Int J Thermophys (2011) 32:361371

DOI 10.1007/s10765-011-0944-8

Calibration of Radiation Thermometry Fixed Points

Using Au/Pt Thermocouples

F. Jahan M. J. Ballico

Received: 6 April 2010 / Accepted: 3 February 2011 / Published online: 2 March 2011
Springer Science+Business Media, LLC 2011

Abstract At NMIA, radiation thermometers are calibrated by comparison with a

number of reference radiation thermometers which are themselves calibrated using
fixed-point cells on the ITS-90 temperature scale (In, Sn, Zn, Al, Ag, and Au). The
suitability of NMIA fixed-point cells used for standard platinum resistance thermom-
eters (SPRTs) is evaluated by the comparison of ensembles of cells at each fixed point,
and by participation in the international BIPM Key-Comparisons K3 and K4. How-
ever, the NMIA fixed-point cells used for radiation thermometry are typically much
smaller (only 110 mm in length) and the thermowell length immersed in the metal much
shorter (85 mm) than those used for SPRTs. Further, the insulation at the front of the
crucible needs to accommodate the F/10 viewing cone of the radiation thermometers,
so significant temperature gradients exist near the top of the crucible. As a conse-
quence, the conduction errors obtained using SPRTs are too large to be of practical
use. A convenient methodology based on the use of a Au/Pt thermocouple, together
with a protective tube assembly to reduce conduction errors, has been developed. This
allows the convenient measurement of the phase transition temperature traceable, at
the 30 mK level, to the fixed-point cells used at NMIA to realize and maintain the
ITS-90 scale. As the measurements are made in situ, the temperature environment,
and hence the geometry and formation of the liquidsolid interface during melting and
freezing, are similar to that occurring when used with radiation thermometers. Results
are presented for ITS-90 fixed points up to Ag, establishing formal traceability of
radiation thermometry fixed-point cells to NMIAs primary ITS-90 cells.

Keywords Au/Pt thermocouples Conduction error Fixed point Meltfreeze

F. Jahan (B) M. J. Ballico

National Measurement Institute of Australia, Lindfield, Australia
e-mail: Ferdouse.Jahan@measurement.gov.au

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1 Introduction

Traditionally, the fixed-point cells used to define the ITS-90 temperature scale were
regarded as primary reference standards, as long as material of sufficient purity was
used in their construction and the quality of the phase-transition plateaus was suffi-
ciently good. The typical calibration uncertainty for NMIAs primary radiation ther-
mometers is at the 0.1 C level, so uncertainties in the primary fixed points at the
50 mK level are adequate. As metal at the 1 ppm impurity level is readily available
for constructing fixed points, and this corresponds to uncertainties at the <1 mK level,
issues of source material purity may be neglected. However, fixed points for radiation
thermometry differ from those used to realize the ITS-90 using SPRTs in several ways,
giving rise to a number of furnace-effects as follows.
(i) The graphite well is usually much shorter than those used for SPRTs. In the
latter, the well must typically be immersed 170 mm to 220 mm into the metal, to
reduce conduction errors in the SPRT to a sufficiently small level. However, for
pyrometry fixed points, a depth of less than 100 mm can achieve a suitably high
cavity emissivity, and longer cavities lead to viewing an increasing proportion
of the cavity wall (due to the finite F-number of the pyrometer). A consequence
is that during melting/freezing, when the outer surface of the crucible is a few
degrees hotter/colder than the liquidsolid interface, a larger fraction of this
temperature difference may be conducted to the cavity base.
(ii) The crucible is usually mounted horizontally in a furnace rather than vertically,
and as a consequence, the heat transfer to the melting or freezing metal is far
from cylindrically symmetric. For example, the crucible has much better ther-
mal contact with the furnace on its underside. Consequently, the liquidsolid
interface may not properly surround the blackbody cavity.
(iii) The low F-number of the radiation thermometers used to view the blackbody
cavity does not allow the crucible to be placed deeply inside a long furnace.
Consequently, the axial temperature gradients are generally much larger, and
the liquidsolid interface often advances axially rather than radially as for SPRT
fixed points.
(iv) Unlike fixed points for SPRT use, no additional inner nucleation is performed
to provide a second solidliquid interface, over the inner well. Consequently,
any breaks in the solidliquid interface surrounding the thermowell will provide
a heat leakage from the well to the furnace.
At present, any systematic errors arising from furnace-effect factors are assessed in
two ways: (a) first, the use of redundant fixed points (e.g., fitting the SakumaHattori
interpolation equation [1] using Zn, Al, and Au points and checking the measured
temperature at the Ag point) and (b) secondly, examination of the meltfreeze dif-
ferences and the flatness of the freeze plateau. Our experience is that the uncertainty
we assign to the radiation thermometry fixed points is dominated by the measured
meltfreeze differences and plateau flatness. However, as part of ongoing work to
improve the quality assurance of NMIAs calibration services, we wish to develop a
formal traceability of radiation thermometry fixed points to NMIA primary standards
validated by participation in a CIPM key comparison. This would confirm that the

