Proposed AASHTO ST Test Method-4mm DSR 112112
Proposed AASHTO ST Test Method-4mm DSR 112112
Proposed AASHTO ST Test Method-4mm DSR 112112
SCOPE
1.1.
This test method covers the determination of the dynamic shear modulus and phase angle of asphalt
binder when tested in dynamic (oscillatory) shear using parallel plate test geometry at low (-40 to
0C) temperature. This test method is intended for determining the linear viscoelastic properties of
asphalt binders as required for specification testing and is not intended as a comprehensive
procedure for the full characterization of the viscoelastic properties of asphalt binder.
1.2.
This standard is appropriate for unaged material, and material aged in accordance with T 240
and R 28.
1.3.
This standard may involve hazardous materials, operations, and equipment. This standard does not
purport to address all of the safety concerns associated with its use. It is the responsibility of the
user of this procedure to establish appropriate safety and health practices and to determine the
applicability of regulatory limitations prior to use.
2.
REFERENCED DOCUMENTS
2.1.
AASHTO Standards:
M 315 Standard Test Method for Determining the Rheological Properties of Asphalt Binder Using
a Dynamic Shear Rheometer
M 320, Performance-Graded Asphalt Binder
R 28, Accelerated Aging of Asphalt Binder Using a Pressurized Aging Vessel (PAV)
R 29, Grading or Verifying the Performance Grade (PG) of an Asphalt Binder
T 40, Sampling Bituminous MaterialsT315, Determining the Rheological Properties of Asphalt
Binder Using a Dynamic Shear Rheometer (DSR)
T 240, Effect of Heat and Air on a Moving Film of Asphalt Binder (Rolling Thin-Film Oven Test)
2.2.
ASTM Standards:
D 7175, Standard Test Method for Determining the Rheological Properties of Asphalt Binder
Using a Dynamic Shear Rheometer
3.
TERMINOLOGY
3.1.
Definitions:
3.1.1.
asphalt binderan asphalt-based cement that is produced from petroleum residue either with or
without the addition of non-particulate organic modifiers.
3.2.
TS-X
T XXX-1
AASHTO
3.2.1.
annealingheating the binder until it is sufficiently fluid to remove the effects of steric hardening.
3.2.2.
complex shear modulus (G*)ratio calculated by dividing the absolute value of the peak-to-peak
shear stress, , by the absolute value of the peak-to-peak shear strain, .
3.2.3.
3.2.4.
dummy test specimena specimen formed between the dynamic shear rheometer (DSR) test plates
from asphalt binder or other polymer to measure the temperature of the asphalt binder held between
the plates. The dummy test specimen is used solely to determine temperature corrections.
3.2.5.
loading cyclea unit cycle of time for which the test sample is loaded at a selected frequency and
stress or strain level.
3.2.6.
phase angle ()the angle in radians between a sinusoid ally applied strain and the resultant
sinusoidal stress in a controlled-strain testing mode, or between the applied stress and the resultant
strain in a controlled-stress testing mode.
3.2.7.
loss shear modulus (G )the complex shear modulus multiplied by the sine of the phase angle
expressed in degrees. It represents the component of the complex modulus that is a measure of the
energy lost (dissipated during a loading cycle).
3.2.8.
storage shear modulus (G )the complex shear modulus multiplied by the cosine of the phase
angle expressed in degrees. It represents the in-phase component of the complex modulus that is a
measure of the energy stored during a loading cycle.
3.2.9.
parallel plate geometryrefers to a testing geometry in which the test sample is sandwiched
between two relatively rigid parallel plates and subjected to oscillatory shear.
3.2.10.
oscillatory shearrefers to a type of loading in which a shear stress or shear strain is applied to a
test sample in an oscillatory manner such that the shear stress or strain varies in amplitude by about
zero in a sinusoidal manner.
3.2.11.
linear viscoelasticwithin the context of this specification refers to a region of behavior in which
the dynamic shear modulus is independent of shear stress or strain.
3.2.12.
3.2.13.
3.2.14.
3.2.15.
thermal equilibriumis reached when the temperature of the test specimen mounted between the
test plates is constant with time.
3.2.16.
3.2.17.
TS-X
T XXX-2
AASHTO
3.2.18.
3.2.19.
normal force the force perpendicular to the surface of the parallel plates.
