1

APMP.T-K3.4: Key comparison of realizations of the ITS-90

over the range -38.8344 °C to 419.527 °C

Final report

Prepared by W. Joung (coordinator) and K. S. Gam

Korea Research Institute of Standards and Science (KRISS)

Republic of Korea

A. Achmadi and B. A. Trisna

Research Center for Metrology-LIPI (RCM-LIPI)

Indonesia

April, 2016

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Table of content

1. Introduction 3

2. Participating laboratories 3

3. Artifact 3

4. Measurement procedure 4

5. Summary of raw data submissions 4

6. Link from APMP.T-K3.4 to CCT-K3 4

6.1. Linkage mechanism 5

6.2. Data analysis 9

7. Bilateral differences 12

8. Incomplete submission 16

Appendix 1: Protocol of the APMP.T-K3.4 17

Appendix 2: Measurement data 23

Appendix 3: Uncertainty of the measurement 25

Appendix 5: Immersion curve 27

Appendix 5: Instrumentation 32

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1. Introduction

The APMP bilateral key comparison APMP.T-K3.4 was initiated by the request of RCM-LIPI (Indonesia)

to link their national standards to the average reference values (ARVs) of the CCT-K3. Korea research

institute of standards and science (KRISS, Republic of Korea) was requested to provide the linkage to the

CCT-K3 for the temperature range from -38.8344 °C to 419.527 °C. The protocol of the comparison

(Appendix 1) was agreed by both the laboratories in 2011, and the comparison was carried out in a

participant-pilot-participant sequence from 2011 to 2013.

In the APMP.T-K3.4, two standard platinum resistance thermometers (SPRTs) were chosen as the artifacts,

and they were calibrated at the ITS-90 fixed-points in the comparison range. The fixed-points in this

comparison included Zn FP (419.527 °C), Sn FP (231.928 °C), In FP (156.5985 °C), Ga MP (29.7646 °C),

and Hg TP (-38.8344 °C). The protocol of the APMP.T-K3.4 provided general guidance of the comparison

and the measurement sequence to be performed. Actual realization of the fixed-points and measurement

with the artifacts were carried out according to the local practice. Participants including the pilot were

asked to make all the required corrections such that the resistance ratios were equivalent to the ITS-90

assigned temperature values at 0 mA.

2. Participating laboratories

KRISS (Republic of Korea)

Wukchul Joung, Kee Sool Gam

Korea research institute of standards and science

267 Gajeong-Ro, Yuseong-Gu

Daejeon 34113, Korea

Email: wukchul.joung@kriss.re.kr

RCM-LIPI (Indonesia)

Aditya Achmadi, Beni Adi Trisna

Research Center for Calibration, Instrumentation and Metrology – Indonesian Institute of Sciences

Kompleks PUSPIPTEK Gedung 420

Tangerang Selatan, BANTEN- INDONESIA

Email: aditya_achmadi@yahoo.com

3. Artifact

The artifacts used for this comparison were two SPRTs, and they were provided by RCM-LIPI. The

specifications of the artifacts are as follows.

4

- Serial number: 136 and 160 (hereafter referred to as artifact 1 and artifact 2)

- Model: 670SQ

- Manufacturer: Isotech

- Sheath type: Quartz sheathed

- Sensing element length: 35 mm (distance from the tip of the thermometer to the mid-point of the sensing

element: around 25 mm)

4. Measurement procedure

The SPRTs were first calibrated at RCM-LIPI before being sent to KRISS, the pilot laboratory. After the

calibration at KRISS, the artifacts were sent back to RCM-LIPI to repeat the calibration. Transportation of

the artifacts was done by hand-carrying. Measurements at fixed-points were performed in order of

decreasing temperatures alternating with measurements at the triple point of water.

5. Summary of raw data submissions

Raw data from the participating laboratories are given in Appendix 2. However, for convenience, the

reported resistance ratios are duplicated here in Tables 1 and 2.

Table 1. Resistance ratios received from participants in APMP.T-K3.4 (artifact 1).

Lab W(Zn FP) W(Sn FP) W(In FP) W(Ga MP) W(Hg TP)

RCM-LIPIpre 2.568 308 1.892 463 1.609 571 1.118 096 0.844 187

KRISS 2.568 322 1.892 464 6 1.609 580 6 1.118 094 7 0.844 194 7

RCM-LIPIpost 2.568 311 1.892 460 1.609 570 1.118 096 0.844 194

Table 2. Resistance ratios received from participants in APMP.T-K3.4 (artifact 2).

Lab W(Zn FP) W(Sn FP) W(In FP) W(Ga MP) W(Hg TP)

RCM-LIPIpre 2.568 37 1.892 55 1.609 610 1.118 100 0.844 184

KRISS 2.568 404 1.892 513 6 1.609 617 0 1.118 101 3 0.844 184 7

RCM-LIPIpost 2.568 400 1.892 512 1.609 606 1.118 102 0.844 182

Measurement uncertainties from the participants are also given in Appendix 3, and for convenience, the

uncertainties at the fixed-points are presented here in Table 3.

Table 3. Uncertainties of the fixed-point resistance ratios in mK at 95 % level of confidence and k = 2.

Lab U(Zn FP) U(Sn FP) U(In FP) U(Ga MP) U(TPW) U(Hg TP)

RCM-LIPI 10 8.0 6.5 5.1 3.2 4.3

KRISS 1.3 0.95 0.96 0.64 0.41 0.51

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6. Link from APMP.T-K3.4 to CCT-K3

6.1. Linkage mechanism

KRISS participated in the CCT-K3 and served as the linking laboratory in the APMP.T-K3.4. The linkage

was from the fixed-point resistance ratios of RCM-LIPI to the ARVs of the CCT-K3 through the

difference between the fixed-point resistance ratios of KRISS and the ARVs of the CCT-K3. The linkage

mechanism is as follows.

