Introduction References Biography Contents
Pages 219 to 237
DYNAMIC SHEAR RHEOMETERS: MAKING
ACCURATE MEASUREMENTS ON BITUMENS
J Carswell, BP Oil International, Sunbury
M J Claxton, BP Oil International, Sunbury
P J Green, BP Oil International, Sunbury
ABSTRACT
The US Strategic Highways Research Programme (SHRP) has developed binder specifications
which require measurements with a Dynamic Shear Rheometer (DSR). However, precision
data for DSR measurements are limited and measurement methods have generally not been
standardised. This paper investigates two important sources of error: accurate temperature
control and appropriate test geometry selection. Key results were:
• 1°C temperature difference resulted in significant variations in measured binder properties.
• 20mm and 25mm parallel plate geometries had upper stiffness limits of 105Pa (gap 0.5-
2mm). For the 8mm plate this increased to 108Pa. Greater stiffnesses are affected by
machine compliance.
DSR test methods must be carefully defined to encompass such findings and other soures of
error (sample preparation, equipment calibration etc.).
Introduction Contents
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INTRODUCTION
In the USA, the Strategic Highways Research Programme (SHRP) has developed bitumen
specifications which classify the grade of a binder on the basis of its performance in a number
of rheological tests. Parameters specified include both the binder complex shear modulus (|G*|)
and the phase angle (δ) both of which are measured using a Dynamic Shear Rheometer (DSR).
Elsewhere, there is also an increasing interest in the use of fundamental rheological parameters
to specify binders. In Europe, the UK’s Highways Agency has issued performance-based
specifications for hot rolled asphalt (HRA) wearing courses using modified binders, which also
require the provision of binder rheological data using a DSR. In France a proposed method for
making rheological measurements has been the subject of a recent round robin exercise. In
Singapore, the SHRP grading system has been adopted when specifying PMBs. In making
these measurements, it is generally assumed that a DSR can accurately measure binder
properties over a wide range of conditions. However, the use of DSRs to characterise bitumen
properties is still in its infancy when compared with well established tests such as penetration,
softening point and viscosity. These tests recognise the importance of closely controlled
conditions and appropriate calibration to obtain reproducible results, particularly for
specification purposes. In contrast, for rheological measurements using DSRs, little work has
been reported to date to identify the factors which may affect the accuracy of results.
This paper discusses some of these factors and quantifies the effects of two important sources
of error: temperature control and sample test geometry.
FACTORS AFFECTING RESULTS ON BITUMENS
A number of factors affect the results of measurements on bitumens using a DSR:
Temperature control
Bitumen is a good thermal insulator and is also highly temperature susceptible. To make
accurate measurements it is important firstly, that the whole sample is at the same temperature
and secondly, that the temperature is accurately controlled. Temperature calibration is
sometimes carried out using a standard viscosity oil which is much less temperature susceptible
than bitumen. In such cases, inaccurate temperature control is much less evident than when
making measurements on bitumens.
Sample Geometry
Bitumen stiffness varies over several orders of magnitude over a relatively narrow temperature
range. DSR manufacturers offer a number of different geometries to measure the wide range of
stiffnesses encountered. However, it is often left to the individual to determine the most
appropriate geometry for the binder and there are no standard geometries which have been
identified for specific ranges of binder stiffness.
Sample Preparation
Conventional bitumen tests such as penetration, softening point and viscosity have long
recognised the importance of sample conditioning and thermal history in obtaining repeatable
and reproducible results. As a result of the SHRP program, a sample preparation method has
been proposed by AASHTO for use with bitumens (AASHTO 1995). A standard in-house
procedure for sample preparation was used for work in this paper.
Equipment Calibration
For calibration purposes, most DSR manufacturers carry out measurements of displacement and
applied torque and confirm such calibrations with measurements in steady shear on a standard
fluid. Unfortunately, these fluids are often low viscosity, Newtonian oils which are very
different in consistency from bitumen, where the range of stiffnesses encountered can be much
higher. Consequently, such calibrations can be misleading, particularly if measurements are to
be made on high stiffness binders.
