Designation: D 572 – 99

Standard Test Method for

Rubber—Deterioration by Heat and Oxygen1
This standard is issued under the fixed designation D 572; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

1. Scope 3. Summary of Test Method

1.1 This test method describes a procedure to determine the 3.1 Specimens of vulcanized rubber are exposed to a dete-
relative deterioration resistance of vulcanized rubber in a high riorating influence at a specified elevated temperature and
temperature and high pressure oxygen environment. There may oxygen pressure for known periods of time, after which their
be no exact correlation between this accelerated test and physical properties are determined. These are compared with
natural aging of rubber because of the varied conditions of the properties determined on the original specimens and the
natural aging. This accelerated test is suitable for laboratory changes noted.
compound or product comparisons. 3.2 Unless otherwise specified, the determination of the
NOTE 1—For evaluating rubber vulcanizates under less severe condi-
physical properties shall be carried out in accordance with Test
tions more nearly approaching natural aging, the use of Test Methods Methods D 412.
D 573 and D 865 is recommended. 3.3 Except as may be otherwise specified in this test
method, the requirements of Practices D 3182 and D 3183 shall
1.2 The values stated in SI units are to be regarded as the
be complied with and are made part of this test method.
standard. The values given in parentheses are for information
3.4 In case of conflict between the provisions of this test
only.
method and those of detailed specifications or test methods for
1.3 This standard does not purport to address all of the
a particular material, the latter shall take precedence.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4. Significance and Use
priate safety and health practices and determine the applica-
4.1 Rubber and rubber products must resist the deterioration
bility of regulatory limitations prior to use. (For specific
of physical properties with time caused by oxidative and
precautionary statement, see Note 2.)
thermal aging. This test method provides a way to assess these
2. Referenced Documents performance characteristics of rubber, under certain acceler-
ated conditions as specified.
2.1 ASTM Standards:
4.2 Please refer to the Annex in Test Method D 573 for
D 412 Test Methods for Vulcanized Rubber and Thermo-
important information on standard compounds used for preci-
plastic Rubbers and Thermoplastic Elastomers—Tension2
sion testing for accelerated test aging evaluation.
D 454 Test Method for Rubber Deterioration by Heat and
Air Pressure2 5. Oxygen-Pressure Vessel
D 573 Test Method for Rubber—Deterioration in an Air
Oven2 NOTE 2—Caution: Adequate safety provisions are important when
heating oxidizable organic materials in oxygen since the rate of reaction
D 865 Test Method for Rubber—Deterioration by Heating may become very rapid in some cases, particularly if large surface area is
in Air (Test Tube Enclosure)2 exposed, and very high pressures may be developed. If the same
D 3182 Practice for Rubber—Materials, Equipment, and equipment is used for the oxygen-pressure test and the air-pressure heat
Procedures for Mixing Standard Compounds and Prepar- test, Test Method D 454, care must be exercised to see that the thermo-
ing Standard Vulcanized Sheets2 static controls are properly set, since the specimens may react very rapidly
D 3183 Practice for Rubber—Preparation of Pieces for Test with oxygen at the temperature of the air-pressure heat test. Liquids
acceptable as heating media for one test may be hazardous when used for
Purposes from Products2
the other test.
D 4483 Practice for Determining Precision for Test Method
Standards in the Rubber and Carbon Black Industries2 5.1 The oxygen-pressure chamber shall consist of a metal
vessel designed to retain an internal atmosphere of oxygen gas
under pressure, with provisions for placing rubber specimens
1
This test method is under the jurisdiction of ASTM Committee D-11 on Rubber within it and subjecting the whole to controlled uniform
and is the direct responsibility of Subcommittee D11.15 on Degradation Tests. temperature. Because of the superior temperature control and
Current edition approved November 10, 1999. Published January 2000. Origi-
nally published as D 572 – 40. Last previous edition D 572–88 (1994)e1.
heat transfer, metal vessels completely immersed in a liquid
2
Annual Book of ASTM Standards, Vol 09.01. medium are recommended for purposes of referee tests. The