K3CCTK3CCT

K3CCTK3.4APMP.T

K3.4APMP.TK3.4APMP.T

K3CCTK3.4APMP.T

ARVKRISS

KRISSKRISS

KRISSLIPIRCM

ARVLIPIRCM

T

T

T

T

(1)

Where

K3-CCTK3.4APMP.T ARVLIPIRCM T is the temperature difference between the

fixed-point resistance ratios of RCM-LIPI in

the APMP.T-K3.4 and the ARVs of the CCT-

K3,

K3.4APMP.TK3.4APMP.T KRISSLIPIRCM T is the fixed-point temperature difference

between KRISS and RCM-LIPI measured in

the APMP.T-K3.4,

K3CCTK3.4-APMP.T KRISSKRISS T is the temperature difference between the

fixed-point cells of KRISS in the APMP.T-

K3.4 and those in the CCT-K3,

K3CCTK3CCT ARVKRISS T is the temperature difference between the

fixed-point resistance ratios of KRISS in the

CCT-K3 and the ARVs of the CCT-K3.

The fixed-point temperature difference between KRISS and RCM-LIPI in the APMP.T-K3.4,

K3.4APMP.TK3.4APMP.T KRISSLIPIRCM T was defined as the average of the measured differences

from the two artifacts.

2K3.4APMP.TK3.4APMP.T

1K3.4APMP.TK3.4APMP.T

K3.4APMP.TK3.4APMP.T

KRISSLIPIRCM

KRISSLIPIRCM

2

1

KRISSLIPIRCM

T

T

T

(2)

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The temperature difference between KRISS and RCM-LIPI for each artifact was defined by the difference

in the resistance ratios at the fixed-point.

T

WWW

T

ii

i

d

dKRISSLIPIRCM

KRISSLIPIRCM

rK3.4APMP.TK3.4APMP.T

K3.4APMP.TK3.4APMP.T

(3)

Here, the subscript, i refers to the each artifact. The resistance ratio of RCM-LIPI for an artifact was

defined as the average of the measurement results before and after the measurement at KRISS.

post,K3.4APMP.Tpre,K3.4APMP.T

K3.4APMP.T

LIPIRCMLIPIRCM2

1

LIPIRCM

ii

i

WW

W

(4)

Here, the resistance ratios i

W K3.4APMP.TLIPIRCM and i

W K3.4APMP.TKRISS were the averages

from the 3 repeated measurements.

The temperature difference between the fixed-point cells of KRISS in the APMP.T-K3.4 and those in the

CCT-K3, K3CCTK3.4-APMP.T KRISSKRISS T accounted for any changes in the fixed-point cells

between these two comparisons. In the APMP.T-K3.4, as the same fixed-point cells were used, this

difference vanished but only had uncertainties.

As for the temperature difference between the fixed-point resistance ratios of KRISS in the CCT-K3 and

the ARVs of the CCT-K3, K3CCTK3CCT ARVKRISS T , the results from the CCT-K3 was used.

Table 4 reproduces these results.

Table 4. Temperature difference between the fixed-point resistance ratios of KRISS in the CCT-K3 and

the ARVs of the CCT-K3, and corresponding expanded uncertainties at 95 % level of confidence and k =

2.

Temperature difference / mK

Uncertainty in the temperature difference / mK Zn FP Sn FP In FP Ga MP Hg TP

K3CCTK3CCT ARVKRISS T -0.41 -0.07 1.79 0.04 0.45

K3CCTK3CCT ARVKRISS TU 0.93 0.62 0.72 0.17 0.21

The uncertainty in the temperature difference between the fixed-point resistance ratios of RCM-LIPI and

the ARVs of the CCT-K3 was evaluated based on the following equation under the assumption of no

correlation between the temperature differences in Eq. (1). The expanded uncertainties were evaluated at

95 % level of confidence and k = 2.

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K3CCTK3CCT2

K3CCTK3.4APMP.T2

K3.4APMP.TK3.4APMP.T2

K3CCTK3.4APMP.T2

ARVKRISS

KRISSKRISS

KRISSLIPIRCM

ARVLIPIRCM

TU

TU

TU

TU

(5)

Where

K3-CCTK3.4APMP.T ARVLIPIRCM TU is the expanded uncertainty in the temperature

difference between the fixed-point resistance

ratios of RCM-LIPI in the APMP.T-K3.4 and

the ARVs of the CCT-K3,

K3.4APMP.TK3.4APMP.T KRISSLIPIRCM TU is the expanded uncertainty in the fixed-point

temperature difference between KRISS and

RCM-LIPI measured in the APMP.T-K3.4,

K3CCTK3.4-APMP.T KRISSKRISS TU is the expanded uncertainty in the temperature

difference between the fixed-point cells of

KRISS in the APMP.T-K3.4 and those in the

CCT-K3,

K3CCTK3CCT ARVKRISS TU is the expanded uncertainty in the temperature

difference between the fixed-point resistance

ratios of KRISS in the CCT-K3 and the ARVs

of the CCT-K3.

The expanded uncertainty in the fixed-point temperature difference between KRISS and RCM-LIPI

measured in the APMP.T-K3.4, K3.4APMP.TK3.4APMP.T KRISSLIPIRCM TU was evaluated

based on the following equations.

2K3.4APMP.TK3.4APMP.T2

1K3.4APMP.TK3.4APMP.T2

K3.4APMP.TK3.4APMP.T2

KRISSLIPIRCM

KRISSLIPIRCM

4

1

KRISSLIPIRCM

TU

TU

TU

(6)

2

rK3.4APMP.T

2K3.4APMP.T

2

K3.4APMP.TK3.4APMP.T2

d

dKRISSLIPIRCM

KRISSLIPIRCM

T

WWUWU

TU

ii

i

(7)

post,K3.4APMP.T

2pre,K3.4APMP.T

2

K3.4APMP.T2

LIPIRCMLIPIRCM4

1

LIPIRCM

ii

i

WUWU

WU

(8)

8

In this comparison, SPRT cutoff criteria were used to ensure that uncertainty associated with the travel,

handling, or stability of either SPRT did not dominate the standard uncertainty of the temperature

difference. In this regard, the test for the stability of the travelling artifacts was based on measurements

done by RCM-LIPI before and after the travel to KRISS. Eqs. (9) and (10) show the cutoff criteria used in

this comparison, and an artifact which met both the two criteria was not included in the calculation.