Linear Viscoelasticity
Many viscoelastic materials such as bitumens do not behave linearly in terms of their stiffness
as a function of strain. Unless measurements are made at strains where the properties are
independent of the level of strain, then comparison with data from different instruments can be
very difficult. This is not discussed further in this paper, except to say that all results were
obtained in the region of linear viscoelastic behaviour.
The effects of temperature control and sample geometry will now be discussed in detail.
MATERIALS AND TEST METHODS
All work was carried out using two commercially available rheometers. DSR 1 had a 20mm
parallel plate (PP) geometry and DSR 2 had 8mm and 25mm PP geometries.
Effect of Temperature Control
The effect of temperature control was studied using an unmodified Class 320 binder, with a
measured viscosity at 60°C of 322 Pa.s.
Rheological testing was carried out using DSR 1 with two temperature control systems. The
first employed a standard Peltier system in which only the temperature of the lower plate was
controlled. This may present a source of error when making measurements on bitumens since
they are poor thermal conductors. To try to quantify the effect of thermal gradients across the
bitumen sample, results obtained with the Peltier temperature control system were compared
using a standard stainless steel upper plate and also a 'Tufnell' upper plate of lower thermal
conductivity. In addition, the effect of using an annular aluminium block around the sample to
try to minimise heat losses from the upper plate was also evaluated. Finally, the effect of water
around the sample as a means of improving heat transfer from the Peltier device to the upper
plate was assessed, in an attempt to obtain a more uniform sample temperature (Figure 1).
The second method of temperature control comprised an Extended Temperature Module
(ETM), which used electromagnetic induction heating of both the upper and lower plates.
It has been shown (Dobson, 1972) that the Williams-Landel-Ferry (WLF) equation, describing
the temperature dependence of viscosity for polymers, could be modified for bitumens :
C(4-log(η)) * K + Te = T (1)
(C-4+log(η))
where η is the viscosity in Pa.s, Te is the temperature at which the viscosity is 104 Pa.s, K is a
constant, T is the temperature in °C and C=8.86 (T≥Te) or 12.5 (T<Te). For a bitumen of
known viscosities at two or more temperatures the viscosity at any temperature may be
calculated. Alternatively, the temperature for a given viscosity may be determined. (Equation 1
is preferred to the reduced Walther equation since it gives a linear plot of viscosity over a wider
temperature range.)
To determine the effects of the different methods of temperature control, the viscosity of the
standard binder was measured in steady shear at 60°C using both temperature control systems
and compared with that obtained using the vacuum capillary method (AS 2341.2). (Both
systems were checked to determine the actual temperature settings required to obtain 60.0°C).
Two gap settings, 0.5 and 1.0 mm were used. Using equation (1), the equivalent temperature
for the measured viscosity was calculated for each geometry to determine whether accurate
temperature control was being achieved.
Effect of Sample Geometry
For the study of different geometries, unmodified 15 pen (much harder than a Class 600) and
200 pen (Class 50) bitumens were used to represent the hard and soft extremes of normal
paving grades.
To assess the effect of sample geometry, both DSRs were used in oscillation mode. In this
mode of operation, a sinusoidal stress is applied to the sample at different frequencies and a
resultant strain is measured. As mentioned previously, the level of strain was selected to be
within the linear visco-elastic region for the binders used. The complex shear modulus, |G*|,
and visco-elastic phase angle, δ, were measured under different temperature and frequency
conditions as shown in Table 1, for different plate diameters and gaps.
Table 1 DSR Test Conditions (Sample Geometry Study)
DSR 1 DSR 2 DSR 2
Strain 0.02 0.02 0.02
Plate diameter (mm) 20 8 25
Gap (mm) 0.01 0.1 0.01
0.5 0.5 1.0
2.0 2.0
Temperature (°C) 5-60 5-60 5-60
Frequency (Hz) 0.1-10 0.1-10 0.1-10
RESULTS
Temperature Control
Table 2 summarises the viscosity results obtained. Acceptable reproducibility of the vacuum
capillary method is defined as results from two laboratories having a difference of less than
12% of their mean value. Although this definition of reproducibility applies to results from a
single test method, it was used to assess agreement between the results using different methods
of temperature control in this study. On this basis, for a viscosity of 322 Pa.s, a result in the
range 303-341 Pa.s from the DSR 1 would be acceptable.
