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THERMOMETERS, CONTACT, DIRECT READING:


CALIBRATION

UDC 536.5:53.088

Key words: Calibration, test method, thermometers

CONTENTS
1.
2.
3.
4.
5.
6.

1.

SCOPE
FIELD OF APPLICATION
REFERENCES
DEFINITIONS
SAMPLING
METHOD OF TEST
6.1 PRINCIPLE
6.2 APPARATUS
6.2.1 Reference thermometer
6.2.2 Thermostat
6.2.2.1 Baths
6.2.2.2 Furnaces
6.2.2.3 Temperature calibrators
6.2.3 Equalising blocks
6.2.4 Immersion test
6.3 PREPARATION OF TEST SAMPLES
6.4 PROCEDURE
6.4.1 Selection of calibration temperatures
6.4.2 Mounting
6.4.3 Readings
6.5 EXPRESSION OF RESULTS
6.6 UNCERTAINTY
6.7 TEST REPORT

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SCOPE

The scope of this method is to function as a guideline for the


calibration of direct-reading contact thermometers by means
of the comparison technique.

2.

FIELD OF APPLICATION

The method can be applied for the calibration of direct-reading


contact thermometers in the approximate range of -100C to
1500C. The method does not apply to liquid-in-glass thermometers which are treated in another NORDTEST method.
Direct-reading thermometers can be of many types, of which
the most common are:
-

The probe and the indicating device are integrated into one
unit. An example of this type is the bimetallic thermometers.

Thermometer systems consisting of one or more temperature probes connected by means of cables to an indicating
or recording device which shows the results digitally by
means of numbers or in anabg form on a graduated scale
or by lines on a graduated paper.

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 Majestys 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. Prces-Verbeaux de sances 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

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ISSN 0283-7226

Proj. 951-90

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NORDTEST METHOD

DEFINITIONS

4.

The definitions in this chapter are mainly extracts from [4].

NT VVS 103 2

6.

METHOD OF TEST

6.1

PRINCIPLE

The operation intended to bring a measuring instrument into a


state of performance and freedom from bias suitable for its use.

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.

Calibration

6.2

The set of operations which establish, under specified conditions, the relationship between values indicated by a measuring instrument or measuring system, or values represented by
a material measure, and the corresponding known values of a
measurand.

6.2.1

Adjustment

Notes
The result of a calibration permits the estimation of errors
of indication of the measuring instrument, measuring system 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.

APPARATUS
Reference thermometer

Any type of thermometer can be used as reference thermometer provided that it covers the required temperature
range and that its calibration is traceable to a national standard. 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 962C. 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 1300C, 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 630C. With a good ice point and a
digital voltmeter, uncertainties of down to 0.3C can be obtained.

Note

A conventional true value is, in general, regarded


as sufficiently close to the true value for the difference to be insignificant for the given purpose.

Up to about 1300C, 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.

Example

Within an organisation, the value assigned to a


reference standard may be taken as the conventional true value of the quantity realised by the
standard.

Above 1300C, the stability of thermocouples of type B is


superior to types S and R, but the output voltage is 35-40%
lower.

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 comparisons.

5.

SAMPLING

Not applicable.

Liquid-in-glass and other direct-reading thermometers of sufficient 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.

NT VVS 103 3

NORDTEST METHOD

Good temperature uniformity so that the temperature


difference between the thermometer and the reference
thermometer is small compared with the uncertainty requirements.

6.2.2.1

Baths

For the most demanding calibration work the stirred liquid bath
is preferred. The liquid and the stirring ensures good temperature 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 aluminium 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 airsaturated water, and it was once a defining point on the
temperature scale. Today it still plays a major role in thermometry 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
4C, 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
Methyl Alcohol
Ethylene Glycol/Water 1:1
Ice point bath
Water
Vegetable oils up to approx.
Silicone oils
Petroleum oils
Potassium Nitrate/
Sodium Nitrite, approx. 1:1 mixture

-112C to 23C
-97C to 23C
-30C to 110C
0C
+1C to 95C
200C
-50C to 300C
100C to 300C
170C to 550C

The temperature range of the alcohols can be extended upwards, 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 experience 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, cottonwaste, 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 0C with an uncertainty better than 0.01 C.


The more sophisticated ice points contain a stirring mechanism constructed in such a way that it keeps the water saturated
with air. The uncertainty in these baths can be better than
0.002C. 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 550C and for less demanding


calibrations above 100C to 200C, 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 temperature 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 combined 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 temperature equalising blocks can be fitted one at a time. The block
contains one or more bores for the thermometers to be calibrated. 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
0.1C, but 0.01C has also been seen.
The stability of these calibrators is often better than 0.1C, but
the lack of a stirred liquid can cause problems with the temperature 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 thermometer with its probe placed in the interchangeable equalising 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 oxidation.
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 thermometer) 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 furnaces 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 pressure. 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.

NT VVS 103 5

NORDTEST METHOD

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 withdrawal, 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 intervals:
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 adjustment of a thermometer, the necessary instructions such as e.g.
the service manual must be available.

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 thermostat.

If adjustments are ordered, the user must decide whether the


thermometer should also be calibrated before the adjustment
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
6.4.1

PROCEDURE
Selection of calibration temperatures

Calibration is performed at the temperatures selected by the


user. If the measuring range of the thermometer includes 0C,
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.

