This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D8363 − 20

Standard Test Method for

Rubber—Stress Relaxation in Tension Under Non-
Isothermal Conditions1
This standard is issued under the fixed designation D8363; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope
1.1 This test method is used to determine the non-isothermal
stress relaxation, also known as temperature scanning stress
relaxation (TSSR). Stress relaxation is a characteristic behavior
of rubber materials.
1.2 Units—The values stated in SI units are to be regarded
as the standard. No other units of measurement are included in
this standard.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:2
D3182 Practice for Rubber—Materials, Equipment, and Pro-
cedures for Mixing Standard Compounds and Preparing
Standard Vulcanized Sheets
D3183 Practice for Rubber—Preparation of Pieces for Test
Purposes from Products
D412 Test Methods for Vulcanized Rubber and Thermoplas-
tic Elastomers—Tension
D4483 Practice for Evaluating Precision for Test Method
Standards in the Rubber and Carbon Black Manufacturing
Industries
1
This test method is under the jurisdiction of ASTM Committee D11 on Rubber
and Rubber-like Materials and is the direct responsibility of Subcommittee D11.10
on Physical Testing.
Current edition approved Nov. 1, 2020. Published December 2020. DOI:
10.1520/D8363-20.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3. Terminology
3.1 Definitions:
3.1.1 standard laboratory temperature, n—temperature of
23 6 2°C (73.4 6 3.6°F).
3.1.2 stress relaxation, n—decrease in stress after a given
time at constant strain.
4. Summary of Test Method
4.1 This test method provides a procedure for non-
isothermal stress relaxation as a function of temperature at
constant elongation and at a specific heating rate.
4.2 This test method is useful for the accelerated determi-
nation of the thermal mechanical behavior of a rubber, for
example, its ageing behavior or the parameters describing the
limits for a thermal application of the material.
5. Significance and Use
5.1 Non-isothermal stress relaxation, also known as tem-
perature scanning stress relaxation, performed at a specific
heating rate, delivers a set of parameters useful to specify the
properties of thermo-plastic elastomers. It can also characterize
the deterioration of the cross-linked rubber network in a
reasonable testing time of a few hours.
5.2 Stress relaxation tests are typically performed as time-
dependent experiments at constant strain and temperature. It is
known that temperature has a strong influence on the relaxation
time of rubber. When evaluating ageing behavior such as
deterioration of the network, a reliable test using isothermal
stress relaxation requires extremely long testing times, for
example, days or weeks depending on the application.
6. Apparatus
6.1 Tensile tester equipped with an oven according to Test
Methods D412 consisting of an electrically driven linear
extension actuator equipped with two grips and capable of
holding the test piece without slipping at a fixed extended
length within 61 % accuracy. It shall be able to measure and
record the force acting on the test piece with an accuracy of 61
%.
6.2 The grips shall be positioned inside the oven for testing
of a single test piece. The oven shall maintain a stable heating

