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THERMOMETERS, CONTACT, DIRECT READING: UDC 536.5:53.088

CALIBRATION

Key words: Calibration, test method, thermometers

CONTENTS 1. SCOPE
1. SCOPE 1 The scope of this method is to function as a guideline for the
2. FIELD OF APPLICATION 1 calibration of direct-reading contact thermometers by means
3. REFERENCES 1 of the comparison technique.
4. DEFINITIONS 2
5. SAMPLING 2
6. METHOD OF TEST 2 2. FIELD OF APPLICATION
6.1 PRINCIPLE 2 The method can be applied for the calibration of direct-reading
6.2 APPARATUS 2 contact thermometers in the approximate range of -100°C to
6.2.1 Reference thermometer 2 1500°C. The method does not apply to liquid-in-glass ther-
6.2.2 Thermostat 2 mometers which are treated in another NORDTEST method.
6.2.2.1 Baths 3
6.2.2.2 Furnaces 4 Direct-reading thermometers can be of many types, of which
6.2.2.3 Temperature calibrators 4 the most common are:
6.2.3 Equalising blocks 4 - The probe and the indicating device are integrated into one
6.2.4 Immersion test 4 unit. An example of this type is the bimetallic thermometers.
6.3 PREPARATION OF TEST SAMPLES 5
6.4 PROCEDURE 5 - Thermometer systems consisting of one or more tempera-
6.4.1 Selection of calibration temperatures 5 ture probes connected by means of cables to an indicating
6.4.2 Mounting 5 or recording device which shows the results digitally by
6.4.3 Readings 5 means of numbers or in anabg form on a graduated scale
6.5 EXPRESSION OF RESULTS 5 or by lines on a graduated paper.
6.6 UNCERTAINTY 6
6.7 TEST REPORT 7
3. REFERENCES
1. The International Temperature Scale of 1990 (ITS-90), H.
Preston-Thomas, Metrologia 27, pages 3-10 (1990).
2. Standard Practise for Preparation and Use of Freezing
Point Reference Baths, ASTM E 563-76.
3. Precautions in the Use of Nitrate Salt Baths, Health and
Safety Executive, Her Majesty’s Stationery Office.
4. International Vocabulary of Basic and General Terms in
Metrology, BIPM, IEC, ISO and OIML, 1984.
5. Bureau International de Poids et Mesures. Pròces-Ver-
beaux de sèances du ClPM 49, 26 (1981). Version in
English published in Metrologia 18, page 44 (1982).
6. Guidelines for the Expression of the Uncertainty of
Measurement in Calibrations, WECC Doc. 19-1990.
7. Temperature Calibration Baths, Alvin B. Kaufman,
Measurements & Control, April 1990, page 121.

