Slovak Journal Vol. 27, 2019, No.

1, 25 – 31
of Civil Engineering DOI: 10.2478/sjce-2019-0004

CHARACTERIZATION OF BITUMEN BINDERS ON THE

BASIS OF THEIR THERMO-VISCOUS PROPERTIES

Michal HOLÝ 1 * , Eva REMIŠOVÁ 1

Abstract Address

Bitumen is one of the basic building materials that is mainly 1

Dept. of Highway Engineering, Faculty of Civil Engineering,
used in road construction. Nowadays, we can observe in- University of Zilina, Zilina, Slovakia
creased requirements for the quality of bituminous binders,
which are due to increased traffic loads, changing climate con- * Corresponding author: [email protected]
ditions, and decreasing crude oil stocks. Besides "traditional"
(empirical) tests (softening point, penetration), new types of Key words
tests have been developed that can better describe the quality
and behavior of bitumen binders. Their composition can also ●●  iscosity temperature susceptibility;
V
●● Bitumen;
be a significant part of the properties themselves. Therefore,
●● Bitumen composition;
the elemental and group composition of bitumen must also
●● Empirical tests.
be observed. The use of the viscosity temperature susceptibility
(VTS) test appears to be well suited to evaluate the properties
of bitumen binders. The VTS parameter is directly dependent
on the viscosity of bitumen, but it is necessary to say that VTS
can be significantly affected by the composition of the bitu-
men. The paper is focused on determining the dependencies
between the VTS and the bitumen´s composition, respectively,
to find out how the composition influences the VTS.

1 INTRODUCTION also contains minor quantities of metals such as vanadium, nickel,

iron, magnesium, and calcium, which occur in the form of inorganic
Bitumen is a complex of high-boiling or non-boiling components. salts and oxides or in porphyrin structures.
These components do not change during the distillation process of The chemical composition of bitumen is extremely complex.
crude oil, which is the reason they are still present in bitumen in their Thus, a complete analysis of bitumen (if it were possible) would be
original unaltered form as in crude oil. Therefore, bitumen, like crude extremely difficult and would produce such a large quantity of data
oil, is a natural product. As far as its chemical composition is con- that any correlation with its rheological properties would be imprac-
cerned, we must realize that for any type of bitumen, as with any tical, if not impossible. However, it is possible to separate bitumen
type of crude oil, we do not yet know completely know it. This can into two broad chemical groups called asphaltenes and maltenes as
be explained by the fact that each type of bitumen is composed of a shown in (Nicholls, 1998; Read and Whiteoak, 2003). Maltenes can
large number of different groups of hydrocarbons that have an aver- be further subdivided into saturates, aromatics, and resins (SARA).
age molecular weight of 600 to 1000 g/mol as well as a relatively high The four groups are not well defined, and there is some overlap be-
proportion of non-hydrocarbons. tween the two main divisions. Based on the precipitation from lower
Bitumen is a complex chemical mixture of molecules that are pre- alkali hydrocarbons, saturated compounds can be included together
dominantly hydrocarbons (carbon: 82 to 88%, hydrogen: 8 to 11%) with aromatics and resins in the malten phase and asphaltenes in
with a small amount of structurally heterocyclic species and func- the asphalt phase (Fig. 1). Asphaltenes can be considered as solid
tional groups containing sulfur, nitrogen, and oxygen atoms. Bitumen particles that thicken bitumen binders. They have a dark brown or