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D8363 − 20
FIG. 1 Left (a) schema of a non-isothermal stress relaxation curve indicating the characteristic temperatures at a specific stress decay,
and right (b) detail schema of the initial slope of the non-isothermal stress relaxation curve
rate of at least 2 6 0.05 K/min (°C/min) at the narrow position
of the dumbbell during the test. The oven is equipped with a
temperature sensor placed close to the surface of the test
specimen.
7. Test Specimen
7.1 The test specimens shall be dumbbells with a standard
thickness of 2.0 6 0.2 mm and a length of 75 6 0.5 mm. The
dimension of the narrow portion of dumbbells shall be 2.0 6
0.2 mm by 25 6 0.5 mm by 4 6 0.5 mm. Test specimens shall
be cut from molded sheets prepared in accordance with
Practice D3182 or from product pieces prepared according to
Practice D3183.
7.2 Test specimens shall be cut with the die cutter parallel to
the milling-grain direction. The die cutter shall be sharp and
free from nicks and oil prior to cutting. Support the sheets on
a suitable cutting surface (cardboard, linoleum, etc.) covered
with a thin plastic film to prevent inclusions. Cut the sheets or
pieces with a single, continuous stroke.
7.3 Discard test specimens having obvious flaws. Before
testing, physically randomize the test specimens from all sheets
of the same compound.
7.4 Test specimens shall be conditioned in an unstrained
state for at least 24 h at standard laboratory temperature before
testing. A minimum of three test specimens per compound is
recommended for testing.
8. Procedure
8.1 Isothermal Conditioning:
8.1.1 Place the test piece between the grips of the tensile
tester in the unstrained condition at the standard laboratory
temperature.
8.1.2 Close the oven door and wait for a stable temperature
reading at the narrow position of the dumbbell.
8.1.3 Extend the dumbbell to a recommended elongation of
50 % strain, ε0, within 1 min. If the test piece breaks, reduce the
elongation stepwise by 10 % strain ε0 until the test piece is able
withstand the applied strain or apply another appropriate
elongation.
2
8.1.4 Record the isothermal force decay F(t) at 23°C as a
function of the time t for 2 h, preferably, or for another
specified duration of the isothermal conditioning. This isother-
mal conditioning might have a strong influence on the results
of the non-isothermal relaxation due to short-term relaxation
processes. Final test results are only comparable if the tests are
performed with identical duration of the conditioning isother-
mal relaxation.
8.2 Non-Isothermal Relaxation:
8.2.1 Record the non-isothermal force decay F(T) as a
function of the temperature, T. The initial value F0 is the force
at 23 °C after completing the isothermal conditioning in 8.1.4.
8.2.2 Increase the temperature of the oven with a constant
heating rate of 2 6 0.05 K/min (°C/min) or other required
heating rates depending on the control stability of the oven.
Results obtained with different heating rates are not compa-
rable.
8.2.3 The sampling rate of the force data shall be at least 1
Hz for the heating rate of 2 K/min (°C/min). If required, the
sampling rate might be adapted to other heating rates.
8.2.4 Stop the test when the test piece breaks, the force
reading is null, the force ratio F(T)/F0 reaches a predetermined
value (for example, 0.5 or 0.1), or when the designated final
temperature has been reached.
9. Calculation or Interpretation of Results
9.1 Parameters obtained from the non-isothermal stress
relaxation curve—The tensile stress σ(T) is the force F(T)
normalized by the cross section A0 of the test piece at the
unloaded initial state. The initial tensile stress σ0 is the stress
measured at the corresponding initial temperature T0. The
relaxation modulus E(T) at a specified temperature T is given
by the ratio of the stress σ(T) and the nominal strain ε0.3,4
3
Vennemann, N., Characterization of Thermoplastic Elastomers by Means of
Temperature Scanning Stress Relaxation Measurements, in: A. Z. El-Sonbati (Ed.),
Thermoplastic Elastomers, INTECH, Rijeka (Croatia), 2012, pp. 347-370.
4
Vennemann, N. , Hündorf, J., and Kummerlöwe, C., Phase Morphology and
Relaxation Behaviour of SEBS/PP Blends, KGK Kautschuk Gummi Kunststoffe 54,
Jahrgang, Nr. 7-8, 2001, pp. 362-367.
 D8363 − 20

FIG. 2 Left (a) schema of a relaxation spectrum corresponding to the non-isothermal stress relaxation curve of a TPE, and right (b) re-
laxation spectrum of natural rubber cured with a CV system

