1、Designation: D5018 89 (Reapproved 2015)1Standard Test Method forShear Viscosity of Coal-Tar and Petroleum Pitches1This standard is issued under the fixed designation D5018; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o
2、f last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTESI units formatting was corrected editorially in May 2015.1. Scope1.1 This test method covers the determination of the appa
3、r-ent shear viscosity of coal-tar and petroleum-based pitcheshaving a Mettler softening point (SP) range of approximately95 C to 120 C.1.2 This test method is applicable only for rotational vis-cometers.1.3 Since this test method is based on theoretical grounds,strict adherence to details of the pro
4、cedure is necessary tocomply with the theoretical requirements.1.4 The values stated in SI units are to be regarded asstandard.1.4.1 ExceptionThe values stated in conventional units(centipoise) are to be regarded as the standard for viscositymeasurement only. The SI unit is the pascal second (Pas) a
5、ndone millipascal second (mPas) = one centipoise (cps); centi-poise is in cgs units.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and
6、 determine the applica-bility of regulatory limitations prior to use. Specific hazardstatements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:2D4296 Practice for Sampling PitchE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summar
7、y of Test Method3.1 The viscosity of a pitch, over the temperature range ofabout 40 C to 100 C above the SP of the material, isdetermined using a rotational viscometer.3.2 The recommended specifications herein are for measur-ing the apparent shear viscosity of binder pitches via aconcentric cylinder
8、 viscometer. Apparent shear viscosity is theratio of shear stress to shear rate in a unidirectional simpleshear flow field at steady state conditions. A concentriccylinder viscometer is useful for measuring the apparent shearviscosity, provided the sample temperature is adequatelycontrolled, the “en
9、d-effects” are negligible, and the gap be-tween rotor/cup is small and remains constant during the test.The extrapolated value of apparent shear viscosity at “zero”shear rate is called shear viscosity.4. Significance and Use4.1 This test method is useful as one element in establishingthe uniformity
10、of shipments.4.2 Viscosity is also valuable for rheological characteriza-tion of binder pitches. Binder pitch imparts consistency to1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility ofSubcommittee D02.
11、05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved April 1, 2015. Published May 2015. Originallyapproved in 1989. Last previous edition approved in 2009 as D5018 89 (2009).DOI: 10.1520/D5018-89R15E01.2For referenced ASTM standards, visit the ASTM website, www.astm
12、.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1carbonaceou
13、s mixes and affects their resistance to deformation.Binder pitch viscosity is important for assessing mix consis-tency and for evaluating the ease of mix extrusion or moldinginto artifacts.5. Apparatus5.1 ViscometerArotational viscometer capable of measur-ing viscosity in the range of about 5 cps to
14、 15 000 cps; theviscometer should be equipped with the appropriate accesso-ries to allow measurements up to about 230 C. Two viscom-eters meeting these requirements are the LVT, LVF,3orequivalent, and the RV100, RV20,4or equivalent.5.2 Sample Temperature Control System Any device ca-pable of maintai
15、ning the sample test temperature within limitsof 61.0 C while allowing viscosity measurements. Examplesare the Thermosel System3and the TP 245with heater.5.3 ThermometerASTM precision thermometer 2C, hav-ing a range of 5 C to 300 C.5.4 Hot Plate5Any hot plate with adjustable temperaturecontrol and s
16、urface temperature indication (to prevent sampleoverheating).5.5 Calibration Fluids6A series of calibrated fluids thatcover the viscosity range of approximately 100 cps to15 000 cps at temperatures up to 150 C.6. Reagents and Materials6.1 Cleaning SolventAny solvent capable of dissolvingpitch, (suit
17、able solvents are quinoline or creosote oils).6.2 Rinsing SolventsToluene and acetone are used forfinal rinsing after initial cleaning.7. Safety Hazards7.1 Fumes of hot pitch or solvents, or both, should beremoved from all working areas by means of proper hoods.Theworking area should be kept free of
18、 sparks and flames.Quinoline fumes should not be inhaled, and prolonged contactwith skin should be avoided. Toluene is toxic and flammable.8. Bulk Sampling8.1 Take samples from shipments in accordance with Prac-tice D4296. Samples shall be free of foreign substances.Thoroughly mix the sample immedia
19、tely before removing arepresentative portion for the determination or for dehydration.9. Sample Preparation9.1 Ensure sample is dry; if there is visible moisture,dehydrate at 50 C in a forced-air or vacuum oven until dry, butno longer than 2 h. (Experience has shown that drying attemperatures in exc
20、ess of 50 C increases the SP and viscosityof the pitch.)9.2 Crush dry lumps of pitch to a size of 6 mm to 12 mm.10. Charging Sample Cup10.1 In a suitable container, or the sample cup, melt pitchwith occasional stirring. Overheating of sample must beavoided as loss of volatiles may affect viscosity.
