DKD-R 5-1-A-DKD-Guidelines-for-calibration-of-Digital-Thermometers
DKD-R 5-1-A-DKD-Guidelines-for-calibration-of-Digital-Thermometers
Guideline Calibration of
DKD-R 5-1 Resistance Thermometers
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Contents
Contents...................................................................................................................................... 3
Preface ....................................................................................................................................... 4
1 Scope .............................................................................................................................. 4
2 Introduction .................................................................................................................... 5
3 Resistance thermometers ................................................................................................ 5
3.1 Metal resistance thermometers ....................................................................................... 5
3.1.1 Standard platinum resistance thermometers (SPRT)...................................................... 5
3.1.2 Industrial platinum resistance thermometers (IPRT)...................................................... 6
3.2 Semiconductor resistance thermometers ........................................................................ 6
4 Fundamentals of the calibration of resistance thermometers ......................................... 6
5 Transport and initial inspection ...................................................................................... 7
6 Aging test........................................................................................................................ 7
7 Thermostat ...................................................................................................................... 8
8 Influencing factors.......................................................................................................... 8
8.1 Thermal load................................................................................................................... 8
8.2 Thermal coupling............................................................................................................ 9
8.3 Electrical measurement procedures ................................................................................ 9
8.4 Connection systems ........................................................................................................ 9
8.4.1 Two-wire connection system.......................................................................................... 9
8.4.2 Three-wire connection system...................................................................................... 10
8.4.3 Four-wire connection system........................................................................................ 10
8.4.4 Parasitic thermovoltage ................................................................................................ 11
8.4.5 Self-heating................................................................................................................... 11
8.4.6 Insulation resistance ..................................................................................................... 11
8.4.7 Asymmetry deviation ................................................................................................... 11
8.4.8 Hysteresis...................................................................................................................... 12
9 Recalibration................................................................................................................. 12
10 Results .......................................................................................................................... 13
Annex A: Measurement uncertainty in the calibration of thermometers by the
comparison method....................................................................................................... 14
Annex B: Uncertainty in measurements using a resistance thermometer ................................ 24
Preface
DKD Guidelines are application documents to the requirements of DIN EN ISO/IEC
17025:2005. DKD Guidelines describe technical and organizational processes serving the
calibration laboratories as examples when laying down internal procedures and regulations.
DKD Guidelines can become integral parts of the quality management documentation of cali-
bration laboratories. By application of the Guidelines equal treatment of the devices to be cali-
brated at the various calibration laboratories is supported and the continuity and verifiability
of the work of the calibration laboratories is enhanced.
The DKD Guidelines should not impede the further development of calibration procedures
and sequences. Deviations from the Guidelines and new procedures are admissible in agree-
ment with the Accreditation Body should this be advisable for technical reasons.
The Guideline was prepared by the Technical Committee "Temperature and Humidity" in
cooperation with the PTB and adopted by the Advisory Board of the DKD. With its publica-
tion it will become binding for all DKD calibration laboratories unless these have compiled
separate procedural instructions which have been approved by the Accreditation Body.
This DKD Calibration Guideline replaces the previous DKD Calibration Guidelines DKD-R
5-1 (1992) and DKD-R 5-2 (1992).
This document is a translation of the German Guideline DKD-R 5-1, Ausgabe 10/2003. In
case of any disputes the respective German version will be binding.
1 Scope
This Guideline was prepared to fulfil the need for a guide in the form of a general document
dealing with the calibration of resistance thermometers. It applies above all to platinum resis-
tance thermometers complying with the requirements of the standard DIN EN 60751 and cov-
ering the temperature range from ─200 °C to 850 °C.
It is also valid for all categories of resistance thermometers among which the following are of
particular importance:
• resistance thermometers from spectrally pure platinum meeting the requirements of the
ITS-90 (temperature range ─259 °C to 962 °C)
• nickel resistance thermometers
• copper resistance thermometers
• semiconductor resistance thermometers (thermistors, NTCs, PTCs)
Furthermore, the Guideline is applicable to:
2 Introduction
Almost all thermometers used in practice belong either to the group of radiation thermometers
or to that of contact thermometers. The operation of the contact thermometer is based on a
sensor which by thermal contact is brought to the temperature of the object to be measured
and whose temperature is then determined by measurement of another quantity (expansion,
electrical resistance, etc.) showing a dependence on temperature.
