818 32

2.218 818 45

2.218 818 37

Cd 96-3

0.35 0.40

0.38

after repair W(Cd) W(Cd) Ar. mK

12

3

2.218 819 53

2.218 819 73

2.218 819 32

Cd 96-5

2.218 819 62

2.218 819 82

2.218 819 59

Cd 96-3

-0.02

-0.02

-0.07

2.218 819 93

2.218 819 87

2.218 819 97

2.218 820 18 2.218 819 86

2.218 820 03

-0.06 0.00

-0.02

-25-
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-218-
Table 29a. Direct and bilateral comparison results for the gallium melting point.

Direct Comparison (Lab X - NIST) Bilateral Differences (Lab X - NIST)

AJ,mK u,(k=^l),mK f/(95%),mK AJ,mK «c(^l), mK t/(95%), mK

IMGC 0.00 0.04 0.12 0.09 0.06 0.13

NPL -0.04 0.12 0.24 -0.17 0.21 0.42

NRC -0.17 0.11 0.25 -0.14 0.13 0.27

VNIIM 0.09 0.02 0.04 0.01 0.08 0.19

VSL 0.25 0.06 0.12 -0.23 0.21 0.41

Table 29b. Indirect and bilateral comparison results for the gallium melting point.

Indirect Comparison (Lab X - NIST) Bilateral Differences (Lab X - NIST)

AJ,mK u^ik=l),mK l/(95%),mK Ar,mK ttc(/r=U,mK £/(95%),mK

BIPM -0.03 0.08 0.16 -0.09 0.08 0.16

BNM 0.00 0.14 0.28 -0.03 0.15 0.29

KRISS -0.27 0.29 0.64 0.00 0.20 0.46

MSL 0.15 0.16 0.32 0.17 0.18 0.36

NIM 0.96 0.23 0.48 -0.59 0.28 0.57

NML 0.09 0.08 0.16 -0.16 0.13 0.26

NRLM 1.16 0.11 0.21 -0.37 0.11 0.22

PTB 0.07 0.11 0.21 0.20 0.12 0.24

SMU 0.06 0.10 0.19 0.04 0.10 0.19

-219-
Table 30a. Direct and bilateral comparison resiilts for the cadmixun freezing point.

Direct Comparison (Lab X - NIST) Bilateral Differences (Lab X - NIST)

Ar,inK Hc(AF=i;,mK Z7(95%),mK Ar,mK «e(ft=l),niK £7(95%), mK

IMGC -0.01 0.07 0.16 -1.47 0.33 0.66

NRC -0.11 0.15 0.34 -0.95 0.21 0.42

VNnM 0.01 0.31 1.30 0.40 0.54 1.46 VSL -0.89 0.06 0.12 -1.14 NA NA

Table 30b. Indirect and bilateral comparison results for the cadmium freezing point.

Indirect Comparison (Lab X - NIST)

Ar,mK u,{k=l),mK t/(95%),mK

Bilateral Differences (Lab X - MST)

Ar,mK Ucik=l),mK Z7(95%),mK

NIM

NML

0.12

-0.37

1.10 0.182.70

0.36

1.28

-1.21

0.87

0.20

1.96

0.41

-220-
s

o

a.

25.558 45

25.558 40

25.558 35 y25.558 30 -

25.558 25 -

25.558 20 -

25.558 15

25.558 10

t

ImK

25 50 75 100 125 150

number of TPW readings

I -NIST#l,0.41mKi

|XNIST#2, 0.49mK

[xNIST#3,0.50mK

|^PTB#l,2.07mK

!BVNIIM,2.46mK

! +PTB#2, 1.44 mK

'•INM, 1.53 mK

PTB#3, 1.83 mK

ASMU, 1.75mK I <>PTB#4, 1.47 mK

UNPL, 2.09mK

©BIPM, 0.21 mK

PTB#5, 1.55 mK

ANIST#4. 0.21 mK

175 200

Figure 1. The resistance of SPRT 4385 (Rosemoimt 162CE) at the triple point of water as obtained by the participants during the course of the comparison.

24.800 6

24.800 4

I

24.800 2 o

Oh^ 24.799 8

24.800

24.799 6 -f"^

24.799 4

^

/-If-

^

I

2niK

25 50 75 100

number of TPW readings

125

-NIST#1 , 0.62 mK

XNIST#2 , 0.43 mK

XNIST#3 0.47 mK

PTB#2, 2.12 mK

INM, 1.52mK

+ PTB#3, 1.78 mK

• SMU,3. lOmK

PTB#4, 1.50 mK

ANPL, 1.91mK • BIPM,0.13mK

OPTB#5, 1.90 mK

ANIST#4 0.50 mK 1 ONIST#5 0.45 mK

150

Figure 2. The resistance of SPRT 1030 (Hart Model 5681) at the triple point of water as obtained by the participants during the course of the comparison.

-221-
25.541 6

25.541 4

25.541 2

•§ 25.541 ^

^ 25.540 8

25.540 6 T

25.540 4 ^

25.540 2

-NIST#l,0.39inK

XNIST#2,0.39mK

XNIST #3, 0.33 mK

NML#l,2.11mK • NML#2, S.llmK

+NML#3,2.75mK

KRISS,0.50mK

NML#4, 1.73mK

DNIM, 1.19niK

ONML#5,3.39iiiK

ANIST #4, 0.21 mK

25 50 75 100 125 150 175 200 225 250

number of TPW readings

Figure 3. The resistance of SPRT 4386 (Rosemoimt 162CE) at the triple point of water as obtained by the participants during the course of the comparison.

25.215 8

25.215 7

E 25.215 or 25.215

25.215 6 -f

5

4

25.215 3

2 -:

1 -r25.215

25.215

25.215

2mK

v^**^^

V

25 50 75

number of TPW readings

100

-NIST#l,0.26mK|

XNIST #2, 0.35 mK

XNIST#3,0.51mK

NML#l,2.21mK|

MSL, 1.14mK • NML#2,4.49mK|

ANIST#4, 0.47mK I

125

Figure 4. The resistance of SPRT 1032 (Hart Model 5681) at the triple point of water as obtained by the participants during the course of the comparison.

-222-
25.291 2

25.291 -

25.290 8

o^ 25.290 6

H

•^ 25.290 4

25.290 2

25.290

- Q.:

2mK

1

.

i • ^

.: j.^-.^^^^m^^eeBR'<*^ ": "" A

^ .

-NIST#l,0.68mK

XNIST#2, O.SlmK

XNIST#3, 0.34mK • VSL, 0.84inK

ANIST#4, 0.45mK

10 20 30 40

number of TPW readings

50 60

Figure 5. The resistance of SPRT 1094 (Hart Model 5681) at the triple point of water as obtained by the participants during the course of the comparison.

o

25.14 53

25.14 52

25.14 51

t

H 25.14 50

25.14 49 T

25.14 48

ImK

^ ^ <•• ^jr

25 50

number of TPW readings

75

-NIST#l,0.33mK

XNIST#2,0.36mK

XNIST#3,0.39mK • NRC, 2.19mK

+NIST#4, 0.35 mK

AIMGC, 0.96mK

NIST#5, 0.37mK

Figure 6. The resistance of SPRT 1098 (Hart Model 5681) at the triple point of water as obtained by the participants during the course of the comparison.

-223-
25.580 8

25.580 6

25.580 4 i

„ 25.580 2

-'-

"o 25.580 ^ 25.579 8

°=^ 25.579 6

25.579 4 i25.579 2 J

25.579 ^

!^

4mK

25 50 75 100

number of TPW readings

125

ANML#1, 14.19 mK

j^NRLM, l.SOmK

i«NML#2, 5.43mK

150

Figure 7. The resistance of SPRT 040 (Isotech Model 0670) at the triple point of water as obtained by NML and NRLM during the course of the comparison.

-224-
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> 2 >

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Measurement Laboratory

'S "? o -J •? H _] -J e;

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ca

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S ai 2; 2 z u

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C) [I

CQ ^ Si J f- 2 2 2 0-

Measurement Laboratory

^ >

^ 2 E

><

t

-2 -

2 S

£: 2

; O In, direct

i D In, inclusive o In, dir. & inc.

-- o o u

<> J.

Measurement Laboratory

<> -r-

<P

CO ^ H J -J C) m 3 2

2 2 2

2

2

a.2 2

1^ 2 >

Figure 20. Differences, with U (95 %), in ITS-90 realizations between laboratories at the In freezing point.

-241-
^ 2

£^

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L.o. ;,{>_; ii

5 51 U "^ -J S

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Z 2 2 '=^ ^ 2 >

z >

Measurement Laboratory Measurement Laboratory

S

3

><

2

>< -2

n .0

O In, direct D In, inclusive O In, dir. & inc.

n

Measurement Laboratory

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nin.

direct

inclusive

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( .:,*

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u =^ -J Q 00 CO S 2 "^ 5 f- -1 -3

-- s CO ;s 0. 3 H S Z 2 Z 2 ^ C

z

"S ^ s s^ S = ^ 00 2

Measurement Laboratory

o In, direct D In. inclusive O In, dir. & inc.

i ; : i

*;' jL; >;- - - T Jim.' \

D

S

S: CO ^ >

Measurement Laboratory Measurement Laboratory

Figure 20. Differences, with U {95 %), in ITS-90 realizations between laboratories at the In freezing point, (continued)

-242-
E

00

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o

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. In4

-

2

-

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Measurement Laboratory Measurement Laboratory

6

4

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Meastrrement Laboratory

; -O' In, direct

I n In, inclusive O In, dir. & inc.

S =

t/5 2

>

Figure 20. Differences, with U (95 %), in ITS-90 realizations between laboratories at the In freezing point, (continued)

-243-
1.5

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Measurement Laboratory

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Measurement Laboratory

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>

Measurement Laboratory

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O Ga, dir. & inc.

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£: 2

ffl ffl ^ ^ E^ ^

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U 5 03

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3 S -' 2 = ^ C/3 Z

Measurement Laboratory

Figure 21. Differences, with 17(95 %), in ITS-90 realizations between laboratories at the Ga melting point.

-244-
-1.5 -

" Ga, direct O Ga, inclusive O Ga, dir. & inc.

JL ; C)

Measurement Laboratory

'•} O Ga, direct

^ Ga, inclusive O Ga, dir. & inc.

Measurement Laboratory

1-5 T

1.0 4

i^ 0.5

t 0.0

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-1.5 ^

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Measurement Laboratory

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1.0 -

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= s^ ^ 2>

Measurement Laboratory

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r

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Measurement Laboratory

5QS=^22:2:zZzg=/,2> — ^ z >

Measurement Laboratory

Figure 21. Differences, with 6^^(95 %), in ITS-90 realizations between laboratories at the Ga melting point, (continued)

-245-
1.5

1.0 ^ 0.5 E

2 0.0

'

C/2

:

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Measurement Laboratory

-1.5

; O Ga, direct

i n Ga. inclusive

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lii22Z2i22|£|> s ° 1 i^Measurement Laboratory

1.3 "

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Measurement Laboratory

Figure 21. Differences, with f7(95 %), in ITS-90 realizations between laboratories at the Ga melting point, (continued)

-246-
i^p

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Measurement Laboratory Measurement Laboratory

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Measurement Laboratory Measurement Laboratory

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ca D :s -J

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Measurement Laboratory Measurement Laboratory

Figure 22. Differences, with U{95 %), in ITS-90 realizations between laboratories at the Hg triple point.

-247-
2.0

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2

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0.0

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Measurement Laboratory

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Measurement Laboratory

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Measurement Laboratory Measxarement Laboratory

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Measurement Laboratory Measurement Laboratory

Figure 22. Difference, with C/(95 %), s in rrS-90 realizations between laboratories at the Hg triple point, (continued)

-248-
2.0 J

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direct

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Measurement Laboratory

Figure 22. Differences, with L'^ (95 %), in ITS-90 realizations between laboratories at the Hg triple point, (continued)

-249-
£ 2

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Measurement Laboratory

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Measurement Laboratory

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Measurement Laboratory

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Measurement Laboratory

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Measurement Laboratory

Figure 23. Differences, with U (95 %), in ITS-90 realizations between laboratories at the Ar triple point.

-250-
6 T

P

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'-) to _! ^ _; C) S

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Measurement Laboratory

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Measurement Laboratory

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u

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Measurement Laboratory

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^^ 2

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Measurement Laboratory

Figure 23. Differences, with L*'(95 %), in ITS-90 realizations between laboratories at the Ar triple point, (continued)

-251-
fc4 D

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Measurement Laboratory

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Measurement Laboratory

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.{),...... ()

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c/o Z

Measurement Laboratory

Figure 23. Differences, with U (95 %), in ITS-90 realizations between laboratories at the Ar triple point, (continued)

-252-
Figure 24. Direct, indirect and bilateral comparison results for the gallium melting point.

1.5

1.0

fe 0.0

>< -0.5

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CQ

2

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II

11

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A bilateral

n *

f

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00

005

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2

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Measurement Laboratory

-253-
Figure 25. Direct, indirect and bilateral comparison results for the cadrnium freezing point.

4

3

E

CO2

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-2

u

o

: ^^ \

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•

; ;

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2

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>

-254-
APPENDIX I

Instructions Provided to Participants.

Note: Documents 1 and 2 referred to below are not included in this Report on Key Comparison

3. PROCEDURES TO BE FOLLOWED BY THOSE PARTICIPATING IN THE CCTORGANIZED, AND NIST COORDINATED, COMPARISON OF REALIZATIONS OF

THE ITS-90 OVER THE RANGE

83.8058 K TO 933.473 K

B. W. MANGUM

THERMOMETRY GROUP

NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY

GAITHERSBURG, MD 20899-0001

NOTE: TRANSFER CELLS OF GALLIUM AND CADMIUM ARE SEALED AND

MUST NOT BE OPENED. KEEP CELLS UPRIGHT AT ALL TIMES.

FOR THE GALLIUM AND CADMIUM TRANSFER CELLS:

The distance from bottom of well to liquid level of molten metal is 20.5 cm.

The transfer SPRT immersion depth (sensor midpoint to liquid level for SPRT

162CE)is 18 cm.

Dimensions of the Cd cell: o.d. = 50.0 ± 0.2 mm; length = 460 ± 1 mm

Dimensions of the Ga cell: o.d. = 51.0 ± 0.2 mm; length = 300 ± 1 mm

THE EVIMERSION HEATER (WITH AN ATTACHED THERMISTOR) IS TO BE

USED IN FORMING THE INNER MELT IN THE GALLIUM TRIPLE-POINT

TRANSFER CELL

The instructions and procedures given below must be followed by the participants in the

comparison of realizations of the ITS-90 by the national laboratories. They must have the

capability and competence to realize the scale, as it is defined, at the highest level of accuracy.

Before proceeding with the detailed instructions given below, read the enclosed document

"Document 1 . Criteria and recommendations for optimal realization of the fixed points argon

through aluminum of the ITS-90" (hereafter, called Doc. 1) to make sure that you realize, or will

realize for this intercomparison, the ITS-90 according to the requirements given in that

document. Also, read the other enclosed document, "Document 2. Recommendations for

intercomparisons of fixed-point cells of gallium and of cadmium at the highest level of

accuracy," (hereafter, called Doc. 2) to make sure that you have the capability, and are willing, to

-255-
make intercomparisons of the Ga (and Cd, if you have a high-purity Cd cell) in the way specified

therein.

The range of temperature covered in this comparison is from the triple point of Ar (83.8058 K)

through the freezing point of Al (933.473 K), using a long-stem SPRT and two fixed-point cells. The cells to be intercompared are a Ga transfer (or traveling) triple-point cell and a Cd transfer

freezing-point cell [if the host laboratory has a high-purity (at least 99.9999% pure) Cd cell].

The comparison of the transfer and host Ga cells will give valuable information on the

reproducibility of high-purity Ga cells and the realization of this defining fixed point in the

various national mefrology laboratories. This is of particular importance in regard to discussions

of using the Ga melting point as a possible replacement for the triple point of water (TPW). The

comparison of the Cd cells also will give valuable information on the reproducibility of this fixed

point, which can be used as a check point for calibrations and as one measure of the nonuniqueness of the ITS-90 between Sn and Zn. The SPRT traveling with the Ga and Cd fixedpoint cells is to be measured at the TPW, at the Ga triple-point temperature in the Ga transfer cell

and then again at the TPW. Then the SPRT is to be annealed and calibrated at all of the fixed

points in the range of comparison, i.e., measurements at TPW, Al, TPW, Zn, TPW, Cd, TPW,

Sn, TPW, In, TPW, Ga, TPW, Hg, TPW, Ar and TPW, in that order. If an Ar triple-point cell for

long-stem SPRTs is not available, then the host laboratory may perform the comparison over the

limited range from the Hg triple point to the freezing point of Al. If neither an Ar triple-point

cell nor a Hg triple-point cell is available, then the host laboratory may perform the comparison

over the more limited range from the TPW to the freezing point of Al. Similarly, if the host

laboratory does not have an Al freezing-point cell, then the upper temperature of the comparison

will terminate at the Zn freezing point.

DETAILED INSTRUCTIONS FOR PARTICIPATING LABORATORIES

1. Upon receipt of the SPRT and the two fransfer cells, the host laboratory must inspect the

devices for damage. Then, the host must call the coordinating laboratory, or the regional

sub-coordinating laboratory, as the case may be, to report the condition of the devices. If

there is damage, the sub-coordinating laboratory will give instructions on how to proceed.

2. If no damage has been sustained and after reporting to the sub-coordinating laboratory, the

host must make measurements of the transfer SPRT at two measuring currents (in order to determine the zero-power value) in a TPW cell and in the Ga fransfer cell. The ice mantle

of the TPW cell must have been prepared, i.e., aged, according to the instructions in Doc. 1. Also, the triple point of Ga must have been prepared as indicated in Doc. 1.

3. After completing measurements according to instruction 2, the mA resistance values of

the fransfer SPRT at the TPW and at the Ga triple point, and the W value (for the triplepoint temperature) for the Ga fransfer cell must be communicated to the sub-coordinating

laboratory before proceeding. After receiving this information, the sub-coordinating

laboratory will advise the host laboratory as to the next step to be taken.

4. Following the completion of instruction 3 and after receiving approval from the subcoordinating laboratory to proceed with the comparison, the host laboratory (if it has an Al

-256-
freezing-point cell) must slowly insert the transfer SPRT into an annealing furnace at a temperature that is no greater than 500 °C and then increase the temperature of the furnace

and SPRT to approximately 675 °C over about 45 minutes. After the furnace and SPRT

have reached a temperature of approximately 675 °C, maintain them at that temperature for

four hours. Then, reduce the temperature of the frimace and SPRT to 500 °C over at least a

three-hour period (that is, reduce the temperature at a rate of about 1 °C/h). Once the

temperature of the ftimace and the SPRT have been cooled to 500 °C, slowly remove the

SPRT from the ftimace directly to the room environment. After the SPRT has cooled to room temperature, measure its resistance at the TPW, then at the Ga point in the Ga

fransfer cell, and then again at the TPW, all as specified in Doc. 1.