3.2.20.
molecular associationa process where associations occur between asphalt binder molecules during
storage at ambient temperature. Often called steric hardening in the asphalt literature, molecular
associations can increase the dynamic shear modulus of asphalt binders. The amount of molecular
association is asphalt specific and may be significant even after a few hours of storage.
4.
4.1.
4.2.
The test specimen is maintained at the test temperature to within 0.1C by positive heating and
cooling of the upper and lower plates or by enclosing the upper and lower plates in a thermally
controlled environment or test chamber. Test temperatures are between -40 and 0C.
4.3.
The complex modulus (G*) and phase angle () are calculated automatically as part of the operation
of the rheometer using proprietary computer software supplied by the equipment manufacturer.
5.
5.1.
The test method is a significant benefit to low temperature rheological testing in several ways: (1)
the method includes a procedure to measure instrument compliance; (2) testing as low as -40C is
achievable by way of a correction for machine compliance; (3) when using 4mm diameter plates,
only 25mg of binder is required for a test (note: in actual practice 150 mg for sample loading and
trimming is required, but that is about 100 times less than required under AASHTO T313 to prepare
1 beam) ; (4) a commercial dynamic shear rheometer is a more precise instrument than a bending
beam rheometer; (5) intermediate test temperatures are achievable: for 4 mm and 8 mm diameter
plates, approximately 0 to 30C and 0 to 45C, respectively.
5.2
Test temperatures are related to the low temperatures experienced by the pavement in the
geographical area for which the asphalt binder is intended to be used. Master curves of G* and
curves at selected temperatures can be developed employing time-temperature superposition. The
master curves can be used to calculate low temperature performance-related criteria in accordance
with M 320.
6.
APPARATUS
6.1.
The dynamic shear rheometer, environmental chamber and control and data acquisition system shall
meet the requirements of T315. Test plates shall be 4.00 0.01 mm or 8.00 0.01mm in diameter,
stainless steel or aluminum with smooth ground surface. In addition, the rheometer shall be equipped
with a normal force sensor.
Note 1When measuring low temperature properties by DSR, errors due to instrument compliance
need to be corrected. For older DSRs, without updated software to do the real-time online
instrument compliance corrections, one can use the method in Appendix 17. For updated DSR the
real-time online instrument compliance correction is made by pre-inputting the instrument
compliance value into the software. Regardless of the way the correction is performed, the value of
instrument compliance is the most important factor. How to measure the instrument compliance is
covered in Appendix 18.
TS-X
T XXX-3
AASHTO
7.
HAZARDS
7.1.
Standard laboratory caution should be used in handling the hot asphalt binder when preparing
test specimens.
8.
PREPARATION OF APPARATUS
8.1.
Prepare the apparatus for testing in accordance with the manufacturers recommendations. Specific
requirements will vary for different DSR models and manufacturers.
8.2.
Inspect the surfaces of the test plates and discard any plates with jagged or rounded edges or deep
scratches. Clean any asphalt binder residue from the plates with an organic solvent such as mineral
oil, mineral spirits, a citrus-based solvent, or toluene. Remove any remaining solvent residue by
wiping the surface of the plates with a cotton swab or a soft cloth dampened with acetone. If
necessary, use a dry cotton swab or soft cloth to ensure that no moisture condenses on the plates.
8.3.
Mount the cleaned and inspected test plates on the test fixtures and tighten firmly.
9.
9.1.
Verify the DSR and its components at least every six months and when the DSR or plates are newly
installed, when the DSR is moved to a new location, or when the accuracy of the DSR or any of its
components is suspect in accordance with T315.
10.
10.1.
Anneal the asphalt binder in a forced draft oven at 70C. For relatively large amounts of material
such as an RTFO-PAV aged sample (50 g) in a standard PAV pan, an annealing time of about 30
min. is required. For smaller amounts of binder (<10 g) only 15 minutes is required. For very small
amounts (<`1 g) an argon blanket should be used to prevent oxidation.
10.2.
While the sample is being annealed, carefully clean and dry the surfaces of the test plates so that the
specimen will adhere to both plates uniformly and strongly. Heat the rheometer oven or Peltier
plates to 30C and stabilize at this temperature for about 20 min. Zero the gap in accordance with
[Preparation of Apparatus].
10.3.
Move the plates apart to 5 mm and preheat the plates to ~ 60C to improve the adhesion between the
asphalt and the plates.
10.4.
Transfer the annealed hot asphalt to the lower fixed plate using a metal spatula or other tools.
10.5.