21、(Maximumtemperature should not exceed 50 C above SP.As a guide, thesurface temperature of the hot plate surface should not exceed200 C.)10.2 Place rotor in cup and preheat both to approximatelythe first test temperature.10.3 Remove rotor and transfer required amount of pitch tothe level specified by
22、 the manufacturer.10.4 Re-insert rotor, check that rotor is immersed to speci-fied depth, and install insulating cover.11. Viscometer Calibration11.1 This step, required only occasionally, is designed toestablish that the temperature and viscosity indicated by theappropriate measuring devices are in
23、 agreement with knownstandards.11.2 Equipment is to be properly leveled and installed inaccordance with manufacturers instructions.11.3 Use the ASTM thermometer (applying the appropriatestem correction) to correlate pitch temperature (in cup) totemperature controller/indicator.Test temperature is co
24、nsideredto be the actual pitch temperature and not the temperatureindicated on the controller.11.4 Calibrate viscometer using calibration fluids.11.4.1 Use high- and low-temperature fluids; see 5.5.11.4.2 Calibrate each rotor/cup combination and use themas a paired set.12. Procedure for Viscosity De
25、termination12.1 The following general principles apply to all viscositymeasurements determined by rotational methods:12.1.1 Maximize rotor diameter.12.1.2 Minimize gap width between rotor and cup.12.1.3 Minimize end effects (use longest available rotor).12.1.4 Prevent viscous heating (due to prolong
26、ed rotation ofrotor at high revolutions per minute).12.2 Select the proper rotor/cup combination that covers theanticipated viscosity range. A typical viscosity-temperature3The sole source of supply of the apparatus known to the committee at this timeis available from Brookfield Engineering Laborato
27、ries, Inc., 240 Cushing St.,Stoughton, MA 02072. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee1, whichyou may attend.4The sole source of
28、 supply of the apparatus known to the committee at this timeis available from Haake Buchler Instruments, Inc., 244 Saddle River Road, SaddleBrook, NJ 07662-6001. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receiveca
29、reful consideration at a meeting of the responsible technical committee1, whichyou may attend.5The sole source of supply of the apparatus known to the committee at this timeis the Hot plate Model 11-496-3 with 11-496-4 dial thermometer, available fromFisher Scientific, 585 Alpha Drive, Pittsburgh, P
30、A 15238. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee1, which you may attend.6Fluids available from Brookfield Engineering Laboratories;
31、 Cannon InstrumentCo., P.O. Box 16, State College, PA 16804, have been found suitable for thispurpose. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible techn
32、ical committee1, which you may attend.D5018 89 (2015)12curve for various coal-tar pitches is given in Fig. 1, and atypical spindle number and revolutions per minute relationshipfor a LV series Brookfield viscometer4is given in Table 1.Ifthere is overlap in rotor/cup selection, select the combination
33、that best meets the criteria set forth in 12.1.1 to 12.1.4.12.3 Determine viscosity from the lowest to the highest testtemperatures.12.4 Turn rotor at low revolutions per minute during heat-up(after sample is melted) and when changing test temperatures.12.5 Stabilize temperature for a minimum of 5 m
34、in but notmore than 15 min before measuring viscosity.12.6 Determine viscosity following manufacturers proce-dure. Ensure that the scale reading has stabilized beforerecording the value; only record values that are between 10 %and 90 % of the maximum scale reading.12.7 Increase temperature controlle
