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VISCOSITY TESTING OF ASPHALT
AND EXPERIENCE WITH
VISCOSITY GRADED
SPECIFICATIONS
A symposium
presented at the
Seventy-fifth Annual Meeting
AMERICAN SOCIETY FOR
TESTING AND MATERIALS
Los Angeles, Calif., 2 5 - 3 0 June 1972
04-532000-08
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© BY AMERICAN SOCIETY FOR TESTING AND MATERIALS 1973
Library of Congress Catalog Card Number: 72-97872
NOTE
The Society is not responsible, as a body,
for the statements and opinions
advanced in this publication.
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Foreword
The Symposium on Viscosity Testing of Asphalt and Experience with
Viscosity Graded Specifications was presented at the Seventy-fifth Annual
Meeting of the American Society for Testing and Materials held in Los
Angeles, Calif., 25-30 June 1972. Committee D-4 on Road and Paving
Materials sponsored the symposium. W. G. Gunderman, Highway Research
Board, National Academy of Sciences, presided as symposium chairman.
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Related
ASTM Publications
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Contents
Introduction 1
Rheology of Asphalt Cements at 60 C (140 F)—H. E. SCHWEYER, J. P. MOORE,
AND J. K. LING 3
Temperature Susceptibility 4
Experimental 7
Results 9
Discussion 12
Conclusions 14
Study of Asphalt Viscosity Testing at 60 F—j. v. EVANS AND J. W. GORMAN 16
Experimental 17
Data and Analysis 18
Conclusions and Recommendations 25
Problems in Determining Viscosity of Asphalts at Low Temperatures with
Shell Sliding Plate Microviscometer—E. O. BUSBY AND L. F. RADER 28
Range of Microviscometer 29
Need for Low-Temperature Viscosities 29
Summary 30
Florida Studies with the Puzinauskas Field Viscosity Cup for Asphalt Cements—
C. F. POTTS 31
Base Chart 32
Puzinauskas-Asphalt Institute Field Viscosity Cup (P-AI) 34
Calculations 35
Experimental Data 36
Acceptability Diagram 37
Viscosity Characterization of Asphalt Cement—L. W. CORBETT and H. E.
SCHWEYER 40
Examination of Typical Asphalt Sources 41
Viscosity at 140 F Versus Penetration at 77 F 41
Identifying Grade While Defining Character 45
Viscosity at 275 F as Dependent Upon Viscosity at 140 F 49
Summary 50
The Rolling Thin-Film Circulating Oven—An Improved Rolling Thin-Film
Oven Test—R. J. SCHMIDT 52
Present Situation 53
Description of Oven 58
Comparison of Temperature Control 58
Test Procedure 58
Comparison of Results 58
Collaborative Test Program 61
Comparison of RTF-C and TFO Exposure by Using Collaborative Test
Results 63
Conclusions and Recommendations 63
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vi CONTENTS
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STP532-EB/Jun. 1973
Introduction
During the past ten years or so there has been a rather concerted drive
to change asphalt cement specifications and tests from the old empirical
or penetration basis to the newer fundamental unit or viscosity basis.
A materials engineer requires knowledge of the consistency of asphalt
cement during mixing, transporting, placing, compaction, and loading
under traffic in order to minimize or avoid failures. Knowledge of the con-
sistency under summer temperatures and shear properties under winter
temperatures is a requisite to providing durable pavements.
Asphalt cement can go from a liquid during mixing, transporting, and
placing to a plastic during compaction and service under traffic, and even
to a solid at low service temperatures. Satisfactory performance requires a
knowledge of the asphalt consistency under all conditions.
It can be readily seen that all asphalts will not meet all of the perform-
ance criteria required and that with asphalts from a wide geographic range
available to a single producer there is and has been a need for better
methods of characterizing, testing and specifying asphalt cements.
This Symposium on Viscosity Testing of Asphalt and Experience with
Viscosity Graded Specifications was organized to bring to the attention of
the entire country the latest viscosity testing which, is somewhat region-
alized, and the experience gained by a few states which have used viscosity
graded asphalt specifications.
Although not intended to be a state of the art, it serves that kind of
purpose in these areas which are still somewhat limited in the scope of
their applications.
This special technical publication should be of use to those individuals
in asphalt testing, to materials engineers or supervisors, and to those con-
cerned with writing specifications.
The information included in this publication illustrates that viscosity
testing of asphalts is very much in a stage of transition with a shift from
Thin-Film Oven Testing to Rolling Thin-Film Oven Testing, and the small
amount of information concerning low-temperature viscosity testing is an
indication of the need for more work and better test methods and equip-
ment.
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It also becomes readily apparent that, although much has been said and
written on the subject of viscosity graded specifications, there is still only
limited experience in their use.
W. G. Gunderman
Engineer of Materials and Construction,
Highway Research Board,
National Academy of Sciences,
Washington, D. C , 20418;
symposium chairman.
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H. E. Schweyer,^ J. P. Moore,^ and J. K. Ling^
Temperature Susceptibility
One outgrowth of the preceding anomalies noted in the literature was an
in-depth study of the temperature susceptibilities of asphalt cements above
the range of 60 C (140 F) in order to quantitize the effect of temperature
variations at 60 C (140 F).
Stanfield [7] studied susceptibility and reviewed the various proposed
evaluations to that date. Crouch and Cameron [14] presented a review of
seven viscosity-temperature equations for lubricants. More recently Jonge-
pier and Kuilman [75] updated such studies, and numerous investigators
have considered correlations based on activation flow energies and shift
factors. Davis [76] has presented data on coal tars and asphalts. Similar
analyses have been summarized by Ling [17]. The ASTM Standard Test
method [18] has been found generally applicable as a quantitative graphical
representation of the temperature relation.
Certain data for asphalt cements are plotted on the ASTM chart in Fig. 1
for asphalts identified in Table 1, and the analysis can be quantitized as
follows:
In (log v) = M In T + In B (1)
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SCHWEYER ET AL ON RHEOLOGY OF ASPHALT CEMENTS 5
347°F 383°F
175°c 195°C
TEMPERATURE
where
ri = viscosity, centipoises
T = absolute temperature, deg R = 459.7 + deg F
M, B = constants derived from analytical geometry
The equation is confirmed by experimental data as shown in Fig. 1 for
data at 140 F and above. Equation 1 may be expressed as
In [(log n)/B\ = MlnT = lnTM (2)
and
log rj = BTM (3)
Thus
•q = e2.303BrW (4)
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6 VISCOSITY TESTING OF ASPHALT
This form, it is recognized, desensitizes the data but does relate the results
empirically as well as any other relation.
The differential rate of change of viscosity with temperature is the
derivative of Eq 4:
dv/dT = (2.3035M)7 w - 1 e 2 - 303BrM (5)
which is seen to be a function of both the constants as well as the absolute
temperature.
To evaluate M, the slope of the viscosity-temperature chart, the two-
point formula is used to evaluate both B and M. If y is the left side of Eq 1,
and x = In T:
(y - yd = - — - O - *0 = *t(x - *o (6)
M — X\
and
In B = - M In T + In (log v) (7)
at 7\ = 1:
B = log T/i (8)
The parameters have been evaluated for the asphalts as listed in Table 1.
In Table 2, the effect of small temperature variations at 60 C is given for
three asphalts with high and low susceptibilities. These results show about
a 7 percent variation in viscosity for an 0.5 C (0.9 F) change in tempera-
ture. These numbers provide a quantitative value for the temperature
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SCHWEYER ET AL ON RHEOLOGY OF ASPHALT CEMENTS
Calculated Viscosities
Parameter, M Viscosity-
Asphalt Table 1 degC (deg F) Kilopoises
Experimental
The experimental work consisted of measurements of absolute viscosities
under varying shear rates and conditions at 60 C (140 F), including some
information at other temperatures.
The apparatus used were the Cannon-Pressure, Cannon-Manning, and
Cannon-Zeitfuchs instruments shown in Fig. 2, with their control panel
and bath arrangement as shown in Fig. 3, and the Florida capillary arrange-
ment [13] as illustrated in Fig. 4.
It should be recognized that there are two basic differences in the modus
operandi of these methods. These differences in flow regimes produce
different rheological results. In the Cannon-Manning instrument the flow is
more or less transient, depending upon the relative size and length of the
flow reservoirs compared with the flow length of the constricted flow tube.
In the Cannon-Pressure instrument the major flow resistance is through an
orifice into a flow tube and reservoir of large diameter. The transient flow
effects here depend upon the relative pressure drops in the two flow sections
(orifice and tube) of the apparatus. In the Florida capillary method, the
transient flow effects are minimized by selection of the apparatus dimen-
sions so that the major portion of the pressure drop occurs in the capillary
tube section.
In all of these apparatus the complex flow patterns where the material
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8 VISCOSITY TESTING OF ASPHALT
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SCHWEYER ET AL ON RHEOLOGY OF ASPHALT CEMENTS 9
COMPRESSION
Uu
LOAD —
CELL
MOVING
CROSSHEAD "
R M Up—
LOAD
CELL
EXTENSION
SELF
RHEOMETER ALIGNING
PLUNGER SUPPORT
FIXED
SUPPORT
--E }
RHEOHETER
BARREL
ASPHALT
SAMPLE
RHEOMETER
SAMPLE TUBE
enters the capillary or orifice result in the material in the center of the
flow path being subject to extension forces, which lead to elongational
viscosity considerations; see Cogswell and Lamb [19].
Results
Comparative viscosity results at 60 C (140 F) on a variety of asphalts
are given in Table 3. The following points are observed and should be
considered in light of the remarks of the preceding section.
In general, there appears to be a trend of higher viscosities at higher
pressure drops in the Cannon-Manning data. This is not true for every
set of data. Data at about 0.70-atm driving force for the Cannon-Manning
and Cannon-Pressure apparatus appear to be in reasonable agreement. In
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10 VISCOSITY TESTING OF ASPHALT
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SCHWEYER ET AL ON RHEOLOGY OF ASPHALT CEMENTS 11
CANNON-MANNING VACUUM
VISCOMETERS
-10.5 -0.73 0.64 1.69" 0.694
- 8.8 -0.40 0.80 1.72'' 0.708"
- 2 -0.13 0.98 1.72" 0.748
CANNON-PRESSURE VISCOMETERS
2 0.12 1.06 2.07 1.25
4 0.24 1.12 1.85 1.03
8 0.54 1.27 1.87 0.976
10 0.68 1.34 1.80 0.972
25 1.70 1.85 1.77 0.904
50 3.4 2.7 1.58 0.890''
100 6.8 4.4 1.45 0.907"
150 10.2 6.1 1.28 0.622"
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12 VISCOSITY TESTING OF ASPHALT
Florida Capillary
Cannon Viscosity
Pressure Complex -
Flow 0.05 1.0 10' ergs
Asphalts 25 psi Index, C s' 1 s-' per s-cm*
Discussion
These differences in viscosity results at 60 C (140 F) are not surprising
when the rheological problems are recognized. For example, it is well known
that asphalts exhibit anomalous or complex flow behavior. They may not
follow the power law over all ranges of stress. Furthermore, in the Florida
Asphalt Laboratory, Lodge [20] has demonstrated that the viscosity of
asphalts at 25 C (77 F) increases with pressure, which obviously can affect
the results of the type presented.
If the data are viewed from a knowledge of these effects, the results seem
to be in order. Thus, as the absolute pressure increases for the transient
vacuum method, the viscosity increases slightly.
For the Cannon-Pressure instrument transient data, the decrease in
viscosity with increased pressure drop for the same instrument is in general
attributed to shear thinning effects by anomalous flow. This results in
lower viscosity at increased pressure drops as shown in Table 4 and Fig. 5.
4.0
• NO. 6 A I R BLOWN
3.0 . 0 ^.v,u.~.
VISCOSITY, KILOPOI
•••
-_#___^
^ - *
3)1
£o? A
«"
2 3 4 5
AVERAGE IMPOSED PRESSURE, ATMOSPHERES
The transient mode gives a generally lower average pressure than that for
a steady-state flow over the same flow path length, which tends to limit the
effect of imposed pressure where the latter causes an increase in observed
viscosity.