eff,95.0

post,K3.4APMP.T2

Rpre,iK3.4APMP.T2

Rr

post,K3.4APMP.Tpre,K3.4APMP.T

LIPIRCMLIPIRCMdd

LIPIRCMLIPIRCM

t

WuWuTW

WW

i

ii

(9)

3

LIPIRCM SPRT,2

K3.4APMP.T2

SPRT,

iii

CuTuCu

(10)

Where

12dd

LIPIRCMLIPIRCM

r

post,K3.4APMP.Tpre,K3.4APMP.T

SPRT,TW

WWCu

ii

i

. (11)

In the cutoff criteria above, i

Wu K3.4APMP.TR LIPIRCM is the combined standard uncertainty from

all sources of random uncertainty for each SPRT, and eff,95.0 t is the appropriate quantile of the Student’s t

distribution with degrees of freedom, eff needed to compute an approximate 95 % level of confidence

for the temperature differences observed after travel to and from KRISS for each SPRT.

The expanded uncertainty in the temperature difference between the fixed-point cells of KRISS used in

the APMP.T-K3.4 and those in the CCT-K3, K3CCTK3.4APMP.T KRISSKRISS TU was evaluated

using the following equation.

K3CCT2

ucK3.4APMP.T2

uc

K3CCTK3.4APMP.T2

KRISSKRISS

KRISSKRISS

TUTU

TU (12)

Here, the subscript uc refers to the uncorrelated uncertainty components in the fixed-point resistance ratio

measurements. In this comparison, only the uncertainties due to the chemical impurity and to the

hydrostatic head correction were assumed to be correlated. This assumption was based on the fact that the

reference fixed-point cells at KRISS had been strictly restricted in use except for international

comparisons and calibrations of other fixed-point cells. Thus, contamination of the samples since the

CCT-K3 was thought to be unlikely. Therefore, as the same fixed-point cells were employed in the

APMP.T-K3.4, uncertainty components related with the physical content and the geometry of the fixed-

9

point cells were assumed to be correlated, which were the uncertainties due to the chemical impurity and

to the hydrostatic head correction.

The expanded uncertainty in the temperature difference between the fixed-point resistance ratios of

KRISS in the CCT-K3 and the ARVs of the CCT-K3 was available in the final report of the CCT-K3, and

is reproduced in Table 4.

6.2. Data analysis

Table 5 shows the results of the cutoff criteria analysis. As shown in the table, since no artifacts failed

both the criteria, the data from the two artifacts were all used in the following analysis.

Table 5. Results of the cutoff criteria analysis.

Fixed-

point

iCu ,SPRT / mK Cutoff criterion 1 value Cutoff criterion 1 result

Artifact 1 Artifact 2 Artifact 1 Artifact 2 Artifact 1 Artifact 2

Zn FP 0.26 2.4 1.9 2.0 Passed Passed

Sn FP 0.31 2.7 3.5 1.6 Passed Passed

In FP 0.028 0.30 0.39 4.8 Passed Failed

Ga MP 0.014 0.076 0.29 0.45 Passed Passed

Hg TP 0.54 0.14 1.6 1.4 Passed Passed

Fixed-

point

i

Tu K3.4APMP.TLIPIRCM

/ mK

Cutoff criterion 2 value

/ mK Cutoff criterion 2 result

Artifact 1 Artifact 2 Artifact 1 Artifact 2 Artifact 1 Artifact 2

Zn FP 4.4 6.2 1.5 1.9 Passed Failed

Sn FP 3.4 5.7 1.1 1.7 Passed Failed

In FP 3.0 3.6 1.0 1.2 Passed Passed

Ga MP 2.4 2.7 0.79 0.91 Passed Passed

Hg TP 2.2 2.3 0.70 0.75 Passed Passed

Table 6 shows the fixed-point temperature differences between RCM-LIPI and KRISS for both the

artifacts and corresponding expanded uncertainties.

Table 6. Fixed-point temperature differences between RCM-LIPI and KRISS for both the artifacts and

corresponding expanded uncertainties (95 % level of confidence and k = 2).

Temperature difference / mK

Uncertainty in the temperature difference / mK Zn FP Sn FP In FP Ga MP Hg TP

1K3.4APMP.TK3.4APMP.T KRISSLIPIRCM T -3.5 -0.8 -2.7 0.3 -1.1

1K3.4APMP.TK3.4APMP.T KRISSLIPIRCM TU 8.9 6.9 6.1 4.8 4.4

10

2K3.4APMP.TK3.4APMP.T KRISSLIPIRCM T -5 4 -2.3 -0.1 -0.4

2K3.4APMP.TK3.4APMP.T KRISSLIPIRCM TU 13 11 7.2 5.5 4.5

Table 7 and Fig. 1 show the averaged fixed-point temperature difference between RCM-LIPI and KRISS,

and the corresponding uncertainty.

Table 7. Averaged fixed-point temperature difference between RCM-LIPI and KRISS, and corresponding

expanded uncertainty (95 % level of confidence and k = 2).

Temperature difference / mK

Uncertainty in the temperature difference / mK Zn FP Sn FP In FP Ga MP Hg TP

K3.4APMP.TK3.4APMP.T KRISSLIPIRCM T -4 1.7 -2.5 0.1 -0.7

K3.4APMP.TK3.4APMP.T KRISSLIPIRCM TU 10 8.1 6.6 5.1 4.3

Fig. 1. Averaged fixed-point temperature difference between RCM-LIPI and KRISS, and corresponding

expanded uncertainty (95 % level of confidence and k = 2).

In order to complete the linkage, it was needed to evaluate the uncertainty in the temperature difference

between the fixed-point cells of KRISS used in the APMP.T-K3.4 and those in the CCT-K3,

K3CCTK3.4-APMP.T KRISSKRISS T . As noted above, since the fixed-point cells used in the APMP.T-

K3.4 were the same as those in the CCT-K3, the temperature difference did not influence the linkage, but

its uncertainty affected the linkage. The uncertainty in that temperature difference accounted for any

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uncorrelated uncertainties in the realization of the fixed-point and in the measurement of the resistance

ratio. In this comparison, only the uncertainties due to the chemical impurity and the hydrostatic head

correction were assumed to be correlated. Table 8 shows the related uncertainty components in the

APMP.T-K3.4 and in the CCT-K3.

