Stabilization of SPRTs for ITS-90 Calibration

Speaker: Dennis B. Minor

National Institute of Standards and Technology
100 Bureau Dr., MS 8363
Gaithersburg, MD 20899
Phone: 301 975 4821; Fax: 301 548 0206
Email: dennis.minor@nist.gov
Authors: Dennis B. Minor and Gregory F. Strouse
National Institute of Standards and Technology
Abstract
At the National Institute of Standards and Technology (NIST), the ITS-90 calibration of standard
platinum resistance thermometers (SPRTs) is performed in the Platinum Resistance
Thermometer Calibration Laboratory over the temperature range from 189 C to 962 C. As
part of the quality system internal measurement assurance program, the stabilization of the SPRT
prior to calibration is used to determine when and if the thermometer is stable enough to be
calibrated within the NIST-assigned ITS-90 realization uncertainties. To qualify for calibration,
the resistance of the SPRT at the triple point of water, R(TPW), must repeat after a stabilization
cycle to within the equivalent of 0.2 mK within five stabilization cycles. The annealing
procedure depends on the calibration temperature range and the amount of change at the TPW
between the as received value and the previous NIST value. The stabilization techniques used
and the impact on the overall stability of the SPRT during a calibration are given.
1. Introduction
The stability of an SPRT is dependent on both the mechanical and thermal shock that the
platinum sensor undergoes during normal use, shipping, and accidents. Stress may also be due to
mechanical constraints introduced during the fabrication process or by re-crystallization of the
platinum wire when the SPRT is heated. Lattice-vacancy site defects will also contribute to the
total stress budget of the SPRT resulting in increasing resistance over time. Such changes cause
cumulative stress in platinum sensor which is seen both as a change in R(TPW) and of the
resistance-temperature relation of the SPRT. Eventually the accumulated stress will cause the
uncertainty in the use of the thermometer to exceed the allowable value. In addition, the
thermometer will become unstable during use above 400 C because of in situ annealing.
There are three distinct types of SPRTs: i) capsule SPRTs, which are not annealed at NIST, ii)
long-stem SPRTs, designed for use to either 500 C or to 660 C, and iii) high-temperature
SPRTs (HTSPRTs), long-stem SPRTs designed for use above 660 C. In this paper, we refer to
all types of SPRTs as SPRTs, except in Section 2.2.
As an integral part of the internal measurement assurance program (IMAP) at the National
Institute of Standards and Technology (NIST), the stabilization protocol of an SPRT is
2005 NCSL International Workshop and Symposium

performed prior to calibration in the range of 189C to 962C to determine if the SPRT meets
the stability requirements to be calibrated within the realization uncertainties assigned by NIST
[1, 2]. Depending on the sub-ranges of ITS-90 used for the calibration, the SPRT will undergo a
different annealing procedure. Proper stabilization of the SPRT is determined by the change in
the calculated 0 mA R(TPW), where R is the measured resistance in ohms at the TPW, measured
after each annealing cycle. After acceptance for calibration, additional stability requirements
must be achieved during calibration for certification as a NIST calibrated ITS-90 defining
standard [2]. If at anytime during the stabilization or calibration cycle the SPRT does not meet
the NIST requirements, it is returned to the customer without calibration values. NIST does not
increase the calibration uncertainty to calibrate SPRTs that cannot meet the 0.2 mK specification.
2. SPRT Stabilization
The NIST Platinum Resistance Thermometer Calibration Laboratory (PRTCL) annealing
procedures are designed to stabilize the SPRT by reducing the accumulated stress in the platinum
sensor such that the R(TPW) measurements (before and after an anneal) are less than the
equivalent of 0.2 mK, for R extrapolated to 0 mA (zero power). If the SPRT cannot achieve this
requirement within five annealing cycles it is rejected for calibration and returned to the
customer. These annealing procedures are not designed to return the SPRT to some past or the
original equipment manufacturer (OEM) resistance value, but rather a stable baseline in order
that the calibration process will meet established NIST calibration uncertainties. Figure 1 gives
an example of the change in the 0 mA R(TPW) value over an eight year period for an SPRT
meeting the 0.2 mK stability criteria prior to each calibration.
25.560

