Influence of Aromatic Content in Rubber Processing Oils on Viscoelastic Behaviour and Mechanical Properties of Styrene-butadiene-

rubber For Tyre Tread Applications

Influence of Aromatic Content in Rubber Processing Oils on

Viscoelastic Behaviour and Mechanical Properties of Styrene-
butadiene-rubber For Tyre Tread Applications
Yotwadee Chokanandsombat1,a and Chakrit Sirisinha1,2,b*
1
Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Mahidol
University, Bangkok, Thailand
2
Rubber Technology Research Centre (RTEC), Faculty of Science, Mahidol University, Salaya Campus, Nakhon
Pathom, Thailand

Summary
In the present study, experiments have been carried out to investigate the effects of aromatic and polycyclic
aromatic compounds (PCAs) contents in rubber processing oils (RPOs) on the processability and mechanical
properties of styrene butadiene rubber (SBR) compounds and vulcanisates. Results obtained suggest that, as
expected, the presence of RPOs leads to a decreased compound viscosity, and thus an enhanced processability.
By incorporating the RPOs into SBR compounds, some mechanical properties, including elongation at break
and tear strength, of cured SBR can be improved, particularly for the RPOs with high aromatic content. This
is believed to be attributed to the increased compatibility of aromatic containing RPOs and the SBR matrix.
Nevertheless, the aromatic and PCA contents play an insignificant role on the crosslink density and bulk viscosity
of the rubber compounds as well as the hardness and compression set of the rubber vulcanisates.

Keywords: Rubber processing oil, Aromatic oil, Cure characteristics, Viscoelastic behaviour,
Mechanical properties

1. Introduction In 1994, the Swedish National content in RPOs must be optimised.

Rubber processing oils (RPOs) are
organic substances which are usually
added to polymers to improve the
processability of such polymers.
Further advantages of the RPOs are
increments in desirable polymer
properties, such as softness, elongation
and low-temperature flexibility.
Moreover, the RPOs provide the
rubber compounds with lowered
intermolecular forces, and so a lower
glass transition temperature (Tg)1,2.
Distillate aromatic extracts (DAEs)
with high contents of poly-aromatic
hydrocarbons (PAHs) and polycyclic
aromatic compounds (PCAs) are
widely used for both synthetic rubbers
and natural rubber (NR)3.
* Corresponding author: Chakrit Sirisinha; chakrit.sir@mahidol.ac.th
©
Smithers Information Ltd., 2014
Chemicals Inspectorate, KEMI,
published a report which initiated a
discussion on the use of high aromatic
extender oils in tyre treads. The oils
with high contents of PAH and PCA,
which are identified as suspected
carcinogens, caused most concern4.
As a result, in 2005, the European
Commission adopted the directive
(EU Substance Directive 67/548/EEC).
This legislation restricts the marketing
and usability of certain PAHs and PCAs
in extender oils for tyre manufacturing.
However, by altering the proportion of
aromatic carbon in the RPOs, changes
in the properties of RPOs resulted5.
Consequently, in order to achieve both
environmental friendliness and effective
rubber compounding, the aromatic
There are published works reporting the
uses of the low aromatic oils in rubber
products in place of high aromatic oils.
For NR, it has been reported that all
non-carcinogenic oils with low aromatic
content could replace high aromatic oils
in NR compounds6. Moreover, at 0 °C,
the compounds plasticised with non-
carcinogenic oils possess slightly higher
loss factor (tan d) than those plasticised
with the DAE. This also gives greater
traction at low temperatures and better
wet grip of the rubber vulcanisates6.
Similar to the NR compounds, for
styrene butadiene rubber (SBR) a
substitution of high aromatic oils by low
aromatic oils affects the tan d slightly
at low and elevated temperatures7. The
low aromatic oil broadens the tan d peak
because of lower compatibility with
the macromolecular backbone of the
rubber matrix5. An investigation of RPO
influence on the dispersion behaviour of
carbon black has also been reported8,9.