Published by NORDTEST Tekniikantie 12 FIN-02150 Espoo FINLAND Tel + 358 9 455 4600 Fax + 358 9 455 4272
ISSN 0283-7226 Proj. 951-90 www.nordtest.org
NORDTEST METHOD
4. DEFINITIONS
The definitions in this chapter are mainly extracts from [4].
Adjustment
The operation intended to bring a measuring instrument into a
state of performance and freedom from bias suitable for its use.
Calibration
The set of operations which establish, under specified condi-
tions, the relationship between values indicated by a measur-
ing instrument or measuring system, or values represented by
a material measure, and the corresponding known values of a
measurand.
Notes
The result of a calibration permits the estimation of errors
of indication of the measuring instrument, measuring sys-
tem or material measure, or the assignment of values to
marks on arbitrary scales.
A calibration may also determine other metrological
properties.
The result of a calibration may be recorded in a document,
sometimes called a calibration certificate or a calibration
report.
The result of a calibration is sometimes expressed as a
calibration factor, or as a series of calibration factors in the
form of a calibration curve.
Conventional true value (of a quantity)
A value of a quantity which, for a given purpose, may be
substituted for the true value.
Note A conventional true value is, in general, regarded
as sufficiently close to the true value for the dif-
ference to be insignificant for the given purpose.
Example Within an organisation, the value assigned to a
reference standard may be taken as the conven-
tional true value of the quantity realised by the
standard.
Traceability
The property of a result of a measurement whereby it can be
related to appropriate standards, generally international or
national standards, through an unbroken chain of compari-
sons.
5. SAMPLING
Not applicable.
NT VVS 103 2
6. METHOD OF TEST
6.1 PRINCIPLE
The temperature sensitive part (probe) of the thermometer is
placed in a thermostat together with a reference thermometer.
The indication of the thermometer is compared with the
reference temperature which is measured with the reference
thermometer.
6.2 APPARATUS
6.2.1 Reference thermometer
Any type of thermometer can be used as reference ther-
mometer provided that it covers the required temperature
range and that its calibration is traceable to a national stan-
dard. Further its calibration and reading uncertainty must be
small compared with the required calibration uncertainty, and
it must be of a sufficient length to avoid influence from the
immersion effect (see 6.2.4).
Standard Platinum Resistance Thermometers (SPRT) fulfilling
the requirements in [1] are used for the most demanding work
up to 962°C. Used with a good measuring bridge and a stable
standard resistor, uncertainties in the range of millikelvins can
be obtained.
A stable Pt-100 probe with a measuring bridge and a standard
resistor or with a good digital thermometer orwith an ohmmeter
can be a useful reference thermometer. Uncertainties of a few
millikelvin have been reported.
For less demanding work and for higher temperatures up to
about 1300°C, a thermocouple of type S has a long proven
reputation of stability. It was also used as an interpolating
instrument in the International Practical Temperature Scale of
1968 (IPTS-68) above 630°C. With a good ice point and a
digital voltmeter, uncertainties of down to 0.3°C can be ob-
tained.
Up to about 1300°C, thermocouples of type R are reported to
have the same stability as thermocouples of type S, but type
R has a 10-12% higher output voltage.
Above 1300°C, the stability of thermocouples of type B is
superior to types S and R, but the output voltage is 35-40%
lower.
Liquid-in-glass and other direct-reading thermometers of suf-
ficient accuracy and stability are convenient due to their ease
of use.
6.2.2 Thermostat
The requirements for the thermostat are:
- Sufficient dimensions to contain both the thermometer and
the reference thermometer.
- Sufficient short-term stability compared with calibration
time and the uncertainty requirements.
NORDTEST METHOD NT VVS 103 3

- Good temperature uniformity so that the temperature
difference between the thermometer and the reference
thermometer is small compared with the uncertainty re-
quirements.
6.2.2.1 Baths
For the most demanding calibration work the stirred liquid bath
is preferred. The liquid and the stirring ensures good tempera-
ture uniformity in the bath and good thermal contact with the
thermometers.
Special calibration baths are commercially available. They
have the necessary depth, and the liquid to air surfase is small.
Some general purpose baths can also be used, but the bigger
the liquid to air surface area the higher is the risk of instability,
and the bigger the bath the higher is, usually, the “from corner
to corner” temperature difference.
A bath with a large amount of liquid is usually very stable, but
it takes a long time to change the calibration temperature while
a small volume bath changes calibration temperature fast but
requires a better control system to be stable.
rise to a ’steam explosion’. In several instances the injuries
have proven fatal. Due to fast oxidation, aluminium or alumi-
nium alloys should not come into direct contact with the molten
nitrate. Neither should quartz encapsulated thermometers
come into contact with molten nitrate as the quartz will be
matted due to the start of a devitrification process.
Further information about precautions and the use of salt baths
can be obtained in [3].
The ice point (Fig. 1) is the equilibrium between ice- and air-
saturated water, and it was once a defining point on the
temperature scale. Today it still plays a major role in thermo-
metry as a secondary fixed point that can be readily achieved
by almost any laboratory with a minimum of resources.
In its simplest form, it consists of a dewar with a mixture of
demineralised or distilled water and crushed or shaved ice
made from demineralised or distilled water. As the ice is
melting continuously and as water has its maximum density at
4°C, one has to make sure that there is ice and not only water
around and below the tip of the probe. Such a bath can give

