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First edition
2020-10

ISO 21736:2020(E)
ISO

Reference number

© ISO 2020
21736

Matériaux réfractaires — Méthodes d'essai de la résistance aux chocs

Refractories — Test methods for
thermal shock resistance
INTERNATIONAL
STANDARD

thermiques
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ISO 21736:2020(E)


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Contents Page

Foreword......................................................................................................................................................................................................................................... iv
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Method 1: water quenching....................................................................................................................................................................... 2
4.1 General............................................................................................................................................................................................................ 2
4.2 Principle......................................................................................................................................................................................................... 2
4.3 Equipment.................................................................................................................................................................................................... 2
4.3.1 Experimental furnace................................................................................................................................................... 2
4.3.2 Cooling water channel.................................................................................................................................................. 2
4.3.3 Test piece clamp................................................................................................................................................................ 2
4.3.4 Drying oven........................................................................................................................................................................... 2
4.3.5 Grid, mesh size of 5 mm × 5 mm......................................................................................................................... 2
4.4 Test pieces.................................................................................................................................................................................................... 2
4.4.1 Sampling.................................................................................................................................................................................. 2
4.4.2 Shape, dimensions and preparation of test pieces.............................................................................. 2
4.5 Test procedure.......................................................................................................................................................................................... 4
4.5.1 Heating...................................................................................................................................................................................... 4
4.5.2 Cooling....................................................................................................................................................................................... 5
4.6 Results expression................................................................................................................................................................................ 5
5 Method 2: compressed air quenching............................................................................................................................................. 5
5.1 General............................................................................................................................................................................................................ 5
5.2 Principle......................................................................................................................................................................................................... 6
5.3 Equipment.................................................................................................................................................................................................... 6
5.4 Test pieces.................................................................................................................................................................................................... 6
5.4.1 Sampling.................................................................................................................................................................................. 6

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5.4.2 Shape, dimensions and preparation of test pieces.............................................................................. 6
5.5 Test procedure.......................................................................................................................................................................................... 7
5.5.1 Heating...................................................................................................................................................................................... 7
5.5.2 Cooling....................................................................................................................................................................................... 7
5.5.3 Determination..................................................................................................................................................................... 7
5.6 Results expression................................................................................................................................................................................ 7
6 Method 3: air quenching............................................................................................................................................................................... 8
6.1 General............................................................................................................................................................................................................ 8
6.2 Principle......................................................................................................................................................................................................... 8
6.3 Equipment.................................................................................................................................................................................................... 8
6.4 Test pieces.................................................................................................................................................................................................... 9
6.4.1 Sampling.................................................................................................................................................................................. 9
6.4.2 Shape, dimensions and preparation of test pieces.............................................................................. 9
6.5 Test procedures....................................................................................................................................................................................... 9
6.5.1 Heating...................................................................................................................................................................................... 9
6.5.2 Cooling....................................................................................................................................................................................... 9
6.5.3 Results expression........................................................................................................................................................... 9
7 Test report................................................................................................................................................................................................................. 10
Annex A (informative) Precision data of thermal shock resistance tests....................................................................11

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Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www​.iso​.org/​directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www​.iso​.org/​patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see
www​.iso​.org/​iso/​foreword​.html.
This document was prepared by Technical Committee ISO/TC 33, Refractories.
Any feedback or questions on this document should be directed to the user’s national standards body. A

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complete listing of these bodies can be found at www​.iso​.org/​members​.html.

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INTERNATIONAL STANDARD ISO 21736:2020(E)

Refractories — Test methods for thermal shock resistance

1 Scope
This document specifies the principle, equipment, test pieces, procedures, result expression and test
report of test methods for thermal shock resistance of refractories.
Three test methods are included in this document. Each one is applicable to a different product type
and their test results are not comparable.
The test method, the test temperature and the test condition are intended to be negotiated by
corresponding parties.
This document does not purport to address all of the safety concerns, if any, associated with its use. It
is the responsibility of the user to establish appropriate safety and health practices and determine the
applicability of regulatory limitations prior to use.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 836, Terminology for refractories
ISO 1927-2, Monolithic (unshaped) refractory products — Part 2: Sampling for testing
ISO 1927-5, Monolithic (unshaped) refractory products — Part 5: Preparation and treatment of test pieces