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uncertainty estimate based on the observed meltfreeze behavior adequately covers

the systematic errors arising from furnace effects. In the region above 960 C, the
key-comparison K5 provides assurance for the Au points that NMIA uses to real-
ize ITS-90. In the region up to 960 C, however, the key-comparisons K3 and K4
considered only the large fixed points used for SPRT calibration. We sought a meth-
odology to calibrate the fixed-point cells together with furnace assemblies used in
our Radiation Thermometry Laboratory. Initial experiments using SPRTs to calibrate
radiation-thermometry fixed points quickly determined that although SPRTs can be
used to measure the temperature at the mK level, the conduction errors when used in
the short cells led to large uncertainties. We therefore attempted to use Au/Pt ther-
mocouples, which, although only able to achieve 30 mK level uncertainties, offered
significantly smaller conduction errors. This approach has allowed NMI to formally
connect the radiation-thermometry fixed points to key comparisons, and to validate
the uncertainty estimates based on the measured meltfreeze behavior.

2 Experimental Details

The NMIA radiation-thermometry fixed-point cells [2,3] are graphite crucibles 95 mm

in length and 43 mm in diameter, containing about 47 cm3 metal. Figure 1 shows a
schematic diagram of a crucible. A re-entrant graphite well 85 mm in length forms the
blackbody cavity. The Al and Ag cell wells have an 8 mm ID, as they are used with
visible or near-IR radiation thermometers with small size-of-source effects (SSE),
whereas the Sn and Zn cells, which are used with longer wavelength pyrometers with
poorer SSE, have 14 mm ID wells. They are held in 50 mm ID Pyrex tubes (for In,
Sn, and Zn) or fused quartz tubes (for Al and Ag), with a series of graphite rings with
increasing internal diameter from the crucible to the end of the tube to give a clear
viewing path for the viewing system of the radiation thermometers. The In and Sn
cells are held in a closed-end Hg heatpipe furnace liner, the Zn cell in a closed-end Cs
heatpipe, and the Al and Ag cells in a Na heatpipe liner open at both the front and the
rear. All the furnaces are mounted horizontally. The front of the crucible is approx-
imately 100 mm from the front of the furnace liner. During meltfreeze realization,
the assembly is filled with high-purity argon (Ar) and held at a slight overpressure
of Ar gas when not being viewed by the radiation thermometers. Freezes and melts
generally have a duration of (1 to 2) h when the furnace temperature is held at 3 C to
5 C above or below the nominal metal freezing point. No additional inner nucleation
is used, although some of the fixed points require a gentle shake to initiate nucleation.
Three NMIA-design Au/Pt thermocouples were used to measure the temperature of
the radiation-thermometry fixed points. They consist of 0.5 mm diameter high-purity
Au and Pt wires in a 4.75 mm diameter high-purity recrystallized alumina twin-bore
insulator. Further construction details are given in [4,5]. One advantage of this design
is that it can be used in vertical as well as horizontal furnaces, as it does not use a
fragile expansion coil. This design is also insensitive to mechanical and thermal shock
[4] and can be put directly into the Ag-point furnace at 960 C, unlike an SPRT, which
needs to be pre-heated gradually from 440 C to 960 C, before use at the Ag point.
The Au/Pt thermocouples were calibrated [6] using NMIA ITS-90 fixed points: ice