CHARACTERIZATION OF BITUMEN BINDERS ON THE BASIS OF THEIR THERMO-VISCOUS PROPERTIES 25

Slovak Journal of Civil Engineering Vol. 27, 2019, No. 1, 25 – 31

Fig. 1 Schematic diagram of the colloidal structure of a bitumen

(Nicholls, 1998)
Fig. 2 Types of equipment and requirements for bituminous binders
sometimes a black color and a higher molecular weight compared to
according to the performance-related approach (Shafiq, 2016)
resins. Asphaltenes can be characterized as aromatic and chlorinated
solvents and also as insoluble in low boiling alkanes. Resins can be
that is influenced by the source of the petroleum and the processing
described either as highly viscous liquids or solids of a reddish-brown
method for the bitumen.
color. It can be stated that asphaltenes are the most important parts of
The main aim in the application of new procedures for determin-
bitumen binders that are dispersed in maltenes and that the resin has a
ing functional characteristics is to become much better in assessing,
significant effect on the stability of the asphaltenes that are dispersed
evaluating, or optimizing bituminous binders. A description of the be-
in the resin. Bitumen from different sources of crude oil has different
haviour of bitumen is used in finished designs that best fits the actual
amounts of constituents and possibly different abilities to react, and
conditions and takes into account factors such as temperature chang-
each manifestation of a change in the behavior of bitumen (such as
es, load changes, or the overall load dynamics of road construction.
aging, etc.) is due to the inter-conversion of one type of constituent
A bitumen binder is considered to be a relatively complex material,
to another type.
and a description of its properties is very demanding. To a great extent a
Currently, the producers of asphalt mixtures use their own tech-
functional approach emphasizes the rheology, which is an important as-
nological processes for improving their quality and ensuring the re-
pect with respect to the viscoelastic nature of bitumen binders. The basic
quired applicability of the products. The required quality is achieved
variable in rheology that characterizes the flow behavior of the material
by ensuring the quality of the materials input, i.e., coarse and fine
is viscosity, and one way of describing the properties of bitumen binders
aggregates and bitumen. The properties of the bitumen are verified by
could be the use of viscosity. In recent years, due to progressive using of
prescribed tests, which the bitumen binder must satisfy and which are
modified bitumen binders, most of research activities were focused on
critical to the designation and definition of bitumen binders. The cri-
measuring of rheological and creep properties as a complex shear modu-
teria for the quality of the bitumen are defined in EU standards and in
lus. Within the scope of the SHRP program in the United States (Peters-
Slovakia in catalog sheets for bitumen (CASB, 2014). The datasheets
en, 1994) the visocisty was studied as performance-related specification
determine how to use bitumen binders for the production of mixtures
to assess the optimal temperature of bitumen during mixing, laydown
for wearing and base courses and binders.
and compaction of asphalt mixtures. Therefore the paper is focused
The quality of the bitumen binders used in the construction and
on thermo-viscous characterisation of bitumen binders. The research is
maintenance of road pavements is currently being assessed by em-
rather focused on the possibility of reducing viscosity by various addi-
pirical tests that were designed around 100 years ago and are based
tives (Peilong and et al, 2018) and consequently reducing the working
on obtaining one value for specific boundary conditions. The consis-
temperatures of WMA mixtures (Kataware and Singh, 2017).
tency of the binders at medium service temperatures (penetration),
increased service temperatures (the softening point), and lower tem-
peratures (the breaking point) is measured, regardless of the compo-
sition of the bitumen and the loads corresponding to actual loads on a
2 VISCOSITY-TEMPERATURE SUSCEPTIBILITY
road. Research work on bituminous binders and asphalt mixtures was
The temperature susceptibility of bitumen is characterized as a
based on the assumption that empirical tests could characterize and
change in its consistency (viscosity or penetration of the bitumen)
classify but not accurately describe the properties of bitumen binders
due to a change in temperature. In (Mallick and El-Korchi, 2009; EN
as viscoelastic materials. The current state of asphalt roads has led
12591, 2009), three parameters can be used to determine the tempera-
to new methods and approaches being sought to better describe the
ture susceptibility of bitumen, i.e., the penetration index (PI), the pen-
properties of bitumen binders and mixtures. One such approach is the
vis number, and the viscosity-temperature susceptibility. The values
“performance-related” approach (Read and Whiteoak, 2003; Shafiq,
of PI are calculated using the following equations:
2016). The system mainly evaluates bitumen binders by thermal sta-
bility tests (short-term RTFOT and long-term PAV) and functional
(1)
tests that determinine the stiffness modules using a dynamic rheome-
ter (DSR) and a deflection beam rheometer (BBR). Bitumen binders
and
are tested not in the state in which they leave a refinery, but in the
state in which they leave an asphalt mixing plant or after a certain
(2)
period of exposure in service on a road (Fig. 2). Primary emphasis is
given to the characterization of their rheological behaviour, i.e., vis-
where penT1 is the penetration value at a temperature of 25o C, and
coelastic behaviour, as a function of the temperature and loading rate.
SP is the temperature of the softening point. Higher values of PI indi-
The behavior of bitumen is primarily seen as a chemical composition

