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SYMPOSIUM ON
FUNDAMENTAL VISCOSITY
OF BITUMINOUS MATERIALS

Presented at the

SIXTY-FIFTH ANNUAL MEETING

AMERICAN SOCIETY FOR TESTING AND MATERIALS


New York, N. Y., June 28, 1962

Reg. U. S. Pat. Off.

ASTM Special Technical Publication No. 328

Price S4.25; to Members $3.40

Published by the
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia 3, Pa.

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© BY AMERICAN SOCIETY FOR TESTING AND MATERIALS 1963
Library of Congress Catalog Card Number: 63-12704

Printed in Baltimore, Md.


April, 1963

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FOREWORD

This Symposium on Fundamental Viscosity of Bituminous Materials re-


views the relation of absolute viscosity of bituminous materials to the prob-
lems associated with the construction and performance of bituminous high-
ways. ASTM Committee D-4 on Road and Paving Materials sponsored this
symposium, which was held June 28, 1962, at the Sixty-fifth Annual Meet-
ing of the Society in New York City. Mr. W. J. Halstead, Bureau of Public
Roads, was Symposium Chairman and presided at the Technical Session.

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NOTE.—The Society is not responsible, as a body, for the statements
and opinions advanced in this publication.

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CONTENTS

PAGI
Introduction—W. J. Halstead 1
Fundamental Viscosity and How It Is Measured—D. F. Levy 3
Relation of Empirical Tests to Fundamental Viscosity of Asphalt Cement—J. M.
Griffith and V. P. Puzinauskas ' 20
Discussion 44
The Relation of Absolute Viscosity of Asphalt Binder to Stability of Asphalt Mixtures
—J. Y. Welborn, W. J. Halstead, and R. E. Olsen 48
Discussion 65
Application of Asphalt Viscosity to Paving Problems—R. L. Griffin, J. O. Izatt, and
J. A. Lettier 67
Viscoelastic Properties of Paving Asphalts—F. C. Gzemski 80
Summary—F. J. Benson 95

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STP328-EB/Apr. 1963

SYMPOSIUM ON FUNDAMENTAL VISCOSITY OF


BITUMINOUS MATERIALS

INTRODUCTION
BY W. J. HALSTEAD1

This symposium reviews existing be desirable to use fundamental units


knowledge and presents new information to measure viscosities of new materials
on the relation of absolute viscosity of and new processes where the industry
bituminous materials to the problems was not already accustomed to the use
associated with the construction and of empirical methods. The potential ad-
performance of bituminous highways. vantages of the use of such units in well
The papers deal with the definitions established fields were also discussed.
of fundamental viscosities, the instru- Three papers given at the 1937 sym-
mentation available for their measure- posium are of particular interest to the
ment, the relation between current em- bituminous technologist. A paper by
pirical measurements of consistency and R. N. Traxler entitled "The Flow Prop-
absolute units, the relation of absolute erties of Asphalts Measured in Absolute
viscosity to laboratory stability meas- Units" described a rotating cylinder
urements, the application of viscosity to device and a vacuum-operated capillary
practical problems in the specification tube viscometer that had been reported
and use of bituminous materials, the to the industry in 1935. This was the
significance of viscosity with respect to viscometer designed by Rhodes, Volk-
the more complex rheology of bitumi- mann, and Barker that is now known
nous materials, and the advantages of as the Koppers viscometer. Traxler also
substituting viscosity units for the pres- pointed out the limitations of the pene-
ent empirical units. tration test—its failure to correlate with
The idea of using absolute viscosity true viscosity and its varying shear rate.
units to measure the consistency of bi- A paper by Rhodes, Volkmann, and
tuminous materials is, of course, not Barker presented at the 1937 symposium
new. At the ASTM Annual Meeting in pointed out the large number of empiri-
1937, a similar symposium was spon- cal consistency tests then being used and
sored by Committee E-l on Methods of stressed the need for the replacement of
Testing. There had been earlier presen- such empirical instruments with instru-
tations in 1923. ments capable of measuring viscosity in
The 1937 symposium highlighted the absolute units. Although practical in-
advantages of using fundamental Theo- struments for absolute viscosity meas-
logical properties of materials. It was urements were then available, it was
emphasized at that time that it would recognized that an interim period would
be needed to permit a general deprecia-
1
Supervisory Chemist, Physical Research tion of the empirical equipment. This
Division, Bureau of Public Roads, Washington,
D.C; Chairman of Symposium Committee. paper, therefore, discussed the relation
1

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2 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

of each of the empirical measurements itations, does serve to differentiate


used in the tar industry with the abso- between grades of asphalts. Furol viscosi-
lute viscosity. ties run at the proper temperature ade-
The third paper, by J. C. Geniesse, quately control liquid grades of asphaltic
discussed viscosity measurements of pe- products; the Engler-viscosity for tars
troleum products and lubricants. His is equally adequate in its limited field.
conclusions stressed the need for, and The situation with respect to highway
the advantages of, adoption of funda- construction, however, is changing.
mental units of viscosity as a replace- Highways must now be built to accom-
ment for the empirical values. modate faster and more frequent traffic;
As is evident from the summaries of there is a demand to permit heavier
these papers, many of the principles loads; and the economic situation re-
being discussed in research papers at the quires that the highways last longer.
present time were clearly set forth at To accomplish these aims, more re-
least 25 years ago, but little practical search is needed. The fundamental
use has been made of the information. principles of pavement design and the
Why has progress been apparently so properties of the materials used must be
limited? determined more precisely. Engineers
One possible explanation is that during and bituminous technologists are realiz-
World War II, and the years immedi- ing that the empirical methods are in-
ately preceding it, fundamental research adequate, and measurements must be
on asphalt was almost completely elimi- made in fundamental units to establish
nated. Even though considerable prog- the desired relationships.
ress was made in the areas of paving The mutual concern of the ad hoc
equipment because of the immediate committee of the Highway Research
need for roads and airfields, there was no Board, The Asphalt Inst., the Bureau of
time to experiment with fundamental Public Roads, and the subcommittees
measurements of consistency. The em- of ASTM Committee D-4 on Road and
pirical tests were adequate to get the Paving Materials has resulted in a de-
job done. termined effort to promote the use of
This latter thought perhaps is the fundamental units for bituminous mate-
most important reason that progress has rials. In the past few years, considerable
been limited insofar as specification research has been concerned with such
limits based on fundamental viscosity units, proposals have been made for
units are concerned. The empirical units using fundamental units in specifica-
in the hands of experienced highway tions, the shear susceptibility of asphalts
engineers and bituminous technologists has been examined critically, and the
have been, and still are, generally ade- importance of viscosity and viscosity
quate for practical purposes. Within the changes in bituminous materials has
relatively limited geographical area of a been discussed. The present symposium
single highway department, the pene- summarizes the old and new information
tration test, despite its recognized lim- and charts the course of future action.

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STP328-EB/Apr. 1963

F U N D A M E N T A L VISCOSITY AND HOW I T IS M E A S U R E D

B Y D. F. LEVY 1

SYNOPSIS

This paper covers definitions of fundamental viscosity, absolute viscosity,


and kinematic viscosity. The various units and terminology used to measure
viscosity are defined. Other factors contributing to a better understanding of
the nature of viscosity are discussed, such as types of fluid flow, Reynolds
number, and initial and apparent viscosity. Several viscometers currently in
use in industry and research are covered briefly. The general range of appli-
cation, operation, and the normally expected precision of each type of
viscometer are discussed.

In recent years, asphalt technology has control and exposure of the end of the
been trying to lift asphalt testing and tube to the air.
use out of the realm of the arts to one of Terms such as fundamental, absolute
science and engineering. Most of the old or dynamic viscosity, kinematic vis-
specifications tell little about this con- cosity, poise, centipoise, stokes, and
struction material that is of actual stress, rate of shear, Newtonian and non-
importance to its ultimate application Newtonian flow, viscoelastic and plastic
and use. These specifications are, for the flow are in common use, but often are
most part, arbitrary physical properties, misunderstood. A clearer understanding
which are a means of identification but of these terms and their connection with
not a means of ensuring or measuring viscosity or the rheology of materials is
quality. necessary to the promotion of scientific
Viscosity is the one test that tells us and engineered quality of asphaltic
most about this complex end product of materials.
crude oil. For years, the value of this
DEFINITIONS
test has been clouded by the use of an
arbitrary method. The Saybolt method Fundamental is defined by Webster as
is an arbitrary measurement of the time pertaining to the foundation or basis;
of efflux for a fixed quantity of fluid to serving for the foundation; essential as a
flow through a fixed orifice. According to principle or law, as a fundamental truth.
Bingham (l),2 the only advantage of the Absolute is defined as being inde-
Saybolt method is its wide use in this pendent as far as possible of arbitrary
country. I t is relatively inaccurate and, standards, especially pertaining to or
in the case of viscous oils, time-con- derived in the simplest manner from,
suming. With volatile solvents, it cannot the fundamental units of length, mass,
be used at all, due to evaporation. Two and time.
sources of error are poor temperature Viscosity is defined as the resistance
1
offered by a fluid to the relative motion
Phillips Petroleum Co., Bartlesville, Okla. of its particles; internal friction.
2
The boldface numbers in parentheses refer
to the list of references appended to this paper. Then aosolute viscosity is the expression

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4 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

of the resistance that a fluid offers to the unit velocity in its own plane. The cgs
relative motion of its particles, measured unit of dynamic or absolute viscosity,
in fundamental units of length, mass, and Va, is the poise, which has the dimen-
time. Hence, a fundamental viscosity. sion grams per centimeter per second.
In 1867 Newton (2) defined the re- Kinematic viscosity of a Newtonian
sistance of a liquid to flow, due to "lack liquid is the quotient of the dynamic or
of slipperiness," by absolute viscosity divided by the density
Va/d, both at the same temperature.
F = VS
The cgs unit of kinematic viscosity,
F Vk , is the stoke, which has the dimension
=
•'•" 5 square centimeters per second.

where:
F = shear stress (force per unit area),
dynes per sq cm,
5 = rate of change in velocity with
distance from the wall (velocity
gradient, strain rate, rate of shear),
cm per sec per cm or sec - 1 , and • ~ . &

r\ = viscosity coefficient (now called FIG. 1.—Definition of Viscosity.


viscosity), dyne-sec per sq cm,
poise. The unit of absolute viscosity, the
poise, derives its name from Poiseuille,
P who in 1842 discovered the law governing
F = - and
A the flow of liquids through capillary
tubes. The unit centipoise is sometimes
dv
S = - used and is one-hundredth of the value
dr of the poise.
Then: The unit of measure for kinematic
viscosity, the stoke, derives its name from
P /dA-i
=
G. Stokes, who in the 1850's developed
" A \dr) formulas for velocities of falling bodies
where: through liquid media. The centistoke is
one-hundredth the value of the stoke.
v = velocity, cm per sec,
This unit is very commonly used in the
A = area of oil film, sq cm,
petroleum industry, primarily in lubri-
P = force, dynes, and
cating oil testing, but recently it is
r = distance between oil films, cm.
being used in cut-back asphalt viscosity
This classic definition of viscosity is
testing (5).
generally shown diagramatically as in
Fig. 1 (2). Fluid Flow:
ASTM Definitions (4); Fluid flow is generally classified into
Alsolute or dynamic viscosity of a two basic types, Newtonian and non-
Newtonian liquid is the tangential force Newtonian.
on unit area of either of two parallel Liquids which flow in accordance
planes at unit distance apart when the with Newton's law are known as New-
space is filled with liquid and one of the tonian liquids. Flow of this type is
planes moves relative to the other with known as viscous, streamline, laminar,

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LEVY ON DEFINITIONS AND MEASUREMENT O

or linear flow. The viscosity, or the ratio The viscosities of non-Newtonian ma-
of shearing stress to rate of shear, is terials must be expressed as a function
constant for Newtonian liquids flowing of the rate of shear, since the ratio of
under these conditions. However, as the shearing stress to rate of shear is not a
fluid flow is increased, the ratio of shear- constant. Examples of various types of
ing stress to rate of shear suddenly flow are shown in Fig. 2 as functions of
decreases at a critical point. This point stress and rate of shear. The Newtonian
marks the transition between viscous fluid will flow when acted upon by any
flow and turbulent flow (hydraulic flow) force, however small. The other types of
in which the liquid no longer behaves in flow shown in this figure are all non-
Newtonian fashion. In turbulent flow Newtonian. The plastic material does
the motion of the fluid is erratic. Rey- not flow until the applied shearing stress
nolds has shown that the critical veloc- exceeds a certain minimum value. This

SHEARING STRESS *~

FIG. 2.—Generalized Curves Showing Four Types of Flow.

ity separating viscous from turbulent yield value is indicated by an intercept


flow through a pipe depends upon the on the stress axis. When this value is
dimensionless function. exceeded, viscous or laminar flow takes
place (6). A pseudoplastic material ex-
PUP
hibits the property of flow readily, but
n
flows more readily when stirred or
where: sheared. A dilitant material shows in-
D = inside diameter, creased resistance to flow as it is agitated
U = velocity of the liquid, or sheared.
P = density of the liquid, and Asphaltic materials are generally non-
11 = viscosity of the liquid. Newtonian, but at temperatures above
The Reynolds number, as it is called, is approximately 140 F they behave like
low for viscous flow and high for turbu- Newtonian bodies. At lower tempera-
lent flow. This transition normally occurs tures and below a certain rate of shear,
at a Reynolds number of about 3000. they may also behave as Newtonian

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(0)

CUT OFF
SQUARE
a FLAME
POLISHED f.
®
IOJ0.2

.--UPPER
* FILLING
MARK

FRONT CAPACITY I ML
ELEVATION REQUIRED ON
SIZES 1-9 ONLY
(c) (d)

(a) Cannon-Fenske.
(b) Zeitfuchs cross-arm.
(c) Lantz-Zeitfuchs t y p e reverse flow.
(d) TJ-tube reverse flow, t y p e B S / I P / R F .
FIG. 3.—Capillary Viscometers for Opaque Liquids (from ASTM Method D 445 - 60).
6
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LEVY ON DEFINITIONS AND MEASUREMENT 7

bodies; for example, they have a vis- approached, because the heating effects
cosity that is independent of both rate caused by viscous flow prohibited meas-
of shear and shearing stress. urements much before the necessary rate
This viscosity, the highest one that of shear was attained.

STD. PYREX

23 MM O.D.

OVER ALL ASSEMBLED HEIGHT = APPROXIMATELY 306 MM

FIG. 4.—Vacuum Capillary Viscometer.

non-Newtonian liquids have, is called MEASUREMENT OF FUNDAMENTAL


initial viscosity (8). Above the limiting VISCOSITY
shearing stress, the viscosity diminishes The measurement Fof fundamental
strongly with increasing rate of shear viscosity can be accomplished by many
until some very high value of the latter different means. Since there are probably
seems to reach a limit. This viscosity hundreds of viscometers that have been
could be called a final viscosity. When developed, each one having some merit
investigating polymers, this final vis- in its particular application, only a few
cosity is only slightly higher than the of the more widely used methods repre-
viscosity of the solvent. In no case with senting various basic types and principles
asphalt could this final viscosity be even of operation will be discussed here.

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SYMPOSIUM ON FUNDAMENTAL VISCOSITY

Capillary Viscometer: The Zeitfuchs cross-arm viscometer


Probably the most widely used vis- appears to be the best adapted to use for
cometer in the petroleum industry is the asphaltic materials. Johnson et al (10)
capillary tube type. This type instrument have called this tube "The All Purpose
was developed by Poiseuille in his experi- Capillary Viscometer," since it also can
ments on the flow of fluids in capillaries, be used for transparent oils. This paper
while studying blood circulatory systems. also compares several capillary tubes to
Many different types of capillary vis- show why the Zeitfuchs merits this
description.
The Zeitfuchs cross-arm viscometer
r f
is now being used by many producers and
user agencies for cut-back asphalt vis-
cosity testing and has enabled all cut-
back materials to be specified at a single
temperature viscosity of 140 F (5).
The Zietfuchs tube has a normal use-
ful range of from 0.5 to 100,000 centi-
stokes. The Zeitfuchs viscometers can
PRECISION BORE be calibrated by a step-up procedure
CAPILLARY starting with the value for the viscosity
of water in a tube and then using an oil
of higher viscosity. This oil of known
viscosity can then calibrate the next
larger tube. This procedure is followed
until the tube with the highest multiplier
is calibrated with a very heavy oil. Of
course, National Bureau of Standards
standard oils can simplify this procedure.
Other advantages of this viscometer
are: (1) small sample size (about 2 ml),
(2) the tube is easily filled with sample,
(3) samples attain equilibrium tempera-
ture in about 5 min, (4) convenient over-
all dimensions (about 25 cm length),
and (5) it is easily and rapidly cleaned
in place.
FIG. 5.—Vacuum Capillary Viscometer (As- The Zeitfuchs cross-arm tube has a
phalt Inst. Type).
precision as stated by Johnson et al (10),
which is as good as other capillary vis-
cometers have been developed, but until
cometers. The Bureau of Public Roads
recently few have been widely used in
(11) reports that with N.B.S. standard
asphalt investigation. ASTM (9) shows
oils, which contained no volatile diluents,
four different types of tubes as being
used for asphalt or opaque liquids. (See the average deviation from the mean
Fig. 3.) They are the Cannon-Fenske, values of efflux times was generally
the Zeitfuchs cross-arm, the Lantz- within the 0.1 per cent level. From pooled
Zeitfuchs, and the BS U-Tube modified data for cut-back asphalts, the deviation
flow viscometer. from the mean was 0.63 per cent as com-

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LEVY ON DEFINITIONS AND MEASUREMENT 9

pared to 1.58 per cent for the Saybolt lary viscometer indicate that the co-
Furol method. efficient of variation increases with the
Recently a modified Zeitfuchs tube viscosity level. He states that duplicate
has extended its useful range to well results by the same operator should be
above 200,000 centistokes. The modified considered suspect if they differ by more
tube has been investigated to a limited than 5.5 per cent of the mean value.
degree by The Asphalt Inst, as a means
of measuring asphalt cement viscosities The Asphalt Inst, has made coopera-
at 140 F. Sufficient data are not avail- tive tests with this instrument, in which
able at this time to give precision esti- it was found possible to determine the
mates for the modified version. viscosity of asphalt cements at 140 F.
The precision of tests was on the order
Much attention has recently been
of 5 per cent within a laboratory and 15
given to the vacuum capillary viscometer
(12,13), a modification of the Koppers per cent between laboratories. Greater
vacuum capillary. The range of this precision can be expected with further
viscometer is from approximately 10 development of this method.
to 100,000 poises. In this range, it can The Asphalt Inst, has offered a modifi-
be used for measurements of viscosities cation of the capillary viscometer which
of asphalt cements at 140 F and for promises to eliminate many of the prob-
cut-back asphalts at 77 F. The rate of lems encountered in the first two develop-
shear may be varied in this instrument, ment stages of The Asphalt Inst. (See
which permits satisfactory measurements Fig. 5.)
of viscosities on non-Newtonian ma- The capillary viscometer is also
terials. adapted to use in a closed pressure sys-
Measurements of viscosity are made
tem using a metal capillary tube. This
by pouring approximately 4 to 6 ml into
principle of determining viscosity of
the outer tube of Fig. 4. The capillary
is inserted into the viscometer, which is liquids has been adapted to both labora-
supported in a constant temperature tory and industrial type instruments.
bath in a vertical position. When the The Franklin Inst. (14) capillary vis-
sample has reached the equilibrium cometer instrument, designed by Phil-
temperature of the test (30 to 60 min), lippoff, is shown in Fig. 6. This instru-
a precontrolled vacuum is applied to the ment is especially suitable for work
with asphalt at high temperature, since
upper end of the capillary tube.
the sample is totally enclosed in a nitro-
The passage of the sample between one
gen atmosphere which minimizes evapo-
or more pairs of marks is timed. The
ration losses and oxidation. In cases
vacuum, for best precision, should be
where data are available from both
at least 10 cm Hg and the flow time at
rotational viscometer and capillary vis-
least 50 sec. cometer measurements, good correlation
The viscosity is calculated from the was found. In this viscometer, measure-
dimensions of the capillary, the vacuum, ments are made under steady-load
and the time of flow. The rate of shear conditions; that is, a constant stress is
at the wall of the tube may also be cal- applied to shear the sample and the
culated. resultant rate of shear is measured. By
Heithaus reports (12) that repeat- varying the pressure head, as many
ability (within-laboratory variability) points as are desired can be obtained to
of measurements with the vacuum capil- define clearly a flow curve for the ma-

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10 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

X M-4

<
o «
£
<
=>
O ^3
t.1 U<

4J
c; ^
O

^"*"* u

>
>*
_rt
i
O.
<3.
U-*

<l
s
Oi
to
'5

to
Q
^ 1

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LEVY ON DEFINITIONS AND MEASUREMENT 11

terial. From these data, the viscosity can Rotational Viscometers:


be calculated (14). Ranges of stress There are three viscometers in this
(dynes per square centimeter) are from classification: the Stormer, the rotary,
about 10 to almost 106. Rates of shear and the Brookfield.

-» STIRRER AND MOTOR

THERMOMETER

NICHROME ASBESTOS
WIRE PAPER
HEATER INSULATION

••THERMOCOUPLE IS R E M O V E D WHEN READINGS ARE TAKEN

FIG. 7.—Cup, Bob, and Oil Bath Assembly of Modified Stormer Viscometer (from Ref. (18)).

can range from 10~3 to 105. This would The Stormer viscometer is available
allow viscosity determinations between commercially from most laboratory
10~3 poises and 108 poises. supply marketers (Fig. 7). The instru-
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UJ
<L3

1=
O-
UJ

i DC

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to

«x
UJ a
UJ
a
z
=3
UJ
_1
O-
z
CO
UJ o
<=)
ac LlJ
=E
z 1— uJ
UJ
CJ _ l ae
o UJ o UJ
i-O W 3

.1 ^
---- -
CJ ---
O-

£g •a- 1/3 C O eo <7» s:

•-^

a.
CJ
UJ
a= 3V
to UJ

o- a:
IL?
to

UJ
UJ ^
1^
1—
U^
UJ trt

^
to U-t
_J ^
1
<JO
o
t o
e^J
ac
* I UJ X
CO K to z
rO o
UJ a : t— t— Z
Z =D
2
«c
oc <z>
^
s:
CJ» i / )
O-
O - <K
to
^
o" • < CS
•«

t o CJ O-
C3

-<=> ^
-£ — to iD

S
m.- -- '- <» -
cv. P O t r a CO CO o

12
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LEVY ON DEFINITIONS AND MEASUREMENT 13

ment consists of a sample cup located in and corrected by reducing the applied
a constant temperature bath capable of load until the effect disappears. The
controlling the test sample to within absolute viscosity is calculated from a
±0.5 F. When the instrument has plot of the revolutions per second of the
reached the correct temperature, a bob bob and the applied load in grams.
is placed in a chuck, and the cup is The modified Stormer viscometer is
raised so that the bob is centered in the capable of viscosity measurement of
cup. The asphalt sample is heated sepa- Newtonian materials to an accuracy
rately to the lowest temperature at better than ± 5 per cent, without de-
which it can be easily poured into the pendence on viscosity standards, over
preheated cup. The cup is rilled to about a range from 1 to 150 poises (6). It can,
0.15 in. The asphalt is then heated or however, be used up to about 1000 poises.

X3
\ \ J*' , ^
O ^^
e
o
— y ^ ^
-*—XI-J-4\

- . — x 2 —» i 2

1
^ ^ ^ b
i
/ I —- ""*
/ b ^ ^ ^

< - » ! - < •
1
/ s' — y ^ ^ ^
yz

\
y> •

\ 1
-*-Xi-»* ti u
TIME, ti = t2

FIG. 9.—Deformation and Recoil Curves (Apparent Viscosity) (from Ref. (15)).
Points x\ j/i and xi j/u demonstrate the relative position of curve b' to b.

cooled to the test temperature, and the The rotational viscometer developed
bob is rotated slowly by hand to ensure at the Franklin Inst. (IS) is used to
homogenous temperature. When the determine the rheological properties of
asphalt is maintained at ±0.5 F, the asphalts over a wide range of shear,
thermometer or thermocouple is removed shearing stresses, and temperature.
and the times of bob rotation under Figure 8 shows a line drawing of this
various loads are determined. Several apparatus and both the high and low
determinations for each load should be shear cups and bobs.
made and should be within 2 to 5 per After an asphalt sample is placed in
cent of each other. the cup, the bob is pressed into place
Some asphalts at higher loads may in the sample and checked for proper
exhibit the Weissenberg effect, that is, position by completion of an electric
a channeling in the asphalt surface or circuit. The viscometer assembly is
a tendency to crawl up the shaft of the placed in a constant temperature bath
bob. This can usually be detected visually to attain test temperature equilibrium.

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14 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

By means of nylon cord or steel tape and or at very low temperatures this rota-
pulley wheels, loads up to as high as 50 tion may be slow, an accurate optical
lb can be applied to rotate the bob in the magnification of the scale is provided,
sample. Since at very low rates of shear Readings can be made to 0.1 deg. The

io- f j • ; : I F . 1 • r
1 !
' i ' 1 1
1
;
; 1 ! ,
11 ;
i • , ! ; ' •

1 i " . /
! i

,/
U- /
/
! 11 i
/
/
10'
(Med. C Asphalt at 100°C) , T
-1-+--

:
i

:
;

, , _- —4 " " -Ji^~


\r
—Ch~
[_ . ' I L
- - — - 1
-~-±_.
t 1
- • i • t *

!
' \ r ----- -J
1 >-~t--t—t—U _ . _, _ _ _ i _ T _ p—. • - -
-o|-o 1 1 "- —i
- • • — - — i

'
i
V
<
LLI
• . , 1
7°: ... _
X
to : ' 1' ; ,'.«j f— : r--^~
'

1 ; • i
Mi! ' —1—. .-fl~-
' • 1 — • ' >

4— -- ^^~
°s ,
3 i ^ ^— — — - —
tr
1: . , - -t.
/ ROTATIONAL VISCOMETER '
10" , . i , j

-H-i _. " - : : : : _ 4 _: : : : ;
• LOW SHEAR
|! !
•• ! i
O HIGH SHEAR
x S - • •
:
IS """ t/ ^ 7T CAPILLARY VISCOMETER i

f i
. i :

|ii
! ©
®
A
NO. 0
NO. 1
NO. 2
io-2 L
X NO 3
— I — =j-rr-r±l I 1—4—r-t-f-j-
// L
1
i 1 i i ! i
ii
10' IO3 IO4 IO5

SHEARING STRESS, T dynes per sq cm


FIG. 10.—Flow Curve Showing Rate of Shear Versus Shearing Stress (from Ref. (14)).

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LEVY ON DEFINITIONS AND MEASUREMENT 15

viscosity is calculated from the applied by taking readings of load, time, and
load and the time for 1 deg of bob rota- degree of rotation for some period of time,
tion. t. These readings reflect both viscosity
The Franklin Inst, has determined and elastic properties. The applied load
viscosity values for various types of is then removed to allow the bob to recoil
asphaltic materials with the instrument. for the same period, t, as a measure of

FIG. 11.—Sliding Plate Microviscometer in Water Bath (from Ref. (17)). Heater and con-
trols not shown.