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ISO  5014, Dense and insulating shaped refractory products — Determination of modulus of rupture at
ambient temperature
ISO 5022, Shaped refractory products — Sampling and acceptance testing

3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 836 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://​w ww​.iso​.org/​obp
— IEC Electropedia: available at http://​w ww​.electropedia​.org/​
3.1
water quenching
rapid quenching of the fast-heated test pieces in flowing water of 5 °C to 35 °C
3.2
compressed air quenching
rapid quenching of the fast-heated test pieces in 0,1 MPa compressed air of ambient temperature
3.3
air quenching
quenching of the fast-heated test pieces in natural air of ambient temperature

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4 Method 1: water quenching

4.1 General
Method 1 (water quenching) is applicable to dense aluminium silicate refractory products, but not
to basic refractory products, silica refractory products, fused cast refractory products, refractory
products with apparent porosity higher than 45 % or the refractories whose thermal shock resistance
is hard to evaluate for low thermal shock cycles or reactions with water.

4.2 Principle
In the conditions of the specified testing temperature and water medium, the test piece with the
specified shape and dimensions suffers thermal shocks. The damage degree of the hot end surface of
the test piece is adopted to describe the thermal shock resistance of the refractories.

4.3 Equipment

4.3.1 Experimental furnace

Use an electric furnace whose temperature can be controlled in accordance with the specifications
in 4.5. The temperature distribution of the test pieces loading area shall be uniform to ensure the
temperature difference between two random points on the hot end surface is not higher than 10 °C. The
uniform temperature zone shall be able to hold at least three test pieces simultaneously. One end of the
thermocouple for temperature determination shall be sealed and 20 mm ± 5 mm away from the hot end
surface of the test pieces. Meanwhile, the temperature record and display devices shall be equipped to
control, record and display the furnace temperature continuously. A diagram of the heating device is
shown in Figures 1 and 2.

4.3.2 Cooling water channel

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The channel shall be able to hold multiple test pieces for rapid quenching simultaneously and ensure
the inflow and outflow water temperature rise is not higher than 10 °C. A diagram of the cooling device
is shown in Figures 3 and 4.

4.3.3 Test piece clamp

The clamp is used to fix test pieces for heating or cooling.

4.3.4 Drying oven

The drying oven shall be able to control the test temperature at 110 °C ± 5 °C.

4.3.5 Grid, mesh size of 5 mm × 5 mm

The grid is used to determine the hot end area of test pieces [114 mm × 64 (74) mm] in grid number.

4.4 Test pieces

4.4.1 Sampling

Sampling of shaped refractory products and monolithic refractories shall be conducted in accordance
with ISO 5022 and ISO 1927-2, respectively, or negotiated by corresponding parties.

4.4.2 Shape, dimensions and preparation of test pieces

Standard bricks with dimensions of 230 mm × 114 mm × 64 (74) mm shall be adopted for testing.

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For oversized bricks, test pieces with these dimensions shall be cut from the original bricks. One test
piece for one brick only. If the test pieces of the specified dimensions cannot be obtained, the other
dimensions can be negotiated by corresponding parties.
Test piece preparation of monolithic refractories shall be conducted in accordance with ISO 1927-5.

Key
1 furnace body
2 heating element
3 thermocouple
4 test pieces
5 heat insulation material

Figure 1 — Side view of heating device

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Key
1 furnace body
2 heat insulation material
3 thermocouple
4 test pieces

Figure 2 — Planform for heating device

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Key
1 test piece
2 water channel
3 water intake
4 water outlet
5 water surface
6 direction of water flow

Figure 3 — Side view of cooling device

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Figure 4 — Elevation view of cooling device

4.5 Test procedure

4.5.1 Heating

Dry the test pieces in an electric desiccator at 110 °C ± 5 °C to a constant mass. Clamp the test pieces
with the test piece clamp at intervals no smaller than 10  mm; overlapping is not permitted. Ensure
that a section with a length of 50 mm from each test piece can suffer the thermal shock. Fill the space
between the clamped parts of test pieces with the insulating materials thicker than 10 mm. Measure
the area of the hot end surface [114 mm × 64 (74) mm] of the test pieces in grid number A1 with a grid
and record.
Preheat the furnace to the test temperature ± 10 °C and hold for 15 min. Transfer the test pieces into the
hearth rapidly. The hot end surface of the test pieces shall be ≥ 50 mm away from the heating element
surface. Fill the space between the test pieces and the furnace door with the insulating materials in time.