26 CHARACTERIZATION OF BITUMEN BINDERS ON THE BASIS OF THEIR THERMO-VISCOUS PROPERTIES

Slovak Journal of Civil Engineering Vol. 27, 2019, No. 1, 25 – 31

important property of paving bitumen, can argue that paving asphalt

temperature susceptibility either does not exist, is not significant, or
is merely the result of an experimental error.

3 EXPERIMENTAL PROGRAM

The aim of the experimental measurements was to determine the

dependencies between the thermo-viscous and empirical properties
(penetration and softening point) and the composition (group and el-
ementary composition) of the bitumen. The purpose of the laboratory
measurements was to study the properties of binders for the produc-
tion of asphalt mixes that are commonly used in practice for asphalt
pavement construction, i.e., paving grade bitumen 50/70 (6 samples
from different producers, marked A1 – A6) and polymer-modified bi-
tumen PMB 45/80-75 (5 samples from different producers, marked
M1 – M5).
The viscosity-temperature susceptibility was determined by a dy-
namic viscosity data evaluation within a temperature range of 120o
to 180o C. The dynamic viscosity measurements were performed
according to EN 13302 using a Brookfield DV-II+PRO viscometer
model with a cylindrical spindle. The empirical properties were deter-
Fig. 3 Graph illustrating different temperature susceptibilities of
mined by conducting the softening point (STN EN 1427, 2015) and
paving bitumen (Mallick and El-Korchi, 2009)
penetration tests (STN EN 1426, 2016).
To realize an elementary analysis and determine the Carbon (C),
cate a lower susceptibility to the temperature. The viscosity-tempera- Hydrogen (H), Nitrogen (N) and Sulphur (S)content, an Elementar
ture susceptibility parameter is determined from the relation between Vario Cube with TCD detection was used. The test was performed by
the viscosity values at a certain temperature. As shown in Figure 3 means of a controlled sample combustion process at a temperature
(ASTM D4402, 2016), a straight line graph results when the log-log of 800 to 1000o C followed by an analysis of the flue gases by the
viscosity of a bitumen is plotted versus the log of its absolute tempera- detector. To determine the content of structurally similar compounds,
ture. The slope of this line provides the temperature susceptibility of a SARA analysis (determining the percentage of saturated hydrocar-
the bitumen. Figure 3 illustrates the temperature susceptibility of three bons, aromatics, resins, and asphaltenes) was carried out using the
bitumens, all of which have the same consistency at 25o C (77o F). combined extraction method and liquid chromatography. These pro-
The viscosity-temperature susceptibility is determined as: cedures required special equipment and chemical agents (n-heptane,
toluene, alumina 507C sorbent, silver nitrate modified silica gel) and
(3) specialized laboratories (VŠCHT, 2017). These analyses were carried
out at the Institute of Oil and Alternative Fuels VŠCHT in Prague.
The viscosity-temperature susceptibility (VTS) has been promot-
ed by the Asphalt Institute (Mallick and El-Korchi, 2009) as a cri-
terion for paving grade bitumen temperature susceptibility. In this 4 RESULTS AND ANALYSIS
approach, the VTS is based on the difference in the log log viscosity
at each of two temperatures, usually 135o C (275o F) and 60 oC (140o The results from the tests of the empirical properties of the bi-
F), which are divided by the difference in the logs of the same two ab- tumen, which were based on a performance-related approach and
solute temperatures. This equation reduces temperature susceptibility composition analysis, are listed in subsequent sections of this paper.
to a very small number, since for example, the value of loglog1000 Table 1 shows the average values of the group and elementary com-
is only 0.4771 and only 0.4312 for 500, with the difference between positions of the paving grade bitumen 50/70 (6 tested samples: A1
them only being 0.0459. With such small numbers, the supporters – A6) and the polymer-modified bitumen 45/80-75 (5 tested samples:
of VTS, who refuse to admit that temperature susceptibility is an M1 – M5). From the results of the chemical composition analysis,