Polymers & Polymer Composites, Vol. 22, No. 7, 2014 599

 Yotwadee Chokanandsombat and Chakrit Sirisinha
It is known that styrene butadiene (Bangkok, Thailand). Stearic acid was
rubber (SBR) is a widely used synthetic purchased from Petch Thai Chemical
elastomer, mainly in tyre tread Co., Ltd. (Bangkok, Thailand). Zinc
application where good mechanical oxide (ZnO) and sulphur (S8) were
properties, excellent abrasion supplied by Chemmin Co. Ltd.,
resistance, good traction and lower heat (SamutPrakan, Thailand). N-t-butyl-
build-up are required10,11. Typically, due 2-benzothiazolesulfenamide (TBBS),
to the presence of aromaticity in SBR, as cure accelerator, was purchased
the aromatic content in RPOs has been from Kitpiboon chemical Ltd., Part.
expected to affect compatibility with (Bangkok, Thailand). The RPOs
the SBR matrix, and thus the properties with variable aromatic content were
of SBR vulcanisates. Although there
supplied by IRPC Plc. Co., Ltd.
are published work focusing on
aromatic content in RPOs on properties
of rubber vulcanisates, the number 2.2 The Characterisation of
of work on property investigation Physico-chemical Properties of
of SBR systems in which aromatic RPOs
content is varied systematically is still
Carbon-type composition, i.e.,
limited. Consequently, this research
aromatic carbon (C a), naphthenic
aims to (i) investigate the effects of
carbon (Cn) and paraffinic carbon (Cp),
aromatic and PCA contents of RPOs
of RPOs was determined as per ASTM
on the viscoelastic and mechanical
D2140. A characterisation method
properties of SBR systems; (ii) to
statistically related to the dominant
provide information as a guideline for
chemical structure of petroleum oil
rubber technologists to reformulate
is the Viscosity-Gravity Constant
their compounds to obtain equivalent
(VGC) measured according to ASTM
properties with lower aromaticity in
D2501. The relative density of each
the RPOs.
RPO was measured as per ASTM
D4052. Referred to ASTM D445, the
2. Experimental viscosity of each of the RPOs was
determined at different temperatures
2.1 Materials (i.e., at temperature of 40 and 100 °C).
All materials used in this work were The aniline point was measured as per
used as received. Styrene butadiene ASTM D611. Total acid number was
rubber (SBR 1502; styrene content measured as per ASTM D664. Very
of 23.5%) was manufactured by relevant to this research is one chemical
Bangkok Synthetic Co., Ltd. (Rayong, test method which has been adopted by
Thailand). Carbon Black (N330) the European Commission, namely, IP
as reinforcing filler was supplied 346. This test method is a criterion of
by Thai Carbon Product Co., Ltd. carcinogenicity classification for base
Table 1. Compound recipe used in this work
Chemicals Function Amount (phr*)
SBR (1502) Raw rubber 100
Carbon black (N330) Reinforcing filler 50
Zinc oxide (ZnO) Cure activator 3 %strain of 1%.
Stearic acid Cure activator 1
RPO **
Processing aid/Softener Variable: 0, 5, 10, 15
TBBS*** Cure accelerator 1 Determination
Sulphur Curing agent 1.75
* = parts per hundred of rubber
** = rubber processing oil
*** = N-tert-Butyl-2-benzothiazolesulphenamide
600 Polymers & Polymer Composites, Vol. 22, No. 7, 2014
oils by determining the PCA content
in the RPOs12,13.
2.3 Compound Preparation
The compounding ingredients, as
shown in Table 1, were mixed using a
2-roll mill (LabTech model LRM 150)
with a two-stage mixing technique.
In the first mixing stage, zinc oxide
(ZnO), stearic acid, carbon black
(CB) and RPO were incorporated
sequentially into the raw rubber with
total mixing time of 14 minutes. Types
and loadings of RPOs were varied in
this step. The mix gained at the first
mixing stage is usually known as
rubber master batch. In the second
mixing stage, the rubber master batch
was masticated for 2 minutes, and then
sulphur and TBBS were incorporated.
Mixing was continued for 5 minutes
to achieve good distribution and
dispersion of the ingredients. Finally
the rubber compounds were sheeted
and cooled.
2.4 Cure Characteristics and
Viscoelastic Properties
Cure characteristics were determined at
the set temperature of 145 ºC with the
use of a moving die rheometer (MDR;
TechPro, USA). Measurement of
Mooney viscosity (ML1+4 at 100 °C)
was carried out using the Mooney
viscometer (TechPro viscTECH+,
USA). A rubber process analyser (RPA
2000; Alpha Technologies, USA) was
utilised for determining rheological
characteristics of rubber compounds
under strain sweep and frequency
sweep tests. The strain sweep test
was measured at a temperature and
frequency of 100 °C and 1 rad/s,
respectively. The frequency sweep test
was measured at 100 °C under a given
2.5 Crosslink Density
Measurement of crosslink density was
conducted via the swelling technique
based on the Flory-Rehner equation
as illustrated in Eq. (1)14. Toluene was
Influence of Aromatic Content in Rubber Processing Oils on Viscoelastic Behaviour and Mechanical Properties of Styrene-butadiene-
rubber For Tyre Tread Applications