T
R

X1

X2

R'

X2'

X1'

R"

Time

Fig. 2. Sequence of readings.

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 probe is placed in the thermostat close to the probe of the


reference thermometer. Several probes can often be calibrated at a time. In furnaces without equalising blocks, the
probes can be tied together with e.g. thermocouple wire.
In a bath, immersion of the probes should be as deep as
possible and not less than 100 mm. See 6.2.4 for a check of
sufficient immersion.
For surface temperature probes, the tip should only be immersed 5 mm into the liquid to simulate its normal use, but the

The table has 4 columns.


a) Temperature t (C)
t is the conventional true value of the temperature and is
calculated as the mean of the 3 readings R of the reference
thermometer corrected for all known errors.

b) Reading tr(C)
tr is the reading of the thermometer. It is calculated as 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 correction 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)
Determination of this number is described in 6.6. The value
is stated with one or two significant decimals.

Example

For a digital instrument, this is normally equal to the resolution 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 normally 20% (1/5) of the smallest graduation. In the case of
coarse graduation lines and/or wide indexes, the reading
uncertainty may be greater.
For both analogue and digital instruments it happens that
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
between the maximum value and the minimum value observed during the short time of the calibration process.

The uncertainty components are combined to a total uncertainty as described by BlPM in [5] or WECC in [6].

0.00
100.57
230.9

0.20
100.25
228.5

-0.20
+0.32
+2.4

0.10
0.16
1 .0

Both descriptions assume that corrections have been made


for all known systematic errors.
The BlPM recommendation defines two categories of uncertainty according to the way in which their numerical values are
est imated:

6.6

UNCERTAINTY

There are at least 4 main sources of uncertainty for the total


calibration uncertainty. Each source can have several uncertainty components involved:
a) The calibration uncertainty of the reference thermometer
as stated on its certificate.
b) The uncertainty of determination of the reference temperature.
This is dependent on the type of instrumentation used.
In case of a direct-reading reference thermometer, the
components are the reading uncertainty and the drift since
last calibration.
In case of a Pt-100 with an ohmmeter, the drifts of the
Pt-100, the ohmmeter, the reading uncertainty and calibration uncertainty of the ohmmeter must be considered.
In case of a SPRT measured at the triple point of water or
ice point for determination of its W at the reference temperature, its drift can be neglected, but uncertainty contributions from the triple or ice point, the measuring bridge
and the standard resistor have to be considered.
c) The uncertainty of the thermostat (instability and gradients).
Please observe that the gradients can be large when
surface temperature probes are calibrated in a bath.
d) The reading uncertainty of the thermometer to be calibrated.

A. Those which are evaluated by applying statistical methods


to a series of repeated determinations.
B. Those which are evaluated by other means.
The WECC guideline treats all components as random variables, even the influence quantities which may affect the
measured value in a systematic way. The results of using the
WECC guideline are consistent with the results of using the
BIPM recommendation.
In the short description below we do not distinguish between
category A and B, and as for the WECC guidelines we treat all
components as random variables.
The principle of the combination method is that the size of each
uncertainty component s i is evaluated at a 1 sigma level. The
1 sigma values are then combined by means of the following
equation:

st=

48 + 4 + ... + 4

ut is then found from:

For this Nordtest method k = 2 is used.

An example of one way of calculating the uncertainty is shown


below. Each component is listed together with an estimate of
its value. The distribution factor for each component is then
estimated, and the 1 sigma value is found by dividing the
component's value by its distribution factor.

NORDTEST METHOD

Cornponent

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Value

Factor

uncertainty is strongly related to this component and is


estimated to be included in it.

1 sigma

value
C

The temperature gradients in the thermostat have a limit of


0.005C with a rectangular distribution.

a) Ref. therm. calibration

0.02

0.01

b) Reading uncertainty of
reference thermometer

0.01

1.73

0.006

Drift of ref.therm.

0.02

1.73

0.012

c) Thermostat instability

0.01

1.41

0.007

6.7

Thermostat gradients

0.005

1.73

0.003

The Test Report called a Calibration Certificate must, if relevant, include the following information:

d) Reading of thermometer
to be calibrated

0.01

1.73

0.058

Root of sum of squares

st= 0.060
~~~

d) The resolution of the thermometer to be calibrated is 0.1C


with a rectangular distribution.

TEST REPORT

a) Name and address of the issuing calibration laboratory.


b) Accreditation number of the laboratory if the laboratory is
accredited by the national accreditation body.
c) (Unique) identification number of the calibration certificate.

Then the uncertainty is calculated as

ut = 2 * st = 0.12C

d) Date of receipt of the instrument or device calibrated,


date(s) on which the calibration was carried out and date
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 0.02C. The calibration laboratory also uses k = 2, thus the 1 sigma value becomes
0.01C.

f) Statement by the accreditation body if the laboratory is


accredited by the national accreditation body.

b) The reading uncertainty of the reference thermometer is


equal to its resolution 0.01C. 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 0.02C.
Again the distribution is estimated to be rectangular.
c) The temperature fluctuations in the thermostat have an
amplitude not exceeding 0.01C. The variations approximately follow a sine function. In such a case the distribution
is U-shaped, and the distribution factor is 2. The type A

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 calibrations 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.

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