5. If the host laboratory does not possess an Al freezing-point cell, then following the

completion of instruction 3 and after receiving approval from the (sub)coordinating

laboratory to proceed with the comparison, the host laboratory must slowly insert the

fransfer SPRT into an annealing ftimace at about 500 °C and maintain it at that temperature

for four hours. After this annealing, slowly remove the SPRT from the ftimace directly to the room environment. After the SPRT has cooled to room temperature, measure its resistance at the TPW, at the Ga point in the Ga fransfer cell, and then again at the TPW, all as specified in Doc. 1.

6. If the decrease in the resistance of the SPRT at either the TPW or the Ga triple point, as measured according to instmctions 2 and 4 or 2 and 5, is equivalent to 0.5 mK or greater,

repeat instmction 4 or 5, as appropriate. If the decrease at both of the fixed points is less

than 0.5 mK, proceed to instmction 8.

7. After repeating instmction 4 or 5, as appropriate, the additional decrease in the resistance

of the SPRT at either of these fixed points should be equal to or less than 0.2 mK. If the

differences in the values are larger than 0.2 mK, communicate with the (sub)coordinating

laboratory for ftirther instmctions.

8. After annealing and measurements at the TPW, at the triple point of Ga, and then again at the TPW, calibrate the SPRT over the entfre range, starting at the Al point (or at the Zn

point, if the Al point is not available). Follow Doc. 1 for realizing each of the fixed points.

After measurements at two currents at each of the fixed points, make measurements at two

measuring currents at the TPW. Determine the W value (using zero-power values of R) for

each fixed point, using the TPW value obtained immediately following the measurements

at the other fixed point.

9. After completion of the calibration of the SPRT, the Ga fransfer cell must be compared

with the Ga cell of the host laboratory, according to Doc. 2.

10. Following the comparison of the Ga cells, the Cd fransfer cell must be compared with the

Cd cell of the host laboratory, according to Doc. 2, if the host laboratory owns a Cd cell.

1 1

After completing all of the above measurements, the host laboratory must fransmit the data

and computations to the sub-coordinating laboratory.

-257-
12. After receiving notice from the sub-coordinating laboratory, the host laboratory must return

the devices to the (sub)coordinating laboratory.

13. The host laboratory must complete all of the measurements and return the SPRT and the Ga

and Cd cells to the sub-coordinating laboratory within 8 weeks of the receipt of the devices.

14. With regard to the transport of the transfer cells and SPRT, they will be sent, or hand

carried, by the sub-coordinator to a participant. The preferred method of transfer between

the sub-coordinator and the participating laboratories is hand-carry, when that is possible.

Upon completion of the measurements, the participating laboratory must return the transfer

cells and SPRT to the sub-coordinator, using the same method that was employed to get the

transfer cells and SPRT to the participant.

The transfer cells and SPRT must be insured, if the devices are not hand carried. This will

be the responsibility of the sub-coordinators. The amount of insurance should be:

US$10,000 for the Ga cell, US$12,000 for the Cd cell and US$8,000 for the SPRT.

Attached to each container for the transfer cells and for the SPRT must be an ATA camet,

which consists of several forms relating to the exportation and importation of the transfer

devices. The procedures required by the various countries' Customs must be obeyed

strictly. The camet forms must be completed carefiilly and accurately. This is the

responsibility of the laboratory doing the shipping or carrying the devices to the other

laboratory. The receiving laboratory must check the camet forms very carefiilly upon

receipt.

For those involved in comparisons with PTB, some kind of pro-forma quotation is required

by EC customs regulations. That will be arranged by PTB.

REQUIREMENTS FOR PARTICIPATING LABORATORIES CONCERNING

REPORTING OF DATA TO THE SUB-COORDINATING LABORATORY

The participating host laboratory must send to the sub-coordinating laboratory the following:

1. Immersion curves of SPRT(s) (belonging to the host laboratory) in each of the host's fixedpoint cells that will be involved in the measurements associated with this intercomparison

of realizations of the ITS-90.

2. Immersion depth (and correction, in mK) of the transfer SPRT in each fixed-point cell,

including the TPW cell, that was used in this intercomparison of realizations of the ITS-90.

3. Freezing curves for In, Sn, Cd, Zn and Al cells and melting curves for Ar, Hg and Ga cells

that belong to the host laboratory. These are to have been obtained before receipt of the

transfer SPRT and transfer fixed-point cells.

4. Melting and freezing curves of the Cd transfer cell and melting curve of the Ga transfer

cell.

-258-
5. Resistance values of the SPRT in each of the fixed-point cells, and in the TPW cell obtained following the measurements in each of those other fixed-point cells.

6. Values ofW= R(T in fixed-point cell)/i?(273.16 K). Note: i?(273.16 K) is the resistance at 273.16 K, i.e., the value corrected for the hydrostatic head in the TPW cell, and NOT the

value directly obtained with the SPRT in the TPW cell.

7. Values of fr= R(defining T of fixed-point)//?(273.16 K). Note: i?(273.16K) is the

resistance at 273.16 K, i.e., the value corrected for the hydrostatic head in the TPW cell,

and A^Orthe value directly obtained with the SPRT in the TPW cell. Also, i?(defming Tof

fixed-point) is the resistance value at the defining fixed-point temperature and NOT the

resistance value directly obtained with the SPRT in the fixed-point cell.

8. The resistances of the SPRT at the host TPW cell temperature and at the triple-point

temperature of the Ga transfer cell, all obtained upon receipt of the SPRT and the transfer

cells.

9. The type of resistance bridge used in the measurements.

1 0. The type of reference resistor used with the resistance bridge and whether or not it is temperature controlled.

11. If the host's fixed-point cells are from a commercial source, the name of the manufacturers

and the model numbers of the cells must be given (the manufacturer's name will not appear

in print).

12. If, contrary to Document 1, a sealed 'transfer' cell, owned by the host laboratory, is used in

the measurements, then that fact must be reported to the sub-coordinating laboratory and

the data giving the comparison of that sealed cell with an open cell must be provided.

13. Submit a progress report to the sub-coordinator at the end of four (4) weeks following

receipt of transfer cells and SPRT. This is to be done by e-mail.

14. Send to the coordinating laboratory (NIST) a copy of everything sent to the subcoordinating laboratory. This also will be done by e-mail, except for curves (freezing,

melting, immersion) of data. Those curves are to be sent by Air Mail.

-259-
APPENDIX II

Instrumentation and experimental details

This appendix contains details of the participants' instrumentation and fixed-point cells,

techniques of nucleation of freezes or preparation of melts, duration of those freezes or melts,

etc.

In this Appendix II we present the information on these topics that was provided by the various

participants. Details of the various participants' instrumentation are given in Table ILL In

Table II.2, we give details of the participants' fixed-point crucibles or containers and of their

furnaces or baths. In Table II.3, we give details of the participants' techniques of nucleation of

freezes or preparation of melts. Also, in this table, we list the duration of those freezes or melts.

Table II. 1 Details of participants' instrumentation used in key comparison 3.

Table II.2. Details of participants' Al, Zn, Cd, Sn, In, Ga, TPW, Hg and Ar cells and their

respective cryostats, furnaces, baths, etc.

Table II.3. Details on participants' techniques of realization of the triple-point, melting-point

or freezing-point temperature of the various fixed points.

-260-
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-262-

J
Table 11.2. 1 . Details of participant's Al cells and their respective furnaces, etc.

NIST NML PTB VNIIM BNM-INM SMU

Cell commercial/Lab made lab made lab made lab made

(HN)

commercial lab made ESfM commercial

Crucible material

(graphite, etc.)

Graphite graphite graphite graphite graphite graphite graphite

Source Ultra Carbon Ultracarbon Isotech Russia Carbone

Lorraine

Carbone of

Amer.

Purity/how purified <5 ppm, F

treated

After manu 99,9999%

(certificate)

99.9995% 99.9997%

Length / cm 24.4 30.0 22 22 28.0 2L0 28.2 Diameter / mm 43 45 42 42 38 34 48

Thermometer well

material

Graphite &

Si02

C/quartz graphite/quart

z

graphite/quartz graphite silica Graphite/

quartz

Thermometer well ID / mm

8 8 8 8 12 7.5 8

Metal sample source Johnson

Matthey

(Spokane)

Johnson

Matthey

(Spokane)

Russia Johnson

Matthey

Johnson

Matthey

Metal sample purity 99.999 96 % 99.9999 % 99.9999 % 99.9999 % 99.9999 % 99.9999 % 99.9999%

Metal sample weight / kg 0.36 0.505 0.360 0.453 0.350 0.35 Crucible container

material

cell: SiOz,

cell holder: Inconel

Quartz

glass

quartz quartz quartz silica cell: Si02,

cell holder: Inconel Open or closed cell Open open sealed closed open closed closed Pressure in cell / kPa 101.325 bled 1 atm

At

(101.325±

0.100) Pa

101.325 81.883

Immersion depth of SPRT

/cm

18 16 17.0 20.0 17.0 17.5/17.0

Crucible container OD / mm

Si02 cell: 48,

Inconel

holder: 51

51 48 48 52 49 54

Furnace details

Furnace or bath? furnace furnace furnace furnace furnace furnace furnace Commercial/Lab made lab made lab made commercial commercial lab made lab made comm. DC or AC heater power dc ac dc ac ac heater ac AC

Furnace control type Automatic Variac Gero Eurotherm Lab made PID PI Furnace controlled by

temperature sensor or by

power settings

temperature

sensor Power controller controller temperature

sensor

sensor temp,

sensor

Temperature stability over

16 hrs (mK)

±8 <100 <100 100 100 <100

How many zones in furnace2 3 2 1 three zones 1 3

Heat pipe liner/working

material

sodium heat pipe

n/a sodium heat pipe

sodium heat pipe

- sodium heat pipe

Uniformity in furnace

(without cell)

<0.01

°C/cm

- <0.1K

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

8 mK range 20 mK 0.01 K o.rc 0.05

-263-
Table II.2. 1 . Details of participant's Al cells and their respective fiamaces, etc. (continued).

NPL BIPM NRC NMiA^SL IMGC MSL

Cell commercial/Lab made lab made no cells lab made lab made lab made no cells Crucible material

(graphite, etc.)

Graphite graphite high density

graphite

graphite

Source Ringsdorf Ultra Carbon LEICO and

Cominco

ULTRA

CARBON

Purity/how purified Baked lOppm 99.9999 % <5ppm

Length / cm 23.4 30 54.0 21.5

Diameter / mm 43 45 50 44

Thermometer well material siKca graphite graphite out, quartz in

sihca

Thermometer well ID / mm 9 11 7.9 10.8 Metal sample source Cominco JME LEICO and

Cominco

Cominco

Metal sample purity 99.9999 % 99.9999 % 99.9999 % 99.9999 %

Metal sample weight / kg 0.237 0.471 0.530 0.350

Crucible container material silica quartz quartz silica Open or closed cell open open open open

Pressure in cell / kPa 101 101.3 101.3+10.1 101.325

Immersion depth of SPRT / cm

17.4 21 24.0 16

Crucible container OD / mm

50 50 44 50

Furnace details

Furnace or bath? fiimace furnace furnace Furnace Commercial/Lab made commercial lab made lab made lab made

DC or AC heater power ac dc dc ac Furnace control type Thyristor pm Eurotherm Automatic

Furnace controlled by

temperature sensor or by

power settings

sensor sensor N-type

thermocouple

temperature

sensor

Temperature stability over

16 hrs (mK)

50 500 50 50

How many zones in furnace 1 1 1 1 Heat pipe liner/working

material

sodium heat pipesodium heat

pipe

sodium heat pipe

Heat pipe

liner Uniformity in furnace

(without cell)

0.2 °C <0.1 °C we have not and

cannot measure(d) this Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

not measured <0.1 °C < 0.03 °C within

stabihty

-264-
Table II.2. 1 . Details of participant's Al cells and their respective furnaces, etc. (continued).

NRLM NIM KRISS

Cell commercial/Lab made graphite lab made lab made

Crucible material

(graphite, etc.)

graphite graphite

Source NIM Ultra carbon

Purity/how purifled 99.995% 99.999%

Length / cm 24.0 25.5 Diameter / mm 34 44

Thermometer well material quartz graphite

Thermometer well ID / mm 8 11 Metal sample source China Johnson

Matthey

Metal sample purity 99.9999 % 99.9999 %

Metal sample weight / kg 0.350 0.5 Crucible container material Silica glass

Open or closed cell closed open

Pressure in cell / kPa 101.325

Immersion depth of SPRT / cm

17.0 16.1

Crucible container OD / mm

50 51

Furnace details

Furnace or bath? furnace furnace furnace

Commercial/Lab made lab made lab made lab made

DC or AC heater power dc ac ac Furnace control type Automatic FID

Furnace controlled by

temperature sensor or by

power settings

temperature

sensor

temperature

sensor

temperature

sensor

Temperature stability over

16 hrs (mK)

10 50

How many zones in furnace yes/NA 3 2 Heat pipe liner/working

material

sodium heat pipe

Uniformity in furnace

(without cell) < 0.2 °C 0.1 °C

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

1.5 °C,

below

0.01 °C

-265-
Table II.2.2. Details of participant's Zn cells and their respective furnaces, etc.

NIST NML PTB VNIIM BNM-INM SMU

Cell commercial/Lab made lab made lab made commercial lab made lab made commercial

Crucible material

(graphite, etc.)

graphite graphite graphite graphite graphite graphite

Source ULTRA

CARBON

ULTRA

CARBON

Isotech Russia Carbone

Lorraine

Carbone of

America

Purity/how purified <5 ppm, F After manufacture

99,9999%

(certificate)

99.9995% 99.9997%

Length / cm 24.4 21.0 22 24.0 21.0 28.2

Diameter / mm 43 45 42 36 34 48

Thermometer well material graphite &

SiO,

pyrex graphite/quart zgraphite sihca graphite &

quartz

Thermometer well ED / mm 8 8 8 12 7.5 8 Metal sample source Johnson

Matthey

(Spokane)

Johnson Matthey (Spokane) Russia Vieille montagne

Johnson

Matthey

Metal sample purity 99.999 968% 99.9999% 99.9999% 99,9999%

(certificate)

99.9999% 99.9999%

Metal sample weight / kg 1.03 1.050 0.887 0.850 0.95 Crucible container material borosihcate Pyrex quartz quartz silica quartz

Open or closed cell open open closed/open open closed sealed

Pressure in cell / kPa 101.325 101.3 101.325 ±0.100 101.325 80.698

Immersion depth of SPRT / cm

18 18.5 17.5 17.0 17.5/17.0

Crucible container OD / mm

50 51 48 52 49 54

Furnace details

Furnace or bath? flimace furnace furnace furnace furnace fiimace

Commercial/Lab made lab made lab made commercial lab made lab made commercial

DC or AC heater power dc ac ac ac ac AC

Furnace control type Automatic Variac Eurotherm Automatic PID PI Furnace controlled by

temperature sensor or by

power settings

temperature

sensor Power controller temperatm-e

sensor

sensor temperature

sensor

Temperature stability over

16 hrs. (mK)

±7 <100 50 100

How many zones in furnace 3

-> 3 3 1 3 Heat pipe liner/working

material

aluminum

core

n/a - - airflow

furnace

Uniformity in furnace

(without cell)

- <0.1K

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

8mK < lOmK/cm 6mK lOmK < 100 mK 0.03 K

-266-
Table II.2.2. Details of participant's Zn cells and their respective furnaces, etc. (continued).

NPL BIPM NRC NMiA^SL IMGC MSL

Cell commercial/Lab made lab made no cells lab made lab made NIST made lab made

Crucible material

(graphite, etc.)

graphite graphite graphite graphite graphite

Source Ringsdorf Ultra Carbon Cominco ULTRA

CARBON

Union

Carbide

Purity/how purified Baked lOppm 99.9999% <5ppm <5 ppm

Lenj»th / cm 23.4 30 49,0 23.5 20.3 Diameter / mm 43 45 50 44 49.5 Thermometer well material silica graphite graphite out, duranin

silica quartz +

graphite

Thermometer well ID / mm 9 11 7.9 10.8 8 Metal sample source Johnson

Matthey

Cominco Cominco Cominco Koch-Light

Metal sample purity 99.9999% 99.9999% 99.9999% 99.9999% 0.5 mg/kg

Metal sample weight / kg 0.638 1.3 0.995 NIST value 0.824

Crucible container material pyrex quartz duran glass pyrex quartz

Open or closed cell open open open open open

Pressure in cell / kPa 101 101.325 101.325 + 10.1 101.325 101.325

Immersion depth of SPRT / cm

17.4 22.5 180 18 12.1 toctr. of sensor Crucible container OD / mm

50 50 44 50 50

Furnace details

Furnace or bath? ftimace furnace furnace furnace furnace

Commercial/Lab made commercial lab made lab made lab made lab made

DC or AC heater power ac dc dc ac ac Furnace control type Thyristor PID Eurotherm Automatic PID 0-xing

Furnace controlled by

temperature sensor or by

power settings

sensor sensor N-type TC temperature

sensor

temperature

Temperature stability over

16 hrs. (mK)

50 100 50 50 200

How many zones in furnace 3 1 3 1 3 Heat pipe liner/working

material

n/a Heat pipe

liner

none

Uniformity in furnace

(without cell)

200 mK <100mK 200 mK

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

not measured <100mK <100mK within

stability

not measured

-267-
Table II.2.2. Details of participant's Zn cells and their respective fiimaces, etc. (continued).

NRLM NIM KRISS

Cell commercial/Lab made commercial lab made lab made

Crucible material

(graphite, etc.)

graphite graphite graphite

Source NIM Ultra Carbon

Purity/how purifled 99.995% 99.999%/B.V

Length / cm 23.0 24.5 25.5

Diameter / mm 57 41 44

Thermometer well material quartz quartz graphite

Thermometer well ID / mm 8 8 11 Metal sample source China Johnson

Matthey

Metal sample purity 99.9999% 99.9999% 99.9999%

Metal sample weight / kg 0.502 0.800 1 Crucible container material quartz silica glass

Open or closed cell open closed open

Pressure in cell / kPa 101.3±1.0 101.325

Immersion depth of SPRT / cm

17.0 17.0 14.0

Crucible container OD / mm

64 49 51

Furnace details

Furnace or bath? furnace fiimace fiimace

Commercial/Lab made commercial fiimace commercial

DC or AC heater power ac ac ac Furnace control type FID Automatic FID

Furnace controlled by

temperature sensor or by

power settings

sensor tenqserature sensortemperature

sensor

Temperature stability over

16 hrs. (mK)

50 mK,

pk-pk

10 10

How many zones in furnace 3 3 3 Heat pipe liner/working

material

Uniformity in furnace

(without cell) <200mK 50 mK

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

20 mK,

pk-pk

1.5 °C,

below

5mK

-268-
Table 11.2.3. Details of participant's Cd cells and their respective furnaces, etc.