Different liquids are used depending on the temperature range:

Ethyl Alcohol -112°C to 23°C

Methyl Alcohol -97°C to 23°C
Ethylene Glycol/Water 1:1 -30°C to 110°C
Ice point bath 0°C
Water +1°C to 95°C
Vegetable oils up to approx. 200°C
Silicone oils -50°C to 300°C
Petroleum oils 100°C to 300°C
Potassium Nitrate/
Sodium Nitrite, approx. 1:1 mixture 170°C to 550°C
The temperature range of the alcohols can be extended up-
wards, but care has to be taken as the fumes are toxic and
explosive.

Different grades of petroleum and silicone oils must be used

to cover the stated ranges. The oils must not have flash points
below the highest calibration temperature nor must they be too
viscous to prevent adequate stirring at the lowest calibration
temperature. At the high end of the temperature range, the
fumes can be rather unpleasant.

Experience with the use of vegetable oils for calibration baths

is limited. [7] gives some examples of flash points and experi-
ence gained with oils such as olive, corn, soybean, peanut,
rape seed and others.

Use of the salt bath with Potassium Nitrate and Sodium Nitrite
requires some precautions. The nitrate salt alone cannot be
made to burn or explode. It is, however, a powerful oxidising
agent, and combustible material coming into contact with
molten nitrate is readily ignited and often burns with explosive
violence. The molten nitrate should therefore never come into
contact with organic materials such as oil, grease, cotton-
waste, rags, sacking, paper, wood, clothing, food and graphite.
Water introduced accidentally into molten nitrate baths will give Fig. 1. Ice point.
NORDTEST METHOD
the temperature 0°C with an uncertainty better than ±0.01 °C.
The more sophisticated ice points contain a stirring mechan-
ism constructed in such a way that it keeps the water saturated
with air. The uncertainty in these baths can be better than
±0.002°C. A description of the preparation and use of the ice
point bath can be found in [2].
6.2.2.2 Furnaces
For temperatures higher than 550°C and for less demanding
calibrations above 100°C to 200°C, a tube furnace is used.
Different models are available. Horizontal instead of vertical
tube furnaces are preferred because of the risk of a chimney
effect in the vertical furnace.
For the most demanding work a three-zone furnace is used. It
has a centre-zone heater and two end-zone heaters each with
a controller. The end-zone controllers can be independent of
the centre-zone temperature, but often they are coupled to give
a constant temperature difference between the centre-zone
and the end-zone. The advantage of the differential coupling
is that the temperature profile is maintained independently of
the temperature variations in the centre-zone. The advantage
of the three-zone furnace is that a long uniform temperature
zone can be established in the centre of the furnace so that an
equalising block can be avoided. A drawback is that the rather
long distance from the opening to the uniform zone can make
the furnace unsuitable for calibration of the shorter sensors.
The single-zone furnace is well suited for short probes, but the
uniform temperature zone is so short that an equalising block
is often used. The short uniform zone and the steep tempera-
ture gradients at the ends of this type of furnace can introduce
the immersion effect (see 6.2.4) and limit calibration accuracy.
6.2.2.3 Temperature calibrators
The thermostat and the reference thermometer can be com-
bined into one instrument, by different manufacturers called a
temperature calibrator or a dry well calibrator. The temperature
is maintained in a chamber in which interchangeable tempera-
ture equalising blocks can be fitted one at a time. The block
contains one or more bores for the thermometers to be cali-
brated. The probe of the reference thermometer is in the
chamber but outside the block and it is connected to a built-in
digital instrument. The resolution of these instruments is often
0.1°C, but 0.01°C has also been seen.
The stability of these calibrators is often better than 0.1°C, but
the lack of a stirred liquid can cause problems with the tem-
perature difference between the reference thermometer and
the thermometer to be calibrated. It is important that the bore
in the block fits closely the thermometer under calibration, and
that the bore is deep enough so that the immersion effect is
small (see 6.2.4). Further there is a time lag between the probe
of the reference thermometer and the probe to be calibrated.
After changing to a new temperature, the built-in instrument
will show that the temperature is stable before the temperature
in a probe to be calibrated is stable.
NT VVS 103 4
For more demanding calibrations, a separate reference ther-
mometer with its probe placed in the interchangeable equali-
sing block should be used.
6.2.3 Equalising blocks
Equalising blocks of thermal conducting materials such as
aluminium and copper can be used in both baths and furnaces.
For use at high temperatures, copper blocks are covered with
a protecting layer of e.g. inconel for protection against oxida-
tion.
The advantage of an equalising block in a bath is primarily its
ability to smoothe the small temperature fluctuations to a few
millikelvin. The temperature differences are usually small in a
stirred bath provided that the distances between probes are
small. This extremely good stability should, however, not make
one forget about other sources of error. If the equalising block
is touching a cold wall in the bath, errors greater than the
fluctuations can easily arise due to gradients. And when a
resistance thermometer (item under test or reference ther-
mometer) is used in an equalising block, the error due to
self-heating is generally greater than when the probe is used
directly in the stirred liquid and may impair the advantage of
the equalising block.
The main advantage of using an equalising block in a furnace
is its ability to even out temperature gradients. Usually fur-
naces are slow, so fluctuations are small during the calibration
measurements.
A drawback of using equalising blocks is that they make the
change to a new temperature slowly. The temperature at the
beginning of the change quickly approaches the set point, but
final stabilisation takes time.
A more advanced form of equalising blocks makes use of the
heat-pipe principle. Heat pipes are hollow, hermetically sealed
and contain a substance which at the working temperature
forms an equilibrium between vapour and liquid under pres-
sure. The vapour will condense at cold spots, and the liquid
will vaporise at hot spots, and the temperature differences are
thereby smoothed.
Heat pipes must be used according to the operating manual.
This often means that the heating rate must be limited until the
lower limit of their operating range is reached. In the operating
range, heat pipes work faster than simple equalising blocks.
For any equalising block as well as the bore in the block of a
temperature calibrator, it is important that the bores are fitted
closely to both the thermometer under calibration and the
reference thermometer to ensure good thermal contact (see
6.2.4).
6.2.4 Immersion test
There is always a heat exchange (immersion effect) between
the surroundings and the temperature sensitive part of the
probe. This heat exchange should be kept so low that its
influence is smaller than the required uncertainty.
NORDTEST METHOD NT VVS 103 5

