VISKOSITNÍ VLASTNOSTI VZDUCHOVANÉHO VISCOUSU BITUMEN

VISCOSITY FEATURES OF AIR-RECTIFIED VISCOUS BITUMEN

PhD in Engineering sciences, Yan Pyrig, KNADU, Kharkiv, Ukraine

Anotace
Viskozita je základním ukazatelem kvality asfaltu, který umožňuje vyhodnotit jejich strukturní a
reologické vlastnosti a předpovědět chování obou pojiv a asfaltových betonů na nich založených. V
práci jsou uvažovány vlastnosti reologických charakteristik oxidovaného asfaltu. Bylo zjištěno, že v
důsledku rozdílů v konstrukčně-reologickém typu je viskozita oxidovaných asfaltů při teplotě 60 °C
podstatně nižší než viskozita destilačních bitumenů odpovídající penetraci. S nárůstem teploty na
135 °C jsou vyrovnány rozdíly ve viskozitách asfaltů vyráběných různými technologiemi. Je uvažován
vliv stárnutí na viskozitní charakteristiky oxidovaného asfaltu. Bylo zjištěno, že u bitumenů vyrobených
ze stejné suroviny a za použití stejné technologie může být viskozita starých bitumenů bez ohledu na
zvolenou metodu stárnutí stanovena výpočtovou metodou s použitím jejich průnikových hodnot.

Abstract
Viscosity is a fundamental indicator of the bitumen quality, which allows to evaluate the structural and
rheological features of both binders and asphalt concrete based on them, as well as to predict their
behavior. Features of the air-rectified bitumen rheological characteristics are discussed in the article. It
is found that due to differences in the structural-rheological type, the viscosity of air-rectified bitumen
at 60 °C is substantially lower than the viscosity of the close penetration distillation bitumen. With a
temperature shift up to 135 ºС, differences in viscosities of bitumen produced by different technologies
are minimized. The influence of a short-term aging on the viscosity characteristics of air-rectified
bitumen is considered. It is found that for bitumen produced from the same crude under the same
technology, the viscosity of aging bitumen can be calculated by their penetration values regardless of
the accepted method of aging.

Introduction
In the European Union the quality of the pavement bitumen is estimated by the indicators that can be
divided on conventional and fundamental. The commonly used indicators, such as penetration,
softening point temperature and Fraas breaking temperature are classified as a conventional. The
values of these indicators are substantially caused by the test conditions (longevity and a rate of the
load implement, temperature and etc.). Due this the values of conventional indicators can’t be used for
the completely and precise predicting of technological and performance characteristics of the
pavement bitumen and asphalt concrete.
Viscosity is referred to the fundamental characteristic foremost. Using viscosity characteristics for a
bitumen quality evaluation enabling an estimation of the structure-rheology features of the binders [1,
2] and their temperature susceptibility [1 – 3], rationing the mixing and compacting temperatures of the
asphalt concrete mixtures [4] and predicting the performance of the binders and asphalt concrete with
them at a wide range of temperature [5].
The common using of the rheology indicators observed in 60-th last century, when the viscosity
system of the bitumen quality evaluation (ASTM D3381) was designed and implemented in the USA.
Though it wasn’t got in common use (now days it is operated in some USA states, Australia, India and
partly in Canada and New Zealand) it initiates the implementation of the viscosity methods (dynamic
viscosity at 60 °C and kinematic viscosity at 135 °C) in the bitumen quality evaluation systems all over
the world.
Till 2017 in Ukraine viscosity was out of the binder quality system, it wasn’t referred in the government
bitumen standards and used in research centers only. The harmonization of the ДСТУ EN 12591:2017
standard [6] caused the need in viscosity values finding at 60 ºС и 135 ºС. Initially EN 12591 was
aimed to estimate the quality of distillated bitumen, which commonly used in Europe. Its test
conditions can be unsuitable for the air-rectified bitumen that mostly presented in the Ukraine and
characterized by the different colloidal type. Taking this into account, as a low level of an equipment
supply in production laboratories it is valuable to investigate the methods of the viscosity assessment
and finding the relationship of bitumen viscosity values with the conventionally quality indicators of the
bitumen (penetration, softening point temperature and etc.).

Objectives of the Research

The comparative analysis of the viscosity values on the distillated bitumen (that is in use in Europe
Union) and on air-rectified bitumen (that is in use in Ukraine) is the aim of this work. The rheology
quality indicators was find in a wide temperature and share rate range for both – distillated and air-
rectified bitumen on purpose of the research.