Since the data in Table 3 for the Florida capillary were taken at a con-
stant rate of shear, it was considered desirable also to compare results at
constant stress by a new method under development by the first author [21].
Some data are shown in Table 6, where it is observed that the Florida capil-
lary constant stress data at 150-psi upstream gage pressure and the constant
shear rate data are about the same magnitude but differ from the results
Viscosity, kilopoises
°6 At 30-cm Hg vacuum.
c
At 10 psig.
d
Regular capillary method, one-atm downstream pressure.
High-pressure method extrapolated to a 1-atm downstream pressure.
' High-pressure run at 400-atm downstream pressure, run at constant rate of shear mode
and read at one reciprocal second.
capillary and sample tube, the imposed pressures, the compressibility of the
material, and its composition must be considered. The first author hopes
to work on a few of these problems in the future.
Conclusions
It is important to recognize that differences in asphalt viscosity results
can be obtained in order that nonbiased inferences are made in asphalt
technology. By exploring the basic underlying physical phenomena the
differences can be explained, and from this information correct conclusions
can be drawn.
The problems associated with the results shown in the paper should not
discourage the use of viscosity grading specifications for asphalts. It is
important first to recognize any problems that might exist, to resolve them
with available knowledge, and then to reconcile the results by different
methods. In general, resolution of the problems will be accomplished
readily for asphalt rheology by standardizing the most appropriate appara-
tus and test procedures used.
References
[/] Stanfield, K. E. and Hubbard, R. L., "Asphalts from Rocky Mountain Crude Oils,"
U.S. Bureau of Mines, Technical Paper 717, 1949.
[2] Traxler, R. H., Schweyer, H. E., and Romberg, J. W., Industrial and Engineering
Chemistry, Vol. 36, 1944, p. 823.
[3] Lewis, R. H. and Welborn, J. Y., Public Roads, Vol. 21, 1940, p. 1.
[4] Lewis, R. H. and Halstead, W. J., Public Roads, Vol. 21, 1940, p. 127.
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SCHWEYER ET AL ON RHEOLOGY OF ASPHALT CEMENTS 15
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J. V. Evans^ and J. W. Gorman^
Experimental
The six laboratories and the instruments they used are given in Table 1.
Except for the falling plunger, each instrument was used by two labora-
tories; one laboratory used two instruments. The nominal viscosities of the
two asphalts (designated A and B) are listed in Table 2.
Sliding Plate
Viscosity
Viscosity, poises at 60 F,
megapoises
Asphalt 275 F 140 F (0.05 s"1)
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18 VISCOSITY TESTING OF ASPHALT
Rigorous Handling"
1. Make sure 3-oz tin cover is in place but the lid is readily removable (some portions of
steps, 2, 3, 4, and 5 are concurrent).
2. Place tin in oven maintained at 275 F + 5 F.
3. Keep tin in 275 F oven for 60 min ± 3 min.
4. Place portion of viscometer equipment related to holding the sample in oven at 140 F
+ 5F.
5. Keep equipment in 140 F over for 30 min ± 3 min.
6. Remove equipment from 140 F oven; remove 3-oz tin from 275 F oven; remove lid
from tin and pour sample. This should be accomplished within 3 min and done in a
room at an ambient temperature between 70 and 80 F.
7. Allow equipment to cool in room for 45 ± 3 min.
8. Place equipment in 60 F bath ± 0.02 F using a calibrated thermometer. Allow to
remain in bath before start of testing for 30 min ± 3 min.
9. Start testing (total lapsed time to this point should be 138 ± 9 min).
Loading Sequence
Increasing—Start with low load to yield approximately 1 X 10~3 rate of shear at equi-
librium and record data necessary for viscosity calculation. Increase load to yield five
shear rates over the range 1 X 10 -3 to 1 X 10_1 s~>.
Decreasing—Reverse of above starting with a load to produce a 1 X 10_1 rate of shear
and decreasing load to yield five shear rates over the range 1 X 10~3 to 1 X 10-' s -1 .
Normal
Use your normal laboratory technique in its entirety. Please describe if it differs from
that published in ASTM.
" The intent of this technique is to require as close attention to (1) sample-handling times
and (2) apparatus and sample heating as is compatible with the different instruments.
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EVANS AND GORMAN ON VISCOSITY TESTING AT 60 F 19
2. Test No. 14
14. Testing d e t a i l s
Viscometer*
Record in order of t e s t Time Constant Constant Shear
Load Displacement (Sees.) (Viscosity) Viscosity (Shear Rate) Rate
grams degrees dynes/cm
500 1 1576.0 128,910 1.26 x 10° 1.615 .001025
1000 1 749.3 257,910 1.20 x 10 8 1.615 .002156
2000 1 305.4 515,910 9.76 x 10 7 1.615 .005288
6000 1 62.5 1,547,910 5.99 x 10 7 1.615 .02584
16000 6 59.8 4,127,910 2.55 x 10 7 1.615 .1620
*Shear Stress
FIG. 1—Typical data report.
There were too few laboratories for any one instrument to give reliable
estimates of instrument repeatability and reproducibility. The data are also
really not suitable for an overall variance estimate.
Within-Laboratory Standard Deviations
Table 5 shows the influence of the two sample-handling procedures on
the within-laboratory standard deviations. Generally, the rigorous pro-
cedure is statistically equivalent to or better than the normal. The two
exceptions are the Bureau of Public Roads and the Asphalt Institute.
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20 VISCOSITY TESTING O F ASPHALT
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EVANS AND GORMAN ON VISCOSITY TESTING AT 60 F 21
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H
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22 VISCOSITY TESTING OF ASPHALT
SHSIOd 'A1ISOOSTA
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EVANS AND GORMAN ON VISCOSITY TESTING AT 60 F 23
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24 VISCOSITY TESTING OF ASPHALT
A. NORMAL
SLIDING PLATE (REG) U4
MEGAP OIS
D SHELL
• ASPHALT INST.
C O N E PLATE
0 AMERICAN t
VISCOS
• ASPHALT INST.
B. RIGOROUS C. RIGOROUS
(INCREASING) (DECREASING)
3 4 5 6 7 8 3 4 5 6 7 8
SAMPLE A. MEGAPOISE SAMPLE A, MEGAPOISE
(controlled shear) test did not demonstrate this effect. There is an indication
in the data that this effect is sample-related which implies that additional
procedural controls are possible.
Handling
Laboratory
Comparison Normal Rigorous
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EVANS AND GORMAN ON VISCOSITY TESTING AT 60 F 25
Acknowledgments
The authors wish to thank the participants in this program: J. Y. Wel-
born and W. J. Halstead, Bureau of Public Roads; V. P. Puzinauskas,
The Asphalt Institute; H. R. Hawthorne, Gulf Oil Canada Ltd; C. C.
Evans, Shell Development Co.; R. L. Dunning and R. S. Hodgson,
Douglas Oil Co.; and L. C. Brunstrum and A. W. Sisko, American Oil Co.
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26 VISCOSITY TESTING OF ASPHALT
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EVANS AND GORMAN ON VISCOSITY TESTING AT 60 F 27
References
[1] Welborn, F. Y., Oglio, E. R., and Zenewitz, J. A., Proceedings, Association of Asphalt
Paving Technologists, Feb. 1966, p. 19.
[2] Puzinauskas, V. P., Proceedings, Association of Asphalt Paving Technologists, Feb.,
1967, p. 489.
[3] ASTM Standards, Part 11, March 1969, pp. 871-896.
[4] Hald, A., Statistical Theory and Engineering Applications, Wiley, New York, 1952,
p. 164.
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E. O. Busby^ andL. F. Rader^
tests as glass plates do. Film thicknesses of 100, 300, and 500 nm are used
on the steel plates depending on the grade of asphalt. Control of film thick-
ness is set by improved spacers. The procedure of testing is easier than with
glass viscometer plates. Since film thickness can be accurately chosen, it is
not necessary to weigh the plates, and the calculations are simplified. Also,
since the procedure with steel plates eliminates certain steps, operator time
and chance for error are reduced.
The linkage between the movable plate holder and the balance was
modified. The standard model instrument employs a chain connected to a
steel rod. With the large loads required for measurements at low tempera-
tures (for example, 39.2 F (4 C)), unexpected large deviations can occur
owing to deformation of the chain. This was partly corrected by replacing
the chain and rod with a phosphor bronze ribbon obtained from the manu-
facturer. The modified linkage and the modified steel viscometer plates
extend the range and precision of the microviscometer.
Despite the reports of superior repeatability by using the steel plates and
phosphor bronze ribbon, it should be pointed out that loads of over 1000
g required for testing at 39.2 F (4 C) overload the beam far beyond its
designed capability. The spring that holds the fixed viscometer plate is
overstressed and frequently gives way. The microviscometer should be com-
pletely redesigned to give satisfactory results at 39.2 F (4 C) and to with-
stand the stresses imposed on the instrument in testing asphalt cement at
this low temperature.
Range of Microviscometer
Evans and Griffin3 stated that the modified microviscometer has a work-
ing range of 10 to 104 megapoises. In spite of the difficulties just described,
Busby4 has verified this upper working range, obtaining a value of 15 000
megapoises on asphalt cement marked "C" at 39.2 F (4 C) (See Table 1),
but he recommends redesign of the instrument.
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30 VISCOSITY TESTING OF ASPHALT
Asphalt Cement
Property
Asphalt Designation A B C
Summary
It is recommended that consideration be given by the manufacturer to
redesign the sliding plate microviscometer instrument to withstand the
stresses imposed by low-temperature testing. This recommendation is based
on the belief that asphalt paving technologists should be able to determine
viscosity of asphalt cements at a low temperature such as 39.2 F (4 C) in
an accurate and satisfactory manner.
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C. F. Potts^
REFERENCE: Potts, C. F., "Florida Studies with the Pnzjnauslcas Field Viscosity
Cup for Asphalt Cements," Viscosity Testing of Asphalt and Experience with
Viscosity Graded Specifications. ASTM STP 532, American Society for Testing
and Materials, 1973, pp. 31-39.
ABSTRACT: An ASTM base chart is shown in the paper to confirm the linearity
of the temperature-viscosity relation forfivedifferent asphalts over the temperature
range of 60 C (140 F) to 195 C (383 F). These data were run in the laboratory
using the procedures in ASTM methods D 2170 and D 2171. All data were cor-
rected to poises for plotting, using densities calculated at the test temperatures.
The viscosity temperature characteristics for different grades of asphalt from
several producers are shown in separate charts. Kinematic viscosities, as measured
with the Puzinauskas-Asphalt Institute (P-AI) field cup, in the laboratory, are
superimposed on these charts to illustrate the agreement of the (P-AI) data with
carefully controlled data from ASTM Methods D 2170 and D 2171.
Field data at actual construction sites were compared with check data rerun on
the field samples in the laboratory for agreement. It was found that for field tests
it is necessary for the cup and the asphalt cement in the cup to be at the test
temperature read on the thermometer. With experienced technicians, the field tests
readily agree with laboratory data.
KEY WORDS: viscosity, asphalts, bituminous cements, penetration, absolute
viscosity, kinematic viscosity, viscometer cup, specifications, bitumens
' Bituminous materials and research engineer. Office of Materials and Research, Florida
Department of Transportation, Gainesville, Fla. 32601.
2 The code form V60 refers to viscosity at 60 C (140 F) and V135 to viscosity at 135 C
(275 F) for purposes of simplification.
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Base Chart
The viscosity grading specification determines an allowable range of
V60, viscosity at 140 F (60 C) in poises, but stipulates only a minimum
V135,2 kinematic viscosity at 275 F (135 C). Accordingly, it is necessary to
establish a band of viscosities at the temperatures at which a field viscosity
will be within acceptable limits. Furthermore, this band may vary for each
supplier. In addition, it is desirable to have a provisional band where final
approval would depend upon verification tests at V60 (140 F) (60 C).
To establish these acceptable bands, it is necessary to develop base data
on typical asphalts such as in Fig. 1. The samples were in Cannon-Manning
vacuum viscometers according to ASTM Method D 2171-66—Absolute
Viscosity of Asphalts— at the lower temperatures and by ASTM Method
D 2170-67—Kinematic Viscosity of Asphalts—for the higher temperatures.