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ISO 21736:2020(E)


The test temperatures shall be negotiated by the corresponding parties and marked in the test report;
the recommended test temperature is 1 100 °C.
After the test pieces are put into the furnace, the furnace temperature drop shall be ≤ 50 °C, and it shall
return to the test temperature within 5 min. The test pieces shall be held at the test temperature for
20 min after regaining temperature.

4.5.2 Cooling

After rapid heating, take out the test pieces and immerse the hot end of the test pieces 50 mm ± 5 mm
deep in the flowing water of 5  °C to 35  °C. The immersed test piece end shall be  ≥  20  mm from the
water channel bottom. The temperature rise between inflow water and outflow water shall be ≤ 10 °C
by adjusting the water flow rate. During quenching, close the furnace door in time to keep the furnace
temperature at the test temperature ± 10 °C.
After water quenching for 3 min in the channel, take out the test pieces rapidly and leave the test pieces
in air for ≥ 5 min. Measure the undamaged area of the hot end surface [114 mm × 64 (74) mm] of the test
pieces in grid number A2 and record.
When the test pieces are left in air for  ≥  5  min and the furnace temperature returns to the test
temperature, transfer the hot end of the test pieces into the furnace rapidly. Repeat these procedures
until (50 ± 5) % of the hot end surface is damaged. Record the thermal shock cycle number or end the
test at the negotiated cycles.
During the test, the mechanical damage between the test pieces and the furnace door or the water
channel is not permitted.

4.6 Results expression

The thermal shock cycle in which half (or more) of the hot end surface of the test piece is damaged
during water quenching is regarded as the result of the thermal shock resistance test.

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The hot end surface damage rate of test pieces is calculated using the grid number of the hot end surface
A1 before the test and the grid number of the undamaged hot end surface A2 after the test according to
Formula (1).
A1 − A2
Ρ= ×100 % (1)
A1
where

  P is the hot end surface damage rate of the test piece, in %;

  A1 is the grid number of the hot end surface before the test;

  A2 is the grid number of the undamaged hot end surface after the test.
The damage rate shall be rounded to the nearest 1 %.
During water quenching, if half of the hot end surface is damaged this thermal shock cycle is valid.
If the test piece is damaged by external forces the test is invalid. In this case, retest.

5 Method 2: compressed air quenching

5.1 General
Method 2 (compressed air quenching) is applicable to basic refractory products, silica refractory
products, fused cast refractory products and the refractories whose thermal shock resistance is hard

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ISO 21736:2020(E)


to evaluate for their less thermal shock cycles or reactions with water. It is also applicable to dense
aluminium silicate refractory products. However, the thermal shock resistance tested by this method
is not the same or comparable to that tested by the water quenching method. It is not applicable to
refractory products with apparent porosity higher than 45 %.

5.2 Principle
In the conditions of the specified testing temperature and cooling medium, the test piece with the
specified shape and dimensions suffers thermal shocks. At the end of each thermal shock, a rupture
test with a certain bending stress (load) or a blowing burst test is conducted on the test piece. The
experienced thermal shock cycle of the test piece is adopted to describe the thermal shock resistance.

5.3 Equipment

5.3.1 Experimental furnace. Use an electric furnace whose temperature can be controlled in
accordance with the specifications in 5.5. The temperature distribution of the test piece loading area
shall be uniform to ensure the temperature difference between two random points on the hot end
surface is lower than 10 °C. The uniform temperature zone shall be able to hold at least three test pieces
simultaneously. One end of the thermocouple shall be sealed. Temperature record and display devices
shall be equipped to control, record and display the furnace temperature continuously.

5.3.2 Blowing device, with a nozzle of 8 mm diameter and 5 mm length.

5.3.3 A steel board (400  mm  ×  250  mm  ×  20  mm), with positional pins for test piece fixing. The
position of the pins shall be proper to let the nozzle target the centre of the test piece according to the
dimensions of the test piece.

5.3.4 Tester of cold modulus of rupture. The curvature radius of the contacts shall be 5 mm ± 0,5 mm.
The distance between the two lower contacts shall be 100 mm ± 1 mm. The other requirements shall be

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in accordance with the specifications of ISO 5014.