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Fig. 1 Schematic diagram

of a radiation-thermometry
fixed-point crucible

85 mm

43 mm

30 mm
95 mm

point, Ga, Sn, Zn, Al, and Ag. A 7 mm OD sealed-end quartz tube is used to sepa-
rate the thermocouple from the fixed-point cells and prevent cross contamination. The
reference junction was immersed 180 mm into a crushed ice slurry in a 30 cm deep
Dewar. Electrical measurements were performed using an HP34420A nanovoltmeter.
The series of graphite rings of increasing diameter placed at the front of the cruci-
ble for radiation thermometry provide very poor thermal contact (a 10 mm to 15 mm
air gap) between the furnace tube and the thermocouple, and inadequate immersion
could be achieved with this arrangement. Instead, several thin carbon disks separated
by 10 mm long quartz tube spacers were used in the region from the front of the
crucible to the front of the furnace. This significantly increased the thermal contact

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from the furnace to the guide tube, without significant disruption to the temperature
environment near the crucible. This is supported by the observation that the furnace
set points are unchanged, and the melt- and freeze-plateaus have the same duration.
A 3 mm thick carbon sleeve was used in the Sn and Zn cells to improve the thermal
contact between the 7 mm quartz thermocouple tube and the 14 mm blackbody cavity.

3 Results and Discussion

For each of the NMIAs radiation thermometry fixed-point cells, several calibrated
Au/Pt thermocouples were used to realize several meltfreeze plateaus. Typical results
in each of the fixed point cells are shown in Figs. 2, 3, 4, 5, and 6. The average results
for each thermocouple are presented in Table 1 and compared to the values obtained in
NMIAs reference cells (only freeze values are considered). There is excellent agree-
ment between the cell temperature difference results obtained by the two (three for
Al) thermocouples.
While the measured values of the freezing plateaus of the radiation thermometry
cells adequately serve the purpose of providing formal traceability of these cells to
the NMIA reference cells, a more detailed examination of the curves provided some
important additional information about the freezing and melting processes.
When the radiation thermometry Zn cell is used to calibrate radiation thermometers,
a meltfreeze difference of about 20 mK is observed, and prior to this measurement, it

4952
4945
0.12 C
30 mK
1 cm out
4950 4944

4943

4948
EMF , V

4942
0 15 30 45 60

4946

Reference Zn cell
4944

4942
0 50 100 150 200 250 300
Time , min
Fig. 2 Freezing plateau of a radiation-thermometry Zn point realized by Au/Pt thermocouple. A conduction
error test is shown in the inset. The EMF value obtained in the reference Zn cell is also shown

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2.569

60 mK
full immersion

2.568

Reference Zn cell
Resistance ratio

2.567
10 mm out

20 mm out

30 mm out
2.566

2.565
60 80 100 120 140
Time , min
Fig. 3 Freezing plateau of a radiation thermometry Zn point realized by an SPRT, showing a conduction
error test. The resistance ratio obtained in the reference Zn cell is also shown