Immediately after the transferring, move the test plates together until approaching the desired testing
gap plus the gap closure to create the bulge: (1) 4 mm diameter plates - the desired testing gap is
1.75 mm and the closure gap for the bulge is 0.120 mm; (2) 8 mm diameter plates - the desired
testing gap is 2.00 mm and the closure gap for the bulge is 0.150 mm).
10.6.
Trim excess asphalt binder by moving a heated trimming tool around the edges of the plates so that
the asphalt binder is flush with the outer diameter of the plates. Use a magnifying lens, external light
source and mirror to observe the entire surface of the trimmed sample and insure a uniform trimmed
surface.
10.7.
Close the chamber door and heat the sample to the preheating temperature (~60C) for about 5 min.
TS-X
T XXX-4
AASHTO
10.8.
Cool the system down to 30C and decrease the gap by the amount of closure gap (0.120 mm for 4
mm plates, and .150 mm for 8 mm plats).
10.9.
11.
PROCEDURE
11.1.
After conditioning the specimen for 20 minutes at 30C the measuring system shall then be cooled to
the target testing temperature and stabilized at the testing temperature for 20 min when testing binder
for compliance with M 320.
Note 2When changing temperature, the metallic rheometer parts and measurement geometries
thermally expand or contract causing an expansion or contraction of the gap. The change in the gap
due to system thermal expansion or contraction must be compensated for to keep the gap constant.
To compensate and keep the gap constant a correction factor must be determined and the gap
adjusted for changes in temperature as discussed Appendix 19.
Note 3Even with the gap correction performed manually or automatically to compensate for
system thermal expansion or contraction, the sample will expand or contract with change in
temperature causing changes in the sample shape and generation of normal force. This is particularly
true at test temperatures close to or below the glass transition temperature of the test materials. In
some cases the build-up in thermal stress may be sufficient to damage the normal force transducer.
To keep a uniform sample shape as well as to avoid machine damage, the moving plate has to be
adjusted to compensate for build up in normal force due to sample expansion or contraction. The
normal force should be monitored when changing temperature and the gap adjusted beyond the
necessary adjustment for system expansion or contraction to keep the normal force at zero. In no
case should the normal force exceed 20 grams during cooling or heating. If performed manually, this
adjustment in the gap to keep the normal force at zero causes a very slight error in the gap, but it is
small enough that it can be neglected. Some rheometers can maintain the normal force at zero and
any slight change in the gap is accounted for eliminating the slight error when the correction is
manually performed.
11.2.
After cooling to the test temperature, which typically takes about 3 to 5 minutes, condition the
sample at the test temperature for 20 minutes. A specific time of 20 minutes is specified to keep the
extent of physical hardening at low temperature uniform during testing.
11.3.
After the 20 minute conditioning period, perform a strain or stress sweep test (a strain sweep if the
rheometer is strain controlled or a stress sweep if the rheometer is stress controlled) to determine the
linear viscoelastic region and select an appropriate linear stain. After the strain or stress sweep test is
finished, a plot of G*, G and G should be developed in the instrument software. Examine the plot
for regions in which all three of these variables form a flat (slope of 0) line. It is in this linear
viscoelastic region of all three variables where the percent strain or stress for the frequency sweep
should be selected. In some cases, the entire plot may be linear, only a small region linear, or no
linearity may be observed. Some instruments can be programmed to perform the strain or stress
sweep and select an appropriate strain or stress level (usually the mid-point of the linear region)
automatically.
11.4.
Perform a frequency sweep test in a frequency range of 0.1 to 50 rad/sec using the linear strain or
stress determined in step 11.3. There will be 15 steps in the frequency sweep as shown in Table 1.
TS-X
T XXX-5
AASHTO
0.15
0.25
0.39
0.63
1.00
Frequency rad/sec
1.58 2.51 3.98 6.31
10.00
15.85
25.12
39.81
50.00
11.5.
Cool the sample to the next isotherm repeating steps 11.2 through 11.4.
12.
INTERPRETATION OF RESULTS
12.1.
The two frequency sweeps performed at, PG+10C and PG+20, are used to develop a storage
modulus G() master curve using time-temperature superposition at a reference temperature of
PG+10C. The relaxation modulus G(t) curve is then determined thru interconversion. The slope
(mr) and magnitude G(t) for M 320 are determined from the relaxation modulus master curve at 60
seconds. Appendix 20 provides further discussion and an example of the process to determine mr and
G(t) at 60 seconds.