5.3.5 Insulating pincher to hold the heated test pieces.

5.3.6 Drying oven, from room temperature to 300 °C.

5.4 Test pieces

5.4.1 Sampling

Sampling of shaped refractory products and monolithic refractories shall be conducted in accordance
with ISO 5022 and ISO 1927-2, respectively, or negotiated by corresponding parties.

5.4.2 Shape, dimensions and preparation of test pieces

Rectangular test pieces with dimensions of (114 ± 3) mm × (64 ± 2) mm × (64 ± 2) mm shall be adopted.

The two surfaces along the length direction shall be parallel. The allowable deviation of the parallelism
between the tensed surface and the compressed surface shall not be larger than 0,5  mm and the
allowable deviation of the parallelism between the two opposite edges of the middle section shall not
be larger than 0,2 mm.
Cut one test piece from the working end of each brick. The working surface shall be the spraying and
tension surface of the test piece. If the working surface cannot be confirmed, the original surfaces
enduring the press during brick shaping shall be considered as the spraying and tension surface.
Meanwhile, the surface shall be well marked. Defects caused by sampling, such as cracks and hydration,
are not allowed. If they occur then resample.

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Test piece preparation of monolithic products shall be conducted in accordance with ISO 1927-5.

5.5 Test procedure

5.5.1 Heating

Dry the test pieces in a drying oven at 110 °C ± 5 °C to a constant mass. Put the dried test pieces into
an electric desiccator preheated to 250 °C to 300 °C and keep for at least 2 h. Preheat the furnace to
the test temperature ± 10 °C and keep for 15 min. Transfer the test pieces into the hearth quickly and
shut the door at once. The temperature drop of the furnace shall not exceed 50 °C. The temperature
shall resume to the test temperature ± 10 °C within 5 min of putting the first test piece into the hearth.
Keep this temperature for 30 min. The test pieces shall be placed on a long surface; overlapping is not
permitted. The intervals between test pieces and the hearth shall be ≥ 10 mm.
The test temperatures shall be negotiated by the corresponding parties and marked in the test report.
The recommended test temperature is 950 °C.

5.5.2 Cooling

Take the test pieces out and place them on a steel plate with positional pins. Make the nozzle face the
centre of the blast surface of the test piece. The nozzle shall be 100 mm ± 2 mm away from the blast
surface centre of the test piece. Blast for 5 min using the compressed air. The compressed air is dry and
ambient temperature. The pressure before the nozzle shall be kept at (0,1 ± 0,01) MPa. Always blast the
same surface.
If the test condition is the same as that in 5.5.1 and 5.5.2, several pieces can be tested simultaneously or
successively.

5.5.3 Determination

After 5 min rapid quenching by compressed air, remove the test piece. Conduct the three-point bending

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test using the blast surface as the tension surface. Load uniformly; the maximum bending stress shall
be (0,3 ± 0,01) MPa. If the test piece can endure the three-point bending test under (0,3 ± 0,01) MPa,
when the furnace temperature resumes to the test temperature, transfer the test piece to the furnace
quickly. Repeat these procedures until the test piece is damaged and cannot be used for the bending
stress test or the test piece fractures during three-point bending test. Record the thermal cycle number
or stop the test at the negotiated cycles.
The repeating thermal cycles shall be carried out continuously. If the test is interrupted, put the test
pieces in a 250 °C to 300 °C desiccator. Restart the test according to these procedures. Tests for silica
products are not allowed to be interrupted.
After the compressed air quenching, the time of the test pieces placed at ambient temperature is not
allowed to exceed 3 min, which includes the time for the bending stress test.
Damage by external forces shall be avoided during testing.

5.6 Results expression

The thermal shock resistance is represented by the thermal shock cycle endured by the test piece
before damage.
The thermal cycle in which the test piece fractures in the bending stress test or is damaged during air
quenching and cannot be used for the three-point bending test is valid.
The thermal cycle in which the test piece is damaged during fast heating and cannot be used for the
three-point bending test is invalid.
If the test piece is damaged by external forces, the testing is invalid. In this case retest.

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ISO 21736:2020(E)


6 Method 3: air quenching

6.1 General
Method 3 (air quenching) is applicable to the refractory products with apparent porosity higher
than 45 %.

6.2 Principle
In the conditions of the specified testing temperature and air medium, the mass of the test piece with
the specified shape and dimensions will change after thermal shocks. The mass loss rate is used to
judge the thermal shock resistance of the refractory products.

