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Figure 3 VISCOTECH DSR stability at 64 °C on an original asphalt binder. Figure 4 VISCOTECH DSR heating transient response 64–70 °C.
16 / JULY 1999
APPLICATION NOTE continued
a b
Figure 7 Shear modulus versus frequency results for samples 1 and 2 at selected temperatures.
ing mode results, the sample has attained steady- greater strength and extendability, especially at low frequencies, the elastic modulus approaches a limit-
state response after 5 min. In a comparable wet sys- temperatures when shrinkage forces and embrittle- ing value, which is the glassy state modulus. At low
tem, this time can exceed 30 min. ment are likely to promote failure. frequencies, the slope of a log–log plot of the elastic
To determine the relative temperature sensitivity of In the past few years, much experience has been modulus versus frequency approaches 2, which sig-
an asphalt binder, a sample of DSR verification fluid acquired in petrochemical research with regard to nifies that viscous flow has been reached, and that
N2700000SP was also run from 64 to 58 °C. The results the rheology of polymers. At the same time, the tech- the asphalt is behaving as a Newtonian fluid. Using
are shown in Figure 6. The asphalt binder shows an ap- nologies applied to the research of rheological char- the characteristic parameters of the master curve,
prox. factor of 2 greater temperature dependence than acteristics of asphalt binders have been developed. along with the mathematical relationships for
the DSR verification fluid in this range. This new research shows that asphalt binders can be time–temperature dependence, it is possible to con-
characterized more rigorously with viscoelastic data. struct a unified mathematical model for the rheo-
logical behavior of asphalt binders.
Polymer-modified asphalt binder
Tests were performed on two asphalt binders in
Time–temperature superposition
Polymers are often added to asphalt binders to im- the temperature range from –10 to 50 °C in order to
prove the performance behavior with particular em- One of the primary analytical techniques used in determine the most significant viscoelastic function.
phasis on obtaining desired viscoelastic properties. analyzing the dynamic viscoelastic data for asphalt At temperatures from –10 to 35 °C, 8-mm-diam par-
As an example, a polymer-modified asphalt demon- involves the construction of master curves for dy- allel plates were used in performing the dynamic
strates increased ring and ball softening point, re- namic complex moduli, complex viscosity, and testing. Shear moduli (G′, G′′) and complex viscosity
duced penetration, increased ductility, and increased phase angle. In constructing such master curv e s , (η*) are plotted versus frequency (rad/sec) in Figure
toughness and tenacity. These effects become more use is made of the time–temperature superposition 7a and b and Figure 8a and b, respectively. The com-
pronounced with increasing polymer loading. Al- principle. In constructing a master curve using plex viscosity (η*) of sample 2 increases considerably
though extensive efforts have been directed at im- time–temperature superposition, dynamic data are with decreasing frequencies. On the other hand,
proving the quality and performance of asphalt first collected over a range of temperatures and fre- sample 1 exhibits Newtonian behavior in the region
paving materials, there appears to be no consensus quencies. A standard reference temperature must of lower frequencies. Unmodified paving asphalt
among the various authorities concerning the least then be selected for the master curve. The data at all usually exhibits Newtonian flow behavior at tem-
expensive and most effective methods to reduce or other temperatures are then shifted with respect to peratures in excess of 50 °C.
eliminate cracking, potholes, distortion, and other time until the curves merge into a single, smooth F i g u res 9 and 1 0 are master curves using the
forms of pavement distress. Since the first sign of function. The time–temperature superposition prin- Williams, Landel, and Ferry (WLF) shifting proce-
pavement failure is usually the formation of tiny, ciple also applies to materials undergoing a transi- dure in the temperature range of –10 to 50 °C for
hairline cracks, it is particularly important to pro- tion such as the glass transition. samples 1 and 2, respectively. In this case, the refer-
duce road surfaces that are tough and crack resistant, In a master curve, one or more of the viscoelastic ence temperature selected was 25 °C. Sample 2, con-
preferably through the use of additives that impart functions is plotted against frequency. At very high taining 5% styrene butadiene rubber (SBR), has a
18 / JULY 1999
APPLICATION NOTE continued
a b
Figure 8 Complex viscosity versus frequency results for samples 1 and 2 at selected temperatures.
crossover point of G′ and G′′, very close to sample 1. strument includes normal force capability for repro-
However, in the terminal zone, sample 1 approaches ducible sample loading history, thermal expansion
Newtonian behavior with a phase angle near 90°, in- measurements, and can be configured with a pat-
dicating a constant viscosity at long times, while ented Differential Pressure Quantitative Normal
sample 2 levels off at 65°, indicating an increasing Force Sensor for quantitative normal stress measure-
viscosity at long times. The addition of a small ments. The diffusion air bearing has a low inertia
amount of SBR results in a dramatic effect on the with high axial and radial mechanical stiffness.
rheological properties and ultimate end-use perfor- The SPECTECH DSR was designed to be applica-
mance characteristics of this asphalt binder in the tions specific for testing of asphalt binders accord-
long time, i.e., low rates of deformation and applica- ing to AASHTO TP5. The instrument features dis-
tion areas such as rutting. posable plates and user-independent, automatic
sample trimming.