NIST NML PTB VNIIM BNM-INM SMU

Cell commercial/Lab made lab made lab made no cells lab made no cells no data provided

Crucible material

(graphite, etc.)

graphite graphite graphite

Source ULTRA

CARBON

Ultracarbon Russia

Purity/how purified <5 ppm, F After

manufacture

99.9999%

Length / cm 24.4 21.0 26.0

Diameter / mm 43 45 36

Thermometer well material graphite Pyrex graphite

Thermometer well ID / mm 8 8 12 Metal sample source Johnson

Matthey

(Spokane)

Johnson

Matthey

(Spokane)

Russia

Metal sample purity 7N 99.9999% 99.9999%

Metal sample weight / kg 1.2 1.200 1.150 Crucible container material borosilicate Pyrex quartz

Open or closed cell open open open

Pressure in cell / kPa 101.325 101.325 101.325±0.100

Immersion depth of SPRT / cm

18 19.0

Crucible container OD / mm

50 51 52

Furnace details

Furnace or bath? Furnace Furnace Furnace Commercial/Lab made lab made lab made lab made lab made

DC or AC heater power do ac ac Furnace control type Automatic Variac lab made

Furnace controlled by

temperature sensor or by

power settings

by

temperature

sensor

Power temperature

sensor

Temperature stability over

16 hrs. (mK)

±6 50

How many zones in furnace 3 3 three zones Heat pipe liner/working

material

aluminum

core

n/a . -

Uniformity in furnace

(without cell)

-

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

6mK <0.01 °C/cm 10 mK

-269-
Table II.2.3. Details of participant's Cd cells and their respective fiimaces, etc. (continued).

NPL BIPM NRC NMiA^SL IMGC MSL

Cell commercial/Lab made no cells no cells lab made lab made lab made no cells Crucible material

(graphite, etc.)

graphite graphite graphite

Source Ultra Carbon Johnson

Matthey / Alpha

ULTRA

CARBON

Purity/how purified lOppm 99.9999% < 5 ppm

Length / cm 30 49.0 21.5

Diameter / mm 45 50 44

Thermometer well material graphite graphite out, duraninsilica

Thermometer well ID / mm 11 7.9 10.8 Metal sample source Johnson

Matthey

Johnson

Matthey / Alpha

Johnson

Matthey

Metal sample purity 99.9999% 99.9999% 99.9999%

Metal sample weight / kg 1.587 1.214 1.18 Crucible container material quartz duran glass pyrex

Open or closed cell open open open

Pressure in cell / kPa 101.325 101.3+10.1 101.325

Immersion depth of SPRT / cm21 20.0 16

Crucible container OD / mm50 44 50

Furnace details

Furnace or bath? Furnace Furnace Furnace fiimace

Commercial/Lab made lab made lab made lab made lab made

DC or AC heater power dc dc ac ac Furnace control type FID Eurotherm Automatic FID 0-xing

Furnace controlled by

temperature sensor or by

power settings

sensor N-type TC temperature

sensor

tercperature

Temperature stability over

16 hrs. (mK)

100 50 50 200

How many zones in furnace 1 3 1 3 Heat pipe liner/working

material

n/a - Heat pipe

liner

none

Uniformity in furnace

(without cell) <100mK 200 mK

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

<100mK <100mK within

stability

not measured

-270-
Table II.2.3. Details of participant's Cd cells and their respective furnaces, etc. (continued).

NRLM NEVT KRISS

Cell commercial/Lab made no cells lab naade no cells Crucible material

(graphite, etc.)

graphite

Source NIM

Purity/how purified 99.995%

Length / cm 24.5

Diameter / mm 41

Thermometer well material quartz

Thermometer well ID / mm 8 Metal sample source China

Metal sample purity 99.9999%

Metal sample weight / kg 0.800

Crucible container material

Open or closed cell closed

Pressure in cell / kPa 101.325

Immersion depth of SPRT / cm

17.0

Crucible container OD / mm

49

Furnace details

Furnace or bath? Furnace Commercial/Lab made lab made

DC or AC heater power ac Furnace control type Automatic

Furnace controlled by

temperature sensor or by

power settings

temperature

sensor

Temperature stability over 16 hrs. (mK)

10

How manv zones in furnace 3 Heat pipe liner/working

material

Uniformity in furnace

(without cell) <0.2°C

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

1.5 K, below

-271-
Table II.2.4. Details of participant's Sn cells and their respective fiimaces, etc.

NIST NML PTB VNHM BNM-INM SMU

Cell commercial/Lab made lab made lab made lab made lab made lab made commercial

Crucible material

(graphite, etc.)

graphite graphite graphite graphite graphite graphite

Source ULTRA

CARBON

After

manufacture

Russia Carbone

Lorraine

Carbone of

America

Purity/how purifled <5 ppm, F After

manufacture

99.9999% 99.9995% 99.9997%

Length / cm 24.4 21.0 22 26.0 21.0 28.2 Diameter / mm 43 45 48 36 34 48

Thermometer well material graphite &

Si02

Pyrex graphite graphite silica graphite &

quartz

Thermometer well ED / mm 8 8 8 12 7.5 8 Metal sample source Johnson

Matthey,

Spokane

Johnson

Matthey,

Spokane

Russia Braconnot Johnson

Matthey

Metal sample purity 99.999998% 99.9999% 99.9999% 99.9999% 99.999 95% 99.9999%

Metal sample weight / kg 1.07 1.100 0.780 1.116 0.823 0.96 Crucible container material borosilicate Pyrex quartz silica quartz

Open or closed cell open open open open closed sealed Pressure in cell / kPa 101.325 101.325 101.325 ±0.100 101.325 80.288

Immersion depth of SPRT / cm

18 17.5 19.0 17.0 17.5/17.0

Crucible container OD / mm

50 51 48 52 49 54

Furnace details

Furnace or bath? Furnace Furnace fiimace fiimace Furnace furnace

Commercial/Lab made Lab made Lab commercial Lab made Lab made commercial

DC or AC heater power dc ac ac ac ac AC

Furnace control type Automatic Variac Eurotherm Lab made PID PI Furnace controlled by

temperature sensor or by

power settings

temperature

sensor Power controller tenperature

sensor

sensor tenperature

sensor

Temperature stability over

16 hrs. (mK)

±6 <0.1°C 50 100

How many zones in furnace 3 3 3 three zones 1 3 Heat pipe liner/working

material

alimiinimi core

n/a - - airflow

fiimace

Uniformity in furnace

(without cell)

- <0.1K

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

5mK <0.01 °C/cm 8mK 10 mK <100mK 0.02 K

-272-
Table II.2.4. Details of participant's Sn cells and their respective furnaces, etc. (continued).

NPL BIPM NRC NMiA^SL IMGC MSL

Cell commercial/Lab made lab made no cells lab made lab made lab made commercial

Crucible material

(graphite, etc)

Graphite graphite graphite graphite graphite

Source Ringsdorf Ultra Carbon Cominco ULTRA

CARBON

unknown

Purity/how purified Baked 10 ppm 99.9999% < 5 ppm unknown

Length / cm 23.4 30 49.0 23.5 20

Diameter / mm 43 45 50 44 43

Thermometer well material silica graphite graphite out, duranin

silica quartz +

graphite

Thermometer well ID / mm 9 11 7.9 10.8 9 Metal sample source Johnson

Matthey

Vulcan Cominco Cominco Leico

Metal sample purity 99.9999% 99.9999% 99.9999% 99.9999% 0.5 mg/Kg

Metal sample weight / kg 0.680 1.183 1.057 NIST value not known

Crucible container material pyrex quartz duran glass pyrex quartz

Open or closed cell open open open open open

Pressure in cell / kPa 101 101.325 101.3+10.1 101.325 101.325

Immersion depth of SPRT / cm

17.4 21.5 20.0 18 13.5 to ctr. of sensor Crucible container OD / mm

50 50 44 50 47

Furnace details

Furnace or bath? Furnace fuinace furnace Furnace furnace Commercial/Lab made Comm. lab lab Lab made commercial

DC or AC heater power ac dc dc ac ac Furnace control type Thyristor PID Eurotherm Automatic Pm 0-xing

Furnace controlled by

temperature sensor or by

power settings

sensor sensor N-type TC temperature

sensor

terrqjerature

Temperature stability over 16 hrs. (mK)

50 100 50 50 200

How many zones in furnace 3 1 3 1 1 Heat pipe liner/working

material

n/a _ Heat pipe

liner

none

Uniformity in furnace

(without cell)

0.2 °C <100mK not measured

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

not measured <100mK <100mK within

stability

not measured

-273-
Table II.2.4. Details of participant's Sn cells and their respective furnaces, etc. (continued).

NRLM NIM KRISS

Cell commercial/Lab made Com. lab made lab made

Crucible material

(graphite, etc.)

graphite graphite graphite

Source NIM Ultra carbon

Purity/how purified 99.995%

99.999%/B.V.

Length / cm 23.0 24.5 25.5

Diameter / mm 57 41 44

Thermometer well material quartz quartz graphite

Thermometer well ID / mm 8 8 11 Metal sample source China Johnson

Matthey

Metal sample purity 99.9999% 99.9999% 99.9999%

Metal sample weight / kg 0.494 0.800 1.0 Crucible container material Pyrex Silica glass

Open or closed cell open open open

Pressure in cell / kPa 101.3±1.0 101.325

Immersion depth of SPRT / cm

17.0 17.0 14.0

Crucible container OD / mm

64 49 51

Furnace details

Furnace or bath? Furnace Furnace F

Commercial/Lab made commercial Lab made commercial

DC or AC heater power ac ac ac Furnace control type FID Automatic FID

Furnace controlled by

temperature sensor or by

power settings

sensor temperature

sensor

temperature

sensor

Temperature stability over

16 hrs. (mK)

50, pk-pk 10 10

How many zones in furnace 3 3 3

Heat pipe liner/working

material

Uniformity in furnace

(without cell) < 0.2 K 50 mK

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

20 mK, pk-pk 1.5 K, below 5mK

-274-
Table II.2.5. Details of participant's In cells and their respective furnaces, baths, etc.

NIST NML PTB VNIIM BNM-INM SMU

Cell commercial/Lab made lab made lab made commercial lab made lab made no cells Crucible material

(graphite, etc.)

graphite graphite graphite Teflon graphite

Source ULTRA

CARBON

Ultracarbon Isotech Russia Carbone

Lorraine

Purity/how purifled <5 ppm, F After

manufacture

99.9999% 99.9995%

Length / cm 24.4 21.0 22 26.5 21.0 Diameter / mm 43 45 42 43 34

Thermometer well material graphite Pyrex graphite/quart z

Teflon silica

Thermometer well ID / mm 8 8 8 8 7.5 Metal sample source Arconium Johnson

Matthey

(Spokane)

Russia Johnson

Matthey

Metal sample purity 99.999 99% 99.9999% 99.9999% 99.9999% 99.9999%

Metal sample weight / kg 1.08 0.990 0.850 0.820

Crucible container material borosilicate Pyrex quartz - silica Open or closed cell open open open open closed Pressure in cell / kPa 101.325 101.325 101.325± 0.100 101.325

Immersion depth of SPRT / cm18 18.5 18.2 17.0

Crucible container OD / mm50 51 48 43 49

Furnace details

Furnace or bath? Furnace Furnace fiimace fiimace Fumace

Commercial/Lab made Lab made Lab commercial Lab made Lab made

DC or AC heater power dc ac ac ac ac Furnace control type Automatic Variac Eurotherm Lab made pro

Furnace controlled by

temperature sensor or by

power settings

temperature

sensor Power controller temperature

sensor

sensor

Temperature stability over

16 hrs./mK

±4 <100 20 100

How many zones in furnace 3 3 3 3 1 Heat pipe liner/working

material

aluminum

core

n/a - - airflow

furnace

Uniformity in furnace

(without cell)

- <0.1 °C

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

5mK < lOmK/cm 8mK 5mK <100mK

-275-
Table II.2.5. Details of participant's In cells and their respective furnaces, baths, etc. (continued).

NPL BIPM NRC NMiA^SL IMGC MSL

Cell commercial/Lab made lab made no cells lab made lab made lab made commercial

Crucible material

(graphite, etc.)

Graphite graphite graphite graphite graphite

Source Ringsdorf Ultra Carbon Preussag pure

metals

ULTRA

CARBON

unknown

Purity/how purified Baked lOppm 99.999 99% < 5 ppm unknown

Length / cm 23.4 30 49.0 21.5 20

Diameter / mm 43 45 50 44 43

Thermometer well material silica graphite graphite out, duraninsilica quartz +

graphite

Thermometer well ID / mm 9 11 7.9 10.8 9 Metal sample source Johnson

Matthey

Arconium Preussag pure

metals

Cominco Leico

Metal sample purity 99.9999% 99.999 99% 99.999 99% 99.9999% 0.5 mg/Kg

Metal sample weight / kg 0.684 1.393 1.063 1.03 not known

Crucible container material pyrex quartz duran glass pyrex quartz

Open or closed cell open open open open open

Pressure in cell / kPa 101 101.325 101.3+10.1 101.325 101.325

Immersion depth of SPRT / cm

17.4 21 18.5 16 13.5 toctr. of sensor Crucible container OD / mm

50 50 44 50 47

Furnace details

Furnace or bath? Furnace furnace fiimace Furnace furnace Commercial/Lab made commercial lab lab made lab made commercial

DC or AC heater power ac do dc ac ac Furnace control type Thyristor FED EuTotherm Automatic PID 0-xing

Furnace controlled by

temperature sensor or by

power settings

sensor sensor N-type TC temperature

sensor

temperature

Temperature stability over

16 hrs./mK

50 100 50 50 200

How many zones in furnace 3 1 3 1 1 Heat pipe liner/working

material

n/a Heat pipe

liner

none

Uniformity in furnace

(without cell)

0.2 °C <100mK not measured

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

not measured <100mK <100mK within

stability

not measured

-276-
Table II.2.5. Details of participant's In cells and their respective furnaces, baths, etc. (continued).

NRLM NIM KRISS

Cell commercial/Lab made Commercial lab made lab made

Crucible material

(graphite, etc.)

graphite graphite Pyrex glass

Source NIM

Purity/how purifled 99.995% cleaning

Length / cm 24.5 18.0 Diameter / mm 41 35

Thermometer well material Quartz Pyrex glass

Thermometer well ED / mm 8 closed 10 Metal sample source China Johnson

Matthey

Metal sample purity 99.9999% 99.9999%

Metal sample weight / kg 0.800 0.7 Crucible container material Pyrex glass

Open or closed cell open closed sealed Pressure in cell / kPa 101.325 101.325

Immersion depth of SPRT / cm

17 11.5

Crucible container OD / mm

49

Furnace details

Furnace or bath? Furnace Furnace Furnace Commercial/Lab made commercial lab made commercial

DC or AC heater power ac ac ac Furnace control type FID Automatic PID

Furnace controlled by

temperature sensor or by

power settings

sensor temperature

sensor

tenqjerature sensor

Temperature stability over 16 hrs./mK

10 10

How many zones in furnace 3 3 3 Heat pipe liner/working

material

Uniformity in furnace

(without cell) <0.2K 50

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

1.5 K,

below

5

-277-
Table II.2.6. Details of participant's Ga cells and their respective furnaces, baths, etc.

NIST NML PTB VNIIM BNM-INM SMU

Cell commercial/Lab made lab made commercial commercial lab made lab made lab made

Crucible material

(graphite, etc.)

virgin PTFE Teflon/nylon Teflon Teflon Teflon PTFE

Source commercial YSI Isotech Russia Weber Mikrotech

Purity/how purified 9 99.9999% chemically

Length / cm 24 32 cm 19.0 18.2 25.1 Diameter / mm 39 36 31 40

Thermometer well material PTFE s/s-nylon Teflon Teflon Nylon PTFE

Thermometer well D) / mm 8 12 8 8.6 8.5 Metal sample source RhonePoulenc

? Russia Alussuisse CMK

Slovakia

Metal sample purity 99.999 995% ? 99.9999% 99.9999% 99.999 99%

Metal sample weight / kg 1.0 7 0.660 0.660 0.93 Crucible container material borosilicate pyrex - Nylon

Open or closed cell open open open open closed open

Pressure in cell / kPa vapor pressure 101.325 101.325±0.100 101.325

Immersion depth of SPRT / cm

18 28.5 12.5 16.5 17.5/17.0

Crucible container OD / mm

51 37 36 50

Furnace details

Furnace or bath? Furnace Water bath calibrator furnace furnace bath

Commercial/Lab made lab made lab made commercial lab made lab made commercial

dc or ac heater power dc dc ac ac ac Furnace control type Automatic electronic Lab made PID PI Furnace controlled by

temperature sensor or by

power settings

teirqjerature sensor PRT temperature

sensor

sensor temperature

sensor

Temperature stability over 16 hrs./mK

±10 10 100 <1

How many zones in furnace 1 1 3 1 Heat pipe liner/working

material

aluminum

core w/

mineral oil

n/a airflow

fiimace

Uniformity in furnace

(without cell) ImK <100mK

over

crucible length

ImK

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

7mK Imk 5mK <100mK

-278-
Table II.2.6. Details of participant's Ga cells and their respective fUmaces, baths, etc. (continued).

NPL BIPM NRC NMiA^SL IMGC MSL

Cell commercial/Lab made lab made commercial

(PyroControle)

lab made commercial lab made commercial

Crucible material

(graphite, etc.) PTFE Teflon Teflon Teflon PTFE PTFE

Source unknown unknown unknown YSI unknown

Purity/how purified acid + water acid + water 99.9999% unknown

Length / cm 19.0 23 20 30.0 17 30

Diameter / mm 38 35 37 approx. 32 28 38

Thermometer well material PTFE Teflon Nylon Teflon SS/Cu PTFE

Thermometer well ID / mm 9 9 11 12 to 13 9 12 Metal sample source Cominco Johnson

Matthey

YSI Alusuisse unknown

Metal sample purity 99.9999% 99.9999% 99.999 99% 99.9999% 99.999 99% 0.5 mg/Kg

Metal sample weight / kg 0.763 1.400 0.400 0.50 unknown

Crucible container material PTFE Teflon quartz aluminum and

Teflon

Pyrex aluminum

and PTFE

Open or closed cell open closed open closed open open

Pressure in cell / kPa 101 101.325 101.325 101.325 vpor

101.325

101.3

Immersion depth of SPRT / cm

17.0 14.2 14 28.0 12 20.5 to ctr. of sensor Crucible container OD / mm

38 50 50 38 50 28

Furnace details

Furnace or bath? Bath furnace,

pulsed air

fiimace oven heater on

metal block

oven

Commercial/Lab made commercial commercial lab made commercial,

YSI

lab made commercial

dc or ac heater power ac dc pulsed dc dc NA

Furnace control type Thyristor PID YSI Automatic electronic Furnace controlled by

temperature sensor or by

power settings

sensor sensor NTC temperature

sensor

temperature

Temperature stability over

16 hrs./mK

100 50 100 10 ±50 not measured

How many zones in furnace 1 1 1 1 1 1 Heat pipe liner/working

material

Pulsed air n/a - Copper

block

none

Uniformity in furnace

(without cell)

100 mK <100mK not measured

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

not measured <100mK 7 within

stability

not measured

-279-
Table 11.2.6. Details of participant's Ga cells and their respective fiimaces, baths, etc. (continued).

NRLM NEM KRISS

Cell commercial/Lab made lab made lab made lab made

Crucible material

(graphite, etc.)