used as liquid medium:
−[ln(1 − υ2 ) + υ2 + χυ22 ] =
1 υ2
V1n[ υ2 3 − ] Shore A scale (Cogenix Wallace, UK)
2 (1)
where n is the number of elastically
active chains per unit volume, V1 is the
molar volume of the solvent, c is the
polymer–solvent interaction parameter
(the interaction parameter between
SBR and toluene =0.44615), and u2
is the volume fraction of polymer in
the swollen sample which could be
calculated from Eq. (2)14,16:
m1ds
υ2 = 3.1 RPO Properties
m1 (ds −dr ) + m2 dr
(2)
where m1 is the weight of the polymer
before swelling; m2 is the weight of
the polymer after swelling; ds is the
density of solvent and dr is the density
of polymer.
2.6 Measurement of the
Mechanical Properties
To p r e p a r e c u r e d s p e c i m e n s
(vulcanisates), the rubber compounds
were compression moulded using a
hydraulic hot-press under a pressure of
10.5 MPa at 145 °C for the optimum
cure time (tc90) as pre-determined from
the MDR. Hardness of vulcanisates
was measured using a durometer with
as per ASTM D2240. Tensile properties
were determined using a universal
testing machine (Instron 5566, USA)
according to ASTM D412, Die C. Tear
strength was determined according to
ASTM D624. Compression set was
measured as per ASTM D395 method
B at 70 °C and 100 °C for 22 h.
3. Results and
Discussion
Physico-chemical properties of the
RPOs used in this research work are
shown in Table 2. The RPOs possess
different contents of aromatic carbon
(C a), naphthenic carbon (C n) and
paraffinic carbon (Cp). This leads to
a difference in the chemical nature of
the oils17. Generally, a higher value
of VGC indicates greater aromaticity
in the RPOs2,18. In accordance with
this, the results illustrated in Table 2
confirm that, for these compounds,
the VGC increases with increasing
aromatic content in the oils used.
Except for the RPO-4, the relative
density of the RPOs tends to increase
with increasing aromaticity in the oils.
However, the oil characteristics as
illustrated in Table 2 show that there
is no simple relationship between the
kinematic viscosity and the aromatic
content of the RPOs. The aniline point
of the RPOs decreases with increasing
aromatic content in the oil, except for
RPO-4. Furthermore, the acid numbers
of each RPO are not significantly
different, so these oils should not affect
the curing characteristics of the rubber
compounds. The PCA content tends
to increase with increasing aromatic
carbon in the RPOs, as expected.
3.2 Cure Characteristics and
Rheological Behaviour of
Rubber Compounds
Figure 1 shows a plot of the torque
differences (MH–ML) against aromatic
content for various concentrations of
RPOs. As reported elsewhere, the (MH–
ML) is an indication of the crosslink
density in a rubber vulcanisates6,14,19.
Apparently, from Figure 1, at any given
RPO loading, the crosslink density
of cured SBRs does not significantly
change with either the aromatic or
the PCA content. By contrast, with an

Table 2. The physico-chemical properties of RPOs

Properties Test Method Unit RPO-1 RPO-2 RPO-3 RPO-4 RPO-5
C-type ASTM D 2140
- Ca % by wt 19 28 31 33 40
- Cn % by wt 23 26 21 27 27
- Cp % by wt 58 46 48 40 33
VGC *
ASTM D 2501 0.849 0.870 0.887 0.895 0.930
Density ASTM D 4052
- at 15 °C g/cm3 0.9255 0.9526 0.9750 0.9615 0.9933
- at 30 °C g/cm 3
0.9161 0.9432 0.9756 0.9521 0.9839
Kinematic Viscosity ASTM D 445
- at 40 °C mm2/s 275.3 901.4 3482 343.8 761.3
- at 100 °C mm2/s 17.85 31.74 55.74 18.22 24.47
Aniline point ASTM D 611 °C 91.75 82.30 73.65 74.35 56.05
Total acid number ASTM D 664 mgKOH/g 0.03 0.02 0.03 0.03 0.05
PCA **
IP 346 % by wt 2.14 3.63 4.04 9.35 15.78
* = viscosity-gravity constant
** = polycyclic aromatic compounds

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 Yotwadee Chokanandsombat and Chakrit Sirisinha