Creep tests
Electronic unit
Creep tests give extremely important practical in-
formation and, at the same time, useful data to one The VISCOTECH DSR instrument electronics are
interested in the theory of the mechanical properties contained within the mechanical unit, and the in-
of asphalt binders. Since asphalt pavements are de- strument is built around a dedicated, high-speed 32- Figure 9 Master curve at 25 °C, sample 1.
signed to be flexible, they must quickly return to their bit CPU. This consolidation enhances performance
original configuration after loading. Rutting, push- and versatility due to having electrical connections
ing, and shoving are just a few of the failure mecha- on the motherboard bus rather than through cables
nisms associated with inelastic or permanent defor- to a separate electronics cabinet. In addition, valu-
mation. Repeated loading without complete binder able bench space is kept to a minimum. The motor
recovery is also a cause of fatigue cracking. Although control is based on digital rather than analog drive
the quality and gradation of the aggregate are impor- technology. The unit includes a built-in diagnostic
tant parts of the asphalt mix performance, the creep system and quick diagnostic service port for service
response of the binder is also a contributing factor. As engineers. Also included is a modem port for re-
creep is a time-dependent function, it is necessary to mote-control operation and fault diagnostics for ser-
monitor recovery per unit time or to stipulate a time vice. The electronics power supply is designed to op-
interval for an expected recovery. An important mea- erate on a line voltage of 180–260 V or 90–140 V and
sure of polymer performance is its ability to recover an operating frequency of 47–63 Hz.
after deformation. Since asphalt pavements are de-
signed to be flexible, they must quickly return to their
original configuration after loading. Figure 11 illus- Software package
trates a creep/recovery test at a constant stress of 1000 The standard software package is a true multitask-
Pa applied over a time of 500 sec and recovery time of ing Microsoft (Redmond, WA) Windows™-based
1000 sec at 25 °C for samples 1 and 2. The results indi- rheological software that has many advantages to
cate that sample 2 creeps less and recovers more the user. The computer is not dedicated to simply
slowly than sample 1. As mentioned above, these running the instrument and is available for other Figure 10 Master curve at 25 °C, sample 2.
data indicate that sample 2 is a stiffer binder with su- use when making measurements. It can be used for
perior long-time creep properties. printing previous results, writing a report, or per-
forming measurements with another instrument. reset to default values using default buttons. An ex-
The software runs under all Windows platforms. ample is the Oscillation Frequency Step measuring
Rheometer setup
The DSR software package offers measuring pro- program, where stresses, delay times, integration
The VISCOTECH DSR and SPECTECH DSR are grams designed to be user friendly with few subdia- periods, and sample sizes can be set individually for
supplied standard will all measuring systems and logue levels and a general recognizable design. Prepro- all frequencies. Another example is the zooming
software to perform asphalt binder testing according grammed test parameters and pass/fail test result function, which is presented in both Vi s c o m e t ry
to AASHTO TP5-97 specification. The base-model limits are included. Additional experiment methods Stress Step and Oscillation Frequency Step, allowing
VISCOTECH rheometer is a modular product with a and analyses are available in the following test modes: any number of steps and increments to be selected.
wide range of measuring systems and accessories. viscometry, yield stress, constant rate, oscillation, os- The instrument also performs controlled strain, and
Additional measuring systems for VISCOTECH are cillation stress sweep, oscillation strain control, constant shear rate measurements, and includes au-
concentric cylinders, cone/plate, parallel plate, dou- creep/recovery, compare, analyze, time–temperature tomatic gap adjustments and compensation using
ble concentric cylinders, closed/pressure cells, and superposition, and spectrum transformation. the normal force sensor. This system enhances mea-
dynamic mechanical analysis (DMA). Special mea- The software includes possibilities to link user- surement reproducibility since the sample loading
suring systems for low volume, high shear rates, and designed methods, including instrument setup and history is reproduced identically each time, using a
high sensitivity are also available. The measuring ge- zero gapping using the project software. The dia- constant loading force.
ometries can be made in stainless steel, titanium, logue windows have many storable, editable func- The VISCOTECH DSR is operated with a separate
polycarbonate, or any user-defined material. The in- tions for unique testing requirements, and can be power supply unit that should be left on continu-
20 / JULY 1999
ously. This reduces startup times and makes it possible for the instrument proces-
sor to maintain values as gap and other user-defined settings.
The VISCOTECH DSR standard temperature control cell is a resistive heating
and adiabatic cooling system. Other temperature cells are available including cir-
culating fluid and cryogenic cooling, covering the range –180 to 500 °C. All mea-
suring geometries are supported, i.e., cone/plate/parallel plate, concentric cylin-
d e r, and solid in torsion. A patented sealed cell for operating at elevated
pressures with full oscillatory capabilities is available.
Mr. Herh is Applications Manager, and Mr. Colo is President, ATS RheoSystems, 52
Georgetown Rd., Bordentown, NJ 08505, U.S.A.; tel.: 609-298-2522; fax: 609-298-
2795; e-mail: atsrheosystems@cwixmail.com; home page: www.atsrheosystems.com/
~ats. Dr. Hedman is with RHEOLOGICA Instruments AB, Lund, Sweden; tel.: 46 46
127760; and Mr. Rudolph is Vice-President, Sales, ATS RheoSystems, Toronto, Ontario,
Figure 11 Creep/recovery results for samples 1 and 2. Canada; tel.: 416-422-5474.
continued on p. 23
AMERICAN LABORATORY / 21