Teflon Teflon Teflon

Source NIM

Purity/how purified cleaning

Length / cm 21.0 31.0

Diameter / mm 41 50

Thermometer well material glass Teflon

Thermometer well ID / mm 8 12 Metal sample source China Johnson

Matthey

Metal sample purity 99.9999% 99.999 99%

Metal sample weight / kg 0.45 0.8 Crucible container material Pyrex glass

Open or closed cell closed open

Pressure in cell / kPa 101.325

Immersion depth of SPRT / cm

14.0 18.0

Crucible container OD / mm

39

Furnace details

Furnace or bath? bath Furnace bath

Commercial/Lab made lab made commercial

dc or ac heater power dc ac Furnace control type Automatic P

Furnace controlled by

temperature sensor or by

power settings

temperature

sensor

temperature

sensor

Temperature stability over

16 hrs./mK

10 5 How many zones in furnace 1 Heat pipe liner/working

material

Uniformity in furnace

(without cell) <0.2K lOmK

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

1 K, above 2mK

-280-
Table II.2.7. Details of participant's TPW cells and their respective baths, etc.

NIST NML PTB VNHM BNM-INM SMU

Manufacturer Jarrett Jarrett Forschungsge

meinschaft

techn. Glas,

Wertheim,

Germany

Lab made NPL SMU made.

Model TBV

Well diameter / mm 13 11 mm 12 8 12 10 Water source and purity? multiple

distilled tap water

Conductivity ~ 4 X best water

The cell has

been

compared to those of some

other NMIs.

double

distillation in quartz apparatus

7 local water

source, conductivity

of water

(after preparation)

at time of

filling less than 40

^siemens

per meter

(corresponds

to 0.02 mK).

Immersion depth of SPRT

in the cell / cm

26.5 26.0 21.5 cm total 19.0 26 24.0 cm for Hart, 23.5 cm for Rosemount

Heat transfer fluid? distilled tap water

water water water Water water

Heat transfer fluid level in

thermometer well (cm)

fiill, 32 cm to mantle

top

21.5 16.0 free level of

the water in the ceil (23

cm)

equal with

the top of

ice mantle

Use of metal bushing? yes, Al

bushing no no no no no

How are mantles

prepared?

immersion

cooler

dry ice/freon

heatpipe

immersion

cooler

Solid CO2 metal rod

cooled with

liquid

nitrogen

crushed

solid CO2

How long are mantles

prepared before use?

10 days >24 hours 36 h 4 days more than

20 hours

minimum of

7 days

How are mantles

maintained - ice or stirred

bath

stirred liquid

bath

distilled water icestirred bath ice stirred bath stirred bath

-281-
Table II.2.7. Details of participant's TPW cells and their respective baths, etc. (continued).

NPL BffM NRC NMiA^SL IMGC MSL

Manufacturer NPL PTB&

KRISS

Jarrett/ Isotech NMi IMGC MSL

Well diameter / mm 12 13 and 12 11 10 10 9

Water source and purity? triple distilled tap water

distilled tap waterfiltered,

demineralised

and doubly

distilled.

triply

distilled tap water

local tap, double

distilled and

degassed

Immersion depth of SPRT

in the cell / cm

19.0 25 23 > 20.0 cm,

dependent on

ceU.

22.5 25.0

Heat transfer fluid? water distilled water

water yes deionized

water

water

Heat transfer fluid level in thermometer well (cm)

20.0 27 15 water 38 24

Use of metal bushing? no no no no no no How are mantles

prepared?

sohd CO2 dry ice dry ice freezing with

special throughflow Uquidnitrogen tubes.

brass rod

precooled in LN2with

alcohol in

the well

liquid N2

boU-off

How long are mantles

prepared before use?

7 days

(for this comparison)

at least 3 days

1 week at least 24

hours.

5 days >3 days

How are mantles

maintained - ice or stirred bath

ice ice, up to 3 monthsice stirred bath,

maintained for several months.

in plexiglass

container in

ice bath

ice

-282-
Table II.2.7. Details of participant's TPW cells and their respective baths, etc. (continued).

NRLM NIM KRISS

Manufacturer commercial NIM commercial

Well diameter / mm 11 8 13 Water source and purity? not evaluated NIM

specific

conductance

(5-1) X

10"^ cm''Ohm''

unknown

Immersion depth of SPRT

in the cell / cm

27.5 24 26.1

Heat transfer fluid? water water water 90% +

ethanol 10%

Heat transfer fluid level in thermometer well (cm) same as the

cell inside water level with SPRT

present

24 30.0

Use of metal bushing? Copper

bushing

no Al bushing

How are mantles

prepared?

Hq N2 cooled

nitrogen gas

liquid N2 Dry Ice powder

How long are mantles

prepared before use?

3 days more than

72 hours

2 months

How are mantles

maintained - ice or stirred

bath

stirred bath ice stirred bath

-283-
Table II.2.8. Details of participant's Hg cells and their respective cryostats, baths, etc.

NIST NML PTB VNIIM BNM-EVM SMU

Cell commercial/Lab made lab made lab made commercial no cells lab made no cells Crucible material

(graphite, etc.)

stainless steel s/s316L high grade

steel SS

Source commercial Whitey Isotech Purity/how purifled ,(2 Length / cm 24 47 19.1 Diameter / mm 38 50 39.2 28

Thermometer well material stainless steel s/s316L high grade

steel SS

Thermometer well ID / mm 8 7 8 8 Metal sample source NIST purified in house Rhones

Alpes mercure Metal sample purity 99.999 999 % < 99.9999 % 99.999 998 % 99.9999%

Metal sample weight / kg 2.3 7 3.00 1.200

Crucible container material stainless steel s/s SS

Open or closed cell closed t/p closed closed Pressure in cell / kPa vapor pressure t/p

Immersion depth of SPRT / cm

15 19 18.0

Crucible container OD / mm

51 39.2

Cryostat details

Cryostat or bath? Bath (with

ethanol)

Alcohol

Bath

calibrator bath

Commercial/Lab made Commercial lab commercial Lab made

DC or AC heater power ac ac Cryostat control type Automatic electronic electronic PID

Cryostat controlled by

temperature sensor or by

power settings

by

tenperature

sensor

byPRT sensor

Temperature stability over

16 hrs./mK

±2 <100 50

How many zones in cryostat

1

Heat pipe liner/working

material

n/a alcohol bath

Uniformity in cryostat

(without cell) ImK <0.05 °C

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

4mK ImK <0.05 °C

-284-
Table II.2.8. Details of participant's Hg cells and their respective cryostats, baths, etc. (continued).

NPL BIPM NRC NMiA^SL IMGC MSL

Cell commercial/Lab made lab made lab made lab made Commercial Commercial

Crucible material

(graphite, etc.)

AISI 304 SS glass glass out, SS/copper in SS steel

Source unknown unknown Cominco commercial unknown

Purity/how purified Acid+water +

steam

99.999 99% unknown

Length / cm 19.5 23.5 25.0 21 23.5 Diameter / mm 35 38 42 40 38

Thermometer well material steel glass glass out, SS/copper in SS steel

Thermometer well ID / mm 10 8 12.5 8 8 Metal sample source Johnson

Matthey

Johnson

Matthey

Cominco commercial unknown

Metal sample purity 99.999 995% 99.999 995% 99.999 99% 99.9999% 20^g/Kg

Metal sample weight / kg 2.430 2.500 2.300 3 unknown

Crucible container material pyrex glass stainless steel pyrex steel Open or closed cell sealed closed closed sealed closed Pressure in cell / kPa Hg vapour triple point vapor

pressure

triple point

Immersion depth of SPRT / cm

16.5 17.5 18.7 15 15.5 toctr. of sensor Crucible container OD / mm

45 63 38 50 39

Cryostat details contains copper

tube as bushing

Cryostat or bath? bath bath bath Heat

exchanger

cryostat

Commercial/Lab made Lab made lab com. ISOT lab made commercial

DC or AC heater power ac dc ac NA

Cryostat control type Thyristor PID Eurotherm electronic Cryostat controlled by

temperature sensor or by

power settings

sensor sensor PtlOO temperature

Temperature stability over

16 hrs./mK

100 100 40 ±0,05 <100

How many zones in cryostat1 1 N/A. 1 1

Heat pipe liner/working

material

n/a alcohol none

Uniformity in cryostat

(without cell)

0.1 °C <0.1 °C not measured

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

<0.1 °C <20mK within

stability

not measured

-285-
Table II.2.8. Details of participant's Hg cells and their respective cryostats, baths, etc. (continued).

NRLM NIM KRISS

Cell commercial/Lab made Commercial lab made Commercial

Crucible material

(graphite, etc.)

none Stainless

steel Source NIM

Purity/how purified - Length / cm 45.0 23.0

Diameter / mm 41 39

Thermometer well material SUS Stainless steel Thermometer well ID / mm 8 8 9.5 Metal sample source China unknown

Metal sample purity 99.9999% unknown

Metal sample weight / kg 2.4 3.0 Crucible container material SUS Stainless steel Open or closed cell sealed closed sealed Pressure in cell / kPa 101.3 Immersion depth of SPRT / cm

>20.0 15.5

Crucible container OD / mm

Cryostat details

Cryostat or bath? bath bath refrigerator

Commercial/Lab made lab made lab made commercial

DC or AC heater power ac ac ac Cryostat control type zero cross Automatic P

Cryostat controlled by

temperature sensor or by

power settings

sensor temperature

sensor

sensor

Temperatiu-e stability over 16 hrs./mK

5 10 10

How many zones in cryostat

1

Heat pipe Uner/working

material

Uniformity in cryostat

(without cell) 5mK lOmK

Temperature distribution over ingot with sample a few kelvins below or above

melting temperature

10 mK 2 K, above 5mK

-286-
Table II.2.9. Details of participant's Ar cells and their respective cryostats, etc.

NIST NML PTB VNIIM BNM-INM SMU

Cell commercial/Lab made lab made commercial lab made no cells Crucible material

(graphite, etc.) OFHC Cu high gradesteel SS

Source BNMINM/CNAM

Purity/how purified chemically

cleaned

chemically

cleaned

Length / cm 15.24 30 (18.0+12.0)

Diameter / mm 79.4 100/30 mm (100/30)

Thermometer well material SS-SPRTs,

Cu-CSPRTs

high grade

steel SS

Thermometer well ID / mm (6@8.1; 1 @

11.3)-SPRTs;

(6@X5.4)-

CSPRTs

8 8

Sample source Airco Air Liquide Air Liquide

gas Sample purity > 99.9999% 99.9998% 99.9999%

Sample weight / kg or moles

15.6 moles

condensed

60 bar / 5 moles0.105

Crucible container material OFHC Cu high grade

steel SS

Open or closed cell closed closed closed Pressure in cell / kPa vapor pressure Immersion depth of SPRT / cm

10.9 30/12 12.0 (m

liquid)

Crucible container OD / mm

(100/30)

Cryostat details

Cryocooler or bath? Liquid N2

bath

Liquid N2

bath

Liquid N2

bath

Commercial/Lab made commercial / lab made

lab made lab made

dc or ac heater power dc

Cryostat control type automatic,

electronic

pressure

control Cryostat controlled by

temperature sensor or by

power settings

temperature

sensor

pressure

control

Temperature stability over

16 hrs./mK

±1 < 50 mK (8 h)

Number of shields for cryostat

1 active, 1 passive

Uniformity in cryostat <200mK

Temperature distribution over sample cell with cell a few kelvins below or above

melting temperature

2mK

-287-
Table II.2.9. Details of participant's Ar cells and their respective cryostats, etc. (continued).

NPL BIPM NRC NMiA^SL IMGC MSL

Cell commercial/Lab made lab made lab made

Crucible material

(graphite, etc.) AISI316or

321 SS

Copper

Source Unknown

Purity/how purified Chemically

cleaned

Length / cm 20 9

Diameter / mm 18 32

Thermometer well material Copper, thin- walled s.s. Thermometer well ID / mm 8 7.4 Sample source Air Liquide

Sample purity 99.9999% 99.9995%

Sample weight / kg or moles

0.03 mol 0.05 mol

Crucible container material foam plastic Cu

Open or closed cell closed Closed

Pressure in cell / kPa vapor pressure 2500 kPa at 20 °C

Immersion depth of SPRT / cm

7.5

Crucible container OD / mm

96

Cryostat details

Cryocooler or bath? liquid N2 liquid No

Commercial/Lab made lab made Lab made

dc or ac heater power ac Dc

Cryostat control type manostat PIDon

shields Cryostat controlled by

temperature sensor or by

power settings

pressure Temperature

sensor

Temperature stability over

16 hrs./mK

<100 ImK

Number of shields for cryostat

2 active shields Uniformity in cryostat not measured

Temperature distribution over sample cell with cell a few kelvins below or above

melting temperature

-

-288-
Table II.2.9. Details of participant's Ar cells and their respective cryostats, etc. (continued).

NRLM NIM KRISS

Cell commercial/Lab made

Crucible material

(graphite, etc.) Source

Purity/how purifled

Length / cm

Diameter / mm

Thermometer well material

Thermometer well ID / mm

Sample source Sample purity

Sample weight / kg or moles

Crucible container material

Open or closed cell Pressure in cell / kPa

Immersion depth of SPRT / cm

Crucible container OD / mm

Cryostat details

Cryocooler or bath?

Commercial/Lab made

dc or ac heater power

Cryostat control type

Cryostat controlled by

temperature sensor or by

power settings

Temperature stability over

16 hrs./mK

Number of shields for cryostat

Uniformity in cryostat

Temperature distribution over sample cell with cell a few kelvins below or above

melting temperature

-289-
Table II.3.1. Details on participant's techniques of realization of the freezing-point temperature of Al.

NIST NML PTB VNIIM BNM-INM

Procedure (freeze or

melt)

freeze freeze HN cells freeze freeze freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight >4h >10h >10h 14 h overnight

Method of nucleation

freeze or melt

induced Self TFP - 0.6 K TFP - 1 K lowering

fiimace

temperature

Method of forming

inner liquid/solid

interface

chilling induced induced induced induced induced

If by chilling, give

method (glass rods,

glass rod 2x rod 1 min cool rod 2x1

min.

cool rod 1 min. two quartz

rods

glass+metal

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

air air air air air air

Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

yes yes no no yes yes

If yes, specify the

material

Inconel quartz tube Inconel Pt

Duration of freeze or melt / h

>16 ~3 10 4 10 6

Was cell used for

freezing point? Melting

point? Triple point?

FP FP FP FP FP FP

-290-
Table II.3. 1 . Details on participant's techniques of realization of the freezing-point temperature of Al. (cont.)

SPRT heat treatment NIST NML PTB PTB VNHM BNM-INM

Was SPRT heated to about 675 °C in preheat furnace before

being transferred to Al

freezing-point cell?

yes yes yes yes yes yes

If yes, how many hours

to reach 675 °C?

1 ~4 4h 2h immediately

After Al freezing point

measurement, was SPRT transferred

directly to annealing

furnace at approximately 675 °C

and then cooled over

several hours to 500 °C

before removing to room temperature?

yes yes yes, 675 °C yes, 670 °C yes yes

If yes, how many

hours?

3.5 ~4 3 to 4 2 4 4

If no, how was SPRT

heat treated?

-291-
Table II.3. 1 . Details on participant's techniques of realization of the freezing-point temperature of Al. (cont.)

SMU NPL BIPM NRC NMiA^SL

Procedure (freeze or

melt)

freeze freeze no cells freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

14 h ~6h overnight typically 12 hours

Method of nucleation

freeze or melt

Furnace temp.

1 °C below FP

until recalescence,

then 3 silica- glass rods for 1 min each, then

fiimace terqj. 0.5 °C below

FP

in furnace T(TP) -4 K

Method of forming

inner liquid/solid

interface

induced induced chilling induced

If by chiUing, give

method (glass rods,

gas, etc.)

silica-glass rod rod rod quartz rod

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

an- air air air

Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

no no no no

If yes, specify the

material

Duration of freeze or melt / h

9.5, minimum 6 >10 6

Was cell used for

freezing point? Melting

point? Triple point?

FP FP FP FP

-292-
Table II.3.1 . Details on participant's techniques of realization of the freezing-point temperature of Al. (cont.)

SPRT heat treatment SMU NPL BIPM NRC NMiA^SL

Was SPRT heated to about 675 °C in pre- heat furnace before

being transferred to Al

freezing-point cell?

yes yes yes yes

If yes, how many hours

to reach 675 °C?

Ih 45 min 1 hour 45 minutes

from 500 °C

to 675 °C

After Al freezing point

measurement, was SPRT transferred

directly to annealing

furnace at approximately 675 °C

and then cooled over

several hours to 500 °C

before removing to room temperature?

maintain at 675 °C for 0.5 h, then decrease to 500 °C over 4 hyes No yes, cooling at

1 °C/min

down to 450 °C

If yes, how many

hours?

4 3.5 3.75

If no, how was SPRT

heat treated?

SPRT placed in 3-zone furnace

at 480 °C and

annealed for approximately

16hrs.

-293-
Table II.3.1. Details on participant's techniques of realization of the freezing-point temperature of Al. (cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

freeze no cells no data provided

freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight overnight 2

Method of nucleation

freeze or melt

induced slow freeze

Method of forming

inner liquid/solid

interface

induced induced induced

If by chilling, give

method (glass rods,

gas, etc.)

silica tube with

alumina

glass rods glass rods

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for

thermal contact

air air air

Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

no no yes

If yes, specify the

material

Inconel

Duration of freeze or

melt / h

40 8 6

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP

-294-
Table II.3. 1 . Details on participant's techniques of realization of the freezing-point temperature of Al. (cent.)

SPRT heat treatment IMGC MSL NRLM NIM KRISS

Was SPRT heated to about 675 °C in pre- heat furnace before

being transferred to Al

freezing-point cell?

yes yes yes

If yes, how many hours

to reach 675 °C?

1 60 min from

500 °C

3

After Al freezing point

measurement, was SPRT transferred

directly to annealing

furnace at approximately 675 °C

and then cooled over

several hours to 500 °C

before removing to room temperature?

yes yes but to <

450 °C

yes

If yes, how many

hours?

4 4 3

If no, how was SPRT

heat treated?

-295-
Table II.3.2. Details on participant's techniques of realization of the freezing-point temperature of Zn.

NIST NML PTB VNIIM BNM-INM

Procedure (freeze or

melt)

freeze freeze freeze freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight >4h >10h 14 h overnight

Method of nucleation

freeze or melt

induced Self TFP - IK lowering

fiimace

temperature

Method of forming

inner Hquid/solid

interface

chilling induced induced induced induced

If by chilling, give

method (glass rods,

gas, etc.)

glass rods 2x rod 1 min thermom. 1 min in air, cool

rod 1 min

two quartz rods glass

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

air air air air air

Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

yes yes no yes yes

If yes, specify the

material

Al quartz tube Al Pt

Duration of freeze or melt / h

>16 -3 8 10 15

Was cell used for

freezing point? Melting

point? Triple point?

FP FP FP FP FP

-296-
Table II.3.2. Details on participant's techniques of realization of the freezing-point temperature of Zn. (cont.)

SMU NFL BIPM NRC NMiA^SL

Procedure (freeze or

melt)

freeze freeze no cells freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

14 h ~6h overnight typically 12 hours

Method of nucleation

freeze or melt

Fimiace temp.

