Calibration ISO IEC 17025 Annex Temperature Metrology
Calibration ISO IEC 17025 Annex Temperature Metrology
Temperature metrology
May 2022
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Specific Accreditation Criteria: ISO/IEC 17025 Application Document, Calibration - Annex, Temperature
metrology
Table of Contents
Purpose 4
Criteria and recommendations for all types of measurement equipment 4
Criteria and recommendations for specific types of measurement equipment 5
Apparatus for fire tests .............................................................................................. 5
Automatic reference junctions ................................................................................... 5
Calibration baths and furnaces .................................................................................. 5
Dry block calibrators .................................................................................................. 5
Dry block heaters ...................................................................................................... 6
Conduction errors ...................................................................................................... 6
Environmental enclosures (e.g. environmental chambers, conditioning rooms,
calorimeter rooms) .................................................................................................... 7
Ovens and furnaces .................................................................................................. 7
Autoclaves................................................................................................................. 7
Thermocyclers ........................................................................................................... 8
All thermometers ....................................................................................................... 9
Liquid-in-glass thermometers .................................................................................... 9
Platinum resistance thermometers .......................................................................... 10
Vapour pressure thermometers ............................................................................... 10
Thermocouples ....................................................................................................... 10
Digital temperature indicators .................................................................................. 11
Radiation thermometers (e.g. pyrometers) .............................................................. 11
Surface probes and calibrators ............................................................................... 11
Humidity .................................................................................................................. 12
Electrical calibration of temperature indicators, such as digital multimeters and digital
temperature indicators............................................................................................. 13
References 14
Amendment Table 15
Temperature Metrology
Purpose
In addition to the ISO/IEC 17025 Standard Application Document (SAD) and the
accompanying Calibration - Appendix, this document provides interpretative criteria
and recommendations for temperature metrology for both applicant and accredited
facilities.
Facilities must comply with all relevant documents in the NATA Accreditation Criteria
(NAC) package for Calibration (refer to NATA Procedures for Accreditation).
For ease of use and to avoid fragmentation of the information, the relevant clause
numbers of ISO/IEC 17025 have not been included.
Conduction errors
When calibrating probe thermometers, the error due to heat conduction along the
probes must be taken into account in the uncertainty. An immersion sensitivity test
may be performed to check for this effect. Conduction errors for probes immersed
more than 200 mm into a fluid bath or 250 mm into a tube-furnace can generally be
assumed to be negligible, and the corresponding enclosure uniformity value alone
used as the transfer error. Probes calibrated in dry-well calibrator or immersed less
than this must have an immersion test performed on each DUT. This consists of
observing the temperature change when the probe is withdrawn a further 20 mm.
This test should be performed at the extreme temperature (Tmax or Tmin of the bath or
furnace) or at a minimum, the extremes of application and propagated proportionally
to (T-Tamb).
Autoclaves
The homogeneity of the thermocouples feeding through to the chamber should be
checked at regular intervals as this is usually also the EMF generating temperature
gradient zone. This can be achieved by placing thermocouple tips in an ice-point,
heating the feed-through with a hot air gun and confirming that changes are
negligible.
Thermocyclers
PCR thermocyclers use a variety of technologies to achieve rapid heating and
cooling sequences across a number of tubes. The accuracy of temperature and hold
time, the magnitude of overshoots and undershoots, the uniformity of temperature,
and heating and cooling rates across the thermal block are critical aspects to the
performance verification of thermocyclers.
Due to the dynamic performance of thermocyclers, they must be verified in a
dynamic way. It must be ensured that the reference equipment used for the
calibration of thermocyclers has suitable evidence of metrological traceability and is
fit for purpose. The following must be taken into account::
each sensor is to have a temperature uncertainty no greater than 1/5th of the
uncertainty of calibration required for the thermocycler under test;
the dynamic response time of the temperature sensors must be suitably rapid
to measure the rise and fall time as well as set point over/undershoot. This
can be assessed by exposing the sensor to a typical step change in
temperature e.g. by quickly withdrawing the sensor to ambient air from a
temperature of 50 °C or above, or vice versa. The response time to measure
63% of the step change should be below 2 seconds;
simultaneous (or near simultaneous) and continuous logging of multiple well
temperatures at each measurement site during the test interval (where the
test interval is one complete cycle of the thermocycler). The sensor
sampling/logging frequency must be 1 Hz or more. The time accuracy of the
logging system must be better than 1 in 105;
the resolution is appropriate for use, e.g. 0.01°C.
