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: D8491 − 23

Standard Test Method for

Recovered Carbon Black—Rheological Non-Linearity of a
Rubber Compound by Fourier Transform Rheology1
This standard is issued under the fixed designation D8491; 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 D3896 Practice for Rubber From Synthetic Sources—

1.1 This test method provides a measure of rheological Sampling
non-linearity of a rubber compound filled with rCB to assess its D6204 Test Method for Rubber—Measurement of Unvulca-
reinforcement capabilities. This test method requires the use of nized Rheological Properties Using Rotorless Shear Rhe-
a sealed cavity rotorless oscillating shear rheometer for the ometers
measurement of the torque with increasing sinusoidal strain D8059 Test Method for Rubber Compounds—Measurement
applied to an uncured rubber compound containing significant of Unvulcanized Dynamic Strain Softening (Payne Effect)
amounts of colloidal fillers, such as recovered carbon black, Using Sealed Cavity Rotorless Shear Rheometers
alone or as blend with virgin carbon black. 3. Significance and Use
1.2 Units—The values stated in SI units are to be regarded 3.1 This test method provides a measure of rheological
as the standard. No other units of measurement are included in non-linearity for filled rubber compounds under oscillatory
this standard. shear conditions: the normalized 3rd harmonic of the torque
1.3 This standard does not purport to address all of the I3/1.
safety concerns, if any, associated with its use. It is the 3.2 Rheological linearity means that the modulus is a
responsibility of the user of this standard to establish appro- function of frequency only. The shear modulus dependency on
priate safety, health, and environmental practices and deter- both frequency and amplitude of a dynamic deformation is a
mine the applicability of regulatory limitations prior to use. non-linear, rheological effect. Filled rubbers show a strain
1.4 This international standard was developed in accor- dependency of the modulus known as Payne effect. A test
dance with internationally recognized principles on standard- method for evaluating the Payne effect can be found in Test
ization established in the Decision on Principles for the Method D8059.
Development of International Standards, Guides and Recom-
3.3 One of the main contributions to the Payne effect is the
mendations issued by the World Trade Organization Technical
so-called polymer-filler interaction in the range of mid ampli-
Barriers to Trade (TBT) Committee.
tude oscillation shear, MAOS. The MAOS amplitude range is
2. Referenced Documents defined as the range where I3/1 is already measurable and
increases according to a scaling law, for example, I3/1 ~ γ2. It
2.1 ASTM Standards:2 has been shown that FT rheological measurements are very
D1485 Practice for Rubber from Natural Sources— sensitive to changes in this interaction, and that it is possible to
Sampling and Sample Preparation quantify the influence of the filler type and content on the
D3191 Test Methods for Carbon Black in SBR (Styrene- nonlinearity. Interactions between the polymer and particle
Butadiene Rubber)—Recipe and Evaluation Procedures surface and between the filler particles create a network
D3192 Test Methods for Carbon Black Evaluation in NR structure in the compound that not only increases the elasticity
(Natural Rubber) of the system but also introduces nonlinear contributions to the
stress response.3
1
This test method is under the jurisdiction of ASTM Committee D36 on 4. Apparatus
Recovered Carbon Black (rCB) and is the direct responsibility of Subcommittee
D36.70 on rCB Testing in Rubber. 4.1 Torsion Strain Rotorless Oscillating Rheometer with a
Current edition approved June 15, 2023. Published July 2023. Originally Sealed Cavity in accordance with Test Method D6204, oper-
approved in 2022. Last previous edition approved in 2022 as D8491 – 22. DOI:
ated in the test mode called strain sweep, in which the strain
10.1520/D8491-23.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Schwab, L. et al., “Fourier-Transform Rheology of Unvulcanized, Carbon
Standards volume information, refer to the standard’s Document Summary page on Black Filled Styrene Butadiene Rubber,” Macromol. Mater. Eng., 2016, 301, pp.
the ASTM website. 457−468.

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

1
 D8491 − 23
amplitude is programmed to change in steps under constant 6.2.1 Temperature: 80.00, in °C.
frequency and temperature conditions. 6.2.2 Offset: 0.00 %.
4.2 Ensure that the oscillating rheometer is capable of 6.2.3 Pressure: 450 kPa (4.5 bar).
performing a Fourier Transform with the appropriate sampling 6.2.4 Time: 4.00 min.
rate and torque sensitivity. 6.3 Perform a strain sweep with the following parameters:
4.3 Check the input signal before performing this test. The 6.3.1 Frequency: 0.20 Hz.
sinusoidal strain signal must be free of higher harmonics. 6.3.2 Temperature: 80.00, in °C.
Specifically, the 3rd harmonic of the strain at γ = 32 % must be 6.3.3 Offset: 0.00 %.
maximal 0.25 % of its 1st harmonic (excitation frequency) 6.3.4 Pressure: 450 kPa (4.5 bar).
when testing a reference test specimen, like an unfilled butyl 6.3.5 Pre-cycles: 3.
rubber. If this is not the case, request a calibration of the 6.3.6 Amplitude steps γ, in %: 8, 16, 32, 64, 128.
rheometer by the manufacturer.
7. Calculations
5. Sampling 7.1 Calculate the non-linearity parameter I3/1 as ratio of the
5.1 A reference compound for evaluation of carbon black in absolute value of the 3rd harmonic of the torque S3 and the
SBR in accordance with Test Methods D3191 shall be used in absolute value of the complex torque S* (1st harmonic) at a
this test method. For this purpose, substitute the virgin carbon frequency ω and a shear strain γ:
black in the formula by recovered carbon black or by the
corresponding filler blend. Alternatively, the reference com- I 3⁄1 ~ γ ! 5
? I ~ 3ω,γ ! ? 5 ? S ~ γ ! ?
3
(1)
pound for carbon black evaluation in natural rubber (NR)
I* ~ ω,γ ! ? S* ~ γ ! ?
according to Test Methods D3192 might be used, bearing in 7.2 Express the value of I3/1 in % by multiplying the ratio
mind that the natural variations of NR can increase the with the factor 100.
variability of the test results.
8. Report
NOTE 1—Increasing the filler loading of the reference compound
increases the rheological non-linearity, and therefore, improves the signal- 8.1 Report the following information:
to-noise ratio of the normalized 3rd harmonic I3/1. A filler loading of 70 8.1.1 A full description of the sample or test specimen(s), or
phr is recommended. both, including their origin.
5.2 The sample shall be taken from the reference compound 8.1.2 Type and model of oscillating rheometer.
as required by the mixing method or other sampling instruc- 8.1.3 The temperature and time for the pre-conditioning
tions. Condition a raw rubber sample in accordance with step.
Practice D1485 or Practice D3896 until it has reached room 8.1.4 The frequency in Hertz and temperature in degrees
temperature (23 6 3°C (73 6 5°F)) throughout. Celsius for the strain sweeps.
5.3 The test specimen shall be circular with a mass of about 8.1.5 Report the non-linearity parameter I3/1 in % for γ = 32
5 to 6 g corresponding to a volume of 4 to 6 cm3, see Test %.
Method D6204.
9. Precision and Bias
6. Procedure 9.1 A precision and bias statement has not been completed
6.1 Place the test specimen in the rheometer chamber and for this test method at this time.
close the chamber. Closing pressure: 450 kPa (4.5 bar).
6.2 Perform a pre-conditioning step with the following 10. Keywords
parameters: 10.1 FT rheology; rCB; reinforcement; RPA

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