It will be noted that all viscosity data are in poises, which means that the
kinematic viscosity data as measured in stokes at the higher temperatures
have been multiplied by the density at the test temperature. The equation
o. il 1 1 i i i i i i i i 1 1—
140 160 180 200 220 240 260 280 300 320 340 360 380
TEMPERATURE, deg F
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POTTS ON PUZINAUSKAS FIELD CUP STUDIES 33
for the density relation including the calculation for viscosity is as follows
(see also ASTM method D 2170-67):
Viscosity in poises = (kinematic viscosity in stokes)
(P - 0.61 AT X 10-3)
(1)
where
p = density at a known temperature and
AT1 = incremental temperature difference in degrees Celsius above
temperature at which the density is known. Celsius is absolute
temperature on a centigrade scale = 273 + deg C.
For example, if p is 1.0147 g/cm3 at 25 C (77 F), and the test temperature
is 135 C (275 F), then 135 C = 408 deg Celsius. For a kinematic viscosity
often stokes, the viscosity in poises becomes (since AT = 408 — 298 = 110
deg Celsius):
V135 = 10(1.0147 - 0.61 X 110 X lO"3) = 10 X 0.948
= 9.48 poises
For any asphalt, if the density at some temperature is known, it is substi-
tuted in Eq 1 and the appropriate temperature increment used. Where
the density of the asphalt is not known, a value of 1.0147 g/cm3 at 25 C
(77 F) may be assumed. For this assumed density at 25 C (77 F), correction
factors for density at other temperatures may be taken from Table 1 or Fig. 2,
_i i i f-K i i i i i i i
150 175 200 225 250 275 300 325 350 375
TEMPERATURE, deg F
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34 VISCOSITY TESTING OF ASPHALT
which agree with the procedure of ASTM D 2170-67. The last column is
the correction density factor for an assumed value of 1.0000 g/cm3 at 25 C
(77 F), which may be of some use.
TABLE 1—Correction factors and densities for assumed conditions.
Calculations
The P-AI field cup as received has a precalibrated constant that, when
multiplied by the efflux time, gives the kinematic viscosity in centistokes
or stokes. However, the desired results are in absolute units or poises, which
requires understanding the basis relations that are readily clarified.
If the instrument constant is C, in stokes per second, then the absolute
viscosity is:
r\p = C,pt, poises (2)
where
t = efflux time, s and
p = density at temperature T, g/cm3.
For a limited temperature range where an average density, pr, may be
considered constant, a combined constant for absolute viscosity, Cp, in
poises per second, may be used so that
•tjj, = Cpt, poises (3)
where the absolute viscosity constant Cp = C,pT- Thus, efflux times are
converted directly to absolute viscosity (in a given temperature range) by
multiplying the time by the C„ constant. (Note: 1 poise = 100 centipoises
and 1 stoke = 100 centistokes.)
The operator measures the efflux time for an "on-site" sample and
multiplies the time by the appropriate constant depending upon the data
desired at the measured temperature. This provides the operator with a
measure of the viscosity and whether or not it has a high probability of
meeting specifications. In making measurements it is assumed that a proper
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36 VISCOSITY TESTING OF ASPHALT
technique is used to ensure that the cup is at temperature and that the
measured temperature is correct for the material in the cup at the time of
test.
Experimental Data
Data obtained on a 5-gal can sample heated in an oven and tested peri-
odically over a range of temperatures are shown in Fig. 4 for asphalts of
two different grades. Experimental laboratory data were obtained in
Cannon viscometers by ASTM Methods D 2170 and D 2171 over a tem-
perature range of 140 F (60 C) up to 383 F (195 C). Data obtained with
the P-AI cup are superimposed on these lines and show excellent agreement
except for several outliers. In all cases, the outliers are explained by in-
sufficient temperature equilibration time or inexperienced operators. The
lines shown in Fig. 4 were arbitrarily drawn parallel through the points
and essentially define the slope to be expected for this source. It is necessary
to know this expected slope from any supplier in order that data at high
temperature in the field may be extrapolated to 140 F (60 C).
Results for one set of field test data are shown in Fig. 5. Good agreement
of the field results with laboratory results on a retained sample are shown.
The outlier shown at the high temperature is attributed to some test error.
The outliers shown at the lower temperature are attributed to cooling of
the sample and viscometer cup during the longer flow times at these tem-
oi I i i i i i i 1 1 i 1 1 1
140 160 180 200 220 240 260 280 300 320 340 360 380 400
TEMPERATURE, deg.F
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POnS ON PUZINAUSKAS FIELD CUP STUDIES 37
l(ft .
02 -
Acceptability Diagram
Based on the above data and other information, a proposed acceptability
basis diagram has been drawn up for one grade (AC-20) of asphalt. The
control chart is in the exploratory stage and must be considered only in a
preliminary manner as demonstrating how field control can be exercised by
use of the P-AI instrument. Any acceptability diagram will vary with the
specification ranges and the suppliers' materials. Accordingly, they must
be designed separately depending upon individual requirements.
A test diagram is shown in Fig. 6 for various situations assuming that a
top limit for V135, viscosity at 275 F (135 C), is twice the minimum of 3.00
stokes (2.84 poises) or 5.68 poises as shown for an AC-20 where V60,
viscosity at 140 F (60 C), is 2000 ± 400 poises.
Line A is for minimum limits, which establishes one temperature suscep-
tibility value (the rate of change in viscosity with temperature) that is
evaluated from the slope of Line A. Line B is drawn as the maximum limits
for the assumed maximum V135 viscosity (275 F) (135 C). Line C is parallel
to Line A and drawn through the maximum of 2400 poises at 140 F. Line D
is drawn through minimum viscosity V135 (275 F) (135 C) and maximum
allowable viscosity at 140 F (V60). It represents a maximum slope. The
line for E was drawn through the minimum V60 (140 F) (60 C) and the
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38 VISCOSITY TESTING OF ASPHALT
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POnS ON PUZINAUSKAS FIELD CUP STUDIES 39
^^
^
^ ^ ^
1.0
0.8 ~
^v. LINE E.MIN. SLOPE
o.e
0.4
0.3 - L I N E D , MAX.SLOPE
1 1 1 1 1 1 1 1 1 1 I I
0.2
270 280 290 300 310 320 330 340 350 360 370 380 390 400
TEMPERATURE, d . g F
central area of Fig. 7, as established for Case I, but not outside the total
area of Fig. 7.
Case III. Rejection: Any confirmed set of multiple points that fall out-
side of the total area would be sufficient cause for rejection.
Acknowledgment
Some portions of the results reported in this paper were obtained under
a research contract sponsored by the Florida Department of Transportation
at the University of Florida's Engineering and Industrial Experiment
Station with H. E. Schweyer as principal investigator.
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L. W. Corbett^ and H. E. Schweyer^
There are numerous methods and relationships by which both the con-
sistency level and the general rheological properties of an asphalt have
been measured, each of which has served a useful purpose. With increasing
use today of standard methods for determining absolute viscosity at 140 F
(60 C) [If and kinematic viscosity at 275 F (135 C) [2], there are better
opportunities for defining the engineering properties of asphalt cement
binders [3,4,5]. Perhaps one of the biggest contributions that viscosity
testing has made is that it is revealing rheological properties that previously
were hidden under the empiricism of the older methods. As a result, new
efforts are being made to grade on viscosity as well as to define related
rheological properties using high- and low-temperature viscosity and pene-
tration [6].
It is the objective of this paper to point out some of the inherent rela-
tionships involving three of the common standard consistency tests being
' Research associate, Esso Research and Engineering Co., Linden, N. J. 07036.
^ Research professor. Department of Chemical Engineering, University of Florida,
Gainesville, Fla. 32601.
' The italic numbers in brackets refer to the list of references appended to this paper.
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42 VISCOSITY TESTING OF ASPHALT
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CORBETT AND SCHWEYER ON ASPHALT CEMENT 43
TABLE 1—Continued.
—T 1 r 1 1 1 r- 1
1
500
400 - "
300 -
V.
K 200 ^v -
o
o
U_
-
•
<
o 100 - -
< \
£ 80
UJ
Z
•v.
UJ
a.
60
40
V
-
30 - -
20
1- -I 1 1 '
200 300 400 600 8 0 0 1000 1500 2000 3000 4 0 0 0 5000
VISCOSITY AT 140 F, poises
FIG. 1—From a single source the relationship between viscosity at 140 F (60 C) and
penetration at 77 F (25 C) may be defined by log-log straight line.
outside limits for this relationship. These observed limits are the lines for
maximum and minimum penetration levels (asphalt Nos. 39 and 10) with
their corresponding slopes. Each of the 84 asphalt series can be plotted
within these outside lines. There also appears to be some degree of uni-
formity in slope (varying from 0.56 to 0.82) with a very slight convergence
of all lines in the direction of lower viscosity. In general, it is noted that
asphalt sources yielding cements with higher penetrations have the lowest
slope factors, and those yielding lower penetration cements have the highest
slope factors.
Figure 3 was prepared to illustrate further the relationships of penetra-
tion with viscosity. For a given source and given viscosity, the penetration
value for that asphalt cement can be calculated from Eq 1, or it can be
determined by plotting the line and determining the penetration graphically.
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CORBETT AND SCHWEYER ON ASPHALT CEMENT 45
200 300 400 600 800 1000 1500 2000 3000 4000 5000
VISCOSITY AT 140 F, poises
FIG. 2—Most asphalt cements fall within outside parameters of viscosity at 140 F (60 C)
versus penetration at 77 F (25 C).
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46 VISCOSITY TESTING OF ASPHALT
I . , , , I , , , , ]
200 300 400 600 800 1000 1500 2000 3000 4000 5000
VISCOSITY AT 140 F, poises
it should also be satisfactory for the upper half of the viscosity range as
well, since only its viscosity level has been changed. Because the viscosity
(140 F) in conjunction with penetration (77 F) largely defines the viscosity-
temperature or the stiffness-temperature properties, both the grade and the
temperature susceptibility of asphalt cement binder can be covered by this
single simple relationship.
These considerations can lead to a better description of asphalt cement
by defining the minimum penetration as a function of the variation of
viscosity level, as illustrated in Fig. 5. This would provide for realistic
variation in penetration as dependent on the viscosity level, thus identifying
the grade while more accurately defining its viscosity-penetration relation-
ship. For the manufacturer or purchaser to determine compliance with
specification would require only a single test for viscosity and a single test
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CORBETT AND SCHWEYER ON ASPHALT CEMENT 47
1 1 T 1 1 1 1 I 1
AC-2|
*— Range*-
FIG. 4—Some specification requirements are not consistent with normal characteristics of
asphalt cement.
for penetration on any one asphalt cement in a given grade and from a
given source. The point that is stressed here, however, is that minimal values
of a dependent variable (penetration) should be related to an identified
level of the independent variable (viscosity) in order to be consistent with
normal viscosity-penetration characteristics. This can be accomplished by
specifying the minimum penetration at the midviscosity level of each grade,
which essentially governs the penetration at both upper and lower limits
for the grade. For example, the specification for an AC-10 asphalt cement
could read, "Penetration (77 F) shall be a minimum of 70 at the viscosity
(140 F) level of 1000 poises."
Several asphalt temperature-susceptibility characteristics can be deter-
mined when computing from a basic reference level; for example, viscosity
at the 90 penetration level or the penetration at the 2000 viscosity level.
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48 VISCOSITY TESTING OF ASPHALT
AC-21
••— Range*.
I . 1 1 1 I I . 1 1 1——J
200 300 400 600 800 1000 1500 2000 3000 4000 5000
VISCOSITY AT 140 F, poises
FIG. 5—Penetration when identified with viscosity level is more consistent with normal
characteristics of asphalt cement.
TABLE 2—Typical intercept and slope factors for high- and low-viscosity asphalts.
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CORBETT AND SCHWEYER ON ASPHALT CEMENT 49
T t
200 300 400 500 600 800 1000 1500 2000 3000 4000 5000
VISCOSITY AT 140 F, poises
FIG. 6—Relationship between viscosity at 140 F (60 C) and viscosity at 275 F (135 C) may
also serve in the characterization of asphalt cement.