Figure 1. Cure torque difference (as an indication of crosslink density) in SBR increase in RPO loading, the crosslink
compounds as a function of oil concentration and aromatic content density decreases at any given aromatic
content. Similar findings are reported
elsewhere20-21. It is postulated that some
portion of curatives might dissolve
in RPO phase which is analogous to
the reduction of curatives content in
rubber phase. This therefore leads to the
reduction in cure efficiency. Also, the
results suggest that the cure efficiency
in SBR compounds is dominated by
the increased diffusivity associated
with the RPO loading rather than by
any aromatic to aromatic interaction
between the oil and the polymer chains.
Indeed other factors, such as the type
and loading of active ingredients in
the compounds are more capable of
controlling the cure behaviour of the
Figure 2. Crosslink density of SBR compounds as a function of RPO
rubber compounds20. For example,
concentration and aromatic content
when increasing the RPO loading the
increased acidity of the RPO might lead
to a reduction in cure efficiency. Similar
findings are reported elsewhere21.

The relationship between the crosslink

density as determined from Flory-
Rehner equation, RPOs type, and the
loading is exhibited in Figure 2. The
results agree well with the crosslink
density results as determined from
the (MH–ML) results, as mentioned
previously.

3.3 Viscoelastic Properties of

Rubber Compounds
Figure 3 shows the Mooney viscosities
Figure 3. Mooney viscosity of SBR compounds with various RPOs of SBR compounds prepared with
different RPO loadings and aromatic
contents. The results show no significant
alteration in Mooney viscosity with
increasing aromaticity as well as PCA
content in the RPOs. Furthermore,
as expected, an increase in RPO
loading reduces the Mooney viscosity,
due to the “plasticisation effect”.
This indicates the improved ease of
processing facilitated by incorporation
of RPO into the compounds.

Logarithmic plots of complex viscosity

(η*) against angular frequency of SBR
compounds filled with various types
and loadings of RPOs are shown in

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Influence of Aromatic Content in Rubber Processing Oils on Viscoelastic Behaviour and Mechanical Properties of Styrene-butadiene-
rubber For Tyre Tread Applications

Figures 4 and 5. These results clearly Figure 4. Complex viscosity as a function of angular frequency of SBR compounds
exhibit a shear-thinning, or so-called incorporated with 5 phr of various types of RPOs
pseudo-plastic behaviour, of all the
SBR compounds11,19. At any given
oil loading and frequency, the η*
does not change significantly with
aromatic or PCA content in the RPO,
as shown in Figure 4. Effect of RPO
loadings on η* of SBR compounds is
shown in Figure 5. Compared to the
SBR compounds without RPO, the
compounds with RPOs display slightly
lower η*. Moreover, regardless of
the RPO type, the η* decreases with
increasing RPO loading, particularly
at low test angular frequencies. The
results appear to be in good accordance
with the Mooney viscosity as discussed
earlier. Therefore, a similar explanation
holds good. Figure 5. Complex viscosity as a function of angular frequency of SBR compounds
incorporated with various loadings of RPO-1
These results emphasise that, for a
broad range of angular frequencies
(or shear rates), the improvement in
processability of SBR compounds
caused by a RPO depends on the
loading, rather than the type of the oil.

The degree of filler dispersion is

a crucial factor controlling the
properties of rubber compounds and
vulcanisates 22,23 . Among various
techniques for determining the degree
of filler dispersion in rubber matrix, the
use of the Payne Effect has proved to
be effective1,24,25. The Payne effect is the
difference between moduli measured
at small and large strains. The smaller
is the discrepancy, the lower is the Figure 6. Payne effect of SBR compounds filled with various RPOs
magnitude of the Payne effect. This
reduction correlates with a greater
degree of filler dispersion. Figure 6
shows the magnitude of the variation
in G’ at low (i.e., 1%) and high (i.e.,
100%) % strains with various amounts
of RPOs having different aromatic
contents.

It is evident that the Payne effect is

reduced with increasing aromatic
and PCA contents, implying an
enhancement in the degree of
filler dispersion. In a 3-component
phenomenon, the interaction between
the rubber and the filler is believed to

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 Yotwadee Chokanandsombat and Chakrit Sirisinha

Figure 7. Hardness of SBR vulcanisates incorporated with RPOs having various be enhanced when the compatibility
aromaticity between the oil (via its aromaticity) and
the rubber matrix (via aromatic nuclei
of SBR) is improved18,26. Therefore,
greater aromaticity in the oils leads
to a higher state-of-mix, known to
cause a decrease in the Payne effect
in SBR compounds. Furthermore,
as mentioned earlier, it was shown
that an increase in RPO loading
reduces the bulk viscosity of the SBR
compound. This could facilitate the
filler distribution during mixing. By
this means, a decreases in the Payne
effect results.