R (TPW),

25.559

25.558
10 mK
25.557

25.556

25.555
10

Years Before Present

Figure 1. An example of the change over eight years of an SPRT R(TPW) after stabilization, but
before calibration.
2005 NCSL International Workshop and Symposium

Some typical reasons of thermometer non-compliance with the R(TPW) 0.2 mK stability
requirement are leakage at the hermetic seal, sheath damage, lack of sufficient oxygen in a
metal-sheathed SPRT, sensor damage, moisture in the sheath, or excessive thermal shock.
Figure 2 shows the 0 mA R(TPW) value for an SPRT that does not meet the R(TPW) 0.2 mK
requirement. This non-compliance is probably due to lack of sufficient oxygen in the sheath.

R (TPW), mK

15

10

0
0

10

20

Number of 475 C anneal cycles

Figure 2. An example of an SPRT that does not meet the R(TPW) 0.2 mK stability requirement.
The dashed line is at 0.2 mK.
For every SPRT type and ITS-90 calibration range there are two additional calibration stability
requirements that are used to determine if the thermometer is sufficiently stable during the
calibration. One, the SPRT is measured at the TPW after every measurement at another fixed
point. If the R(TPW) is more that 0.3 mK (before and after any other fixed-point measurement)
the SPRT is either re-stabilized or rejected after the second calibration attempt. Two, if the
R(TPW) changes by more than 0.75 mK during the entire calibration process then the SPRT is
either re-stabilized or rejected after the second calibration attempt.
2.1 Pre-calibration inspection
As the SPRT is extremely susceptible to mechanical shock, it is carefully inspected for physical
damage to the sheath, head, or signal wires; discoloration (HTSPRT fused silica sheaths only);
2005 NCSL International Workshop and Symposium

devitrification [fused silica sheathed SPRT]; alignment of the sensor windings [glass-sheathed
SPRT]; and sufficient insulation resistance (metal-sheathed SPRTs only) when it arrives at
NIST. After visual inspection, R(TPW) is measured using a 9.5 digit ac resistance ratio bridge
with two excitation currents for extrapolation to 0 mA. Details of the PRTCL measurements
systems are found in references [2-5]. As many thermometers are returned for calibration at
NIST over many years, a database was developed to track the calibration history of each SPRT.
This database is used internally to monitor any change in the R(TPW) as well as changes in the
fixed-point resistance ratios [W(T90)=R(T90)/R(TPW)] of each SPRT over time. An excerpt
database example of one SPRT is given in Table 1 giving the year and batch of calibration, the
NIST ID tracking number, the calibration service ID that identifies the temperature range of
calibration, the 0 mA R(TPW) value as measured at the end of the calibration, and the equivalent
temperature change in the R(TPW) value from calibration to calibration.
Table 1. PRTCL Database excerpt example of one SPRT sent to NIST for multiple calibrations.
Year &
Batch
NIST ID
Service ID
R(TPW),

R(TPW),
mK

96P

98B

98K

99I

01A

01H

03B

740
33200C

812
33200C

854
33190C

904
33190C

950
33190C

996
33200C

1041
33200C

25.555813

25.555977

25.557616

25.557606

25.557870

25.558420

25.559023

1.6

16.4

-0.1

2.6

5.5

6.0

If the as received R(TPW) differs by more than 10 mK from the previous database value, the
customer is contacted to discuss possible causes of the gross change. This is useful because large
changes can indicate accidental abuse (known or unknown), physical changes in the
thermometer, or shipping abuse. Information gained from the customer on the possible cause of
the gross change is used to suggest changes to the customers use of the SPRT, tailor the
annealing procedure to accommodate the excessive change in the R(TPW), and inform the
customer of an increase in calibration turn-around time due the probable increase in the
annealing duration required to stabilize the thermometer. Figure 3 displays an SPRT with a
>10mK change in the R(TPW) value with respect to the previous calibration.
It is useful for the customer to measure the R(TPW) at their facility prior to shipping or hand
carrying the SPRT and to send the R(TPW) value with the thermometer. This information can
help decide if the SPRT suffered severe mechanical shock during transport to NIST. If the SPRT
is shipped to NIST, a difference in the customer R(TPW) value from the NIST as received
R(TPW) value is a combination of the mechanical shock incurred during shipping, difference in
the realization of the ohm, and TPW realization uncertainties. If the SPRT is hand carried to
NIST, then the difference in the customer R(TPW) value from the NIST as received R(TPW)
value is primarily the difference in the ohm realization and TPW realization uncertainties.