Table 2 Viscosities of the standard binder
System Gap Viscosity at 60°C
(mm) (Pa.s)
No mod Al Block Al Block/Water Jacket
ETM 0.5 345 - -
1.0 354
Peltier 0.5 540 460 420
(steel plate) 1.0 720 564 426
Peltier 0.5 413 365 387
(Tufnell) 1.0 500 383 383
Results using the ETM to heat the upper and lower plates show the closest agreement with the
AS 2341.2 method. However, none of the results meet the reproducibility criteria. The effect
of heating only one side of the sample is shown clearly in the results using the steel plate with
the Peltier system and to a lesser degree using the Tufnell plate. As expected, increasing the
gap resulted in a higher measured viscosity further away from that obtained using AS 2341.2,
indicating the problem of temperature gradients across the sample. Heating the air space
around the sample or use of a water jacket (particularly for the steel plate) improved the
agreement.
The viscosities and stiffnesses of bitumen are highly temperature susceptible. From equation
(1) a change of just ± 1°C at 60°C will change the viscosity of this bitumen by 45Pa.s i.e. a
variation from 282-367 Pa.s. Therefore, it is not surprising that AS 2341.2 specifies close
temperature control of the water bath in which the sample is immersed. Although the control of
temperature to this level of accuracy is well established for conventional tests on bitumen, it is
only relatively recently that such accuracy and precision have been available with modern
rheometers. The largest deviation in Table 2 (720Pa.s) corresponds to an average sample
temperature of just 54.2°C. The best measurement with the Peltier system (365Pa.s)
corresponds to an average sample temperature of 59.0°C and again indicates the problem of
heating the sample from one side only. The ETM gives better agreement and shows the benefit
of heating the sample both top and bottom. However, there were disadvantages found with
using this ETM for routine testing including difficulty in trimming the sample.
Developments within the industry have led to improvements and simplifications being made to
rheometers in order to make them more readily useable for routine testing. In order to achieve
accurate temperature control of the sample, a number of DSRs are now being marketed which
incorporate a water bath in which the sample is fully immersed. Provided sufficient time is
allowed for the sample to reach thermal equilibrium, accurate temperature control can be
achieved.
Plate Geometry
The results for the 15 pen and 200 pen bitumens are shown in Figures 2 to 8. Figure 2 shows
the data for the 15 pen bitumen as often presented in research papers. Initially, results appear as
would be expected with increases in |G*| and a gradual reduction in phase angle (δ) as the
binder becomes more elastic at higher frequencies and/or lower temperatures. However, closer
inspection of Figure 2 suggests that the limiting elastic stiffness for the 15 pen binder is not
around 109 Pa, the approximate value found for all bitumens, but a value closer to 108 Pa.
An alternative way of presenting these results is to plot |G*| and delta against temperature at a
single frequency. Figure 3 shows |G*| and δ at 0.4Hz for the 200 pen bitumen plotted against
temperature using the 8mm and 25mm parallel plates, using 0.5mm and 1mm gaps respectively.
Figure 4 shows results for the 15 pen bitumen.
From Figures 3 and 4, it is clear that there are differences between the results obtained using
the two sample geometries. These differences increase as the stiffness of the binder increases
or the temperature decreases. At 0.4Hz with the 200 pen bitumen, there are large differences in
δ with the two plate geometries at all temperatures below about 40°C while significant
differences in the values obtained for |G*| are seen below about 25°C. At 10Hz with the 15 pen
bitumen, significant differences in |G*| are obtained below about 35°C, while the values
measured for δ, are very different over nearly the entire temperature range.
To eliminate the effect of temperature on the results obtained, |G*| may be plotted against δ
over the temperature and frequency range used. In such a plot, δ decreases as |G*| increases
and the value of |G*| when δ is 0° should be the limiting stiffness of the bitumen i.e. 109 Pa.
Figure 5 and Figure 6 show these plots for the 200 and 15 pen bitumens respectively. The
following conclusions may be drawn from the data :
• The limiting value of |G*| (109 Pa) is never attained with either DSR for all the geometries
(plate diameter and gap) used.