6.3 Equipment

6.3.1 Experiment furnace. Use an electric furnace whose temperature can be controlled in accordance
with the provisions in 6.5. Others refer to 5.3.1.

6.3.2 Manipulator or clamp, which shall be able to clamp the test pieces and put them on the
cooling rack.

6.3.3 Test piece cooling rack, which shall be a steel frame spread with parallel refractory bricks with
180 mm of spacing, as shown in Figure 5.

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Figure 5 — Test piece cooling rack

6.3.4 Drying oven, which can control the temperature at 110 °C ± 5 °C.

6.3.5 Steel rulers.

6.3.6 Balance, with less than 5 g of precision.

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6.4 Test pieces

6.4.1 Sampling

Sampling of shaped refractory products and monolithic refractories shall be conducted in accordance
with ISO 5022 and ISO 1927-2, respectively, or negotiated by corresponding parties.

6.4.2 Shape, dimensions and preparation of test pieces

Standard bricks with the dimensions of 230 mm × 114 mm × 64 (74) mm with intact edges and angles
without cracks shall be adopted for testing. For oversized bricks, test pieces with these dimensions
shall be cut from the original bricks. Only one test piece is cut from each brick.
Test piece preparation of monolithic products shall be conducted in accordance with ISO 1927-5.

6.5 Test procedures

6.5.1 Heating

Dry the test pieces in a drying oven at 110 °C ± 5 °C to a constant mass. Cool the test pieces to ambient
temperature then weigh using a balance and record the mass.
Heat the furnace to the test temperature ± 10 °C and keep for 30 min. Put the test pieces into the furnace
with a bottom surface of 230 mm × 64 (74) mm. The intervals between test pieces shall not be less than
30 mm. Overlapping is not permitted.
The test temperatures shall be negotiated by the corresponding parties and marked in the test report.
The recommended test temperature is 1 000 °C.
Shut the furnace door after the test pieces are put into the furnace. The furnace temperature shall
return to the test temperature ± 10 °C within 10 min. After this, hold for 20 min.

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6.5.2 Cooling

Open the furnace after temperature holding, take the test pieces out and put them on the cooling rack.
After natural quenching in air for 5 min, weigh them again.
During quenching, forced convection ventilation and bulk metallic heat conductors around the test
pieces are not permitted. The furnace door shall be closed and the furnace temperature shall be kept at
1 000 °C ± 10 °C.
Repeat these procedures until the mass loss reaches 20 %. Record the thermal shock cycle number or
end the test at the negotiated cycles.
Damage by external forces shall be avoided during testing.

6.5.3 Results expression

The thermal shock cycle in which the mass loss of test pieces reaches 20  % is used to express the
thermal shock resistance.
If the mass loss of the test piece reaches 20 % during quenching, the cycle is valid.
If the test piece is damaged by the external forces, the testing is invalid. In this case, retest.
See Annex A for precision data.

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ISO 21736:2020(E)


7 Test report
The test report shall include at least the following:
a) test items;
b) test date;
c) a reference to this document (i.e. ISO 21736:2020);
d) test materials used (e.g. manufacturer, variety, batch number);
e) quantity of samples to be measured;
f) test temperature and quenching conditions;
g) thermal shock cycle number.

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ISO 21736:2020(E)


Annex A
(informative)

Precision data of thermal shock resistance tests

Six laboratories were selected to conduct the thermal shock resistance verification test, adopting the
three test methods based on three kinds of bricks: bauxite-based brick with an alumina content of 70 %,
bauxite-based insulating brick with bulk density of 1,0  g/cm3 and magnesia brick with a magnesia
content of 91 %. The calculation results are shown in Table A.1.

Table A.1 — Precision calculation data of thermal shock resistance

Average of
Standard Standard
thermal
Materials deviation deviation Repeatability Reproducibility Relative Relative
shock
and testing within between interval interval repeatability reproducibility
resistance
methods laboratories laboratories
results, r R r% R%
Sr SR
cycles
Bauxite-based
brick
(1 100 °C, 11 2,57 2,97 1,66 3,08 14,96 27,81
water
quenching)
Magnesia
brick (950 °C,
compressed 4 1,78 1,76 0,43 1,90 10,14 44,74
air
quenching)
Bauxite-based
insulting

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brick 11 3,13 4,18 2,92 27,05 4,22 39,10
(1 000 °C, air
quenching)

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ISO 21736:2020(E)

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ICS 81.080