Table 8. Uncertainty component for KRISS in the APMP.T-K3.4 and CCT-K3. Uncertainty components

correlated between the APMP.T-K3.4 and the CCT-K3 are in boldface. Expanded uncertainty was

evaluated at 95 % level of confidence and k = 2. All the uncertainties are in mK.

Uncertainty

component

Zn FP Sn FP In FP Ga MP Hg TP

CCT APM

P CCT

APM

P CCT

APM

P CCT

APM

P CCT

APM

P

Repeatability 0.19 0.051 0.15 0.029 0.060 0.039 0.060 0.056 0.060 0.008

Chemical

impurity 0.31 0.33 0.17 0.17 0.27 0.27 0.008 0.008 0.001 0.011

Hydrostatic

head 0.016 0.016 0.013 0.013 0.019 0.019 0.007 0.007 0.031 0.041

Heat flux 0.023 0.077 0.023 0.093 0.026 0.060 0.001 0.072 0.017 0.026

Gas pressure 0.017 0.017 0.012 0.013 0.017 0.019 0.006 0.008 0.023 0.021

Slope of plateau 0.12 0.026 0.058 0.077 0.12 0.088 0.029 0.040 0.029 0.049

Propagated from

TPW 0.17 0.51 0.12 0.38 0.10 0.32 0.012 0.22 0.012 0.17

Bridge

nonlinearity 0.004 0.20 0.006 0.19 0.017 0.18 0.014 0.17 0.006 0.17

Bridge

repeatability 0.017 0.015 0.017 0.014 0.017 0.014 0.017 0.014 0.017 0.013

SPRT

self-heating 0.052 0.035 0.052 0.040 0.040 0.031 0.012 0.038 0.012 0.023

Rs stability 0.005 0.012 0.003 0.008 0.003 0.007 0.002 0.005 0.017 0.003

SPRT oxidation 0.00 0.016 0.00 0.015 0.00 0.002 0.00 0.001 0.00 0.00

Total A 0.19 0.05 0.15 0.03 0.06 0.04 0.06 0.06 0.06 0.01

Total B 0.38 0.65 0.23 0.47 0.32 0.47 0.04 0.30 0.06 0.25

Total 0.85 1.31 0.55 0.95 0.65 0.96 0.15 0.64 0.17 0.51

Ucorrelated 0.62 0.65 0.35 0.34 0.54 0.54 0.02 0.02 0.06 0.09

Uuncorrelated 0.57 1.14 0.42 0.89 0.35 0.79 0.15 0.64 0.16 0.50

U{ΔT(KRISS)}† 1.3 0.99 0.87 0.66 0.52

† U{ΔT(KRISS)} designated K3CCTK3.4-APMP.T KRISSKRISS T .

Based on the above analysis and using the temperature difference between the fixed-point resistance

ratios of KRISS in the CCT-K3 and the ARVs of the CCT-K3 in Table 4, the temperature difference

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between the fixed-point resistance ratios of RCM-LIPI in the APMP.T-K3.4 and the ARVs of the CCT-K3

and its uncertainty were calculated. Table 9 and Fig 2 show the result.

Table 9. Temperature difference between the fixed-point resistance ratios of RCM-LIPI in the APMP.T-

K3.4 and the ARVs of the CCT-K3, and corresponding expanded uncertainty (95 % level of confidence

and k = 2).

Temperature difference / mK

Uncertainty in the temperature difference / mK Zn FP Sn FP In FP Ga MP Hg TP

K3-CCTK3.4APMP.T ARVLIPIRCM T -5 1.6 -0.7 0.1 -0.3

K3-CCTK3.4APMP.T ARVLIPIRCM TU 10 8.2 6.7 5.2 4.4

Fig. 2. Temperature difference between the fixed-point resistance ratios of RCM-LIPI in the APMP.T-

K3.4 and the ARVs of the CCT-K3, and corresponding expanded uncertainty (95 % level of confidence

and k = 2).

7. Bilateral differences

The bilateral differences from RCM-LIPI in the APMP.T-K3.4 to CCT-K3 participants were calculated

based on the following equations. In doing so, it was assumed that the differences between the CCT-K3

participants were uncorrelated.

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K3CCTK3CCT

K3CCTK3.4APMP.T

K3.4APMP.TK3.4APMP.T

K3CCTK3.4APMP.T

LabKRISS

KRISSKRISS

KRISSLIPIRCM

LabLIPIRCM

T

T

T

T

(13)

K3CCTK3CCT2

K3CCTK3.4APMP.T2

K3.4APMP.TK3.4APMP.T2

K3CCTK3.4APMP.T2

LabKRISS

KRISSKRISS

KRISSLIPIRCM

LabLIPIRCM

TU

TU

TU

TU

(14)

Where

K3CCTK3.4-APMP.T LabLIPI-RCM T is the fixed-point temperature difference

between RCM-LIPI in the APMP.T-K3.4 and

a participant of the CCT-K3,

K3CCTK3CCT LabKRISS T is the fixed-point temperature difference

between KRISS and a participant of the CCT-

K3,

K3CCTK3.4-APMP.T LabLIPI-RCM TU is the expanded uncertainty in the fixed-point

temperature difference between RCM-LIPI in

the APMP.T-K3.4 and a participant of the

CCT-K3,

K3CCTK3CCT LabKRISS TU is the expanded uncertainty in the fixed-point

temperature difference between KRISS and a

participant of the CCT-K3.

The bilateral differences between KRISS and participants of the CCT-K3 and the corresponding

uncertainties are reproduced in Table 10.

Table 10. Bilateral differences between KRISS and participants of the CCT-K3 and corresponding

expanded uncertainties (95 % level of confidence and k = 2).