Fig. 4 Equipment for the tests performed (from the left: penetration, softening point, elementary analysis, group analysis)

CHARACTERIZATION OF BITUMEN BINDERS ON THE BASIS OF THEIR THERMO-VISCOUS PROPERTIES 27

Slovak Journal of Civil Engineering Vol. 27, 2019, No. 1, 25 – 31

Tab. 1 Content of components in the bitumen samples tested

Content of components in samples (%)

Type of bitumen Saturates Aromatics Resins Asphaltenes
50/70 6.17 - 10.09 32.9 - 37.76 39.09 - 48.24 10.53 - 17.54
Average 50/70 8.41 36.03 42.41 13.15
PMB 45/80-75 6.18 - 11.62 33.03 - 34.71 37.09 - 47.73 12.52 - 15.02
Average PMB 45/80-75 8.50 35.62 40.65 15.23
Type of bitumen C H N S
50/70 82.7 - 85.29 9.92 - 10.45 0.371 - 0.712 3.21 - 6.12
Average 50/70 84.50 10.26 0.58 3.95
PMB 45/80-75 84.31 - 85.35 10.15 - 10.39 0.476 - 0.581 2.99 - 4.72
Average PMB 45/80-75 84.96 10.37 0.54 3.64

it can be stated that the greatest difference is between the PMB and C, and the range of penetration is from 54.6 to 74.3 x 0.1 mm. The
PG in the aromatics content (the PG has a +1.76% higher content of results are within the prescribed limits defined in the specifications
aromatics compared to the PMB) and asphaltenes (the PMBs have for bitumen. Influence of bitumen composition on empirical proper-
a +2.08 % higher content of asphaltenes compared to the PG). In ties is more specifically described in the paper “Impact of bitumen
the group composition we can see that the paving grade bitumen has composition on empirical properties” (Remišová and Holý, 2018). In
higher values of aromatics and resins, while the polymer-modified bi- research have been found intermediate dependencies have been dis-
tumen has higher values of saturates and asphaltenes. From the point covered between binder penetration and aromatics content (correla-
of view of the elemental composition, we can see that both types of tion in range of 0.64 PG bitumen to 0.48 PMB bitumen), softening
bituminous binders have relatively the same nitrogen and hydrogen point and resins content (correlation in range of 0.785 PG bitumen
contents and that the differences can be observed in the carbon (the to 0.469 PMB bitumen), penetration and carbon content (correlation
PMB has a +0.46% higher C content when compared to the PG) and in range of 0.86 PG bitumen to 0.76 PMB bitumen), softening point
sulphur (the PG has a +0.31% higher S content when compared to and hydrogens content (correlation in range of 0.73 PG bitumen to
the PMB) content. Differences in the specific numerical values of the 0.999 PMB bitumen).
contents of the individual components are influenced by the origin of The VTS values were calculated according to the equation men-
the crude oil itself as well as by the technological processes used in tioned above. The dynamic viscosity measurement values (recorded
refineries in the production of bitumen binders. by a Brookfield viscometer at 120,130,135,140,150,160,165,170, and
As mentioned above, the quality of the bituminous binders was 180° C) were used for determining the VTS. The VTS values calcu-
verified by empirical tests that are defined in the standards (EN 1426, lated for both the modified and paving grade bitumen are in Table 3.
2010; EN 1427, 2010), or catalog sheets (CSAB, 2014), of bitumen The modified bitumen has lower VTS values (from -1.081 to 1.199)
binders. A “suitable” bitumen is a bitumen that meets the condition compared to the paving grade bitumen (from -1.287 to 1.480).
that the measurement value of the bitumen is either between two
boundaries for PG bitumen (penetration or a softening point) or the Tab. 3 Values of the VTS for modified and paving grade bitumen
value of the measured property is higher than the minimum limit (as
is the case with the softening point of the PMB). The values from the The value of the VTS (-)
measurements of the softening point and penetration of the bitumen
binders tested are presented in Table 2. Despite using the same grade A1 A2 A3 A4 A5 A6
Bitumen 50/70
of bitumen, we can observe a relatively high degree of variability in -1.322 -1.336 -1.416 -1.364 -1.480 -1.287
the results. In the case of the paving grade bitumen, the range of the
softening points is from 48o C to 51o C, and the range of penetration M1 M2 M3 M4 M5 -
is from 54.3 to 70.03 x 0.1 mm. In the case of the polymer-mod- PMB 45/80-75
-1.111 -1.081 -1.199 -1.111 -1.115 -
ified bitumen, the range of softening points is from 75.4o C to 86o