1 °C below FP

until recalescence,

then 3 silica- glass rods for 1 min each, then

ftimace tenjp. 0.5 °C below

FP

in furnace T(TP) -0.2 K

Method of forming

inner liquid/solid

interface

induced induced chilling induced

If by chilling, give

method (glass rods,

gas, etc.)

silica-glass rod rod rod quartz

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

air air air anLiquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

no yes no no

If yes, specify the

material

Al

Duration of freeze or melt / h12 12 >10 >10

Was cell used for

freezing point? Melting

point? Triple point?

FP FP FP FP

-297-
Table II.3.2. Details on participant's techniques of realization of the freezing-point temperature of Zn. (cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

freeze freeze freeze freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight overnight >5h overnight 2

Method of nucleation

freeze or melt

induced slow freeze freeze - slow freeze

Method of forming

inner liquid/solid

interface

induced chilling induced induced induced

If by chilling, give

method (glass rods,

PRT glass rods glass rod glass rods stainless steel

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for

thermal contact

air air air air air

Liquid fluid level in thermometer well / cm

NA

Use of bushing with

REC SPRT?

no no no no yes

If yes, specify the

material

Inconel

Duration of freeze or melt / h

75 10 >10 5 13

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP FP FP

-298-
Table II.3.3. Details on participant's techniques of realization of the freezing-point temperature of Cd.

NIST NML PTB VNIIM BNM-INM

Procedure (freeze or

melt)

freeze freeze freeze freeze no cells

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight >4 hours >10h 14 hours

Method of nucleation

freeze or melt

induced Self Tfp-1K lowering

furnace

temperature

Method of forming

inner liquid/solid

interface

chilling chill chilling induced

If by chilhng, give

method (glass rods,

gas, etc.)

glass rods 2x rod 1 min thermom. 2 min in air, cool

rod 1 min

two quartz rods

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

air air anLiquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

yes yes no yes

Ifyes, specify the

material

Al quartz tube Al

Duration of freeze or melt / h

>16 ~ 3 hours 11

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP FP

-299-
Table II. 3. 3. Details on participant's techniques of realization of the freezing-point temperature of Cd. (cont.)

SMU NFL BIPM NRC NMiA^SL

Procedure (freeze or

melt)

freeze (NIST's cell)freeze no cells freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

14 hours ~6h overnight typically 12 hours

Method of nucleation

freeze or melt

Furnace temp.

1 °C below FP

until recalescence,

then silica- glass rods 3 X

for 1 min.

each, then

fiimace temp.

0.5 °C below

FP

in furnace tpp -0.4 K

Method of forming

inner liquid/solid

interface

chilling chilling chilling chilling

If by chilling, give

method (glass rods, gas, etc.)

silica-glass rod rod rod quartz rod

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for

thermal contact

air air air air

Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

yes no no

If yes, specify the

material

(fromNIST)

Duration of freeze or melt / h

11 16 >10 >10

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP FP

-300-
Table II.3.3. Details on participant's techniques of realization of the freezing-point temperature of Cd. (cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

freeze freeze (NIST's cell) no cell freeze no cell

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight overnight overnight

Method of nucleation

freeze or melt

induced slow freeze

Method of forming

inner liquid/solid

interface

chilling chilling chilling

If by chilling, give

method (glass rods,

gas, etc.)

PRT glass rods glass rods

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

air air air

Liquid fluid level in thermometer well / cm

NA

Use of bushing with

REC SPRT?

no no no

Ifyes, specify the material

Duration of freeze or melt / h

37 10 5

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP

-301-
Table II.3.4. Details on participant's techniques of realization of the freezing-point temperature of Sn.

NIST NML PTB VNIIM BNM-INM

Procedure (freeze or

melt)

freeze freeze freeze freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight >4h >10h 14 h overnight

Method of nucleation

freeze or melt

outside of

fiimace

nucleation

outside of

furnace

nucleation

Tpp-IK outside furnace

nucleation

Method of forming

inner liquid/solid

interface

chilling forms imaided chilling induced dulling

If by chilling, give

method (glass rods,

gas, etc.)

glass rods N/A ingot 2 min in

air, cool rod 1 min

two quartz rods glass rods

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

air

Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

yes yes no yes yes

If yes, specify the

material

Al Quartz tube Al Pt

Duration of freeze or melt / h

>16 ~ 3 hours 9 12 15

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP FP FP

-302-
Table II.3.4. Details on participant's techniques of realization of the freezing-point temperature of Sn. (cont.) SMU NPL BIPM NRC NMiA^SL

Procedure (freeze or

melt)

freeze freeze no cells freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

14 h ~6h overnight typically 12 h

Method of nucleation

freeze or melt

Furnace temp.

1 °C below FP

until recalescence,

then nitrogen gas for 2.5 min, silica glass rod 2 x

for 5 min each,

then ftimace

temp. 0.5 °C

below FP

cell outside

ftimace in air

cell outside

furnace to nucleate, tpp - >20K

Method of forming

inner liquid/solid

interface

chilling chilling chilling chilling

If by chilling, give

method (glass rods,

gas, etc.)

silica-glass

rod, gas

air rod quartz rod

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

air air air air

Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

no no no no

If yes, specify the

material —

Duration of freeze or melt / h12 22 >10 >10

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP FP

-303-
Table II.3.4. Details on participant's techniques of realization of the freezing-point temperature of Sn. (cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

freeze freeze freeze freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight overnight >5h overnight 2h

Method of nucleation

freeze or melt

induced withdrawal

from fiimace

freeze cell outside furnace

cell outside

fiimace

Method of forming

inner liquid/solid

interface

chilling chilling freeze induced

If by chilling, give

method (glass rods,

gas, etc.)

cold gas glass rods gas stainless steel

If by heating, give

method (glass rods,

heater, etc.)

Fluid used in thermometer well for thermal contact

air air air air air

Liquid fluid level in thermometer well / cm

NA

Use of bushing with

REC SPRT?

no no no yes

If yes, specify the

material

Inconel

Duration of freeze or melt / h

52 8 >7 3 11

Was cell used for

freezing point? Melting

point? Triple point?

FP FP FP FP FP

-304-
Table 11.3.5. Details on participant's techniques of realization of the freezing-point temperature of In.

NIST NML PTB VNHM BNM-INM

Procedure (freeze or

melt)

freeze freeze freeze freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight >4 hours >10h 14 hours overnight

Method of nucleation

freeze or melt

induced Self Tpp - IK lowering

furnace

temperature

Method of forming

inner liquid/solid

interface

chilling chill induced chilling

If by chilling, give

method (glass rods,

gas, etc.)

glass rods 2x rod 1 min two quartz rods glass

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for

thermal contact

air siHcone oil air silicone oil

Liquid fluid level in

thermometer well / cm

10

Use of bushing with

REC SPRT?

yes quartz tube no

If yes, specify the

material

Al

Duration of freeze or melt / h

>16 ~3 9 10 10

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP FP FP

-305-
Table II.3.5. Details on participant's techniques of realization of the freezing-point temperature of In. (cont.)

SMU NPL BIPM NRC NMiA^SL

Procedure (freeze or

melt)

no In cell freeze no In cell freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

~6h overnight typically 12 hours

Method of nucleation

freeze or melt

in furnace tpp - 0.5 K

Method of forming

inner liquid/solid

interface

chilling chilling cold rod

If by chilling, give

method (glass rods,

gas, etc.)

rod rod quartz

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for

thermal contact

air air air

Liquid fluid level in thermometer well / cm

n/a

Use of bushing with

REC SPRT?

yes no

If yes, specify the

material

Al

Duration of freeze or melt / h

16 >10 >10

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP

-306-
Table II.3.5. Details on participant's techniques of realization of the freezing-point temperature of In. (cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

freeze freeze freeze freeze freeze

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight overnight >5hrs overnight 2h

Method of nucleation

freeze or melt

induced slow freeze freeze induced slow freeze

Method of forming

inner liquid/solid

interface

chilling chilling chilling chilling induced

If by chilling, give

method (glass rods,

gas, etc.)

PRT glass rods glass rod glass rods stainless steel

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

air air air air air

Liquid fluid level in thermometer well / cmNA

Use of bushing with

REC SPRT?

no no no yes

If yes, specify the

material

Al

Duration of freeze or melt / h42 10 >12 9

Was cell used for freezing point? Melting

point? Triple point?

FP FP FP FP FP

-307-
Table II.3.6. Details on participant's techniques of realization of the melting-point or triple-point temperature of Ga.

NIST NML PTB VNIIM BNM-INM

Procedure (freeze or

melt)

melt melt melt melt melt

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

>10h

Method of nucleation

freeze or melt

induced melt Tmp + 0.5 K increasing

furnace

temperature

Method of forming

inner liquid/solid

interface

immersion

heater

heater heating

If by chilling, give

method (glass rods,

gas, etc.)

15 min

If by heating, give

method (glass rods,

heater, etc.)

40 °C for 45 m water 40 °C heater in thermometer

well

heater

Fluid used in thermometer well for thermal contact

mineral oil water Water oil

Liquid fluid level in thermometer well / cm

full, 22.5 to top of

surface Ga

10

Use of bushing with

REC SPRT?

yes Quartz tube no

If yes, specify the

material

Al

Duration of freeze or melt / h

>16 ~3 14 24 15

Was cell used for freezing point? Melting

point? Triple point?

TP MP MP MP,TP MP

-308-
Table II.3.6. Details on participant's techniques of realization of the melting-point or triple-point temperature of Ga.

(cont.) SMU NPL BIPM NRC NMiA^SL

Procedure (freeze or

melt)

melt melt melt melt melt

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

14hrs

Method of nucleation

freeze or melt

chill 12 h, put

into 30°C bath,

then 40 min. in 40°C bath,

then into 30 °C

bath, then

heater for 30

min

heat slightly

above melting

point

in famace NA

Method of forming

inner liquid/solid

interface

heating heating Heater heating

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.)

heater heater heating in pulsed air furnaceHeater warm water

Fluid used in thermometer well for thermal contact

water oil oil Air water

Liquid fluid level in thermometer well / cmto top level of

Ga

200 mm to top level of

Ga

n/a to height of

Ga

Use of bushing with

REC SPRT?

no no no no

If yes, specify the

material

Duration of freeze or melt / hmin. 20 20 33 >10 6

Was cell used for freezing point? Melting

point? Triple point?

MP TP, MP MP MP MP

-309-
Table II. 3.6. Details on participant's techniques of realization of the melting-point or triple-point temperature of Ga.

(cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

melt melt melt melt melt

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

>ovemight

Method of nucleation

freeze or melt

induced warming heating heating slow melting

Method of forming

inner liquid/solid

interface

heating warming heating induced

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.)

heater warm water glass rods heater

Fluid used in

thermometer well for thermal contact

alcohol water transformer oil water

Liquid fluid level in thermometer vfell 1 cm

45 10 6 30.0

Use of bushing with

REC SPRT?

no no no yes

If yes, specify the

material

Al

Duration of freeze or melt / h

150 >10 >12 21

Was cell used for

freezing point? Melting

point? Triple point?

MP, TP MP MP MP MP

-310-
Table II.3.7. Details on participant's techniques of realization of the triple-point temperature of H2O.

NIST NML PTB VNIIM BNM-INM

Procedure (freeze or melt)Melting, one week after preparing

mantle

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

Method of nucleation

freeze or melt

Mantle

prepared with

immersion

cooler Method of forming

inner liquid/solid

interface

Heating

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.)

Glass rods

Fluid used in thermometer vt^ell for thermal contactWater

Liquid fluid level in thermometer well / cmTo top of well

Use of bushing with

REC SPRT?

Yes

If yes, specify the

material

Al

Duration of freeze or melt / h

Was cell used for

freezing point? Melting

point? Triple point?

TP

-311-
Table 11.3.7. Details of participant's techniques of realization of the triple-point temperature of H2O. (cont.) SMU NPL BIPM NRC NMiA^SL

Procedure (freeze or

melt)

Melting, after preparing

mantle

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze Method of nucleation

freeze or melt

Mantle

prepared with

powdered solid CO2

Method of forming

inner liquid/solid

interface

Heating

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.)

Brass rod

Fluid used in thermometer well for

thermal contact

Water

Liquid fluid level in thermometer well / cm

About 18 cm

Use of bushing with

REC SPRT?

No

Ifyes, specify the

material

Duration of freeze or

melt / h

Was cell used for freezing point? Melting

point? Triple point?

TP

-312-
Table II. 3. 7. Details on participant's techniques of realization of the triple-point temperature of H2O. (cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

If by freezing, give

lengtti of time sample

heated above melting

point before nucleating

freeze Method of nucleation

freeze or melt

Method of forming

inner liquid/solid

interface

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

Ifyes, specify the

material

Duration of freeze or melt / h

Was cell used for freezing point? Melting

point? Triple point?

-313-
Table II. 3. 8. Details on participant's techniques of realization of the triple-point temperature of Hg.

NIST NML PTB VTSTIM BNM-INM

Procedure (freeze or

melt)

melt freeze melt no Hg cells measured

melt

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

>4 hours

Method of nucleation

freeze or melt

induced Self Ttp + 0.3 K

Method of forming

inner liquid/solid

interface

warming chill warming heating

If by chUling, give

method (glass rods,

gas, etc.)

liquid N2

cooled Cu rod

If by heating, give

method (glass rods,

heater, etc.)

copper rods glass rod heater

Fluid used in thermometer well for

thermal contact

ethanol alcohol oil alcohol

Liquid fluid level in thermometer well / cm

full, 42.5 19.0 10

Use of bushing with

REC SPRT?

yes yes no

If yes, specify the

material

Al Quartz tube

Duration of freeze or

melt / h

>16 ~ 3 hours 15 h 8 hours

Was cell used for

freezing point? Melting

point? Triple point?

TP FP(TP) TP TP

-314-
Table II.3.8. Details on participant's techniques of realization of the triple-point temperature of Hg. (cont.)

SMU NFL BIPM NRC NMiA^SL

Procedure (freeze or

melt)

no Hg cells measured

melt no Hg cells measured

melt melt

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

Method of nucleation

freeze or melt

mbath NA

Method of forming

inner liquid/solid

interface

rod NA

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.)

rod rod ext. heater only

Fluid used in thermometer well for thermal contactmethanol alcohol or dry alcohol between

therm well and bushing

but not in bushing

Liquid fluid level in thermometer well / cm20.0 10 cmor cm to metal

height

Use of bushing with

REC SPRT?

no no yes

If yes, specify the

material

copper

Duration of freeze or melt / h

>20h >10 hours >10 hours

Was cell used for

freezing point? Melting

point? Triple point?

TP TP TP

-315-
Table II.3.8. Details on participant's techniques of realization of the triple-point temperature of Hg. (cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

freeze melt freeze - melt

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

overnight >3.5 hrs >5hrs

Method of nucleation

freeze or melt

induced warming both slow melting

Method of forming

inner liquid/solid

interface

chilling wanning

If by chilling, give

method (glass rods,

gas, etc.)

precooled

brass rod

glass rod

If by heating, give

method (glass rods,

heater, etc.)

SPRT glass rod

Fluid used in thermometer well for thermal contact

alcohol ethanol ethanol alcohol

Liquid fluid level in thermometer well / cm

45 18 18 frill

Use of bushing with

REC SPRT?

no no no yes

If yes, specify the

material

Al

Duration of freeze or melt / h

34 >10 3 days 20 3

Was cell used for freezing point? Melting

point? Triple point?

TP TP TP (both) TP TP

-316-
Table II. 3. 9. Details on participant's techniques of realization of the triple-point temperature of Ar.

NIST NML PTB VNIIM BNM-EVM

Procedure (freeze or

melt)

melt data not provided

melt no At cells measured

melt

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze Method of nucleation

freeze or melt

heating after freezing

sample with

hq. N,

Ts + 20 mPC

Method of forming

inner liquid/solid

interface

heating heating

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.)

heater

Fluid used in thermometer well for thermal contact

He gas He gas none

Liquid fluid level in thermometer well / cm

>30cm

Use of bushing with

REC SPRT?

yes no

If yes, specify the

material

stainless steel

Duration of freeze or

melt / h

as long as desired but

always >72 h

5h 8 hours

Was cell used for freezing point? Melting

point? Triple point?

TP TP TP

-317-
Table II.3.9. Details on participant's techniques of realization of the triple-point temperature of Ar. (cont.) SMU NPL BIPM NRC NMiA^SL

Procedure (freeze or

melt) no At cells measured

Melt no At cells measured

Melt data not provided

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze

Method of nucleation

freeze or melt

Heating after freezing

overnight

Method of forming

inner liquid/soHd

interface

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.) Fluid used in thermometer well for thermal contact

none He gas

Liquid fluid level in thermometer well / cm

Use of bushing with

REC SPRT?

No

If yes, specify the

material

Duration of freeze or melt / h

About 3.5 hr meh

>10hrs

Was cell used for freezing point? Melting

point? Triple point?

TP TP

-318-
Table II.3.9. Details on participant's techniques of realization of the triple-point temperature of Ar. (cont.)

IMGC MSL NRLM NIM KRISS

Procedure (freeze or

melt)

data not providedno At cells measured no At cells measured

data not provided no At cells measured

If by freezing, give

length of time sample

heated above melting

point before nucleating

freeze Method of nucleation

freeze or melt

Method of forming

inner liquid/solid

interface

If by chilling, give

method (glass rods,

gas, etc.)

If by heating, give

method (glass rods,

heater, etc.) Fluid used in

thermometer well for

thermal contact Liquid fluid level in

thermometer well / cm

Use of bushing with

REC SPRT?

If yes, specify the

material

Duration of freeze or

melt / h

Was cell used for

freezing point? Melting

point? Triple point?

-319-
APPENDIX III

Immersion Curves

Immersion curves provided by the participants for SPRTs in their fixed-point cells are presented

in Fig. ni.l through Fig. III.9. Not all participants provided the immersion data, although they were requested to do so in the instructions to the participants (see Appendix I). Those not

providing immersion curves were: BIPM, BNM-INM, MSL (NIST Cd only) and NMi-VSL.

Comments on immersion that were provided by BLPM and BNM-INM are given below.

NIM immersion data and curves (there are some problems)

Al - never immersed enough

Zn - unusual behavior

Cd - never immersed enough, but nearly so (4386 may be OK)

Sn - may be immersed enough

In - probably immersed enough, although significant scatter (4386 may be

OK)

Ga - appears to be OK

Hg - curves but no data; may be OK at 0.05 mK level

Ar - no data or curves BIPM SPRTs withdrawn 3 cm in Ga # 128; effect within stated uncertainties

BNM-INM Ar SPRTs raised 3 cm, in 1 cm steps, from bottom of well; temperature

variation observed in accordance with predicted (in sign and magnitude)

Hg SPRTs raised 5 cm, in 1 cm steps, from bottom of well; temperature

decreased in accordance with predicted (in sign and magnitude)

H2O variation of temperature in agreement with predicted

Ga SPRTs raised to 1.5 cm, 3 cm and 5 cm from bottom of well; temperature

variation in agreement with predicted

In SPRTs raised to 1.5 cm, 3 cm and 5 cm from bottom of well; temperature

variation not in perfect agreement with predicted. At 3 cm, the observed

value was 0.3 mK whereas theory predicts 0.1 mK. Difference included in

spurious heat flux component of uncertainty. (Stated to be 0.12 mK)

Sn SPRTs raised to 1.5 cm, 3 cm and 5 cm from bottom of well; temperature

variation not in perfect agreement with predicted. At 3 cm, the observed

value was 0.14 mK whereas theory predicts 0.07 mK. Difference included

in spurious heat flux component of uncertainty (Stated to be 0.05 mK)

Zn SPRTs raised to 3 cm and 5 cm from bottom of well; temperature

variation not in perfect agreement with predicted. At 3 cm, the observed

value was +0.1 mK whereas theory predicts -0.08 mK. Difference

included in spurious heat flux component of uncertainty (Stated to be

0.10 mK)

Al SPRTs raised to 3 cm and 5 cm from bottom of well; temperature

variation not in perfect agreement with predicted. At 3 cm, the observed

value was +0.3 mK whereas theory predicts -0.05 mK. Difference

included in spurious heat flux component of imcertainty (Stated to be

0.20 mK)

-320-
MSL no data or curves except for NIST Cd; MSL believes immersion curves are unnecessary since they have demonstrated to their satisfaction that the

SPRT readings in the various cells are independent of furnace temperature

variations

NMi-VSL no data or curves

For participants that in general provided immersion data and curves, some did not provide

immersion results for a few of the fixed points. These are listed below by fixed point.