The range of application is as follows: the elastic element. Measurements of


Shearing stress, dynes per the recoil time and degrees of rotation
sq cm 10 to 106 (up to 50 are taken. Figure 9 shows a typical
lb in load) deformation and recoil curve for a
Rate of shear, sec -1 10~5 to 103
Viscosity, poises 1 to 108 viscoelastic asphalt: dr is the degrees of
Temperature range, deg rotation and / is the time from the
Cent - 20 to 300
beginning of the test. Curve a is the
Rates of shear and shear strains are deformation curve, b is the recoil curve,
measured at constant shearing stresses b' is curve b inverted and plotted from
(steady load conditions prevail). By the origin, c is curve b' subtracted from
varying the shearing stresses and then curve a. Curve a represents the total
measuring rates of shear, a point-by- effect of the viscous and elastic com-
point determination of viscosity and ponents responding simultaneously to
elasticity can be readily obtained. the applied force. Curve b (and b') re-
Most asphaltic materials exhibit some flect the elastic response after the ex-
degree of elasticity, which is measured ternal force has been removed. Curve c

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16 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

represents the net effect, or the viscous the viscous resistance to the induced
response, of the sample under a specific movement. This is accomplished by
force at one temperature. The slope of driving the immersed element, which is
this curve c is used to determine the called a spindle, through a beryllium
viscosity. copper spring. The degree to which the
The flow curve, rate of shear versus spring is wound, indicated by the position

FIG. 12.—Sliding Plate Microviscometer (from Ref. (17)).

shearing stress, in Fig. 10 shows correla- of the red pointer on the viscometer's
tion data obtained from the Franklin dial, is proportional to the viscosity of
Inst, rotational viscometer and the the fluid for any given speed and spindle.
capillary viscometer. The viscometer is able to measure over
a number of ranges since, for a given
Brookfield Viscometer:
drag, or spring deflection, the actual
"The instrument rotates a cylinder viscosity is proportional to the spindle
or disc in the sample (fluid) and meas- speed, and it is also related to the
ures the torque necessary to overcome spindle's size and shape. For a material
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L E V Y ON D E F I N I T I O N S AND MEASUREMENT 17

of a given viscosity, the drag will be to the base of the viscometer, and plate
greater as the spindle size and/or rota- B is clamped to the loading device.
tional speed increases. The minimum The loading device consists of a simple
range of any viscosity model is obtained beam with the movable plate suspended
by using the largest spindle at the from one end and the load from the other.
highest speed—the maximum range by The beam is pivoted on steel knife edges
using the smallest spindle at the lowest and agate bearings.
speed" (16). Displacement of the sliding plate B
Goodwin (16) makes the following is followed by a simple resistance con-
observations in working with this in- tact servo system. The servo motor
strument: drives an insulated metric micrometer,
1. A 1000-ml sample size is required. M, causing it to maintain a high-re-
2. Continuous stirring is necessary to sistance contact between the point on
maintain uniform temperature. the micrometer, and the flag, F, attached
3. Rapid heating is needed to mini- to the plate holder.
mize vaporization of volatile solvents Readings of the micrometer with time
from cut-back asphalts. are recorded either visually or by a
4. Viscosity should be determined as recording instrument. The recorder use
soon as possible after reaching constant is highly recommended since it magnifies
temperature owing to temperature drop the plate movement 250 times, which
at center of sample. makes it possible to run tests at several
5. Preheating of the spindles gives shear rates with very slight plate move-
more uniform viscosity values. ment. The sliding plate assembly is
6. For best accuracy it is necessary placed in a constant temperature bath
to select a spindle size and speed to give a during the running of the test.
scale reading not requiring use of the Equilibrium test temperatures can be
upper or lower portion of the dial. reached in less than 2 min between 39.2
7. Results of tests of cut-back asphalts and 140 F. The range of the viscometer
tested at or near room temperature have is from 102 to 1011 poises. Viscosities
been correlated satisfactorily with Say- must be determined at two or more
bolt Furol determinations. shear rates to permit interpolation to the
8. This instrument is a valuable tool desired shear rate. The film thickness is
for fairly rapid routine control for vis- computed from weight, area, and specific
cosity specification monitoring. area.
Sliding Plate Viscometer: Viscosity is calculated from the
formula for the viscosity of Newtonian
The sliding plate viscometer (Figs. 11 liquids:
and 12) is the most popular instrument
for measuring absolute viscosities and dv
So = n ~
flow properties of asphalt in the lower dr
temperature ranges. This instrument
shears a thin film of asphalt placed be- where:
tween two parallel flat plates by action So = shearing stress, dynes per square
of a constant shearing stress. Its prin- centimeters = load in grams X
ciple is shown diagramatically in Fig. 1. 980/area of plate in centimeters
A thin layer of sample is placed be- ,, and
tween the two polished pyrex glass plates — = rate of shear in sec - 1 = movement
(A and B) of Fig. 12, which are mounted in centimeters/time in seconds X
in a vertical position. Plate A is clamped film thickness in centimeters
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18 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

Repeatability of viscosity determina- within ± 2 per cent of full scale for


tions using the sliding plate viscometer Newtonian materials of low viscosity
are reported as within the area of ± 1 (approximately 2000 cps). Reproduci-
to 3 per cent of the mean value. bility of readings for non-Newtonian
materials is stated as being within ± 1
OTHER VISCOMETERS
per cent of full scale.
Bendix Ultraviscoson:
Dynatrol Viscometer:
This instrument is available both as a
This instrument3 can be used for both
laboratory model and an industrial type
laboratory and industrial applications.
for use in continuously monitoring
A driving coil receives a 60-cycle current
stream viscosity. A probe reed made of
which produces a 120-cycle vibration in
magnetostrictive iron, which changes its
a hairpin type probe. The probe vibration
physical dimensions in a magnetic field,
is proportionally damped by viscous
is placed in a sample or a stream of
fluids. The pick-up end of the probe
liquid. One half of this reed is inside the
assembly contains a permanent magnet
probe assembly. Concentric to this reed
and coil which give an output signal
is a probe coil. A current pulse in the
proportional to the amplitude of the
coil sharply changes the magnetic field
damped vibration. This signal is then
about the reed element and the blade
amplified electronically and calibrated
or reed is shocked into vibration. This
to read viscosity in poises on a continuous
vibration is on the order of 28,000 cps
recording chart.
with an amplitude of about \ n.
This instrument has an operating
The reed is alternately energized by
range from 1 to 100,000 centipoise.
the coil current and damped by the
Temperature compensation accessories
viscous liquid as its vibration reaches
enable this instrument to measure the
some small value. The higher the vis-
viscosity at line or sample temperature
cosity, the more rapid the damping and
and record viscosity at another tempera-
the more frequent the driving pulse.
ture.
By measuring the average current which
results from these driving pulses, the Industrial Type Capillary Viscometers:
instrument can be calibrated in terms of
At least two viscometer instruments
viscosity.
for laboratory or industrial process ap-
The electronic computer reads out on plication use the principle of flow through
a meter, or the data can be transmitted a capillary tube. The Standard Oil
to a recorder for continuous viscosity Co. (Indiana) continuous viscometer has
monitoring. an operating range of 30 to 2500 Say-
This instrument has a normal range bolt Universal sec (500 centistokes) at 100
for viscosity up to 50,000 centipoise to 210 F, and a special range up to 30,000
times density and can be extended to Saybolt Universal sec (6000 centistokes)
500,000 centipoise times density with a up to 250 F. Accuracy is reportedly within
special probe. One could say that for ±0.3 per cent.
asphaltic materials with specific gravity A similar continuous recording vis-
close to 1, the instrument has a range of cometer of the Shell Development Co.
50,000 to 500,000 cps. It can be operated has an operating range of up to 2500
up to 650 F, and from vacuum to 1000 centipoise and up to 400 F. Over-all
psi. When calibrated with oils of known
viscosity and rechecked occasionally, 3
Manufactured by Automation Products,
the instrument is capable of accuracy Inc., Houston, Tex.

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LEVY ON DEFINITIONS AND MEASUREMENT 19

accuracy is reportedly within ± 1 per study of flow properties of asphaltic


cent. materials. In time, these properties, can
Both of these instruments depend possibly be correlated with other physi-
upon very accurate temperature control. cal properties and performance data.
Viscosity and flow characteristics in
CONCLUSIONS themselves will most probably not pro-
This discussion has touched upon vide a cure-all answer, but they do pro-
some of the means of measuring absolute vide a starting place pointed toward
viscosity. These instruments and others replacing the arts in asphalt technology
to be developed will greatly aid in the with science and engineering.

REFERENCES

(1) E. C. Bingham, Fluidity and Plasticity, Halstead, "Comparison of Zeitfuchs Cross-


McGraw-Hill Book Co., New York, N. Y., Arm and Saybolt Furol Viscometers for
1922. Measuring Viscosity of Cut-Back As-
(2) A. Bondi, Physical Chemistry of Lubricating phalt," Public Roads, Vol. 31, No. 12, Feb.,
Oils, Reinhold Publishing Corp., New York, 1962, p. 248.
N.Y.,1951. (12) J. J. Heithaus, "Measurement of Asphalt
(3) W. L. Badger and W. L. McCage, Ele- Viscosity with a Vacuum Capillary Vis-
ments of Chemical Engineering, McGraw- cometer," ASTM STP. No. 309, Am.
Hill Book Co., New York N. Y., 1936. Soc. Testing Mats., 1961, p. 63.
(4) Method of Test for Calculation of Absolute (13) J. Y. Welborn and W. J. Halstead, "Abso-
Viscosity (D 1745-60 T), 1961 Book of lute Viscosity as a Specification Control for
ASTM Standards, Part 7, p. 935. Bituminous Binders," Public Roads, Vol-
(5) D. F. Levy, F. E. Fassnacht, G. P. Hibler, 31, No. 12, p. 243, Feb., 1962.
R. D. Umbach, and D. VV. Gagle, "Funda- (14) F. H. Gaskins, "Use of the Capillary
mental Viscosity versus Saybolt Furol Viscometer," Technical Report R-7, Frank-
Viscosity for Refinery Control of Cut-Back lin Institute Laboratories for Research
Asphalt," ASTM STP No. 252, Am. Soc. and Development, Jan., 1955.
Testing Mats., 1959, p. 211. (15) F. H. Gaskins, "Use of NARC Rotational
(<5) E. K.Fischer and C. H. Lindsley, "Rheologi- Viscometer," Technical Report R-6, Frank-
cal Measurements with the Rotational Vis- lin Institute Laboratories for Research and
cometer," Textile Research Journal, Vol. Development, Aug. 1, 1954.
XVIII, No. 6, 1948, p. 325. (16) VV. A. Goodwin, "Correlation Between
(7) H. H. Zuidema, Performance of Lubricating Saybolt-Furol Viscometer and the Brook-
Oils, Reinhold Publishing Corp., New field Syncro-Lectric Viscometer for Meas-
York, N. Y., 1952. uring Viscosity of Cut-Back Asphalts,"
(8) W. Pbilippoff, "Summary of the Progress Proceedings, Assn. Asphalt Paving Tech-
on the Rheology of Asphalt During the nologists, Vol. 30, 1961, p. 447.
Operation of the NARC," Technical (17) R. L. Griffin, T. K. Miles, C. J. Penther,
Report R-8, Franklin Institute Laboratories and W. C. Simpson, "Sliding Plate Vis-
for Research and Development, July, 1955. cometer for Rapid Measurement of Asphalt
(9) Method of Test for Kinematic Viscosity Viscosity in Absolute Units," ASTM
(D 445-61), 1961 Book of ASTM Stand- STP No. 212, Am. Soc. Testing Mats.,
ards, Part 7, p. 189. 1956, p. 36.
(10) J. T. Johnson, R. L. LeTourneau, and R.
Matteson, "All Purpose Capillary Vis- (18) D. H. Russell, "Use of the Modified
cometer," Analytical Chemistry, Vol. 24, Stormer Viscometer," Technical Report
p. 1505, 1952. R-3, Franklin Institute Laboratories for
(11) E. R. Oglio, J. A. Zenewitz, and W. J. Research and Development, April 17, 1953.

Copyright by ASTM Int'l (all rights reserved); Thu Dec 22 07:49:02 EST 2011
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STP328-EB/Apr. 1963

R E L A T I O N OF E M P I R I C A L TESTS TO F U N D A M E N T A L
VISCOSITY OF ASPHALT C E M E N T

B Y J. M. GRIFFITH 1 AND V. P. PUZINAUSKAS 2

SYNOPSIS

Duiing the past two years, a cooperative viscosity testing program under
the sponsorship of The Asphalt Institute, has been conducted on a range of
commercially available asphalt cements. The program was designed (1) to
develop an accurate method for viscosity measurement of asphalt cements at
140 F and (2) to compare the consistency characteristics of asphalt cements as
measured by a fundamental viscosity test. The results of this program to date
are discussed.

During its application and use, asphalt ments obtained by any of these tests
cement is subjected to heat, changes in represent only a single point on a con-
temperature, variable shear or loadings, sistency-temperature curve and are
and weathering. These factors change the expressed in variable units of time,
consistency or hardness of asphalt and, length, or temperature. Because the
consequently, influence the performance tests have limitations and because differ-
of the material. Several purely empirical ent measurement units result, it is
tests such as penetration, ductility, difficult to establish an accurate cor-
softening point, and Saybolt Furol vis- relation between the results of the various
cosity have been devised to measure the tests or between the test results and the
consistency of the material. These tests performance of the material.
generally define and characterize asphalt Even with their inherent shortcomings,
so that to some extent, at least, its flow these tests have served reasonably well.
behavior (rheology) and performance However, with the advent of more
under these variable conditions can be exacting road-building procedures and
controlled and predicted. more rigid specifications for the finished
These empirical tests can be described product, there is a need for more accurate
as rheological or consistency tests when tests that will describe the properties of
considered as a group. Individually, asphalt cement under a wide range of
however, these tests are limited as a conditions with the same units of meas-
measure of asphalt's wide spectrum of urement.
rheological behavior when it is subjected The use of fundamental viscosity
to the influences of time, temperature, measurements appears to be a logical
and shear. Furthermore, the measure- step in this direction. However, high
viscosity and extremely large changes in
1
Director of Research and Development, viscosity of asphalt with changing tem-
The Asphalt Inst., College Park, Md. peratures posed instrumentation prob-
2
Assistant Research Engineer, The Asphalt lems. This was perhaps the main objec-
Inst., College Park, Md.
20

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Copyright" 1963 by ASTM ASTM Int'l
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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 21

tion in the early days of asphalt Co., the temperature range at which
technology to the use of viscosity as a asphalt cement viscosities could be
basis for classifying asphalt grades. In measured reliably was further extended.
1935, the problem was partially al- However, even with these developments,
leviated by the development of the instrumentation problems still exist with
vacuum capillary viscometer by Rhodes, regard to measuring asphalt cement
Volkmann, and Barker (l).3 This instru- viscosity at or near freezing tempera-
ment was modified in 1940 by Lewis and tures.

T A B L E I.—SUM-MARY OF VARIABILITY OF VISCOSITY OF ASPHALT


C E M E N T S A T 140 F .

Testing Phase 1
Testing Phase 3

Asphalt E Asphalt F Asphalt G Asphalt H

T y p e of viscometer" . . V V V Z V V zc
N u m b e r of coopera-
tors 9 9 9 0 9 18 13 12
Average viscosity,
poises or stokes. . . . 8615 9500 604 583 1693 1822 381 389 1886 1817 1390
Standard deviation
between tests
within laboratories
poises or s t o k e s . . . . 115 330 15 30 58 22 10 45 47 91
Coefficient of varia-
tion within labo-
ratories, per c e n t . . . 1.3 3.5 2.4 5.1 3.4' 1.3 2.4 2.6 2.4 2 6 4.7
Repeatability, per
cent 3.6 9.71 0.7 1 4 . 1 9.4 3.6 6.7 7.2 6.7 7 1 13.0
Standard deviation
between labora-
tories, poises or
stokes 777 1818 52 38 83 236 21 21 87 236 81
Coefficient of varia-
tion between labo-
ratories per c e n t . . . 9.1 19.2; 8.5 6.5 4.9 13.0 4.9 4.8 4.6 13 0 4.2
Reproducibility, per
cent 25 53 24 18 14 36 14 13 13 45 12

" V = V a c u u m , Z = Zeitfuchs, C = C a n n o n .

Halstead (2) who demonstrated that it COOPERATIVE VISCOSITY


would provide accurate viscosity deter- TESTING PROGRAM
minations of different asphalt cements
within the temperature range of 100 to The Asphalt Institute's cooperative
200 F. Further refinement of the instru- testing program was conducted in three
ment and measuring techniques was re- phases. The first and third phases were
ported to ASTM in 1961 by Heithaus (3). to evaluate the repeatability and re-
With the development of the sliding plate producibility of instruments and test
microviscometer (4) by the Shell Oil methods considered suitable for the
measurement of the viscosity of asphalt
3
cements at 140 F. The second phase
T h e boldface n u m b e r s in p a r e n t h e s e s refer
t o t h e list of references a p p e n d e d t o this paper. was to compare viscosity test results

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22 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

with various empirical test properties of In phase 3, an 85 to 100 penetration


different asphalt cements. In this testing asphalt cement, furnished by one manu-
phase 63 asphalts were used. These facturer from a single source, was used.
asphalts, supplied by different producers, Quart samples of this asphalt were
were considered generally to be repre- distributed among 23 cooperating labora-
sentative of commercially available tories. Three types of viscometers—
products. Koppers vacuum capillary, Zeitfuchs
In phase 1, four asphalts, widely cross-arm, and Cannon asphalt—were
differing in viscosity, were used. Two of evaluated by measuring the viscosity
these asphalts were 60 to 70 penetration of this asphalt at 140 F. Eighteen of the
grade, and two others were 200 to 300 23 cooperators used vacuum capillary
penetration grade. In each grade, one viscometers, and 14 used the Zeitfuchs
asphalt represented low-viscosity and cross-arm and Cannon types.

ozr

vr/
Ky
A B C D
NORMAL MOOFIED CANNON ASPHALT
CROSS-ARM TYPE CROSS-ARM TYPE TYPE
FIG. 1.—Gravity Flow Viscometers for Asphalt Cements.

the other high-viscosity materials. Two Because phase 1 testing had indicated
types of viscometers—(1) Koppers vacu- that sample preparation and handling
um capillary and (2) gravity flow, normal or procedures before viscosity measurement
modified Zeitfuchs cross-arm—were eval- influenced the accuracy of the test re-
uated. For the vacuum capillary viscom- sults, all cooperators were instructed to
eter, procedures were used as described follow carefully identical sample prepara-
by the Shell Oil Co. (3). For the Zeitfuchs tion and testing procedures for all types
cross-arm viscometers, a slight modifica- of viscometers in phase 3 tests. (These
tion of the procedure described by ASTM test procedures are described in the
Method D 445 - 53 T 4 was used. Appendix.)
Of the ten cooperators who partic- In phases 1 and 3, three viscosity
ipated in phase 1, nine measured the measurements were made by each co-
viscosity of four asphalts by vacuum operator on each test sample of asphalt
capillary viscometers; six of the ten cement. These test data are analyzed
used Zeitfuchs cross-arm gravity flow in Table I.
viscometers. In phase 3, the viscosity of asphalt
4
cement at 140 F after thin film oven test
Method of Test for Kinematic Viscosity
(D 4 4 5 - 6 1 ) , 1961 Book of ASTM Standards, heating also was determined. Sixteen
Part 7, p. 189. cooperators made these measurements
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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 23

with the vacuum capillary type vis- were included in the group. Asphalt
cometer, and eight used modified manufacturers submitted samples repre-
Zeitfuchs cross-arm viscometers. In some senting asphalt cements of high- and
instances, the cooperators made three low-temperature susceptibility. This
measurements. In others, two measure- group of 63 asphalts therefore constituted
ments were made. A statistical analysis a representative sampling of major types
of viscosity data after the thin film oven of asphalt cements and probably repre-
test also was made. However, variability sents the extreme of those now in general
in viscosity measurements and differ- use for road building in this country.
ences in heating oven performance TEST APPARATUS AND PROCEDURES
contributed to a wide variance in these
test results. Therefore, a statistical Gravity Flow Viscometers:
interpretation of these data is not in- Figure 1 shows the four gravity flow
cluded here. instruments used in this cooperative

H in

W w
STRAIGHT CAPLLARY CANNON-MANNING ASPHALT INSTITUTE
(KDPPER'S) TYPE TYPE TYPE

FIG. 2.—Vacuum Type Viscometers for Asphalt Cements.

In phase 2, temperature-viscosity testing program. Figures 1(a), (b), and


relationships of 63 different asphalt (c) are the conventional and modified
cements were determined for comparison Zeitfuchs cross-arm type viscometers.
with various empirical test values such as Figure 1(a) is the Zeitfuchs cross-arm,
penetration before and after the thin reverse flow viscometer described in
film oven test, and softening point. ASTM Method D 445 - 53 T, Appendix
Viscosities of the original asphalt ce- F. This instrument was used to measure
ment were established at 77, 140, and viscosities of asphalt cements at 275 F.
275 F. Viscosity of the asphalt cements For this test program, Zeitfuchs cross-
at 140 F after thin film oven test heating arm viscometers were modified to provide
and at softening point temperature also viscometers having constants of 100
were determined for each asphalt. All and 300. This viscometer is shown in
testing in this phase was done by the Fig. 1(b). Figure 1(c) shows another
Asphalt Institute laboratory. modification of the Zeitfuchs cross-arm
The 63 asphalt cements of varying viscometer. With this modification,
properties were supplied by 16 manu- viscometers having constants of 500 and
facturers for this phase of the testing. 1000 were used. These large constants
Asphalts used in certain test roads also required radical changes in viscometer

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24 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

design. The diameter of the glass capil- mersed in the molten asphalt cement.
lary was considerably enlarged and the The conventional and modified Zeitfuchs
over-all length of the instrument was cross-arm viscometers are filled by
substantially decreased. pouring the liquefied asphalt through a

TEMPERATURE
BATH

(a) Apparatus for temperature and vacuum control (type 1).


FIG. 3.—Auxilary Apparatus for Measuring Viscosity of Asphalt Cements.

Figure 1(d) shows the Cannon gravity larger viscometer arm until the sample
flow viscometer for asphalt cements. reaches the indicated mark. During
This is a U-shaped glass tube having an filling, the small viscometer arm is
enlarged bulb as a sample container. To closed.
fill this viscometer, the instrument is Since a liquid of known viscosity and
inverted and suction is applied to one arm density is used to calibrate all gravity
of the tube while the other arm is im- flow instruments, viscosities measured

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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 25

by these instruments are expressed in The modified Koppers instrument


stokes or centistokes which are the (Fig. 2(a)) has been described in detail
units of kinematic viscosity. elsewhere (1-3). This viscometer consists

I
TEMPERATURE
BATH WITH CONTROLS
VISCOMETERS

(b) Apparatus for temperature and vacuum control (type 2).


FIG. 3.—Continued.

Vacuum Capillary Viscometers: of a sample container and a precision


bore straight glass capillary tube of
Figure 2 shows three types of vacuum known radius. This capillary is ac-
capillary viscometers currently available. curately subdivided into intervals of
Although the testing described here was equal length. The time required for the
accomplished with the modified Koppers asphalt to rise in the capillary between
viscometer (Fig. 2(a)), the other two several intervals, under the influence of
instruments are shown to indicate their vacuum, is measured. The viscosity is
general features. then calculated by using the Poiseuille
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TABLE II.—VISCOSITY OF ASPHALT C E M E N T S AT D I F F E R E N T T E M P E R A T U R E S .
ASPHALT INSTITUTE VISCOSITY TESTING PROGRAM: SECOND PHASE.

Penetration, Viscosity"
Asphalt 100 g per 5
sec at 77 F
77 F, poises 140 F, c poises 275 F, stokes

No. 1 84 1 0 . 8 0 X 10 5 1 1 . 5 3 X 10 2 2.90
No. 2 131 4.66 5.59 2.19
No. 3 222 1.60 2.54 1.72

No. 4 57 33.75 N 21.23 3.59


No. 5 87 9.88 N 8.80 2.37
No. 6 161 2.22 3.39 1.60

No. 7 39 61.10 33.49 4.13


No. 8 86 9.10 10.40 2.34
No. 9 236 1.28 2.57 1.23
No. 10 47 52.60 56.56 6.80
No. 11 94 9.15 16.76 3.83
No. 12 193 2.30 5.85 2.33

No. 13 59 24.15 24.78 4.06


No. 14 86 10.25 13.75 3.20
No. 15 231 1.65 3.69 1.80

No. 16 202 1.45 3.82 1.85


No. 17 89 8.15 10.62 2.82
No. 18 55 18.40 20.72 3.61
No. 19 192 1.80 5.33 2.67
No. 20 85 9.50 18.16 4.76
No. 21 62 25.25 37.98 6.56

No. 22 85 10.20 8.48 1.79


No. 23 193 1.65 2.47 1.16

No. 24 199 1.80 N 5.45 2.25


No. 25 63 23.50 78.61 nN 6.57
No. 26 96 7.45 9.61 1.67
No. 27 159 2.30 3.13 1.53

No. 28 37 73.63 54.50 4.39


No. 29 93 9.53 16.52 3.74

No. 30 89 12.60 27.53 11.68


No. 31 142 5.95 10.67 6.80
No. 32 224 1.48 5.67 4.76

No. 33 34 59.25 28.74 3.55


No. 34 62 26.40 40.33 6.90
No. 35 88 12.85 25.70 5.26
No. 36 220 1.72 6.42 2.75

No. 37 89 12.30 6.78 2.04


No. 38 95 9.05 16.61 4.40

No. 39 41 42.00 N 23.39 2.46


No. 40 85 9.82 N 9.23 1.68
No. 41 199 1.88 3.44 1.11

No. 42 58 24.80 26.85 4.11


No. 43 85 14.20 15.45 3.17
No. 44 168 3.19 5.71 2.43

No. 45. 42 65.75 166.00dnN 6.58


No. 46. 37 130.50 2570.00dnN 24.31

26
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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 27

TABLE II.—Concluded.