9.2 Temperature at a specific stress decay Txx—The course
of the non-isothermal relaxation curve can be described by the
temperature at a specific decay Txx. Thus, the temperature
needed for a stress decay of, for example, 50 % is T50, for 90
% it is T90, etc. See Fig. 1a.
9.3 Relaxation Index RI—A quantification of the non-
isothermal relaxation within the temperature range needed to
reach 90 % force decay is given by the Relaxation Index RI
defined as follows:
T 90 T 90
*
T0
σ ~ T ! ⁄σ 0 dT *
T0
F ~ T ! ⁄F 0 dT
RI 5 5 (1)
T 90 2 T 0 T 90 2 T 0
9.4 Cross-link Density:
9.4.1 With increasing temperature, both rubber and TPE
show an increase of stress due to the entropy elastic behavior.
At higher temperatures, stress relaxation and the corresponding
thermally induced decay become dominant. Nevertheless, the
initial slope of the tensile stress curve described by the
temperature coefficient κ gives information about the entropy
elastic behavior of the material.
9.4.2 According to the neo-Hookean material model, the
stress is σ5v·R·T ~ λ 2 λ 22 ! where R is the universal gas
constant, in J·K−1·mol−1, λ the deformation ratio, and ν the
cross-link density in mol/cm3. The first derivative at the first
inflection point (slope at Ti) of the non-isothermal stress
relaxation curve for a constant deformation λ delivers the
so-called temperature coefficient (see Fig. 1b).
κ 5 ~ ] σ ⁄ ] T ! λ 5 ν·R· ~ λ 2 λ 22 !
and respectively, the cross-link density is:
κ ρ
ν5 5
R· ~ λ 2 λ 22 ! M 'c
where ρ is the density and Mc the average molar mass be-
tween cross-links.
9.5 Parameters Obtained from the Relaxation Spectrum:
9.5.1 The temperature dependent relaxation spectrum for a
temperature scanning with the heating rate β can be expressed
in analogy to the time relaxation spectrum of the Maxwell
model.
9.5.2 Peaks appear in the relaxation spectrum at the posi-
tions of the inflection points of the relaxation curve. The
intensities and temperatures associated with these peaks de-
scribe changes in the elastomer network:
9.5.2.1 In TPE samples, both the glass temperature and the
melting temperature of the rigid phases involved can be
determined (see Fig. 2a).
9.5.2.2 In rubbers cured with sulfur, the deterioration of
mono-, di- and poly-sulfidic cross-links can be determined (see
Fig. 2b).5 Aging can affect the respective peak position and
amplitude.
9.5.2.3 Other components in rubber compounds, like resins
and reinforcing fillers, can also be associated with peaks in the
relaxation spectrum at characteristic temperatures.
10. Report
10.1 The test report shall include the following information:
10.1.1 Sample Details:
10.1.1.1 A full description of the sample and its origin;
10.1.1.2 Compound details, curing time, temperature, and
date, if appropriate; and
10.1.1.3 The method of preparation of test specimens from
sample.
10.1.2 Test Method and Test Details:
10.1.2.1 The number of this standard as reference;
10.1.2.2 A description of the principles of the testing device;
10.1.2.3 The type and dimensions of the test pieces;
(2) 10.1.2.4 The standard laboratory temperature used for iso-
thermal conditioning;
10.1.2.5 The duration of the isothermal conditioning;
(3) 10.1.2.6 The heating rate, the initial temperature T0, and the
final temperature set;
10.1.2.7 The nominal strain ε0 applied to the test piece; and
10.1.2.8 Details of any deviations from the procedures
specified in this document.
10.1.3 Test Results:
10.1.3.1 The number of test pieces tested;

H ~ T ! 5 2∆T S dE non2iso
dT D β5
∆T
∆t
5const.
(4) 5
Vennemann, N., et al., Advanced Materials Research, Vol. 844, 2014, pp.
482-485.

3
 D8363 − 20
10.1.3.2 The median value of the initial stress σ0, the 11. Precision and Bias
selected temperatures Txx, the relaxation index RI, and the 11.1 Precision and bias statements according Practice
temperature coefficient κ, if applicable; D4483 have not been generated but will be available within
10.1.3.3 The stress curves and the relaxation spectra of each five years of publication of the test method.
specimen tested, plotted as a function of temperature indicating
temperature and amplitude of peaks; and 12. Keywords
10.1.3.4 Date of test. 12.1 force decay; stress relaxation; TSSR

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