• Extrapolating lines to the x-axis indicates different values of the limiting stiffness for the
different geometries all of which are significantly less than 109 Pa. The extrapolated value
for the limiting stiffness depends on both the DSR and sample geometry.
Figures 5 and 6 show very clearly that making measurements with plates of different diameters
can lead to quite different results and all are significantly less than the limiting stiffness of the
bitumen which would be expected at low temperatures. However, the diameter of the plate is
not the only variable when selecting a suitable test geometry. The user also selects the height
of the bitumen sample, or the gap.
Figure 7 shows the effect of different gap settings for each plate diameter on results for the 15
pen bitumen obtained using DSRs 1 and 2 (test frequency of 0.4Hz). With the gap set to 10
microns, surprisingly low and constant stiffness values of about 3-4x104 Pa were obtained for
the 20mm (DSR 1) and 25mm (DSR 2) parallel plate geometries. Under these conditions of
low temperature and high binder stiffness, the displacement measured is believed to be almost
entirely due to the compliance of the measuring system. Increasing the gap (sample height)
reduces the problem but the effect is still significant, causing lower than expected |G*| values as
δ tends to zero. Reducing the diameter of the plate to 8mm improves the situation but, even
with a combination of reduced plate diameter and increased sample height (2mm), it does not
appear possible to measure the limiting elastic stiffness of 10 9 Pa. (This can be seen by
extrapolation of the δ vs |G*| plot for this geometry in Figure 7). Use of an even larger gap may
extend the measurement range further. It is clear that the gap setting affects the results, in
addition to the diameter of the plate, although the gap selected does not have quite such a large
effect.
Figures 5 to 7 (plots of δ vs |G*|) show how it is possible, by extrapolation, to estimate a
maximum stiffness which can be measured for a given sample geometry. However, it is not
easy from such plots to estimate an upper limit of stiffness beyond which results may be
inaccurate. Research by BP in the late 1960s found a linear relationship between the logarithm
of (1+tan δ) and the logarithm of |G*| for penetration grade bitumens, within the range of 0 to 1
for log(1+tanδ) (Dobson 1967, Dobson 1969). When plotted in this form the limiting stiffness
may be more readily extrapolated and it is also easier to identify the point of departure from
linearity where lower than expected values of |G*| are obtained. Figures 8 and 9 show plots of
log(1+tanδ) versus log|G*| for both bitumens.
From Figure 8 it can be seen that disagreement in the values of |G*| measured using the two
plates occurs at about 105 Pa. For the 25mm plate (1mm gap), the extrapolated value for the
limiting stiffness is about 107 and inaccurate values of stiffness would be obtained in the range
105-107 Pa. However, for the 8mm PP geometry (0.5mm gap), extrapolation of the line gives a
value for the limiting stiffness which is close to 109 Pa, although departure from linearity may
occur above 2x107 Pa, where the points are observed beginning to diverge from the line.
Figure 8 also shows that, for values of log(1+ tan δ) greater than about 1, the linear relationship
does not hold, because tan δ tends to infinity and consequently there is a lot of scatter in the
data. A similar plot for the 15 pen bitumen (Figure 9) using the 8mm PP geometry (0.5mm
gap) gives a similar value for the limiting stiffness. Departure from linearity appears to occur
at a similar stiffness to that observed in Figure 8, i.e. 2x107 Pa, although points are only just
beginning to diverge.
DISCUSSION
Work presented in this paper indicates that care is required to obtain accurate rheological
measurements on bitumens. Small variations between the set temperature and the actual
temperature of the binder can cause large variations in the results obtained. Accurate
temperature control of the whole environment around the bitumen, for example by a fluid bath,
is essential.
The choice of sample geometry can also have a large influence on the results. This is
considered to be due to machine compliance, the extent of which depends on both the
rheometer and the plate diameter and gap. The problem is measuring small displacements
which contain contributions from both the binder and the machine using a particular geometry.
As the binder stiffness increases, the strain (or displacement) in the binder decreases until a
point is reached where torsional movements in the machine itself become significant. The
instrument and software assumes the torsional movement is entirely due to the binder. Where
this is not the case, this will result in a lower measured stiffness, as shown in this study.