Penetration, Viscosity0
Asphalt 100 g per 5
sec at 77F
77 F, 6 poises 140 F, c poises 275 F, stokes

No. 47 86 9.55 13.10 2.69


No. 48 87 9.42 12.61 3.38
No. 49 84 11.88 17.32 3.98
No. 50 43 54.95 94.42 4.92
No. 51 42 59.62 38.88 4.50

No. 52 90 9.78 16.60 4.40


No. 53 122 5.12 10.48 3.58
No. 54 215 1.50 N 4.81 2.63
No. 55 90 7.05 N 9.10 2 57
No. 56 137 3.44 N 5.43 2 12
No. 57 220 1.38 N 3.20 1 67

N o . 58 59 22,02 32.88 5 18
N o . 59 66 18.00 30.46 5.40

N o . 60 87 10.10 15.29 3 25
N o . 61 78 14.45 19.09 3.45
N o . 62 87 10,95 17.60 3.80

N o . 63 94 8.42 10.45 2.91

" Viscosities at 77 F determined with sliding plate microviscometer (shear rate 5 X 10~2 sec -1 ).
Viscosities at 140 F determined with vacuum capillary method. Viscosities at 275 F determined
with gravity flow Zeitfuchs cross-arm viscometers.
b
All asphalts show non-Newtonian properties except where indicated by N (Newtonian).
c
All asphalts show Newtonian properties except where indicated by nN (non-Newtonian).
d
Viscosities measured with sliding plate microviscometer.

equation for capillary flow. The shear rate of liquid flow into the expanded
susceptability of asphalts can be deter- measuring bulbs. Depending on the
mined by making separate determina- magnitude of the asphalt viscosity, the
tions of different values of vacuum. time required to fill either or both meas-
Also, since the rate of flow of asphalt uring bulbs is measured. The viscosity
decreases with the gradual rise of liquid of the asphalt is then calculated by
in the capillary, flow measurements at multiplying the filling time by the bulb
different levels during the same test can constant, expressed in poises per second.
be used to calculate the shear suscepti- With this viscometer, the asphalt ce-
bility within a relatively narrow range ment is in direct contact (through the
of shear rates. Details of the test proce- glass wall of the instrument) with the
dures used with this instrument are bath heating medium; therefore, the
described in the Appendix. All viscom- time necessary for preheating the sam-
eters of this type used in the testing ple to the test temperature is somewhat
program were manufactured by the in- shorter than with the modified Koppers
dividual cooperators. type. However, since both measuring
The Cannon-Manning vacuum asphalt bulbs of the Cannon-Manning viscom-
viscometer (Fig. 2(b)) has two enlarged eter are filled with asphalt flowing at a
measuring bulbs on one arm of the bent constant rate, the detection of complex
tube. Located below these two bulbs is flow behavior of asphalt requires at
a short section of precision bore glass least two tests using different vacuums
capillary. This capillary governs the or two viscometers of different capillary
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TABLE I I I — C O M P A R I S O N OF T H I N FILM OVEN TEST AND SOFTENING POINT
T E S T P R O P E R T I E S ON VISCOSITY BASIS (SECOND PHASE)

Thin Film Oven Test (TFOT) Softening Point

Penetration Retained Viscosity at 140 F,


g per 5 sec
Weight Loss 100 at Penetra- poises Viscosity Softening
or Gain, 77 F
tion of Increase Point (R
per cent Original, Original, & B), deg
per cent per cent Fahr
Original Heated Original Heated

-0.107 84 43 51.2 1153 5 202 351.2 120.0


-0.179 131 60 45.8 559 2 467 341.3 111.5
-0.899 222 74 33.5 254 1 235 386.2 103.5

-0.137 57 29 50.9 2123 6 282 195.9 123.7


-0.235 87 43 49.4 880 2 664 202.7 117.0
-0.284 161 76 47.2 339 965 184.7 109.7

-0.000 39 23 59.0 3349 12 126 262.1 128.2


-0.000 86 41 47.7 1040 3 290 216.3 116.2
-0.108 236 96 40.7 257 775 201.5 100.7
-0.446 47 28 59.6 5656 23 240 310.9 131.0
-0.604 94 46 48.9 1676 7 021 318.9 116.5
-1.482 193 76 39.4 585 3 686 530.0 106.2

-0.176 59 36 61.0 2478 7 638 208.2 122.5


-0.028 86 50 58.1 1375 4 194 205.0 116.2
-0.307 231 113 48.9 369 978 165.0 101.5

0.121 202 130 64. 382 602 57.6 103


0.107 89 58 65. 1062 1 977 86.1 114
0.123 55 40 72. 2072 3 290 58.8 122
-0.098 192 106 55. 533 1 281 131.6 105
0.088 85 54 63. 1816 4 485 147.0 119
0.060 62 40 64 3798 12 965 241.4 127

-0.005 85 42 49 848 2 294 170.5 116.0


-0.326 193 70 36 247 771 212.1 105.5

-1.030 199 84 42.2 545 2 247 312.3 103.0


-0.101 63 42 66.6 7861 58 824 648.3 133.0
-0.314 96 45 46.9 961 2 923 204.2 124.5
-0.450 159 75 47.2 313 948 202.9 116.5

-0.503 37 20 54.0 5450 17 409 219.4 132.5


-0.807 93 50 53.8 1652 6 407 287.8 117.2

0.088 89 63 70.8 2753 5 427 97.1 122.5


0.063 142 93 65.5 1067 2 104 97.2 111.2
0.082 224 147 65.6 567 1 022 77.4 100.7

0.033 34 22 64.7 2874 9 438 228.4 125.5


-0.459 62 37 59.7 4033 19 552 384.8 126.5
-0.840 88 44 50.0 2570 11 062 330.4 119.5
-1.751 220 87 39.5 642 3 346 421.2 104.7

0.160 89 49 55. 678 1 243 83. 119.5


0.098 95 62 65. 1661 4 611 177. 119.2

-0.093 41 22 53. 2339 7 806 233. 123.2


-0.303 85 43 50. 923 2 539 175. 114.2
-0.783 199 102 51. 344 876 154. 102.0

0.064 58 39 67. 2685 6 368 137. 126.5


0.059 85 55 64. 1545 3 142 103. 118.5
-0.254 168 90 53. 571 1 402 145. 107.5

28
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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 29

T A B L E I I I —-Concluded.

Thin Film Oven Test (TFOT) Softening Point

Penetration, Viscosity at 140 F, Viscosity


Asphalt Retained Viscosity Softening at Soften-
Weight Loss 100 at
g per 5 sec
78 F Penetra- poises Increase Point (R ing Point
or Gain, tion of Original, & B), deg Tempera-
per cent Original, per cent Fahr ture,
Original Heated per cent Original Heated poises

N o . 45 -0.032 42 28 66.6 16 600 144.5 11 186


N o . 46 37 257 000 178.0 29 037

No. 47 -0.413 86 46 53.5 1 310 3 708 183.0 113.2 15 042


No. 48 -0.040 87 48 55.2 1 261 3 764 198.4 115.5 11 898
No. 49 -0.098 84 51 60.7 1 732 4 963 186.5 116.0 15 694
No. 50 -0.380 43 23 53.5 4 942 12 045 143.7 129.0 13 673
No. 51 -0.190 42 25 59.5 3 888 11 078 184.9 122.5 24 459

No. 52 -0.030 90 54 60.0 1 660 5 862 253.1 116.5 12 824


No. 53 0.005 122 72 59.0 1 048 3 479 232.0 112.2 10 702
No. 54 -0.066 215 120 55.8 481 1 168 242.8 104.0 7 813
No. 55 0.148 90 57 63.3 910 1 909 109.8 113.5 9 340
No. 56 0.115 137 89 65.0 543 984 81.2 103.2 12 851
No. 57 0.089 220 129 58.6 320 588 83.7 102.2 6 705

N o . 58 -0.100 59 36 61.0 3 288 11 325 244.4 123.7 14 278


N o . 59 -0.104 66 39 59.1 3 046 10 792 254.3 123.0 14 017

N o . 60 -0.108 87 49 56.3 1 529 4 504 194.6 114.0 15 498


N o . 61 -0.047 78 43 55.1 1 909 8 865 364.4 119.2 14 032
N o . 62 -0.040 87 57 65.5 1 760 4 571 159.7 119.0 10 860

N o . 63 0.079 94 54 57.4 1 045 3 558 240.5 116.0 9 177

size. Limited test data indicate that the operation are described in Reference 4
accuracy of this viscometer is good. and other publications.
Figure 2(c) shows another vacuum
Auxiliary Apparatus for Measuring Vis-
capillary viscometer designed by Asphalt
cosity of Asphalt Cements:
Institute personnel. One arm of this
viscometer consists of a straight pre- Since a complete description of auxil-
cision bore capillary divided into several iary apparatus is included in the Appen-
segments of equal length. Basically, this dix, only a general description is given
viscometer is a combination of the good here.
features of both instruments described Constant Temperature Bath.—For ac-
previously. First, the asphalt sample is curate measurement of asphalt cement
not separated from the bath medium by viscosity, close temperature control is
the air space. Second, the instrument is important. All cooperators used baths
also adaptable for the detection of the capable of controlling temperatures to
asphalt cement's complex flow behavior, ±0.2 F (Fig. 3(a)). Other baths availa-
using a single test. ble include a toggle valve arrangement
to permit several simultaneous viscosity
Sliding Plate Microviscometer: tests under the same vacuum (Fig. 3(b)).
The sliding plate microviscometer was Vacuum System.—Vacuum capillary
used to determine the viscosity of as- viscometers require a vacuum source,
phalts at 77 F. This instrument and its such as a vacuum or aspirator pump.

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30 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

The vacuum system should be provided assure homogeneity of the sample. The
with a manometer and a satisfactory liquefied sample was poured into 3-oz
arrangement for adjustment and vacuum containers so that only one heating of
control. Vacuum can be controlled by the quart sample was necessary. The
the bleed valve or by the manostat con- 3-oz samples, after cooling, were stored
nected to the vacuum system, as shown until subsequent viscosity determina-
in Fig. 3(a). Another vacuum control tions were made. Duplicate or triplicate
device, marketed by the Cannon Instru- viscosity determinations were made on
ment Co., and shown in Fig. 3(6), is an each sample of the asphalt cement de-
automatically controlled manometer
pending on the phase of the cooperative
equipped with a movable metal probe
testing program. Thus, in the case of the
and electronic relay system. By moving
vacuum capillary method, since three
the metal probe up or down in the
manometer glass tube, the desired measurements at different length inter-
vacuum is pre-set. When the mercury vals on the capillary were made in each
column in the manometer rises and test, a total of six or nine measurements
touches the tip of the probe, the vacuum was obtained for each sample. When the
pump in the system is automatically other viscometers were used, two or
shut off. Such an arrangement accu- three measurements were made for each
rately controls and maintains the vacuum sampling of the asphalt cement.
in the system. Sample uniformity is most important.
This is particularly true for viscosity
Apparatus and Testing Procedures Used tests with the sliding plate microviscom-
for Tests Other Than Viscosity: eter. The use of a small sample cut from
Tests for penetration and softening the top layer of asphalt without reheat-
points, as well as thin film oven tests, ing and restirring the entire 3-oz sample
were performed by the cooperators. may introduce a substantial error in
Apparatus and testing procedures de- viscosity determinations.
scribed in ASTM and AASHO publica-
tions were used for these tests. TEST RESULTS

Sampling and Sample Preparation: Properties of Asphalt Cements Used in


The asphalt cements, usually received Different Phases of the Testing Pro-
in 1-qt containers, were heated in an gram:
oven at temperatures not exceeding 275 Five different asphalt cements were
F for the time period necessary to liquefy used in phases 1 and 3 of the coopera-
the material. During the heating, the tive testing program. Properties of these
asphalt was stirred intermittently to asphalts are tabulated as follows:

Testing Phase 1
Testing
Asphalt Phase 3

H F G E

P e n e t r a t i o n (100 g p e r 5 sec) a t 77 F 224 214 62 62 87


Softening p o i n t (ring a n d ball) 99 101 120 134 116.5
Specific g r a v i t y a t 77 F 1.008 1.013 1.009 1.006 1.021
Viscosity a t 140 F , poises 365 552 1660 8870 1750

N O T E . — A s p h a l t E exhibited a p r o n o u n c e d complex flow a t 140 F .

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G R I F F I T H AND PUZINAUSKAS ON EMPIRICAL T E S T S 31

Similar test data for the 63 asphalt 15 per cent. For asphalt E, complex
cements used in phase 2 of the testing flow behavior of this material among
program are shown in Tables I I and I I I . other factors may contribute to this dis-
All of these test data were obtained at crepancy. The reasons are not clear for a
the Asphalt Institute laboratory. similar discrepancy for asphalt F.
For asphalt cements, the precision
Repeatability and Reproducibility of Vis- limits for gravity flow viscosity instru-
cosity Measurements with Different ments are larger than for the vacuum
Viscometers: capillary viscometers. Such larger limits
Statistical results from test data ob- are indicated by both phases of testing.
tained in the first and third phases of the For high-viscosity asphalts, the repro-
cooperative testing program are sum- ducibility value for the Zeitfuchs cross-
marized in Table I. The analysis indi- arm instruments may be about twice
cates that the standard deviation of vis- that of vacuum capillary viscometers.
cosity values within a single laboratory Many factors may influence viscosity
or values from different laboratories values in a nonrandom manner. First,
increases as the viscosity of the asphalt most of the cooperators initially were in-
increases. This was true with all viscom- experienced in such testing. Second, the
eters used in the investigation except vacuum capillary viscometers in most
for the Cannon asphalt viscometer, where cases were manufactured and calibrated
the data are not sufficient to establish by the cooperators themselves, and some
such a trend. In general, variability be- factors may be traced to these sources.
tween or within the laboratories tends Also, certain sample preparation and
to be larger for gravity flow instruments handling procedures were not under
than for vacuum viscometers. proper control at all times. The influ-
The variability between laboratories ence of these factors is being investi-
generally is much greater than the varia- gated in the continuing studies.
bility within individual laboratories. After completing phase 1 and before
This indicates that certain factors asso- starting phase 3, sample preparation
ciated with the use of the instruments in and handling procedures were stand-
the different laboratories may influence ardized and improved. These improved
the viscosity values in a nonrandom procedures were used by the cooperators
manner. Because of this, it appears im- in the third testing phase. A comparison
practical to apply confidence limits to of the statistical analysis data as ob-
the test results. However, if 95 per cent tained on asphalt G in phase 1 with
confidence limits for the expected per- phase 3 data (both asphalts of approxi-
centage difference of two viscosity deter- mately the same viscosity) reveals that
minations are applied, repeatability of changes in test procedures influenced the
approximately 5 per cent and reproduci- test results only slightly. The accuracy
bility of 15 per cent could be suggested of the vacuum capillary viscometers was
for the asphalt cement viscosity meas- improved, while the accuracy of Zeit-
urements at 140 F with the Koppers fuchs cross-arm viscometers was ad-
vacuum capillary method. versely affected.
Phase 1 test results indicate that the The test results and the comments re-
reproducibility of high-viscosity asphalt ceived from different cooperators indi-
E and medium-viscosity asphalt F lies cate that vacuum capillary viscometers
outside the suggested reproducibility of are more adaptable to viscosity meas-

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32 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

urements of asphalt cements at 140 F ence, are tabulated below:


than are the gravity flow instruments.
Most comments also indicated difficul- Viscosity Range, poises
ties in cleaning, calibration, accurate
meniscus reading, and long flow times of Minimum Maximum
the gravity flow viscometers.
Sliding p l a t e micro-
viscometer 10 000 10 000 000
Viscosity of Asphalt Cements at Different V a c u u m capillary-. . . 50 50 000
Temperatures and Comparison of Vis- Zeitfuchs cross-arm . . 0.01 100.00
cosity with Empirical Test Properties:
The purposes of phase 2 of the testing These broad viscosity ranges are arbi-
program were (1) to establish the vis- trary and should be regarded only as a
cosity-temperature relationships for dif- rough guide for selecting a proper vis-
ferent asphalt cements, and (2) to com- cometer for a given viscosity.
pare viscosity characteristics with results Before actual viscosity measurement,
of empirical tests (penetration, softening the same sample preparation procedures
point, etc.). All tests for phase 2 were were used for all viscometers. Based on
performed by the Asphalt Institute replicate determinations, the following
laboratories. These test results are sum- approximate repeatability limits of the
test results as obtained by the Asphalt
marized in Tables II and III.
Institute laboratory for the individual
Temperature-Viscosity Relationship of viscometers could be indicated: Zeitfuchs
Different Asphalts.—Table II summa- cross-arm is ±1.5 per cent, vacuum capil-
rizes the viscosities of 63 asphalt cements lary is ±3.0 per cent, and sliding plate
at 77, 140, and 275 F. For comparison microviscometer is ±6.0 per cent of the
purposes, penetration values at 77 F are mean. These values represent the accu-
also included in this table. racy of viscosity tests at different tem-
Viscosities at 77 F were measured by peratures by one laboratory and, there-
the sliding plate micro viscometer. In all fore, should not be confused with the
these tests 50-/i film thickness was used. repeatability values shown in Table I.
At 140 F two Koppers vacuum capillary Since viscosities at different tempera-
viscometers were used (see Fig. 2(a)). tures were measured with relative ease,
One had a capillary radius of 0.01524 the viscosity test results (Table II)
cm, and the radius of the other was prove the advantage of viscosity meas-
0.05080 cm. At 275 F a single conven- urement over any currently used empiri-
tional Zeitfuchs cross-arm viscometer cal test. Such empirical tests are unable
of 1.0 constant (Fig. 1(a)) was sufficient. to indicate temperature-consistency re-
Selection of these instruments for meas- lationships for different asphalt cements
uring viscosity at the indicated tempera- between 77 and 275 F.
tures was based on the viscosity ranges In regard to the shear susceptibility
for which these instruments are con- of 63 asphalts listed in Table II, at 140
veniently adaptable. Such viscosity F the viscosities of only three increased
distinctly with decreasing shear rate.
ranges, in poises, as indicated in litera-
However, for the same group tested at
ture for different types of viscometers
77 F, the viscosities of 54 asphalts were
or based on previous laboratory experi- affected by the changes in the shear

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GRIFFITH AND PUZINATJSKAS ON EMPIRICAL TESTS 33

rate, the viscosities decreasing with in- perature relationship of six asphalt ce-
creasing shear rate. On this basis, it can ments plotted on a modified ASTM vis-
be assumed that all asphalts at 275 F cosity-temperature chart. A double
would behave rheologically as simple logarithmic scale for asphalt viscosity
liquids, that is, the viscosities would in poises and the logarithmic scale for
not be affected by the shear rate. It temperature, expressed in degrees Ran-
should be mentioned that with the slid- kine, are used as coordinates. The six

I0 7
2.5
I0 6 W . ASPHALT NO. 28
5
25
I0 5
5
2.5
I0 4
5
2.5 \ \ ASPHALT NO. 25

3
I0
7.5
5
o 2.5
0_
\ \ N ^ ^ ASPHALT NO O
I0 2
6
4

ASPh ALT NOS 9; 23, 41 ^ X .

I
70 77 140 275 290
TEMPERATURE,DEG FAHR
FIG. 4.—Viscosity-Temperature Relationship for Six Representative Asphalt Cements.

ing plate microviscometer it is possible asphalts were selected from the group
to obtain a somewhat broader range of of 63 asphalts (Table II) and represent
shear rate than with vacuum capillary the highest and the lowest viscosities at
viscometers. However, the range of shear three test temperatures (77, 140, and
rate of both instruments is relatively 275 F). Viscosity ranges thus represent
narrow and lies between 1.0 and 0.001 minimum and maximum viscosities for
sec -1 . Generally, viscosity changes within the 63 samples. For this plot, viscosities
these shear rate limits were small, and at 275 F were converted to poises by
it was apparent that such changes de- multiplying measured viscosities in
creased with increasing test temperature. stokes by the asphalt density at 275 F.
Figure 4 illustrates the viscosity-tem- Such corrections resulted only in small

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34 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

changes in the numerical viscosity perature normally attained by the sur-


values. A shear rate of 5.0 X 1CM recip- face layer of an asphalt pavement in
rocal seconds was used to plot viscosi- service, where the viscosity of the
ties of asphalt cements at a temperature asphalt binder contributes least to the
of 77 F. This shear rate is approximately strength of the pavement. In addition,
an average for both the sliding plate all paving asphalts behave essentially as
and Koppers vacuum capillary viscom- simple liquids at or above 140 F.
eters. Also since asphalt no. 25 was one A second temperature of 275 F is sug-
of the asphalts which showed complex gested for consideration since it is near
flow behavior at 140 F, viscosity of this the maximum normally reached during
asphalt at 5.0 X 10~2 reciprocal seconds construction operations. Viscosity of
was used. Thus, all viscosities shown in asphalt cements at 275 F may be meas-
this graph were determined at the same ured accurately and rapidly with existing
shear rate. gravity flow viscometers. When used in
Figure 4 indicates that differences in conjunction with a viscosity measure-
the viscosity of different asphalt cements ment at 140 F, the viscosity at any tem-
normally tend to increase as the tem- perature above 140 F may be determined
perature decreases. At 275 F, viscosities with accuracy by interpolation or ex-
of asphalt cements may vary from about trapolation, when plotted on a chart as
one to twelve poises. At 140 F, the vis- shown in Fig. 4. At temperatures below
cosity range lies between approximately 140 F, viscosities also can be extrapolated
250 and 9000 poises. At 77 F, this range from such a chart with reasonable accu-
varies from about 120,000 to 8,000,000 racy when the asphalts are known to
poises. The almost parallel lines, except have Newtonian or near-Newtonian
for asphalt no. 30, suggest that the properties at lower temperatures. How-
influence of temperature on the viscosity ever, in any specific case, the effects of
of different asphalts usually is quite shear rate on the viscosity of a majority
similar. In addition, the change in slope of asphalts should be considered. It
of asphalt no. 25 below 140 F should be should be noted that in regard to pave-
noted. This change in slope may indi- ment performance, the effects of differ-
cate a material often referred to as gel- ent shear rates remain to be determined.
type asphalt. The temperature-viscosity slope may
Temperature-viscosity data in Table be calculated by
II, plotted similar to that in Fig. 4, sug-
gest that viscosity at any temperature, log log 112 - log log m
or temperature-viscosity susceptibility,
of most cements could be predicted with
reasonable accuracy from a measure- YJ2 — viscosity in centipoises at Ri, and
ment of the viscosity at a single tem- rji = viscosity in centipoises at R\.
perature. However, as indicated in
Fig. 4, the viscosity of some asphalts Temperatures are expressed in deg Ran-
may vary differently with changing kine. Note that the negative values for
temperature. Thus a measurement of these slopes are indicative of direction
viscosity at two temperatures serves a only. The sign does not affect the nu-
useful purpose. There is reasonable merical magnitude.
justification for selecting 140 F as one The average slope for most asphalts
temperature for viscosity measurement shown in Table II is to approximately
since this is about the maximum tem- — 3.8. For asphalt No. 30, however, the

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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 35

slope is about —3.0 from 77 to 275 F.


For asphalt No. 25, the slope is about too
§0
7n |
- 3 . 8 above 140 F and about - 3 . 0 be- 60 \
50 ^*7r
low 140 F. 1i \ - ! M
::-i • - -

Comparison Between Viscosity and Q


«30
1- -
»; < • '
Empirical Test Properties of Asphalt 1 i' i
CO
\ ,«
] [v>
t

Cements.—In addition to determining SO ? o >. \ i


the viscosity of the 63 asphalt cements
0-
l ! v* > X
at different temperatures, penetration o '0 , \ 111 . J \
y
H i '
v
'
I 7
100 J
* '
< 6 \ t
70 _«^:: £ 5 - J A-
60 _J_ _L
0\J-Tet o 4
. \\ m
l
,
50
« 3 -- e ' • \\
40 ^ j» ^
5
«, 30 > - ~*~ \ m
ji:
o i ^ •V
2
\\ \
20 . i v\
to
. \\
\ l# 1
o iO 2 0 3 0 5 0 OO 200300500
Q.
10 PENETRATION AT 77 F, 100 GM, 5 SEC
v
i. 8 % x\ —
^ 7 \7
v
> \
FIG. 6.—Correlation Between Viscosity at
* X
J 140 F and Penetration at 77 F for Different As-
i~ 5 phalt Cements.
<
. 4
\ \
fn 3
o \ •\ i 100
\ ffi
\\ \ 60
\i f 50
40
\
1
O 20 30
_L50
DO 200 300 500
N <n
* 30
P
,
\
1

PENETRATION AT 77 F, 100 GM, 5 SEC CO

20
u_
FIG. 5.—Correlation Between Viscosity at
77 F and Penetration at 77 F for Different As-
phalt Cements. i- 10
.
1 X

at 77 F before and after thin film oven S fi : •F •<k


*\
R 5 I

test (TFOT) heating, and softening •


•f

> • 1
' .
point by the ring-and-ball method were 3 m
**^ 1 f mt
measured. For comparison purposes, i
2 '-.. * •<
viscosities at 140 F after TFOT heating ^ • * 1
• • *

and viscosities at the softening point V


*"*•*,

1 H/
temperature also were measured. Test 10 20 30 50 100 200 300 500
data are summarized in Table III. PENETRATION AT 77 F, 100 GM, 5 SEC
Viscosity Versus Penetration.—Fig- FIG. 7.—Correlation Between Viscosity at
275 F and Penetration at 77 F for Different As-
ures 5, 6, and 7 compare viscosity at 77, phalt Cements.
140, and 275 F, respectively, with the
original penetration at 77 F of the 63 85 to 100 penetration grade asphalts
original asphalts. These figures show the may vary approximately from 0.5 to
expected viscosity ranges for asphalt 1.6 million poises. Figure 6 indicates
cements of different penetration. Figure that at 140 F the viscosity range for this
5 indicates that at 77 F the viscosity of grade of asphalts varies between about

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36 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

600 and 3600 poises. At 275 F a viscosity range between about 70 and 170. At
range from 0.5 to 12 stokes is indicated 275 F, the range is between about 10
for this grade of asphalt (Fig. 7). and 200 penetration points for 5-stoke
Alternatively, if the penetration range viscosity as indicated on Fig. 7. Thus,
bOO 1• I
4
ORIGINAL ASPHALT HEATED ASPHALT
85/100 PEN. GRADE ASPHALTS •

ABOVE 85/100 PEN. GRADE a
? ^ °°J 0 > y- BELOW 85/100 PEN. GRADE
* a
v|.
\ CD
\ o

\\ i
a
r
B \ , i n *A 3 "
S N c• t e w * •
F fi S • -*. B

'~* • U
§ *> -* i r*» • •
4 "^^-^.^
t 4 V A- r i «•a! 1 6 "« •
z v ^« 4 a •fa i.
rr1 * V. 1
a
? ->•v •

10
3 4 56 8 10 2 3 4 56 8 O2 3 4 500

FIG. 8.—Effect of Thin Film Oven Test Heating on Viscosity and Penetration of Asphalt Ce-
ments.