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

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 D 572
apparatus shall conform to the following requirements: determination of the original properties on three specimens and
5.1.1 The size of the chamber shall be optional but shall be also on three or more specimens for each exposure period of
such that the specimens may be suspended therein vertically the test. At least 24 h must elapse between completion of the
without undue crowding and without touching each other or the vulcanization of the samples and the start of the aging test.
sides of the chamber. 6.2 When minimum requirements are specified, one test on
5.1.2 The source of heat is optional but shall be located three dumbbells shall be considered sufficient. But if the results
outside of the aging chamber proper. are below the specified requirements, two additional specimens
5.1.3 The heating medium is optional. Water, air, or other shall be prepared from the original sample and tested. Should
fluids known to be safe in the presence of oxygen may be used. the results of either of these tests be below the specified
Water has an advantage because of its rapid heat transfer and requirements, the sample shall be considered to have failed to
noncombustible nature. If air is used, the heated air shall be meet the specifications.
thoroughly circulated by means of mechanical agitation, and
baffles shall be used as required to prevent local overheating 7. Test Specimens
and dead spots. Oils or other combustible fluids are extremely 7.1 Dumbbell-shaped specimens prepared as described in
hazardous in the presence of oxygen, and should not be used as Test Methods D 412 shall be considered standard. Their form
heating media for this test. shall be such that no mechanical, chemical, or heat treatment
5.1.4 Automatic temperature control of the heating medium will be required after exposure in the pressure chamber. If any
by means of thermostatic regulation shall be used. The regu- adjustments (for example, to thickness) are necessary, they
lation system shall be provided with power failure protection should be performed prior to exposure.
and over-shoot protection to prevent accidental runaway tem- 7.2 The cross-sectional dimensions of test specimens for
perature increase. calculating the physical properties shall be measured prior to
5.1.5 The temperature should be automatically recorded exposure in the aging chamber. Gage lines used for measuring
over the entire test period using a temperature-measuring elongations shall be applied after the specimens have been
device capable of measuring at the specific temperature to aged. Only specimens of similar dimensions having approxi-
within 61°C. For apparatus not equipped with automatic mately the same exposed areas may be compared with each
recording capabilities, temperature shall be measured with other.
sufficient frequency to ascertain that the temperature limits
specified in 10.2 are adhered to. If the pressure chamber is 8. Number of Test Specimens
completely immersed, the temperature may be taken as that of 8.1 At least three test specimens shall be used to determine
the heating medium. The sensitive element of the temperature- the original physical properties of each sample and also three
measuring device shall be close to the pressure chamber but not or more specimens of the same material for each exposure
touching it. If the pressure chamber is not completely im- period of the test.
mersed in the heating medium, the sensitive element may be 8.2 When minimum requirements are specified, one test
placed in a thermometer well extending into the pressure shall be made for tensile strength and elongation. If the results
chamber. The thermometer well should be filled with water, or are below the specified requirements, two additional specimens
oil, to a depth sufficient to cover the element, in order to shall be prepared from the original sample and tested. Should
facilitate heat transfer. If it is confirmed by actual check that the results of either of these tests be below the specified
the temperature of the oxygen within the chamber is the same requirements, the samples shall be considered to have failed to
as that of the heating medium, the temperature may be taken in meet the specifications.
the heating medium instead of in the thermometer well. If air
is used as the heating medium, a check of the oven temperature 9. Tests of Unaged Specimens
shall be made by means of temperature-indicating devices 9.1 Determine the stress-strain properties or tensile strength
placed in various parts of the oven to verify the uniformity of and ultimate elongation and any other required properties of
heating. In any case, it is desirable to verify the recorded the original unaged specimens within 96 h of the start of the
temperature by checking with a temperature-indicating device aging period. Discard results on specimens that are found to be
having its sensitive element directly exposed to the oxygen imperfect and retest.
within the pressure chamber. 9.2 When rubber compounds are to be tested for the purpose
5.1.6 Positive, rapid, and complete circulation of the heating of determining compliance with specifications, it shall be
medium shall be maintained so as to assure accurate, uniform permissible to determine the original properties required in 9.1
heating. simultaneously with the determination of the values after the
5.1.7 The pressure chamber shall be equipped with a reli- first aging period even though the elapsed time exceeds 96 h.
able safety valve or rupture diaphragm set for release at 3450
kPa (500 psi) pressure. 10. Procedure for Accelerated Aging
5.1.8 No copper or brass parts shall be exposed to the 10.1 Place the specimens for aging in the aging chamber
atmosphere, nor used in the pressure chamber and tubing or after it has been preheated to the operating temperature. It is
valves leading to it. recommended that not more than 10 % of the volume of the
pressure chamber be occupied by rubber or oxidizable sub-
6. Sampling stance. Avoid simultaneous aging of a mixed group of different
6.1 The sample size shall be sufficient to allow for the compounds if possible. For instance, high-sulfur should not be