The better the thermal contact between the medium and the
probe the smaller the immersion effect will be. This means that
closely fitting bores in blocks and long immersion lengths
should be used.
A simple test for the immersion effect can be performed by
withdrawing the probe from the medium in small increments
and reading its temperature after stabilisation at each step. If
the temperature changes on the first few increments of with-
drawal, the immersion length was too short or more precisely
the contact between the medium and the probe was too poor.
reference thermometer should be placed deep enough to
measure the temperature of the liquid.
In a furnace, the tip of the probes should reach the centre of
the uniform temperature zone.
6.4.3 Readings
When the temperature is sufficiently stable, the reference
thermometer (R) and the thermometers to be calibrated (Xi)
are read in the following order (Fig. 2) at constant time inter-
vals:

R, X1 , X2 .... Xn, R', Xn' .... X2', X1', R"

6.3 PREPARATION OF TEST SAMPLES
If necessary, the probe of the thermometer is cleaned with
water, water and soap or alcohol and rinsed with demineralised
water in order to avoid contamination of the liquid in the bath
and the other calibration equipment.
Except for the cleaning mentioned above, the thermometers
are normally calibrated "as received". If a user asks for adjust-
ment of a thermometer, the necessary instructions such as e.g.
the service manual must be available.
If adjustments are ordered, the user must decide whether the
thermometer should also be calibrated before the adjustment
The mean of the three readings of the reference thermometer
is the basis for the average calibration temperature. The mean
of the pairwise readings of the thermometers to be calibrated
is used as their reading at average temperature.
Provided that the difference in time constants between the
reference thermometer and the thermometers to be calibrated
is sufficiently small, this way of reading will compensate for a
slightly increasing or decreasing temperature in the thermo-
stat.