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50 VISCOSITY TESTING OF ASPHALT
TABLE 3—Typical intercept and slope factors for high- and low-viscosity asphalts
when based on viscosity-viscosity relationships.
The viscosity (140 F) at the 300 centistokes level (275 F) as well as the
viscosity (275 F) at the 2000 poise level (140 F) both appear to have possi-
bilities for identifying temperature-susceptibility qualities in the same
fashion, as when dealing with viscosity (140 F) and penetration (77 F). Of
these two, the viscosity (275 F) at the 2000 poise (140 F) level, or at any
other grade level, appears to best satisfy the need for identifying the grade
while describing the viscosity-susceptibility properties.
Summary
1. The relationship between viscosity (140 F) and penetration (77 F) as
well as between viscosity (140 F) and viscosity (275 F) can be described
by power-law logarithmic functions when applied to asphalt cements of
varying consistency level derived from a single source.
2. Asphalt cements from each source therefore can be characterized by
penetration intercept and slope factors using these functions. When con-
sidering asphalt cements prepared from 84 sources, it is found that the
overall relationship of viscosity to penetration is represented by a nesting
of lines with significant differences in penetration level but with only minor
differences in slope.
3. Because the relationship between viscosity (140 F) and penetration
(77 F) is characteristic of the source of an asphalt cement, these two tests
can be used to identify the viscosity grade while indicating temperature
susceptibility as measured by the penetration.
4. The viscosity (275 F) at a given viscosity (140 F) level also appears
to have possibilities for identifying the viscosity grade, as above, while
describing the viscosity-susceptibility properties as related to the source
of the asphalt cement.
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CORBETT AND SCHWEYER ON ASPHALT CEMENT 51
References
[I] ASTM Standard Method D 2171-66.
[2] ASTM Standard Method D 2170-67.
[3] Fundamental Viscosity of Bituminous Materials, ASTM STP 328, American Society
for Testing and Materials, 1962.
[4] Grading of Paving Asphalts by Viscosity at 140 F Versus Penetration at 77 F, ASTM
STP 424, American Society for Testing and Materials, 1966.
[5] Highway Research Record, No. 350, 1971.
[6] AASHO Viscosity Graded Asphalt Cement Specification M 226-70, American Asso-
ciation of State Highway Officials.
[7] Halstead, W. J. and Welborn, J. Y., Highway Research Record, Vol. 350, 1971.
[8] Puzinauskas, V. P., Proceedings, Association of Asphalt Paving Technologists, Vol. 36,
1967, p. 489.
[9] Welborn, J. Y., Oglio, E. R., and Zenewitz, J. A., Proceedings, Association of Asphalt
Paving Technologists, Vol. 35, 1966, p. 19.
[10] Corbett, L. W., Proceedings, Association of Asphalt Paving Technologists, Vol. 39,
1970, p. 481.
[11] LeFebvre, J. A., Proceedings, Association of Asphalt Paving Technologists, Vol. 39,
1970, p. 443.
[12] Fromm, H. J. and Phang, W. A., Highway Research Record, Vol. 350, 1971, p. 30.
[13] Burgess, R. A., Kopvillem, O., and Young, F. D., Proceedings, Association of Asphalt
Paving Technologists, Vol. 40, 1971, p. 148.
[14] Duthie, J. L., Proceedings, Association of Asphalt Paving Technologists, Vol. 41,1972.
[15] Christison, J. T., Murray, D. W., and Anderson, K. O., Proceedings, Association of
Asphalt Paving Technologists, Vol. 41, 1972.
[16] New Jersey, New York, and New England States Testing Engineers Association modi-
fication of AASHO Viscosity Graded Asphalt Cement Specification M 226-70.
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R. J. Schmidt^
' Senior research associate. Chevron Research Company, Richmond, Calif. 94802.
^ The italic numbers in brackets refer to the list of references appended to this paper.
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54 VISCOSITY TESTING O F ASPHALT
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SCHMIDT ON A ROILING THIN-FILM OVEN TEST 55
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56 VISCOSITY TESTING OF ASPHALT
1.0
0.8
0.6
0.4-
0.2- AS B D
B
Xo 0 S S C P G°
o C s r B
=> o>
i I o. i _
0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6
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FIG. 1—Comparison of TFO and RTFO weight losses obtained in cooperative test program.
20
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Penetration Grades
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SCHMIDT O N A ROLLING THIN-FILM O V E N TEST 57
1.0
• Weight Losses on Tables 1 and 2
0.6
A k
0.4 -
o
u.
I—
0.2
0.1
~r^r
0.1 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6
TFO W e i g h t Loss, %
are established for each test exposure. The latter alternative seems im-
practical.
A good solution to this dilemma would be another oven exposure which
affects asphalts in the same way as the TFO. This objective has been sub-
stantially accomplished by converting the RTF oven from a convection
oven to a forced-draft oven. The extra circulation not only improves the
uniformity of oven temperature but also changes the type of exposure so
its effect on asphalt is more nearly like the TFO exposure. The added circu-
lation causes more volatile loss to occur. This modified oven is identified
as the rolling thin-film circulating (RTF-C) oven.
» "" -10 ••
FIG. 4—Differences in percent penetration retained between TFO and RTFO exposures.
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58 VISCOSITY TESTING OF ASPHALT
Description of Oven
The RTF-C oven is shown in Fig. 5. The change involves installation3 of
a blower which takes air directed by a plenum chamber from the bottom
of the oven. The plenum chamber is only a sheet-metal insert, The squirrel-
cage blower is driven by a shaft passing through a pair of high-temperature
ball bearings. This blower shaft is coupled to the motor shaft by a flexible
coupling. Thermistor control elements from the electronic proportional
controller are no longer placed in the center of the oven chamber but, in-
stead, are placed in the center of the blower discharge. Also placement of
the thermometer is moved to the side so it can be readily observed. If left
in the center rear, it would be hidden by the blower.
RTFO RTF-C
Cycle Cycle
Avg, deg F Spread, deg F Avg, deg F Spread, deg F
Test Procedure
The procedure is identical with the California Division of Highways
Test Method 346-D and ASTM D 2872-70 except that the modified oven is
3
A kit to modify existing RTFO can be obtained from Cox and Sons, P. O. Box 674,
Colfax, Calif. 95713.
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SCHMIDT ON A ROLLING THIN-FILM OVEN TEST 59
/ SI
Comparison of Results
In Tables 1 and 2 are shown the results of testing a number of asphalts
by three different test exposures: the TFO, RTFO, and RTF-C. Com-
parison and differences between the TFO and RTF-C weight losses and
percent penetration retained (PPR) are illustrated in Figs. 6 and 7. Weight
losses are shown in Fig. 6 to be very nearly equal for both tests. Our TFO
No. 1 oven is slightly more severe; whereas, our TFO No. 2 oven is slightly
less severe than the RTF-C.
Examination of Fig. 7 shows a similar relationship for PPR. The differ-
ence between our No. 1 TFO PPR and the PPR after RTF-C exposure is
at most 5.3 percentage points. The ASTM repeatability precision of the
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60 VISCOSITY TESTING OF ASPHALT
10
A
t*
r
A
A
fr A
A
-10
-20
40/50 60/70 85/100 120/150 200/300
Penetration Grade
FIG. 7—Comparison of differences between percent penetration retained between TFO and
RTF-C exposures.
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SCHMIDT ON A ROLLING THIN-FILM OVEN TEST 61
gests that our repeatability on the PPR is as good as our ability to repeat
penetration tests. Similarly, the repeatability of the weight losses appears
to be exceptionally good. Reliable repeatability studies on the RTFO for
PPR and weight losses are not available for comparison. However, our own
experience indicates the RTF-C precision to be better than the RTFO.
Six typical straight-run, quite different, West Coast asphalts were chosen:
two California Valley, two California Coastal, and two Los Angeles Basin.
One member of each pair of asphalts was a 60-70 penetration grade and
the other member a 200-300 penetration grade.
Each laboratory determined, for each asphalt, the penetration and
viscosity at 140 F (60 C) and 275 F (135 C) of the original asphalt and of the
TFO and RTF-C residua. Also determined were the weight losses resulting
from the TFO and RTF-C exposures. Duplicate exposures and tests were
made on all samples exposed to the RTF-C oven. This permitted repeat-
abilities as well as reproducibilities to be determined. Only reproducibilities,
however, could be calculated on the tests on the original asphalts and on
the TFO exposure.
Repeatability and reproducibility of the test methods determined in
accordance with ASTM STP 335 are included in Table 5, in which it is
shown that the reproducibility of test values found on the RTF-C residua
is slightly poorer than is found on the RTFO and TFO residua. This find-
ing is not unexpected because most of the collaborators had never used the
RTF-C oven before the 1971 test program. Since the program, informal
questioning by the author of several of the collaborators revealed cases
where some of them had not fully complied with the test procedures.
Examples were: use of on-off oven controls instead of an electronic pro-
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62 VISCOSITY TESTING OF ASPHALT
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SCHMIDT ON A ROLLING THIN-FILM OVEN TEST 63
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64 VISCOSITY TESTING OF ASPHALT
5.2
u_ «-
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FIG. 10—Comparison of TFO and RTF-C, viscosity at 140 F (60 Q (collaborative study).
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SCHMIDT ON A ROLLING THIN-FILM OVEN TEST 65
Its precision is better, and it is faster to do. Unfortunately, the two expo-
sures differ enough that they should not be used interchangeably without
separate specification limits for each test. A third oven exposure, the
RTF-C, is proposed which not only gives exposures very close to the well-
accepted TFO, but also seems to be at least as precise as the RTFO. Also,
it is just as fast to perform. It is suggested that this new oven exposure be
considered as a replacement for the RTFO test.
Acknowledgment
Repeatability and reproducibility estimates of the 1971 collaborative
tests and the computer plots in Figs. 8; 9, and 10 were made by M. J.
Hillyer of the Shell Development Company. Their permission to include
these data is appreciated.
References
[/] Lewis, R. H. and Welborn, J. Y., Proceedings, Association of Asphalt Paving Tech-
nologists, Vol. 12, 1940, p. 14.
[2] Schmidt, R. J. and Santucci, L. E., Proceedings, Association of Asphalt Paving
Technologists, Vol. 38, 1969, p. 39.
[3] Lewis, R. H. and Welborn, J. Y., Public Roads, Vol. 22, No. 2, 1941.
[4] Lewis, R. H. and Halstead, W. J., Public Roads, Vol. 24, No. 8, 1946.
[5] Pauls, J. T. and Welborn, J. Y., Proceedings, Association of Asphalt Paving Tech-
nologists, Vol. 21, 1952, p. 48.
[6] Santucci, L. E. and Schmidt, R. J., Grading of Paving Asphalts by Viscosity at 140 F
versus Penetration at 77 F, ASTM STP 424, American Society for Testing and
Materials, 1967.
[7] Hveem, F. N., Zube, Ernest, and Skog, John, Proceedings, Association of Asphalt
Paving Technologists, Vol. 33, 1963, p. 271.
[8] Skog, John, Proceedings, Association of Asphalt Paving Technologists, Vol. 36, 1967,
p. 387.
[9] Hveem, F. N., Zube, E., and Skog, J., Symposium on Road and Paving Materials,
ASTM STP 277, American Society for Testing and Materials, 1959.
[10] Schmidt, R. J., Painter, L. J., Skog, J. B., and Puzinauskas, V. P., Proceedings, Asso-
ciation of Asphalt Paving Technologists, Vol. 37, 1968, p. 476.
[If] Santucci, L. E. and Schmidt, R. J., Proceedings, Association of Asphalt Paving Tech-
nologists, Vol. 38, 1969, p. 65.
112] Santucci, L. E. and Schmidt, R. J., Highway Research Board Bulletin, No. 333, 1962,
pp. 1-9.
[13] Welborn, J. Y., "AASHO Viscosity Grading System for Asphalt Cement Specifica-
tions," Minutes of the 8th Pacific Coast Users and Producers Conference (1969),
Appendix C, p. 4.
[14] Youden, W. T., "Statistical Techniques for Collaborative Tests," Association of
Official Analytical Chemists, 1967.
[IS] 1971 Annual Book of ASTM Standards, Part 11, American Society for Testing and
Materials.