80 LEGEND: | |
--. • 85/100 PEN. GRADE ASPHALTS
o ABOVE 85/100 PEN GRADE
70 • ^ - ^
i a BELOW 85/I0O PEN GRADE
rr
ui
a. •
o •• «
60 • 9 ^p>
%9 " " - ^ ^
o
< ^ • o
or o
• * * •
50 o » «

Q i o
o
o
^40 1 ^ - ^ o
1
0 100 200 300 400
30 VISCOSITY INCREASE OF ORIGINAL ASPHALT, PER CENT
FIG. 9.—Correlation Between Viscosity at 140 F and Penetration at 77 F of Asphalts Heated in
Thin Film Oven.

at constant viscosity is compared, simi- the penetration range at constant vis-


lar variations are observed. Figure 5 cosity, or viscosity at constant penetra-
indicates that asphalts having a viscosity tion, if expressed on per cent basis,
of 1 million poises at 77 F may vary tends to increase with the temperature
from about 75 to 105 in penetration. at which the viscosity is measured.
For asphalts of 1000 poise viscosity at Furthermore, Figs. 6 and 7 indicate
140 F, Fig. 6 indicates a penetration that at 140 and 275 F the dotted lines
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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 37

indicating viscosity-penetration ranges Comparison of Penetration and Vis-


tend to spread when extended in the cosity After the Thin Film Oven Test.—
direction of higher viscosity or lower To evaluate the effects of heating on the
penetration. At 77 F (Fig. 5), however, consistency of asphalts, penetrations at
these lines are essentially parallel. 77 F and viscosities at 140 F were deter-
While penetration at 77 F provides a mined for the 63 asphalts before and
rough indication of consistency at 77 F, after TFOT heating. These data are
the indicated correlation (Fig. 5) leaves summarized in Table III and compared
much to be desired. At 140 and 275 F this in Figs. 8 and 9. Table III indicates

25 c

co
UJ LE SEND:
CO • 85/100 PEN GRADE ASPHALT 3
o o ABOVE 85/100 PEN GRADE
9 BELOW 8 5 / O 0 PEN GRADE
Q. 20
UJ
CC 9
r>
H
<
UJ • 9
9
0_ • 9
UJ
15
I- • •• a
9

o
• 9 t
o
o
• «
• 9
a. 9
o° *| • /
r, C o

10'
• • • 99
o D O
o
o
cP
• ( I

o
°o o •
O 0
CO <s
I-
< O

>- o •
H •
co
o
o 0
co
95 105 115 125 135
SOFTENING POINT RSB.DEGFAHR
F r c 10.—Viscosities at Softening Point Temperatures of Different Asphalt Cements.

correlation becomes progressively worse. that (1) TFOT heating results in lower-
Poor correlation between penetration ing of penetration and increase in vis-
and viscosity may be attributed to cosity of asphalt cements and (2) as-
several factors. Differences in shear rates phalts which gain weight during heating
of these two tests may be considered as tend to be less heat susceptible than the
one of the principal reasons for such a asphalts which show weight loss when
poor correlation, especially at 77 F. In heated.
the case of the penetration test, the shear Figure 8 compares penetration at 77 F
rate is not controlled and changes gradu- and viscosity at 140 F before and after
ally during the testing. In the case of the TFOT heating for 63 asphalt cements.
viscosity tests, however, the value of This chart indicates that (1) the pene-
shear rate is known; it is either constant tration-viscosity relationship before and
or its value can be controlled. after TFOT heating remains essentially
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38 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

the same and (2) after heating the vis- softening points of the 63 asphalt ce-
cosities of higher-penetration asphalts ments were determined by the ring-and-
lie within narrower ranges than the ball method. Viscosities of these asphalt
viscosities of the low-penetration as- at softening point temperatures were
phalts. measured by the modified Koppers
A comparison of the test results in vacuum capillary viscometers. The test
Fig. 9 reveals that the penetration and results are summarized in Table I I I and
viscosity tests do not indicate changes of shown in Figs. 10 and 11.
similar magnitude after T F O T heating. In Fig. 10, softening point tempera-
For example, the group of 85 to 100 tures are plotted against viscosities of
penetration grade asphalts, after heating, asphalts at these temperatures. This
falls within a relatively narrow range of figure shows that the softening points of

w 20
tr
i-
<
rr
15
^ » a

I-

o i
no / °
f°°o ,
O
CO
I-
< LEGEND.
• 85/100 PEN GRADE ASPHALTS
o ABOVE 85/KX) PEN GRADE
s BELOW 85/100 PEN GRADE
CO
o
o I
CO

> VISCOSITY AT 140 F, POISES x 10 J


FIG. 11.—Relationship Between Viscosities at 140 F and Softening Point Temperatures for
Different Asphalt Cements.

approximately 40 to 60 penetration the asphalt cements are in the tempera-


units. On the other hand, the same group ture range of 100 to 135 F. (Asphalts
of asphalts initially ranging between nos. 45 and 46 were high-softening-
approximately 700 to 2800 poises, after point asphalts and are not included in
heating, range between 1100 to 11,000 this figure.) This figure also indicates
poises. The average increase in viscosity that within the softening point tempera-
for the whole group of asphalts is about ture range of 100 to 135 F, viscosities
threefold. Thus, it seems that viscosity of asphalts may vary between about 2000
measurements are considerably more and 20,000 poises. Examination of vis-
sensitive and accurate in the indication cosities at different rates of shear for
of heat susceptibility of different as- individual asphalts reveals that in this
phalts than are the penetration test group of 63 asphalts, 25 behaved as com-
values. plex liquids at the softening point tem-
Viscosities of Asphalt Cements at perature.
Softening Point Temperatures.—The The scatter of experimental points in
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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 39

Fig. 10 indicates that the softening point ments was suitable for the measurement
does not represent an equiviscous point of viscosity over the entire range of
for asphalt cements. Differences in temperatures to which asphalt cements
softening point temperatures and the are subjected during their application
change in shear rate during the softening and use.
point tests (shear rates are dependent 2. Three types of instruments—the
on temperature and consistency of sliding plate microviscometer, the vac-
asphalt) contribute to the random dis- uum capillary, and the gravity flow
tribution of the experimental points. viscometer—presently are required to
Figure 11 is similar to Fig. 10, except establish viscosity-temperature relation-
that in Fig. 11 viscosity at 140 F is com- ship of different asphalt cements over a
pared with viscosity at the softening relatively wide range of temperatures.
point temperature. In this figure, the However, the range of these instruments
distribution of the experimental point is inadequate for the measurement of
is considerably less random, and a gen- viscosity at temperatures near freezing.
eral pattern of increasing viscosities at 3. Asphalt cements normally used in
softening point temperatures with in- pavement construction usually behave
creasing viscosity at 140 F is evident. as simple liquids at 140 F and above.
This trend tapers off when viscosities of However, many of these asphalts be-
asphalts at 140 F reach about 15,000 have as complex liquids below this tem-
poises. The reason may be that at this perature. For these reasons, and because
viscosity the differences between soften- 140 F is normally the maximum tem-
ing point temperature and 140 F are perature reached by an asphalt pavement
small. The less random distribution of in service, consideration should be given
experimental points in Fig. 11 (as com- to classifying asphalt cements on an
pared with Fig. 10) further suggests
absolute viscosity basis at 140 F.
that viscosity is considerably more
4. Vacuum capillary viscometers ap-
suitable for measuring consistency of
pear to be the most suitable type now
asphalt cements than are empirical de-
available for measuring viscosity of
terminations such as softening point
asphalt cements at 140 F.
tests expressed in degrees Fahrenheit.
5. On the basis of the cooperative
SUMMARY AND CONCLUSIONS viscosity testing program test results
(phases 1 and 3), 15 per cent reproduci-
During the past two years, The As- bility and 5 per cent repeatability are
phalt Institute and its member com- suggested for the vacuum capillary vis-
panies have conducted a cooperative cosity test at 140 F. Other types of in-
viscosity testing program on a wide struments appear to be less precise.
range of commercially available asphalt
6. Viscosity measurements provide a
cements (1) to develop an accurate
means of measuring the consistency of
method for viscosity measurement of
asphalt cements in fundamental units
asphalt cements at 140 F and (2) to
over a wide range of temperatures. This
compare the consistency characteristics
of asphalt cements as measured by the is not possible with any of the empirical
conventional, currently used, empirical test methods now in use.
tests with consistency as measured by a 7. Heat susceptibility of asphalt ce-
fundamental viscosity test. Results of ments may be measured more accurately
the program collected to date lead to the by viscosity tests than by the currently
following tentative conclusions: used empirical tests.
1. None of the investigated instru- 8. Shear susceptibility of asphalt ce-
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40 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

ments tends to increase with increasing Thus, the empirical measurements, such
viscosity, decreasing temperature, and as penetration or softening point, are not
progressive heating. Within relatively suitable to indicate shear susceptibility
narrow ranges of shear, an indication of of asphalt cements.
such susceptibility may be obtained 10. The softening point does not
from viscosity measurements. represent the equiviscous point for
9. Variable and uncontrolled rates of different asphalts. Also, temperatures at
shear inherently are included in cur- softening point of paving-grade asphalt
rently used empirical test methods. cements tend to lie below 140 F.

REFERENCES
(1) E. O. Rhodes, E. W. Volkmann and C. T. (7) D. F. Fink and R. L. Griffin, "Measure-
Barker, "New Viscometer Has Extended ment of the Consistency of Paving Cements
Range," Engineering News-Record, Vol. at 140 F with the Sliding Plate Micro-
115, Nov. 21, 1935. viscometer," ASTM STP No. 309, Am.
(2) R. H. Lewis and W. J. Halstead, "Deter- Soc. Testing Mats., 1961, p. 79.
mination of the Kinematic Viscosity of
Petroleum Asphalts with a Capillary Tube (8) J. Y. Welborn and W. J. Halstead, "Ab-
Viscometer," Public Roads, Vol. 21, No. 7, solute Viscosity as a Specification Control
Sept., 1940, pp. 127-139. for Bituminous Binders," Public Roads,
(3) J. J. Heithaus, "Measurement of Asphalt Vol. 31, No. 12, Feb., 1962, pp. 243-247.
Viscosity with Vacuum Capillary Viscome- (9) P. R. Wood and H. C. Miller, "Rheology of
ter," ASTM STP No. 309, Am. Soc. Bitumens and the Parallel Plate Micro-
Testing Mats., 1961, p. 63. viscometer," Bulletin 270, Highway Re-
(4) R. L. Griffin, T. K. Miles, C. J. Penther, search Board, 1960, pp. 38-46.
and W. C. Simpson, "Sliding Plate Micro-
(10) F. H. Gaskins, J. G. Brodnyan, W. Philip-
viscometer for Rapid Measurement of
poff, and E. Thelen, "The Rheology of
Asphalt Viscosity in Absolute Units,"
Asphalt: Flow Characteristics of Asphalt,"
ASTM STP No. 212, Am. Soc. Testing
Mats., 1956, p. 36. Transactions, Soc. of Rheology, Vol. 4,
1960, pp. 265-278.
Partial Bibliography of Recent Articles: (11) R. N. Traxler, Asphalt—Its Composition,
(5) J. Huet, "Study on the Thermal Suscepti- Properties and Uses, Reinhold Publishing
bility of the Viscosity of Bitumens," pre- Corp., 1961, pp. 68-71.
sented at Third International Asphalt (12) H. Abraham, Asphalts and Allied Sub-
Congress, Paris, Oct., 1958. stances, Fifth Edition, Vol. 2, 1945, pp.
(6) W. J. Halstead and J. A. Zenewitz, 969-974.
"Changes in Asphalt Viscosities During (13) J. Ph. Pfeiffer, "The Properties of Asphal-
Thin-Film Oven and Microfilm Durability tic Bitumen," Chapter II, Rheological
Tests," Public Roads, Vol. 31, No. 11, Dec', Properties, by R. N. J. Saal, Elsevier Pub-
1961, pp. 211-218. lishing Co., Inc., 1950, pp. 49-76.

APPENDIX

M E T H O D OF T E S T FOR VISCOSITY OF PAVING ASPHALTS:


VACUUM CAPILLARY M E T H O D *

Scope: viscometer. I t is applicable to materials


having viscosities in the range of from 10
1. This method describes a procedure for
to 50,000 poises.
determining the absolute viscosity of as-
phalts by means of a vacuum capillary Method Summary:
* Methods described are now being recom- 2. The liquid is drawn up through a
mended in somewhat modified form by ASTM
Committee D-4 on Road and Paving for publi- capillary tube by means of a vacuum. T h e
cation as tentatives. velocity at which the liquid moves through
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GRIFFITH AND PUZINAUSKAS ON EMPIRICAL TESTS 41

S x

:<
,2 00
** a
S'>
* ca

IB O

S.t!

-*> o

>>
nj

Q.
rf
O
St B
i 3
>
Vac
306

C t4 -<o
03
l
el
iscome
)aratu

h-

T~J (wo gi) xavw


NOSiGIWi WTWINMI
<
s
X
> c
PPR

-WW Z2Z-

< an
1-
ID

UJ ^

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42 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

the tube is measured. The viscosity is a Sample Preparation:


function of the velocity of flow, the magni-
4. Heat the sample container in an oven
tude of the vacuum, and the dimensions of
controlled at 275 ± 10 F until the asphalt
the capillary. The rate of shear decreases as
is sufficiently fluid to pour into a viscosity
the liquid moves u p the tube; it can also be
tube. Occasionally stir the sample to aid
varied by changing the magnitude of the
heat transfer and assure thorough mixing.
vacuum. Thus, measurements can be made
At the same time, pre-heat the sample tube
on both Newtonian and non-Newtonian
in the same oven, or in an oil bath, controlled
materials.
at 275 F. Pour a required amount of fluid
Apparatus: asphalt through a pre-heated 40-mesh sieve
into a sample tube. (See Note 1.) Allow the
3. (a) Vacuum-Operated Capillary Vis- sample tube to remain for 10 ± 2 min in a
cometer.—The viscometer consists of a bath or oven at 275 F. (This pre-conditions
capillary tube attached to a ground glass the asphalt and allows air bubbles to escape.)
joint to fit the sample tube. A mark is ruled
on the capillary approximately 1 cm from NOTE 1.—Total elapsed time between intro-
the lower end, and additional exact gradua- duction of asphalt into the sample tube and meas-
tions are marked a t least 2 cm apart above urement of viscosity must not exceed 1 hr.
the first (see Fig. 12). Several viscometers
Test Procedure:
of varying bore should be available to permit
measurements over a wide viscosity range. 5. Remove the sample tube from 275 F
(b) Sample Tubes.—At least one for each bath or oven and allow to cool at room
capillary. T h e lower end of the glass capillary temperature for 4 to 6 min. Place the sample
should clear the sample tube by at least 2 tube in a 140 ± 0.2 F bath so that the tube
mm at all points. Sample tubes should be is immersed at least 15 cm below the surface
provided with holders enabling the place- of the bath liquid. Insert the capillary
ment of the tube in the constant temperature viscometer into the asphalt, and allow to
b a t h in a vertical position. stand for 25 to 30 min. During this time,
(c) Vacuum Source.—Such as vacuum or establish the desired vacuum by means of a
aspirator p u m p . vacuum or aspirator p u m p and the bleed
(d) Vacuum Control Apparatus (Op- valve. After 25 to 30 min open the viscometer
tional).—The Cartesian type Manostat to the vacuum system, thus causing the
(such as Emil Greiner Co., Catalogue No. asphalt to flow upward in the capillary.
G 1 5077) may be used. Time the passage of the liquid meniscus
(e) Manometer.—Mercury type having between one or more pairs of graduations
1-mm graduations is suitable. (preferably three). Record the vacuum and
(f) Constant Temperature Bath.—Con- the time of flow between chosen marks.
stant to ± 0 . 2 F and constructed so that the (See Note 2.)
viscometers can be easily observed and
having provisions for vertical positioning of NOTE 2.—The vacuum drawing asphalt
through capillary should be at least 10 cm of Hg.
the viscometers.
The measured flow time should be at least 50
(g) Viscosity Bath Thermometer.—A sec. Select a capillary of such size that these
total immersion thermometer of suitable conditions are fulfilled. In general, if there is a
range graduated to 0.1 or 0.2 F (0.05 or choice between two capillaries, use the smaller
0.1 C) and conforming to the general re- one.
quirements of A S T M Specification E 1 - 6 1 . 5
A S T M Saybolt viscosity thermometers and 6. The cleanliness of both the capillary
ASTM kinematic viscosity thermometers are and the sample tube is very important.
suitable. Clean both with hot high boiling point
aromatic oils or nitrobenzene followed by
5 acetone; then flush with warm dry air.
Specification for ASTM Thermometers
( E l - 6 1 ) , 1961 Book of ASTM Standards; Periodically (at least after e v e n ' five tests),
Part 4, p. 1423; Part 7, p. 1363; Part 8, p. 1741. the capillary viscometer and the sample

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G R I F F I T H AND PUZINAUSKAS ON EMPIRICAL T E S T S 43

tube should be washed with fresh chromic pairs of marks for each tube. These equations
acid cleaning solution. will be of the form:

Calculations: ahH
Viscosity = ———
bli + 1
1. (a) Calculate the viscosity from the
following equation: where:
6.7312 X 104.R2
3LWgm a =
~ l2Dh(.Li> - ii 2 ) + 8 </(£/ - Lfl i;3 - ii3
20.301 (H - ii 2 )
where: b = •
V = viscosity, poises, L? - W
D = density of mercury a t room tempera- Precision:
ture, g per cu cm,
8. (a) Repeatability.—Duplicate results
d = density of liquid, g per cu cm,
by the same operator should be considered
g = acceleration due to gravity, 980 cm
suspect if they differ by more than 5 per
per sq sec, cent of the mean value.
/; = manometer reading, cm Hg,
(b) Reproducibility.—Results on the
R = radius of capillary bore, cm,
same paving asphalt by different laboratories
/ = time required for liquid meniscus to
should not vary by more than 15 per cent
move from lower mark to upper mark,
of their mean value.
sec,
L\ = length from end of capillary to lower Calibration of Viscometer:
mark, cm, and
The viscometer is calibrated by measuring
L« = length from end of capillary to upper
the dimensions of the capillary tube.
mark, cm.
Measure the distance from the lower end of
Since the calculated viscosity is rela-
the capillary tube to each of the marks ruled
tively insensitive to variations in the density
on it with a micrometer microscope to the
of the liquid, for asphalt cements d may be
nearest 0.01 mm. These distances are the
set equal to 1.
values of L required in the equations in
Then, if D = 13.5339 g per cu cm and Sections 7(a) and 7(c).
g = 980 cm per sq sec, we have
Measure the radius of the capillary as
T 6.7312 X WWIiH follows: Place a small amount of clean
mercury in the capillary. Measure the length
~ 20.301//(i, 2 - i, 2 ) + (is 3 - ii 3 )
of the mercury column to the nearest 0.01
(b) When measurements have been made mm with a micrometer microscope. T h e
between more than one pair of marks and length of this column should be measured
the largest and smallest calculated vis- when the mercury is at several locations in
cosities do not differ by more than 10 per the tube. Record the temperature in the
cent of the mean value, average the cal- immediate vicinity of the capillary tube a t
culated values. the time these measurements are made.
(c) If the difference between the largest Weigh a clean weighing bottle to the nearest
and smallest calculated viscosities is greater 0.1 mg. Transfer the mercury to the weighing
than 10 per cent of the mean value, calculate bottle and weigh again to the nearest 0.1
the shear rate from nig. At least 10 mg of mercury should be
used in this procedure.
Shear rate (sec ') = Calculate the radius of the tube from
Rl
Report both the viscosities and the cor-
responding shear rates.
where:
NOTE 3.—It will usually be found convenient R = radius of capillary, cm,
to set up calibration equations for a number of M = weight of mercury, g,

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44 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

D = density of mercury at temperature of two marks between which the liquid menis-
measurement, g per cu cm, and cus is being timed.
L = length of mercury column, cm.
NOTE 4.—Calibration of viscometers as de-
In applying the equations for viscosity scribed above could be verified by determining
and shear rate, Sections 7(a) and 7(c), the viscosities of NBS standard viscosity oils
use the average capillary radius between the (such as oil P) at temperature at which the oil
lower end of the tube and the upper of the has been standardized.

DISCUSSION
1
M R . R. A. DUNLEAVY. —The author i r g r W f f - W<
.(1)
stated that some of the materials tested &LV
for viscosity were found to be non- where:
Newtonian in character. How was this 77 = absolute viscosity, poises,
factor taken into account in reducing and PHIS = density of mercury at room tem-
correlating the test data? perature, g per cu cm,
M R . V. P . PUZINAUSKAS {author).—In L = capillary length, cm,
the case of non-Newtonian asphalts, V = fill-bulb volume, cu cm,
viscosities a t a constant shear rate of 0.05 r = capillary radius, cm,
reciprocal seconds were used for com- g = acceleration due to gravity, cm
parisons such as shown in Fig. 4. per sq sec,
MR. R. E. MANNING 2 (presented in H = applied vacuum (or pressure), cm
written form).—The Cannon Instrument
Co. has been calibrating three types of h = average head of liquid sample,
vacuum viscometers discussed by Messrs. cm Hg, and
Griffith and Puzinauskas as being / = fill-bulb time, sec.
suitable for measuring the absolute For routine testing it is convenient to
viscosity of asphalt cements at 140 F. fix the applied vacuum (or pressure) at
While our experience indicates that the 30.0 cm Hg, and Eq 1 reduces to the
Cannon-Manning vacuum (or pressure) very simple
viscometer is the most accurate and
precise, the Asphalt Institute modifica- v = AV (2)
tion and the Koppers type can also be where A"i = the viscometer constant in
used with satisfactory results (see Fig. 2). poises per second.
The viscosity equations, however, have For research purposes it may be
been reexamined and simplified without desirable to vary the applied vacuum to
loss of accuracy. extend the range of the viscometer or
The Cannon-Manning vacuum (or study the effect of shear rates, and
pressure) viscometer allows absolute Eq 1 reduces to
viscosity measurement over the range of
0.06 to 80,000 poises, a range that allows v = K,(H - h)l. .(3)
the measurement of viscosity of both
where A"2 = viscometer constant in
asphalt cutbacks and cements at 140 F.
poises per cm Hg per sec.
The viscosity equation for the viscometer
The viscometer constants K\ and K2
is
are not dependent on temperature. ATi ,
1
Supervisor, Chemical and Physical Test of course, changes with applied vacuum
Dept., Thiokol Chemical Corp., Wasatch Div. but Kz does not.
Brigham City, Utah.
2
Technical Director, Cannon Instrument
Table IV shows standard sizes, ap-
Co., State College, Pa. proximate viscometer K\ constants, and
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DISCUSSION ON EMPIRICAL TESTS 45

TABLE IV.—STANDARD SIZES, APPROXIMATE K, CONSTANTS (H = 30.0


CM HG) AND VISCOSITY RANGES OF CANNON-MANNING VACUUM
(OR PRESSURE) VISCOMETER.

Approximate KL Constant, poise


per sec Viscosity Range, poise

Bulb C Bulb D

0.2 to 0.S 0.06 to 0.24


0.6 to 2.4 0.2 to 0.8
2 to 8 0.6 to2.4
0 to 24 2 to 8
20 to 80 6 to 24
60 to 240 20 to 80
200 to 800 60 to 240
600 to 2 400 200 to 800
2 000 to 8 000 600 to 2 400
6 000 to 24 000 2 000 to 8 000
20 000 to 80 000 6 000 to 24 000

recommended viscosity ranges for each head due to the hydrostatic head of the
size. liquid sample, it resulted in a significant
The viscosity equation for the error under certain conditions.
Asphalt Institute viscometer and the Rhodes et al (2) continued this work by
Koppers viscometer also reduces to a improving this viscometer and rederiving
simple equation, although some of the the equation to correct for the loss of
recently used equations for this type hydrostatic head:
viscometer are quite formidable. •n =
Pochettino (I)3 in his work in 1914 used
the following equation for the Koppers
vacuum viscometer: (5)
tfpH ;
+x •(k-h)
= HpBlHrH
V -(4)
4(V - h2) )-<•
where: where:
r = capillary radius, cm X = average height of the liquid from
h = capillary length to the first the bottom of the capillary to the
timing mark, cm outside meniscus, cm and
l-i = capillary length to the second p = density of liquid sample, g per cu
timing mark, cm cm.
/ = time for the meniscus to pass While accurate, this equation is too time-
from h to l2, sec, and consuming to solve to be of convenience.
pHK = density of mercury, g per cu cm. Accordingly, the natural log term was
Since the derivation of this equation did expanded by use of an infinite series
not take into account the loss of driving expression giving:
gr2pt
2 1 3
(6)
h - h h - h* U} - /i4
+

3
Since the denominator converges rapidly,
The boldface numbers in parentheses refer
to the list of references appended to this discus-
only the first two terms are normally
sion. used. By using two constants and a
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46 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

given pair of timing marks, Heithaus and calculated the degree of agreement
(3) shows this equation to reduce to the between their Eq 9 and Eq 6.
form: Each of these six equations is either
am approximate or too complicated for
•n = (l)
bH + 1 convenient use.
However, the viscosity equation can
With assumptions, Rhodes et al (2) be derived in a manner similar to Eq 4,
simplified Eq 6 to
by replacing the applied vacuum H by
•n = (ell - d)rH (8; the average driving force, (H — h), thus
while Lewis and Halstead (4) simplified giving
Eq 6 to the equivalent of gprHeKH - h)t
.(10)
V = (K'H + pa.C)l (9) 4(/22 - m '

TABLE V.—AGREEMENT OF VISCOSITY EQS 5 AND 13 FOR THE ASPHALT


INSTITUTE AND KOPPERS VACUUM VISCOMETERS.

Viscosity Equation, poises


per sec
Difference,
per cent
Eq 13 Eq5
" - K, 1
I

H - 3 . 0 0 cm H g U = 1.0
2.976 2.980 0.1
X = 0 . 5 cm h = 3.0

p = 1.00 g per cu cm U = 3.0


1.416 1.417 0.1
Pile ~ 13.534 g per cu cm h = 5.0

h = 5.0 0.8938 0.8942 0.0


It = 7 . 0

H = 3 0 . 0 cm H g h = 1.0
30.96 30.96 0.0
X = 0 . 5 cm h = 3.0

p = 1.00 g per cu cm 2i = 3 . 0 15.41 15.41 0.0


p H e = 13.534 g per cu cm /» = 5 . 0

h = 5.0 10.22 0.0


10.22
h = 7.0

TABLE VI.—RECOMMENDED STANDARD SIZES OF THE ASPHALT


INSTITUTE AND KOPPERS VISCOMETERS.

Viscometer Constant, Kt, poises per sec,


II = 30.0 cm Hg
Capillary Viscosity Range, poises
Size Radius, cm Fill-time 100 to 400 sec
h = 1.0 cm 3.0 cm 5.0 cm
h = 3.0 cm 5.0 cm 7.0 cm

N o . 12 0.0063 0.50 0.25 0.17 17 to 200


N o . 25 0.0125 2.0 1.0 0.7 70 to 800
N o . 50 0.025 8.0 4 3 300 to 3 200
N o . 100 0.050 32 16 10 1 000 to 12 800
N o . 200 0.100 128 64 40 4 000 to 52 000

Copyright by ASTM Int'l (all rights reserved); Thu Dec 22 07:49:02 EST 2011
DISCUSSION ON EMPIRICAL TESTS 47

where h is the average hydrostatic head upon to closer than 5 per cent. Calcula-
of the sample whose viscosity is being tion of Ki by instrument dimensions
determined with the unit of centimeters may involve such errors as the capillary
of mercury. More exactly, h can be being elliptical instead of round, and the
shown to be effective length of capillary should in-
'VZi2 + li p
clude the "Couette" corrections, and
h = .(ID some term for the length of the leading
PHg
edge of the meniscus.
For a given viscometer and pair of timing The data in Table V show excellent
marks, Eq 10 reduces to agreement between the very simple Eq
r, = K3(H - h)t. .(12) 13 and the more complex Eq 5. Note
that the difference in results is 0.1 per
The Cannon Instrument Co. recom- cent or less.
mends that for use in a standard test
Since the Koppers viscometer has not
method, the applied vacuum be specified
had standard sizes and recommended
as 30.0 cm Hg, in which case, since the
viscosity ranges, they are recommended
effect of the density of liquid is small,
in Table VI.
absolute viscosity is given by the simple
expression We believe the Cannon-Manning
vacuum viscometer is best for this work.
v = K4 (13) But for those who wish to use either of
where K4 is the viscometer constant in the other two types, standardization as
poises per second. The viscometer can indicated in Table VI will reduce con-
be calibrated by the use of viscosity fusion, and the use of a constant applied
standards; Ki can also be calculated, as vacuum of 30.0 cm Hg and the simple
has been done in the past, but this Eq 13 will greatly simplify the procedure
calculated value should not be depended for the calculation of absolute viscosity.