T
is carried out. Temp.

Electrical instruments supplied from the mains are connected,

set to ON and warmed up for a minimum of 4 hours before the
measurements start. This does not apply to battery supplied
instruments, but they should be allowed to stabilise at room
temperature before calibration commences.

6.4 PROCEDURE
6.4.1 Selection of calibration temperatures I R X1 X2 R' X2' X1' R" Time

Calibration is performed at the temperatures selected by the Fig. 2. Sequence of readings.

user. If the measuring range of the thermometer includes 0°C,
the user is advised to have a calibration performed at the ice
point, as this point can easily be reproduced by the user and
serve as a future check-point. 6.5 EXPRESSION OF RESULTS
The result is stated in a table in which all numbers are rounded
to the same number of decimals as the uncertainty d).
6.4.2 Mounting
The table has 4 columns.
The probe is placed in the thermostat close to the probe of the
reference thermometer. Several probes can often be cali- a) Temperature t (°C)
brated at a time. In furnaces without equalising blocks, the
t is the conventional true value of the temperature and is
probes can be tied together with e.g. thermocouple wire.
calculated as the mean of the 3 readings R of the reference
In a bath, immersion of the probes should be as deep as thermometer corrected for all known errors.
possible and not less than 100 mm. See 6.2.4 for a check of
sufficient immersion. b) Reading tr(°C)

For surface temperature probes, the tip should only be im- tr is the reading of the thermometer. It is calculated as the
mersed 5 mm into the liquid to simulate its normal use, but the mean of the 2 readings Xi and Xi'.
NORDTEST METHOD NT VVS 103 6

c) Correction tc(°C)
tc is calculated from the following equation:
tc = t - tr
When the thermometer is used after calibration, the correc-
tion tccan be added to the reading tr ,of the thermometer to
give the best estimate of the true temperature:
t = tr + tc
d) Uncertainty ut( ± °C)
For a digital instrument, this is normally equal to the reso-
lution or meaning of the least significant digit. However, it
can sometimes be observed that due to too poor resolution
of the ADC, some numbers never appear as the least
significant digit. In such cases a higher reading uncertainty
must be accounted for.
For analogue instruments the reading uncertainty is nor-
mally 20% (1/5) of the smallest graduation. In the case of
coarse graduation lines and/or wide indexes, the reading
uncertainty may be greater.

Determination of this number is described in 6.6. The value For both analogue and digital instruments it happens that
is stated with one or two significant decimals. the readings vary more than the previously determined
reading uncertainty indicates. In such cases the reading
uncertainty can be calculated as half of the difference
Example between the maximum value and the minimum value ob-
served during the short time of the calibration process.
The uncertainty components are combined to a total uncer-
tainty as described by BlPM in [5] or WECC in [6].
0.00 0.20 -0.20 0.10 Both descriptions assume that corrections have been made
100.57 100.25 +0.32 0.16
230.9 228.5 +2.4 1 .0 for all known systematic errors.
The BlPM recommendation defines two categories of uncer-
tainty according to the way in which their numerical values are
est imated:
6.6 UNCERTAINTY A. Those which are evaluated by applying statistical methods
There are at least 4 main sources of uncertainty for the total to a series of repeated determinations.
calibration uncertainty. Each source can have several uncer- B. Those which are evaluated by other means.
tainty components involved:
The WECC guideline treats all components as random vari-
a) The calibration uncertainty of the reference thermometer
ables, even the influence quantities which may affect the
as stated on its certificate. measured value in a systematic way. The results of using the
b) The uncertainty of determination of the reference tempera- WECC guideline are consistent with the results of using the
ture. BIPM recommendation.