In practical temperature measurement, the greatest measurement deviation is frequently due to
the fact that the sensor temperature and the temperature of the object to be measured are not
identical. A contact thermometer always measures "only" its own temperature. In this sense,
calibration of a contact thermometer means the metrological determination of the relation be-
tween the temperature of the sensor and the output quantity of the thermometer. It is the task
of the user to ensure that the temperature of the sensor corresponds to the temperature to be
measured. Measurement uncertainties due to poor thermal coupling at the user's are not in-
cluded in the measurement uncertainty of thermometer calibration.
3 Resistance thermometers
The operation of resistance thermometers relies on the fact that the electrical resistance of
metal conductors and semiconductors is temperature-dependent. The temperature measure-
ment is thus traced back to the measurement of an electrical resistance. In practice (disregard-
ing the low-temperature range with t < ─200 °C), the following materials are mainly used as
resistance sensors:
6 Aging test
Mechanical stresses which have, for example, arisen during transport can in part be eliminated
by annealing (aging) at higher temperatures. To check the thermometers for adequate stability,
an aging test is usually carried out at a fixed temperature value (nominal value temperature,
ice point, triple point of water).
If a resistance thermometer is used, the resistance at the ice point is normally measured first.
Then the temperature sensor is heated over an appropriate period of time (approx. 8 h to 12 h)
to 10 K beyond the maximum calibration temperature taking into account that the maximum
operating temperature as stated by the manufacturer must not be exceeded. Afterwards, the
resistance of the thermometer is again measured at reference temperature (ice point). If the
difference between the two measurements at the ice point exceeds 30 % of the measurement
uncertainty aimed at, the aging procedure is to be repeated. If after the repeat measurement
the reference value deviates again from the preceding measurement by more than 30 %, the
calibration item is to be rejected as not calibratable.
If the thermometer is recalibrated and has not changed since the last calibration by more than
30 % of the measurement uncertainty aimed at, the aging test can be dispensed with.
The initial value before aging should be separately stated in the calibration certificate.
7 Thermostat
Platinum resistance thermometers and semiconductor sensors are calibrated either by the com-
parison method or in defined fixed points of the applicable temperature scale. Combination of
the two methods is permissible. In the comparison method the resistance thermometers or
semiconductor sensors to be calibrated are compared in temperature-stabilized baths or in
suitable furnaces using reference/working thermometers. Fixed points and standard ther-
mometers must be traceable to national measurement standards.
Within the scope of the determination of the measurement uncertainty, the spatial and tempo-
ral temperature distribution in the working space must be quantitatively determined and taken
into account for the thermostat used for calibration (thermostated bath, furnace).
For the determination of the temporal and spatial distribution, calibrated thermometers of
identical type are positioned on the boundaries of the working space (horizontal, vertical) of
the thermostat. After thermal stabilization, the temperatures measured with the thermometers
are continuously recorded (over a period longer than 20 min). The maximum resulting tem-
perature difference between the thermometers is allowed for as uncertainty component in the
uncertainty budget (rectangular distribution).
Temperature gradients in temperature-stabilized baths or furnaces can be reduced by provid-
ing a metallic compensation block with boreholes to accommodate the standards and calibra-
tion items.
For the calibration in defined fixed points of the applicable temperature scale, the preparation
of the fixed point cells must take place in accordance with the “Supplementary Information
for the International Temperature Scale of 1990”.
The calibration of a thermometer takes place after both the thermostat and the thermometer
itself have reached thermal equilibrium.
The number of calibration temperatures is to be agreed between customer and calibration
laboratory. For the determination of characteristic curves, refer to the DKD Guideline “De-
termination of Characteristic Curves” (DKD-R 5-6).
8 Influencing factors
The measurement uncertainty in the calibration of a thermometer is determined by different
influencing factors. These are not only the measurement uncertainty in the realization of the
temperature but also influences emanating from the calibration item itself. They can in part
amount to many times the measurement uncertainty in the temperature realization (accredited
measurement uncertainty of the calibration laboratory). In the following, these influencing
factors will be described in detail.