2005 NCSL International Workshop and Symposium

20

R (TPW), mK

15

10

5
10

Years Before Present

Figure 3. An example of an SPRT that shows a >10mK change in the R(TPW) value with respect
to the previous calibration.
A shipped SPRT, regardless how well packaged, will suffer from mechanical shock due to
handling during transport. A properly packaged SPRT will be in a sturdy wooden or fiberglass
case (preferably not cardboard), with adequate foam padding surrounding the OEM SPRT box.
In addition, several SHOCK WATCH indicators should be applied to both the manufacturers
box and the external package. If the package arrives at NIST with the SHOCK WATCH
activated, the owner of the SPRT is immediately notified before the package is opened.
Thermometers shipped back to a customer from NIST are returned with new SHOCK
WATCH indicators attached to their original container (if wood or fiberglass) or in a new
cardboard box. Customers should always measure the R(TPW) of the SPRT on receipt from
NIST and note if the SHOCK WATCH is activated.
2.2 NIST SPRT annealing procedures
There are three different annealing procedures used to stabilize the SPRT. Each procedure is
designed to stabilize the thermometer for the requested ITS-90 calibration temperature range. A
description of each procedure is outlined below. In some cases SPRTs are not annealed prior to
calibration, such as thermometers used over the temperature range from 200 C to 30 C,
capsule SPRTs, or by special request of the customer. However as indicated above, a long-stem
SPRT that indicates a gross change of 10 mK at the R(TPW) should be stabilized prior to
calibration and the options are discussed with the customer.

2005 NCSL International Workshop and Symposium

For an SPRT requiring calibration between the argon triple point (189.3442 C) and the zinc
freezing point (419.528 C) the following annealing procedure is followed.
Prior to an annealing cycle, the SPRT sheath is wiped clean with acetone and then ethanol (190
proof). This is done to remove grease and oil that may possibly cause damage (e.g.,
devitrification of the fused silica) to the sheath at elevated temperatures. The SPRT is placed in
vertical furnace operating at 475 C for 12 hours. After annealing, the SPRT is carefully
removed and allowed to cool to ambient while in a vertical position. The R(TPW) is measured
and if the R(TPW) difference between the R(TPW) measured prior to and after the anneal is
greater the equivalent of 0.2 mK, then the SPRT is re-annealed. For a 25.5 SPRT, a R(TPW)
change of 20 is equivalent to a change of 0.2 mK. If the R(TPW) is less than 0.2 mK, then
the SPRT is properly stabilized and the calibration may proceed.
For an SPRT requiring calibration between the argon triple point (189.3442 C) and the
aluminum freezing point (660.323 C) the following annealing procedure is followed.
Prior to an annealing cycle, the SPRT sheath is wiped clean with acetone and then ethanol (190
proof). This is done to remove grease and oil that may possibly cause damage (e.g
devitrification of the fused silica) to the sheath at elevated temperatures. To keep the
thermometer sheath clean, thermometers are handled while wearing disposable, powder free
latex gloves. The SPRT is placed in a programmable vertical furnace that heats the thermometer
from 100 C to 675 C over a 2-hour period (280 C/hr), heat treated at 675 C for 3 hours, cools
to 500 C over a 3-hour period (58 C/hr), and then cools to the furnace holding temperature of
100 C. The SPRT is carefully removed when the temperature is below 475 C and allowed to
cool to ambient in a vertical position. The R(TPW) is measured and if the R(TPW) difference
between the R(TPW) measured prior to and after the anneal is greater the equivalent of 0.2 mK,
then the SPRT is re-annealed. For a 2.5 HTSPRT, a R(TPW) change of 2 is equivalent to
a change of 0.2 mK. For a 0.25 HTSPRT, a R(TPW) change of 0.2 is equivalent to a
change of 0.2 mK. If the R(TPW) is less than 0.2 mK, then the SPRT is properly stabilized and
the calibration may proceed.
For an HTSPRT requiring calibration between the TPW and the silver freezing point (961.78 C)
the following annealing procedure is followed.
Prior to annealing cycle, the HTSPRT sheath is soaked in 20% nitric acid to remove any possible
metallic contaminants on the surface of the fused-silica sheath and rinsed with distilled water.
The HTSPRT is then wiped clean with acetone and then ethanol (190 proof) to remove any
grease and oil that may possibly cause damage (e.g devitrification of the fused silica) to the
sheath at elevated temperatures. To keep the thermometer sheath clean, thermometers are
handled while wearing disposable, powder free latex gloves. The HTSPRT is placed in a
programmable vertical furnace that heats the thermometer from 100 C to 975 C over a 3.5-hour
period (250 C/hr), heat treated at 975 C for 2.5 hours, cools to 500 C over a 5-hour period
(95 C/hr), and then cools to the furnace holding temperature of 100 C. The HTSPRT is
carefully removed when the temperature is below 475 C and allowed to cool to ambient in a
vertical position. The R(TPW) is measured and if the R(TPW) difference between the R(TPW)