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 D 572
aged with lower-sulfur compounds, and those containing 12. Calculations
antioxidants should not be aged with those having no antioxi- 12.1 Express the results of the aging test as a percent of the
dants. Some migration is known to occur. When starting a test, change in each physical property (tensile strength, ultimate
flush the air out of the oxygen-pressure chamber by releasing elongation, or tensile stress), calculated as follows:
the oxygen pressure and refilling, and check the chamber to
P 5 @~A 2 O!/O# 3 100 (1)
make certain the apparatus does not leak.
10.2 The operating temperature shall be 70 6 1°C (158 6 where:
1.8°F) determined as described in 5.1.5. P 5 percentage change in property,
10.3 The pressure of oxygen supplied to the aging chamber O 5 original value, and
shall be 2100 6 100 kPa (300 6 15 psi) as measured by a A 5 value after aging.
calibrated pressure gage. 12.2 Increases will be indicated as positive and decreases as
negative.
10.4 Start the aging interval at the time the specimens are
placed in the heated chamber and continue for a measured time 13. Report
interval. The selection of suitable intervals of aging will 13.1 The report shall include the following results calcu-
depend on the rate of deterioration of the particular materials lated in accordance with Section 12:
being tested. Time intervals frequently used are 24, 48, 72, and 13.1.1 All observed and recorded data on which the calcu-
96 h. lations are based,
10.5 The aging intervals used shall be such that the dete- 13.1.2 Type of aging test,
rioration will not be so great as to prevent determination of the 13.1.3 Aging interval,
final physical properties. In experimental work, it is desirable 13.1.4 Aging temperature,
to use a range of periods, while for routine tests of known 13.1.5 Duration, temperature, and date of vulcanization of
materials fewer intervals may be employed. the rubber, if known,
10.6 At the termination of the aging interval, remove the 13.1.6 Dates of original and final determinations of physical
specimens from the aging chamber, cool to room temperature properties, and
on a flat surface, and allow to rest not less than 16 h nor more 13.1.7 Dimensions of test specimens.
than 96 h before determination of the physical properties. In
relieving the pressure from the oxygen-pressure chamber 14. Precision and Bias3
preparatory to removing the aged specimens, it is essential that 14.1 This precision and bias section has been prepared in
the release be slow and uniform, requiring at least 5 min so as accordance with Practice D 4483. Refer to this practice for
to avoid possible formation of porosity in the specimen. Then terminology and other statistical calculation details.
apply to the specimens gage lines used for measuring elonga- 14.2 A Type 2 (interlaboratory) precision was evaluated in
tions: 1974. Both repeatability and reproducibility are short term, a
period of a few days separates replicate test results. A test result
NOTE 3—Caution: For the evaluation of rubber compounds intended is expressed on the basis of a median value, as specified by Test
for service at elevated temperatures, the above test methods may be used
Methods D 412 obtained on 3 determinations or measurements
with an operating temperature of 80 6 1°C (176 6 1.8°F), employing
time intervals as suggested in 10.4, or as otherwise agreed upon. It should of the property or parameter in question.
be noted that by increasing the aging temperature to 80°C (176°F) from 14.3 Six different materials were used in the interlaboratory
70°C (158°F) the rate of oxidation may be expected to be approximately program, and were tested in 3 laboratories on 2 different days.
double, and if the rubber compound may be expected to be approximately These precision results were obtained for a variety of com-
double, and if the rubber compound is of a rapid aging type, or if it is pounds prepared in accordance with Method D 15 prior to its
contaminated with such materials as copper or manganese, the rate of removal from the Annual Book of ASTM Standards. Please see
oxidation may be catalyzed to such extent as to become violent.
the Annex of Test Method D 573 for more details on this work.
11. Test of Aged Specimens 14.4 The results of the precision calculations for repeatabil-
ity and reproducibility for both percent tensile strength change
11.1 Determine the tensile strength and ultimate elongation and percent elongation change are given in Table 1, in
or the stress - strain properties of the specimens, aged for ascending order of material average or level, for each of the
different intervals, as the intervals terminate, disregarding the materials evaluated.
fact that more specimens may still be aging. In determining the 14.4.1 The precision of this test method may be expressed in
physical properties after aging, consider as the final values the the format of the following statements that use an appropriate
median of results from three specimens except that under the value of r, R, ( r), or (R), that is, that value to be used in
following conditions expose and test two additional specimens decisions about test results (obtained with the test method).
and use the median of the values for the five specimens: The appropriate value is that value of r or R associated with a
11.1.1 If one or more values do not meet the specified mean level in the precision tables closest to the mean level
requirements when testing for compliance with specifications, under consideration at any given time, for any given material in
or routine testing operations.
11.1.2 If referee tests are being made. After completion of
the tests, examine the broken specimens visually and manually 3
Supporting data have been filed at ASTM Headquarters. Request RR: D-11-
and note their condition. 1055.