Al NML and NRLM did not provide any data

Cd KRISS, NPL, NRLM, PTB and SMU did not provide any data because they have no cells

In NML and SMU did not provide any data; SMU has no cell

Ga NML and NRLM did not provide any data

H2O IMGC, NIM, NML, NPL and NRC did not provide any data

Hg NIM, NML, SMU and VNIIM did not provide any data; SMU and VNIIM have no cells

At IMGC, KRISS, NIM, NML, NPL, NRC, NRLM, PTB, SMU and VNIIM did not provide

any data; KRISS, NRLM, SMU and VNIIM have no cells

-321-
NIST IMGC

0.50

0.25

^ 0.00

-0.25

-0.50 2 4 6 8 10

Distance from bottom of well, cm

KRISS

0.50

0.25

U 0.00

-0.25

-0.50

._ i..

! O KRISS

n 162CE,4386

hydrostatic head

i

4

i ~-~pm

!

i <>

1 <^

2 4 6 8 10

Distance from bottom of well, cm

NRC

0.50

0.25

^ 0.00

-0.25

-0.50

ii O NRC

hydrostatic head

8 10

0.50

0.25

^ 0.00 t&

-0.25

-0.50

<>

i

: o

u

Hart, 1st set

Hart, 2nd set

- hydrostatic head

1

i

' D D

n

j

! o

!

0.50

0.25

^ 0.00 4

-0.25

-0.50

i^

0.50

0.25

0.00

-0.25

-0.50

2 4 6 8 10 Distance from bottom of well, cm

NIM

e ^

~0

O NIM

hydrostatic head

2 4 6 8 10

Distance from bottom of well, cm

PTB

i o PTB

-hydrostatic head „

^__6^

j

1

i «-—-T—~-^

i '

2 4 6

Distance from bottom of well, cm

Figure III. 1 . Immersion curves for the various participants for aluminum.

2 4 6 8 Distance from bottom of well, cm

10

-322-
SMU VNIIM

0.50 1

0.25

I

0.00 <>

-0.25

-0.50

'

1 O SMU 1

hydrostatic head

•

o

< >

:

1

2 4 6 8 10

Distance from bottom of well, cm

0.50

0.25

^ 0.00

-0.25

-0.50

-

1 O VNIIM

I hydrostatic head

o

i

•

2 4 6 8 10

Distance from bottom of well, cm

Figure HI. 1 . Immersion curves for the various participants for aluminxim. (continued)

-323-
NIST IMGC

0.1

0.0

-0.1

-0.2

-0.3

O Hart 5681

D Rosemount 162CE

hydrostatic head

^.

2 4 6 8 10

Distance from bottom of well, cm

KRISS

O KRISS

D 162CE,4386

hydrostatic head

2 4 6 8 Distance from bottom of well, cm

NML

10

i^

0.1 ^

o

1 <> NML ^ ^ hydrostatic head

0.0 <

0.1

0.2

0.3

^ O

i

, ]^^

•

0.1

0.0

-0.1

-0.2

-0.3

^ O Hart 5681

hydrostatic head

^N^;

t o i

!

<>

2 4 6 8 10

Distance from bottom of well, cm

NIM

0.1

0.0

=i -0.1

-0.2

-0.3

TL * A "A J'\ " •— ,.....-: ^1 O NIM !

points off scale hydrostatic head , ^

/

\ i

' :

2 4 6 8 10

Distance from bottom of well, cm

NPL

0.1

0.0

-0.1

-0.2

-0.3

) 2 4 6 8 10

Distance from bottom of well, cm

Figure 111.2. Immersion curves for the varioxis participants for zinc.

-324-

V >N. y >t

j O NPL

1 hydrostatic head

^.^^ < >

_ .

. -_^ ^ ^ ^^\

<> *

1

2 4 6 8

Distance from bottom of well, cm

10
NRC NRLM

0.1

0.0

-0.1

-0.2

-0.3

O NRC ;

1 hydrostatic head

• "'^^^

1 ' ^V^

j ^^"Sis.

2 4 6 8 10

Distance from bottom of well, cm

PTB

^

0.1

0.0

-0.1

-0.2

-0.3

1 O PTB 1

j hydrostatic head |

1 ^""^'^v^

2 4 6 8 10

Distance from bottom of well, cm

VNIIM

0.1

0.0

=^-0.1

-0.2

-0.3 J

^ ^ \ O VNIIM

1 1 hydrostatic head

^\ o ! ;

1 i

^^"\.

o

o

0.1

0.0

p -0.1

-0.2

-0.3

<> pomts

1 L

off scale

i^ \ O NRLM

"hydrostatic head \

2 4 6 8 10

Distance from bottom of well, cm

SMU

0.1 T

2 4 6 8 10

Distance from bottom of well, cm

2 4 6 8 10

Distance from bottom of well, cm

Figure III. 2. Immersion curves for the various participants for zinc, (continued)

-325-
NIST IMGC

0.1

0.0

-0.1

-0.2

-0.3

-0.4

-0.5

a n

Hart 5681

Rosemount 162CE

^. -hydrostatic head ^^|2V^

"^

; :-^

ox

2 4 6 8 Distance from bottom of well, cm

NIM

10

0.1

0.0

-0.1

-0.3

-0.4

-0.5

O \ O NIM

hydrostatic head

• ""

;

^

:

i

! \\

2 4 6 8

Distance from bottom of well, cm

NRC

10

0.1

0.0

-0.1

-0.2

-0.3

-0.4

-0.5

<> NRC i

^'^'X.. ^

hydrostatic head j

! ^'^si ;

i O 1 \^

1

1 ^

0.1

0.0

-0.1

-0.2

-0.3

-0.4

-0.5

'§mm^-'

O IMGC, Hart

hydrostatic head

^\^

o\

0.1

0.0

-0.1

1-0.2

-0.3

-0.4

-0.5

2 4 6 8 Distance from bottom of well, cm

NML

10

1 o NML

'^^ - hydrostatic head

o

\\ o O

A

1 X o

i \^ i

:

: \

10

Distance from bottom of well, cm

VNIIM

2 4 6 8 10

Distance from bottom of well, cm

Figure in.3. Immersion ctirves for the various participants for cadmiunL

2 4 6 8 10 Distance from bottom of well, cm

-326-
NIST IMGC

0.1

0.0

-0.1

-0.2

-0.3 J

? 3

o

n

Hart 5681 | Rosemount 162CE

-hydrostatic head

^^^-sa ^SS^ ' ^

15

Q\.^^

j <>

1 i

2 4 6 8 10

Distance from bottom of well, cm

KRISS

O KRISS

D 162CE,4386

hydrostatic head

2 4 6 8 10

Distance from bottom of well, cm

0.1

0.0

-0.1

-0.2

-0.3

O IMGC, Hart

r :

|: hydrostatic head

0^"^^

i

1 O

2 4 6 8 10 Distance from bottom of well, cm

NIM

0.1

-0.2

-0.3

O NIM —hydrostatic head

2 4 6 8 10

Distance from bottom of well, cm

NML NPL

0.1

0.0

i -0.1

-0.2

-0.3 J

• O NML j

hydrostatic head i M^ o

L o <^

1 o^--.^

1

i

8 10

-0.3 2 4 6

Distance from bottom of well, cm

Figure III.4. Immersion curves for the various participants for tin.

2 4 6 8 Distance from bottom of well, cm

10

-327-
NRC NRLM

i^

0.1

0.0

-0.1

-0.2

-0.3

o

>

O NRC

hydrostatic head ! ^

o <> ^^\^-s^ ^ ^ o ^

i O A

i

f O

<>

•

1

j

1

2 4 6 8 10

Distance from bottom of well, cm

PTB

U

2 4 6 8 10 Distance from bottom of well, cm

VNIIM

0.1

0.0

-0.1

-0.2

-0.3

O VNIIM ^

1 hydrostatic head

">^ i 1

'—.

' < o

<>

i

~ o

^

0.1

0.0

-0.1

-0.2

-0.3

' o !

\ 1 O NRLM

hydrostatic head

^^^~-^'"""-

' o 1

;

t

2 4 6 8 10

Distance from bottom of well, cm

SMU

0.1

0.0

-0.1

-0.2

-0.3

\

• O SMU

1

: hydrostatic head ; o < >>->.^

\ O T-^

1 o 1 ,.1 i

1

1 1

2 4 6 8 10

Distance from bottom of well, cm

2 4 6 8 10

Distance from bottom of well, cm

Figure in.4. Immersion curves for the various participants for tin. (continued)

-328-
NIST IMGC

S

0.1

0.0

-0.1

-0.2

-0.3

-0.4

i O Hart 5681

D Rosemount 162CE

.

hydrostatic head

1

1

,.,i„

,

1 v*\^^

1 ''^^^^^

1 ; o\

i :

1

'

2 4 6 8 10

Distance from bottom of well, cm

KRISS

0.1

0.0

-0.1

O KRISS

D 162CE,4386,w/bushiiig

A 162CE, 4386, no bushing

hydrostatic head

2 4 6 8

Distance from bottom of well, cm

NPL

10

0.1

0.0

-0.1

-0.2

-0.3

-0.4

<lft ^ j

1 hydrostatic head j \ V O

V \\ 1

.

- o

2 4 6 8 Distance from bottom of well, cm

1^S

0.1

0.0

-0.1

t

-0.2

-0.3

-0.4

,, O IMGC, Hart

hydrostatic head ^-^

A^

2 4 6 8 10 Distance from bottom of well, cm

NIM

0.1

0.0

-0.1

s

-0.2

-0.3

-0.4

<,_^^_J>

<> NIM

—^—hydrostatic head - o ^-s^

1 1 A i !

1 ' '

'

'• i

2 4 6 8 10 Distance from bottom of well, cm

NRC

0.1

0.0

-0.1

-0.2

-0.3

-0.4

O NRC

<<^ r

[

1

1

,

\ ^>

i <r\^

i o ^^^^

10 2 4 6 8 10 Distance from bottom of well, cm

Figiire III. 5. Immersion curves for the various participants for indium.

-329-
NRLM PTB

fe4B

0.1

0.0

-0.1

-0.2

-0.3

-0.4

: 1

1 O NRLM

'~^

<r^^^^l^ 1 "-#

'

' ' {

i

i

^s, ^--vO

i

i !

!

2 4 6 8

Distance from bottom of well, cm

VNIIM

10

0.1

0.0

-0.1

-0.2

-0.3

-0.4

j^...„<y„.^....___.^ VNHM

'K^<^

hydrostatic head

^\^ I

"

2 4 6 8

Distance from bottom of well, cm

10

0.1

0.0

-0.1

-0.2

-0.3

-0.4

o

j

i PTB 1

. "^

hydrostatic head ' ^.^ j

^^^--..

. i

i o

'

2 4 6 8 10 Distance from bottom of well, cm

Figure III.5. Immersion curves for the various participants for indium, (continued)

-330-
NIST IMGC

0.15

-0.05 2 4 6 8 10

Distance from bottom of well, cm

KRISS

0.15

0.10

^ 0.05

0.00

-0.05

O KRISS

hydrostatic head \^

t 1 ^

^ ^-^ \ 1

>

i

'

2 4 6 8 10

Distance from bottom of well, cm

NPL

^

0.15

0.10

0.05

0.00

-0.05

jV

i • J >s. : _;. v- A

<

it^"""^ y\

i j

1

1

^^ V

: O NPL

; hydrostatic head 1

2 4 6 8 10

Distance from bottom of well, cm

0.15

0.10

0.05

0.00

-0.05

; O IMGC, Hart

: hydrostatic head \

; i

^,,y^^

i \ 1

i

i !

2 4 6 8 10 Distance from bottom of well, cm

NIM

0.15 n

0.10

0.05

0.00

-0.05

O NIM

hydrostatic head

2 4 6 8 10

Distance from bottom of well, cm

NRC

0.15

0.10 -

^ 0.05

0.00

-0.05

O NRC

hydrostatic head

4>

2 4 6 8 10

Distance from bottom of well, cm

Figure III.6. Immersion curves for the various participants for galliimi.

-331-
PTB SMU

i^

0.15

0.10

0.05

0.00

-0.05 2 4 6 8 10

Distance from bottom of well, cm

VNIIM

0.15

0.10

0.05

0.00

-0.05

^

0.15

0.10

0.05

0.00

-0.05

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! o

O

<

o

-^

^

o

^^

' : j :

2 4 6 8 Distance from bottom of well, cm

2 4 6 8 10

Distance from bottom of well, cm

Figure 111.6. Immersion curves for the various participants for galliimi. (continued)

10

-332-
NIST KRISS

0.15

0.10

s

0.05

0.00

1 O Hart 5681

i D Rosemount 162CE

hydrostatic head

u

o

g .^^

0.15

0.15

0.10 -\

0.05

0.00

-0.05

O NRLM '

\

hydrostatic head j

0.15

0.10

0.05

0.00

-0.05

2 4 6 8 10

Distance from bottom of weU, cm

NRLM

2 4 6 8 10

Distance from bottom of well, cm

PTB

0.15

0.10

% 0.05 -

0.00

-0.05 J

O PTB

hydrostatic head ;

:—

e

1

\

' V

n^^-^^"^"^^

: ' ; i

2 4 6 8 10

Distance from bottom of well, cm

SMU

2 4 6 8 10

Distance from bottom of well, cm

VNIIM

o

-_i

SMU

- hydrostotic head ._

\

i

\ O

o

i i

P^^"

\

0.15

0.10 -

0.05

0.00

-0.05

O VNIIM

hydrostatic head

[ ^^-

^^.^^r-^^"^^

<

02468 10 02468 10

Distance from bottom of well, cm Distance from bottom of well, cm

Figure 111.7. Immersion curves for the various participants for water.

-333-
NIST IMGC

^

0.0

-0.1

-0.2

-0.3

-0.4

-0.5

-0.6

2 4 6

Distance from bottom of well, cm

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2 4 6

Distance from bottom of well, cm

NRC

•V :

; N-

\.

1 >s ON]R.C 1 N$> <>

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^

0.0

-0.1

-0.2

-0.3

-0.4

-0.5 -

-0.6

V

V

^\

«"

\

j - O IMGC, Hart

hydrostatic head 1

2 4 6

Distance from bottom of well, cm

NPL

0.0

-0.1

-0.2

-0.3

-0.4

-0.5

-0.6

O >v

TMJ\ <> ^

) O NPL

hydrostatic head

2 4 6

Distance from bottom of well, cm

NRLM

3 2 4 6 8 "

Distance from bottom of well, cm

Figure in.8. Immersion curves for the various participants for mercury.

2 4 6

Distance from bottom of well, cm

-334-
PTB

2 4 6 8

Distance from bottom of well, cm

Figure III.8. Immersion curves for the various participants for mercury, (continued)

-335-
NIST

^

0.00

-0.05

-0.10

-0.15

-0.20

O Hart 5681

D Rosemount 1 62CE

hydrostatic head

2 4 6

Distance from bottom of well, cm

Figure III.9. Immersion curves for the various participants for argon.

-336-
Appendix IV

Uncertainty Budgets

The suggested components of the uncertainty budget, in addition to the standard deviation, for

key comparison 3 were provided to the participants by the coordinating laboratory, after

consultation with the sub-coordinating laboratories and with the chairman of the CCT Working

Group 3. Those suggested components are given in Table IV. 1(a), IV. 1(b) and rv.l(c).

In this Appendix IV, we also give in Table IV.2 through Table rV.16 the detailed uncertainty

budgets, provided by the participating laboratories, leading to the expanded uncertainty values in

the results reported by the participants.

-337-
Table IV. 1(a). The uncertainty budget reported should include the following.

COMPONENTS OF UNCERTAINTY BUDGET FOR THE

TRIPLE POINT OF WATER

1. Chemical impurities

2. Hydrostatic-head errors (due to error in location of SPRT sensor)

3. Bridge-measurement errors

• effects of changes in reference resistor(s) (due to temperature changes,

etc.) • repeatability of bridge readings

• non-linearity ofbridge

• quadrature effects in ac measurements

4. SPRT self-heating errors

5. Heat flux - immersion errors

6. Effects of moisture on leads, etc. on the measurements

7. Effects of isotopic variations

8. Residual gas pressure in cell (must be of the order of only a few |j.K if cell is acceptable for use)

-338-
Table FV. 1(b). The uncertainty budget reported should include the following.

COMPONENTS OF UNCERTAINTY BUDGET FOR W AT THE

TRIPLE POINT/MELTING POINT/FREEZING POINT, AS

APPROPRIATE, OF

Ar, Hg, Ga, In, Sn, Cd, Zn and AI

1

.

Chemical impurities

2. Hydrostatic-head errors (due to error in location of SPRT sensor)

3. Bridge-measurement errors

• effects of changes in reference resistor(s) (due to temperature changes,

etc.) • repeatability of bridge readings

• non-linearity of bridge

• quadrature effects in ac measurements

4. Uncertainty propagated from the TPW

5. SPRT self-heating errors

6. Heat flux - immersion errors

7. Effects of moisture on leads, etc. on the measurements

8. Errors in gas pressure in the fixed-point cell

9. Errors in choice of fixed-point value as derived from plateau of the

melt/freeze

1 0. High-temperature insulation degradation of SPRT

-339-
Table IV. 1 (c). The uncertainty budget reported should include the following.

UNCERTAINTY BUDGET FOR THE COMPARISON OF

FIXED-POINT CELLS

1

.

Hydrostatic-head errors (due to error in location of SPRT sensor; must include

error in attaining equal fraction of material frozen in the different cells)

2. Adequacy of immersion errors

3. SPRT self-heating errors

4. Bridge-measurement errors

• effects of changes in reference resistor(s) (due to temperature changes,

etc.) • repeatability of bridge readings

• quadrature effects in ac measurements

5. Effects of moisture on leads, etc. on the measurements

-340-
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-368-
Appendix V

Control Charts

In this Appendix, we present the NIST control charts for the NIST check SPRTs in the fixedpoint cells of Al, Zn, Cd, Sn, In, Ga, Hg and Ar.