A thermocycler calibration system will thermally load the thermocycler in terms of
thermal mass and thermal conductivity (heat leaks) differently to a set of PCR
samples. Consequently different calibration equipment may lead to different results
for the same thermocycler. The facility must consider:
the magnitude of systematic error due to the combination of the calibration
system and the thermocycler;
assessment of the systematic effects of loading by the calibration system
must be undertaken. This may be performed by comparing the calibration
results from the calibration system to that of a basic method with known small
uncertainties. For example, a 0.1 mm diameter calibrated thermocouple wire
placed into a sample tube containing a drop of oil. An error of less than 1/5th
of the uncertainty of calibration required for the thermocycler under test is
considered acceptable. This term would be included in the reported
uncertainty of measurement.
Thermocyclers often have a heated lid preventing condensation and evaporation.
Opening the heated lid can influence the calibration results therefore, when possible,
calibrations should be performed with the lid closed to replicate in-use conditions.
Temperature uniformity must be reported across the thermal block and as such the
number of sensors be selected proportionate to the number of wells with
consideration to the size of the block. The number of sensors should be at least
12.5% of the number of wells for thermocyclers with up to 96 wells, subject to a
minimum of 5 sensors for thermocyclers with 8 or more wells, and a minimum of 12
sensors for thermocyclers with more than 96 wells. Sensors must be placed in the
four corner positions and spatially and evenly distributed over the middle and edges
of the block.
The report must state if the calibration was performed with the heated lid opened or
closed and if closed during calibration, report the heated lid temperature. If during
calibration the lid is open, the report must indicate that temperatures reported may
be different to that during normal use with the lid closed.
In order to suitably verify the performance of a thermocycler the following items
should be reported pending the application and requirements of the thermocycler:
the mean block temperature measured after a 15s to 30s stabilisation period
and the temperature correction to the indicated temperatures at the lowest
and highest temperature settings, a low- to mid-range setting and a mid- to
high range setting to match the in-use temperature range. For example,
15°C, 55°C, 72°C and 95°C may suit most users or 4°C, 55°C, 72°C and 98°C
if the customer intends to use the device at the cycler’s full range;
the stabilisation period;
the temperature heating and cooling rates and set point overshoot/undershoot
for each sensor which may be stated in a graphical form during a typical cycle;
the maximum overshoot and undershoot at each measurement point;
time at temperature after overshoot/undershoot for each temperature set;
temperature uniformity across the thermal block.
All thermometers
The report must state whether the reported uncertainty includes a component for
linearity/interpolation error, or is valid only at the reported calibration points.
The report must state any annealing procedure applied to the thermometers prior to
calibration.
Liquid-in-glass thermometers
Temporary depression must be measured by measuring the correction at a
reference temperature (usually the ice-point) before and after exposure to
temperatures away from ambient and any shift included as a component in the
uncertainty calculations.
If the thermometer is for >0°C usage and the ice-point mark is not provided on the
scale, the reference temperature should be the lowest cardinal temperature.
Thermocouples
It is important to note that the EMF in a thermocouple is produced in a temperature
gradient and not at the thermocouple tip and thus the effects of inhomogeneity must
be considered along with the following:
thermocouple reports must state the EMF-to-T reference function used (e.g.
ASTM…);
the inhomogeneity of a thermocouple must be included as a component in the
uncertainty calculations, For new thermocouples a default value of 0.1% for
base metal and 0.02% for rare-metal thermocouples should be used, For used
thermocouples it must be measured, for example, by measuring the correction
over a range of at least 100 mm in immersion depths;
the inhomogeneity uncertainty component can be propagated proportionally to
temperature;
because base metal thermocouples can experience significant drift during
calibration, the calibration procedure for base metal thermocouples must
require measurements over at least a ½ hour period at mid and highest
temperature of calibration and the variation obtained included as an additional
uncertainty component (drift);
ceramic or fibreglass insulated base metal wire test method must specify that
air can circulate freely to ensure binder vapours do not contaminate the
thermoelements;
for MIMS thermocouples with a head, where a junction involves different
wires, the calibration procedure must estimate any error due to different wires
in the MIMS and extension leads (e.g. by putting the sensor in an ice-point
and noting any change when the head is warmed or cooled);
for the calibration of reels of thermocouple wire, inhomogeneity in the reel
must be evaluated. The estimated inhomogeneity may need to be revised if
the measured variation between samples is significantly different to that
estimated (could be lower or higher). In this case additional homogeneity
measurements may be required.