In the measurement of the electrical resistance, effects influencing the measurement result
must be allowed for and, if need be, taken into account when determining the measurement
uncertainty. The resistance measurement is made either with a constant alternating or a (vary-
ing) direct current. Kind and choice of the measuring instruments depend on the measurement
uncertainty aimed at for the calibration.
In the case of thermistors, an asymmetry effect can arise which is dependent on the direction
the current flows through the sensor element.
In the two-wire circuit the connection between sensor element and measuring instrument is
ensured by a two wire cable. As all other electrical conductors, this too has a resistance which
is connected in series with the sensor element. The two resistances thus add leading to a tem-
perature indication which is systematically higher. This is reflected in the calibration value
but it is omitted from consideration that during use the electrical resistance of the lead also
varies due to external temperature influences. If the thermometer to be calibrated is provided
with a lead, the user must allow for additional measurement deviations which depend on the
temperature of the lead.
The calibration certificate also states the temperature of the lead during calibration.
Example:
Platinum resistance thermometer Pt-100 with 2,5 m lead (copper, cross section:
0,25 mm2)
Resistance of lead at room temperature: 410 mΩ
If the lead has a temperature of 70 °C, the loop resistance of the lead rises to
492 mΩ.
This corresponds to a temperature indication higher by +0,2 K.
As the measuring instruments employed for the calibration operate, however, in the four-wire
technique, the loop resistance must be measured separately and be compensated by computa-
tion.
Example:
Resistance thermometer Pt-100
Measurement current: 1 mA
Thermovoltage: 25 µV
U 25 µV
Resulting offset from thermovoltage: =R= = 25 mΩ
I 1 mA
This corresponds to a temperature value of 0,063 K.
8.4.5 Self-heating
For the determination of the electrical resistance, an electrical measurement must be carried
out for which a measurement current must be fed through the sensor. The measurement cur-
rent leads to the sensor being heated (self-heating) and thus to the measurement result being
falsified. This effect is dependent not only on the magnitude of the measurement current but
also on the measurement conditions themselves. In the calibration, the self-heating mechanism
is to be investigated or a measurement current is to be chosen at which this effect is negligi-
ble.
Should this not be possible, the calibration value is to be extrapolated to I = 0 A by calibration
at different measurement currents.
8.4.8 Hysteresis
For accurate measurements it is further to be borne in mind that many thermometers (includ-
ing platinum resistance thermometers) show a hysteresis effect, i.e. the relation between tem-
perature and resistance is dependent on the previous history of the thermometer. This effect
arises, for example, if platinum is closely bonded with a ceramic carrier and the difference in
thermal expansion leads to mechanical stresses. For IPRTs this can result in a difference in the
indication of up to 0,5 K according to whether the thermometer was used before at higher or
at lower temperatures.
9 Recalibration
For measurements with the thermometer, the statements in a calibration certificate are not
valid for an unlimited time. The various influences acting on a thermometer during its use
lead to changes; the thermometer drifts. The influencing factors are:
• thermal load during the measurement
o temperature value
o period of use
o fast temperature changes
• mechanical stress
o vibration
o shock
• chemical influences
o diffusion of foreign matter into the resistor material
o structural changes in the resistor material
To get an idea of the changes, it is indispensable to recalibrate the thermometer at certain inter-
vals of time. The calibration periods cannot be laid down in the calibration certificate as they
depend very strongly on the required measurement uncertainty and the load during operation. So
the user is compelled to define the calibration periods himself according to the load during use.
The data from the successive calibrations in the same temperature range then allow a history
to be established for the thermometer. The drift values determined from the previous calibra-
tions are used for further evaluation. The user can himself adjust the recalibration periods to
the specific requirements placed on the measurement uncertainty and the history.
Example: A Pt-100 resistance thermometer has been calibrated four times on the whole at the
triple point of water. After the first calibration a drift has taken place during use, then the val-
ues are confirmed by the recalibrations, so that the recalibration period can, for example, be
doubled.
0,07
0,06
0,05
indication at TPW / K
0,04
0,03
0,02
0,01
0
1. calibration 2. calibration 3. calibration 4. calibration
10 Results
As a result of the calibration, a calibration certificate is issued.