3.4 Mechanical Properties

Figure 7 shows the hardness results of
Figure 8. Tensile strength of SBR vulcanisates incorporated with RPOs having cured SBR incorporated with various
various aromatic contents
types and loadings of RPOs. Compared
with the control, the SBR systems
with RPOs show lower hardness.
This decreases with increased RPO
loading. This is normal and is due to
the plasticisation effect1,26,27.

Tensile properties of SBR vulcanisates

as affected by RPOs are shown in
Figures 8 and 9. At any RPO loading,
the increase in aromaticity of the
RPO gives a slight increase in tensile
strength. This might be attributed
to an improved state-of-mix arising
from the enhanced RPO-SBR-filler
compatibility, as discussed previously.
In addition, with an increase in RPO
Figure 9. Elongation at break of SBR vulcanisates softened with RPOs having loading, the tensile strength decreases
various aromatic contents as is normally attributed to the
combined effect of plasticisation and
decreased crosslink density. Likewise,
elongation at break appears to increase
slightly with aromatic and PCA
contents. Again this could be caused
by the enhanced RPO-rubber matrix
compatibility and thus the state-of-mix.
As expected, the elongation at break
increases with increasing RPO loading,
which is due to the decreased crosslink
density, the enhanced plasticisation and
the increased state-of-mix.

Figure 10 shows the tear strength of

SBR vulcanisates with various RPOs.
The tear strength tends to increase

604 Polymers & Polymer Composites, Vol. 22, No. 7, 2014

Influence of Aromatic Content in Rubber Processing Oils on Viscoelastic Behaviour and Mechanical Properties of Styrene-butadiene-
rubber For Tyre Tread Applications

with RPO loading, aromatic and Figure 10. Tear strength of cured SBR incorporated with various RPOs types and
PCA content. This increase, too, can loadings
be explained by the improvement in
RPO-SBR-filler compatibility and the
state-of-mix, as well as the decreased
crosslink density and increased
plasticisation.

Compression set is generally used

to represent the capability of an
elastomeric matrix to maintain its
elastic contribution after prolonged
compressive stress at a given test
temperature. Figures 11 and 12
demonstrate the compression sets at
70°C and 100 °C of the vulcanisates
with various loadings and types of
RPOs. For any given loading there is
no significant change in compression Figure 11. Compression set at 70 °C of SBR vulcanisates incorporated with
set with increasing aromatic and various loadings and types of RPOs
PCA content, regardless of the
test temperature. By contrast, with
an increase in RPO loading, the
compression set increases at any given
aromatic content. These observations
result from the promotion of molecular
flow due to a decrease in crosslink
density in association with enhanced
plasticisation.

4. Conclusions
The present work investigated the
effect of aromatic and polycyclic
aromatic compounds (PCAs) in
rubber processing oils (RPOs) on
the processability and mechanical
properties of styrene butadiene rubber Figure 12. Compression set at 100 °C of SBR vulcanisates with various loadings
(SBR) compounds and vulcanisates. and types of RPOs
From the results obtained, it can
be stated that the variation with
aromatic content in RPOs affects the
state-of-mix (i.e., enhancement of
the Payne effect via the increase in
compatibility between RPO and SBR
matrix), but plays no significant role
on other physical properties such as
bulk viscosity and cure characteristics.
In contrast, the cure efficiency and
bulk viscosity in SBR compounds
are dominantly influenced by RPO
loading. Furthermore, by incorporating
the RPOs into the SBR compounds,
some mechanical properties, including
the elongation at break and tear

Polymers & Polymer Composites, Vol. 22, No. 7, 2014 605

 Yotwadee Chokanandsombat and Chakrit Sirisinha
strength, of cured SBR are improved.
The increases in these properties
with oil loading are attributed to
the decreased crosslink density and
increased plasticisation. The effect
on these mechanical properties is
slightly greater for the RPOs with
high aromaticity and PCA content.
Nevertheless, the aromatic and PCA
contents have relatively slight influence
on the hardness and compression set
of rubber vulcanisates.
Acknowledgements
The authors would like to acknowledge
the IRPC Plc. Co., Ltd. for kindly
supplying RPOs with various aromatic
and PCA contents. The authors also
gratefully acknowledge the Center of
Excellence for Innovation in Chemistry,
PERCH-CIC for the financial support
of this research. Finally, it is a pleasure
to acknowledge Prof. Dr. Alastair M.
North for his valuable suggestion and
supervision.
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