Post on 27-Feb-2020
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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-
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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