Tab. 2 Measured values of the penetration and softening points

Bitumen 50/70 Bitumen PMB 45/80-75

Parameter
A1 A2 A3 A4 A5 A6 M1 M2 M3 M4 M5

Penetration (0.1mm) 64.1 63.8 62.8 61.0 70.0 54.3 54.3 54.6 74.3 60.5 51.6

Softening point (°C) 49.8 49.8 49.0 48.0 49.0 51.0 85.2 80.8 75.4 78.4 86.0

28 CHARACTERIZATION OF BITUMEN BINDERS ON THE BASIS OF THEIR THERMO-VISCOUS PROPERTIES

Slovak Journal of Civil Engineering Vol. 27, 2019, No. 1, 25 – 31

Tab. 4 Linear dependencies between the VTS parameter and the elemental and group composition of bitumen

Coefficient of determination R2
Parameter
Saturates Aromatics Resins Asphaltenes C H N S
Bitumen 50/70 0.482 0.368 0.605 0.150 0.469 0.881 0.215 0.565
Bitumen PMB 45/80-75 0.305 0.001 0.108 0.109 0.512 0.938 0.119 0.594
Parameter Resins/Asphaltenes Aromatics/Asphaltenes Asphaltene index H/C
Bitumen 50/70 0.280 0.478 0.781 0.674
Bitumen PMB 45/80-75 0.104 0.131 0.166 0.897

In the following steps, the relationship between the VTS and the The highest correlation dependencies are shown between the VTS and
elemental respective group composition of the bitumen for a partic- hydrogen content (Figure 5). The values of reliability in the relation
ular bitumen was studied. If a relationship exists, it is important to between the VTS and hydrogen are in a range from 0.881 (for paving
know how greatly the elemental versus group composition of the grade bitumen) to a value of 0.9383 (for polymer-modified bitumen),
bitumen influences the VTS of the bitumen binders. The relation which means a correlation in a range of 0.968 (polymer-modified bitu-
between the VTS and elemental composition and the group compo- men) to 0.938 (paving grade bitumen). These values of the correlation
sition versus the empirical tests (softening point and penetration) is show that between the VTS and hydrogen, some dependence exists.
expressed by a linear function. High dependencies can also be observed with the sulphur and res-
The regression dependences and penetration (Figure 4) of the in content (the PG bitumen). In addition to the group and elemental
VTS show a high value of the determination coefficient R2 for both analysis, the dependence of the most important combination of the in-
types of bitumen, i.e., polymer-modified bitumen and paving grade dividual parameters commonly used in foreign research was observed
bitumen. The values of reliability in the relation between the VTS and to examine whether there is any dependence between the VTS and the
penetration are in a range from 0.624 (for paving grade bitumen) to given ratios (e.g., a high H/C ratio indicates the presence of straight-
a value of 0.799 (for the polymer-modified bitumen), which means a chain compounds, whereas a low H/C ratio is a good indication of the
correlation in a range of 0.789 (paving grade bitumen) to 0.893 (poly- presence of polynuclear aromatic systems. Very high dependencies
mer-modified bitumen). The relationship between the softening point have been shown in the H/C ratio for both types of bitumen (0.674
and the VTS was also examined. However, the dependencies were for the PGB and 0.897 for the PMB) and in the asphaltene index for
small (R2 = 0.386 for the PGB and R2 = 0.359 for the PMB). the PG bitumen (R2 = 0.781).
The linear dependencies between the VTS and elemental and The results of the regression analysis of the bitumen´s group
group composition determined of the bitumen are shown in Table 4. composition and viscosity-temperature susceptibility are in Table 4.