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 D 572
TABLE 1 Type 2—Precision Results—Aging at 70°C precision tables. Two single test results, obtained under normal
NOTE 1— test method procedures, that differ by more than this tabulated
Sr 5 within laboratory standard deviation. r (for any given level) must be considered as derived from
r 5 repeatability (in measurement units). different or non-identical sample populations.
SR 5 between laboratory standard deviation. 14.6 Reproducibility— The reproducibility R, of this test
R 5 reproducibility (in measurement units).
NOTE 2—Averaging both 48 and 96 h of aging for Part 2 increases the
method has been established as the appropriate value tabulated
DF for precision estimates. in the precision tables. Two single test results obtained in two
Part 1—Percent Change in Tensile Strength, Aged 48 h at 70°C
different laboratories, under normal test method procedures,
that differ by more than the tabulated R (for any given level)
Material or Mean Test Within Between must be considered to have come from different or non-
Compound Level Laboratories Laboratories
identical sample populations.
Sr r SR R
14.7 The precision results indicate that the repeatability and
CR (2D) −0.4 3.61 10.2 8.48 24.0 reproducibility of both percent tensile strength change and
NR (1G) −77.6 1.41 4.0 ... ...
SBR (9B) −3.0 2.39 6.76 5.96 16.9 percent elongation change are essentially the same. Also the
OESBR (10B3) −2.8 7.20 20.4 10.1 28.6 value of r or R, or both does not vary with the magnitude of
IIR (2E) −5.9 4.85 13.7 6.8 19.2
NBR (1F) −5.6 15.7 44.4 15.1 42.7
percent elongation or percent tensile strength change. No
values are given for (r) or (R) because of the near zero average
Pooled Values: ... 7.55 21.4 9.83 27.8
values for some of the materials.
Part 2—Percent Change in Elongation, Average of 48, 96 H Aging 14.8 Bias—In test method terminology, bias is the differ-
Precision Values
ence between an average test value and the reference (or true)
NR (1G) −92.0 0.99 2.80 9.6 27.2 test property value. Reference values do not exist for this test
NBR (1F) −15.5 9.4 26.6 9.4 26.6 method since the value (of the test property) is exclusively
SBR (9B) −13.8 3.53 10.0 7.58 21.5
OESBR (10B3) −7.8 5.54 15.7 7.54 21.3
defined by the test method. Bias, therefore, cannot be deter-
CR (2D) −0.0 5.32 15.1 7.59 21.5 mined.
IIR (2E) −4.6 5.50 15.6 5.50 15.6
Pooled Values: ... 5.64 16.0 8.00 22.6 15. Keywords
15.1 elevated temperature; oxidative aging; pressure cham-
14.5 Repeatability— The repeatability r, of this test method ber; pressure vessel; rubber articles; rubber products; thermal
has been established as the appropriate value tabulated in the aging

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