ASTM D4402/D4402M-23

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Designation: D4402/D4402M − 15 (Reapproved 2022) D4402/D4402M − 23
Standard Test Method for
Viscosity Determination of Asphalt at Elevated
Temperatures Using a Rotational Viscometer
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 U.S. Department of Defense.
1. Scope
1.1 This test method outlines a procedure for measuring the apparent viscosity of asphalt from 3840 to 260 °C [100 to 500 °F]
using a rotational viscometer and a temperature-controlled thermal chamber for maintaining the test temperature.
1.2 The values stated in either SI units or cgs and inch-pound units are to be regarded separately as standard. The values stated
in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used
independently of the other, and values from the two systems shall not be combined.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. See 10.6 for specific precautionary information.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
E644 Test Methods for Testing Industrial Resistance Thermometers
E1137/E1137M Specification for Industrial Platinum Resistance Thermometers
E2975 Test Method for Calibration or Calibration Verification of Concentric Cylinder Rotational Viscometers
3. Terminology
3.1 Definitions:
3.1.1 apparent viscosity, n—the ratio of shear stress to shear rate for a Newtonian or non-Newtonian liquid.
3.1.2 filled asphalt, n—an asphalt blend that contains finely dispersed insoluble mineral matter.
3.1.3 Newtonian liquid, n—a liquid for which the rate of shear is proportional to the shearing stress. The constant ratio of the
This test method is under the jurisdiction of ASTM Committee D08 on Roofing and Waterproofing and is the direct responsibility of Subcommittee D08.03 on Surfacing
and Bituminous Materials for Membrane Waterproofing and Built-up Roofing.
Current edition approved May 1, 2022Feb. 15, 2023. Published May 2022February 2023. Originally approved in 1984. Last previous edition approved in 20152022 as
D4402/D4402M – 15.D4402/D4402M – 15 (2022). DOI: 10.1520/D4402_D4402M-15R22.10.1520/D4402_D4402M-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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 the ASTM website.
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D4402/D4402M − 23
shearing stress to the rate of shear is the viscosity of the liquid. The viscosity of a Newtonian liquid is therefore not dependent
on its shear rate. If the ratio is not constant, the liquid is non-Newtonian. Many liquids exhibit both Newtonian and non-Newtonian
behavior, depending on the shear rate or temperature, or both.
3.1.3.1 Discussion—
The constant ratio of the shearing stress to the rate of shear is the viscosity of the liquid. The viscosity of a Newtonian liquid is
therefore not dependent on its shear rate. If the ratio is not constant, the liquid is non-Newtonian. Many liquids exhibit both
Newtonian and non-Newtonian behavior, depending on the shear rate or temperature, or both.
–1
3.1.4 shear rate, n—the measure of the speed in reciprocal seconds (sec ) at which the intermediate layers of the liquid move with
–1
respect to each other. Its unit of measure is the reciprocal second (sec ).
3.1.5 shear stress, n—the force per unit area required to produce the shearing action. Itsin pascals (Pa) for SI or dynes/cm SI unit
of measurement is the pascal, and its cgs unit of measurement is dynes/cmfor cgs required to produce the shearing action. .
3.1.6 viscosity, n—the ratio between the applied shear stress and the rate of shear is called the coefficient of viscosity. This
coefficient is a measure of the resistance to flow of the liquid. The SI unit of viscosity is the pascal second (Pa·s). The centimetre
gram second (cgs) unit of viscosity is the poise (dyne·s/cm ) and is equivalent to 0.1 Pa·s. Frequently, centipoise (cP)—equal to
one millipascal second (mPa·s)—is used as the viscosity unit.