For calibration of surface probes, the report must identify the surface used for the
calibration and the nature of the ambient air flow (e.g. “calibrated on a polished
aluminium plate in still air”).
Humidity
The CMC in the Scope of Accreditation will include the temperature (range) to which
the humidity is reported with corresponding uncertainty of measurement across
humidity range and temperature range.
Users of humidity measuring equipment must ensure the temperature component is
calibrated to suit the intended use.
The unit to be used for values of relative humidity expressed as a percentage is
“%rh”. The term Relative Humidity may be abbreviated to RH.
Hysteresis is the maximum difference in sensor response when exposed to the same
reference humidity/temperature condition following recent exposure to a higher or
lower humidity at the same temperature. It is recommended to calibrate impedance-
type humidity sensors over the range of use and not wider, as the largest hysteresis
loops are experienced when the sensor is exposed to the widest range of relative
humidities, especially to levels of humidity above 70 %rh.
When calibrating an impedance-type humidity sensor over a wide range, evaluation
of the hysteresis may be made by repeating measurements at mid-range humidity
between 35 %rh and 65 %rh, before and after each low and high humidity excursion.
Appropriate soak time between measurement points must be considered, taking into
account the manufacturer’s recommendations on the use of the device. This
evaluation of the hysteresis can be considered as a short-term drift contribution to
the uncertainty calculation. The report must include a statement that the uncertainty
includes a component for the effect of hysteresis.
When evaluating the hysteresis characteristic, consideration should be given to the
calibration temperature demonstrating the largest effect; typically this would be the
highest calibration temperature. If the evaluation of hysteresis can not be performed,
a value of 0.3 %rh to 1 %rh is considered appropriate for a sensor soaked at 70 %rh
to 95 %rh, and 0.2 %rh if the highest humidity is below 70 %rh.
A minimum of three humidity calibration points spanning the customer’s humidity
range of use is recommended to be conducted during a hygrometer calibration.
The recommended reference equation for the calculation of vapour pressures above
water and ice, used in the calculation of relative humidity, is the saturation vapour
pressure formulation given by Sonntag. The formula and coefficients can be found in
the Appendix of NMI Monograph 8: Humidity and its Measurement.
Aqueous salt solutions may be used for the calibration of humidity sensors, using a
calibrated reference hygrometer for traceability. The device containing the solution
used for maintaining a stable humidity environment (hygrostat), must be operated in
a tightly temperature-controlled environment with no draughts and no direct sunlight,
and in accordance with the manufacturer’s recommendations on the use of the
device. Sufficient time must be allowed for the sensors, air and solution within the
measuring space of the hygrostat to reach temperature equilibrium. As aqueous salt
solutions are very sensitive to ambient humidity leaks, an air-tight seal is required.
The report must state the temperature range for which the humidity range is valid.
References
This section lists publications referenced in this document. The year of publication is
not included as it is expected that only current versions of the references shall be
used.
Standards
AS 1530.1 Methods for fire tests on building materials, components and
structures - Combustibility test for materials
AS 1530.3 Methods for fire tests on building materials, components and
structures - Simultaneous determination of ignitability, flame
propagation, heat release and smoke release
AS 1530.4 Methods for fire tests on building materials, components and
structures - Fire-resistance test of elements of construction
AS 3864.2 Medical refrigeration equipment - For the storage of blood and
blood products - User-related requirements for care,
maintenance, performance verification and calibration
IEC 60068.3.5 Environmental testing - Supporting documentation and
guidance - Confirmation of the performance of temperature
chambers
IEC 60068.3.6 Environmental testing - Supporting documentation and
guidance - Confirmation of the performance of
temperature/humidity chambers
ISO/IEC 17025 General requirements for the competence of testing and
calibration laboratories
NATA Publications
NATA Accreditation Criteria (NAC) package for Calibration
General Accreditation Criteria ISO/IEC 17025 Standard Application Document
Specific Accreditation Criteria ISO/IEC 17025 Standard Application Document,
Calibration - Appendix
Other Publications
EURAMET cg-13 Calibration Guide, Calibration of Temperature Block Calibrators
EURAMET cg-20 Calibration Guide, Calibration of Temperature and/or Humidity
Controlled Enclosures
NMI Monograph 1 Uncertainty in Measurement: The ISO Guide, RE Bentley
NMI Monograph 8 Humidity and its Measurement
Amendment Table
The table below provides a summary of changes made to the document with this
issue.