2005 NCSL International Workshop and Symposium

measured prior to and after the anneal is greater the equivalent of 0.2 mK, then the HTSPRT is
re-annealed. If the R(TPW) is less than 0.2 mK, then the HTSPRT is properly stabilized and the
calibration may proceed.
3. Results
Stabilization of the SPRT is an integral part of the NIST ITS-90 thermometer calibration IMAP.
The controls placed upon the change in R(TPW) during the calibration process are dependant
upon the stabilization of the SPRT through a specified annealing program with specific time and
temperature values. While very few SPRTs cannot be brought into compliance within the five
cycle specification, the occurrence of such an event requires an explanation. The development of
the NIST SPRT Calibration Database, allows for the review of both the calibration history of an
individual SPRT and the annealing history for the specific calibration. Table 2 displays an
excerpt from the database for ten randomly selected SPRTs giving the NIST ID#, platinum coil
sensor type, calibration service ID, the number of anneals required to stabilize the SPRT to
within the 0.2 mK criterion, the change in the R(TPW) value during the stabilization, the
R(TPW) values from the last and previous calibrations, and the equivalent temperature change in
the R(TPW) values.
Table 2. Excerpt from the NIST PRTCL database for ten randomly selected SPRTs.

25.482955
25.546750
25.509878
25.467036

R(TPW)
previous
cal
25.483010
25.546368
25.509914
25.466964

R(TPW)
(last prev.),
mK
0.5
3.8
0.4
0.7

5.2

25.570897

25.570896

0.0

4
2

3.8
5.0

25.544063
25.522721

25.545041
25.522744

9.8
0.2

33190C

1.7

25.564889

25.564947

0.6

33200C
33190C

5
3

7.9
5.9

25.280549
25.580068

25.280525
25.580116

0.2
0.5

33180C
33200C
33190C
33200C

# of
anneal
cycles
2
4
1
3

R(TPW) during
stabilization,
mK
2.1
4.1
0.0
0.1

33280C

33200C
33190C

NIST
ID#

Sensor
Type

Service
ID

1095
1052
1061
1065

coiled helix
birdcage
coiled helix
birdcage
singlelayer
bifilar
birdcage
coiled helix
singlelayer
bifilar
coiled helix
birdcage

2018
1082
1059
1053
1084
1094

R(TPW)
last cal

As seen in Table 2, the R(TPW) between the final TPW recorded at the end of the calibration
and the as received TPW value is not an indicator of the number of anneal cycles that will be
necessary to bring the SPRT to within the 0.2 mK stabilization criterion, but does indicate the
amount of change to the platinum sensor. Figure 4 gives an example of one of the ten SPRTs
from Table 2 showing the equivalent temperature change in the R(TPW) relative to the first
calibration R(TPW) value and the change in the R(TPW) values measured during the last
stabilization process. Note that during the annealing cycles the SPRT was not brought back to the
original R(TPW) value.

