ASTM D5018-89(2009)
(Test Method)Standard Test Method for Shear Viscosity of Coal-Tar and Petroleum Pitches
Standard Test Method for Shear Viscosity of Coal-Tar and Petroleum Pitches
SIGNIFICANCE AND USE
This test method is useful as one element in establishing the uniformity of shipments.
Viscosity is also valuable for rheological characterization of binder pitches. Binder pitch imparts consistency to carbonaceous mixes and affects their resistance to deformation. Binder pitch viscosity is important for assessing mix consistency and for evaluating the ease of mix extrusion or molding into artifacts.
SCOPE
1.1 This test method covers the determination of the apparent shear viscosity of coal-tar and petroleum-based pitches having a Mettler softening point (SP) range of approximately 95 to 120°C.
1.2 This test method is applicable only for rotational viscometers.
1.3 Since this test method is based on theoretical grounds, strict adherence to details of the procedure is necessary to comply with the theoretical requirements.
1.4 The values stated in conventional units (centipoise) are to be regarded as the standard. The SI unit is the pascal second (Pa·s) and one millipascal second (mPa·s) = one centipoise (cps); centipoise is in cgs units.
1.5 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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.
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Designation: D5018 − 89 (Reapproved2009)
Standard Test Method for
Shear Viscosity of Coal-Tar and Petroleum Pitches
This standard is issued under the fixed designation D5018; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope concentric cylinder viscometer.Apparent shear viscosity is the
ratio of shear stress to shear rate in a unidirectional simple
1.1 This test method covers the determination of the appar-
shear flow field at steady state conditions. A concentric
ent shear viscosity of coal-tar and petroleum-based pitches
cylinder viscometer is useful for measuring the apparent shear
having a Mettler softening point (SP) range of approximately
viscosity, provided the sample temperature is adequately
95 to 120°C.
controlled, the “end-effects” are negligible, and the gap be-
1.2 This test method is applicable only for rotational vis-
tween rotor/cup is small and remains constant during the test.
cometers.
The extrapolated value of apparent shear viscosity at “zero”
1.3 Since this test method is based on theoretical grounds, shear rate is called shear viscosity.
strict adherence to details of the procedure is necessary to
comply with the theoretical requirements. 4. Significance and Use
4.1 Thistestmethodisusefulasoneelementinestablishing
1.4 The values stated in conventional units (centipoise) are
to be regarded as the standard.The SI unit is the pascal second the uniformity of shipments.
(Pa·s) and one millipascal second (mPa·s)=one centipoise
4.2 Viscosity is also valuable for rheological characteriza-
(cps); centipoise is in cgs units.
tion of binder pitches. Binder pitch imparts consistency to
1.5 This standard does not purport to address all of the carbonaceousmixesandaffectstheirresistancetodeformation.
safety concerns, if any, associated with its use. It is the
Binder pitch viscosity is important for assessing mix consis-
responsibility of the user of this standard to establish appro- tency and for evaluating the ease of mix extrusion or molding
priate safety and health practices and determine the applica-
into artifacts.
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 7.
5. Apparatus
5.1 Viscometer—Arotationalviscometercapableofmeasur-
2. Referenced Documents
ing viscosity in the range of about 5 to 15000 cps; the
2.1 ASTM Standards:
viscometer should be equipped with the appropriate accesso-
D4296Practice for Sampling Pitch
ries to allow measurements up to about 230°C. Two viscom-
E691Practice for Conducting an Interlaboratory Study to 3
eters meeting these requirements are the LVT, LVF, or
Determine the Precision of a Test Method 4
equivalent, and the RV100, RV20, or equivalent.
3. Summary of Test Method
5.2 Sample Temperature Control System—Any device ca-
pable of maintaining the sample test temperature within limits
3.1 The viscosity of a pitch, over the temperature range of
of 61.0°C while allowing viscosity measurements. Examples
about 40 to 100°C above the SP of the material, is determined
3 5
are the Thermosel System and the TP 24 with heater.
using a rotational viscometer.