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p. S. Kandhal,^ L. D. Sandvig} W. C. Koehler} and
M. E. Wenger^
or both are needed. Hence, it has been the intent to study these suggested
viscosity-related parameters in relation to the performance of the in-service
pavements, to gather more information in order to develop optimum
specifications for paving asphalts.
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VISCOSITY TESTING O F ASPHALT
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KANDAHL ET AL ON PAVEMENTS IN PENNSYLVANIA 69
B 24 30 3§ W
TIME - MONTHS
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70 VISCOSITY TESTING OF ASPHALT
Viscosity
Viscosity at 77 F has been determined for shear rates of 0.05 and 0.001
s~\ and also at a constant shear stress of 1.63 X 104 dynes/cm 2 . This
shear-stress value has no particular significance except that so far it has
conveniently avoided any extrapolation of the experimental data at 77 F
for all the test asphalts. This constant-shear-stress system was included in
the study to determine an aging index similar to the one reported by
Chipperfield and Welch [9].
Plots of viscosity at 77 F (shear rate of 0.05 s -1 ) versus time in months
and absolute viscosity at 140 F versus time in months are given in Figs. 2
and 3, respectively.
Aging Index
Aging indexes have been determined considering the changes in viscosity
at 77 F (both 0.05 and 0.001 s _1 shear rates and at constant shear stress)
and viscosity at 140 F, as follows:
viscosity after aging
aging index =
viscosity before aging
40
MONTHS
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KANDHAl ET AL ON PAVEMENTS IN PENNSYLVANIA 71
SLM^O—I { i i | J4 Jo j . U'E 1 M
0 20 40 60 80
TIME - MONTHS
The use of this index (ratio) eliminated the variability caused by difference
in the viscosities of the original asphalts and gives a clearer picture of the
hardening rate [10].
Plots of these indexes versus time periods of aging were made. A typical
plot is given in Fig. 4.
Shear Susceptibility
The shear susceptibility (or shear index) value as employed in this study
is the tangent of the angle of log shear rate versus log viscosity determined
during performance of the viscosity test using the microviscometer. Shear-
susceptibility values have been determined for the six asphalts after in-
creasing periods of aging. Results are shown graphically in Fig. 5. The
relationship between shear susceptibility and aging index (based on vis-
cosity at 77 F) is shown in Fig. 6.
Temperature Susceptibility
To define the temperature susceptibility of the asphalt cements, a double
logarithm of viscosity in poises has been plotted against the logarithm of
the absolute temperature expressed in degrees (that is, empirical Walther's
equation). The numerical values for slopes of these lines have been indi-
cated as the temperature susceptibility of the asphalt cements within the
specified temperature ranges. At lower than 140 F temperature, slopes of
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72 VISCOSITY TESTING OF ASPHAIT
SS« 0.58
20 40 60
TIME - MONTHS
FIG. 4—Aging index [based on viscosity at 77 F (25 C), 0.05 sr1] versus time in months.
06
£4 80 86 Me
20 40 60 80
TIME-MONTHS
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KANDHAL ET AL ON PAVEMENTS IN PENNSYLVANIA 73
30
20
in
o
d
t
o
>
a . 78 M
X 42 M
s • 30M
x LOG Y = 0.579 + I.I79X
CORR. COEFF. * 0.893
8
z
FIG. 6—Aging index [based on viscosity at 77 F (25 C), 0.05 s'1] versus shear susceptibility.
the lines tend to deviate from slopes as established between 140 F and
higher temperatures, because shear-dependent viscosities are encountered
at lower temperatures. Therefore, the temperature-susceptibility data on
original and aged asphalts have been reported in Table 2 separately for
temperature ranges 39.2 to 77 F, 77 to 140 F, and 140 to 275 F. These data
are based on the average of four cores.
Temperature Susceptibility
39.2 to 77 range 77 to 140 F range 140 to 275 F range
Discussion of Results
While discussing the results, as follows, the pavement evaluation ratings
may be kept in view.
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74 VISCOSITY TESTING OF ASPHALT
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KANDHAL ET AL ON PAVEMENTS IN PENNSYLVANIA 75
Viscosity
Viscosity Viscosity at77F
Performance at77F at77F 1.63 X 10* Viscosity
Rating 0.05 s-1 0.001 s-1 dynes/cm2 at 140 F
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76 VISCOSITY TESTING OF ASPHALT
indexes. Very good correlation was obtained between aging indexes (based
on viscosity at 77 F) and the shear susceptibility values for these asphalts
(Fig. 6). This indicates that shear susceptibility is one of the major factors
affecting the pavement performance.
Therefore, it appears necessary to control the gain in shear susceptibility
during pavement service life. Skog [5] had stated that a most important
problem in asphalt specification requirements is the determination of the
maximum amount of shear susceptibility that may develop in a paving-
grade asphalt prior to pavement failure. Since Asphalt 1 is showing signs
of distress, referring to Fig. 5, it seems that this value is 0.58. However,
raveling started to show up in Asphalt 1 pavement after 24 months when
the shear-susceptibility value was around 0.40.
In Fig. 4, three distinct groups of asphalts can be seen according to aging
indexes and pavement performance ratings after 78 months in service:
Group 1
Asphalt 1 High shear susceptibility (>0.55). Performance poor.
Group 2
Asphalt 2
Asphalt 6 Intermediate shear susceptibility (0.35 to 0.45). Perform-
Asphalt 4 ance fair to good.
Group 3
Asphalt 3 Low shear susceptibility (<0.35). Performance good to
Asphalt 5 very good.
Unfortunately, no data are available on shear-susceptibility values for
these six asphalts just after mixing or for TFO residue. However, it appears
from Fig. 5 that except for Asphalt 1 the shear-susceptibility values for
Asphalts 2 through 6 were probably less than 0.20 just after mixing. It is
expected that Asphalts 2 through 6 will still be in serviceable condition for
three more years and thus will have at least 10 years' service life before
failure.
Therefore, based on this study, it is believed that a pavement will be
reasonably durable if the shear susceptibility at 77 F of the asphalt cement
after pugmill mixing is less than 0.20 and the pavement is compacted under
traffic during the first 18 to 24 months to the extent that it will have no
more than 5 percent air voids. Shear-susceptibility requirements for TFO
residue can be substituted in place of the ductility test since a good correla-
tion between these two properties was found by Welborn et al [4].
Temperature Susceptibility
Temperature susceptibility has been considered as one of the parameters
specifying the rheological behavior of paving asphalts [12]. Many re-
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KANDHAL ET AL ON PAVEMENTS IN PENNSYLVANIA 77
Conclusions
Based upon the rheological properties of the six asphalts studied and the
preceding discussions, the following conclusions are drawn:
Acknowledgments
The authors wish to express their appreciation to David Streby for con-
ducting all the microviscosity tests, to Richard Basso and June Viozzi for
assistance in compiling the data, and to Edward Macko for preparing the
illustrations. Cooperation of W. S. Myers and I. L. Myers in the per-
formance evaluation of the test pavements is also appreciated.
References
[/] Sandvig, L. D. and Kofalt, J. A., Proceedings, Association of Asphalt Paving Tech-
nologists, Vol. 37, 1968, p. 602.
[2] Gzemski, F. C , Fundamental Viscosity of Bituminous Materials, ASTM STP 328,
American Society Testing and Materials, 1962, p. 80-94.
[3] Hveem, F. N., Zube, E., and Skog, J., Proceedings, Association of Asphalt Paving
Technologists, Vol. 32, 1963, p. 271.
[4] Welborn, J. Y., Oglio, E. R., and Zenewitz, J. A., Proceedings, Association of Asphalt
Paving Technologists, Vol. 35, 1966, p. 46.
[5] Skog, John, Proceedings, Association of Asphalt Paving Technologists, Vol. 36, 1967,
p. 407.
[<5] Chipperfield, C. H., Duthie, J. L., and Girdler, R. B., Proceedings, Association of
Asphalt Paving Technologists, Vol. 39, 1970, p. 576.
[7] Kandhal, P. S., Sandvig, L. D., Koehler, W. C , and Wenger, M. E., "Asphalt
Viscosity Related Properties of In-Service Pavements in Pennsylvania," Bureau of
Materials, Testing & Research, Pennsylvania Department of Transportation, Research
Report, Feb. 1972.
[8] Olsen, R. E., Welborn, J. Y., and Vallerga, B. A., Proceedings, Association of Asphalt
Paving Technologists, Vol. 38, 1969, p. 317.
[9] Chipperfield, E. H. and Welch, R. R., Proceedings, Association of Asphalt Paving
Technologists, Vol. 36, 1967, p. 421.
[10] Traxler, R. N., Proceedings, Association of Asphalt Paving Technologists, Vol. 36,
1967, p. 546.
[11] Sisko, A. W. and Brunstrum, L. C , Proceedings, Association of Asphalt Paving
Technologists, Vol. 37, 1968, p. 467.
[12] Dobson, G. R., Proceedings, Association of Asphalt Paving Technologists, Vol. 38,
1969, p. 123.
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R. J. Schmidt^
Laboratory-Hardened AC Specimens
Four asphalts, listed in Table 1, were chosen for the preliminary study
of the influence of varying RMFO exposure conditions on the relative
hardening of asphalts. Asphalt A was made from Smackover crude oil.
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SCHMIDT O N LABORATORY MEASUREMENT O F DURABILITY 81
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82 VISCOSITY TESTING OF ASPHALT
This widely used asphalt is usually considered to be one of the most durable
asphalts known. Asphalts C and D are made from the same heavy Cali-
fornia Coastal crude oil. This asphalt has been widely and successfully used
not only in most of the Western states but in Alaska and the Pacific islands
as well. Asphalt B was made by vacuum reducing Asphalt D to a hard
grade and subsequently softening it to an 80 penetration with a heavy
lube oil extract. According to TFP tests, as well as RMFO tests conducted
by the CDH, Asphalt C hardened much more than Asphalt B; yet in the
Benicia, California, test road (see Table 4), Asphalt B hardened slightly
more than Asphalt C.
A number of AC specimens, each containing 5 percent (weight) of one of
these four experimental asphalts, were made from Cache Creek gravel
graded according to the curve shown in Fig. 1. This high-voids grading
(22 percent voids in mineral aggregate (VMA)) was used so that asphalt
hardening would proceed rapidly. These AC specimens were then exposed
in a 140 F (60 C) oven. At appropriate intervals, two specimens from each
group were removed and the asphalt recovered by the Abson extraction
procedure. In these extractions, 15 percent methanol was used along with
the benzene to effect more complete removal of the asphalt from the
simulated weathered specimens. Microviscosities on these residua, inter-
polated to 100 days' laboratory exposure, are shown next and also in Item 1
of Table 2.
Viscosities of Asphalts Recovered from
AC Specimens Exposed for 100 Days at 140 F (60 C)
Asphalt A B C D
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SCHMIDT O N LABORATORY MEASUREMENT OF DURABILITY 83
FIG. 1—Gradation of Cache Creek aggregate used in AC specimens at 140 F (60 CI-
Viscosity, megapoises6
Asphalt
Reference
Item Exposure B D
Control: AC specimens
1 100 days at 140 F (60 C) 27 95 95 125
RMFO conditions
2 Open, 24 h at 210 F (98.9 C) 14 36 194 191
3 Open, filled, 1 /2 h at 300 F (148.9 C), 48 h
at 180 F (82.2 C) 12 24 158 135
In RTF-C forced-air oven, 24 ft at 210 F (98.9 O
4 Open 14 30 394 406
5 0.041-in.—ID capillary 15 25 25 25
6 0.17-in.—ID capillary 15 23 26 25
7 0.041-in.—ID capillary (RTFO residue) 16 31 52 51
8 0.041-in.—ID capillary oxygenflushed(RTFO 18 32 56 55
residue)
In RTF-C forced-air oven, 48 ft at 210 F (98.9 C)
9 0.041-in.—ID capillary 31 73 77 76
" All viscosities are reported in megapoises and were determined at 77F (25 C) with a
uniform stress of 167 g/cm2.
* Results in all columns are the average of at least two exposures.