-369-
Control Chart for NIST Al FP Cell

Check SPRT 0033, ASL F18, 1 mA

25 50 75 100

number of readings

125 150

Control Chart for Cadmium FP Cell

SPRT 009, ASL F18, 1 mA

OCd 78-1, 5N5 pure n=266. s. d -0 25 mK. r- 1 00 mK. ACU 96-6, 7N pure n=35, s.d =0.12 mK, r=0.45 m}C_

100 200 300

number of readings

Control Chart for Indium FP Cell

SPRT 0041, ASL F18, 1 mA

400

0.3

0.2

Oln-l, 6N5 pure. s:> well inside PITli w-cll n=l 84. i. d =0.09 mK, r=0.28 mK

A In 96-3, 7N pure, graphite well n=84, s d.-=0 04 mK, r-O 11 mK

50 100 150 200

number of readings

250 300

Control Chart for NIST Zn FP Cell

Check SPRT 0051, ASL F18, 1 mA

-0.6 100 200 300 400 500

number of readings

Control Chart for NIST Sn FP Cell

Check SPRT 004, ASL F18, 1 mA

-On=302, s.d.-O.lI mK, t-=0.51 mK

100 200 300

nmnber of readings

400

^

>

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0.04

0.02

0.00

-0.02

-0.04

Control Chart for NIST Ga TP CeU

Check SPRT 007, ASL F18, 1 mA

.

: —- On=288,s.d.=0.02mK, r=0.07mK

'^'^""^' o

50 100 150 200 250 300

number of readings

-370-
Control Chart for NIST Hg TP Cell Check SPRT 007, ASL F18, 1 mA

O foam container, n=222,

s,d.=0.08 mK. r=0.37 mK

O' Astirred liquid bath. n=38,

s.d.=0.02 mK, r^0.06 mK

50 100 150 200

number of readings

250 300

Control Chart for NIST Ar TP Cell Check SPRT 008, ASL F18, 1 mA

0.06

0.04

0.02 O, ^'

^ -0.04 4

o ^o On=266,s.d.=0.03mK

=0. 1 i mK

50 100 150 200

number of readings

250 300

-371-
Appendix VI

Additional Tables

Table VI. 1. Standard uncertainties for a single measurement (« = 1) for the fixed points used for

the various participants.

AlFP ZnFP CdFP SnFP InFP GaFP HgTP ArTP

BIPM

TypeA(yt=l,«=l)/mK 0.05

deg. jfreedom 9

TypeB(^=l)/mK 0.07

deg. freedom Inf Mc(>t=l,n=l),mK 0.09

deg. freedom 72.92

k for (95%) 1.99 C/(95%,K=l)/mK 0.18

BNM

TypeA(yt=l,«=l)/mK 0.10 0.46 0.27 0.10 0.04 0.05 0.13

deg. freedom 5 5 5 5 5 5 5 TypeB(yt=l)/mK 1.12 0.45 0.46 0.32 0.15 0.28 0.28

deg. freedom Inf Inf Inf Inf Inf Inf Inf Mc(>t=l,«=l),mK 1.12 0.64 0.53 0.33 0.15 0.29 0.31

deg. freedom 79935.37 19.14 75.78 605.00 1051.25 5580.61 155.51 k for (95%) 1.96 2.09 1.99 1.96 1.96 1.96 1.98 t/(95%,n=l)/mK 2.20 1.35 1.06 0.65 0.30 i 0.57 0.61

IMGC

TypeA(yt=l,«=l)/mK 0.47 0.27 0.15 0.10 0.15 0.05 0.04 0.19

deg. freedom 8 7 8 7 6 11 11 4

Type B (/t=l) / mK 0.41 0.32 0.29 0.18 0.28 0.03 0.12 0.13

deg. freedom Inf Inf Inf Inf Inf Inf Inf Inf Mc(/t=l,«=l),mK 0.62 0.42 0.32 0.21 0.31 0.06 0.13 0.23

deg. freedom 24.99 40.42 181.17 140.93 117.81 18.00 976.96 9.07 k for (95%) 2.06 2.02 1.97 1.98 1.98 2.10 1.96 2.26

t/(95%,«=l)/mK 1.28 0.85 0.63 0.41 0.62 0.13 0.25 0.52

KRISS

TypeA(^=l,«=l)/mK 1.00 0.50 0.40 0.20 0.20 0.20

deg. freedom 6 6 6 9 9 9

TypeB(A:=l)/mK 0.48 0.38 0.23 0.32 0.04 0.06

deg. freedom Inf Inf Inf Inf Inf Inf Mc(/t=l,«=l),mK 1.11 0.63 0.46 0.38 0.20 0.21

deg. freedom 9.11 14.82 10.49 112.03 9.81 10.52

it for (95%) 2.26 2.13 2.21 1.98 2.23 2.21 {7(95%,n=l)/mK 2.51 1.34 1.02 0.74 0.46 0.46

MSL

TypeA()fc=l,n=l)/mK 0.89 0.35 0.20 0.01 0.09

deg. freedom 1 2 1 3 1 TypeB(A=l)/mK 0.47 0.31 0.33 0.18 0.17

deg. freedom Inf Inf Inf Inf Inf

Me (^=1, n=l), mK 1.01 0.47 0J9 0.18 0.19

deg. freedom 1.63 6.41 14.23 289715.30 21.25

k for (95%) 5.39 2.41 2.14 1.96 2.08 ?7(95%,«=l)/mK 5.42 1.13 0.83 0.35 0.40

-372-
Table VI. 1 (cont'd.). Standard uncertainties for a single measurement (n

used for the various participants.

1) for the fixed points

AlFP ZnFP CdFP SnFP InFP GaFP HgTP ArTP

NIM

TypeA(/t=l,n=l)/mK 1.70 0.57 1 1.05 0.57 0.42 0.17 0.26 0.26

deg. freedom 7 7 ! 5 7 7 7 6 6 TypeB(A:=l)/mK 0.70 0.39 0.44 1.54 0.34 0.25 0.14 0.11 deg. freedom 262 25 34 2 33 29 43 30

Mc(^l,«=l),mK 1.84 0.69 1.14 1.64 0.55 0.31 0.30 0.28

deg. freedom 9.62 14.39 6.85 2.84 17.67 33.15 i 9.64 8.03 k for (95%) 2.24 2.14 2.37 3.29 2.10 2.03 i 2.24 2.30 i7(95%,«=l)/mK 4.12 1.47 1 2.71 ! 5.39 1.15 0.62 0.67 0.66

1

NIST

TypeA(/t=l,n=l)/mK 0.28 0.18 0.12 0.12 0.04 0.02 0.07 ' 0.03 deg. freedom 129 405 35 301 83 287 259 265

TypeB(yt-l)/mK 0.16 0.10 0.03 0.02 0.03 0.01 0.01 0.03 deg. freedom Inf Inf lof Inf Inf Inf Inf Inf

Mc (^1, n=\), mK 0.32 0.21 0.12 0.12 0.05 0.02 0.07 0.04

deg. freedom 227.00 693.58 39.51 317.95 202.64 448.44 269.68 1060.00

k for (95%) 1.97 1.96 2.02 1.97 1.97 1.97 1.97 1.96 t/(95%, n=l)/mK 0.64 0.40 0.25 0.24 0.10 0.04 0.14 1 0.08

NML

TypeA(^l,n=l)/mK 0.50 0.21 0.15 0.09 0.06 0.04 ' 0.02 0.01 deg. freedom 120 180 180 180 180 180 180 120

TypeB(A:=l)/mK 0.35 0.18 0.17 0.15 0.41 0.13 0.13 0.49 deg. freedom 120 180 180 180 180 180 180 120

«c (^1, «=1), mK 0.61 0.28 0.23 0.17 0.42 0.13 0.13 0.49

deg. freedom 216.62 354.42 355.79 298.66 186.97 208.12 i 191.10 120.04

k for (95%) 1.97 1.97 1.97 1.97 1.97 1.97 1.97 1.98 U (95%, n=l) / TDK 1.20 0.55 0.45 0.34 0.82 0.26 0.25 0.96

NPL

TypeA(yt=l,«=l)/mK 0.11 0.13 0.13 0.10 0.11 0.22 deg. freedom 8 8 8 2 3 4

TypeB(^=l)/mK 0.43 0.35 0.33 0.20 0.18 0.33 deg. freedom Inf Inf Inf Inf Inf Inf u^{k=l,n=\),mK 0.44 1 0J7 0.35 0.22 0.21 0.40 deg. freedom 2120.57 544.30 443.28 50.00 43.37 43.76

k for (95%) 1.96 1.96 1.97 2.01 2.02 2.02 i7(95%,«=l)/mK 0.87 0.73 0.70 0.45 0.42 0.80

NRC

TypeA(yt=l,«=l)/mK OJO 0.05 0.15 0.17 0.10 ! 0.11 0.06 0.04 deg. freedom 8 9 9 9 9 9 9 9 TypeB(A:=l)/mK 0.43 0.13 0.12 0.34 0.09 0.06 0.05 0.15

deg. freedom Inf Inf Inf Inf Inf Inf Inf Inf uAk=l,n=l),mK 0.53 0.14 0.19 0.38 0.13 0.13 0.08 0.15

deg. freedom 76.76 522.25 25.18 231.87 27.32 15.01 32.81 1281.76

k for (95%) 1.99 1.96 2.06 1.97 2.05 2.13 2.03 I 1.96 U(95%,n=\)/mK. 1.05 0.27 0.40 0.75 0.27 0.27 0.15 ! 0.30

-373-
Table VI. 1 (cont'd.). Standard uncertainties for a single measurement (n = 1) for the fixed points

used for the various participants

AlFP ZnFP CdFP SnFP InFP GaFP HgTP ArTP

NRLM

TypeA(yt=l,n=l)/niK 1.01 0.28 0.17 0.42 0.02 0.15

deg. freedom 3 3 3 2 Inf Inf

TypeB(yk=l)/niK 0.80 0.87 037 0.38 0.11 0.26

deg. freedom Inf Inf Inf Inf Inf Inf Mc(^l,n=l),inK 1.29 0.92 0.41 0.57 0.11 0.30

deg. freedom 7.94 342.15 106.59 6.60 Inf Inf

it for (95%) 2.31 1.97 1.98 2.39 1.96 1.96 U (95%, n=l) / ifK 2.97 1.80 0.81 1.36 0.21 0.58

PTB

TypeA(A=l,n=l)/mK 0.30 0.15 0.15 0.20 0.05 0.05 0.15

deg. freedom 49 149 149 49 199 49 49

TypeB(A=l)/mK 0.83 0.64 0.43 0.56 0.12 0.14 0.27

deg. freedom Inf Inf Inf Inf Inf Inf Inf Ucik=l, n=l), mK 0.88 0.66 0.46 0.59 0.13 0.15 0.31

deg. freedom 3670.07 54952.79 12660.15 3829.13 9093.82 3829.13 880.90

ytfor(95%) 1.96 1.96 1.96 1.96 1.96 1.96 1.96 t/(95%,«=l)/mK 1.73 1.29 0.89 1.17 0.25 0.29 0.61

SMU

TypeA(yt=l, «=l)/mK 0.52 0.35 0.35 0.05

deg. freedom 2 2 2 2

TypeB(yt=l)/mK 0.36 0.36 0.41 0.09

deg. freedom Inf Inf Inf Inf

Mc(it=l,«=l),mK 0.63 0.50 0.53 0.11

deg. freedom 4.44 8.52 11.22 35.81

A: for (95%) 2.67 2.28 2.20 2.03

C/(95%,K=l)/mK 1.69 1.14 1.17 1 0.22

VNIIM

TypeA(A-l,«=l)/mK 0.89 0.89 0.89 0.45 0.45 0.11

deg. freedom 4 4 4 4 4 4

TypeB()fc=l)/mK 0.17 0.15 0.11 0.10 0.13 0.04

deg. freedom Inf Inf Inf Inf Inf Inf

Ucik=l,n=l),mK 0.91 0.91 0.90 0.46 0.47 0.12

deg. freedom 4.29 4.23 4.12 4.41 4.70 5.09

k for (95%) 2.70 2.72 2.74 2.68 2.62 2.56

t/(95%,«=l)/mK 2.46 2.47 2.47 1.23 1.22 030

VSL

TypeA(yt=l,n=l)/mK 0.65 034 0.31 0.29 0.12 0.18 0.32

deg. freedom 64 52 118 42 92 128 64

TypeB(A=l)/mK 0.42 0.34 0.20 0.15 0.17 0.10 0.07

deg. freedom Inf Inf Inf Inf Inf Inf Inf Uc(k=l, «=1), mK 0.77 0.48 0J7 0.33 0.21 0.20 0.33

deg. freedom 129.14 205.57 239.48 66.36 979.51 211.17 70.74

k for (95%) 1.98 1.97 1.97 2.00 1.96 1.97 1.99 U(95%,n=l)/mK 1.53 0.95 0.73 0.65 0.41 0.40 0.65

-374-
Table VI.2. Standard uncertainties quantifying potential changes in SPRTs (listed in column 1)

that were used in KC 3. The associated degrees of freedom {DF) are given also.

SPRT Al Zn Cd Sn In Ga Hg Ar

1030A WspRT / niK 0.239 0.133 0.121 0.094 0.085 0.000 0.000 0.020

DFsfKi 5.254 3.948 7.304 4.421 32.621 NA NA 3.168

1030B WspRT / niK 0.239 0.133 0.121 0.094 0.085 0.000 0.000 0.020

-^^SPRT 5.254 3.948 7.304 4.421 32.621 NA NA 3.168

1032 MspRT / niK 0.000 0.000 0.124 0.128 0.085 0.048 0.000 0.000

DFsfKI NA NA 4.793 5.129 20.093 26.104 NA NA

1094 MsPRT / HlK 0.000 0.000 0.114 0.000 0.057 0.000 0.000 0.000

DFspKT NA NA 4.063 NA 9.281 NA NA NA

1098A MsPRT / mK 0.000 0.125 0.000 0.000 0.073 0.000 0.000 0.000 ^^SPRT NA 2.290 NA NA 14.977 NA NA NA

1098B WspRT / niK 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000

-^' SPRT NA NA NA NA NA NA NA NA

4385 Msprt/ihK 0.000 0.000 0.101 0.000 0.062 0.016 0.000 0.000

DFsPKT NA NA 3.224 NA 10.689 2.900 NA NA

4386 MspRT / niK 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.027

DFsPKT NA NA NA NA NA NA NA 3.733

040 MspRT / niK 1.332 0.510 0.314 0.179 0.074 0.000 0.000 0.000

DFspKT 21.591 17.800 12.701 11.591 4.948 NA NA NA

-375-
Table VI.3. Actual coverage probabilities for expanded uncertainties with different coverage

factors and different degrees of freedom.

Actual

Degrees Coverage

of Probabilities

Freedom for k=l

Actual Value of A: Coverage Needed to Probabilities Obtain 95%

for A=2 Coverage

1 0.500 0.705 12.706

2 0.577 0.816 4.303

3 0.609 0.861 3.182

4 0.626 0.884 2.776

5 0.637 0.898 2.571

6 0.644 0.908 2.447

7 0.649 0.914 2.365

8 0.653 0.919 2.306

9 0.657 0.923 2.262

10 0.659 0.927 2.228

60 0.679 0.950 2.000

Infinity 0.683 0.954 1.960

-376-
Appendix VII. Comments by Participants on Key Comparison Reference Values

The votes by the participating laboratories for and against the use of key comparison reference

values for this comparison were as follows.

Participants opposed to thie use of key comparison reference values

IMGC (Marcarino, Steur) - opposed to a KCRV

KRISS (Gam, Kang) - no KCRV

MSL (White) - no KCRV, but believes that position to be untenable

NIM (Tuning) - no KCRV, unbiased KCRV difficult to obtain

NIST(Mangum, Strouse, Guthrie) - strongly opposed to a KCRV

NMi-VSL (de Groot) - no KCRV, fixed points similar to Josephson volt and

quantum hall resistance comparisons

NRC (Hill) - supports NIST's position. No KCRV.

NRLM (Arai) - no KCRV, impurities bias results

SMU (Duris) - no KCRV, WG should explain why K3 is an "exceptional case"

VNIIM (Pokhodun) - agrees with NIST. No KCRV

Participants in favor of the use of key comparison reference values

BIPM (Stock, Pello) - recommend a KCRV but will agree to the majority opinion

BNM-ENM (Bonnier, Hermier, Renaot) - MRA requires a KCRV, proceed with

the calculation

NML (Connolly) - KCRV required

NPL (Rusby) - KCRV required for Draft B

PTB (Tegeler) - KCRV required by MRA and in assessing Appendix C claims,

but will agree to the majority opinion

Totals: 10 opposed to a KCRV, 5 in favor of a KCRV (BIPM and PTB will agree with the

majority opinion).

The comments that were received from the participating laboratories regarding key comparison

reference values for this comparison are given below. These comments have been extracted

from e-mails sent to NIST.

BIPM (Stock, Pello) - As Terry wrote, the KCRV is part of the MRA which was discussed and

signed by your directors, and so the idea of KCRVs should no longer be questioned

principally, hi paragraph T.3 of the MRA it is stated that 'in exceptional cases' for 'technical

reasons' the results of a KC can be expressed without reference to a KCRV. From this it is clear that the use of a KCRV is to be considered as the norm and indeed a number of KCs has

reached final status expressing the results as d.o.e. with a reference value.

If the calculation of a KCRV is to be considered as the norm, it will be usefiil to think about

its significance. Clearly, there are two distinct purposes: First, a reference value allows to represent the equivalence of laboratories in a concise way without loosing any information

and without wasting too much paper. For this purpose, the actual choice of the reference

value is completely arbitrary in that the differences between pairs of laboratories are always

-377-
the same. In former years (before the MRA) in most cases the results of the pilot laboratory were used as a common reference. This could of course still be done today, but due to the

gain in importance a 'neutral' reference value would nowadays appear as a better choice. This

could be the simple (unweighted) mean, the weighted mean, the median, or any other

statistical indicator.

The second purpose of a KCRV is to provide a 'close, but not necessarily the best,

approximation to the SI value'. Here of course, the technique to determine the KCRV

becomes crucial and it is up to the expertise of the CCT to choose. It would even be possible

to use a KCRV only to represent the results in a simple way, without giving it a physical

significance.

In our opinion, there is clearly no reason against the use of a KCRV in the first sense, that is, to represent the results of KC3 in a concise way. There is no simpler way to represent the

results of a large-scale comparison: one graph per fixed-point which shows all results at the

same time. If the results are presented in a form which is too difficult or too time-consuming

to understand there is the danger that they are not used at all. Seen the limited time left, we

would propose as KCRV the simple mean which avoids discussions about the validity of the

estimated participants' uncertainties, needed for the weighted mean. WG 7 seems to us the

best place where this discussion should take place. The meaning of a KCRV in its relation to the defined temperatures of the ITS-90 needs more consideration. This question was

addressed briefly by Ken. Our opinion is that the defined temperatures of the ITS-90 with

their zero-uncertainty, are applicable to 'ideal' realizations of the corresponding fixed-points.