Materials of the Research

The rheology indicators finding for air-rectified bitumen is undertaken on the bitumen produced in the
research laboratory. For this purpose petroleum crude (bitumen with a penetration 214 × 0.1 mm and
a softening point 37.2 °C) has been blown with an air in a laboratory oxidation column for getting 7 air-
rectified bitumen samples (B0 … B6) in a penetration range from 40 × 0.1mm to 193 × 0.1 mm. For
the rheology researches as distillated bitumen the Nynas (Akzo Nobel, Sweden) bitumen in a same
penetration range are chosen. The values of conventional quality indicators of all these bitumen are
given in Table 1.
Considering the intermediate “sol-gel” structural type (with a tendency to “gel”) inherent to the air-
rectified bitumen, the condition of approaching its penetration value at the softening point temperature
to the 800 × 0.1 mm level isn’t fulfilling. Due this the calculation of the penetration index using the
softening point temperature (ІРТр) with the EN 12591-2009 equation is unacceptable, because it can
leads to the misconception about a bitumen structural type. According to this for the each bitumen
penetrations are found at different temperatures in a range from + 5 °C to + 35 °C. On these data the
penetration-temperature dependences are plot and used for the temperature values finding at
800 × 0.1mm penetration level (Т800). Then the index penetration ІРТ800 is calculated for the all bitumen
with the EN 12591-2009 equation, replacing the softening point temperature by the experimentally
found temperature Т800 (form. 1) [7]. According to the calculated values ІРТ800 distillated bitumen can
be described as sol structure bitumen, while the type of air-rectified bitumen “get” closer to the gel
one.
20  Ò800  500  lg Ï 25  1952
IP800  (1)
Ò800  50  lg Ï 25  120
The values of the dynamic viscosity is obtained for each one bitumen in this work by the spindle
rheometer “ПВР-2” at a wide range of temperatures (+ 25 ºС … + 160 ºС) and shear rates (1,6 …
200 с-1). On the base of this data the temperature-viscosity are plot and set the values of the viscosity
at 60 ºС и 135 ºС and 40 s-1 shear rate.

Table 1: Properties of chosen for the study bitumen

Indicators of the bitumen quality

Penetration Softening Penetration Viscosity, Viscosity
Bitumen at 25 ºС, point index Pа×s at anomaly at
0.1 mm temperature,
ºС ІРТр ІРТ800 60 ºС 135 ºС 60 ºС 135 ºС
(distillation)

NB1 60 48.9 -1.05 -2.42 630.96 1.45 0.88 0.92

Nynas

NB2 84 45.7 -1.08 -1.61 436.52 0.80 0.98 0.98

NB3 141 43.0 -0.30 -1.46 251.19 0.58 0.98 1.00
NB4 189 39.2 -0.64 -1.20 141.25 0.44 1.00 1.00
B6 40 60.6 0.61 1.33 630.96 3.25 0.53 0.96
B5 61 52.6 -0.08 0.36 501.19 1.42 0.78 0.96
(air-rectified)
laboratory

B4 82 47.9 -0.51 0.07 316.23 1.00 0.80 0.98

B3 120 44.6 -0.33 -0.03 135.52 0.73 0.81 1.00
B2 130 43.3 -0.49 -0.08 104.95 0.67 0.83 1.00
B1 179 41.2 -0.02 -0.11 90.36 0.49 0.90 1.00
B0 193 40.7 0.11 -0.19 77.09 0.39 0.92 1.00
Analysis of bitumen viscosity characteristics
The viscosity-penetration dependencies, obtained in this study, are given in figure 1 for the both –
distillated and air-rectified bitumen. Due to the analysis of this dependencies the viscosity at 60 °C of
the distillated bitumen in a 1.6 – 1.8 times higher than the one of the air-rectified bitumen with the
equal penetration.

Figure 1: Dependence of viscosity at 60 ºС and 135 ºС on penetration of air-rectified and