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84 VISCOSITY TESTING OF ASPHALT
Asphalt A B C D
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SCHMIDT ON LABORATORY MEASUREMENT OF DURABILITY 85
Asphalt A B C D
The ranking found is much the same as occurred in the original RMFO
exposure, that is, in Item 2. Apparently, neither lowering the exposure
temperature nor adding a realistic amount of mineral surface appears to
improve the agreement of the test exposure with the core exposure shown
in Item 1.
Asphalt A B C D
Asphalts A and B are seen to harden to almost the same level as in the
original RMFO in Item 2, Table 2. Asphalts C and D harden more than
twice as much as before. The significant difference from the RMFO in
exposure condition is that the bottles revolve into the direct air blast of the
blower. This large air blast entering the bottles is supplementary to the air
delivered into the bottles from the air jet. Also just shown and in Item 4,
Table 3, are the weight losses measured in this modified exposure. Asphalts
A and B are shown to lose less than 2 percent weight; whereas Asphalts C
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86 VISCOSITY TESTING OF ASPHALT
Refer- Asphalt
Item Exposure A B C D
and D lose about 8 percent by weight. Asphalts B and D are nearly identical
in composition, except that in Asphalt B the light oil component was re-
moved and replaced with a heavy lube oil extract. Other experiments
demonstrated that the composition of the lube oil extract was not respon-
sible for the reduced hardening rate. In this additional experiment, the low-
volatility lube extract was replaced with a low-volatility oil fraction made
from Asphalt D. The hardening rate was almost identical to those shown
for Asphalt B just described. The conclusion evident from this experiment
is that the difference in apparent durability measured by the RMFO be-
tween Asphalts B and C is a consequence of a difference in volatility be-
tween the two asphalts.
A further possible conclusion is that in actual AC mixes the light oils
are lost to a considerably lesser extent than they are in the various acceler-
ated laboratory exposures. Apparently, in the AC mixes, those oil mole-
cules which vaporize must diffuse through long, narrow passages before
they escape into the atmosphere. Under these circumstances, most of the
vaporized oil is reabsorbed by the asphalt before it escapes. These findings
suggest that simulation of field hardening of asphalts will require a pro-
cedure that provides sufficient oxygen but which inhibits, at the same time,
escape of the light oils from the asphalts during exposure.
(with the air jet off), oxidation proceeds much as before, but the evapora-
tion is minimized. Listed next and in Item 5, Tables 2 and 3, are the results
of this exposure on these same four asphalts.
Asphalt A B C D
Asphalt A B C D
Asphalt A B C D
Also important are the results listed next and in Item 8 of Table 2. This
exposure is identical to the ones described above except that the bottle was
flushed with oxygen just before the capillaries were fitted into place. The
values shown below are essentially the same as those shown above. This
is further evidence that sufficient oxygen is present to provide for the
oxidation needs of the asphalt during exposure. The reaction does not
appear to be oxygen limited by the capillary tube.
Viscosities of RMF-C Residua (0.041-In.-ID Capillary) on RTFO
Exposure 85 Min at 325 F (162.8 C), Exposure at 210 F (98.9 C)
for 24 H, Oxygen Flushed
Asphalt A B C D
Asphalt A B C D
iooor
500-
100-
50-
\ft i i i i i i i i L_LJ i i ! I
10 50 100
Viscosity of R M F - C R e s i d u e , 77F ( 2 5 C ) ,
M e g a p o i s e s , 167 g / c m !
FIG. 2—Comparison of viscosities of RMF-C residua with asphalt residua recovered from
AC cores exposed 100 days at 140 F (60 C).
These same 2-W asphalts were exposed to the RMF-C exposure. The
viscosities of the hardened asphalts are compared in Fig. 3 with the life
of the various test sections to 10 percent cracking in this test project. A
slightly better correlation is obtained with the RMF-C than previously
was obtained with the RMFO exposure, that is, the correlation coefficient
increased from 0.8258 to 0.8961. Also, the standard error decreased from
32 to 23 percent.
The C D H reported [15,18] interim results of their recent field tests com-
paring a number of experimental asphalts with normally available asphalts.
Extracts of their data are shown as Table 4. All cores extracted were taken
from t h e outer wheel track of the traffic lane. In Fig. 4 are plotted t h e
viscosities at 0.05 s _ 1 (obtained by the C D H ) . These viscosities were o b -
tained on asphalts recovered from the last set of cores in each test project.
They are plotted on Fig. 4 versus the R M F - C viscosity (also calculated at
0.05 s _ 1 ). When examining this figure, one should keep in mind that, except
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SCHMIDT ON LABORATORY MEASUREMENT OF DURABILITY 91
Viscosity of
Pavement Recovered
Age Asphalt,
When 77 F (25 C),
CDH Cores 0.05 s _1
Identification Removed, Shear Rate,
Project Location and Type Number Supplier month megapoises
Martinez:
Control, 85/100 R-4219 0 3.5
22 23
48 224
Special R-4215 D 0 3.5
22 31
48 197
Los Altos:
Control, 85/100 R^1238 D 0 2.2
19 17
45 28
Special R-4236 D 10 2.3
19 20
45 28
Ludlow:
AC-12 R^1298 0 2.2
20 16
40 28
AC-12 R-4299 0 2.6
20 26
40 45
85/100 R-4300 0 4.3
20 41
40 60
Control, 85/100 R^l301 0 3.5
21 36
40 65
Special R-4305 0 4.6
19 26
38 41
Special R-4306 0 2.3
18 15
35 31
Olivehurst:
Control, 85/100 R-4331 0 6.6
15 24
33 25
Special R-4329 0 6.6
15 16
33 30
Special R-4330 0 5.7
15 15
33 30
(Continued)
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92 VISCOSITY TESTING OF ASPHALT
TABLE A—Continued.
Viscosity of
Pavement Recovered
Age Asphalt,
When 77 F (25 C),
CDH Cores 0.05 s"1
Identification Removed, Shear Rate,
Project Location and Type Number Supplier month megapoises
Blythe:
Control, 200/300 R-4471 H 8 1.74
25 4.78
Special R-4433 H 6 6.1
24 29
Willits:
Special, 5.5 kilopoises R-4005 D 0 2.8
22 4.9
62 6.6
Special, 4.5 kilopoises R-4006 D 0 2.6
22 3.8
62 5.7
Special, 3.5 kilopoises R-4007 D 0 2.1
22 3.2
62 6.4
Control, 85/100 R-4008 G 0 3.6
22 7.2
62 11.2
Folsom:
Control 85/100 R-4110 or C 0 3.4
(Asphalt C in Table 1) R-4111 29 17
52 21
Special R-4099- D 0 4.2
R-4102 29 23
52 25
Benicia:
Control 85/100 R-4159 B 0 4.6
(Asphalt C in Table 1) 30 20
57 26
Special R-4158 D 0 4.9
(Asphalt B in Table 1) 30 27
57 36
for the slope, only the results from any one test road should be considered
at a time because each set of data is obtained from different pavements
existing at widely separate locations. The general relationship appears to
be quite good considering the difficulties inherent in obtaining representa-
tive field samples.
When the data were fitted with the regression model, the slope for In
(recovered viscosity) versus In (viscosity RMF-C) was found to be 0.611
± 0.089. The multiple correlation coefficient for the overall regression was
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SCHMIDT ON LABORATORY MEASUREMENT OF DURABILITY 93
Period H.
Period I
10 100 1000
Viscosity at 77F, 167 g / c m z , Megapoise
1000
Martinez
100
o u
Olivehurst
CD Legend of
10 Projects
o Martinez
x Ludlow
+ Olivehurst
7 Los Altos
o Benicia
o Blythe
• Willits
a Folsom
uL _i_
1 10 100
V i s c o s i t y at 77F (25C) Megapoises, 0.05 S e c . - 1
RMF-C Exposure
48 Hr at 210F (98.9C)
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94 VISCOSITY TESTING OF ASPHALT
0.98547. The correlation coefficient for the viscosity slope alone was found
to be 0.8790, which is an excellent correlation considering that several test
projects are included. The percentage error in predicting the recovered
viscosity from the RMF-C viscosity is approximately 21 percent.
The slope of 0.611 can be used as follows: If two asphalts have an
RMF-C viscosity ratio of 10:1, then after field exposure they would be ex-
pected to have a (recovered) viscosity ratio of 1 0 0 6 u : l = 4.09:1.
A more complete description of the multiple-regression analysis is given
in Appendix II.
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SCHMIDT ON LABORATORY MEASUREMENT OF DURABILITY 95
APPENDIX I
Rolling Microfilm Circulating Oven (RMF-C) Durability Test
1. Weigh 0.500 g of the asphalt into a 150-ml beaker using an analytical balance.
Dissolve the sample with approximately 10 g of benzene (reagent grade). Filter the
dissolved sample through a 10 to 15 ^m sintered glass filter directly into an RTF
sample bottle. Use a small pressure bulb to force solution through filter. Rinse the
beaker and filter clean with additional benzene. The dissolved, filtered asphalt is
now in the RTF bottle dissolved in approximately 15 to 20 g of benzene.
2. Place the RMF-C bottle (from this point forward, the RTF bottle containing
benzene and 0.5-g sample is referred to as an RMF-C bottle) into the RTF-C oven
[13]. (See Fig. 6.) The oven was previously set at 210 F (98.9 C). A210F(98.9C)
thermometer, similar to a 275 F (135 C) ASTM C-13 thermometer,4 is hung from the
center of the oven 1 in. from the side. Turn on vacuum to top vents in oven. (See
Fig. 6.) Turn the power to the oven off when adding the benzene-diluted samples.
Rotate for 15 min to evaporate the benzene; turn oven power "on," and run
evaporation cycle an additional 15 min with heat to achieve a positive benzene
evaporation. Without turning power off, remove bottles (in pairs), and insert
aluminum-foil-covered cork stoppers through which extend 2-in. long, 0.041 in.
inside diameter glass tubes. Turn power on and run for 48 h. The 0.5-g residue gives
a film thickness on the inside of the RMF bottle of approximately 20 ^m. The
oven should be equipped with the electronic proportional controller specified in the
RTF-C procedure, CDH Test Method 346-E.
3. At the conclusion of the 48-h RMF-C exposure, remove the bottle and allow
to cool (about 10 min). Scrape out all residue (by means of a razor blade attached
to a handle) from the wall (ignore the asphalt on the ends), and place in one of the
wells of a porcelain spot plate (Coors Size 00, Van Waters and Rogers Catalog
No. 53636) using a small spatula to clean residue from scraper. Within 30 min,
heat the spot plate on a steam or hot plate until the asphalt is fluid [approximately
250 F (121.1 C)] and mix well with the spatula.
4
These thermometers can be ordered from the Brooklyn Thermometer Company.
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96 VISCOSITY TESTING OF ASPHALT
4. Make up microviscosity plates as soon as the asphalt is fluid. Use metal plates
supplied by Hallikainen or Cannon. We have incorporated several new pro-
cedures in the preparation of microviscosity plates. They include:
(a) Use numbered paired plates— measure the thickness at each end of the pair
set together without shims over the central part with a metric micrometer capable
of measuring to 1 ^m.
(b) Prepare a duplicate set of plates from the residuum in the spot plate.
(c) Dab small amounts of sample with the same spatula used above onto the
metal test surfaces on both the top and bottom microviscosity plates. The plates
should be warm so the sample can flow and wet the entire test surface. Do not
touch the sample or plate with your fingers!
(d) Move the coated plates to a flat, cool surface. Position shims, invert, and
locate top metal plate. (See Sketch A in Fig. 5.)
(e) Place a spacer over top metal plate that clears the tops of the side spacers.
(A glass microviscosity plate works fine.)
(/) Transfer entire assembly on a flat surface such as J/g-in.-thick, 3-in. by 6-in.
aluminum plate to 275 F (135 C) oven. Leave in oven for 15 min; then place a
500-g weight, which has been preheated in the oven, on top of the spacer, and
leave for another 15 min. (See Sketch B, Fig. 5.)
(g) Remove assembly. Replace hot 500-g weight with a cold weight. Place
assembly on a flat metal surface, check shim drag to be sure of seating, and allow
to cool in the air for 1 h.