The results indicate that, for practical purposes, the 25mm PP and 20mm PP geometries with
gaps of 0.5-2 mm are not suitable for the accurate measurement of binder stiffnesses above
about 105 Pa without some correction for machine compliance. For the 8mm PP geometry, the
upper limit of binder stiffness appears to be approximately 108 Pa for a gap of 2mm. These
limiting stiffness values occur over the temperature ranges normally selected for characterising
the rheological behaviour of bitumens. In order to measure higher stiffnesses, it would be
advisable to consider either an alternative geometry, for example tension-compression, or an
alternative instrument, such as the Bending Beam Rheometer. Although the lower operational
limits in terms of binder stiffness were not specifically addressed in this study, for a given DSR,
there was good agreement between the geometries at stiffness values between 103 and 105Pa.
CONCLUSIONS
The major conclusions from this study are as follows :
• A difference of 1°C in temperature can lead to significant variations in the binder properties
measured using a DSR. To ensure accurate temperature control it is recommended that the
sample is in a temperature-controlled environment, e.g. a water bath.
• To check the accuracy of DSR measurements, a plot of log(1+tanδ) versus log|G*| may be
made and the limiting stiffness of the binder (|G*|) estimated. The limiting stiffness for
unmodified bitumens should be about 109 Pa.
• With 20mm and 25 mm diameter PP geometry, a practical stiffness limit appears to be about
105Pa for gaps in the range 0.5-2 mm for both DSRs. For the 8mm PP geometry, an upper
limit of 108 Pa seems to apply for a gap of 2mm. This limit may increase for a larger gap,
although clearly there are practical working limits. Stiffness measurements exceeding these
values will be affected by machine compliance which is both DSR and geometry dependent.
The plate diameter selected has a more significant effect on the results than the gap.
Modified binders were not tested as part of this study, but the measurable stiffness range in
order to guarantee accurate results remains the same. However, the linear relationship of
log(1+tan δ) against log(|G*|) will not be valid for modified materials which exhibit highly
elastic behaviour over the in-service temperature range.
Since empirical relationships between binder properties and the in-service performance of
asphalt mixes may not always be valid for modified binders (Claxton 1996), it is important that
future specifications are developed which are valid for these binders. The use of fundamental
rheological measurements, is therefore of increasing importance. However, it is essential that
the methods for making such measurements, including accurate temperature control and
selection of an appropriate geometry are carefully defined to ensure accurate and reproducible
results. The effects of sample preparation, equipment calibration and non-linear visco-elastic
behaviour should not be overlooked.
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REFERENCES
American Association of State Highway and Transportation Officials (1995). AASHTO
provisional standard TP5-93: standard test method for determining the rheological properties of
asphalt binder using a dynamic shear rheometer. AASHTO, Washington DC.
Australian Standards (1993). Method of testing bitumen and related roadmaking products.
Method 2: determination of dynamic (coefficient of shear) viscosity by flow through a
capilliary tube. AS 2341.2-1993. Standards Australia, NSW.
CLAXTON M J, LESAGE J, PLANQUE L, GREEN P G (1996), The use of binder rheological
properties to predict the performance of asphalt mixes. Australian Road Research Board
Conference, 1996.
Dobson G R (1967). An apparatus for measuring the dynamic elastic properties of bitumens.
Journal of Scientific Instrumentation, Vol 44, p375, 1967.
Dobson G R (1969). The dynamic mechanical properties of bitumen. Proceedings of the
Association of Asphalt Paving Technologists, Vol 38, p123-139, 1969. AAPT, Minnesota.
Dobson G R (1972). Interrelationships between rheological tests for bitumens. BP Internal
Report 20 666. BP, Sunbury.
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AUTHOR BIOGRAPHIES
Peter Green is Manager of the Bitumen Technical Unit at the BP Research and Engineering
Centre, Sunbury, UK. He graduated in 1976 from Kingston University with a chemistry degree
and has been working in bitumen product development since 1984. Since that time he has been
involved in many bitumen product development projects in support of BP’s bitumen activities
worldwide.