The calibration certificate must meet the requirement of the publication DKD-5 “Instructions
for Issuing a DKD Calibration Certificate”. Within the scope of this Guideline, the following
is to be referred to:
(e) reference to the specifications or procedures applied.
It is recommended to describe the calibration procedure in detail.
(h) the measurement results and the associated measurement uncertainties or a statement on
the conformity with an established metrological specification.
It is recommended to state both the measurement results and the characteristic curve cal-
culated from them, together with the assigned measurement uncertainties.
(o) if an instrument to be calibrated was adjusted or calibrated, any calibration results avail-
able for the time before and after the adjustment or repair must be stated.
This is valid also for direct-indicating thermometers in particular.
δRR correction due to the measurement uncertainty in the calibration of the standard resis-
tor: The relative measurement uncertainty of the standard resistor is given in the cali-
bration certificate as 3 ⋅ 10-6 (k = 2). For an actual resistance of the SPRT of approx.
43 Ω, this corresponds to an uncertainty of 0,13 mΩ (k = 2) and to a standard uncer-
tainty of 0,07 mΩ. Experience has shown that the drift of the resistor since the last
calibration can be neglected.
δtBr correction due to the measurement uncertainty of the resistance measuring bridge. For
the measurement range used, the calibration certificate states an expanded uncertainty
(k = 2) of 3 mK. The indication of the bridge shows six digits but at the interface to the
data acquisition seven digits are available over which temporal averaging is carried
out. So measurement uncertainties due to the limited resolution can be neglected in
contrast to the other contributions to the measurement uncertainty.
δtWaN correction due to a possible heat conduction by the SPRT: Pulling the SPRT 20 mm
out of the bath led to a temperature change of 2 mK (which due to the temperature
variations of the bath could be estimated only inaccurately). From this a standard un-
certainty of 2 mK / √3 = 1,2 mK follows.
δtEWN correction for self-heating of the SPRT: The calibration certificate states that a meas-
urement current of 1 mA in a water triple point cell has led to a heating of 2.1 mK.
This contribution is neglected in the following as the thermometer is both calibrated
and used now at a measurement current of 1 mA.
δtWAP correction due to a possible heat conduction by the calibration item: Pulling the cali-
bration item 20 mm out of the bath led to a temperature change of 1 mK (which due to
the temperature variations of the bath could be estimated only inaccurately), measured
with the resistance bridge. This contribution is neglected. In part of the examples, it
would not have been possible to detect any effect due to the low resolution of the cali-
bration items.
tHom correction due to inhomogeneities in the thermostat: It is known from previous inves-
tigations that the temperature difference between calibration item and standard ther-
mometers due to inhomogeneities in the bath can amount to ±8 mK at most. From this a
standard uncertainty of 8 mK / √3 = 4,6 mK follows.
δtStab correction due to temporal instabilities in the bath: It is known from previous investi-
gations that the temperature difference between calibration item and standard ther-
mometers due to temporal instabilities in the bath can amount to ±6 mK at most. From
this a standard uncertainty of 6 mK / √3 = 3,5 mK follows.
Compared with these contributions, further influences such as, for example, the short-time
stability of the measuring instruments during measurement can be neglected.
The individual contributions to the uncertainty of the temperature of the calibration item are
summarized in Table A.1.
δRBr correction due to the measurement uncertainty in the calibration of the resistance
measuring bridge: The relative uncertainty of the resistance measuring bridge is given
in the calibration certificate with 3⋅10-6 (k = 2), from which a standard uncertainty of
0,15 mΩ (related to the standard resistor) results. The indication of the bridge shows
six digits but at the interface to the data acquisition seven digits are available over
which temporal averaging is carried out. Compared to the other contributions to the
measurement uncertainty, measurement uncertainties due to the limited resolution can
therefore be neglected.
δRPar correction due to parasitic thermovoltages: The influence of parasitic thermovoltages
can be neglected if the measurements are carried out with an AC bridge. If the resis-
tance thermometer is intended to be operated with a DC measuring instrument, the de-
termination of measurement errors due to parasitic thermovoltages requires supple-
mentary measurements (upon agreement with the customer).
