ASTM D5018-89(2004)
(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[dot]s) and one millipascal second (mPa[dot]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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Standards Content (Sample)
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An American National Standard
Designation: D 5018 – 89 (Reapproved 2004)
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope ratio of shear stress to shear rate in a unidirectional simple
shear flow field at steady state conditions. A concentric
1.1 This test method covers the determination of the appar-
cylinder viscometer is useful for measuring the apparent shear
ent shear viscosity of coal-tar and petroleum-based pitches
viscosity, provided the sample temperature is adequately con-
having a Mettler softening point (SP) range of approximately
trolled, the “end-effects” are negligible, and the gap between
95 to 120°C.
rotor/cup is small and remains constant during the test. The
1.2 This test method is applicable only for rotational vis-
extrapolated value of apparent shear viscosity at “zero” shear
cometers.
rate is called shear viscosity.
1.3 Since this test method is based on theoretical grounds,
strict adherence to details of the procedure is necessary to
4. Significance and Use
comply with the theoretical requirements.
4.1 Thistestmethodisusefulasoneelementinestablishing
1.4 The values stated in conventional units (centipoise) are
the uniformity of shipments.
to be regarded as the standard.The SI unit is the pascal second
4.2 Viscosity is also valuable for rheological characteriza-
(Pa·s) and one millipascal second (mPa·s)=one centipoise
tion of binder pitches. Binder pitch imparts consistency to
(cps); centipoise is in cgs units.
carbonaceousmixesandaffectstheirresistancetodeformation.
1.5 This standard does not purport to address all of the
Binder pitch viscosity is important for assessing mix consis-
safety concerns, if any, associated with its use. It is the
tency and for evaluating the ease of mix extrusion or molding
responsibility of the user of this standard to establish appro-
into artifacts.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard
5. Apparatus
statements are given in Section 7.
5.1 Viscometer—Arotationalviscometercapableofmeasur-
2. Referenced Documents ing viscosity in the range of about 5 to 15000 cps; the
2 viscometer should be equipped with the appropriate accesso-
2.1 ASTM Standards:
ries to allow measurements up to about 230°C. Two viscom-
D4296 Practice for Sampling Pitch
eters meeting these requirements are the LVT, LVF, or
E691 Practice for Conducting an Interlaboratory Study to
equivalent, and the RV100, RV20, or equivalent.
Determine the Precision of a Test Method
5.2 Sample Temperature Control System— Any device ca-
3. Summary of Test Method pable of maintaining the sample test temperature within limits
of 61.0°C while allowing viscosity measurements. Examples
3.1 The viscosity of a pitch, over the temperature range of
3 5
are the Thermosel System and the TP 24 with heater.
about 40 to 100°C above the SPof the material, is determined
5.3 Thermometer—ASTM precision thermometer 2C, hav-
using a rotational viscometer.
ing a range of−5 to 300°C.
3.2 The recommended specifications herein are for measur-
ing the apparent shear viscosity of binder pitches via a
concentric cylinder viscometer.Apparent shear viscosity is the
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.,
Stoughton, MA02072. If you are aware of alternative suppliers, please provide this
This test method is under the jurisdiction of ASTM Committee D02 on information to ASTM International Headquarters. Your comments will receive
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee careful consideration at a meeting of the responsible technical committee , which
D02.05 on Properties of Fuels, Petroleum Coke and Carbon Material. you may attend.
Current edition approved Nov. 1, 2004. Published November 2004. Originally The sole source of supply of the apparatus known to the committee at this time
e1
approved in 1989. Last previous edition approved in 1999 as D5018–89(1999) . 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.
D 5018 – 89 (2004)
5.4 Hot Plate —Any hot plate with adjustable temperature 11. Viscometer Calibration
control and surface temperature indication (to prevent sample
11.1 This step, required only occasionally, is designed to
overheating).
establish that the temperature and viscosity indicated by the
5.5 Calibration Fluids —A series of calibrated fluids that
appropriate measuring devices are in agreement with known
covertheviscosityrangeofapproximately100to15000cpsat
standards.
temperatures up to 150°C.
11.2 Equipment is to be properly leveled and installed in
accordance with manufacturer’s instructions.
6. Reagents and Materials
11.3 Use theASTM thermometer (applying the appropriate
6.1 Cleaning Solvent—Any solvent capable of dissolving
stem correction) to correlate pitch temperature (in cup) to
pitch, (suitable solvents are quinoline or creosote oils).
temperaturecontroller/indicator.Testtemperatureisconsidered
6.2 Rinsing Solvents—Toluene and acetone are used for
to be the actual pitch temperature and not the temperature
final rinsing after initial cleaning.
indicated on the controller.
11.4 Calibrate viscometer using calibration fluids.
7. Safety Hazards
11.4.1 Use high- and low-temperature fluids; see 5.5.
7.1 Fumes of hot pitch or solvents, or both, should be
11.4.2 Calibrate each rotor/cup combination and use them
removedfromallworkingareasbymeansofproperhoods.The
as a paired set.
working area should be kept free of sparks and flames.
Quinoline fumes should not be inhaled, and prolonged contact
12. Procedure for Viscosity Determination
with skin should be avoided. Toluene is toxic and flammable.
12.1 The following general principles apply to all viscosity
measurements determined by rotational methods:
8. Bulk Sampling
12.1.1 Maximize rotor diameter.
8.1 Take samples from shipments in accordance with Prac-
12.1.2 Minimize gap width between rotor and cup.
tice D4296. Samples shall be free of foreign substances.
12.1.3 Minimize end effects (use longest available rotor).
Thoroughly mix the sample immediately before removing a
12.1.4 Preventviscousheating(duetoprolongedrotationof
representativeportionforthedeterminationorfordehydration.
rotor at high rpm).
9. Sample Preparation
12.2 Selecttheproperrotor/cupcombinationthatcoversthe
anticipated viscosity range. A typical viscosity-temperature
9.1 Ensure sample is dry; if there is visible moisture,
curve for various coal-tar pitches is given in Fig. 1, and a
dehydrateat50°Cinaforced-airorvacuumovenuntildry,but
typical spindle number and rpm relationship for a LV series
no longer than 2 h. (Experience has shown that drying at
Brookfield viscometer is given in Table 1. If t
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