2005 NCSL International Workshop and Symposium

40

R (TPW), mK

30

[R(TPW) 1st R(TPW)]

calibration
[R(TPW) change during
last stabilization]

20

10

10

Figure 4. An example of one of the ten SPRTs from Table 2 showing the equivalent temperature
change in the R(TPW) relative to the first calibration R(TPW) value and the change in the
R(TPW) values measured during the last stabilization process.
As seen in Figure 5, no correlation was found in the number of annealing cycles required to
properly stabilize the SPRT prior to calibration as function of the manufacturers thermometer
construction (e.g., different sheath materials, overall instrument lengths, wire supports and head
configurations). However, for these randomly selected ten SPRTs, a coiled helix wound sensor
appears easier to anneal. The choice of sheath material, whether metal, borosilicate glass, or
fused silica, appeared to have no discernable effect upon either the annealing process or the
measured change in R(TPW) during calibration over any of the ITS-90 subranges.
The goal of properly stabilizing the SPRTs is that the thermometers can meet the NIST ITS-90
calibration uncertainties. It is critical that the SPRT be properly stabilized to meet the allowable
change of 0.75 mK at the R(TPW) during the thermometer calibration. Figure 6 shows the
maximum change (in equivalent temperature) in the R(TPW) during the last calibration of the ten
SPRTs listed in Table 2. Thermometers not meeting this 0.75 mK stability criterion the first time
are re-stabilized and then re-calibrated. SPRTs not meeting this 0.75 mK stability criterion the
second time are considered non-defining standards of the ITS-90 and returned to the customer
without calibration values.

2005 NCSL International Workshop and Symposium

Anneal Cycles for Acceptance

5
4
3
2
1
0
Single-Layer Bifilar

Birdcage

Coiled Helix

Maximum R (TPW), mK

Figure 5. Number of annealing cycles required to stabilize SPRTs as a function of sensor coil
type (coiled helix , birdcage , single-layer bifilar ).

0.75

0.00
0

10

SPRT

Figure 6. The maximum equivalent temperature change in the R(TPW) during the last calibration
of ten randomly selected SPRTs from the NIST PRTCL database. The dashed line represents the
maximum allowable change during a calibration.
2005 NCSL International Workshop and Symposium

4. Conclusions
As evidenced by the results given in Figure 5, there appears to be a possible correlation between
and the SPRT coil sensor design and number of annealing cycles required to stabilize the SPRT
to the NIST 0.2 mK pre-calibration stability criterion. Further investigation, using the data from
the NIST PRTCL database, is needed to confirm the correlation between the SPRT coil sensor
design and number of annealing cycles required to properly stabilize the SPRT. No correlation
was found in the number of annealing cycles required to properly stabilize the SPRT from
different manufacturers (e.g., different sheath materials, overall instrument lengths, wire
supports and head configurations). The results from Figure 6 for the same ten SPRTs displayed
in Figure 5 show that properly stabilized SPRTs can routinely meet the NIST calibration stability
criterion of 0.75 mK. The use of these stability requirements as part of the PRTCL IMAP is
critical to ensuring that the thermometer calibrations meet the NIST SPRT uncertainty claims.
5. References
1. H. Preston-Thomas, The International Temperature Scale of 1990 (ITS-90), Metrologia,
1990, 27, pp 3-10; ibid. p. 107.
2. G.F. Strouse, Internal Measurement Assurance for the NIST Realization of the ITS-90 from
83.8 K to 1234.93 K, Temperature: Its Measurement and Control in Science and Industry,
edited by D.C. Ripple, Vol. 7, (American Institute of Physics, New York, 2003), pp. 879884.
3. B.W. Mangum and G.T. Furukawa, "Guidelines for Realizing the International Temperature
Scale of 1990 (ITS-90)", NIST TN1265, 1990, pp. 190.
4. G.F. Strouse, "NIST Implementation and Realization of the ITS-90 Over the Range 83 K to
1235 K. Reproducibility, Stability, and Uncertainties," in Temperature: Its Measurement and
Control in Science and Industry, edited by J.F. Schooley, Vol. 6, (American Institute of
Physics, New York, 1992), pp. 169-174.
5. R.S. Kaeser, and G.F. Strouse, An ITS-90 Calibration Facility, NCSL Conference, 1994.

2005 NCSL International Workshop and Symposium