Fixed-point

K3CCTK3CCT LabKRISS T / mK

K3CCTK3CCT LabKRISS TU / mK

BIPM BNM IMGC MSL NIM NIST NML

Zn FP ΔT

-1.0 0.3 -0.3 -1.4 -1.0 -0.4

U 1.7 1.6 5.6 1.8 1.4 1.4

Sn FP ΔT

0.0 -0.4 0.3 0.7 -0.5 0.9

U 1.4 1.1 1. 6 5.7 1.0 1.1

14

In FP ΔT

1.96 1.59 1.7 2.9 1.33 3.5

U 0.98 0.97 1.1 1.2 0.75 1.1

Ga MP ΔT 0.09 0.02 -0.09 -0.17 0.59 0.00 0.29

U 0.48 0.54 0.47 0.58 0.73 0.46 0.52

Hg TP ΔT

0.87 0.59 0.24 0.29 0.50 0.79

U 0.73 0.54 0.62 0.68 0.47 0.52

Fixed-point

K3CCTK3CCT LabKRISS T / mK

K3CCTK3CCT LabKRISS TU / mK

NPL NRC NRLM PTB SMU VNIIM VSL

Zn FP ΔT -0.9 0.1 1.5 0.2 -0.6 -1.1 -0.7

U 1.6 1.5 2.5 1.9 1.6 2.0 1.7

Sn FP ΔT -0.3 0.8 0.9 -0.7 -0.4 -0.7 -0.1

U 1.3 1.3 1.3 1.3 1.3 1.3 1.3

In FP ΔT 2.0 2.36 2.9 1.6

1.2 2.6

U 1.0 0.81 1.2 1.3 1.0 1.0

Ga MP ΔT 0.16 0.13 0.50 -0.21 -0.04 -0.01 0.22

U 0.62 0.53 0.51 0.52 0.50 0.49 0.62

Hg TP ΔT 0.40 0.28 0.85 0.56

0.46

U 0.60 0.50 0.74 0.54 0.62

Based on the above equations and the bilateral differences between KRISS and participants of the CCT-

K3, the bilateral differences between RCM-LIPI in the APMP.T-K3.4 and participants of the CCT-K3

were calculated, and the result is shown in Table 11.

Table 11. Bilateral differences between RCM-LIPI and participants of the CCT-K3 and corresponding

expanded uncertainties (95 % level of confidence and k = 2).

Fixed-point

K3CCTK3.4-APMP.T LabLIPI-RCM T / mK

K3CCTK3.4-APMP.T LabLIPI-RCM TU / mK

BIPM BNM IMGC MSL NIM NIST NML

Zn FP ΔT

-5 -4 -5 -6 -5 -5

U 10 10 12 10 10 10

Sn FP ΔT

1.7 1.3 2.0 2 1.2 2.6

U 8.3 8.2 8.3 10 8.2 8.2

In FP ΔT

-0.6 -0.9 -0.8 0.4 -1.2 1.0

U 6.7 6.7 6.8 6.8 6.7 6.8

Ga MP ΔT 0.2 0.1 0.0 -0.1 0.7 0.1 0.4

U 5.2 5.2 5.2 5.2 5.2 5.2 5.2

15

Hg TP ΔT

0.1 -0.1 -0.5 -0.4 -0.2 0.1

U 4.4 4.4 4.4 4.4 4.4 4.4

Fixed-point

K3CCTK3.4-APMP.T LabLIPI-RCM T / mK

K3CCTK3.4-APMP.T LabLIPI-RCM TU / mK

NPL NRC NRLM PTB SMU VNIIM VSL

Zn FP ΔT -5 -4 -3 -4 -5 -6 -5

U 10 10 10 10 10 10 10

Sn FP ΔT 1.5 2.5 2.6 1.0 1.3 1.0 1.6

U 8.2 8.3 8.3 8.3 8.3 8.2 8.2

In FP ΔT -0.5 -0.2 0.4 -0.9

-1.3 0.0

U 6.7 6.7 6.8 6.8 6.7 6.7

Ga MP ΔT 0.3 0.2 0.6 -0.1 0.1 0.1 0.3

U 5.2 5.2 5.2 5.2 5.2 5.2 5.2

Hg TP ΔT -0.3 -0.5 0.1 -0.2

-0.3

U 4.4 4.4 4.4 4.4 4.4

16

8. Incomplete submission

Laboratories failing to submit data for APMP.T-K3.4 report draft A:

(1) RCM-LIPI: Instrumentation list

Appendix 1: Protocol of the APMP.T-K3.4

Appendix 2: Measurement data

Appendix 3: Uncertainty of the measurement

Appendix 4: Immersion curve

Appendix 5: Instrumentation

17

Appendix 1: Protocol of the APMP.T-K3.4

Bilateral Comparison from the Hg TP to the Zn FP between KRISS and KIM-LIPI

Objective: This comparison is designed to compare the realization of the ITS-90 through the calibration

of SPRTs. The range of temperature covered in this comparison is from the triple point of Hg (234.3156 K)

to the freezing point of Zn (692.677 K). The transfer standards used will be long-stem SPRTs.

NMI Participants:

Pilot: KRISS, Wukchul Joung, wukchul.joung@kriss.re.kr

Participating lab: KIM-LIPI, Beni Adi Trisna, beni@kim.lipi.go.id

Projected Timeline:

Protocol Agreement June 30, 2011

Transfer Standards Sent to KRISS September 30, 2011

Transfer Standards Returned to KIM-LIPI December 31, 2011

Transfer Standards Re-Measured by KIM-LIPI March 31, 2012

Draft A Report Completed April 30, 2012

Participants will supply the following information:

2 ITS-90 calibrated SPRTs

o NMI participant will select their own SPRTs based on their own criteria for

suitability and will convey the selection criteria to the Pilot Laboratory

o SPRTs must be calibrated by NMI participant before measurements are made by

the pilot and then again on return from the pilot

o SPRTs are to be measured at every available fixed-point cell over the range of the

comparison including the In FP and Ga MP

Calibration results supplied in FPW with all corrections applied by the NMI such that

the FPW values are equivalent to the ITS-90 assigned temperature values for 0 mA.