13.
REPORT
13.1.
13.2.
Mr(60 sec) to one decimal place and G(60 sec) to the nearest whole number
14.
14.1.
15.
KEYWORDS
15.1.
Dynamic shear rheometer; DSR; storage modulus; relaxation modulus, asphalt binder.
16.
REFERENCES
16.1.
Olusanya, A., A Comparison of Techniques for Monitoring the Cure of Adhesives, MTS
Adhesives Project 5, Measurements for Optimizing Adhesives Processing Report 10, NPL Report
CMMT(B104) National Physical Laboratory, Teddington, Middlesex, UK, ISSN 1361-4061,
November 1996.
16.2.
16.3.
Sui, C., M. J. Farrar, W. H. Tuminello, and T. F. Turner, 2010, New Technique for Measuring LowTemperature Properties of Asphalt Binders with Small Amounts of Material. Transportation
Research Record 2179, 23-28.
16.4.
16.5.
Schrter, K., S. A. Hutcheson, X. Shi, A. Mandanici, and G. B. McKenna, Dynamic Shear Modulus
of Glycerol: Corrections Due to Instrument Compliance, J. Chem. Phys., 125, 214507, 2006.
TS-X
T XXX-6
AASHTO
16.6.
Hutcheson, S.A. and G. B. McKenna, The measurement of mechanical properties of glycerol, mtoluidine, and sucrose benzoate under consideration of corrected rheometer compliance: An in-depth
study and review, The Journal of Chemical Physics 129, 074502, 2008.
17.
APPENDIXES
17.1.
(Mandatory Information)
A1.
A1.1.
Scope:
A1.1.1.
This is a mathematical method for correcting errors due to instrument compliance and is applicable
to the data collected on a DSR that does not have a real-time online instrument compliance
correction function.
A1.2.
Mathematical methodology:
For low temperature rheological measurements, the stiffness of the test material could be comparable
to that of the instrument so instrument compliance cant be neglected in order to obtain reliable
results. The measured data has to be properly corrected by taking the instrument compliance into
account.
In 1996, Rides and Olusanya proposed an instrument compliance correction for oscillatory shear
rheometry (Olusanya 1996). Franck proposed a similar correction in 2006.
Schroter et al (2006) and Hutcheson and McKenna (2008) demonstrated that error from not properly
taking into account rheometer compliance can be quite significant and that the resulting inaccuracies
in the determined mechanical properties can result in mistakes in material modeling, design, and
theory.
Sui et al. (2010) were the first to apply an instrument compliance correction to asphalt binder low
temperature oscillatory shear measurements (~ 5C to -40C) using parallel plate geometry.
TS-X
T XXX-7
AASHTO
A1.2.1.
Where
and
are the sample complex modulus and the measured complex modulus respectively.
For the parallel plate geometry, the sample complex shear modulus is
(9)
TS-X
T XXX-8
AASHTO
The Equation (8) can be rewritten in the form of storage and loss moduli as
(10)
(11)
(12)
(13)
The geometry constant or geometry conversion factor k g for the commonly used rheometer fixture
geometry is listed below:
For parallel plate, kg was shown in Equation (6).
For cone and plate,
(14)
Where R is the plate radius and
A2.
A2.1.
Scope:
A2.1.1.
A2.2.
Procedure:
A2.2.1.
Prepare the DSR in accordance with Section 8 of this standard using 4 mm parallel plates and allow
approximately the plates to come to room temperature (approximately 20 minutes). Insure that any
compliance correction values in the instrument software are set to zero.
A2.2.2.
Apply a drop of SuperGlue (cyanoacrylate or any other type of super glue) to the center of the
lower plate.
A2.2.3.
Close the gap by moving the movable plate to form a thin layer (about 0.05 mm) of super glue
between two plates. Ensure the thin layer of super glue film between plates is uniform.
TS-X
T XXX-9
AASHTO
A2.2.4.
A2.2.5.
Allow for sufficient time to fully cure the super glue (approximately 3 hours). Monitor the normal
force as the cyanoacrylate will have a slight volume loss as it cures. Adjust the gap as necessary to
maintain a normal force of 0 N.
A2.2.6.
A2.2.7.
Plot angle displacement (angular rotation) versus torque obtained from the strain/stress test, and the
instrument compliance is the slope of the linear fit (as shown in Figure 1).
