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THERMOMETERS, CONTACT, DIRECT READING: CALIBRATION

Key words: Calibration, test method, thermometers

UDC 536.5:53.088

CONTENTS
1. 2. 3. 4. 5. 6. 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 1 1 1 2 2 2 2 2 2 2 3 4 4 4 4 5 5 5 5 5 5 6 7

1.

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.

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4.

DEFINITIONS

6.
6.1

METHOD OF TEST PRINCIPLE

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.

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
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. 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.

6.2
6.2.1

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.

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 difference to be insignificant for the given purpose. 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.

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.
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

Above 1300C, 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 sufficient accuracy and stability are convenient due to their ease of use.

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.

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.

5.

SAMPLING

Not applicable.

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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

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

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. 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.

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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].

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

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.

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).

6.2.2.3

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.

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.

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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. If adjustments are ordered, the user must decide whether the thermometer should also be calibrated before the adjustment is carried out. 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.

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.

Temp.

T
R X1
X2

6.4
6.4.1

PROCEDURE
Selection of calibration temperatures

R'

X2'

X1'

R"

Time

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.

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 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.

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

b) Reading tr(C)
tr is the reading of the thermometer. It is calculated as the mean of the 2 readings Xi and Xi'.

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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.

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.

Example

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.

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Cornponent

Value
C

Factor

1 sigma

value
C
2

uncertainty is strongly related to this component and is estimated to be included in it. The temperature gradients in the thermostat have a limit of 0.005C with a rectangular distribution.

a) Ref. therm. calibration

0.02
0.01

0.01 0.006

b) Reading uncertainty of reference thermometer

Drift of ref.therm. c) Thermostat instability Thermostat gradients d) Reading of thermometer to be calibrated Root of sum of squares

1.73 1.73 1.41 1.73 1.73

d) The resolution of the thermometer to be calibrated is 0.1C with a rectangular distribution.

0.02
0.01 0.005 0.01

0.012

0.007
0.003

6.7

TEST REPORT

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

0.058
st= 0.060
~~~

Then the uncertainty is calculated as

ut = 2 * st = 0.12C
The uncertainty components were found as follows: 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. 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

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. e) Number of pages comprising the certificate. 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 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.