δT correction due to the uncertainty of the temperature of the calibration item: In Table
A.1 it is stated that the standard uncertainty assigned to the temperature of the calibra-
tion item is 10,3 mK.
These contributions are summarized in Table A.2.
1
The case is not a normal one when the probability distribution is such that a coverage probability of 95% cannot be
achieved with a coverage factor of k = 2. The above note is then to be modified stating the value of the coverage
factor. More detailed explanations are given in DKD-3 or can be obtained from the DKD Accreditation Body.
1
The case is not a normal one when the probability distribution is such that a coverage probability of 95% cannot be
achieved with a coverage factor of k = 2. The above note is then to be modified stating the value of the coverage
factor. More detailed explanations are given in DKD-3 or can be obtained from the DKD Accreditation Body.
tx temperature of the thermometer: According to Table A.1, the temperature of the ther-
mometer is 180,234 °C with a standard uncertainty of 10,3 mK.
A(tx) reading of the thermometer: The thermometer displays a temperature of 180,25 °C.
During a measurement time of 5 min, this temperature was constantly indicated; the
statistical variation thus can be neglected within the resolution.
δtAuf correction due to the limited resolution of the thermometer: At a resolution of 10 mK,
the reading is possible only within ±5 mK. From this a standard uncertainty of 5 mK / √3
= 2,9 mK follows.
These contributions are summarized in Table A.4.
Quantity Brief description Estimate Standard Distribution Sensitivity Uncertainty
uncertainty coefficient contribution
tx Temperature - 180,234 °C 10,3 mK normal 1 10,3 mK
thermometer
A(tx) Reading 180,25 °C 0 mK normal 1 0 mK
δtAuf Resolution 0K 2,9 mK rectangular 1 2,9 mK
K(tx) Correction ─16 mK 10,7 mK
K(tx) k=2 21 mK
1
The case is not a normal one when the probability distribution is such that a coverage probability of 95% cannot be
achieved with a coverage factor of k = 2. The above note is then to be modified stating the value of the coverage
factor. More detailed explanations are given in DKD-3 or can be obtained from the DKD Accreditation Body.
1
The case is not a normal one when the probability distribution is such that a coverage probability of 95% cannot be
achieved with a coverage factor of k = 2. The above note is then to be modified stating the value of the coverage
factor. More detailed explanations are given in DKD-3 or can be obtained from the DKD Accreditation Body.
The above examples A.1 to A.4 relate to the calibration of a thermometer at one temperature
only. Usually, a thermometer is calibrated at several temperatures (temperature points) for
which, as a rule, different measurement uncertainties result. As the user also employs the
thermometer to carry out temperature measurements between the calibration points, it is, how-
ever, helpful if the calibration certificate also contains statements on the use of the thermome-
ter in the whole temperature range. This is frequently achieved by giving a characteristic
curve (see DKD-R 5-6) whose uncertainty is naturally greater than that of a calibration in one
point.
At the customer's, the thermometer is possibly used under conditions which are different from
those under which the calibration was carried out. So contributions to the measurement uncer-
tainty might dominate which could remain unaccounted for in the calibration. The measure-
ment uncertainty in use can therefore considerably exceed the measurement uncertainty in
calibration. The essential factors influencing the measurement uncertainty when resistance
thermometers are used are summarized in Table B.1.
Maximum contribution to
Influence quantity Evaluation
measurement uncertainty
Up to more than 10 % of the
Temperature difference Different immersion
temperature difference
between object measured depths, flow velocities,
between object measured and
and thermometer coupling, positions, …
environment
Recording of measure-
ments, check using Up to the amount of the tem-
Temporal instabilities
thermometers with a perature variations
different time constant
Investigation of the
dependence of the previous
Hysteresis of the thermometer Up to 0,5 K
history on the measurement
result
Calculation of the line
Resistance of the leads Up to some K
resistance
Parasitic thermovoltages Reversal Up to 0,2 K for Pt-100
Drift of the thermometer, Check at fixed points
Up to 0,5 K
long-time stability (ice point)
Electronic evaluation unit
(for direct-indicating Data sheet Up to 0,5 K
thermometers)
Table B.1: Factors influencing the uncertainty in measurements using resistance thermometers