3,000
2,500
y = 3.0245x
R = 1
2,000
1,500
1,000
Machine compliace = 3.0245 rad/(gram cm)
500
Note: y intercept was set to 0.0
200
400
600
800
1000
Torque (g cm)
Figure 1Example: Determination of Instrument Compliance from the Slope of the Linear Fit of the Angle
Displacement and Torque Measurements
A3.
A3.1.
Scope:
A3.1.1.
This procedure is used to measure the thermal expansion of the measuring system on DSR.
A3.2.
Procedure:
A3.2.1.
Mount the parallel plates onto DSR and leave the plates 1 mm apart.
A3.2.2.
Heat the measuring system to 30C and stabilize at this temperature for at least 30 min.
A3.2.3.
Zero the gap using the normal force transducer and the instruments Zero Gap function, and move
the moveable plate so the plates are 1 mm apart. Lower the temperature to 20C and condition for 20
TS-X
T XXX-10
AASHTO
minutes. Then move the moveable plate to the point where it just touches the fixed plate (indicated
by a change in the normal force, note: the normal force should not exceed 10 g). The gap deviation
from the zero position is the thermal expansion or change in length (L ) of the measuring system
from the 10C change in temperature (T) The gap correction factor (g) of the system is
g = (L) / (T)
(16)
Adjust the gap when changing temperature to adjust for the thermal contraction or expansion of the
system, e.g., assuming g = 2 m C-1) then when changing from 30C to20C the gap adjustment
(h) is
(h) = g * (T) = 2 m/ C * 10C = 20 m, i.e., the moveable plate is moved towards the
stationary plate a distance of 20 m.
A4.
A4.1.
Scope:
A4.1.1.
This section provides an example of time temperature superposition (TTS) and master curve
development of G() from the two frequency sweeps, interconversion from G() to G(t) and
estimation of mr and G(t) at 60 seconds from the G(t) master curve at the PG+10C.
A4.2.
Definition of terms:
A4.2.1.
A4.2.2.
A4.2.3.
A4.2.4.
A4.2.5.
mr(60 s) slope of the relaxation modulus at a reference temperature of PG+10C and 60 seconds
A4.2.6.
A4.2.7.
Frequency (r/s)
A4.2.8.
A4.2.9.
t time (seconds)
A4.3.
Example:
A4.3.1.
A series of steps are involved when calculating the slope ( mr ) and magnitude of the relaxation
modulus G(t) from dynamic oscillatory shear data (frequency sweeps) at 60 seconds and a reference
TS-X
T XXX-11
AASHTO
temperature of PG+10C. The first step is to generate a G() master curve at a reference
temperature of PG+10C.
Plot the two frequency sweeps determined in Section 1. A typical representation of test data is
shown in Figure 2. Fit the PG+10C frequency sweep with a second order polynomial.
Figure 2PG+10C and PG+20C Frequency Sweeps from Section 11, Procedure
A4.3.2.
Use ExcelTM solver to determine the horizontal shift factor (aT) to translate the PG+20C frequency
sweep along the abscissa so that it overlaps the PG +10C frequency sweep. The horizontal
translation is accomplished by multiplying the PG+20C frequencies by aT and plotting the storage
modulus as a function of the multiplied frequencies. The basis for the shift factor is known as timetemperature superposition (TTS). Table 2 demonstrates the calculation of the shift factor. To avoid
error from extrapolation of the 2nd order polynomial, only G() data that approximately overlap are
used to estimate aT.
A4.3.3.
TS-X
Using the aT determined in section 20.2.2 shift the PG+20C frequency sweep so that it overlaps the
PG+10C frequency sweep. The process is illustrated in Figure 3.
T XXX-12
AASHTO
A4.3.4.
The relaxation modulus G(t) is then determined thru interconversion of the storage modulus G()
by the approximate expression developed by Christensen (1982).
(17)
Figure 4 shows the relaxation modulus determined using Equation 17. The relaxation modulus is fit
with a 2nd order polynomial using the time points that bracket 60 seconds ( 0.78 to 2.78 in log scale)
to generate the polynomial. The resulting 2nd order polynomial is
3311
(18)
The slope of the relaxation modus at 60 seconds is determined by taking the first derivative of the
2nd order polynomial
(19)
Solve Equation 18 for G(60s) and Equation 19 for the slope, mr at 60 s.
G(60 s) = 66.85 MPa
mr (60 s) = -0.35
TS-X
T XXX-13
AASHTO
TS-X
T XXX-14
AASHTO