This is dependent on the type of instrumentation used. In the short description below we do not distinguish between
category A and B, and as for the WECC guidelines we treat all
In case of a direct-reading reference thermometer, the
components as random variables.
components are the reading uncertainty and the drift since
last calibration. The principle of the combination method is that the size of each
uncertainty component s i is evaluated at a 1 sigma level. The
In case of a Pt-100 with an ohmmeter, the drifts of the
1 sigma values are then combined by means of the following
Pt-100, the ohmmeter, the reading uncertainty and calibra-
equation:
tion uncertainty of the ohmmeter must be considered.
In case of a SPRT measured at the triple point of water or st= 48 + 4 + ... + 4
ice point for determination of its W at the reference tem-
ut is then found from:
perature, its drift can be neglected, but uncertainty con-
tributions from the triple or ice point, the measuring bridge
and the standard resistor have to be considered.
For this Nordtest method k = 2 is used.
c) The uncertainty of the thermostat (instability and gra-
An example of one way of calculating the uncertainty is shown
dients).
below. Each component is listed together with an estimate of
Please observe that the gradients can be large when its value. The distribution factor for each component is then
surface temperature probes are calibrated in a bath. estimated, and the 1 sigma value is found by dividing the
component's value by its distribution factor.
d) The reading uncertainty of the thermometer to be cali-
brated.
NORDTEST METHOD NT VVS 103 7

uncertainty is strongly related to this component and is

Cornponent Value Factor 1 sigma
value estimated to be included in it.
±°C ±°C The temperature gradients in the thermostat have a limit of
a) Ref. therm. calibration 0.02 2 0.01 0.005°C with a rectangular distribution.

b) Reading uncertainty of 0.01 1.73 0.006 d) The resolution of the thermometer to be calibrated is 0.1°C
reference thermometer with a rectangular distribution.

Drift of ref.therm. 0.02 1.73 0.012

c) Thermostat instability 0.01 1.41 0.007 6.7 TEST REPORT

Thermostat gradients 0.005 1.73 0.003 The Test Report called a Calibration Certificate must, if rele-
vant, include the following information:
d) Reading of thermometer 0.01 1.73 0.058
to be calibrated a) Name and address of the issuing calibration laboratory.

Root of sum of squares st= 0.060 b) Accreditation number of the laboratory if the laboratory is
~~~
accredited by the national accreditation body.

c) (Unique) identification number of the calibration certificate.

d) Date of receipt of the instrument or device calibrated,
Then the uncertainty is calculated as date(s) on which the calibration was carried out and date
ut = 2 * st = ±0.12°C of issue of the certificate.

The uncertainty components were found as follows: e) Number of pages comprising the certificate.

a) The calibration certificate for the reference thermometer
states the uncertainty to be ±0.02°C. The calibration labor-
atory also uses k = 2, thus the 1 sigma value becomes
±0.01°C.
b) The reading uncertainty of the reference thermometer is
equal to its resolution 0.01°C. The distribution is estimated
to be rectangular, thus the distribution factor is √ 3.
The history of the reference thermometer shows that the
drift between two calibrations has never exceeded 0.02°C.
Again the distribution is estimated to be rectangular.
c) The temperature fluctuations in the thermostat have an
amplitude not exceeding 0.01°C. The variations approxi-
mately follow a sine function. In such a case the distribution
is U-shaped, and the distribution factor is √ 2. The type A
f) Statement by the accreditation body if the laboratory is
accredited by the national accreditation body.
g) Name(s) and signature(s) of authorised person(s)
h) Suitable identification of the client.
i) Identification of the instrument or device calibrated.
j) The conditions (e.g. environmental) under which the cali-
brations were performed.
k) Identification of this and any other procedure employed
and of any deviation from the procedures.
I) Statement of traceability of the calibration results.
m) Calibration results and the associated uncertainty of the
measurements.