Since the isotopic composition of the samples is not defined, already fi-om this (incomplete)

definition of the ITS-90 a variation in the temperature of different ideal cells results. The best

way to resolve this problem is to collect a large number of fixed-point cells and to assign the

ITS-90 value to the mean of these cells, some cells giving slightly higher, some slightly

lower temperatures. In addition there are temperature differences due to non-perfect

realizations of the fixed-points due to impurities etc... Again, one way to solve this problem

is to assign the ITS-90 value to the mean. If a model exists about the effect of the impurities,

this information can of course be included, and the ITS-90 value could for example be

assigned to the highest temperature. There really is no paradox in that all laboratories realize

the (same) defined ITS-90 fixed points, but fmd different temperatures. The reason is simply

that no realization is perfect, they all have uncertainties. If this were not so, why do we

perform comparisons? To summarize, we would opt for the calculation of a KCRV, for two

reasons: First it is required by the MRA and we see no reason which would exclude it under

clause T.3 of the MRA. Secondly, it really facilitates the representation of the results of a key

comparison.

(Stock) - The calculation of the pair-wise differences and the corresponding uncertainties

depends not at all on the use or the special choice of a reference value. The only thing you

need for this is a common reference, normally the pilot laboratory, which allows to compare

everyone's results. The decision to introduce a reference value, calculated by one way or the

other, to represent the 'unilateral' results, does in no way influence the bilateral results.

-378-
We also think that the treatment of asymmetric errors is a problem which is not specific to the calculation of reference values. This problem occurs whenever you have to give the result

of a measurement in the form result +/- uncertainty, so in every calibration certificate, etc. So

this problem has to be discussed anyway, not only in the context of key comparisons.

BNM-INM (Bonnier, Renaot, Hermier) - As it was recalled by Terry Quinn and some others,

the MRA is henceforth signed up and, as a consequence, almost any Key comparison must be

associated to a KCRV. The time for discussing the interest of KCRV is now over and we

have, consequently, to turn our attention toward the calculation of its value.

The very difficulty is to find out a method for calculating an unbiased and neutral KCRV

value. To avoid a large and somehow incoherent (web) discussion we should be glad if the

relevant CCT working group was taking the charge of estabhshing a suitable method.

IMGC (Marcarino, Steur) - MGC opposes to a KCRV, but will agree to the opinion of the

majority.

KRISS (Gam, Kang) - KRISS oppose to a KCRV, but will agree to the majority opinion.

MSL (White) - (1) It seems to me that most of the dis-ease/ill-health associated with the KCRV

has to do with the MRA statement that the KCRV "is a good but not necessarily the best

representation of the SI". This is for many comparisons an untestable assertion. For some

cases (including KC3) it is clearly incorrect. However MSL's main objection is that the

statement carries a sense of BIPM approval of the value as a single point of traceability for all measurements on that scale, i.e. replacing the SI. (MSL has always held the view that the

statement should be removed firom the MRA.)

(2) In all but a few comparisons (e.g. where the value of the artifact is known through

independent measurements) a choice of KCRV based only on the measurements submitted to the KC is completely arbitrary. (See the paper submitted as CCT/2000-2 for rationale). In

KC3 for example we could freely choose the NIST value for any one of seven thermometers,

or the results of any other laboratory - any number will do. (In this context assigning an

uncertainty to KCRV is also nonsense)

(3) Following (2): in order to define a KCRV information/data external to the comparison has

to be employed. For example the lOpF comparison of the CCEM recognized that only a few

laboratories have calculable capacitors, which do realize the SI Farad. Therefore the KCRV

was based on a weighted average of their results only. In this case the KCRV does reflect in

some sense the best knowledge of the SI Farad. Note, external information is required to give

meaning to the KCRV and hence to help identify a procedure for calculating the KCRV.

(4) KC3 has little to do with the SI (the unit kelvin). KC3 has compared (indirectly through

SPRTs) the realizations of several natural physical phenomena (the melting and freezing

points) held by the various NMIs. Any W values we measure and the W value we might

choose for a KCRV are dimensionless ratios, and the observed ratios and differences are quite

independent of definition of the kelvin or ITS-90.

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(5) The nature of the uncertainties and errors in our W values are such that we expect a tendency for laboratories with the lowest uncertainties to have the highest W values. I'm not aware of any statistical treatment that can provide a "best value' from such data. (Perhaps we

should in future apply corrections for impurities?)

(6) I am reassured by the conspicuous lack of status accorded the KCRV in the KC reports

published on the BEPM web site. In some cases a numerical value is not given.

NIM (Yuning) - l.NIST method give the results clear enough. 2. How to get a KCRV without

bias is very difficult not only for K3 but also for some other KCs. In this case NIST method is more objective.

NIST(Mangum, Strouse, Guthrie) - Our line of thinking focuses on the fact that to compute a reasonable KCRV in a key comparison in which different laboratories have made

measurements using non-identical transfer standards, the data must first be normalized to a common basis. The normalization of the data usually introduces correlations between

different laboratories' results, and this complicates the computation of the uncertainties of the

pair-wise differences between the laboratories. For the users of KC 3 to be able to make these

complicated and unfamiliar calculations, an extra correlation matrix would be required to obtain correct bilateral uncertainties. This certainly lessens the value of using a KCRV. ... We

are also in agreement with the analysis presented by Alan Steele that shows that reasonable

methods of computing a KCRV can yield qualitatively different results for apparent

agreement between particular laboratories and the KCRV.

NMi-VSL (de Groot) - The assumption that NMi-VSL was not objecting to the position of

NIST: no KCRV, is correct. We understand the arguments of NIST against it as that it shall

generate a lot of work (and a big delay in the processing of draft B) and that fixed points key

comparisons do not allow for a key comparison reference value. The latter argument could fit in the exception clause T.3 of the technical annex of the MRA....So, back to the KCRV. I understand the argument of NIST to be that fixed points have a distribution that does not

allow a simple KCRV. Mainly, I think this is because comparisons we have had so far do not

give enough information about the distribution between fixed points. We do not know the

underlying statistics well enough to be able to choose a KCRV that we think is acceptable for a good indicator for an SI value. For this, we argue that the fixed points are defined for pure

substances. In the ITS-90 only reference is made to isotopic composition being "natural". The

supplementary information (section 2.2.2) refers to metal ingots that must be 6N pure to achieve "the highest possible accuracy". The statement that I so often hear, that the ITS-90 is defined only for pure materials, is something I do not necessarily read in it, though one must

argue that this is the implicit background of the definition. In a way, the statement in T.4 of

the MRA supplement it says that "in some chemical measurements, there may be difficulty in

relating results to the SI. Discussing this with Marten Durieux we thought that perhaps only if

in the report of the key comparison the reference value is defined in terms of being an average

of a number of highest accuracy realizations of the reference points and to specifically state that reference to the SI value is not possible because of the unknown statistical part involved,

we could find a leeway out of this problem? However, in this case we are not looking at a

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pure comparison of fixed points, but it is through travelling SPRTs, except for gallium and

cadmium. This use of SPRT as a transfer for most of the fixed points involved could (I think)

undermine the applicability of clause T.3 and most of what I wrote here. On the other hand,

the added uncertainty of the SPRT could well be a dominant term in the inter-comparison and

than we find that the SI is not well enough approximated by the results this key comparison.

As to other fields, I found Key Comparison Reference Values have not been apphed yet in the case of the comparison of Josephson standards or of the Quantum Hall standards. I consider

this to be equivalent to our (fixed point) case. I understand fi-om my colleague in this field that

the CC-members are not charmed by the idea of a KCRV. I suppose it is based on the same

fear that seems to dominate our field. I think that the pilot representing all the participants has

to be supplied with good arguments in support of its position so that, when we sit round the

CCT-table and debate the report of K3, it shall be very clear that this case is an exception as meant by those writing the MRA. As it is now, I see that we might have not enough

arguments or at least they have not been summarized clearly enough. So either we have to find some more or clearer arguments, or we have to ask NIST to rewrite and recalculate the

data to include a KCRV, which I can imagine to be a very extensive job, almost as large as analyzing the data so far. I can understand and sympathize with the NIST position. Probably

we are in this position because NIST has been very active and soon in processing the data and

while doing had to make assumptions on the MRA: they expected it not to include a KCRV.

As the MRA appeared in its present form this proved to be wrong. I think that the arguments

so far are only just enough to possibly validate this as an exception to the clause in the MRA.

It is the Sl-relation of the KCRV that is worrying me a bit. NRC (Hill) - It seems to me that this "significant unresolved deviation from the key comparison

reference value" issue can be avoided by following the "no KCRV" approach. Otherwise, it appears that we must hope that our uncertainties overlap the KCRV, however defined, or risk

having either to withdraw our cmc's from Appendix C or increase our uncertainties. This

reinforces the point of view that the KCRV represents the "correct" value which we must try to achieve and further raises the spectre of whether we should realize the ITS-90 according to the ideal of the definition, or whether we are forced to seek the "consensus value" represented

by the KCRV.

NML (Connolly) - On the KCRV question I personally do not have a problem with no KCRVs

being specified in the report. My view is that if one wants a reference to difference off one can

achieve this by just eyeballing a graph. I have not been able to obtain his (Director of NML)

view on the interpretation of Page 31 in the MRA. However I am sure he would not insist on

us holding up publication of the report if the majority favours the exclusion of KCRVs.

(Ballico) - Whilst I am not a fan of KCRVs on scientific grounds, I think it is worthwhile to consider two other points that users will have in favour of KCRVs.

(1) It will make life a lot easier for RMOs to link their regional-key-comparisons to the keycomparisons, i.e. without KCRVs I'm not sure how to do it at all (short of a huge matrix). If its clear to anyone I would appreciate some comment.

-381-
(2) As a member of the APMP-CMC review committee I will require a simple, single value

performance indicator for review of CMC entries. If one is not made available, I may need to generate it. Other CMC reviewers will be in a similar position.

NPL (Rusby) - First, it is stated in the MRA that key comparisons lead to the derivation of a KCRV (paragraph 4 of the preamble and Clause Tl), so if we do not do this, we are asking for an exemption. If NIST presents Draft B (or a summary of it) to the CCT without deriving

KCRVs, there will some obligation to give reasons.

Second, I presume that since defining KCRVs is expected to be the norm, arguments for not

doing so are hkely to be effective only if there is some overwhelming scientific or technical reason for not doing so. I don't think the argument that they may be misleading or misused will

carry any more weight in our case than for other comparisons.

Third, as a point of procedure, CCT WG7 and then the CCT itself will debate the report and

decide whether to approve it, and it will no doubt consider the question of whether KCRVs

should be defined and if so how. In fact the question was raised at the CCT meeting in April

but the discussion was interrupted and has not been resumed, apart firom Terry's explanatory

note of 28 April. In it he points out that 'the method chosen for calculating the KCRV is a matter for the participants in each comparison, but in each case the decision must be approved

by the key comparison working group and, in due course, by the Consultative Committee'.

In summary, we will be expected to produce KCRVs unless there are convincing reasons why

we should not. I personally think they will at least have some convenience in providing

baselines for the comparison, whatever 'health warnings' may be needed about their misuse.

As it is, the essential results of CCT-K3 are as given in Tables 21 to 28, but to represent them

graphically (as we should do) requires 15 graphs per fixed point. A KCRV would reduce this

to one.

Finally, I have some difficulty with the view that ours is a special case because of the

symmetric probability distribution of uncertainty. If this is a problem, we have largely ignored

it up to now, in that we routinely issue calibrations to customers using the defined ITS-90

values and normally distributed uncertainties. I think there is an analogy here. To sort it out we

may need some statistical dexterity (but it will never be fiilly rigorous). Otherwise we can

hardly object to defining KCRVs by a conventional method.

NRLM (Arai) - Among the several reasons, we consider that the following point is the most

important: Calculating the simple (or the weighted) mean, without taking account of the effect

of the impurities in the material of the fixed point used in the Key Comparison, would

definitely not reduce the bias caused by the impurities, and is physically meaningless.

PTB (Tegeler) - 1 would like to explain shortly why PTB has changed its position and is now in

favour of a KCRV. I still think that fi-om a metrological point of view there is no need for a KCRV, and I also see the danger that it may be misleading.

-382-
But to my present understanding of the MRA, key comparisons are not primarily a tool for the

improvement of temperature metrology, but an instrument to establish international

equivalence of measurements under regulations described in the MRA and its appendices.

My interpretation of the MRA is that key comparisons can only be included into the key

comparison database if there is a KCRV with an assigned uncertainty. Only on the basis of

this information the RMOs and the JCRB can judge the calibration and measurement

capabilities of the NMIs.

So without the KCRV there might be no accepted CMCs in the Appendix C of the MRA. This

would fundamentally undermine the idea of the MRA, and I think all doubts from the

metrological viewpoint are not worth the struggle that would arise if there are no CMCs. At

least in Europe the consequences for the traceability of temperature measurements between

countries and also between NMIs and accredited laboratories would be a catastrophe.

If my interpretation of the MRA is correct, I think we should accept that there has to be a KCRV. But of course it is the decision of the participants how the KCRV and its uncertainty

will be calculated. My proposal is the weighted mean with a cutoff.

SMU (Duris) - We suppose that now the NIST position is acceptable (no KCRV). We are afraid

that now it is late and not very important to open the discussion concerning the KCRV for the

publishing of draft B. It would be the big job (with doubt of its meaning) and at present it will cause the delay of the presentation of the results. Of course that it (no KCRV) is the situation

of the "exception". We are afraid that for "correct" evaluation of the KCRV there are not

enough information and we were not ready for it in the beginning of the measurement. There

is also the question that there is not the physical significance of this value.

VNIIM (Pokhodun) - I shall try once again to explain the absence of scientific grounds for

KCRV for ITS-90.There is a thermodynamic scale and its approximation ITS-90. Each time,

when improving the ITS we are trying to make it closer to the thermodynamic scale and to improve its smoothness. Each NMI tries to reproduce the ITS-90 as close to the ITS

determination as possible. After the introduction of the KCRV the NMIs will strike to approach to KCRV, but not to the ITS-90 determination. Thus, the infroduction of KCRV will

replace the ITS-90 by some fimction, that has neither physical nor scientific grounds. I think

that KCRV is a random function at an extremely small number of realizations. That is why if

is not possible to speak about the best approximation of KCRV to ITS-90 and moreover after

approval of KCRV to speak about the scale smoothness and its joining with other scale

intervals. Moreover, the comparisons of each reference point result in a set of W values of,

obtained in measurements. The value of some individual thermometer (weighted mean or

other mean value) cannot be considered as KCRV of a particular reference point. We have to assign to the above W value the temperature value according to ITS-90, that cannot be

considered as KCRV. The weighted mean value W (or some other mean value W defined by

some other way) can be used only for determination of the mean line calculated from the

results of measurements carried out by all NMIs and then for evaluating deviations of the

NMIs results from this mean line. So, where is KCRV here? In which form do we hope to get

it, and in what units? Everything, that has a real base in comparisons of reference point, are

-383-
the deviations of results obtained by each NMI, from the mean hne with the uncertainty value

these deviations. The KC3 is over earlier that the document MRA was signed by NMI

directors. I consider that this circumstance is a reason of the arisen problems. I think that it is not possible to neglect the metrology because of not perfected official document (MRA).

Letter from NIST concerning deferment of K3 KCRV (12/01/00):

Dear Key Comparison 3 Participants:

We have reread all of the recent correspondence on the definition of a KCRV for Key

Comparison 3. In this letter, we propose a course of action that we hope the participants can

adopt as a consensus position.

First, let us summarize the results of the polling conducted by Ken Hill. Of the 15 participants,

10 are opposed to a KCRV and 5 are in favor. Of the minority 5, at least two will defer to the

majority vote. Consequently, a position of strictly no KCRV does not appear to meet the

requirement of consensus, which is the absence of significant, sustained opposition. In brief, the

arguments for and against a KCRV are as follows.

Arguments for a KCRV

1

.

The MRA mandates the use of a KCRV, especially for the purpose of computing "significant

unresolved deviations" between the results of an individual laboratory and the KCRV.

2. The display of data in Appendix B and in publication in the open literature is simplified.

Arguments against a KCRV

1

.

There are significant differences in the KCRV value depending on the choice of the KCRV

definition, and there is insufficient information to determine the best choice of the definition.

2. If a KCRV is used, a statistically valid calculation of the uncertainty between laboratories

requires a relatively complex correlation matrix, eliminating the simplicity of presentation

intended by introduction of a KCRV.

3. The asymmetric errors resulting from impurities in fixed-point cells infroduce a bias that is hard to remove from any definition of a KCRV.

4. There is a risk that any KCRV will be interpreted to have a physical meaning that is inappropriate and misleading.

These summaries are not inclusive of all arguments for and against a KCRV, and we refer you to the extensive correspondence for a full statement of all of the arguments for and against.

It is clear to us that a sfrong majority favors the absence of a KCRV, but it is also clear that consensus for this position will be difficult to obtain. Our highest priority is completion of K3,

and with this in mind, we propose the following approach as a compromise:

1. The final Draft A report will not have a KCRV. The report will contain all of the figures and

tables that have previously been sent to you.

2. For publication in the open literature and in Appendix B of the MRA (through the BEPM

website), the data of the comparison will be presented as a bilateral table of differences, with

-384-
associated uncertainties, and a single plot with no identified baseline, such as the sample shown

by Alan Steele for aluminum.

3. Following adoption of Draft B of the report by the CCT, the question of defining "significant

unresolved deviations" will be addressed by the body deemed most appropriate for the task by

the CCT. If a KCRV proves necessary for the purpose of identifying "significant unresolved

deviations" or for other purposes related to the MRA, as identified by the CCT, one will be

generated at that time. As the pilot laboratory, NIST will perform the calculations of such a KCRV if requested to do so.

As documentation of the discussions that have taken place, we also suggest that the e-mails

stating the positions of each participant be placed in an appendix to the final Draft A report. This

appendix would serve as a starting point for fiirther discussions.

This approach has several advantages:

1. Completion of K3 will be as prompt as possible, enabling data entry into Appendix B.

2. With the data complete and agreed upon, there is no temptation for participants to alter uncertainties or data to "cover" their deviation from a KCRV.

3. Neither the CCT as a body nor the K3 participants have considered how "significant

unresolved deviations" are to be defined. In the event that this discussion is lengthy, the

discussion will not impede publication of the K3 results.

At this point, we need each of the participants to respond back to us by Monday, November 20th,

2000, stating whether they can or cannot accept this proposal. If we do not receive a response,

we will interpret that as agreement with this proposal. If consensus cannot be obtained, we fear

that the matter will not be resolved until the next CCT meeting in September of 2001 . A delay of

this length would be very unfortunate and counter-productive.

We thank Franco Pavese and Ken Hill especially for their efforts in clarifying both the content of

the MRA and the positions of all the participants. We thank the participants for all of their

contributions to this discussion, and we look forward to receiving your positions on this

proposal.

Letter from NIST to participants (12/14/00) giving results associated with the NIST letter

of 12/01/00 on a proposed course of action.

Thank you to those participants who responded by the deadline (12/12/00) to the e-mail dated

12/01/00. Based on the vote, the steps outlined in the e-mail dated 12/01/00 concerning the

KCRV will be followed.

K3 Participants in favor (by e-mail vote) of above approach to KCRV in K3:

BIPM, BNM-INM, IMGC, MSL, NIST, NML, NPL, NRC, NRLM, PTB, VNIIM and VSL

K3 Participants in favor (by no response) of above approach to KCRV in K3:

KRISS, NIM and SMU

-385-

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