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: D8471 − 22a

Standard Practice for

Silica—Reference Compound1
This standard is issued under the fixed designation D8471; 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 3.2 Definitions:

1.1 This practice covers the standard raw materials,
formulation, and mixing procedure for the evaluation and
quality control of silica and related technologies, such as
silanes and functionalized polymers, in a standardized rubber
compound.
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
D1566 Terminology Relating to Rubber
D3182 Practice for Rubber—Materials, Equipment, and Pro-
cedures for Mixing Standard Compounds and Preparing
Standard Vulcanized Sheets
D5900 Specification for Physical and Chemical Properties of
Industry Reference Materials (IRM)
3. Terminology
3.1 The following terms are defined in accordance with
Terminology D1566.
1
This practice is under the jurisdiction of ASTM Committee D11 on Rubber and
Rubber-like Materials and is the direct responsibility of Subcommittee D11.20 on
Compounding Materials and Procedures.
Current edition approved Oct. 1, 2022. Published October 2022. Originally
approved in 2022. Last previous edition approved in 2022 as D8471 – 22. DOI:
10.1520/D8471-22A.
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.
3.2.1 silanization, n—chemical reaction of organosilane
molecules with the silanol groups of synthetic amorphous silica
covering its surface and improving its compatibility with
rubber leading to an enhanced dispersion.
3.2.2 silica (as related to rubber technology),
n—nanostructured, synthetic amorphous silicon dioxide (SAS)
typically based on primary particles bound to form aggregates
and agglomerates as secondary particles, covered by silanols
and siloxanes, and produced either by conversion to a solid
from a supersaturated solution of silicate salts in water (pre-
cipitated SAS), or by a pyrogenic process in a flame (fumed
SAS).
4. Summary of Practice
4.1 This practice shall be used for specific procedures used
in silica technology for rubber compounds. A reference com-
pound is required for quality control of production, for research
and development purposes, and for comparison of different
materials.
5. Significance and Use
5.1 This practice may be used to characterize silica or silane
in terms of specific properties of the standard compound. This
practice is useful for the quality assurance of silica production.
It may also be used for the preparation of reference compounds
for compounding experiments, to confirm the day-to-day
reliability of testing operations used in the rubber industry, for
the evaluation of experimental compounds, and for quality
control of production compounds.
6. Standard Test Formula
6.1 The standard formula in Table 1 has been formulated for
a silica with a CTAB surface area of 160 m2/g using TESPD
silane, and for a S-SBR 2548 oil extended with 37.5 phr
TDAE. If different silica grades or silane types are used,
adjustments of the recipe might be required.
6.2 NR is needed to increase mixing efficiency for this
formula. Both Standard Malaysian Rubber grade L (SMR L)
and Standard Thai Rubber grade L (STR L) are recommended
to give satisfactory performance. Other sources of rubber
should be previously checked to ensure that results are equiva-
lent.

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1
 D8471 − 22a
TABLE 1 Standard Formula 7. Mixing Procedure
Material Quantity, parts by massE
S-SBR 2548, 37.5 TDAEA 123.75 7.1 The mixing procedure for a Standard Internal Mixer
NR 10.00 according to Practice D3182 is described in Table 2 (times in
Silica, precipitated 95.00
ZnO 2.50
seconds).
Stearic acid 2.50
Antioxidant (6PPDB ) 2.00 7.2 If internal mixers of other sizes are used, adjustments of
Wax 2.00 batch masses, ram pressure, rotor speeds or mixing times will
Silane 6.84
DPGC 2.00
be required to obtain equivalent results. The use of other mixer
CBSD 2.00 sizes shall be recorded with the reported data. For general
Sulfur, soluble 2.00 information regarding mixing procedures see Practice D3182.
Total: 250.59
A
Treated Distillate Aromatic Extract.
B
N-(1,3-dimethylbutyl)-N’-phenyl-p-phenylenediamine.
8. Keywords
C
1,3-Diphenylguanidine.
D
N-Cyclohexylbenzothiazol-2-sulphenamide.
8.1 formulation; mixing procedure; recipe; silane; silaniza-
E
Weigh rubber and silica to the nearest 1 g, sulfur and accelerator to the nearest tion; silica
0.02 g, and all other compounding materials to the nearest 0.1 g.

6.3 The use of Industry Reference Materials (IRM) as

specified in Specification D5900 is recommended for standard
rubber test formulas.3

3
The current list of Industry Reference Materials for rubber can be found on the
webpage of the Committee D11 under the section Additional Information
(www.astm.org/COMMITTEE/D11).

2
 D8471 − 22a
TABLE 2 Mixing Procedure for Standard Internal Mixer
1st Step Duration, s Accumulation, s
Fill factor 0.62 to 0.72, rotation speed 6.3 to 8.1 rad/s (60 to 77 rpm)
Lower Ram pressure 0.5 to 0.6 MPa 0 0
Add polymers 15 15
Ram down and pre-mastication 30 45
Add silica, silane, stearic acid, antioxidant, wax and oil 30 75
Mix and adjust speed to target temperature 150 to 160 °C 90 165
Continue mixing at target temperature 180 345
Discharge and record dump temperature (recommended: 140 to 150°C) 5 350
Store compound for 12 to 24 h @ RT before 2nd step
2nd Step
Fill factor 0.58 to 0.68, rotation speed 5.2 to 6.8 rad/s (50 to 65 rpm)
Lower Ram pressure 0.5 to 0.6 MPa 0 0
Add 1st mixing step, ZnO 20 20
Add ingredients: DPG, CBS, sulfur 20 40
Mix and adjust speed to target temperature 90 to 110 °C 100 140
Discharge and record dump temperature (recommended: 90 to 110°C) 5 145
Store compound for 12 to 24 h @ RT before curing

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