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Designation: D4402/D4402M  −  13

Standard Test Method for


Viscosity Determination of Asphalt at Elevated
Temperatures Using a Rotational Viscometer 1
This standard is issued under the fixed designation D4402/D4402M; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

1. Sco
Scope
pe 3.1.2  filled asphalt, n— an
an asphalt blend that contains finely
1.1 This test method outlines
outlines a procedure
procedure for measuring
measuring the dispersed insoluble mineral matter.
apparent viscosity of asphalt from 38 to 260°C [100 to 500°F] 3.1.3   Newtonian
Newtonian liquid
liquid,, n— a liquid for which the rate of 
using
using a rot
rotatio
ational
nal vis
viscom
cometer
eter and a temp
tempera
eratur
ture-c
e-cont
ontrol
rolled
led shear is proportional to the shearing stress. The constant ratio
thermal chamber for maintaining the test temperature. of the shearing stress to the rate of shear is the viscosity of the
1.2 The values stated in either SI units or inch-pound
inch-pound units liquid
liquid.. The vis
viscos
cosity
ity of a New
Newton
tonian
ian liq
liquid
uid is the
theref
refore
ore not
are to be regarded separately as standard. The values stated in dependent on its shear rate. If the ratio is not constant, the
each system may not be exa exact
ct equ
equiva
ivalen
lents;
ts; the
theref
refore
ore,, each liquid is non-Newtonian. Many liquids exhibit both Newtonian
system shall be used independently of the other. Combining and non-Newtonian behavior, depending on the shear rate or
values from the two systems may result in non-conformance temperature, or both.
with the standard. 3.1.4   shear rate, n— the
the measure of the speed at which the
1.3   This standar
standard d doe
doess not purport
purport to add
addreress
ss all of the intermediate layers of the liquid move with respect to each
safet
safetyy co
conc
ncer
erns
ns,, if an
anyy, as
asso
socia
ciate
ted
d wi
with
th its ususe.
e. It is th
thee other. Its unit of measure is the reciprocal second (sec -1).
responsibility of the user of this standard to establish appro- 3.1.5   shear
shear str
stress,
ess, n— the
the force per uni
unitt are
areaa req
requir
uired
ed to
 priate safety and health practices and determine the applica- produce the shearing action. Its SI unit of measurement is the
bility
bility of reregul
gulato
atory
ry limi
limitati
tations
ons pri
prior
or to use
use.. See   10.6 for pascal, and its cgs unit of measurement is dynes/cm 2.
specific precautionary information.
3.1.6   viscosity, n— the
the ratio between the applied shear stress
2. Referenc
Referenced
ed Documents
Documents and the rate of shear is called the coefficient of viscosity. This
coefficient is a measure of the resistance to flow of the liquid.
2.1   ASTM Standards: 2 Thee SI un
Th unit
it of vi
visc
scos
osity
ity is th
thee pa
pasc
scal
al se
seco
cond
nd (P
(Pa·s
a·s).
). Th
Thee
E644 Test
E644  Test Methods for Testing Industrial Resistance Ther- centime
cen timetre
tre gram sec second
ond (cgs) unit of visviscos
cosity
ity is the poise
mometers 2
(dyne·s/cm ) and is equivalent to 0.1 Pa·s. Frequently, centi-
E1137 Specification
E1137  Specification for Industrial Platinum Resistance Ther- poise (cP)—equal to one millipascal second (mPa·s)—is used
mometers as the viscosity unit.

3. Terminology 3.2  Definitions of Terms Specific to This Standard:


3.2.1   apparatus-
apparatus-measu
measuring
ring geome
geometry
try,, n— the
t he pa
part
rt of ththee
3.1   Definitions:
equipment that is immersed in the asphalt sample, the dimen-
3.1.1  apparent viscosity, n— the
the ratio of shear stress to shear
sions
sions of whiwhich
ch are used, in con
conjun
junctio
ction n wit
withh the rotationa
rotationall
rate for a Newtonian or non-Newtonian liquid.
resisti
resisting
ng tor
torque
que,, to calc
calcula
ulate
te the app
apparearent
nt vis
viscos
cosity
ity.. Thi
Thiss
geometry may be referred to by the equipment manufacturer as
a spindle, bob, inner concentric cylinder, vane, and so forth.
1
This test method is under the jurisdiction of ASTM Committee D08
Committee D08 on  on Roofing
and Waterproofi
Waterproofing ng and is the direct respo
responsibil
nsibility
ity of Subco
Subcommitte
mmitteee   D08.03 on
Surfacing
Surfacing and Bitum
Bituminous
inous Materials for Membra
Membrane ne Waterpr
aterproofing
oofing and Built
Built-up
-up 4. Summ
Summary
ary of Test
Test Method
Roofing.
Curren
Cur rentt edi
editio
tion
n app
approv
roved
ed Jun
Junee 15, 201
2013.
3. Pub
Publis
lished
hed Jul
July
y 201
2013.
3. OriOrigin
ginall
ally
y
4.1 A rotati
rotational
onal viscometer
viscometer,, as described in this test method,
method,
approved in 1984. Last previous edition approved in 2012 as D4402 – 12. DOI: is used to measure the apparent viscosity of asphalt at elevated
10.1520/D4402_D4402M-13. tempe
tem perat
ratur
ures.
es. Th
Thee tor
torqu
quee on the ap appar
paratu
atus-
s-mea
measu
surin
ring
g
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
geometr
geo metry y, rot
rotatin
ating
g in a the
thermo
rmosta
statica
tically
lly con
contro
trolled
lled sam
sample
ple
contact ASTM Customer Service at service@astm.org. For  Annual Book of ASTM 
Standards volume information, refer to the standard’s Document Summary page on holder containing a sample of asphalt, is used to measure the
the ASTM website. relativee resistance to rotatio
relativ rotation.
n. The torque and speed are used to