3.1.6.1 Discussion—
This coefficient is a measure of the resistance to flow of the liquid. The SI unit of viscosity is the pascal second (Pa·s). The
centimetre gram second (cgs) unit of viscosity is the poise (dyne·s/cm ) and is equivalent to 0.1 Pa·s. Frequently, centipoise
(cP)—equal to one millipascal second (mPa·s)—is used as the viscosity unit.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 apparatus-measuring geometry, n—the part of the equipment that is immersed in the asphalt sample, the dimensions of
which are used, in conjunction with the rotational resisting torque, to calculate the apparent viscosity. This geometry may be
viscosity referred to by the equipment manufacturer as a spindle, bob, inner concentric cylinder, vane, and so forth.
4. Summary of Test Method
4.1 A rotational viscometer, as described in this test method, is used to measure the apparent viscosity of asphalt at elevated
temperatures. The torque on the apparatus-measuring geometry, rotating in a thermostatically controlled sample holder containing
a sample of asphalt, is used to measure the relative resistance to rotation. The torque and speed are used to determine the viscosity
of the asphalt in pascal seconds, millipascal seconds, or centipoise.
5. Significance and Use
5.1 This test method is used to measure the apparent viscosity of asphalts at handling, mixing, or application temperatures.
5.2 Some asphalts may exhibit non-Newtonian behavior under the conditions of this test method, or at temperatures within the
range of this test method. Since non-Newtonian viscosity values are not absolute properties, but reflect the behavior of the fluid
within the particular measurement system, it should be recognized that measurements made by this test method may not always
predict field performance under the conditions of use.
5.3 Comparisons between non-Newtonian viscosity values should be made only for measurements made with similar conditions
of temperature, shear rate, and shear history.
6. Apparatus
6.1 Rotational Viscometer, capable of measuring the torque required to rotate the selected apparatus-measuring geometry at a
selected constant speed while submerged in asphalt at constant desired test temperature, and with the capability to convert the
torque measurement to viscosity in pascal seconds, millipascal seconds, or centipoise. This calculation may need to be done
manually for some instruments.
NOTE 1—A dynamic shear rheometer meeting the requirements of 6.1 is also acceptable.
D4402/D4402M − 23
6.2 Apparatus-Measuring Geometry, of various shapes and sizes, for measurement of various viscosities of asphalt.
6.3 Temperature-Controlled Thermal Chamber Heater, for maintaining the sample of asphalt at the test temperature.
6.4 Sample Chambers, reusable or disposable.
6.5 Temperature Controller, capable of maintaining the specimen temperatures to 61.0 °C [62.0 °F] for test temperatures between
38 and 150 °C [100 to 300 °F] and to 62.0 °C [64.0 °F] for test temperatures between 150 and 260 °C [300 to 500 °F].
6.6 Balance, readable to 0.1 g, for determining the mass of asphalt sample.
6.7 Platinum Resistance Thermometer (PRT), with a probe which conforms to the requirements of Specification E1137/E1137M,
for measuring the temperature of the thermal chamber. The PRT shall have a three- or four-wire connection configuration and
overall sheath length shall be at least 50 mm [2 in.] greater than the immersion depth. Calibrate the PRT system (probe and readout)
in accordance with Test Methods E644.
7. Reagents and Materials
7.1 Solvents for cleaning sample chamber, apparatus-measuring geometry, and accessories.
8. Preparation of Apparatus
8.1 The rotational viscometer and thermal chamber heater shall be leveled and prepared as recommended by the instrument
manufacturer.
9. Calibration and Standardization
9.1 The viscometer shall be zeroed before use, or as needed, or both, according to the manufacturer’s instructions.
9.2 The accuracy of the viscometer shall be checked at least annually using a certified reference fluid of known viscosity at various
temperatures, using the procedure described in Test Method E2975. The reference fluid shall be certified to be Newtonian in
behavior over the full range of expected test temperatures and shear rates. The reference fluid shall be certified at a temperature
within 50 °C [90 °F] of the temperature(s) to be used during the test. The viscosity measured shall be within 62 % of the certified
value, or else a calibration constant (viscosity of the calibration fluid/viscosity indicated by the apparatus) must be determined and
applied.
9.3 The accuracy of the temperature reading and the temperature stability of the temperatur
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