Fig. 5 Regression dependences between the VTS and penetration - PG bitumen (left), PMB bitumen (right)

Fig. 6 Regression dependences between the VTS and hydrogen content of the PG bitumen (left), PMB bitumen (right)

CHARACTERIZATION OF BITUMEN BINDERS ON THE BASIS OF THEIR THERMO-VISCOUS PROPERTIES 29

Slovak Journal of Civil Engineering Vol. 27, 2019, No. 1, 25 – 31

A relatively good level of regression was determined with the content Acknowledgment
of the saturates and resins (Figure 6). The values of reliability in the
relation between the VTS and resins show a value of 0.605 (the PGB The research was partially supported by the Scientific Grant
bitumen) and the values in the relation between the VTS and saturates Agency of the Ministry of Education, Science and Sport of the Slovak
show a value of 0.108 (the PMB bitumen), which means there is a Republic and Slovak Academy of Science VEGA Grant No.1/0300/17
correlation in a range of 0.777 (the PGB) to 0.522 (the PMB). These - Research of performance-related and rheological properties of bitu-
values of correlation show that between the VTS and resins, some minous binders.
dependence exists.

5 CONCLUSIONS

The quality of the bituminous binders used in the construction and

maintenance of road surfaces is currently being assessed by empirical
tests based on obtaining one value for specific boundary conditions.
A characteristic feature of bitumen binders is that they change their
consistency and properties with the temperature. The use of a viscos-
ity-temperature susceptibility test that is influenced by the composi-
tion of the bitumen appears to be well-suited for an evaluation of the
properties of bitumen binders. The goal of the presented paper was to
determine the correlation between the VTS parameter and the phys-
ical properties and composition in the form of elemental and group
compositions of unmodified and modified bitumen samples.
The values of reliability in the relation between the VTS and pen-
etration are in a range from 0.624 (for the paving grade bitumen) to a
value of 0.799 (for the polymer-modified bitumen). The relationship
between the softening point and the VTS was also examined. How-
ever, the dependencies were only very small (R2 = 0.386 for the PGB
and R2 = 0.359 for the PMB). In addition to the group and elemental
analyses, high dependencies were shown with the H/C ratio for both
types of bitumen (0.674 for the PGB and 0.897 for the PMB) and with
the asphaltenes index for the PG bitumen (R2 = 0.781). In the case
of the elemental composition, the values of reliability in the relation
between the VTS and hydrogen content were in a range from 0.881
(the paving grade bitumen) to a value of 0.9383 (the polymer-modi-
fied bitumen). These values of the correlation indicate that between
the VTS and hydrogen content, some dependence exists. Relatively
good correlations were determined between the VTS and resin con-
tent with a value of reliability of 0.605 (for the paving grade bitumen)
and between the VTS and saturates content with a value of 0.108 (for
the polymer-modified bitumen). The results show that the VTS is not
only dependent on viscosity but is also significantly dependent on the
penetration and the group and elemental compositions.

30 CHARACTERIZATION OF BITUMEN BINDERS ON THE BASIS OF THEIR THERMO-VISCOUS PROPERTIES

Slovak Journal of Civil Engineering Vol. 27, 2019, No. 1, 25 – 31

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CHARACTERIZATION OF BITUMEN BINDERS ON THE BASIS OF THEIR THERMO-VISCOUS PROPERTIES 31