REFERENCES
(1) Pochettino, Nuovo Cimenlo, Serie 6, Vol. 8, (4) R. H. Lewis and VV. J. Halstead, Public
No. 2, 1914, pp. 77-108. Roads, Vol. 21, No. 7, 1940, p. 127.
(2) E. O. Rhodes, E. W. Volkmann, and C. T. (5) V. P. Puzinauskas, The Asphalt Inst., Col-
Barker, Engineering News-Record, Vol. 115, lege Park, Md., Private Communication.
1935, pp. 714-718. (6) M. R. Cannon and R. E. Manning, "New-
(3) J. J. Heithaus, "Measurement of Asphalt High Shear Viscometers and New Vacuum
Viscosity with a Vacuum Capillar}- Vis- Viscometers for Viscous Materials," Private
cometer," ASTM STP No. 309, Am. Soc. Report. Free copies are available from
Testing Mats., 1961, p. 63. Cannon Instrument Co., State College, Pa.

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STP328-EB/Apr. 1963

T H E R E L A T I O N OF ABSOLUTE VISCOSITY OF ASPHALT B I N D E R TO


STABILITY OF ASPHALT M I X T U R E S

B Y J. Y. WELBORN, 1 W. J. HALSTEAD, 1 AND R. E. OLSEN 1

SYNOPSIS

Several investigations have correlated various consistency measurements


with stabilities of asphalt paving mixes. However, because of the experi-
mental variations encountered and the time-consuming tests required to se-
cure complete information, the quantitative relationship of viscosity to
compressive strength for mixtures of various types has not been specifically
established. In addition to generally reviewing the literature, this paper re-
ports the results of a study of the relationship of absolute viscosity to com-
pressive strength tests for several asphalts from different sources and at
different temperatures. Most comparisons have been made on the basis of the
viscosity of the asphalt recovered from the strength-test specimen.

The major goal of the asphalt paving penetration grades of asphalt as the
technologist is to design asphalt paving binder for paving mixtures for use under
mixtures that will have (1) strength to specific conditions of traffic and weather.
resist displacement of the asphalt pave- Initially the grade of asphalt was
ment in the form of shoving or rutting selected on a trial and error basis. The
under traffic and (2) flexibility, skid lower penetration materials were used in
resistance, and durability. Many re- warmer areas and for heavier traffic,
search studies have evaluated such fac- and the higher penetration asphalts were
tors as (1) the type, quality, and grada- used in colder areas and for lighter
tion of aggregates and (2) the character traffic.
and amount of bituminous binder and During the 1930's, the great amount of
construction variables that affect the cracking found in pavements precipitated
quality and performance of the pave- a trend towards the use of softer, or
ment. higher penetration, asphalts in sheet
In the United States, the consistency asphalt and asphalt concrete construc-
of the asphalt binder in paving mixtures tion in many areas of the country. Since
has always been an important variable that time laboratory stability tests have
affecting performance. The penetration come into general use for designing
test and other empirical consistency paving mixtures. With these tests the
measurements were developed, and it is researcher and engineer have developed
common practice to specify certain a much better knowledge and under-
1 standing of the properties of aggregates,
Chief of Bituminous and Chemical Branch,
Supervisory Chemist, and Research Engineer, mineral fillers, and bituminous binders
respectively, Physical Research Div., Bureau of that influence the stability of various
Public Roads, U. S. Dept. of Commerce, Wash-
ington, D. C. types of paving mixtures.
48

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WELBORN ET AL ON STABILITY MEASUREMENTS 49

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50 SYMPOSIUM OX FUNDAMENTAL VISCOSITY

Several research studies show the properties of highway asphalts produced


effect of asphalt consistency on labora- in the United States reported by the
tory stability. Although these studies Bureau in 1959 and 1960 (i,2).2 Table I
generally agree with respect to the shows the sources, methods of refining,
qualitative relationships involved, the and some of the more important physical
quantitative effects of type and grada- characteristics of the asphalts as given in
tion of aggregates and consistency of the the earlier reports. The same identifica-
asphalt binder on stability are not well tion number used in these reports for
defined. Consistency as measured by each sample has been used in this report
penetration and viscosity have been to permit convenient cross reference.
used in the various studies. Some authors Table II shows the composition of the
state that for a given mixture there selected 85 to 100 penetration asphalts
should be no difference in stability when and changes in composition during aging
asphalts of the same consistency are tests as determined by Rostler and White
used. However, others report that prop- and reported in their paper presented at
erties of the binder other than con- the 1962 meeting of the Association of
sistency have a significant effect on Asphalt Paving Technologists (3). The
stability. No specific information was composition shown is based on the
found that showed the relative effect of Rostler-Sternberg method in which the
asphalts of different viscosity-tempera- asphaltenes are first precipitated with
ture or shear susceptibility characteristics normal pentane and then the dissolved
in mixtures made with different aggre- fractions are treated successively with
gates where internal friction varied sulfuric acid of specified strength.
widely. The series of Texas asphalts (samples
The study reported here was under- 154, 69, and 226) are 60 to 70, 85 to 100,
taken to determine the effect of viscosity and 120 to 150 penetration grades from
on the stability of pavement mixtures as the same producer and represent the
measured by laboratory test. No attempt most temperature-susceptible materials
was made to correlate the test data with found in the previous studies where three
characteristics of the pavement in place, grades were available. Some 85 to 100
but the relative effects indicated should grade asphalts from California sources
serve as valuable criteria for further have lower Furol viscosities at 275 F than
studies on the design of mixtures in the does sample 69, the 85 to 100 material
laboratory and for predicting the per- in this series, but the difference is not
formance of asphalt pavements in large. The series of Mexican asphalts
service. (samples 121, 3, and 196) are 60 to 70,
Summaries of some of the more im- 85 to 100 and 120 to 150 penetration
portant research reports on the subject grades and represent the materials with
are given in Appendix I and are arranged the lowest viscosity-temperature suscep-
in approximate chronological order to tibility tested in the earlier study. The
provide a general picture of the develop- other four asphalts selected for this
ment of knowledge concerning the basic study were of the 85 to 100 grade. Sam-
relationships involved. ple 13, a Venezuelan material, is typical
of much of the asphalt used on the East
MATERIALS USED Coast. Sample 38, a Mid-Continent
The asphalts used for the tests re- material, is highly resistant to hardening
ported here were selected from the 2
The boldface numbers in parentheses refer
group included in the studies of the to the list of references appended to this paper.

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WELBOEN ET AL ON STABILITY MEASUREMENTS 51

in both the microfilm and thin-film tests so that their behavior should provide a
(4). This material showed a relatively general cross-section of all types of
high shear susceptibility. Sample 56 materials encountered with commercial
was also shown to have high shear grades of asphalts.
susceptibility and low ductility of the The aggregates used in this study were
thin-film residue (4). Rostler and White selected to give mixtures of three distinct

T A B L E I I . — C O M P O S I T I O N O F 85 T O 100 P E N E T R A T I O N ASPHALT."
c
Compositior
A' + Ai Durability
Asphalt Condition6
P+ At Rating
A .V A, A, P

No. 3 Original 30.7 16.0 20.6 23.7 9.0 1.12 2


Mixed 34.3 16.9 18.1 22.2 8.9 1.14
Aged 36.0 18.3 16.2 21.5 8.0 1.17

No. 13 Original 28.8 22.5 23.0 18.9 6.8 1.77 5


Mixed 32.0 23.5 18.5 19.1 6.9 1.61
Aged 36.0 24.8 17.1 15.5 6.6 1.90

No. 38 Original 20.3 18.4 23.8 24.8 12.7 1.13 2


Mixed 24.6 16.2 21.9 26.7 10.6 1.02
Aged 30.2 16.5 19.7 23.8 9.8 1.08

No. 56 Original 20.3 12.1 21.0 30.8 15.8 0.71 1


Mixed 22.7 12.4 21.3 29.7 13.9 0.77
Aged 25.0 11.9 14.8 34.7 13.6 0.55

No. 69 Original 21.0 14.6 23.9 31.0 9.5 0.96 7


Mixed 22.7 20.4 23.0 24.4 9.5 1.28
Aged 25.7 20.7 27.5 26.8 9.5 1.05

N o . 100 Original 33.4 21.7 23.1 13.2 8.6 2.06 7


Mixed 55.6 21.7 19.7 16.3 6.7 1.80
Aged 41.8 20.7 16.5 14.1 6.9 1.87

" T a k e n from p a p e r b y Rostler a n d W h i t e presented at meeting of Association of Asphalt P a v i n g


Technologists, N e w Orleans, La., F e b r u a r y , 1962.
b
Original = as received.
Mixed = after mixing with O t t a w a sand 6 min at 325 F .
Aged = after aging 7 d a y s a t 140 F .
c
Composition d e t e r m i n e d b y Rostler-Sternberg m e t h o d :
A = asphaltenes
N = nitrogen base resins
A\ = first acidaffins
Ai = second acidaffins
P — paraffins

(3) reported that this material had types with widely varying stability
excellent abrasion resistance as measured characteristics. These are identified
by their test although field performance as sand, gravel, and stone mixtures.
records of a similar asphalt showed poor The aggregate for the sand mixture was
service. Sample 100 was a California a blend of concrete and sheet asphalt
asphalt, with a relatively high loss and sands and limestone dust. For the gravel
low percentage of retained penetration mixture, the aggregate was composed of
in the thin-film test. These asphalts uncrushed gravel, natural sand, and
have sufficiently different characteristics limestone dust. The aggregate for the

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52 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

stone mixture was entirely crushed stone content of the mixtures given in the
including the material passing the No. table are also averages of the group of
200 sieve. The compositions of the sand, specimens tested.
gravel, and stone mixtures are shown in Figure 1(a) shows the effect of tem-
Table III together with the aggregate perature on compressive strength of the
gradations. three types of mixtures containing
asphalts 3 and 69. Although these are
TABLE III.—COMPOSITION AND GRAD- both 85 to 100 penetration grade, they
ING OF AGGREGATE M I X T U R E S .
represent the extremes of temperature
susceptibility of the asphalts included
Per Cent of Total
in this study.
Aggregate As expected, there was a large differ-
Aggregate ence in strength of the three types of
Sand
Asphalt Gravel Stone mixtures, especially at the higher tem-
Mixture Mixture Mixture
peratures. For example, at 120 F the
R e d Hill g r a n i t e 100
sand mixture for asphalt 69 had a
M a s s o p o n a x gravel 58 strength of 8 psi, the gravel mix a
P o t o m a c River s a n d . . . . 36 strength of 32 psi (interpolated), and
W h i t e M a r s h concrete
60 the crushed stone mix 102 psi. At lower
P o t a m a c R i v e r sheet a s - temperatures the differences were less
38.5 pronounced. The strength at 60 F for
Limestone dust 1.5 6
P e r cent a s p h a l t (ag- asphalt 69 was 327 psi for the sand
gregate basis) 8.5 6.0 6.0 mixture, 440 psi (interpolated) for the
gravel, and 486 psi for the stone mixture.
Gradation of Aggregates Differences in the compressive strength
Sieve Size Per Cent Passing
of mixtures containing asphalt 3 were
about the same order of magnitude.
Hin 100 Note the flatter slope of the plotted line
90 100 for the crushed stone mixtures. This
No. 4 100 62 82
N o . 10 90 42 36
reflects the greater interlocking or
N o . 20 72 32 internal friction present in the crushed
N o . 40 52 19 13 stone aggregate.
N o . 80 17 9 9
N o . 200 4 6 4 The same type of aggregate mixtures
made with asphalts of the same pene-
tration grade but from different sources
VARIATION OF COMPRESSIVE STRENGTH
also had significantly different compres-
WITH TEMPERATURE
sive strengths. The differences in strength
Results of the compressive strength resulting from differences in asphalt
test on specimens 3 in. in diameter and source were greatest with the sand
3 in. high at various temperatures and mixture and least with the stone mixture.
using each of the aggregates with each For example, the strength of the sand
asphalt are shown in Table IV. The mixture at 120 F containing asphalt 3
details of mixing, molding, and testing was 2.6 times the strength of a similar
these specimens are given in Appendix II. mixture containing asphalt 69. At this
The compressive strength reported for temperature, the ratios of the strengths
each asphalt at each test condition is of the gravel and stone mixtures were
the average of four individual specimens. 1.8 and 1.3, respectively for the same
The bulk specific gravity and the voids two asphalts.

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WELBORN ET AL ON STABILITY MEASUREMENTS 53

The variation in compressive strength but differ significantly in slope from the
with temperature for gravel aggregate curves for mixtures made with cor-
mixtures made with asphalts from the responding grades of asphalt from a
same source but different penetration different source.
grades is shown in Fig. 1(b). The data The relative position of the curves
plotted are for the mixtures containing for the mixtures containing 60 to 70

T A B L E IV.—COMPRESSIVE S T R E N G T H S OF M I X T U R E S M A D E WITH
D I F F E R E N T ASPHALTS AND AGGREGATES.

Compressive Strength, psi


Type of Bulk, Air
Asphalt Aggregate" specific Voids,
gravity per cent At At At At At At At At
40 F 59 F 60 F 82 F 95 F 100 F 120 F 140 F

No. 154 Gravel 2.255 7.4 1228 585 205 90 22

No. 69 Sand 1.939 18.2 708 327 33 8


Gravel 2.256 7.3 1084 469 440 c 166 90' 71 32« 16
Stone 2.365 8.1 1383 486 169 102

No. 226 Gravel 2.251 7.7 774 327 130 48 11

N o . 121 Gravel 2.275 6.7 999 547 252 136 50

No. 3 Sand 1.953 17.7 558 273 55 21


Gravel 2.272 6.7 785 396 390 c 192 125< 106 59 e 38
2.380 7.4 959 411 193 133
Stone
No. 196 2.270 6.9 676 320 146 75 23
Gravel
No. 13 1.955 17.4 298 48 14
Sand 2.273 6.2 428 122 54
Gravel 2.383 7.3 448 177 123
Stone
No. 38 Sand 1.944 17.3 256 38 12
Gravel 2.263 6.2 362 110 46
Stone 2.355 7.6 382 188 122

No. 56 Sand 1.941 17.2 249 72 29


Gravel 2.267 6.4 366 139 78
Stone 2.372 7.2 381 198 140

N o . 100 Sand 1.958 17.2 324 56 18


Gravel 2.272 6.4 451 132 58
Stone 2.383 7.3 554 197 130

" See T a b l e I I I for grading a n d composition of mixtures,


b
E a c h value is a n average of results for four test specimens.
c
I n t e r p o l a t e d values

60 to 70 and 120 to 150 grades of the grade Texas asphalt (sample 154) and
Mexican and Texas asphalts, represent- those containing the 120 to 150 grade
ing the extremes of temperature-suscep- Mexican asphalt (sample 196) are of
tibility. The curve for mixtures made interest. These mixtures had approxi-
with the 85 to 100 Mexican asphalt is mately the same strength at 140 F, but
also included for comparison. As shown, at 40 F the strength of the mixture con-
the curves for different grades from a taining sample 154 was almost double
given source are substantially parallel that for sample 196. On the other hand,

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54 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

the mixtures with sample 3 (85 to 100 of compaction of the laboratory speci-
grade Mexican asphalt) and sample men and the percentage of asphalt also
226 (120 to 150 grade Texas asphalt) would influence the strength relationships
had the same strength at 40 F but widely obtained with each mixture composi-
different strengths at 140 F. These tion.

l.OVAJ

800

200

2
O

30 40 50 60 70 80 90 100 MO 120 130 140


TEMPERATURE, deg Fahr

(a) Different aggregates and asphalts.


FIG. 1.—Relation Between Log Strength and Temperature.

comparisons illustrate the effect of the VARIATIONS OF COMPRESSIVE STRENGTH


temperature susceptibility of asphalts WITH VISCOSITY
on mixture strengths. To show the extent to which the
The general relations shown in Fig. 1 differences in laboratory stability of
are well known from the qualitative bituminous mixtures can be attributed
standpoint and will be exhibited by all to differences in viscosity of the con-
types of mixtures, but the amount of tained asphalt, the asphalts were re-
change in strength will differ and will covered from test specimens representing
depend on both the asphalt character- each type of mixture and their viscosities
istics and differences in aggregate such were determined at several temperatures.
as grading, particle shape, etc. The degree The viscosities of the original asphalts

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WELBORN ET AL ON STABILITY MEASUREMENTS 55

were also determined over the same ture chart using the ASTM coordinates.
temperature range to measure the hard- The basis for this chart is log-log vis-
ening that occurred during the prepara- cosity in centistokes, which is essentially
tion and testing of the specimens. equivalent to centipoises for these ma-
All viscosities were determined with terials, plotted against log of absolute
the sliding plate microviscometer. This viscosity in degrees Rankine (deg

L s-
r\\, v
.X
rx^x D - 7 0 G =!ADE ( 1 !
NN . x^

Vs
.. V X V — 6 0 - 7 0 G )A0E (121)
Vs.
V xx >. X.
I2C - 1 5 0 GR ADE (196)
\
\ 1. • XX . \ s - 8 5 - 1 0 0 GRADE (3)
\ X
N . 'i
120-150 GRADE ( Z 2 6 ) - ^ \

\v
N^-
rX>

NS NX ^
l X
> \
X
-,
*%J
>NX
N
X
x

30 40 50 60 70 80 90 100 110 120 130 140


TEMPERATURE, deg Fahr

(6) A s p h a l t s of different grades.


F I G . 1.—Conlinusd.

instrument has been adequately de- Fahr + 459.7). The viscosities reported
scribed elsewhere (14,15). Determinations in Tables V and VI are values extra-
for each material were made at four tem- polated or interpolated from the plotted
peratures covering the normal working lines based on the best straight line
range of the instrument. While there were through the determined data points.
some exceptions, most of the determina- Such extrapolated values may not be
tions were made at 60, 77, 95, and 110 F. exact for the upper and lower tempera-
All viscosities were computed on the basis tures (120 or 140 and 40 F) but they
of a shear rate of 0.05 sec""1. These data are sufficiently precise for the purposes
were then plotted on a viscosity-tempera- of this study.

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56 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

The data in Table V for the 85 to 100 different. The greatest difference found
grade penetration asphalts include vis- was with asphalt 38. The material recov-
cosities of the original asphalts and the ered from the sand mix with this asphalt

TABLE V.—VISCOSITY OF ORIGINAL AND RECOVERED ASPHALTS AT


VARIOUS TEMPERATURES (85 TO 100 GRADE).
Viscosit; a, poises
Test
Asphalt Temper-
ature, Source of Recovered Asphalt
deg Fahr Original Asphalt,
poises
Sand Mixture Gravel Mixture Stone Mixture

No. 3 40 1200 X 10 5 1900 X 10 5


59 87 200
60 83 200 X 10 5 200 X 10 5
77 11 34 30 28
82 5.2 18
95 1.3 4.7 3.9
100 0.85 3.4
120 0.15 0.55 0.39
140 0.033 0.18

No. 13 60 110 170 150 170


77 12 24 21 22
95 2.3 3.0 2.4 2.7
120 1.8 0.30 0.24 0.24

No. 38 60 100 150 150 130


77 12 29 21 19
95 1.3 3.3 2.0 2.3
120 0.13 0.40 0.20 0.16

No. 56 60 80 130 190 160


77 17 38 37 37
95 2.1 6.5 4.6 6.3
120 0.34 0.70 0.68 0.93

No. 69 40 5200 12 000


59 180 320
60 160 300 260
77 10 29 21 26
82 5.7 11
95 1.1 2.6 2.7
100 0.66 1.0
120 0.083 0.18 0.20
140 0.015 0.021

N o . 100 60 110 240 230 220


77 12 31 24 33
95 1.9 3.8 3.5 3.9
120 0.19 0.33 0.36 0.35

• Shear rate 0.05 sec 1.

asphalts recovered from mixes made with had approximately twice the viscosity at
each of the aggregates. All of the recov- 120 F as material recovered from the
ered asphalts had higher viscosities than other aggregate mixes, but at 60 F the
the original asphalt and generally the viscosities for all three recovered asphalts
viscosity increase occurring with each were essentially the same.
type of aggregate was not significantly Table VI shows the data for both the

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WELBORN ET AL ON STABILITY MEASUREMENTS 57

original and recovered asphalts for the plotted against the logarithm of the vis-
90 to 70 and 120 to 150 grades. Asphalts cosity of the recovered asphalt at the
of these grades were recovered from only same temperature. Regardless of the
the gravel mixtures. source or penetration grade of the asphalt
Table VII compares the penetrations used, the data points fall on three distinct
of the original and recovered asphalts at curves, one for each type of aggregate
77 F. The penetration data provides a mixture. The influence of the aggregate
more familiar evaluation of the hardening system in the mixtures is again illustrated

TABLE VI.—VISCOSITY OF ORIGINAL AND RECOVERED ASPHALTS AT


VARIOUS TEMPERATURES (60 TO 70 AND 120 TO 150 GRADES).

60 to 70 Grade 120 to 150 Grade


Test
Temper-
ature, Viscosity," poises Viscosity," poises
deg Fahr Asphalt Asphalt
Original Recovered6 Original Recovered6

40 No. 121 3400 X 10 s 3500 X 10 5 No. 196 610 X 10 5 3300 X 10 5


59 No. 121 290 360 No. 196 46 110
77 No. 121 31 56 No. 196 5.8 13
82 No. 121 13 36 No. 196 2.3 6.9
100 No. 121 2.0 6.8 No. 196 0.44 1.1
140 No. 121 0.063 0.36 No. 196 0.017 0.042

40 No. 154 12 000 24 000 No. 226 1600 5800


59 No. 154 390 690 No. 226 67 140
77 No. 154 23 48 No. 226 3.5 8.8
82 No. 154 11 22 No. 226 2.4 4.6
100 No. 154 1.3 2.1 No. 226 0.31 0.42
140 No. 154 0.025 0.044 No. 226 0.0078 0.0085

" Values for shear rate of 0.05 sec 1.


6
Asphalt recovered from gravel mixture.

occurring during the mixing and curing TABLE VII.—COMPARISON OF PENE-


TRATION OF ASPHALTS RECOVERED
of the various specimens and show that FROM TEST SPECIMENS WITH PENE-
the increase in consistency as measured TRATION OF ORIGINAL ASPHALTS.
by the penetration at 77 F is equivalent Penetration, 100 g, 5
to approximately a one grade change in sec, at 77 F
penetration. For the 85 to 100 grade ma-
Source of Recov-
terials, the original penetration at 77 F Sample Grade ered Asphalt
Origi-
varied from 78 to 92. Sample 56, which nal
As-
had a penetration of 78, was out of grade.
Gravel

phalt
Mix

Mix
Mix

Stone
Sand

The recovered asphalts varied in pene-


tration from a low of 53 (sample 69, sand
mix) to a high of 70 (sample 38, stone No. 3 85 to 100 92 61 63 63
No. 13 85 to 100 88 62 66 65
mix). Generally, the hardening during the No. 38 85 to 100 89 63 68 70
mixing and curing of the sand mixtures, No. 56 85 to 100 78 54 61 57
No. 69 85 to 100 88 53 61 56
as measured by penetration at 77 F, was No. 100 85 to 100 90 54 59 58
greater than that for the gravel and stone No. 121 60 to 70 66 47
mixtures. No. 154 60 to 70 61 43
No. 196 120 to 150 127 91
In Fig. 2(a), the logarithm of the com- No. 226 120 to 150 145 89
pressive strength at each temperature is

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58 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

IO 3 io4 io5 io6 io7 io8 io9 IO1


VISCOSITY, POISES
(a) Log viscosity.

VISCOSITY, POISES

(6) Log-log viscosity.


FIG. 2.—Relation Between Log Strength and Viscosity of Asphalt.

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WELBORN ET AL ON STABILITY MEASUREMENTS 59

by the different level and slope of the gravel mixture. The data for the stone
curves. Although there is some curvature mixture was less definite, but it is be-
in the plotted lines, small segments can lieved that strength values at higher vis-
be considered to be straight and the cosities than obtained in this study would
slopes of such segments can be used to show this trend.
indicate the ratio of change in strength to Others have studied the relation of
change in viscosity. Examination of these asphalt viscosity to laboratory stability,
slopes in the range of viscosity from 10" and some have indicated that a straight
to 106 poises, which is approximately line results when log strength is plotted
equivalent to viscosities at summer tem- against log-log viscosity. Summaries of
peratures, show that a 10-fold increase in three studies using this relation are in-

1,5001 1 1 1—

1,000
3 S69 GRAVE L~\S

150
56-GRAVEL-
100

^3-SAN [
50
/T^-( 9-SAND
30

15

10

7
10 10 10 10 10 10

VISCOSITY, POISES

FIG. 3.—Relation Between Log Strength and Log-Log Viscosity of Selected Asphalts.

viscosity produces approximately a 3.2- cluded in Appendix I. These are reports


fold increase in strength for the sand mix- by Weetman and Hurlburt (7), Neppe
ture, a 2.4-fold increase for the gravel (8), and Wood and Goetz (9). To examine
mixture and a 1.5-fold increase for the this relationship for the data obtained
stone mixture. Corresponding values for here, the values in Tables IV, V, and VI
higher viscosities such as would exist for were plotted in this manner as shown in
winter temperatures in the range from Fig. 2(b). It should be noted that al-
108 to 109 poises could not be estimated though the horizontal axis of the plot
precisely. However, further increase in shows viscosity in poises, the basis for
viscosity produced by decrease in tem- locating the points was the log-log vis-
perature probably would not cause as cosity in centipoises.
large an increase in strength as shown The data for the gravel mixtures with
above. This tendency is indicated by the all asphalts fall on a straight line over the
curvature of the plotted line for the sand entire viscosity range explored. The data
mixture and to a lesser extent for the for the sand and stone mixtures with all

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60 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

asphalts closely approximate straight can be "bracketed" by actual test results.


lines for values of viscosity less than 107 This rate of shear, however, does not cor-
poises, but for greater viscosity values respond to the rate of shear in the mix-
the lines show some curvature. ture specimen during the strength test.
As was mentioned earlier, some authors Based on the average film thickness of
have indicated that factors other than the asphalt in the mixture and the speed
viscosity have a significant effect on of the test, the rate of shear in the com-
strength measured by laboratory stabil- pressive strength specimen at failure is
ity tests. It is obvious from Fig. 2 that most likely in the range of 1 to 2 sec-1.
much of such an effect, if it existed, would Attempts were made to extrapolate the
be masked by aggregate systems having viscosity test data to these shear rates,
good inherent stability. Special attention but the extent of the extrapolation so
was therefore directed to the results ob- greatly reduced the precision of the esti-
tained with certain asphalts in the sand mation that the results proved to be of
and gravel mixtures. Figure 3 shows vis- no value.
cosity and strength data for three Possibly more precise measurements of
asphalts replotted on the same basis as strength would show greater deviations
used in Fig. 2(b). These are asphalts 3 in strength for the same viscosity than
and 69, which represent the extremes of are indicated here, but it is believed that
temperature susceptibility, and asphalt more study of this factor is needed to
56, which has the greatest degree of com- determine the significance of strength
plex flow. Although tests were made at differences for asphalts at the same vis-
only three temperatures for the sand cosity.
mixture with each asphalt, there are
some indications that the data points DISCUSSION OF RESULTS
form a slightly different line for each Essentially all of the relationships
asphalt. Data were available at five tem- shown by the tests conducted in this
peratures for the gravel mixtures for study have been indicated in previous
samples 3 and 69 and, as indicated, no research reports, some of which are sum-
difference in the plotted line could be de- marized in Appendix I. However, such
tected. There is some indication that the previous studies were limited in their
three data points for the gravel mixture consideration of tests on mixtures of dif-
curve for sample 56 form a slightly differ- ferent distinctive types of aggregates
ent line than that obtained with samples with asphalts from different sources
3 and 69, but this may be experimental tested over a wide range of temperature.
error. The data reported here provide a quan-
One possible cause of some of the de- titative estimate of the effect of these
viations indicated in Fig. 3, especially variables. The variations in strengths of
for values at lower temperatures, is the mixtures produced by differences in vis-
effect of the shear rate used to determine cosity-temperature susceptibility of the
the viscosities of the asphalts. All of the asphaltic binder are much greater for
viscosities reported in this study are sand mixtures than for gravel or crushed
based on a shear rate of 0.05 sec -1 . This stone mixtures. These differences are
value was selected because it is the shear most pronounced at higher temperatures,
rate most commonly used with the slid- but as the temperatures decrease the dif-
ing plate microviscometer. It can be de- ferences between aggregates become less
termined with relatively good precision important.
for the tests made on these asphalts as it For asphalts of the same viscosity re-

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WELBORN E T AL ON STABILITY MEASUREMENTS 61

gardless of source or penetration grade, the basis of their viscosities at 140 F


differences in the strength of the sand, rather than penetration at 77 F . Differ-
gravel, and stone mixtures were greatest ences in viscosities of asphalts at 140 F
at the maximum service temperature are more critical, insofar as compressive
(140 F ) . These differences decreased with strength is concerned, than differences at
decrease in temperature or increase in lower temperatures.
viscosity, and at about 40 F the effect of This study failed to show significant
viscosity became approximately constant
differences in compressive strength values
for the three mixtures. I t is believed that
for asphalts of the same viscosity from
a t such high viscosities the asphalts cease
different sources. There was some indica-
to behave as plastic materials and act
more nearly as solids. Tests to measure tion that different asphalts having the
properties such as brittleness, stiffness, or same viscosity may produce slightly dif-
fatigue resistance may be more realistic ferent strengths for weak aggregate sys-
at such temperatures in order to evaluate tems at high temperatures, but differ-
tendencies for poor durability that might ences of the order indicated would have
result from cracking or raveling of the no practical significance. Even these
pavement. small differences were minimized at lower
In certain aspects, these data indicate temperatures and with strong aggregate
that asphalt cement should be graded on systems.