(A) As soon as the plates have cooled to room temperature, recheck shim drag
by sliding them back and forth. If the shims move freely with no drag, the plates
were not properly seated against the shims. If this is the case, prepare another plate
immediately. After the plates have stood for 1 h in air (with the weight still in
place), remove the weight and spacer and measure the thickness of the plates (at
each end) containing the shims and sample with the metric micrometer. Subtract
the thickness at each end from the corresponding thickness of the bare plates. If
the difference is more than a few microns from the shim thickness, prepare another
plate immediately. If the thickness is close, place the plates and shims in the 77 F
(25 C) water bath. The asphalt film thickness used in calculating the viscosity is the
difference between the measurements taken at Step (a) and Step (h). Do not assume
thickness is equal to shim thickness.
5. After a period of 5 min in the water bath, remove the shims, place the plates
in the microviscometer, and proceed with the measurement as follows:
(a) Apply a load of 1000 g. Allow a movement of exactly four large divisions (high
speed) on the Varian recorder. This represents approximately 0.20-mm movement
on the plates. By using the same movement on each sample, a consistent shear
history on the sample is established.
(b) Remove 1000-g weight. Apply a 200-g weight. Allow the measurement to
proceed until a steady rate of shear is obtained—usually at least two large divisions
across the chart. If the slope with the 1000-g load was >25 deg, use the slow chart
speed with the 200-g loading.
(c) Calculate viscosities at the two load levels (1000 g and 200 g) by using the
angle of the recorded line and the average thickness as measured by the difference
between the bare plates and the plates containing the specimen. If the viscosities on
duplicate plates differ by more than 10 percent, prepare another duplicate set of
plates from the same residuum in the spot plate and repeat the viscosity measure-
ment.
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SCHMIDT ON LABORATORY MEASUREMENT OF DURABILITY 97
SAMPLE
METAL
MICROVISCOSITY
SIDE SPACER PLATES
AND SHIM
TOP SPACER
SAMPLE
METAL
SIDE SPACER MICROVISCOSITY
AND SHIM PLATES
APPENDIX II
Description of Fitting Procedure for RMF-C Viscosity Versus
Recovered Viscosity at Several Locations
The data for the several sites were fitted with the following equation:
y = In (recovered viscosity) = aL + b • In (RMF-C viscosity)
where QL is an initial constant (level effect) fitted for each site, and b is a common
slope fitted across all the data.
The fitting was done with a standard least-squares regression program on an
electronic computer, with the aL values being obtained as the coefficients of a group
of variables (one for each test site) having the values 1 or 0, depending on whether
or not theyth data point came from that site. Thus, .y, = aiXJ + a^Xij + atX3j- • •
+ a»Xtj + b In (RMF-C viscosity), with XL, = 1 if y, is from site L; all other
Xa = 0 for this./'.
The results obtained in the regression analysis are summarized next:
site ah e>Ll
References
[1] Lewis, R. H. and Welborn, J. Y., Proceedings, Association of Asphalt Paving Tech-
• nologists, Vol. 12, 1940, p. 14.
[2] Schmidt, R. J. and Santucci, L. E., Proceedings, Association of Asphalt Paving
Technologists, Vol. 38, 1969, p. 39.
[3] Lewis, R. H. and Welborn, J. Y„ Public Roads. Vol. 22, No. 2, 1941.
[4] Lewis, R. H. and Halstead, W. J., Public Roads, Vol. 24, No. 8, 1946.
[5] Pauls, J. T. and Welborn, J. Y., Proceedings. Association of Asphalt Paving Tech-
nologists, Vol. 21, 1952, p. 48.
[<5] Hveem, F. N., Zube, Ernest, and Skog, John, Proceedings, Association of Asphalt
Paving Technologists, Vol. 32, 1963, p. 271.
[7] Skog, John, Proceedings, Association of Asphalt Paving Technologists, Vol. 36, 1967,
p. 387.
[8] Hveem, F. N., Zube, E., and Skog, J., Road and Paving Materials, ASTM STP 277,
American Society for Testing and Materials, 1959.
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SCHMIDT ON LABORATORY MEASUREMENT OF DURABILITY 99
[9] Santucci, L. E. and Schmidt, R. J., Grading of Paving Asphalts by Viscosity at 140 F
Versus Penetration at 77 F, ASTM STP 424, American Society for Testing and
Materials, 1967.
[70] Santucci, L. E. and Schmidt, R. J., Highway Research Board Bulletin, No. 333, 1962,
pp. 1-9.
[11] Schmidt, R. J., Painter, L. J., Skog, J. B., and Puzinauskas, V. P., Proceedings, Asso-
ciation of Asphalt Paving Technologists, Vol. 37, 1968, p. 476.
[12] Santucci, L. E. and Schmidt, R. J., Proceedings, Association of Asphalt Paving
Technologists, Vol. 38, 1969, p. 65.
[13] Schmidt, R. J., Viscosity Testing of Asphalt and Experience with Viscosity Graded
Specifications, ASTM, STP 532, American Society for Testing and Materials, 1973,
pp. 52-63.
[14] Griffin, R. L., Miles, T. K., and Penther, C. J., Proceedings, Association of Asphalt
Paving Technologists, Vol. 24, 1955, p. 31.
[15] Simpson, W. C , Griffin, R. L., and Miles, T. K., Road and Paving Materials, ASTM
STP 277, American Society for Testing and Materials, 1959.
[16] Beaton, J. L. and Sherman, G. B., Minutes of 9th Pacific Coast Users and Producers
Conference, 1971.
[17] Skog, J., Road and Paving Materials, ASTM STP 277, American Society for Testing
and Materials, 1959.
[18] Kemp, G. R. and Johnson, M. H., Viscosity Testing of Asphalt and Experience with
Viscosity Graded Specifications. ASTM STP 532, American Society for Testing and
Materials, 1973, pp. 100-121.
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G. R. Kemp^
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102 VISCOSITY TESTING OF ASPHALT
Starting in 1964 with the Willits test section, a series of test sections were
placed in various climatic areas of the state. In these test sections, special
asphalts, which were manufactured to meet the proposed tentative asphalt
specifications, were placed and evaluated, along with a selected portion
of the job asphalt as a control. The test sections were located, besides the
Willits [2] location, at or near Folsom [3], Benicia [4], Martinez [5], Los
Altos [6], Ludlow [7], Olivehurst [8], and Blythe [9], California. Table 2
TABLE 2—Durability test sections.
Structural Section
Date Thickness and Type
Location Placed AsphaWs
Contract (% Climatic Seal, Surface Base
Road asphalt)* Area Type® (ID) ft. (special), ft (type), ft
1
S = special.
C « control.
TS = tentative specification.
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 103
° TS = tentative specification.
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104 VISCOSITY TESTING OF ASPHALT
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 105
Heithaus Value P
The Heithaus test [16] provides a method for studying the internal phase
relationship of an asphalt. The technique provides a measure of the pep-
tizing power of the malthenes Po, and the peptizability of the asphaltenes
Pa. When the two factors are combined the state of peptization P [P =
Po/(l — Pa)] can be determined. The higher the value of P, the more
stable the internal phase of the asphalt system.
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106 VISCOSITY TESTING OF ASPHALT
rotating the bottle in the RTF oven for a specified period with the power
off till the benzene is evaporated. After complete evaporation, the bottle
is stoppered except for a small capillary tube through the stopper, and the
weathering period is then conducted for 48 h in the RTF oven at 210 F
(99 C) at the specified 15 rpm with no air being used. The weathered residue
is then removed and tested. The concept of the weathering is that there is
hardening through oxidation but that the evaporation present is contained
and resolvated into the system as is theorized to happen to the asphalt in
the enclosed void spaces in the pavement.
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 107
>>
Sand Mix
Sand Mix
'late
+ £
void;
Briquette 90 i
Field Density
0001
Field ^ 53
00 h
Asphalt Results o. PS
•O M
Test Type0 — •8« S . « "1 3 c
J". S3^ K "^
o
201 F
140 F
Exten
WeatI
1 fc
Percei
Chevi
Ottaw
Origii
Heith
a+
RTF,
Section (source 30 50
Road grade) month month
o 3 as 5
1
Willits S(D)5.5 5.3 6.1 15 13 13 20 1.25 5.2 6.0 18
01-Men S(D)4.5 4.2 5.0 14 13 11 18 0.95 5.1 6.3 13
S(D)3.5 3.6 5.2 12 12 9 15 1.22 6.7 6.0 10
C(G)85/100 7.9 9.8 24 29 44 110 1.85 6.5 3.3 36
Folsom S(D)TS 23 25 21 26 37 108 1.98 7.0 3.5 29
03-Sac, C(C)85/10O 17 21 26 45 23 52 1.24 7.8 3.3 21
ED-50
Benicia S(D)TS 27 34 23 16 32 103 28 1.78 8.2 3.5 45
10-Sol-21 C(B)85/100 20 22 32 91 50 192 31 1.90 8.3 3.9 44
Martinez S(D)TS 72 197 22 29 43 100 1.83 10.3 3.5 37
04-CC-4 C(B)85/100 59 224 21 41 24 71 1.63 8.7 4.2 45
Los Altos S(D)TS 25 29 23 33 32 80 1.80 6.4 3.6 35
04-SC1-280 C(D)85/100 25 29 26 83 22 89 1.70 4.8 4.1 41
Ludlow S(E)AC12 22 13 12 11 28 17 1.50 4.0 5.8 9
08-SBd-40 S(A)AC12 36 25 27 27 100 26 1.70 5.1 3.8 23
(A)85/100 52 27 31 39 105 28 1.80 6.4 3.5 30
C(F)85/100 50 27 74 27 80 35 1.59 5.4 3.8 40
S(A)TS 36 30 25 52 135 30 1.50 6.8 3.6 39
S(A)LV TS 24 16 17 26 74 19 1.40 5.8 3.6 20
Olive- S(C)TS 27 27 34 32 76 31 1.37 7.0 3.4 28
hurst S(A)TS 26 28 24 50 125 35 1.47 6.6 3.5 27
03-Yub-70 C(C)85/100 25 25 34 28 78 31 1.22 9.8 3.5 35
Blythe S(H)TS 36 28 31 17 44 1.45 7.2 4.3 27
ll-Riv-10 C(H)200/300 5.4 2.5 6 3.8 12 1.50 4.4 4.4 2
C(M)85/100 135 28 44 48 132 6.9
• S = special asphalts.
C = control asphalts.
TS = Calif. Tentative Specification (4000 to 6000 poises at 140 F after RTF).
The special asphalts used in the Folsom, Benicia, Martinez, and Los Altos
test sections come from one refinery. All of these sections were laid within
18 months of each other as can be seen in Table 2. Figures 2 through 5
show how the special asphalts compared with the control asphalts. As can
be seen in Fig. 6, which compares the special asphalts from the different
sections, they are each weathering similarly except for the Martinez test
section which had the largest percentage of initial voids.
In the Ludlow test section, as shown in Fig. 7, special asphalts designed
to meet The Asphalt Institute AC 12 grading were compared with special
asphalts meeting the 1966 California tentative specification. In addition to
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108 VISCOSITY TESTING OF ASPHAIT
TABLE 5—Asphalt durability test sections—Recovered asphalt test results (surface course).
Tests
Microviscosity
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 109
TABLE 5—Continued.
Tests
Microviscosity
* TS = tentative specification,
VFS = very fast setting.
FS = fast setting.
MS = medium setting.
the regular 85/100 contract control asphalt, 85/100 asphalt from another
source meeting the standard specifications was placed as an additional test
section. As seen in Fig. 7, the various asphalts are weathering individually
somewhat differently, but the whole group of asphalts shows that the con-
ditions evident in this test section are affecting the group similarly.