distillation bitumens

The difference in the viscosity values at 60 °C can be caused by the different colloidal type of the air-
rectified and distillated bitumen. “Sol-gel” and “gel” type bitumen (to which air-rectified bitumen are
refer) are characterized by a presence of a coagulation structural net of asphaltenes and high amount
of low molecular weight hydrocarbons [8], which results in higher softening point temperatures. For the
example bitumen NB1 and B5 with the same penetration 60 × 0.1mm have a 3.7 °C difference in a
softening point temperature, while bitumen NB2 and B4 with the 82 and 84 penetration respectively
have a 2.2 °C difference in a softening point temperature. Due the features of the air-rectified bitumen
structure there is a significant difference in a viscosity of the intact and totally ruined structure
(especially at a temperature less than 90 – 100 °C). This is a reason of the viscosity anomaly
appearing (Figure 1, Table 2). After the structural net ruining the “sol-gel” and “gel” type bitumen
viscosity is causing by the low molecular weight hydrocarbon medium, which, in comparison with the
resins, has much lesser viscosity.
Distillated bitumen by their colloidal type generally are identified as a “sol” type, that is described as a
“suspension of asphaltenes in a highly structured by resins dispersion medium” [8]. These kinds of
bitumen are characterized by the absence of the yield strength and a difference between values of
intact and totally ruined structure as a consequence.
The viscosity anomaly that inherent to air-rectified bitumen at 60 °C makes to set the normalized value
of the shear rate in the viscosity test, or to measure the viscosity value at the most possible low shear
rates, that can make difficulties in the case of hard air-rectified bitumen.
At the temperature 135 °C the values of distillated and air-rectified bitumen viscosity are getting close
to each other at the equal penetration. The reason is that at such a high temperature the
microstructure bonds are ruined in binder, its viscosity depends only on the viscosity of low molecular
weight hydrocarbons [7], which is close as for the distillated as for the air-rectified bitumen.
 Figure 2: Dependence of viscosity at 60 ºС on the shear rate of air-rectified and distillation
bitumen

Rheological indexes of the binder, such as the other quality indexes, substantially changes both - at
the stage of asphalt mixture production, and at the stage of the further life cycle of the asphalt
concrete, due technological and performance hardening of the binder. During the hardening process
the viscosity values changes much more than the other quality indicators (penetration, softening point
temperature) [9 – 10].
In presented research the changing of the quality indicators as a result of air-rectified bitumen short-
time hardening by the method TFOT, that is implemented in the Ukraine road practice, is evaluated
and given in a Table 2.

Table 2: Changes in the quality indicators of air-rectified bitumen after aging by the TFOT
method

Values of quality indicators for bitumen

Quality indicators
B6 B5 B4 B3 B2 B1 B0
Retained penetration, % 82.5 83.6 76.8 68.3 70.8 61.5 57.0
Increase in softening point, ºС 3.3 2.8 2.6 2.6 2.4 2.4 2.7
Change of mass, % -0.018 -0.012 -0.016 0.001 -0.007 0.020 0.01
Viscosity, 60 ºС 1258.93 549.54 354.81 199.07 166.34 161.06 162.55
Pа × s at 135 ºС 3.20 1.77 1.34 0.91 0.73 0.60 0.62

The obtained experimental data show the increasing of the viscosity in 1.2 – 2.11 times for the all
bitumen grades. The rate of the viscosity changes is higher for the bitumen with the higher penetration
it means that the hardening is more significant when the viscosity of the binder is low. It is illustrated
by the data, given in Table 2. For the retained penetration of the hardened bitumen its value in the
case of the penetration 40 × 0.1mm is on the level of 82.5 %, while for bitumen with the penetration
193 × 0.1 mm the retained penetration reach the level of 57 %. At the same time the “Increase in
softening point” index almost unable to provide the information – whatever the bitumen grade is its
value stay on the level of 2.4 – 3.3 °C (Table 2). Due this the viscosity is the most sensitive index to
the changes of the bitumen properties during hardening.
The comparative analysis of the viscosity-penetration dependencies of initial and hardened bitumen
shows that for bitumen produced on the same crude by the same technology these dependencies can
be described by the common exponential equation with the high approximation level (Figure 3).
 Figure 3: Viscosity-penetration dependence of the original and hardened bitumen

The comparative data of the distillated and air-rectified bitumen hardened by the TFOT and RTFOT
method by the [9] confirming the gained results. The shown in Figure 4 dependencies proves that the
exponential equation is validate when the bitumen crude and produce technology are the same
irrelevant to the hardening method that was used in research.

Figure 4: Viscosity-penetration dependence of the original and hardened bitumen at 60 °С,

according to [7]

According to this for the refinery it is possible to calculate the equation of the viscosity-penetration
dependence of the petroleum bitumen (if the bitumen crude and produce technology aren’t changes)
and use it to express calculation of the viscosity values as for the initial as for the hardened bitumen.
Conclusions
1. The dynamic viscosity values at 60 °C are significantly higher for the distillated bitumen than for air-
rectified bitumen at the close penetration. At the 135 °C the viscosity values of the distillated and air-
rectified bitumen are almost identical.
2. The normalization of the dynamic viscosity values at 60 °C for the air-rectified bitumen is possible
only with the normalized shear rate setting. Otherwise the results will be incomparable.
3. It was found the possibility to calculate the viscosity values on the penetration data for the initial and
hardened by the different methods bitumen.
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