APPENDIX I

SUMMARY OF PREVIOUS RESEARCH

The following papers show the general gave somewhat more plastic mixtures, al-
development of information and the present though only one section was laid with as-
state of knowledge concerning the correla- phalts having each of these consistencies.
tion of various consistency measurements No influence of the consistency of the
and the stabilities of asphalt paving mixes. asphalt cement on the service characteristics
Only a brief summary of each paper and the of the coarse-graded asphaltic concrete was
major conclusions drawn are included. apparent. Stable mixtures were laid with
In 1934 Emmons (10) reported a study by asphalts ranging from 45 to 75 penetration.
the Bureau of Public Roads that was con- In 1940, Hillman (11) reported the effect
ducted to establish performance data for the of consistency and type of asphalt on the
development of laboratory strength tests for Hubbard-Field stability of sheet asphalt
bituminous pavement mixtures. Experi- mixtures. Mixtures were made with ten dif-
mental pavement sections of a wide variety ferent grades of Mexican asphalt ranging in
of compositions were constructed on a circu- penetration from 23 to 182 from the same
lar roadway 180 ft in mean diameter, and producer and two grades (50 to 60 and 85 to
their performance was observed under 100) from each of five widely different
controlled traffic. Asphalts varying in pene- sources. The mixtures prepared with the
tration were used as binders in sheet asphalt various asphalts were tested for Hubbard-
and asphaltic concrete paving mixtures. Field stability at temperatures of 104, 122,
Observations on the performance of the test and 140 F. This study found that:
sections containing asphalts of different 1. For asphalts from the same source, the
consistency showed that for sheet asphalt stability of sheet asphalt mixtures depends
stable mixtures resulted from the use of on the consistency of the asphalt at the tem-
asphalts of 35 to 55 penetration. Softer steam perature of the stability test.
refined asphalts of 63 and 72 penetration 2. There are greater differences in the

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62 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

stability of mixtures made with the same temperature range of about 15 C (59 F) to
penetration grade of asphalts from different 180 C (355 F) on several asphalts of approxi-
sources than there are in the stability of mix- mately 65 penetration from several sources.
tures made with SO and 100 penetration Rotating cylinder, Ostwald, and falling
asphalts from the same source. cylinder viscometers were used to cover the
3. There is some characteristic of asphalt temperature range. Their tests on speci-
which caused mixtures made with asphalts mens of road-surfacing mixtures made with
from different sources to vary in stability the various asphalts indicated that the tem-
even when the consistency of the asphalts perature susceptibility of the road mixture
(measured by penetration) was the same. is determined by that of the binder. How-
In 1948 Lewis and Welborn (12) reported ever, their tests also indicated that differ-
on the effect of the characteristics of asphalts ences in the plastic and elastic properties of
on the physical properties of bituminous the asphalts were of more significance in
mixtures. This report included results of determining the mechanical properties of
laboratory tests on a particular bituminous mixtures than differences in viscosity-tem-
mixture and a review of other investigations. perature coefficients.
I t was concluded that: Weetman and Hurlburt (7) in 1947 in-
1. The strength of a given mixture is de- vestigated the effect of temperature and
pendent upon the consistency of the con- asphalt viscosity on the punching shear sta-
tained asphalt at the test temperature. bility of a sheet asphalt mixture. Three
2. The test data from other investigations penetration grade asphalts from each of two
indicate that there are some characteristics of sources varying widely in temperature sus-
asphalts which cause comparable mixtures ceptibility were used. Stability of a sheet
prepared with different asphalts to vary in asphalt mixture using each asphalt was
strength even when the contained asphalt determined over a temperature range of 40
has the same consistency. to 160 F. Absolute viscosity of the asphalts
In these reports, information was devel- recovered from the stability specimens was
oped showing the relation of consistency of determined at several temperatures within
bituminous binder, as measured by the pene- this range by a coaxial cylinder viscometer.
tration test, to the physical properties of The following conclusions were drawn:
paving mixtures and the performance of 1. The punching shear stability of sheet
pavements in service. Note that in general asphalt mixtures at temperatures in the
the researchers reported that there were range of 40 to 160 F are linear semi-log
some characteristics other than consistency functions of temperature.
as measured by penetration that influenced 2. For asphalts of the same penetration
the stability of mixtures when asphalts from at 77 F, the highly susceptible asphalts had
different sources were used. higher stabilities at lower temperatures and
In 1950, Lee and Warren (13) of the Road lower stabilities at high temperatures than
Research Laboratory commented on the fact asphalts of lower susceptibility.
that the flow properties of asphalt or other 3. Comparable stabilities at 140 F can be
types of bituminous binders are recognized as obtained by using a low susceptible asphalt
being of primary importance in road con- having an appreciably higher penetration at
struction. These authors stated that most of 77 F than a highly susceptible asphalt. For
the specification tests such as penetration, the two asphalt sources reported this differ-
softening point, ductility, and furol viscosity ence in penetration was approximately 50.
had no relation to the fundamental nature of 4. Stabilities of mixtures made with as-
flow and that up to that time little reliable phalts from the same source but of widely
information had been established to corre- different penetrations at 77 F are directly
late road behavior with fundamental char- related to the asphalt viscosity at the shear-
acteristics of binders. ing temperatures. A linear relation between
To develop such fundamental informa- log-log viscosity and log stability was found
tion, the Road Research Laboratory ob- but the curves for the series of asphalts were
tained viscosity temperature relations over a not coincident. This indicated that some

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WELBOKN E T AL ON STABILITY MEASUREMENTS 63

factor other than viscosity, such as absorp- proximately a direct function of the log-log
tion, affected the stability of the sheet viscosity of the contained binder at that
asphalt mixture. temperature and is independent of the
In 1951, Fink and Lettier (14) reported on source, nature, and proportion of the latter
a study concerned primarily with the effects constituent.
of the absolute viscosity of asphalt on 3. The fluidity characterization factor,
Marshall stability. Nine asphalts represent- which is the numerical difference of log-log
ing a wide variety of sources and methods of viscosities at 77 and 275 F multiplied by 100,
manufacture and varying widely in tempera- is directly proportional to the softening
ture susceptibility were used. Viscosities of point number. Therefore, the softening point
the asphalts were determined with the va- number is also a direct measure of the tem-
cuum capillary viscometer in the range of 120 perature susceptibility of bitumens.
to 205 F. The Saybolt furol viscometer was In 1958 Wood and Goetz (9) used a com-
used at higher temperatures. The furol pressive strength test to study the effect of
values were converted to absolute viscosities. asphalt viscosity on mixture stability. One
Marshall stability specimens were made us- of the objectives was to determine the rela-
ing one aggregate composition with each of tion between the viscosity of the binder and
the asphalts. Specimens for mixtures with
compressive strength of a mixture at various
each asphalt were molded at temperatures at
temperatures and rates of shear. The parallel
which the asphalt had a viscosity of 6 poises
plate microviscometer was used to determine
and tested at temperatures at which the
the viscosities at 40, 100, and 140 F over a
viscosity as 1400 poises. This study
range of shear rates for four asphalts from
emphasized that the stability value was
strongly influenced by the viscous resistance different sources.
of the binder. Sheet asphalt mixtures composed of 74 per
cent sand, 17 per cent filler (material passing
In 1953 Neppe (8) reported the results of the No. 200 sieve) and 9 per cent asphalt
compressive strength tests on (1) mixtures were prepared with the four asphalts. Speci-
made with aggregate of one type and grad- mens 2 in. in diameter and 4 in. in height
ing and (2) 40 asphalt cements of different were molded by the double plunger method.
penetration grades and rheological properties. Compressive strength tests were made at 40,
The author calculated stability values from
100, and 140 F at three rates of deforma-
the times required for the specimens of the
tions. Relationships between viscosity and
mixture to deform by predetermined amounts
maximum compressive strength at various
during the application of a compressive load
shear rates were determined. Conclusions
which was increasing at a uniform rate. The
drawn from the study were:
tests were made at 77, 104, 122, and 140 F
for each asphalt mixture. The viscosity of 1. The shear rate has a marked effect on
the asphalts were determined at several viscosity of some asphalts and little effect on
temperatures. This report emphasized the others. The effect of shear rate on viscosity
usefulness of "softening point number" as a also varies with temperature.
characterization factor for determining the 2. A plot of log compressive strength
influence of rheological characteristics of the versus temperature gives a simple means of
binder on mechanical properties of mixtures. evaluating temperature susceptibility of
The effect of the viscosity of the asphalt mixtures.
on compressive strength of the mixtures was 3. No direct relationship was found be-
also reported. The following conclusions tween compressive strength of sheet asphalt
were drawn: mixtures and the viscosity of the contained
1. The results of compressive strengths at asphalt even though the effects of shear rate
77 F showed no marked differentiation be- were taken into consideration. This indi-
tween mixtures prepared either from bitu- cated that factors other than viscosity of the
mens of low or high softening point number. binder have an effect on mixture strength.
2. The mechanical stability of a bitu- In a paper presented at the 1961 Annual
minous mixture at any temperature is ap- Meeting of ASTM, Verdi Adam (15) showed

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64 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

the effect of asphalt viscosity on the Marshall varied from 3.5 X 104 to 3.6 X 105 (the
stability of an asphalt concrete mixture using values being converted from absolute vis-
several different asphalts. The four asphalt cosity at 140 F). The author showed a good
cements used in his tests varied from 60 to relationship between furol viscosity and
70 to 120 to 150 penetration at 77 F. The Marshall stability, both at 140 F, for the
furol viscosity of these asphalts at 140 F different asphalts.

APPENDIX II

COMPRESSION TEST PROCEDURE

Mixture Preparation: For each specimen the mixture in the


heated mold was spaded once around the
The aggregates for the gravel and stone
inside of the mold, then subjected to a 3000
mixtures were separated on various coarse
psi compaction load held for 2 min using the
and fine sieve sizes, including the No. 200
double plunger technique.
sieve. Portions of each size were then recom-
bined to meet predetermined gradations in Test Procedure:
batches of sufficient amounts to mold two After removal from the molds, the speci-
specimens. Similar test batches for the sand mens were allowed to cool to room tempera-
mixture were prepared by combining con- ture and then placed in a forced draft oven
crete sand, sheet asphalt sand, and limestone at 140 F for 24 hr. The specimens were then
dust in definite proportions. All batches of cooled overnight at room temperature and
aggregates were heated overnight in a forced the bulk specific gravity of each determined
draft oven at 325 F. The asphalt for each by the water displacement method. The air
batch was prepared by putting a slight excess voids were calculated on the basis of effec-
of the amount required per batch in a sealed tive specific gravity of the aggregate as
8-oz tin which was then placed in a 300 F determined by the Rice vacuum saturation
oven 45 min prior to blending with the method. The specimens were placed in air
heated aggregate. The required amount of baths controlled at the various test tem-
asphalt was added to the aggregate in a peratures indicated in Table IV. In general,
modified Hobart mechanical mixer and the the time in the air bath was § hr more than
materials mixed for 2 min. Each batch con- that required for a dummy specimen to
tained slightly more mixture than that re- reach the desired test temperature, as
quired for two 3- by 3-in. cylindrical speci- measured with a thermocouple inserted in
mens. the center of the specimen. The bearing
blocks of the testing machine were also
Molding Procedure:
placed in the air baths to bring them to the
After mixing, the amount of material re- test temperature. The compressive strength
quired to mold one specimen was transferred of the specimens were determined at a load-
to a heated mold. The bowl with the re- ing rate of 0.15 in. per min. Each of the
maining mixture was placed in the 325 F values for compressive strength and specific
oven for approximately 3 min after which gravity given in Table IV is the average
the second specimen was molded. result for four duplicate test specimens.

REFERENCES
(1) J. Y. Welborn and W. J. Halstead, "Prop- Part II, Various Penetration Grades,'
erties of Highway Asphalts: Part I, 85-100 Public Roads, Vol. 31, No. 4, Oct., 1960,
Penetration Grade," PubHc Roads, Vol. 30, D. 73.
No. 9, Aug., 1959, p. 197. (3) F. S. Rostler and R. M. White, "Composi-
(2) J. Y. Welborn, \V. J. Halstead, antl J. G. tion and Changes in Composition of High-
Boone. "Properties of Highway Asphalts: way Asphalts, 85-100 Penetration Grade,"

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DISCUSSION ON STABILITY MEASUREMENTS 65

Proceedings, Assn. of Asphalt Paving Tech- sive Strength of a Bituminous Mixture and
nologists, Vol. 31,1962, p. 35. Viscosity of the Binder," Proceedings,
(4) W. J. Halstead and J. A. Zenewitz, Assn. Asphalt Paving Technologists, Vol.
"Changes in Asphalt Viscosities During 27, Feb., 1958, p. 563.
Thin-Film Oven and Microfilm Durability (10) \Y. J. Emmons, "Stability Experiments on
Tests," Public Roads, Vol. 31, No. 11, Dec, Asphaltic Paving Mixtures," Public Roads,
1961, p. 211. Vol. 14, No. 11, Jan., 1934, p. 197.
(5) R. L. Griffin, T. K. Miles, C. J. Penther, (11) W. O'B. Hillman, "The Effect of Con-
and W. C. Simpson, "Sliding Plate Micro- sistency and Type of Asphalt on the Hub-
viscometer for Rapid Measurement of bard-Field Stability of Sheet Asphalt
Absolute Viscosity in Absolute Units," Mixtures," Public Roads. Vol. 21, No. 4,
ASTM STP No. 212, Am. Soc. Testing June, 1940, p. 75.
Mats , 1957, p. 36. (12) R. H. Lewis and J. V. Welborn, "The Ef-
(6) D. F. Fink and R. L. Griffin, "Measure- fect of Characteristics of Asphalts on
ment of the Consistency of Paving Ce- Physical Properties of Bituminous Mix-
ments at 140 F with the Sliding Plate tures," Public Roads, Vol. 25, No. 5, Sept.,
Microviscometer," ASTM STP No. 309, 1948, p. 85.
Am. Soc. Testing Mats., 1962, pp. 79-94. (13) A. R. Lee and J. B. Warren, "The Flow
(7) B. Weetman and D. H. Hurlburt, "The Properties of Asphaltic Bituminous With
Fffect of Asphalt Viscosity on Stability of Reference to Road Behavior," Proceedings,
Asphalt Paving Mixtures," Proceedings, Assn. Asphalt Paving Technologists, Vol.
Assn. Asphalt Paving Technologists, Vol.
11, Jan., 1940, p. 340.
16, Feb., 1947, p. 249.
(14) D. F. Fink and J. A. Lettier, "Viscosity Ef-
(8) S. L. Neppe, "The Influence of Rheological
fects on the Marshall Stability Test,"
Characteristics of the Binder on Certain
Proceedings, Assn. Asphalt Paving Tech-
Mechanical Properties of Bitumen-Ag-
nologists, Vol. 20, Feb., 1951, p. 246.
gregate Mixes," Proceedings, Assn. Asphalt
Paving Technologists, Vol. 22, Jan., 1953, (15) Verdi Adam, "Effects of Viscosity in
p. 428. Bituminous Construction," ASTM STP
(9) L. E. Wood and VV. H. Goetz, "The Rela- No. 309, Am. Soc. Testing Mats., 1962
tionship Between the Unconfined Compres- pp. 121-132.

DISCUSSION
1
MR. J. M. GRIFFITH (presented in varying viscosity at 140 F and penetra-
written form).—One of the statements tion at 77 F were used. Marshall test
made by Welborn, Halstead, and Olsen specimens were prepared at several
was that "This study failed to show sig- asphalt contents with each of the eight
nificant differences in compressive asphalts.
strength values for asphalts of the same The curves on the chart show Marshall
viscosity from different sources." stability versus asphalt content for each
The Asphalt Institute also has made of the eight asphalts. Marshall stability
studies comparing the strength charac- is plotted as the ordinate and asphalt
teristics of asphalt paving mixes both content as the abscissa. In the first col-
with absolute viscosity at 140 F and with umn to the right of each curve is shown
penetration at 77 F of the asphalt cement the absolute viscosity at 140 F of the
binder. The accompanying Fig. 4 illus- asphalt used to prepare the test speci-
trates one such comparison. In this test mens represented by the curve. Simi-
series, the aggregate gradation was held larly, penetration at 77 F is shown in the
constant, and a sheet asphalt grading was second column to the right of each curve.
used. Eight asphalt cements of widely Note that Marshall stability increases in
1 a consistent manner with increasing vis-
Director of Research and Development.
The Asphalt Inst., College Park, Md. cosity. A similarly consistent trend does

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66 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

not hold true, however, for penetration gate, surface texture characteristics of the
Note particularly the substantial differ- aggregate, the amount and type of min-
ences in Marshall stability for two as- eral filler, and the degree of compaction
phalts both having a penetration value also have a substantial bearing on these
of 37. One curve indicates Marshall strength characteristics. Furthermore,
stability values about twice those of the high-viscosity asphalts may possibly in-
other. These data indicate that (1) vis- troduce some problems in regard to pave-
cosity is an important property of the ment performance at low temperatures.
asphalt binder and (2) viscosity has a Thus, while consistency classifications on

2000

10.5 11.0 11.5 12.0 12.5


ASPHALT CONTENT IN TOTAL MIXTURE, PER CENT
FIG. 4.—Effect of Asphalt Viscosities on Marshall Test Properties of Sheet Asphalt Mixtures.

direct relationship to the strength char- a viscosity basis appear to offer consid-
acteristics of the paving mixture. Such a erable promise for future improvements
relationship, however, does not seem to in asphalt cement specifications, further
be indicated for the penetration test. studies will be required to fully appraise
Therefore, perhaps the viscosity meas- these initial indications. The cooperation
urements at 140 F are potentially more and complete understanding of asphalt-
valuable as a consistency classification user agencies will be essential in a final ap-
for asphalt cements than penetration at praisal of the validity and potential value
77 F. of this promising change in asphalt
However, viscosity of the asphalt specifications. I trust that the American
binder is not the sole factor governing the Society for Testing and Materials will be
strength characteristics of paving mixes. among the leaders in appraising this
Gradation and angularity of the aggre- promising new approach.

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STP328-EB/Apr. 1963

APPLICATION OF ASPHALT VISCOSITY TO PAVING P R O B L E M S

B Y R. L. G R I F F I N , 1 J. O. IZATT,' 2 AND J. A. LETTIER 3

SYNOPSIS

Information on (1) the viscosity levels that permit the most efficient pave-
ment construction operations and (2) the viscosity factors most desirable for
pavement performance is meager and clouded by the influences of asphalt mix
compositions. The temperature viscosity and viscosity rate of shear charac-
teristics of the asphalts can be measured on the original material and on ma-
terial separated from the mixes and from the pavement. These viscosity factors
can be used in the design and construction of the asphalt pavement and for
comparing the performances of the asphalts.

Asphalt viscosity measurements have sliding plate microviscometer (l)4 which


practical application in the preparation is suitable for measuring not only viscos-
and placement of the pavement and in ity but also the shear susceptibility of
studies of the performance of the pave- the asphalt at any selected temperature.
ment. For Newtonian-type asphalts, there
The viscosity of an asphalt changes is a constant relationship between the
with temperature. I t is equally well shearing stress and the rate of shear so
known that the level of viscosity at any that the viscosity remains independent
specified temperature changes due to of the shear rate or the rate of movement
chemical and physical effects, oxidation, of the plates in the microviscometer.
and volatilization. Such changes are rapid Many asphalts, however, are non-New-
at mixing temperature and slow at pave- tonian, especially in the lower tempera-
ment temperature. These temperature- ture ranges, and their measured viscos-
viscosity relationships and the changes ities are a function of the rate of shear or
can be measured for any temperature the rate at which the plates are moved
throughout the entire range from that of with respect to each other. The shear
heating in the hot-plant to freezing in susceptibility of the asphalt can be meas-
the pavement. In the high temperature ured with the microviscometer by a
ranges, the measurements may be made series of weights if the film thickness is
with the capillary flow type viscometers. constant. A plot of the log viscosity
In the low temperature ranges, the meas- versus log shear rate normally gives a
urements may be made with the Shell straight line from which the viscosity at
intermediate shear rates can be ascer-
1
Asphalt Research Chemist, Martinez Re- tained.
search Laboratory, Shell Oil Co., Martinez,
Calif. (Deceased.) The importance of measuring shear
2
Asphalt Technologist, Products Application susceptibility can be illustrated by con-
Dept.,
3
Shell Oil Co., New York, N. Y. 4
Asphalt Technologist, Products Application The boldface numbers in parentheses refer
Dept., Shell Oil Co., San Francisco, Calif. to the list of references appended to this paper.
67

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68 SYMPOSIUM OK FUNDAMENTAL VISCOSITY

sidering the different stresses affecting viscosity of 85 sec Saybolt Furol." The
pavement performance. Deflections of viscosity range advocated by The As-
the pavement under traffic are at high phalt Inst, and most commonly specified
shear rates, whereas deflection from is 75 to 150 sec Saybolt Furol (SSF)
settlement of the structure are at low (about 1.5-3.0 poises).
shear rates. Dormon (2) has estimated
SPREADING
the rate of loading for the former to be
of the order of 10 -3 reciprocal seconds. During transportation from the hot-
When properly measured, the rheological mix plant to the job site, the tempera-
properties of asphalts, viscosity and shear ture of the asphalt mix will drop slowly
susceptibility, enable the comparison of but usually will be in the range of 225
the mechanical properties of asphalts to 300 F at the time of placement. At
at any temperature of interest and study these temperatures, the asphalt behaves
of the relationships of these properties as a viscous liquid and its viscosity will
to performances in the hot-plant and in influence the ease of handling and place-
the pavement. ment of the mix. However, thanks to the
efficiencies of the modern finishing and
HOT-PLANT MIXING paving machines, the differences in the
The temperature at which the asphalt viscosities of the paving grade asphalts
and the aggregates are mixed in the hot- under these conditions do not present
plant is usually specified in the range of appreciable problems.
250 to 325 F. At these temperatures and
under the conditions in the pug-mill, the COMPACTING
asphalt behaves as a simple viscous or Proper compaction of the asphalt mix
Newtonian liquid, but all asphalts of the is perhaps the most important factor in
same penetration grade at 77 F do not the construction of the pavement since
have the same viscosities at the same the degree of compaction can profoundly
high temperature. Tucker (3) explained affect both the performance and the life
this problem over two decades ago: "As- of the pavement. Compaction require-
phalts from different crudes or prepared ments are usually specified in terms of
by different processing methods may pavement densities, and the literature is
differ appreciably in viscosity at mixing replete with studies of mix temperatures
and placing temperatures and these tem- and compactive efforts required in the
peratures should be adjusted to the vis- field to achieve these densities. In the
cosity characteristics of the asphalt being laboratories the compactive effort re-
used." Tucker then showed the differ- quired to produce a desirable density for
ences in the kinematic viscosities in the a given aggregate composition has been
temperature range of 300 to 400 F of directly related to the viscosity of the
three asphalts of the same penetration contained asphalt, and this compactive
at 77 F. effort has been found to be different for
The practice of selecting the tempera- different asphalts at the same tempera-
ture to provide the proper mixing viscos- tures.
ity is now well established. For example, In a recent comprehensive study,
the State of Louisiana (4) has the follow- Serafin and Kole (5) said: "The tempera-
ing requirement: "The asphalt cement ture at which the asphalt mix is com-
Grade AC-3 (60-70 penetration) and/or pacted appears to be of primary impor-
AC-5 (80-100 penetration) shall be tance. Although the roller weight and
heated to a temperature that will give a compactive efforts should affect the

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GRIFFIN ET AL ON ASPHALT VISCOSITY AND PAVEMENTS 69

CO
O
CL

in
o

O
<n
00
<

70 90 110 130 150 170 190 210 230 250 280


TEMPERATURE,DEG FAHR
FIG. 1.—Viscosity-Temperature Characteristics of Asphalt D. NOTE. Newtonian behavior at all
temperature levels.

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70 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

density results, they apparently are sub- rolling could hardly be compared on the
jected or dependent to a large extent basis of temperature of the mix and com-
upon the temperature at which the com- pactive effort only. Viscosity must be
paction process occurs. . . . Time, an considered.
important element on any construction Although many investigators have
project, is another factor dependent on determined the importance of mix tem-
temperature. The time available for perature during compaction, few have
effective utilization of any compactive related this directly to the viscosity of
effort is a function of the temperature the contained asphalt in their field stud-
of the mix and the ambient air tempera- ies. Adam (6), however, pointed out the
ture." The same study gives "pavement importance of viscosity and determined
cooling data of bituminous concrete in field studies that the most effective
wearing course mixture for various ranges compaction (for a given aggregate com-
of air temperatures," from which the position) was achieved with a three-wheel
following values were selected for an air roller when the viscosity of the asphalt
temperature range of 60 to 70 F: was around 400 SSF (about 8 poises) and
similarly around 5500 SSF (about 110
Time, min Temperature, deg Fahr poises) for a pneumatic roller. Construc-
tion specifications will eventually evolve
0 266 around the viscosities of the contained
2 238
5 214
asphalt rather than around temperatures
10 190 for the control of this important opera-
20 160 tion.