was unclear how much systematic error in the actual Zn-point temperature this implied.
The Au/Pt thermocouple data in Fig. 2 also show a meltfreeze difference (0.1 C),
although larger than that obtained with radiation thermometry. The conduction-error
test, in which the thermocouple is withdrawn by 10 mm, shows a change of only about
15 mK, confirming that the meltfreeze difference is a real effect. The thermocou-
ple data show that the actual cell temperature is within the range of the meltfreeze
data, confirming that this effect arises from the conduction effects within the cell, and
that the meltfreeze range provides a good estimate of the associated uncertainty. For
comparison, a freezing plateau of the same Zn cell realized by an SPRT in this same
assembly is shown in Fig. 3. With the SPRT withdrawn by 20 mm, the conduction
errors are significant, about 0.12 C, consistent with the measured freeze value at full
immersion being apparently 60 mK lower than the reference cell; as expected, the
40 mm long SPRT sensor is more sensitive to conduction from the furnace.
The thermocouple results obtained using the Sn cell (Fig. 4) show a nearly 0.1 C
difference between the melt and the freeze curves, and indicate that both the melt
and the freeze are biased towards the furnace temperature outside the cell (the melt is
higher and the freeze is lower). When the cell is viewed by a radiation thermom-
eter a similar, but slightly smaller difference of 40 mK to 70 mK is observed. These
thermocouple results support the use of the meltfreeze difference as an uncertainty
estimate.

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2242

2240

150 mK
2238
EMF , V

2236
Reference Sn cell

2234
1 cm out

2232

2230
0 50 100 150 200 250 300 350
Time, min
Fig. 4 Typical meltfreeze curve of a radiation-thermometry Sn point realized by a Au/Pt thermocouple.
The EMF value obtained in the reference cell is also shown

Measurements using the Au/Pt thermocouple in the Al and Ag cells (Figs. 5, 6)

show much smaller conduction errors (4 mK and 10 mK, respectively) than the results
obtained for the Sn and Zn cells, attributable to the smaller diameter thermowells in
these cells. The measured meltfreeze differences for the Al and Ag cells are also much
smaller than for the Sn and Zn cells, indicating smaller furnace effects. This is also
observed when the cells are used for radiation thermometry, where meltfreeze differ-
ences of about 10 mK are observed. Nonetheless, the measured meltfreeze difference
can be used to give a good estimate of the error in the actual plateau temperature.
Table 2 gives typical values of the uncertainty components in the measurement of
temperature differences between the cells. The dominant contributions to the uncer-
tainty arise from the calibration uncertainty of the Au/Pt thermocouple and from the
conduction errors in the use of the thermocouple to measure the radiation thermometry
cells. The thermocouple calibration uncertainty [6] is mainly due to the measured inho-
mogeneity of the thermocouple wires (Fig. 7). At NMIA, thermocouple inhomogeneity
is measured [7] for every thermocouple and included in its calibration uncertainty. It
is important that this effect be properly considered, as the immersion depths in the
ITS-90 reference cell furnaces are much deeper than in the radiation thermometry
furnaces. Consequently, a different region of the thermocouple wire generates the
thermoelectric signal in each cell. As it is already included in the calibration uncer-
tainty of the thermocouple, it is not necessary to add this component again in Table 2.
The other significant uncertainty contribution, the conduction error, is experimentally

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9323

50 mK
9322

9321
EMF , V

9320

Reference Al cell 1 cm out

9319

9318

9317
0 50 100 150 200 280 300 320
Time , min
Fig. 5 Typical meltfreeze curve of radiation thermometry Al point realized by a Au/Pt thermocouple
showing a conduction error test. The EMF value obtained in the reference Al cell is shown

determined for each cell by withdrawing the thermocouple by 10 mm, and noting the
change in the measured EMF. For these thermocouples we have determined [8] that
the conduction error roughly doubles for each 8 mm to 10 mm of immersion in a close
fitting tube, so we use this value as the uncertainty contribution for this term. The
conduction error in the Sn and Zn cells is significantly higher than for the Al and Ag
cells, and this is attributed to the larger well diameter for these cells, and the poorer
radiative heat transfer at low temperatures.
Other minor contributions to the uncertainty arise from: the choice of position on
the freezing plateau, which we take as the width of the central half of the freezing
plateau; the estimated 5 mK uncertainty in the crushed-ice-point reference junction;
the reproducibility of the plateau between realizations; and the calibration and drift of
the 34420A nanovoltmeter used to measure the thermocouple EMF.
Considering the estimated measurement uncertainties, the measured temperatures
of the freezing plateaus of the radiation thermometry cells can be considered to be
consistent with those of the NMIA reference cells [9].