Melanie Claxton is a Research Leader in the Bitumen Technical Unit at the BP Research and
Engineering Centre, Sunbury, UK. She graduated with a BSc (Hons) in physics from the
University of St Andrews and joined BP in 1988. In 1993 she joined the Bitumen Technical
Unit where she has worked mainly on binder rheological measurements and their correlation
with asphalt performance. She was a member of the Eurobitume Technical Committee which
compiled a Glossary of Rheological Terms published in 1996.
James Carswell is a Research Leader in the Bitumen Technical Unit at the BP Research and
Engineering Centre, Sunbury, UK. He graduated with a BSc (Hons) in physics from the
University of Exeter and in 1975 joined the Transport Research Laboratory (TRL) as a scientist
and Project Manager. He was involved in most aspects of bituminous road materials and
highway design and specialised in surfacing layers and the use of modifiers to improve
performance. He joined BP in 1996 as a Research Leader on asphalt related topics.
Rubber Shield
Aluminium Block
Water
Sample Plate
Peltier Temperature
Control System
Figure 1 Schematic of DSR 1 with water jacket and aluminium block
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|G*| (Pa) δ (deg)
9
10 100
8
10
60C 80 60C
7
10
45C 45C
10
6
30C 60 30C
25C 25C
5
10 40
20C 20C
4
10 10C 10C
3
20
10
2
10 0
0.03 0.1 0.3 1 3 10 30 100 0.03 0.1 0.3 1 3 10 30 100
Frequency (Hz) Frequency (Hz)
Figure 2 DSR 2 results for 15 pen bitumen (8mm PP, 0.5mm gap)
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|G*| (Pa) δ (deg)
108 |G*|, 8mm PP
δ
80
7 |G*|, 25mm PP
10
60 δ, 8mm PP
106
δ, 25mm PP
40
105
G*
10 4 20
103 0
10 20 30 40 50 60 70
Temperature (°C)
Figure 3 DSR 2 results for 200 pen bitumen (0.4 Hz)
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|G*| (Pa) δ (deg)
10 8 |G*|, 8m m PP
80
10 7 δ |G*|, 25m m PP
60 δ, 8m m PP
10 6
δ, 25m m PP
G* 40
10 5
10 4 20
10 3 0
10 20 30 40 50 60 70
Temperature (°C)
Figure 4 DSR 2 results for 15 pen bitumen (10Hz)
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δ (deg)
8mm PP
80
25mm PP
60
40
20
0 2
10 103 104 105 106 107 108 109
|G*| (Pa)
Figure 5 Phase angle versus |G*| for 200 pen bitumen (0.4Hz)
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δ (deg)
DSR 2
80 8mm PP
DSR 2
25mm PP
60
DSR 1
20mm PP
40
20
0 5
10 106 107 108 109
|G*| (Pa)
Figure 6 Phase angle as a function of |G*| for 15 pen bitumen (10Hz)
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δ (deg)
DSR 2
80 8mm PP (0.5mm)
DSR 2
8mm PP (2mm)
DSR 2
60 8mm PP (0.1mm)
DSR 1
20mm PP (0.5mm)
DSR 1
40 20mm PP (2mm)
DSR 1
20mm PP (.01mm)
DSR 2
20 25mm PP (1mm)
DSR 1: 20mm PP, DSR 2: 25mm PP, DSR 2
0.01mm GAP 0.01mm GAP 25mm PP (.01mm)
0 3
10 104 105 106 107 108 109 1010
|G*| (Pa)
Figure 7 Effect of plate diameter and gap on δ and |G*| (15 pen bitumen)
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Log (1+tan δ)
3 DSR 2
8mm PP
2.5
DSR 2
25mm PP
2
1.5
0.5
0
102 104 106 108 1010
|G*| (Pa)
Figure 8 Log(1+tanδ) vs log|G*| for 200 pen bitumen
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Log (1+tan δ)
1 60C
0.8 50C
45C
0.6
40C
0.4 30C
25C
0.2
20C
0 3
10 104 105 106 107 108 109 1010
|G*| (Pa)
Figure 9 Log(1+tanδ) vs log|G*| for 15 pen bitumen
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