This information may be used to illus- IN-SERVICE PERFORMANCE


trate the importance of viscosity meas- Under the repetitive action of traffic,
urements. The viscosity levels for as- the asphalt pavement deflects and re-
phalts of the same penetration grade may bounds as the load passes. Nijboer (7)
be quite different, especially after hard- and others have measured the magnitude
ening in the hot-plant before placement of these deflections and have developed
of the mix. As an example, the viscosities considerable evidence that asphalt pave-
of asphalts D and E, which will be dis- ments may be subject to fatigue and
cussed in detail later, have been read cracking under these flexural strains.
from Figs. 1 and 2, respectively, and Monismith (8) recently summed up the
added to the above table for comparison: role of the asphalt when he stated that
primary factors influencing the flexibility
Tempera- Viscosity, poises characteristics of an asphalt paving
ture, deg
Fahr Asphalt D Asphalt E
mixture are the physical and chemical
properties of the asphalt and that among
266 2 7 these properties one of the most impor-
238 5 18 tant is viscosity. He pictures an idealized
214 13 50
190 32 160 relationship of viscosity versus tempera-
160 160 1000 ture in which the asphalt would be suffi-
ciently fluid to facilitate preparation and
The differences are obvious. Asphalt E placing of the mix but would have prac-
is six times as viscous as asphalt D at tically no change in viscosity over the
160 F. The performances of the mixes range of temperatures in the pavements.
containing these two asphalts under During the short times of loading en-

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GRIFFIN ET AL ON ASPHALT VISCOSITY AND PAVEMENTS 71

39.2 77 140 275


.ip 30 50 70 90 110 130 150 170 190 210 230 250 280
1
I0" | i i i 1 1 1 — : I

•n" I 1 i , 1 1 1 i 1 1 1 u
1
30 50 70 90 110 130 150 170 190 210 230 250 280
TEMPERATURE,DEG FAHR
FIG. 2.—Viscosity-Temperature Characteristics of Asphalt E. NOTE. Width of bands is difference
between viscosities at shear rates of 10~3 sec -1 {top line) and 1 sec~' {bottom line).

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72 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

countered under moving traffic and even in the pavement has been charted by
at temperatures as high as 140 F, the investigators who have recovered the
asphalt may exhibit non-Newtonian flow. asphalt and measured its properties in
The asphalt is shear susceptible. Tbere- terms of penetration, softening point, or

TABLE I. -VISCOSITY-TEMPERATURE CHARACTERISTICS


OF ORIGINAL ASPHALTS.
Viscosity, poises
Project Ductility Penetra- Softening Penetra- Shear
Identification at 77 F tion at Point, tion
77 F deg Fahr Index"
Rate,
sec -1
At 77 F At 140 At 275
At 39.2 F F F»

1 2 . 3 X 10 7 1.22 X 10 5
B-l 100 + 251 101 + 0.3 0.05 3.4 1.40 393 1.76
0.01 5.2 1.65

1 8.77 1.48
A 100 + 219 101 -0.3 0.05 8.77 1.48 374 1.35
0.01 8.77 1 48

1 4.29 1.00
C 100 + 244 100.5 0 0.05 4.29 1.00 354 1.16
0.01 4.29 1.00

1 4.90 1.48
II 100 + 231 101.5 0 0.05 5.60 1.65 472 1.60
0.01 6.70 2.04

1 1.0 1.45
G 100 + 241 102.5 + 0.5 0.05 2.46 1.93 766 2.23
0.01 7.90 2.80

1 2.58 1.27
J 100 + 240 101.5 + 0.3 0.05 4.10 1.44 973 2.45
0.01 7.80 1.72

1 1.70 1.40
E 100 + 231 102.5 +0.3 0.05 2.65 2.03 951 2.59
0.01 4.85 3.80

1 5.10 1.20
D 100 + 236 99 -0.6 0.05 5.10 1.20 340 1.31
0.01 5.10 1.20

1 4.05 1.28
F 100 + 212 103.5 -0.2 0.05 6.00 2.30 706 2.32
0.01 9.60 4.90

" See Ref. (14).


b
Capillary viscometer.

fore, the complete rheological properties ductility, or all three. These investigators
obtained should include the effect of tem- have found that asphalt hardening was
perature on viscosity as well as the effect influenced by the many factors of en-
of shear rate, since both are necessary to vironment and that pavement failures
characterize the material properly and could be associated with the hardening.
to permit valid correlations with pave- Over two decades ago Hubbard and
ment performance. Gollomb (9) concluded that sheet asphalt
The hardening of asphalts in service pavements were susceptible to cracking

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GRIFFIN ET AL ON ASPHALT VISCOSITY AND PAVEMENTS 73

when the penetrations at 77 F of the pavements were generally free from


recovered asphalts were below 20 and cracking.
that serious difficulty with cracking The literature contains many similar
would not occur if the penetrations could studies in which the hardening of the

TABLE II.—VISCOSITY-TEMPERATURE CHARACTERISTICS OF ASPHALTS


RECOVERED FROM HOT-PLANT MIXES.

Penetra- Softening Penetra- Shear Viscosity, poises


Project Ductiliy tion at Point, deg tion Rate,1
Identification at 77 F" 77 F" Fahr" Index6 sec^ At 77 F At 140 F At 275 F c

1 3 . 2 0 X 10 5
B-l 100 + 147 110 0 0.05 4.20 881 2.70
0.001 5.25

1 2.72
A 100 + 164 106 -0.4 0.05 2.72 521 1 66
0.001 2.72

1 2.74
C 100 + 154 104 -1.1 0.05 2.74 668 ] 61
0.001 2.74

1 4.35
H 100 + 159 105 -0.7 0.05 5.00 986 2 35
0.001 6.10

1 7.80
G 105 119 + 0.4 0.05 17.7 3400 5 07
0.001 52.0

1 3.00
J 100 + 187 104 -0.3 0.05 4.20 1450 3 05
0.001 6.50

1 10.0
E 100 + 98 118 0 0.05 17.2 3846 5.55
0.001 35.5

1 2.51
D 100 + 184 103 -0.6 0.05 2.51 559 1.67
0.001 2.51

1 6.60
F 100 + 112 116 + 0.2 0.05 11.1 2023 3 96
0.001 22.5

"See Ref. (11).


b
See Ref. (14).
c
Capillary viscometer.

be kept above 30. About this same time asphalt has been charted in terms of
Vokac (10) observed that when the pene- time-honored test methods. But the
tration at 77 F of the recovered asphalt significance of these tests is widely de-
was less than 18, the pavements were bated. The tests are expressed in unre-
definitely of the cracking type. When lated terms and are not easily translated
the penetration was between 18 and 25, one to another. The penetration and
the pavements were prone to crack and softening point are indirect measure-
when the penetration was over 25 the ments of the viscosity of asphalts but

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74 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

only at one shear rate. A notable excep- an extended range ASTM type chart
tion to these field studies is the Zaca- based on the Walther equation. The
Wigmore Test Road (11), sponsored by asphalt is unique since originally it was
the State of California where the harden- Newtonian at all test temperatures and
ing of the asphalts was also charted in remained Newtonian after mixing in the
terms of viscosity. hot-plant and after aging up to 44
months in the pavement. Asphalt D
T H E ZACA-WIGMORE TEST ROAD hardened in the hot-plant as expected.
The Zaca-Wigmore Test Road was The viscosity increased from 1.31 poises
constructed in the fall and winter of to 1.67 poises at 275 F and from 340
1954-1955 with asphalts from nine poises to 559 poises at 140 F, barely suffi-
sources, each in a different test item in cient to raise it to the viscosity level of
two periods of construction (Period 1 asphalt F before mixing. The hardening
and Period 2). The viscosities of the of asphalt D in service was studied from
original asphalts together with their viscosity measurements at 77 F. It in-
conventional test properties are shown creased in viscosity from 2.51 X 105
in Table I. The letter designations used poises when laid to 1.14 X 106 poises at
are those assigned by the California 12 months and to 6.7 X 106 poises after
Highway Dept. The viscosities of these 44 months in service. This is a 50-fold
asphalts as recovered after hot-mixing viscosity increase at 77 F. Its rating in
are listed in Table II. Table III is a com- the pavement test items was "fair."
posite listing of the viscosity-temperature These changes are easy to describe
characteristics and shear-susceptibility since shear rate need not be specified for
properties of the same asphalts for the a Newtonian liquid. But this asphalt was
original samples and as recovered from the exception among the four.
freshly prepared plant mixtures and
from pavement samples. All tests apply Asphalt E:
to asphalts from Period 1. Although Figure 2 sketches the temperature-
these data reveal familiar anomalies, viscosity and shear rate of asphalt E as
they show the way in which the rheologi- plotted on the ASTM type viscosity
cal properties of asphalts change in chart. Here, however, viscosity bands are
service. shown for the lower temperature ranges
The service records of these asphalts which are bounded by lines connecting
in the Test Road have been charted and viscosity measurements made at the
correlated by Hveem (li). Correlations different shear rates of 1 sec -1 and 10~3
between the microfilm durability test and sec -1 . In all instances the viscosities are
the service records of each have also been higher as the rate of shear is lower. As-
developed by Simpson (12). The viscosity phalt E was non-Newtonian before in-
characteristics of four of these asphalts corporation into the mix. After mixing,
(D, E, F, and J) will be detailed here to the non-Newtonian flow properties be-
illustrate differences and changes with came more pronounced at higher tem-
service. peratures and the variations of viscosity
with rate of shear continued to increase
Asphalt D: with service in the pavement. Again, if
Asphalt D is represented by the dia- we choose 77 F as a base line for compari-
grams in Fig. 1 which show lines connect- son, asphalt E had a viscosity band of
ing viscosities measured at the tempera- 1.0 X 106 to 3.6 X 106 poises at shear
tures of 39.2, 77, 140, and 275 F. This is rates of 1 sec^1 and 10~3 sec-1, respec-

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199

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C reserved); <
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EST <
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76 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

39.2 77 140 275

TEMPERATURE, DEG FAHR


FIG. 3.—Viscosity-Temperature Characteristics of Asphalt F. NOTE. Width of bands is difference
between viscosities at shear rates of 10~3 sec -1 (top line) and 1 sec^1 (bottom line).

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GRIFFIN ET AL ON ASPHALT VISCOSITY AND PAVEMENTS 77

39.2 77 140 275


l 2 30 50 70 90 110 130 150 170 190 210 230 250 280
1 i i
!

! !
! !

m sX ; i

^ V V v X^AFTER 20 MONTHS IN PAVEMENT

>^-*-AFTER 12 MONTHS IN PAVEMENT

*FTER HOT-PLANT MIXING

0RIGINAL-\

! . ! ,

i ' i •• ':

50 70 90 110 130 150 170 190 210 230 250 280


TEMPERATURE, DEG FAHR

FIG. 4.—Viscosity-Temperature Characteristics of Asphalt J. NOTE. Width of bands is difference


between viscosities at shear rates of 10~3 sec -1 (top line) and 1 sec -1 (bottom line).

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78 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

tively, when the mix was placed. After of 5 X 10~2 sec - 1 after 30 months of
12 months in the pavement, the viscosity service.
band at the same rates of shear was Changes in the shear susceptibility of
7.5 X 106 to 3.2 X 107 poises; and when the asphalts such as E are related to
failure occurred at 44 months, the viscos- changes in chemical composition. Rela-
ity band had increased as shown by tionships between these properties have
viscosities of 1.13 X 108 to 4.70 X 108 been found by Simpson (13) who noted
poises. This is an increase in viscosity that increasing the resin content at a
of approximately 100-fold. These prop- constant ratio of saturates to aromatics
erties were markedly different from those leads to a decrease in shear susceptibility
of asphalt D, and so were the respective of the asphalt which, although pertinent,
performances of each material. is outside the scope of this paper.

Asphalts F and J: USE or THE D A T A

Analyses of asphalts F and J are shown There are several practical uses of as-
in Figs. 3 and 4, respectively. Their prop- phalt viscosity in the preparation and
erties are somewhat in between the prop- placement of the asphalt pavement and
erties of D and E. After 54 months, as- in the studies of pavement performances.
phalt F failed whereas, asphalt J was in The performance of the asphalts can be
excellent condition. Determination of followed throughout their service his-
viscosity at much lower shear rates than tories by measurements of their viscosity
10~3 sec - 1 may distinguish the differences characteristics which offer a sound basis
in the performance of asphalts D, E, F, for comparisons and for interpretations
of the role of the asphalt in the pavement.
and J by their physical properties. Simp-
son (12) has shown that the field per- A cknowledgment:
formances of all the asphalts in Period 1
The data in this paper were obtained
correlate well with their recovered vis-
at Shell Development Co.'s Emeryville
cosities measured at 77 F at a shear rate
Research Center by the late R. L. Griffin.

REFERENCES
(1) R. L. Griffin, T. K. Miles, and C. J. Pen- (6) Verdi Adam, "The Effects of Viscosity in
ther, "Sliding Plate Microviscometer for Hot Mix Construction," ASTM STP No.
Rapid Measurement of Asphalt Viscosity 309, Am. Soc. Testing Mats., 1961, p. 121.
in Absolute Units," ASTM STP No. 212, (7) L. W. Nijboer and C. Van der Poel, "A
Am. Soc. Testing Mats., 1957, p. 36. Study of Vibration Phenomena in Asphaltic
(2) G. M. Dormon and A. W. Jarman, "Some Road Constructions," Proceedings, Assn.
Factors Influencing the Behavior of Bitu- Asphalt Paving Technologists, Vol. 22,
men Road Surfacings," Journal of Applied 1953, p. 197.
Chemistry, Vol. 8, December, 1958, p. 832. (8) L. Monismith, "Flexibility Characteristics
(3) E. B. Tucker, "Factors in the Hardening of Asphaltic Paving Mixtures," Proceed-
of Hot-Mix Asphaltic Materials," Pro- ings, Assn. Asphalt Paving Technologists,
ceedings, The Montana National Bitumi- Vol. 27, 1958, p. 74.
nous Conference, p. 139, 1939.
(9) P. Hubbard and H. Gollomb, "Handling
(4) State of Louisiana, Specifications Section 6 of Asphalt with Relation to Development
(New), "Bituminous Mixture for Hot
of Cracks in Asphalt Pavements," Pro-
Application," Rev. 10/60, Part 6.20.
ceedings, Assn. Asphalt Paving Technolo-
(5) J. Serafin and L. Kole, "Comparative
gists, Vol. 8, 1937, p. 165.
Studies of Pneumatic Tire Rolling," Pro-
ceedings, Assn. Asphalt Paving Technolo- (10) Roland Vokac, "Correlation of Laboratory
gists, 1962, to be published. Tests of Bituminous Mixtures with Service

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GRIFFIN ET AL ON ASPHALT VISCOSITY AND PAVEMENTS 79

Behavior," Proceedings, Montana National mental Project," ASTM STP No. 277,
Bituminous Conference, 1939, p. 226. Am. Soc. Testing Mats., 1959, p. 52.
(11) F. N. Hveem, E.Zube.and J. Skog, "Prog- (13) W. C. Simpson, R. L. Griffin, and T. K.
ress Report on the Zaca-VVigmore Experi- Miles, "Relationship of Asphalt Properties
mental Asphalt Test Project," ASTM STP to Chemical Constitution," Journal of
No. 277, Am. Soc. Testing Mats., 1959, p. 3. Chemical and Engineering Data, Vol. 6,
(12) W. C. Simpson, R. L. Griffin, and T. K. No. 3, July, 1961, p. 462.
Miles, "Correlation of the Microfilm (14) Ph. J. Pfeiffer and P. M. van Doormal,
Durability Test with Field Hardening Journal, Inst, of Petroleum, Vol. 22, 1936,
Observed in the Zaca-Wigmore Experi- p. 414.

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STP328-EB/Apr. 1963

VISCOELASTIC P R O P E R T I E S OF PAVING ASPHALTS

B Y F. C. GZEMSKI 1

SYNOPSIS

This paper reviews the basic flow properties of asphalts and presents experi-
mental data on the effect of shear rate on viscosity of paving asphalts at various
temperatures. The oversimplified flow or rheological patterns of asphalts pre-
sented here are intended primarily to create an awareness of the basic param-
eters and engineering yardsticks which, when applied, will lead to a better
understanding of asphalt pavement behaviors and eventually lead to their
implementation in the engineering design of pavements.
A basic understanding of the language of rheology, a knowledge of the basic
theory of the rheology of asphalt, and a familiarity with the necessary instru-
mentation are required before these concepts can be effectively implemented as
performance standards.

An Asphalt Inst.-industry group has study of the rate at which these proper-
been engaged during the past year in a ties change under various mechanical
program relating to the viscosity-tem- and environmental conditions should be
perature characterization of paving considered. When understood, asphalt
asphalts. Methods and instrumentation pavement performance specifications will
are being developed to accurately meas- reflect the rate at which the rheological
ure viscosity of asphalts at several or flow properties of the asphalts change
temperatures. I t is believed that a in service.
viscosity grading of asphalt cements in
place of the present penetration method T H E PROBLEM
will more accurately reflect pavement
Although considerable literature has
behaviors and aid in the design of pave-
been published on the flow properties of
ments.
asphalts, asphalt-filler suspensions, and
The deformation character of asphalt asphalt-filler-aggregate systems, design
pavements under a wide range of en- criteria for asphaltic pavements assume
vironmental conditions is complex. How- asphalt to be merely a high-consistency
ever, when the physical and chemical fluid.
properties of the asphalt component are
Several factors are involved in the
better known, a more sophisticated
performance and durability of asphalt
understanding of the behavior of the
pavements. The behavior of asphalts
pavement structure will follow.
in service is governed by their initial
When the relative influence of the
engineering properties as well as by the
initial properties of asphalts in pavement
mechanical and environmental condi-
service have been ascertained, a basic
tions to which they are subjected. The
1
The Atlantic Refining Co., Philadelphia, Pa. physical state of extremely thin asphalt
80

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GZEMSKI ON VlSCOELASTIC PROPERTIES 81

films (1,2),2 their chemical reaction at the stresses (4) resulting from rapid or gradual
asphalt-mineral interface, the rate at temperature changes could possibly turn
which the film hardens due to oxidation out to be the prime factor in pavement
—each of these factors no doubt con- durability. An unfavorable response in
tributes to the behavior of the asphalt the form of film fracture, loss of cohesion,
pavement. Therefore, studies relating to or adhesion undoubtedly can be the
more durable pavements must consider precursor to the more overt pavement
the engineering properties of the pave- failure.
ment structure as well as the physical Most important, however, are the
and chemical properties of the asphalt rates at which all of these properties
component of the pavement, be it only change with time. In the final analysis,
the minor component volumetrically. the durability of an asphalt pavement
To bring this matter into proper is a function of this rate of change.
perspective, one must consider the non- The application and service require-
cohesive nature of the aggregate used in ments for asphalts in pavements cover
asphalt paving mixtures. Cohesiveness is a broad spectrum of temperatures and
effected by the addition of an asphalt mechanical responses. Temperatures
binder material, and cohesivity improves ranging from 0 to 140 F are experienced
upon compaction of the mix. Maximum under actual service conditions and from
cohesion is obtained when maximum 200 to 325 F in the manufacture, applica-
density is reached. This means, ideally, tion, and compaction of the paving mix.
that the aggregate particles are statisti- The deformation patterns for asphalts
cally distributed and properly oriented in and asphalt pavements over the span of
an asphalt or asphalt-filler continuum. temperatures and load requirements are
The bearing strength of the compacted quite complex and not fully understood,
mix then becomes a function of the as has been revealed in recent research
thickness of the asphalt film and the literature (3-7). In the temperature range
physical or mechanical properties of encountered during the mixing laydown
these thin films in shear, tension, and and compaction of the pavement, the
compression. The properties of the film flow properties of asphalt can be de-
can also be affected by interactions at scribed as being viscous in nature. In
the aggregate-mineral interface, which in service, asphalt flow assumes a dual
effect are caused by the forces of adhe- character. Depending on the tempera-
sion, the strong intermolecular forces ture, the nature of the load application
evidenced by the high viscosity of the pattern, and the characteristics of the
asphalt, and the viscoelastic properties asphalt, viscous flow and elastic deforma-
under different loading conditions. tion can occur simultaneously. Asphalts
The functions of the asphalt binder and asphalt pavements in service are
film are to effect cohesion of the aggre- properly described as generally visco-
gate components, to waterproof the pave- elastic bodies.
ment, and to effectively transmit the
NON-NEWTONIAN BEHAVIORS OF
energy resulting from transient or sus-
PAVING ASPHALTS
tained loads, without unduly deforming
the structure or fracturing the asphalt Measurement of flow properties of
film. The response of this film to thermal asphalts or the deformational character-
2
The boldface numbers in parentheses refer
istics of asphalt pavements is concerned
to the list of references appended to this paper. with their response to the magnitude and

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82 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

duration of the applied stress. Under truly a flow property, it indicates that
static steady-state conditions, flow and the energy input exceeded the cohesive
deformation will depend on the time forces (elastic modulus) of the material
of loading (rate of shear) and tempera- and therefore is important in defining
ture. Under dynamic conditions, de- the strength of the material under im-
formation will be a function of frequency pact conditions.
of loading. The two types of loading are For a purely viscous fluid, rate of shear
correlative, as has been shown by several is proportional to stress without any
investigations (3,6). Both types of load- change in viscosity as shown in A A1

<r
<
B
L<
i> i1
^A
tn
)
u. J
/
o /
UJ / A
1-
<
cc yf
/
SHEAR STRESS RATE OF SHEAR
(a) Versus stress. (b) Versus viscosity.
FIG. 1.—Rate of Shear.

I22F

SHEAR STRESS RATE OF SHEAR


(a) Versus shear stress. (b) Versus rate of shear (temperature).
FIG. 2. -Viscosity.

ings are commonly experienced under curves of Fig. 1. This behavior will pre-
service conditions. vail for asphalts under specific load
The flow behavior of asphalt can vary conditions or until a critical rate of shear
greatly, depending on the conditions is reached, after which it will deviate
under which flow is induced. This can be from pure viscous flow as shown in the
simply demonstrated by taking a strip B segments of the curves. Beyond the
of paving asphalt and pulling it apart critical rate of shear, the mechanical
slowly. It will behave as a viscous fluid. properties of asphalts will depend on the
If it is bent or pulled apart rapidly, but rate of shear, and the asphalts will
not fast enough to fracture, it will show exhibit non-Newtonian or viscoelastic
some elasticity. If struck a rapid blow, it flow. The effects of such viscoelastic
will fracture. Although fracture is not properties become more manifest with

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GZEMSKI ON VlSCOELASTIC PROPERTIES 83

increasing rates of shear. Behaviors in tained for a specific temperature. This


the viscoelastic area were described by maximum viscosity, defined as initial
Van der Poel (8) by a stiffness modulus, viscosity or "the viscosity," is an in-
or a time-dependent elastic modulus. trinsic property of an asphalt (Fig. 2(6)).
Brodnyan (4) resolved this modulus into The initial or Newtonian viscosity ex-

SHEAR RATE

60 120 180 240 300 330


TEMPERATURE, dsg Fahr

FIG. 3.—Viscosity of 95-Penetration Asphalts (from National Asphalt Research Center Reports,
1953).

its viscous and elastic components andl tends over a broader range of shear rate
thereby gave a better insight as to their as the temperature increases. For as-
magnitude under different static and1 phalts having the same penetration,
dynamic loading conditions. initial viscosity at a specific temperature
When the viscosity of a paving asphaltt will vary with the sol-gel nature of the
at temperatures generally below 77 F iss asphalt as shown in Fig. 3. A gel-type
plotted against shear stress (less thanl (95 penetration) asphalt at 32 F can
3000 dynes per sq cm) as shown in Fig. have an initial viscosity of 1015 poises as
2(a), a constant viscosity will be ob- compared to 107 poises at shear rate of

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84 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

1 sec -1 . A sol 95-penetration asphalt, The viscoelastic response of this type of


which in this case is slightly shear sus- asphalt to a constant stress as a function
ceptible, has an initial viscosity of 109 of time is shown in Fig. 4. Curve A A1
poises at this temperature. Viscosity of represents its over-all flow or strain
an asphalt other than its initial value is behavior when a stress is applied over the
defined as an apparent viscosity, since time t\ and then removed. Part of the
each value at a constant temperature will strain is recoverable as shown by curves
depend on the rate of shear. The rate of B1 and C1. This process is, therefore,
change of viscosity with rate of shear is reversible and represents the elastic
referred to as shear susceptibility and, component of strain. Curve C represents
like initial viscosity, can be considered the instantaneous elastic component and
as an intrinsic property of the material. B the delayed part. Curve D represents

— TOTAL
•• •"• INSTANTANEOUS
ELASTIC
^ * * \ ...... DELAYED ELASTIC
I . . . . . VISCOUS FLOW

f B ....
^

\ ^
STRAIN

/ /
— ... V
/..---°-""
t*-*
t| (STRESS REMOVED)
TIME

FIG. 4.—Deformation of Asphalt (Elastic Response).

As the apparent viscosity of an asphalt viscous flow and is not recoverable.


decreases with increasing rate of shear, Curve Bl depicts the rate of elastic
its elastic modulus increases. Both of recovery.
these parameters decrease as temperature This type of strain-time curve, al-
increases and pure viscous flow is ap- though possibly exaggerated here, repre-
proached. These flow components can sents the flow behavior of many asphalts
vary for asphalts which have been ob- under specific conditions. Response to
tained by various processing means such loading (rate of shear) will vary with
as oxidation, reaction with P2O5, or by temperature and the sol-gel characteris-
the addition of rubber, polymer, or filler tics of the asphalt. For a highly sol
products. asphalt, which is essentially a viscous
Brown (9), in his study of the visco- body, the flow behavior under similar
elastic properties of a commercial gel 65- conditions would probably be repre-
penetration paving asphalt describes sented by curve D rather than by curve
this behavior at winter temperatures. A.

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GZEMSKI ON VlSCOELASTIC PROPERTIES 85

ANALYSIS OF PENETRATION The calculations were made, using the


Since asphalts behave in a viscoelastic Pendleton equations (10). A needle-point
manner at service temperatures, and correction parameter was introduced to
because of the large number of asphalt calculate stress. The rate of shear was
sources that are available, it is not sur- calculated from the equation used in the
prising that viscosity-temperature prop- Pochittino moving cylinder viscometer
erties do not correlate with penetration. method. The ASTM dimensions for the
The penetrometer is a moving cylinder- penetrometer cup and needle replaced

TABLE I.—PENETRATION-VISCOSITY RELATIONSHIPS.

Temperature, deg Fahr Penetration Load, g Time, sec Stress, dynes Rate of Viscosity, poises
Grade per sq cm Shear, sec^1

77 200 100 5 1.8 X 10* 1.0 1.8 X 10*


77 60 100 5 8.4 X 10* 0.30 2.8 X 10*
77 30 100 5 2.6 X 10 6 0.15 1.8 X 10 7
39 30 200 60 5.4 X 10 6 0.012 4.3 X 10 8
39 15 200 60 1.6 X 10' 0.006 2.7 X 10 9
77 94 100 5 4.6 X 10* 0.4 9.2 X 10*
77 94 100 0.5 1.9 X 10 6 1.9 10.0 X 10*

200 r-

100

QC 60 -

40

O
O
20

_|_ J_ _L
0.5 I 5 20
LOG TIME, SEC.