4 Conclusions

We have demonstrated that the temperatures realized by the small fixed-point cell
assemblies used for radiation thermometry can be measured traceably to ITS-90 fixed

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16121.5

20 mK
16121.0

16120.5

Reference Ag cell
EMF , V

16120.0

16119.5
1 cm withdrawn

16119.0

16118.5
0 30 60 90 120 150
Time , min
Fig. 6 Typical meltfreeze curve of radiation thermometry Ag point realized by a Au/Pt thermocouple
shows conduction error test during freeze. The EMF value obtained in the reference Ag cell is also shown

Table 1 Summary of the average EMF for several Au/Pt thermocouples in the freezing plateaus of the
NMIA reference ITS-90 fixed points and the radiation thermometry fixed points

Reference cell Radiation TC serial Average EMF (V) measured TDUT TITS90
thermometry cell number at the fixed points (mK)

NMI Radiation
reference thermometry
cell cell

Ag2006/1 Ag/P2 PtAu-0805 16119.80 16120.02 +8 31

PtAu-0203 16120.20 16119.96 10 31
Al2006/2 Al/85 PtAu-0804 9320.20 9320.04 8 23
PtAu-0805 9319.96 9320.03 +3 23
PtAu-0203 9320.12 9319.98 7 23
Zn02/02 Zn/95 PtAu-0804 4945.48 4944.99 30 29
PtAu-0805 4945.18 4944.72 31 29
Sn95/1 Sn/95 PtAu-0801 2235.64 2235.11 41 52
PtAu-0203 2235.90 2235.14 57 52
The difference and its associated expanded (k = 2) uncertainty are also given

points using simple and robust Au/Pt thermocouples. The method allows the in situ
measurement of the meltfreeze plateaus of the radiation thermometry fixed-point
cells, using the same furnaces with which they are normally used. The uncertainty

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-0.2

-0.4
16 mK
-0.6

-0.8
E , V

-1.0

-1.2

-1.4
TC:PtAu-0805
-1.6 TC:PtAu-0203
TC:PtAu-0804

-1.8
100 200 300 400 500 600
Immersion , mm
Fig. 7 Thermoelectric scans of three Au/Pt thermocouples at 200 C indicating their level of homogeneity

Table 2 Typical values of the uncertainty components for the calibration of radiation thermometry fixed
points using an Au/Pt thermocouple

Components Standard uncertainties, u i (V)

Ag Al Zn Sn

Uncertainty of AuPt TC 0.320 0.184 0.117 0.089

Plateau determination 0.10 0.10 0.10 0.15
Conduction error 0.130 0.05 0.15 0.25
Reference junction temperature 0.062 0.05 0.041 0.031
Reproducibility 0.05 0.03 0.08 0.1
Calibration of DVM 0.05 0.05 0.05 0.05
Drift/use of DVM 0.096 0.056 0.028 0.013
Combined uncertainty, u c 0.385 0.237 0.241 0.327
Expanded uncertainty, U95 (k = 2) 0.78 0.47 0.474 0.643
U95 in mK 31 23 29 52

achieved, typically 30 mK, is sufficiently low to allow confirmation that meltfreeze

differences provide a reasonable estimate of the errors due to furnace effects for these
cells; however, conduction errors remain the limiting factor for measurement of the
large aperture low-temperature radiation thermometry cells.

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Acknowledgment We would like to acknowledge Mr. Steve Meszaros for constructing the parts of the
assembly and general assistance during measurement.

References

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5. F. Jahan, M.J. Ballico, in Proceedings of 6th Biennial Conference of MSA (Metrology Society of Aus-
tralia, Canberra, 2005), pp. 4853
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