Uncertainties, iSPRTFPWu , may be specific to each SPRT or a nominal uncertainty may

be given for both SPRTs. The calibration results should be based on 3 repeated

measurements at each fixed point.

18

o Appendix A gives a reporting worksheet

The measurement equation used to compute each calibration result with an indication of

which inputs vary randomly for each realized equilibrium and which inputs are systematic

across all equilibria for each fixed point within this comparison

o Any quantities in the measurement equation that are a mixture of random and

systematic effects for each SPRT should be broken into constituent parts that are

either purely random or purely systematic within this comparison.

An example of an SPRT measurement is given in Appendix B.

Uncertainty budget compliant with CCT WG3 that includes degrees of freedom associated

each component

o A suggested fixed-point cell uncertainty budget is given in Appendix C

Sources of uncertainty may be added or deleted as needed

An NMI may choose to supply their own uncertainty budget (CMC and

WG3 compliant) that includes degrees of freedom for each source of

uncertainty

Please identify which components of the uncertainty budget are associated

with random effects in FPW and which are associated with systematic

effects in FPW within this comparison.

Heat Flux (Immersion) profile for each fixed-point cell used

o [R(FP), 0 mA] and corresponding [immersion depth (sensor midpoint), cm]

Reporting the calibration results:

The participating NMIs should report FPW to the independent party within 2 weeks after completing

the measurement without informing the results to the other participating laboratory. After receiving all

results from the participating laboratories (two results from KIM-LIPI, one from KRISS), the independent

party will forward the results to the pilot laboratory. After reporting FPW to the independent party,

the participating NMI (KIM-LIPI) should send all the results and required information to KRISS

(Wukchul Joung, wukchul.joung@kriss.re.kr).

If you have questions about any aspect of the protocol or are not sure how to report something

that is requested, please contact Wukchul Joung prior to submitting your report. After reviewing a

ll submitted reports, we will contact you if there is anything that is unclear to us or if any addi

tional information is needed to complete the analysis of the data.

Method of Analysis:

19

The fixed-point realization temperature differences between KRISS and KIM-LIPI will be calculated

using the following equations:

21 SPRTLIPI,KIMSPRTLIPI,KIMLIPIKIM

2

1 TTT

where

i

ii

i SPRTr

SPRTKRISS,SPRTLIPI,KIM

SPRTLIPI,KIMdd

FPFPC

TW

WWT

.

iCSPRT is a term used to account for uncertainty associated with the travel, handling, or stability of each

SPRT and is taken to have a value of iSPRTC and a standard uncertainty,

iSPRTCu , of

12dd

FPFP

r

KRISSPre,SPRTLIPI,KIMKRISSPost,SPRTLIPI,KIM

SPRTii

iTW

WWCu

.

An SPRT cutoff criterion for use in calculating values of LIPIKIMT will be used to ensure that

uncertainty associated with the travel, handling, or stability of either SPRT does not dominate the

standard uncertainty of LIPIKIMT , LIPIKIMTu . The cutoff criterion will be based on the statistical

agreement between each SPRT’s resistance ratios before and after its travel to KRISS and the magnitude

of iSPRTCu .

The mathematical definition for the cutoff criterion will be:

usedbenotwillSPRTfromResults

3Cu

and

FPFP

ddFPFP

i

2SPRT

2LIPIKIM

SPRT

,95.02

KRISSPre,SPRTLIPI,KIMR

2

KRISSPost,SPRTLIPI,KIMR

rKRISSPre,SPRTLIPI,KIMKRISSPost,SPRTLIPI,KIM

i

i

eff

ii

ii

CuTu

t

WuWu

TWWW

In the cutoff criterion above, iSPRTLIPI,KIMR FP Wu is the combined standard uncertainty from all

sources of random uncertainty for each SPRT and eff,95.0 t is the appropriate quantile of the Student’s t

distribution with eff degrees of freedom needed to compute an approximate 95 % confidence interval

for the temperature difference observed after travel to and from KRISS for each SPRT.

20

Appendix A: Measurement Reporting Worksheet

Participating NMI

Before sending SPRTs to pilot laboratory

SPRT 1

1SPRTFPWu

, mK

Number of

equilibria

realized SPRT 2

2SPRTFPWu

, mK

Number of

equilibria

realized

ZnW

SnW

InW

GaW

HgW

Final R(TPW)

On return to participating laboratory

SPRT 1

1SPRTFPWu

, mK

Number of

equilibria

realized SPRT 2

2SPRTFPWu

, mK

Number of

equilibria

realized

ZnW

SnW

InW

GaW

HgW

Final R(TPW)

Fixed-point cell information

s/n

Immersion

depth, cm Pressure, kPa

Zn

Sn

In

Ga

Hg

Resistance ratio

bridge model

Reference resistor

model

Resistor enclosure

stability, mK

21

Measurement system

Appendix B: Example of an SPRT measurement

Tmeas.(FP) = T90(FP) + pressure correction + immersion correction

W(FP) = Wcalc.(FP) + (Tmeas. – T90) / dWr/dT

Before sending SPRTS to pilot laboratory

pressure immersion

correction, mK ucorrection, mK correction, mK ucorrection, mK

ZnW

SnW

InW

GaW

HgW

After sending SPRTS to pilot laboratory

pressure immersion

correction, mK ucorrection, mK correction, mK ucorrection, mK

ZnW

SnW

InW

GaW

HgW

22

Appendix C: Suggested Fixed-Point Cell Uncertainty Budget

Participating NMI

Type A Hg Ga In Sn Zn Systematic

or random mK df mK df mK df mK df mK df

Phase transition

realization repeatability

Total A

Type B

Chemical impurities

Hydrostatic-head

Propagated TPW

SPRT self-heating

Heat flux

Moisture

Gas pressure

Slope of plateau

Total B

Combined standard

uncertainty

Expanded uncertainty

(k = 2 level, using

effective df)