FIG. 5.—Penetration at 77 F Versus Time.

type viscometer that indicates an ap- those of the coaxial cylinders. The
parent viscosity under a specific set of apparent viscosity in poises were ob-
conditions. For viscous or Newtonian tained by
asphalts, the penetration value can be stress
converted to viscosity with a relatively viscositv — N = —-
rate of shear
high degree of accuracy, but for as-
phalts having significant shear suscepti- Since viscosities of many paving as-
bility, this conversion is not precise. phalts vary with rate of shear at 77 F
Shear and stress relationships calcu- and lower, the calculated ASTM stand-
lated for different asphalts at different ard penetrometer viscosities for different
penetrometer load-time conditions are asphalt grades (200 to 30) are determined
given in Table I. at different rates of shear and therefore
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86 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

are not comparable. The extent to which With reference to the well-known
differences in asphalt properties, such as penetration ratio 39 F to 77 F viscosity,
shear susceptibility, and the differences comparisons are made under rather
in test conditions can affect the results of different rates of shear as shown below.
the penetration test is shown in the fol-
lowing examples. The literature (11) shows Shear Shear
Stress Rate Viscosity
that log penetration - log time slopes of Penetration
asphalts differ, depending on whether they at 39 F 30 5.4 X 106 0.012 4.3 X 108
are viscous- or elastic-type materials. The Penetration 94 4.6 X 105 0.4 9.2 X 105
lines will intersect at a specific time point at 77 F

0 60 120 180 240 300


TEMPERATURE, Deg Fahr
FIG. 6.—Viscosity of 1961 Paving Asphalts (46 Samples).

and indicate a common penetration for A comparison of this type could be signi-
the asphalts in question. For two sol and ficant if it were intended to reflect a
gel asphalts, each having 74 penetration, particular functional or service condition.
(Fig. 5) the penetrations are 23 and 44 Unfortunately, the penetration test con-
respectively for the first 0.5 sec. Data for ditions were selected because of test
a second pair of sol and gel asphalts limitations, brevity of time, and for the
having a 95 penetration show that the purpose of obtaining large enough num-
lines intersect at this 5-sec period. The bers to ensure reasonable reproducibility.
sol and gel slopes are parallel. The 95- The shear rates for different grades of
penetration gel asphalt intersects the asphalt (200 to 30 penetration) at a
74-penetration sol asphalt at the 11-sec specified ASTM test condition (such as
time interval where they have a common 77 F, lOOg, 5 sec) are significantly differ-
penetration of 110. ent. Equally significant is the difference

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GZEMSKI ON VlSCOELASTIC PROPERTIES 87

in shear rate within the specified time of groups show definite overlapping. The
5 sec. This is shown in Table I for the slopes also differ so that the limiting
0.5-sec time interval for the 94-penetra- curves for some groups cross those of
tion asphalt. Therefore, the characteriza- others.
tion of asphalts by the penetration The convergent group of viscosity-
method, which dimensionally is expressed temperature curves shown in Fig. 7
as length (decimillimeters), does not reveal no distinct pattern of behavior.
adequately define the flow properties of
asphalts. I09 r

EFFECT OF TEMPERATURE
107 -
An analysis of the viscosity-tempera-
ture relationships of 63 asphalt cements
has been reported by Griffith and
10 =
Puzinauskas (see p. 20). For convenience,
these asphalts have been grouped in the
following manner:
io-
Number of Asphalts
Represented by:

Penetration Range Con- Total


Parallel vergent
Viscosity- Viscosity-
Tempera- Tempera-
ture Slopes ture Lines
10 _ PENETRATION RANGE
34 to 60 15 5 20 3 4 to 60
85 to 100 17 7 24
85 to 100
122 to 161 5 1 6
193 to 236
199 to 236 9 4 13

Total 46 17 63

0 60 120 180 240 300


The viscosity-temperature curves were TEMPERATURE, deg Fahr
drawn as straight lines between the FIG. 7.—Viscosity of 1961 Paving Asphalts
experimental data points for 140 and (17 Samples).
275 F and then extrapolated to 77 F. They represent a more varied viscosity
Since the viscosities at the experimental spectrum at each of the three tempera-
temperatures 140 and 275 F are New- tures considered here.
tonian, the extrapolated values at Although it has been generally as-
77 F represent initial viscosities. Further sumed for practically a half century that
extrapolation to any lower temperatures asphalts of the same penetration have
may be carried out to obtain initial similar consistency responses, the data
viscosity, at that temperature. presented here point out a wide variation
For each of the individual penetration in the viscosity-temperature behavior of
groups listed above, Fig. 6 shows the asphalt cements when based on a pene-
limiting viscosity-temperature curves, tration classification.
that is, the highest and lowest curve for
each group. Although the groups based CHANGES IN TEMPERATURE
on penetration at 77 F are distinguished AND RATE OF SHEAR
by penetration gaps between groups, the The viscosity behavior of another
viscosity ranges indicated for the same group of 12 asphalts was studied in the
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SYMPOSIUM ON FUNDAMENTAL VISCOSITY

50 to 275 F range. The rate of shear, shear susceptible with a 10,000 per cent
using the Shell microviscometer at 50 difference in viscosity at 50 F and 1000
and 77 F was varied from 10"4 to 1 sec - 1 to per cent at 77 F for the respective shear
determine the viscosity response to this rates. Shear susceptibility is evident in
parameter. A vacuum capillary and this case at 120 F. The curve represented
Cannon-Manning viscometer were used by the 10" 4 rate of shear point at 50 F
for measurements at 140 F and a Zeit- for asphalt E can be considered the initial
fuchs cross-arm viscometer at 275 F. viscosity-temperature curve for this
particular asphalt. The initial viscosity-
SHEAR RATE SEC" temperature slopes for all four asphalts
10' in this group are parallel. The shear
susceptibility of gel asphalt F (200 to
ASPHALT E
I07 ASPHALT G 300 penetration) at 50 F is small (250 per
cent) compared to 10,000 per cent gel
asphalt E (60 to 70 penetration).
10=
These data illustrate certain basic or
intrinsic properties such as shear sus-
ceptibility and initial viscosity of as-
phalts at service temperatures. They in
turn can bear a significant relationship to
lO 3
performance and durability of asphalt
pavements which are subjected to
various mechanical and environmental
influences.

R A T E OF SHEAR-VISCOSITY-TEMPERA-
TURE RELATIONSHIPS OF ASPHALT
10 -
CEMENTS FROM D I F F E R E N T
C R U D E O I L SOURCES

It has been established that variables


such as asphalt source, temperature,
rate of shear, and grading by penetration
60 120 180 240 300 influence the viscosity of an asphalt
TEMPERATURE, deg Fahr (Fig. 10). Three groups of bar graphs are
FIG. 8.—Asphalt Paving Grade Viscosity Co- shown for 60- to 70-, 85- to 100-, and 200-
operative Asphalt Inst. Program (60- to 70- to 300-penetration grade asphalts. The
Penetration Asphalts).
effect of rate of shear (1 sec^1 to 10 - 4
sec -1 ) on viscosity is shown for each
Figures 8 and 9 represent two sol and
group at 50, 77, 140, and 275 F. Six
two gel commercial asphalts. This group
was recently used in the asphalt industry- different asphalt sources are reported for
Asphalt Inst, asphalt viscosity study. the 60- to 70- and 200- to 300-penetra-
Asphalts G and H are 60 to 70 and 200 to tion grades and eight for the 85- to 100-
300 penetration sol asphalts respectively, penetration grade.
and E and F are the gel counterparts. The results shown in Fig. 10 can be
The sol asphalts are not shear susceptible summarized as follows:
in the shear range considered. The gel 1. The 60- to 70-penetration grades at
60 to 70 asphalt (asphalt E) is decidedly 50 and 77 F are most shear susceptible.

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GZEMSKI ON VlSCOELASTIC PROPERTIES 89

The 200- to 300-penetration grades are however, the differences are smaller than
the least shear susceptible. at 50 F.
2. Greater shear susceptibility is 5. Asphalt 1, a propane asphalt, is
shown at 50 F than at 77 F. essentially Newtonian under all described
3. With the exception of asphalt 8, test conditions, whereas the oxidized
essentially no shear susceptibility is asphalt cements appear to be non-New-
evident at 140 F. tonian or most shear susceptible under

8 _SHEAR RATE SEC"


10'
10"'
I

I06 -

10+ -

ASPHALT H

<o

to

10

-20 0 60 120 180 240 300


TEMPERATURE, dag Fahr

FIG. 9.—Asphalt Paving Grade Viscosity Cooperative Asphalt Inst. Program (200- to 300-Pene-
tration Asphalts).

4. Where shear susceptibility is indi- similar conditions. The group of four


cated, the viscosity increases as the Venezuelan asphalts showed a variable
rate of shear decreases. For example, response.
at 50 F asphalt 8, in the 60- to 70-penetra- These data illustrate the several
tion group, has a viscosity of 4 X 106 parameters which govern the viscosity
poises at 1 sec"1 shear rate and 1.5 X 109 of an asphalt cement and the need for
poises at 10~4 sec -1 rate of shear. In con- precisely indicating the conditions for
trast, asphalt 1 under the same condi- a particular viscosity measurement.
tions shows very little susceptibility.
VISCOELASTIC PROPERTIES or ASPHALT
This holds true for the higher penetra-
PAVING MIXTURES
tion grades also; however the differences
become smaller with increasing penetra- The current practice in the design of
tion. The same is true at 77 F. Over-all, asphalt pavements and the control of
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90 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

pavement construction is of the same this can be illustrated from the research
general order of quality as the measure- by Wood (13) on the effect of compression
ment of asphalt properties by means of speed on the Marshall stability of as-
the penetration test. Whereas sample phalt concrete. As the rate of deforma-
preparation for testing mixtures has tion shown in Fig. 11 decreased, the
received considerable attention and prog- Marshall stability decreased. The rate of

i i0"2 icr4 i io~2 i0"4 i IO -2 lo - 4


SHEAR RATE, SEC"1
PEK-
60 to 70 85 to 100 200 to 300
FIG. 10.—Asphalt Paving Grade Viscosity.

ress has been made in that direction, strain at the normal rate of 2 in. per min
such testing has been developed pri- deformation is 8 X 10~3 sec -1 and at the
marily for speed rather than for the 0.002 in. per min rate it decreases to
measurement of parameters which might 8 X 10 -6 sec -1 . These data could be
reflect service conditions. Methods cur- interpreted as meaning that the material
rently used in the measurement of has a higher elastic (compression)
mechanical properties of paving mixtures modulus at the higher rate of shear than
are disassociated from stress-strain pat- at the lower one. Naturally particle
terns of behavior and from the effect friction is an important factor in either
of time of loading. A good example of case. This raises a very basic question as
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GZEMSKI ON VlSCOELASTIC PROPERTIES 91

to the engineering significance of the the moduli obtained by each of these test
Marshall test or other similar tests which methods when the rates of deformation
attempt to correlate pavement perform- are the same.
ance of a viscoelastic body from a single The Marshall tests and others would
point on a hypothetical stress-strain be more meaningful if the deformation
curve at a single rate of strain. characteristics were defined by a com-
A further complication in our current plete stress-strain curve. This type of
testing practices for asphalt pavements test development is now in progress at
stems from the fact that the testing the Pennsylvania State Highway Dept.
conditions for the better known test laboratory (IS). The effect of other

1400 • -

1200

800

<r> 6 0 0 -
<
5

400

200
0.001 0.01 0.1 1.0
COMPRESSION SPEED. IN. PER MIN.

FIG. 11.—Effect of Marshall Compression Rate.

methods are different. Please (14) re- variables such as rate of deformation and
ported the following calculated shear temperature are also being considered.
rates for three test methods: The Marshall test begins to have more
significance when the data are correlated
Test Method Compressive R a t e with viscosity. The data of Adam (16) of
of Strain, sec - 1
the Louisiana Department of Highways
Marshall 8 X 10" 3 and Please (14) of the British Road
Hveem stabilometer 3 X VT* Research laboratory show a definite
Triaxial 2 x i(r 6 proportionality between Marshall sta-
bility and asphalt binder viscosity at
It can be safely assumed that each of 140 F. These data are shown in Fig. 12.
the test methods measure a different Significantly a ten-fold increase in asphalt
service condition, yet each of the viscosity results in a two-fold increase in
methods are used to do the same design Marshall stability.
job. It would be interesting to compare We can expect real progress, however,
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92 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

only when we expand the scope of this 2. Both moduli increase with increas-
development as exemplified in the works ing frequency or rate of shear.
of Papazian (6), Secor and Monismith 3. The transverse modulus is nomi-
(7), and others. As in the case of the nally two to three times the elastic
published work of the National Asphalt modulus and is a function of the axial
Research Center on the viscoelastic stress.
behavior of asphalts, these works have 4. Both the elastic and transverse
considered the viscoelastic behaviors of moduli increase with increasing viscosity
asphalt pavements, the approach being (decreasing penetration).
one of the resolution of the viscous and 5. Both moduli decrease with in-
elastic components under different static creasing amounts of asphalt.

1500 r 60 to 70 PEN.
85 to 100 PEN.
o 120 to 150 PEN.
\ 200 to 300 PEN.
< \
1000 > .

< ^
i-
to
_j

< 500
X
(O
or
< I i 1 _1
s _1_

10" I03 10*


VISCOSITY AT I 4 0 F , POISES

FIG. 12.—Marshall Stability Versus Asphalt Viscosity.

TABLE II—RATES OF SHEAR IN 6. Both elastic modulus and tractive


PAVEMENT PERFORMANCE.
viscosity decrease with increasing tem-
Rate of Shear, sec ' Deformation Condition perature.
3 X 1(T 7 Settlement RATE OF SHEAR IN PAVEMENT
2 X 1CT5 Light loads (static) PERFORMANCE
3 X 10~ 4 H e a v y loads (static)
2 X KT1 P e n e t r a t i o n test The asphaltic pavement as we know
1 X 10 1 M o v i n g traffic (slow)
1 X 10 3 M o v i n g traffic (fast)
it is a flexible-type structure which by
performance standards behaves visco-
elastically. Table II shows that the pave-
and dynamic loading conditions and ment is subject to a broad spectrum of
temperatures. stress conditions. These data were ob-
The nature of this research work can tained from several sources (3,13,17). This
be best summarized from the data from means that under favorable conditions
Papazian (6). These data illustrate the it is desirable that the film respond in a
following viscoelastic responses: viscous manner in one case and elastically
1. Both the elastic and transverse in another. Under unfavorable condi-
moduli decrease with increasing tem- tions, due to poor base support, poor
perature at a constant frequency or rate design, excess of binder, and undesirable
of shear. asphalt properties, adverse effects can
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GZEMSKI ON VlSCOELASTIC PROPERTIES 93

result from any one or more of several The status of our current methods for
deformation conditions in action at the testing asphalt paving mixtures was dis-
time. The effect of different rates of shear cussed in relation to the parameters
is related to the existing temperature. involved. As in the case of asphalts, the
Settlement is a long duration process analysis of the needs for basic methods
(low rate of shear (3 X 10"-7 sec-1)) and of characterization applies equally to
can occur over a wide range of tempera- paving mixtures.
tures, it is more rapid at the higher sum- An analysis of the penetrometer as a
mer temperatures if an unstable base viscometer showed that a single measure-
condition exists. Cracking due to exces- ment of an asphalt as now specified by
sive strain can occur as settlement con- the ASTM penetration test is of little
tinues. Thermal stressing is associated value since the calculated values of the
with relatively low rates of shear of 10~4 stress and shear parameters of viscos-
sec -1 and, if temperature drops are rapid, ity—and therefore the viscosities—are
film fracture can occur if the resultant variable for the duration of the test and
stresses are greater than the elastic also from grade to grade. The penetra-
modulus of the film. Stresses are set up tion-time slope varies with asphalt type.
as the result of differences in the coeffi- The same variations apply to measure-
cients of expansion of the asphalt film ment of penetration at different tempera-
and the aggregate. tures.
Shoving can occur at 77 F and higher The viscosity-temperature properties
in 4 X 10_1 sec -1 range. Indentation of a large group of commercial paving
occurs under static load conditions asphalts have been evaluated. The
(10~4 to 10~5 sec4). Bleeding occurs under viscosity-temperature slopes for specific
moderate moving traffic conditions grades varied considerably. There is no
usually during summer season. correlation with penetration at 77 F.
Ravelling requires fast traffic condi- Viscosity-temperature behavior at 10 -4
tions (103 sec-1) and usually is manifest to 1 s e c 1 shear rates was discussed for
at lower temperatures. sol and gel types of asphalt. Sol asphalts
Cracking is the result of moving traffic were not shear susceptible in the shear
(101 to 103 sec^1) and is the result of rate range studied and can be represented
undue deformation or hardening of the by a single viscosity curve. Gel asphalts
asphalt. were shear susceptible at temperatures
usually below 100 F. Gel asphalts can be
SUMMARY represented by initial viscosity-tem-
This review of the viscoelastic proper- perature curves. These curves represent
ties of asphalts and asphalt concretes the viscosity of asphalts either at low
pointed out that these properties change rates of shear, where they are no longer
with rate of shear, temperature, asphalt shear susceptible or at high temperatures
type, and in general with service condi- where they are not shear susceptible. It
tions. It was also pointed out that the was suggested that initial viscosity-
rate at which these properties change temperature slope and shear susceptibil-
should be the final criterion in the char- ity are intrinsic properties of asphalts and
acterization of these materials and pave- therefore can reflect the deformation
ment performance. behavior of asphalt pavements.

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94 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

REFERENCES

(1) C. Mack, "Physical Properties of Asphalts and Its Relation to Routine Test Data,"
in Thin Films," Industrial and Engineering Journal of Applied Chemistry (London),
Chemistry, Vol. 44 (1957), p. 422. Vol. 4 (1954), p. 221.
(2) P. R. Wood, "Rheology of Asphalts and (9) A. B. Brown, "Viscoelastic Properties of a
Its Relation to Behavior in Paving Mix- Penetration Grade Paving Asphalt at
tures," Bulletin 192, Highway Research Winter Temperature," Proceedings, Assn.
Board, 1958, pp. 20-25. Asphalt Paving Tech., Vol. 27 (1958), p. 35.
(3) National Asphalt Research Center Reports (10) W. W. Pendleton, "The Penetrometer
(unpublished). Method for Determining the Flow Proper-
(4) J. C. Brodyan, "Use of Rheological and ties of High Viscosity Fluids," Journal of
Other Data in Asphalt Engineering Applied Physics, Vol. 14 (1943), p. 170.
Problems," Bulletin 192, Highway Re- (11) R. N. J. Saal and J. W. A. LaBout, "Rela-
search Board, 1958, pp. 1-19. tion Between Asphaltic Viscosity and
(5) H. F. Gaskins, J. G. Brodnyan, W. Philli- Penetration of Asphaltic Bitumens,"
poff, and E. Thelen, The Rheology of Physics, Vol. 7 (1936), p. 408.
Asphalt: Part II, "Flow Characteristics of (12) Asphalt Inst, (unpublished data).
Asphalt;" Part III, "Dynamic Mechanical (13) P. R. Wood, "Rheology of Rubberized
Properties of Asphalt," Transactions, Soc. Asphalts" (unpublished).
Rheology, 1960, pp. 265-298, 279-296. (14) A. Please, "Use of the Marshall Test for
(6) H. S. Papazian, "The Response of Linear Evaluating Dense Bituminous Surfacings,"
Viscoelastic Materials in the Frequency Journal of Applied Chemistry, Vol. 11
Domain, A Dissertation," Report No. (1961), p. 73.
172-2, Engineering Experiment Station, (15) J. Kofalt, private communication, Pennsyl-
The Ohio State University, December, vania Dept. of Highways, Harrisburg, Pa.
1961. (16) V. Adams, "Effects of Viscosity in Bi-
(7) K. E. Secor and C. L. Monismith, "Visco- tuminous Construction," ASTM STP No.
elastic Properties of Asphalt Concrete," 309, Am. Soc. Testing Mats., 1962, p. 121.
presented at 41st Annual Meeting, High- (17) G. M. Dormon and H. W. Jarman, "Some
way Research Board, 1962. Factors Influencing the Behavior of
(8) C. Van der Poel, "General System De- Bitumen Road Surfacings," Journal of
scribing Viscoelastic Properties of Bitumen Applied Chemistry, Vol. 8 (1958), p. 832.

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STP328-EB/Apr. 1963

SUM?
BY F. J. BENSON1

Asphaltic materials have been suc- This symposium has been concerned
cessfully used as waterproofers and with the viscosity of asphaltic materials.
adhesives for many years. ASTM speci- Viscosity is defined as "that property or
fications for asphaltic materials date quality of gaseous or fluid bodies, re-
back to the earliest years of the society. sulting from molecular attraction, which
Most authorities, however, admit that makes them offer a resistance to flow."2
asphalt technology is still more art than Griffith and Puzinauskas note that a
science. Although asphalt technology is number of test procedures are used to
hampered by several testing procedures assess this quality including penetration
and theories that are more traditional (at several temperatures), ductility,
than factual and scientific, these proce- softening point, and Saybolt Furol
dures and theories have persisted because viscosity. The units for these procedures
nothing better has been offered in are, respectively, penetration in 0.1 mm,
replacement. ductile elongation at failure in centi-
The fact that asphalts are chemically meters, temperature in degrees, and flow
extremely complex materials was stated time in seconds. All of these procedures
or implied in all of the papers of the presumably measure resistance to flow
symposium. Furthermore, there are under certain fixed conditions. In fair-
fundamental differences in asphalts, even ness, it must be noted that they have
when they all meet the same current served the profession well.
specification. Variability exists for ma-
terials meeting the specifications in both Significant Points in Common:
chemical composition and physical prop- The important points concerning the
erties. The profession has only limited viscosity of asphaltic materials presented
knowledge of the fundamental properties in this symposium are summarized as
of asphaltic materials and even less follows:
knowledge of the effect of their properties 1. The viscosity of an asphalt changes
when they are used as binders and with temperature. This well-established
waterproofers in pavements. These gaps fact was included in each paper of the
in our knowledge were discussed by symposium.
Welborn, Halstead, and Olsen. It seems 2. The viscosity over an appreciable
reasonable to conclude, therefore, that range of temperature, including the
any attempt to develop a better funda- normal temperature range of use, is de-
mental understanding of asphaltic ma- pendent on the rate of loading for many
terials and the meaning of their physical asphaltic materials. Griffin, Izatt, and
and chemical properties is important to Lettier presented data supporting this
asphalt technologists. principle of asphalt viscosity.
1 2
Dean of Engineering and Executive Officer, Webster's New Twentieth Century Dic-
Texas Transportation Inst., A & M College of tionary, Unabridged, Second Edition, 1960,
Texas, College Station, Tex. p. 2043.

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96 SYMPOSIUM ON FUNDAMENTAL VISCOSITY

3. Asphaltic materials meeting current for mixing, distributor application,


specifications for the same grade may spreading, compaction, and use can be
have rather different viscosities at the stated in terms of this fundamental
standard temperature and substantially unit, thus avoiding the confusion of a
different viscosity temperature relation- number of methods and units for the
ships. Griffith and Puzinauskas gave measurement of viscosity.
evidence to support this point in their A second reason for changing to a
paper. fundamental method for evaluating the
4. Asphaltic materials increase in viscosity of asphaltic materials is to
viscosity during mixing and placing achieve uniformity in the specifications.
operations and with time in service in Our present use of the many procedures
the pavement. This was noted by and units for the expression of viscosity
Welborn, Halstead, and Olsen and by at different temperatures for the same
Griffin, Izatt, and Lettier. material and for different materials at
5. The viscosity of asphaltic materials the same temperature can lead only to
is important in determining the physical confusion. Only the most experienced
characteristics of the mixtures in which practitioners can interpret penetration,
the materials are used, particularly the softening point, and Furol viscosity in
stability values as measured by many of terms of the actual physical state of the
the stability test procedures. Welborn,
material. Interpretations based on funda-
Halstead, and Olsen covered these
mental viscosity should be easier to
influences in considerable detail.
make and less subject to errors in judg-
Griffin et al point out the importance
ment when mastered by the professional
of viscosity in the use of asphaltic
people dealing with asphaltic materials.
materials. They state that proper mixing
of asphaltic materials with aggregates A third reason is the fact that control
depends upon having the asphalt at the procedures will be simplified. If the
proper viscosity during mixing. Others viscosity can be measured easily and
have shown that viscosity is a factor in rapidly over a broad temperature range
distributor application. In the spreading with a single instrument, then it can be
and compaction of mixtures, the time- easily used both for the control of
temperature-viscosity relationship is very refinery operations and for checking
important. Significant stresses occur in materials for compliance with the
the pavement under widely differing specifications. Present time-consuming
shear rates, with deflections under methods are virtually valueless for
traffic being a high-shear-rate process refinery control, and the time lag in-
and stresses from thermal effects a low- volved in the methods leaves much to be
shear-rate process. desired in their use to determine com-
pliance. Rapid tests for control of
Why Measure in Fundamental Units? materials in manufacture and use are
In the past, viscosity of asphalt has required to supply the needs of the
been used only for the specification of profession.
materials; today it is recognized as a tool A change to fundamental units for the
for design and for construction control. measurement and statement of the
For these purposes a single method or viscosity of asphaltic materials is de-
unit for evaluating viscosity has an pendent upon the development and
advantage. The proper viscosity range general acceptance of one or two test

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SUMMARY 97

procedures which will yield the needed Conclusions:


information rapidly for a broad range of The use of fundamental units for the
temperatures, such as 40 to 300 F. viscosity of asphaltic materials, over the
range of temperatures of interest, is an
Studies of A vailable Instruments and Test
excellent method for fixing and evalu-
Procedures:
ating this property of asphaltic materials.
Griffith and Puzinauskas reported the Viscosity is valuable for specification
studies being made by The Asphalt purposes, for estimating strength or
Inst, and its members with several types stability, for the control of materials
of viscometers. Levy and Gagle discussed during construction operations, and for
the methods for measuring absolute evaluating in-service changes in the
viscosity and the instruments and pro- materials. The development of equip-
cedures that are available for making the ment and methods of testing to measure
measurements. Although adequate in- viscosity in fundamental units, within
struments and procedures are not now the range of temperatures and shear
available for making fundamental vis- rates of interest, is the subject of much
cosity measurements, the studies are serious study that should result in a
promising and the measurement problem solution acceptable to the asphalt
will probably be solved satisfactorily. technologist.

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i H I S PUBLICATION is one of many
issued by the American Society for Testing and Materials
in connection with its work of promoting knowledge
of the properties of materials and developing standard
specifications and tests for materials. Much of the data
result from the voluntary contributions of many of the
country's leading technical authorities from industry,
scientific agencies, and government.
Over the years the Society has published many tech-
nical symposiums, reports, and special books. These may
consist of a series of technical papers, reports by the
ASTM technical committees, or compilations of data
developed in special Society groups with many organiza-
tions cooperating. A list of ASTM publications and
information on the work of the Society will be furnished
on request.
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