ASTM D5018-89(1999)e1

Standard Test Method for Shear Viscosity of Coal-Tar and Petroleum Pitches

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.

General Information

• Status: Historical
• Publication Date: 09-Dec-1999
• ICS: 75.140 - Waxes, bituminous materials and other petroleum products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.05 - Properties of Fuels, Petroleum Coke and Carbon Material

Relations

• Replaced By: ASTM D5018-89(2004) - Standard Test Method for Shear Viscosity of Coal-Tar and Petroleum Pitches
• Effective Date: 01-Nov-2004

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
e1
Designation: D 5018 – 89 (Reapproved 1999)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Editorial corrections were made to Fig. 1 and in paragraph 14.2 in December 1999.
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 con-
95 to 120°C.
trolled, the “end-effects” are negligible, and the gap between
1.2 This test method is applicable only for rotational vis-
rotor/cup is small and remains constant during the test. The
cometers.
extrapolated value of apparent shear viscosity at “zero” shear
1.3 Since this test method is based on theoretical grounds,
rate is called shear viscosity.
strict adherence to details of the procedure is necessary to
comply with the theoretical requirements.
4. Significance and Use
1.4 The values stated in conventional units (centipoise) are
4.1 Thistestmethodisusefulasoneelementinestablishing
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) 5one 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
2. Referenced Documents 5.1 Viscometer—Arotationalviscometercapableofmeasur-
ing viscosity in the range of about 5 to 15000 cps; the
2.1 ASTM Standards:
2 viscometer should be equipped with the appropriate accesso-
D4296 Practice for Sampling Pitch
ries to allow measurements up to about 230°C. Two viscom-
E691 Practice for Conducting an Interlaboratory Study to
3 eters meeting these requirements are the LVT, LVF, or
Determine the Precision of a Test Method
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
4 5
are the Thermosel System and the TP 24 with heater.
using a rotational viscometer.
5.3 Thermometer—ASTM precision thermometer 2C, hav-
3.2 The recommended specifications herein are for measur-
ing a range of−5 to 300°C.
ing the apparent shear viscosity of binder pitches via a
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.05.OFon Industrial Pitches. Available from Brookfield Engineering Laboratories, Inc., 240 Cushing St.,
Current edition approved Nov. 24, 1989. Published January 1990. Stoughton, MA 02072.
2 5
Annual Book of ASTM Standards, Vol 05.02. Available from Haake Buchler Instruments, Inc., 244 Saddle River Road,
Annual Book of ASTM Standards, Vol 14.02. Saddle Brook, NJ 07662-6001.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5018
5.4 Hot Plate —Any hot plate with adjustable temperature 11.2 Equipment is to be properly leveled and installed in
control and surface temperature indication (to prevent sample accordance with manufacturer’s instructions.
overheating). 11.3 Use theASTM thermometer (applying the appropriate
5.5 Calibration Fluids —A series of calibrated fluids that stem correction) to correlate pitch temperature (in cup) to
covertheviscosityrangeofapproximately100to15000cpsat temperaturecontroller/indicator.Testtemperatureisconsidered
temperatures up to 150°C. to be the actual pitch temperature and not the temperature
indicated on the controller.
6. Reagents and Materials
11.4 Calibrate viscometer using calibration fluids.
6.1 Cleaning Solvent—Any solvent capable of dissolving
11.4.1 Use high- and low-temperature fluids; see 5.5.
pitch, (suitable solvents are quinoline or creosote oils).
11.4.2 Calibrate each rotor/cup combination and use them
6.2 Rinsing Solvents—Toluene and acetone are used for
as a paired set.
final rinsing after initial cleaning.
12. Procedure for Viscosity Determination
7. Safety Hazards
12.1 The following general principles apply to all viscosity
7.1 Fumes of hot pitch or solvents, or both, should be measurements determined by rotational methods:
removedfromallworkingareasbymeansofproperhoods.The
12.1.1 Maximize rotor diameter.
working area should be kept free of sparks and flames. 12.1.2 Minimize gap width between rotor and cup.
Quinoline fumes should not be inhaled, and prolonged contact
12.1.3 Minimize end effects (use longest available rotor).
with skin should be avoided. Toluene is toxic and flammable.
12.1.4 Preventviscousheating(duetoprolongedrotationof
rotor at high RPM).
8. Bulk Sampling
12.2 Selecttheproperrotor/cupcombinationthatcoversthe
8.1 Take samples from shipments in accordance with Prac-
anticipated viscosity range. A typical viscosity-temperature
tice D4296. Samples shall be free of foreign substances.
curve for various coal-tar pitches is given in Fig. 1, and a
Thoroughly mix the sample immediately before removing a
typical spindle number and RPM relationship for a LV series
representativeportionforthedeterminationorfordehydration.
Brookfield viscometer is given in Table 1. If there is overlap
in rotor/cup selection, select the combination that best meets
9. Sample Preparation
the criteria set forth in 12.1.1 to 12.1.4.
9.1 Ensure sample is dry; if there is visible moisture,
12.3 Determine viscosity from the lowest to the highest test
dehydrateat50°Cinaforced-airorvacuumovenuntildry,but
temperatures.
no longer than 2 h. (Experience has shown that drying at
12.4 Turn rotor at low RPM during heat-up (after sample is
temperatures in excess of 50°C increases the SP and viscosity
melted) and when changing test temperat
...