23

Appendix 2: Measurement data

Participating NMI RCM-LIPI

Before sending SPRTs to pilot laboratory

Fixed-point

Artifact 1 Artifact 2

FPR / Ω Number of

equilibria

realized

FPR / Ω Number of

equilibria

realized

TPWR / Ω TPWR / Ω

W U / mK W U / mK

Zn FP

64.279 752

2

65.279 62

2 25.028 052 25.416 74

2.568 308 9.0 2.568 37 15

Sn FP

47.364 689

2

48.100 63

2 25.028 061 25.415 82

1.892 463 6.9 1.892 55 15

In FP

40.284 459

2

40.910 975

2 25.028 078 25.416 700

1.609 571 6.1 1.609 610 8.4

Ga MP

27.983 714

2

28.418 421

2 25.028 009 25.416 696

1.118 096 5.0 1.118 100 6.5

Hg TP

21.128 53

2

21.456 38

2 25.028 26 25.416 70

0.844 187 4.7 0.844 184 5.1

Final R(TPW) 25.028 026 Ω 25.416 707 Ω

24

On return to participating laboratory

Fixed-point

Artifact 1 Artifact 2

FPR / Ω Number of

equilibria

realized

FPR / Ω Number of

equilibria

realized

TPWR / Ω TPWR / Ω

W U / mK W U / mK

Zn FP

64.279 978

3

65.280 974

3 25.028 109 25.416 977

2.568 311 8.7 2.568 400 8.7

Sn FP

47.364 684

3

48.101 928

3 25.028 109 25.416 973

1.892 460 6.8 1.892 512 6.7

In FP

40.284 531

3

40.911 309

3 25.028 129 25.416 969

1.609 570 5.9 1.609 606 5.9

Ga MP

27.983 830

3

28.418 794

3 25.028 117 25.417 007

1.118 096 4.6 1.118 102 4.8

Hg TP

21.128 59

3

21.456 59

3 25.028 12 25.417 02

0.844 194 4.0 0.844 182 4.2

Final R(TPW) 25.028 161 Ω 25.417 043 Ω

25

Participating NMI KRISS

Fixed-point

Artifact 1 Artifact 2

FPR / Ω Number of

equilibria

realized

FPR / Ω Number of

equilibria

realized

TPWR / Ω TPWR / Ω

W U / mK W U / mK

Zn FP

64.279 461

3

65.280 794

3 25.027 803 25.416 867

2.568 322 1.3 2.568 404 1.3

Sn FP

47.364 179 2

3

48.101 748 0

3 25.027 775 1 25.416 857 6

1.892 464 6 0.96 1.892 513 6 0.97

In FP

40.284 597 4

3

40.911 498 7

3 25.028 009 3 25.416 915 8

1.609 580 6 0.99 1.609 617 0 0.95

Ga MP

27.983 409 9

3

28.418 615 0

3 25.027 763 4 25.416 851 2

1.118 094 7 0.75 1.118 101 3 0.62

Hg TP

21.128 514

3

21.456 577

3 25.028 010 25.416 921

0.844 194 7 0.51 0.844 184 7 0.41

Final R(TPW) 25.028 018 Ω 25.416 922 Ω

26

Appendix 3: Uncertainty of the measurement

Participating NMI RCM-LIPI

Type A Hg TP TPW Ga MP In FP Sn FP Zn FP Systematic

or random

Phase transition

realization repeatability 0.082 0.48 0.14 0.035 1.5 1.1 random

Total A 0.082 0.48 0.14 0.035 1.5 1.1

Type B

Chemical impurities 0.062 0.030 0.008 0.081 0.034 0.068 systematic

Hydrostatic-head 0.002 0.00 0.00 0.001 0.001 0.001 systematic

Heat flux 0.052 0.066 0.10 0.069 0.058 0.082 systematic

Gas pressure 0.001 0.001 0.001 0.001 0.00 0.001 systematic

Slope of plateau 0.024 0.00 0.38 0.052 0.077 0.14 systematic

Propagated from TPW 1.5 - 2.0 2.9 3.4 4.5 systematic

Isotopic variation - 0.002 - - - - systematic

Bridge nonlinearity 1.5 1.5 1.5 1.6 1.6 1.7 systematic

Bridge repeatability 0.11 0.11 0.11 0.12 0.12 0.13 random

SPRT self-heating 0.023 0.025 0.026 0.032 0.032 0.033 systematic

Rs stability 0.007 0.008 0.009 0.014 0.016 0.024 systematic

SPRT oxidation 0.00 0.00 0.00 0.00 0.00 0.00 systematic

Total B 2.1 1.5 2.5 3.3 3.7 4.9

Combined standard

uncertainty / mK 2.1 1.6 2.5 3.3 4.0 5.0

Expanded uncertainty

/ mK

(95 % level of

confidence, k = 2)

4.3 3.2 5.1 6.5 8.0 10

27

Participating NMI KRISS

Type A Hg TP TPW Ga MP In FP Sn FP Zn FP Systematic

or random

Phase transition

realization repeatability 0.008 0.022 0.056 0.039 0.029 0.051 random

Total A 0.008 0.022 0.056 0.039 0.029 0.051

Type B

Chemical impurities 0.011 0.030 0.008 0.27 0.17 0.33 systematic

Hydrostatic-head 0.041 0.004 0.007 0.019 0.013 0.016 systematic

Heat flux 0.026 0.085 0.072 0.060 0.093 0.077 systematic

Gas pressure 0.021 0.006 0.008 0.019 0.013 0.017 systematic

Slope of plateau 0.049 0.00 0.040 0.088 0.077 0.026 systematic

Propagated from TPW 0.17 - 0.22 0.32 0.38 0.51 systematic

Isotopic variation - 0.014 - - - - systematic

Bridge nonlinearity 0.17 0.17 0.17 0.18 0.19 0.20 systematic

Bridge repeatability 0.013 0.013 0.014 0.014 0.014 0.015 random

SPRT self-heating 0.023 0.025 0.038 0.031 0.040 0.035 systematic

Rs stability 0.003 0.004 0.005 0.007 0.008 0.012 systematic

SPRT oxidation 0.00 0.00 0.001 0.002 0.015 0.016 systematic

Total B 0.25 0.20 0.30 0.47 0.47 0.65

Combined standard

uncertainty / mK 0.25 0.20 0.30 0.47 0.47 0.65

Expanded uncertainty

/ mK

(95 % level of

confidence, k = 2)