In the Olivehurst and Blythe test sections, two additional sources of
special tentative-specification asphalt were employed. The Olivehurst sec-
tion compares two sources of tentative-specification asphalt, one of which
is the same as used in the Ludlow test section; while the special asphalt in
the Blythe test section is represented by yet another source. Figures 8 and 9
show how the different asphalts compare with each other in the Olivehurst
and Blythe test sections. The data for these three sections are not as con-
clusive, as the weathering period has been only about 30 months. This is
evident in the Blythe test section, as shown in Fig. 9, by the wide separation
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1 10 VISCOSITY TESTING OF ASPHALT
40
SURFACE COURSE
30 —> SPECIAL (5.5) VERY FAST SET ASPHALT
—• SPECIAL ( 4 5) FAST SET ASPHALT
20- --o SPECIAL (3.5) MEDIUM SET ASPHALT
—• CONTROL 85/100 ASPHALT
2.'"
at in
£ in
— o
>- o
tuT
tn •
o £"
10 20 30 40 50
MONTHS FIELD WEATHERING
between the weathering curves. Partly this can be attributed to the control
asphalt being a 200/300 material, but the special 85/100 control asphalt
is just as different from the tentative-specification asphalt as the 200/300
asphalt. Further weathering in this area should clarify the weathering
picture.
An analysis of all of the test sections shows that in each the control
asphalt is weathering at about the same rate as the special asphalt. Excep-
tions are the Willits and Blythe test sections where the control 85/100
10 20 30 40 50 60
MONTHS FIELD WEATHERING
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 111
0 10 20 30 40 50 60
MONTHS FIELD WEATHERING
10 20 30 40 50 60 70
MONTHS FIELD WEATHERING
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112 VISCOSITY TESTING OF ASPHALT
SURFACE COURSE
10 20 30 40 50 60 70
MONTHS FIELD WEATHERING
test sections and has similar climatic conditions, the weathering has been
dramatically increased. The asphalts in the Martinez section have penetra-
tions of 10 and 12 for the control and special asphalts, where in the other
test sections the asphalts average penetrations of 22 and 23, respectively,
for the special and control asphalts for about the same weathering period.
Table 6 shows the results of visual observations for cracks and deflection
measurements. In the Martinez section we see that the road has extensive
block and chicken-wire cracking in both the special and control sections.
None of the other test sections exhibit any cracking at this time. In all the
i i i l S ;
100
80 /
60 /
"4>
£ QL 40 X _
_
a> v>
E m 20
— O
>- o
O ^ 10 - yy
/y
/^~ ' 1
O 1^- e Jy
_
> 6 /ft
7/fl ° o FOLSOM TEST SECTION -
• • BENICIA TEST SECTION
4 *7
I' " « MARTINEZ TEST SECTION -
/i a -o LOS ALTOS TEST SECTION
0
{ I > I ,
10 20 30 40 50 60 70
MONTHS FIELD WEATHERING
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KEM? ON DURABILITY TESTS AND FIELD HARDENING 113
Deflection Data
Visual Inspection
Wheel Track Data
Test
Section Asphalt Inner, Outer, Latest Cracks, Latest
Road (source) Grade0 in. in. Date etc. Date
Willits special (D) 5.5 VFS 0.006 0.005 4 69 some reflection cracking 7 71
Ol-Men-101 special (D) 4.5 FS 0.007 0.007 4 69 some reflection cracking 7 71
special (D) 3.5 MS 0.008 0.006 4 69 some reflection cracking 7 71
control (G) 85/100 0.008 0.006 4 69 some reflection cracking 7 71
Folsom special (D) TS 0.005 0.004 4 71 no cracking 5 71
03-Sac, ED-50 control (C) 85/100 0.004 0.004 4 71 no cracking 5 71
Benicia special (D) TS 0.013 0.013 2 71 no cracking 3 71
lO-Sol-21,680 control (B) 85/100 0.011 0.011 2 71 no cracking 3 71
Martinez special (D) TS 0.013 0.012 4 71 block and alligator 3 71
04-CC-4 control (B) 85/100 0.012 0.011 4 71 cracking both asphalts 3 71
Los Altos special (D) TS 0.001 0.001 3 71 no cracking ' 5 71
04-SC1-280 control (D) 85/100 0.001 0.001 3 71 no cracking 5 71
Ludlow special (E) AC-12 0.003 0.003 3 69 no cracking 1 71
08-SBd-40 special (A) AC-12 0.0014 0.0013 3 69 no cracking 1 71
(A) 85/100 0.0014 0.0013 3 69 no cracking 1 71
control (F) 85/100 0.0014 0.0013 3 69 no cracking 1 71
special (A) TS 0.001 0.0005 3 69 no cracking 1 71
special LV (A) TS 0.0015 0.0017 3 69 no cracking 1 71
Olivehurst special (C) TS 0.012 3 70 no cracking 5 71
03-Yub-70 special (A) TS 0.020 3 70 no cracking 5 71
control (C) 85/100 0.019 3 70 no cracking 5 71
Blythe special (H) TS no cracking 1 71
ll-Riv-10 control (H) 200/300 no cracking (extensive 1 71
bleeding)
(M) 85/100 no cracking 1 71
° TS = tentative specification.
VFS = very fast setting.
FS = fast setting.
MS = medium setting.
100 I I I i
80 '
60
,- ^ ^
.- ^—*G'
•
//
- •''•'/
.'^^^^
>'//
E in
—O -- / / / -
-!/'./ -° SPECIAL AC-12 ASPHALT "E"
10 20 30 40 50 60
MONTHS FIELD WEATHERING
FIG. 7—Ludlow test section, Road 08-SBd-40, R 28.4/R 42.1 (surface course).
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1 14 VISCOSITY TESTING OF ASPHALT
SURFACE COURSE
20
0 10 20 30 40 50 60 70
MONTHS FIELD WEATHERING
test sections the deflection values are low, even in the Martinez test section.
This indicates that the structural sections were well designed as there is no
instability, although there is extensive bleeding in various portions of the
control 200/300 asphalt of the Blythe test section. No bleeding is evident
in the tentative specification asphalt section or the special 85/100 asphalt
section, even though they used the same mix design and asphalt content as
the 200/300 asphalt. No bleeding is evident in any of the other test sections.
i i i i
100 ?
80 — t
2 - / -
10 20 30 40 50 60
MONTHS FIELD WEATHERING
FIG. 9—Blythe test section, Road ll-Riv-10, R 133.51R 149.5 (surface course).
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 1 15
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116 VISCOSITY TESTING OF ASPHALT
NOTE—Y = Aebx used for Heithaus P, percent voids, and Rostler ratio.
Y = AXh used in all other correlations.
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 1 17
Findings To Date
1. All of the tentative specification asphalts graded on the basis of RTFO
residue viscosity had excellent "setting" properties regardless of supplier.
2. The superior qualities of the experimental asphalts used in the Willits
test section appear to be a combination of moderately low voids and good
asphalt durability properties.
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118 VISCOSITY TESTING OF ASPHALT
s o I O A -ivNiaiao iN30«3d
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iN3ioud300 Nouvn3ayoo
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 1 19
| SOIOA 1VNIOIMO %
1 „d„ SnVHXI3H
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120 VISCOSITY TESTING OF ASPHALT
3. In most of the test sections it appears that the special asphalts did
not weather significantly different than the control asphalts and that the
test-section conditions also dictated the weathering rates of the asphalts
involved.
4. The original void content of the pavement appears to be a definite
factor in long-term asphalt durability. The evidence was most indicative
at the 50 months weathering correlation.
5. All of the test sections were in good physical condition at 30+
months except for the Martinez test section, which is exhibiting extensive
block cracking in both the special and control-asphalt areas, and the con-
trol 200/300 asphalt portion of the Blythe project which is exhibiting
"bleeding."
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KEMP ON DURABILITY TESTS AND FIELD HARDENING 121
Conclusions
1. Grading asphalt on the basis of viscosity at 140 F (60 C) after a treat-
ment test that simulates field mixing (rolling thin-film test or thin film test)
will produce mixes that have better uniformity in "setting" during rolling.
This uniformity was consistent regardless of manufacturer.
2. Initial pavement air voids is an important factor in controlling early
asphalt hardening. Pavement air voids should be as low as possible without
sacrificing stability or causing pavement "bleeding."
3. More field weathering time is needed before final conclusions can be
made on the reliability of the various laboratory test methods for predict-
ing asphalt durability.
Acknowledgments
The author wishes to acknowledge the work of J. B. Skog in starting this
study to improve asphalt specifications. Acknowledgment is given C. A.
Frazier for supervising the statistical treatment. Special acknowledgment
is given N. H. Predoehl for his help in all phases of the work. Acknowledg-
ment is also given to the asphalt producers for their cooperation in furnish-
ing the tentative specification asphalts.
This work was done in cooperation with the U. S. Department of Trans-
portation, Federal Highway Administration. The opinions, findings, and
conclusions expressed in this report are those of the author and not neces-
sarily those of the Federal Highway Administration.
G. B. Sherman is the principal investigator, and M. H. Johnson and G. R.
Kemp are the co-investigators of the research project from which the infor-
mation contained in this report was obtained.
References
[]] Hveem, F. N., Zube, E., and Skog, J. B., Proceedings, Association of Asphalt Paving
Technologists, Appendix D, San Francisco, 1963, p. 318.
[2] Zube, E. and Skog, J. B., "Experimental Asphalt Test Section, Road 01-Men-l-E,
Wits.," Research Report 643185, State of California, Department of Public Works,
Division of Highways, Materials and Research Department, Feb. 1967.
[3] Zube, E., Skog, J. B., and Kemp, G., "Experimental Asphalt Test Section, Road
03-Sac, ED-50," Research Report 643229, State of California, Department of Public
Works, Division of Highways, Materials and Research Department, Aug. 1966.
[4] Zube, E., Skog, J. B., and Kemp, G., "Experimental Asphalt Test Section, Road
lO-Sol-21, 680," Research Report 643229, State of California, Department of Public
Works, Division of Highways, Materials and Research Department, Aug. 1966.
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122 VISCOSITY TESTING OF ASPHALT
[5] Zube, E., Skog, J. B., and Kemp, G., "Experimental Asphalt Test Section, Road
04-CC-4-4.4/9.8," Research Report 643229, State of California, Department of Public
Works, Division of Highways, Materials and Research Department, Sept. 1967.
[6] Zube, E., Skog, J. B., and Kemp, G., "Experimental Asphalt Test Section, Road
04-SC1-280-11.5/18.9," Research Report 643229, State of California, Department of
Public Works, Division of Highways, Materials and Research Department, Aug. 1967.
[7] Zube, E. and Skog, J. B., "Experimental Asphalt Test Section, Road 08-SBd-
R28.4/R42.1," Research Report 633134, State of California, Department of Public
Works, Division of Highways, Materials and Research Department, June 1968.
[8] Zube, E., Skog, J. B., and Kemp, G., "Experimental Asphalt Test Section, Road
03-Yub-70-0.1/R8.9," Research Report 633134, State of California, Department of
Public Works, Division of Highways, Materials and Research Department, March
1968.
[9] Sherman, G. B., Kemp, G. R., and Predoehl, N. H., "Experimental Asphalt Dura-
bility Test Section, Road ll-Riv-10-R133.5/R149.5," Research Report 633134, State
of California, Department of Public Works, Division of Highways, Materials and
Research Department, Sept. 1971.
[10] Skog, J. B., "Setting and Durability Studies of Paving Grade Asphalts," Proceedings,
Association of Asphalt Paving Technologists, Denver, 1967.
[II] Skog, J. B. and Sherman, G. B., "Viscosity Grading for Asphalt Cements," Research
Report 633134, State of California, Department of Public Works, Division of High-
ways, Materials and Research Department, presented at 50th Annual Meeting of the
Highway Research Board, Jan. 1971.
[12] Skog, J. B., "The Operation, Control, and Application of the Infrared Weathering
Machine—California Design," Road and Paving Materials, ASTM STP 212, American
Society for Testing and Materials, 1957.
[13] Proposed Method of Test for: Aging Index of Bituminous Materials, 1964 Annual
Book of ASTM Standards, American Society for Testing and Materials, p. 665.
[14] Materials Manual, California Test Method 346-D, State of California, Department of
Public Works, Division of Highways.
[75] Rostler, F . S. and White, R. M., "Composition and Changes in Composition of
Highway Asphalts, 85-100 Penetration Grade," Proceedings, Association of Asphalt
Paving Technologists, New Orleans, 1962.
[16] Heithaus. J. J., "Measurement and Significance of Asphaltene Peptization," Sym-
posium on Fundamental Nature of Asphalt, sponsored by Division of Petroleum
Chemistry of the American Chemical Society, New York, Vol. 5, No. 4-A, Sept. 1960.
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