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4402/D4402M − 13

determine the viscosity of the asphalt in pascal seconds, 9. Calibration and Standardization
millipascal seconds, or centipoise.
9.1 The viscometer shall be zeroed before use, or as needed,
or both, according to the manufacturer’s instructions.
5. Significance and Use
9.2 The accuracy of the viscometer shall be checked at least
5.1 This test method is used to measure the apparent
annually using a certified reference fluid of known viscosity at
viscosity of asphalts at handling, mixing, or application tem-
various temperatures, using the method described by the
peratures.
supplier of the reference fluid. The reference fluid shall be
5.2 Some asphalts may exhibit non-Newtonian behavior certified to be Newtonian in behavior over the full range of 
under the conditions of this test method, or at temperatures expected test temperatures and shear rates. The reference fluid
within the range of this test method. Since non-Newtonian shall be certified at a temperature within 50°C [90°F] of the
viscosity values are not absolute properties, but reflect the temperature(s) to be used during the test. The viscosity
behavior of the fluid within the particular measurement system, measured shall be within 62 % of the certified value, or the
it should be recognized that measurements made by this test viscometer requires recalibration.
method may not always predict field performance under the
conditions of use. 9.3 The accuracy of the temperature reading and the tem-
perature stability of the temperature controller are to be
5.3 Comparisons between non-Newtonian viscosity values checked at least every six months by placing an asphalt sample
should be made only for measurements made with similar or high flash point oil in the test chamber, and equilibrating to
conditions of temperature, shear rate, and shear history. a temperature within 50°C [90°F] of the temperature(s) to be
used during the test. The sample temperature shall then be
6. Apparatus measured to within 60.1°C [60.2°F] by using a NIST trace-
6.1  Rotational Viscometer,  capable of measuring the torque able measuring device, as described in Test Methods  E644. If 
required to rotate the selected apparatus-measuring geometry at any temperature differential is indicated, the set point of the
a selected constant speed while submerged in asphalt at temperature controller shall be offset accordingly.
constant desired test temperature, and with the capability to
convert the torque measurement to viscosity in pascal seconds, 10. Procedure
millipascal seconds, or centipoise. This calculation may need
10.1 Follow the manufacturer’s instructions for the opera-
to be done manually for some instruments.
tion of the instrument.
6.2   Apparatus-measuring geometry , of various shapes and
10.2 Allow the instrument electronics to warm up for at
sizes, for measurement of various viscosities of asphalt.
least five minutes before conducting any calibrations or analy-
6.3   Temperature-Controlled Thermal Chamber Heater, for ses.
maintaining the sample of asphalt at the test temperature.
10.3 Set the temperature controller to the desired test
6.4   Sample Chambers , reusable or disposable. temperature, taking into account any offset determined in 9.3.
6.5   Temperature Controller,   capable of maintaining the 10.4 Select an apparatus-measuring geometry that will de-
specimen temperatures to 61.0°C [62.0°F] for test tempera- velop a resisting torque between 10 and 98 % of the instrument
tures between 38 and 150°C [100 to 300°F] and to 62.0°C capacity at the selected speed. Generally, measurements will be
[64.0°F] for test temperatures between 150 and 260°C [300 to more accurate at higher torque readings.
500°F].
10.5 Preferably, preheat the sample chamber and the se-
6.6   Balance,  readable to 0.1 g, for determining the mass of  lected apparatus-measuring geometry until temperature equi-
asphalt sample. librium has been obtained for at least 15 min. If filled asphalts
6.7   Platinum Resistance Thermometer (PRT),  with a probe are being measured, this step is mandatory.
which conforms to the requirements of Specification   E1137,
10.6 Add the volume of sample specified by the manufac-
for measuring the temperature of the thermal chamber. The
turer for the apparatus-measuring geometry to be used to the
PRT shall have a 3- or 4-wire connection configuration and
sample chamber. A convenient way for measuring the volume
overall sheath length shall be at least 50 mm [2 in.] greater than
is by weighing out the amount calculated from approximate
the immersion depth. Calibrate the PRT system (probe and
density data for the sample and then returning the sample
readout) in accordance with Test Methods  E644.
chamber to the temperature controlled chamber heater. Thor-
oughly stir filled asphalts to obtain a representative sample
7. Reagents and Materials
before weighing.
7.1 Solvents for cleaning sample chamber, apparatus- NOTE  1—Exercise caution to avoid sample overheating, and to avoid
measuring geometry, and accessories. the ignition of samples with low flash points.
10.7 Do not overfill the sample chamber, but ensure that the
8. Preparation of Apparatus measuring portion of the apparatus-measuring geometry will
8.1 The rotational viscometer and thermal chamber heater be completely immersed. Follow the manufacturer’s instruc-
shall be leveled and prepared as recommended by the instru- tions. The sample volume is critical to meet the system
ment manufacturer. calibration standard.
D4402/D4402M − 13

14. Keywords
14.1 asphalts; rotational viscometers; viscosities

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