3.2 The recommended specifications herein are for measur-
ing the apparent shear viscosity of binder pitches via a
The sole source of supply of the apparatus known to the committee at this time
is available from Brookfield Engineering Laboratories, Inc., 240 Cushing St.,
This test method is under the jurisdiction of ASTM Committee D02 on Stoughton, MA02072. If you are aware of alternative suppliers, please provide this
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee information to ASTM International Headquarters. Your comments will receive
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material. careful consideration at a meeting of the responsible technical committee , which
Current edition approved April 15, 2009. Published July 2009. Originally you may attend.
approved in 1989. Last previous edition approved in 2004 as D5018–89(2004). The sole source of supply of the apparatus known to the committee at this time
DOI: 10.1520/D5018-89R09. is available from Haake Buchler Instruments, Inc., 244 Saddle River Road, Saddle
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Brook,NJ07662-6001.Ifyouareawareofalternativesuppliers,pleaseprovidethis
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM information to ASTM International Headquarters. Your comments will receive
Standards volume information, refer to the standard’s Document Summary page on careful consideration at a meeting of the responsible technical committee , which
the ASTM website. you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5018 − 89 (2009)
5.3 Thermometer—ASTM precision thermometer 2C, hav- 10.3 Remove rotor and transfer required amount of pitch to
ing a range of−5 to 300°C. the level specified by the manufacturer.
5.4 Hot Plate —Any hot plate with adjustable temperature 10.4 Re-insert rotor, check that rotor is immersed to speci-
control and surface temperature indication (to prevent sample fied depth, and install insulating cover.
overheating).
6 11. Viscometer Calibration
5.5 Calibration Fluids —A series of calibrated fluids that
covertheviscosityrangeofapproximately100to15000cpsat 11.1 This step, required only occasionally, is designed to
establish that the temperature and viscosity indicated by the
temperatures up to 150°C.
appropriate measuring devices are in agreement with known
6. Reagents and Materials
standards.
6.1 Cleaning Solvent—Any solvent capable of dissolving
11.2 Equipment is to be properly leveled and installed in
pitch, (suitable solvents are quinoline or creosote oils).
accordance with manufacturer’s instructions.
6.2 Rinsing Solvents—Toluene and acetone are used for
11.3 Use theASTM thermometer (applying the appropriate
final rinsing after initial cleaning.
stem correction) to correlate pitch temperature (in cup) to
temperaturecontroller/indicator.Testtemperatureisconsidered
7. Safety Hazards
to be the actual pitch temperature and not the temperature
indicated on the controller.
7.1 Fumes of hot pitch or solvents, or both, should be
removedfromallworkingareasbymeansofproperhoods.The
11.4 Calibrate viscometer using calibration fluids.
working area should be kept free of sparks and flames.
11.4.1 Use high- and low-temperature fluids; see 5.5.
Quinoline fumes should not be inhaled, and prolonged contact
11.4.2 Calibrate each rotor/cup combination and use them
with skin should be avoided. Toluene is toxic and flammable.
as a paired set.
8. Bulk Sampling
12. Procedure for Viscosity Determination
8.1 Take samples from shipments in accordance with Prac-
12.1 The following general principles apply to all viscosity
tice D4296. Samples shall be free of foreign substances.
measurements determined by rotational methods:
Thoroughly mix the sample immediately before removing a
12.1.1 Maximize rotor diameter.
representativeportionforthedeterminationorfordehydration.
12.1.2 Minimize gap width between rotor and cup.
12.1.3 Minimize end effects (use longest available rotor).
9. Sample Preparation
12.1.4 Preventviscousheating(duetoprolongedrotationof
9.1 Ensure sample is dry; if there is visible moisture, rotor at high rpm).
dehydrateat50°Cinaforced-airorvacuumovenuntildry,but
12.2 Selecttheproperrotor/cupcombinationthatcoversthe
no longer than 2 h. (Experience has shown that drying at
anticipated viscosity range. A typical viscosity-temperature
temperatures in excess of 50°C incre
...
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