0.51 0.41 0.64 0.96 0.95 1.3

28

Appendix 4: Immersion curve

Appendix 4.1: Zn FP

29

Appendix 4.2: Sn FP

30

Appendix 4.3: In FP

31

Appendix 4.4: Ga MP

32

Appendix 4.5: Hg TP

33

Appendix 5: Instrumentation

Appendix 5.1: Resistance measuring device

Laboratory RCM-LIPI KRISS

Bridge manufacturer MI ASL

AC/DC DC, 6010C AC, F900

If AC, give

Frequency 30 Hz

Bandwidth 0.1 Hz

Gain 104

Quad gain 10

Output IEEE-488

Normal measuring current 1 mA

Self-heating current 1.414 mA

Unity reading 1.000 000 032

Zero reading 0.000 000 000

Compliment check error 9.45 × 10-9

If DC, give

Gain

Period of reversal 4 s

Output IEEE-488

Reference resistor

Type DC, standard resistor 10 Ω AC/DC

Manufacturer Tinsley Tinsley

Temperature 23 °C 25 °C

Temperature coefficient 1.0 × 10-6

/ °C 1.25 × 10-6

/ °C

Linearity of bridge 2.72 × 10-6

7.74 × 10-8

34

Appendix 5.2: Triple point of water cell

Laboratory RCM-LIPI KRISS

Cell manufacturer PTB KRISS

Water source and purity Distilled deionized water

Well diameter 15 mm 11 mm

Immersion depth 260 mm 260 mm

Heat transfer liquid: water? Alcohol Water

Cell maintained in: ice bath/water bath? Water bath mixed with

alcohol Ice bath

Ice mantle:

Method of preparation Dry ice Dry ice

Annealing time before use 1 week 2 weeks

35

Appendix 5.3: Other fixed-point cell

Laboratory RCM-LIPI

Fixed-point Zn FP Sn FP In FP Ga MP Hg TP

Cell

Cell manufacturer Hart

Scientific

Hart

Scientific

Hart

Scientific Hart Scientific

Open/closed? Open Open Open Closed Closed

Pressure in cell 101.3 kPa 101.3 kPa 101.3 kPa MP TP

Crucible

Crucible material

Graphite Graphite Graphite PTFE

Austenitic

Stainless

Steel

Crucible manufacturer Hart

Scientific

Hart

Scientific

Hart

Scientific Hart Scientific

Hart

Scientific

Crucible length 250 mm 250 mm 250 mm 168 mm 213 mm

Metal sample

Sample source Hart

Scientific

Hart

Scientific

Hart

Scientific Hart Scientific

Hart

Scientific

Sample purity 99.9999 % 99.9999 % 99.9999 % 99.99999 % 99.99999 %

Sample weight 1 kg 1 kg 1 kg

Thermometer well

Well material

Graphite Graphite Graphite PTFE

Austenitic

Stainless

Steel

Well ID (mm) 8 mm 8 mm 8 mm 7 mm 7 mm

Immersion depth of

SPRT 170 mm 170 mm 170 mm 143 mm 188 mm

Furnace/Bath Furnace Furnace Furnace Furnace Bath

Manufacturer Hart

Scientific

Hart

Scientific

Hart

Scientific Hart Scientific

Hart

Scientific

Control type PID PID PID PID PID

How many zones? 3 Zone 3 Zone 3 Zone

Furnace heater

AC/DC? AC AC AC

Thermoelectric

Heater AC

Heat pipe liner? No No No

ITS-90 realization

Freeze/melt? Freeze Freeze Freeze Melt Melt

Technique Induced

Freeze

Induced

Freeze

Induced

Freeze Heater

Induced

melt

Heat transfer fluid Air Air Air Air Halocarbon

Duration of freeze/melt 16 hours 16 hours 6 hours 120 hours 18 hours

Cell used as FP/MP/TP? FP FP FP MP TP

36

Laboratory KRISS

Fixed-point Zn FP Sn FP In FP Ga MP Hg TP

Cell

Cell manufacturer KRISS KRISS KRISS KRISS Isotech

Open/closed? Open Open Closed Open Closed

Pressure in cell 101 325 Pa 101 325 Pa 101 325 Pa 101 325 Pa TP

Crucible

Crucible material Graphite Graphite Pyrex Teflon Stainless

steel

Crucible manufacturer Ultra carbon Ultra carbon NA NA Isotech

Crucible length 255 mm 255 mm 180 mm 310 mm 230 mm

Metal sample

Sample source Johnson

Matthey

Johnson

Matthey

Johnson

Matthey

Rhone-

Poulenc Unknown

Sample purity 99.9999 % 99.9999 % 99.9999 % 99.99999 % 99.99999 %

Sample weight 1.0 kg 1.0 kg 0.7 kg 0.8 kg 3.0 kg

Thermometer well

Well material Graphite Graphite Pyrex Teflon Stainless

Steel

Well ID 11 mm 11 mm 10 mm 12 mm 9.5 mm

Immersion depth of SPRT 140 mm 140 mm 115 mm 180 mm 155 mm

Furnace/Bath Furnace Furnace Furnace Bath Refrigerator

Manufacturer Isotech Isotech Isotech Hart Isotech

Control type PID PID PID PID PID

How many zones? 3 3 3 NA NA

Furnace heater

AC/DC? AC AC AC NA NA

Heat pipe liner? No No No NA NA

ITS-90 realization

Freeze/melt? Freeze Freeze Freeze Melt Melt

Technique Induced

freeze

Outside

nucleation,

induced

freeze

Induced

freeze Heater

Induced

melt

Heat transfer fluid Air Air Air Water Ethanol

Duration of freeze/melt 15 hours 8 hours 20 hours 50 hours 15 hours

Cell used as FP/MP/TP? FP FP FP MP TP

37