35、r to next higher testtemperature and repeat 12.4 through 12.7.12.8 Record test temperature and corresponding scale read-ings and convert scale readings to viscosity using appropriatefactors supplied by manufacturer or determined by calibration.12.9 Pitch is generally regarded as a Newtonian liquid (
36、theviscosity is independent of shear rate (rotational velocity orrevolutions per minute). To ensure that the pitch sample is infact Newtonian, determine the viscosity at different revolutionsper minute at a given temperature. If viscosities at differentrevolutions per minute are different (at same t
37、emperature), butare within 10 % of the average of the readings, report theaverage value. If the viscosities, at different revolutions perminute but the same temperature, differ by more than 10 %from the average, the material is non-Newtonian and theviscosity for each shear rate (revolutions per minu
38、te) should bereported.12.10 Occasionally, the pitch volume in the cup can de-crease when heated to higher temperatures due to loss ofmoisture or entrapped air. Consequently, the rotor will not becompletely immersed in pitch and the viscosity at highertemperatures will be lower than the true value. A
39、lso, theviscosity at lower temperatures will be inaccurate due tofoaming. To ensure that this did not occur, check the level inthe cup after the test is completed and the temperature is about150 C. If the rotor is not completely immersed, repeat the testtaking care to expel any moisture or entrapped
40、 air prior tocharging the cup. Moisture can be eliminated by drying at50 C, see 9.1. Entrapped air can be removed by carefullymelting the pitch and stirring gently until no foaming isobserved; avoid overheating the pitch, see 10.1. Also, en-trapped air can be minimized by avoiding the use of fine pi
41、tchparticles; use 6 mm 12 mm sized particles, see 9.2.13. Cleaning13.1 After completion of test, cool to about 40 C above SP,remove rotor and place rotor into a container of quinoline orother high-boiling aromatic solvent (in hood), or wipe rotorusing toluene or quinoline.13.2 Remove cup and pour ou
42、t pitch; clean with quinoline,or other appropriate solvent, and toluene.FIG. 1 Viscosity of Coal-Tar Pitch as a Function of TemperatureTABLE 1 Brookfield Thermosel Spindle Factors LV SeriesViscometersASpeed, r/minSpindle Number18 31 3460 0.5 5 1030 1 10 2012 2.5 25 506 5 50 1003 10 100 2001.5 20 200
43、 4000.6 50 500 10000.3 100 1000 2000AViscosity (centipoise) is determined by multiplying the scale reading (0 to 100) bythe appropriate spindle factor. If the usable scale readings are 10 % to 90 % ofmaximum (see 12.6), then the viscosity range for spindles 18, 31, and 34 are 5 to9000, 50 to 90 000,
44、 and 100 to 180 000 centipoise, respectively.D5018 89 (2015)1313.3 After the cup and rotor are clean and cool, rinse bothwith acetone to remove any oil residue.14. Report14.1 Report viscosity, for each test temperature, to thenearest centipoise.14.2 The data can be reported in simple tabular form or
45、plotted on suitable graph paper. (Usually a plot of log viscosityversus 1/T (Celsius) gives a straight-line relationship.)15. Precision and Bias15.1 The precision was determined by an interlaboratorystudy conducted in accordance with Practice E691. Fourteenlaboratories tested four materials (three c
46、oal-tar pitches andone petroleum pitch) in the temperature range of 150 C to210 C (150 C to 230 C for the petroleum pitch); the viscosi-ties ranged from 12 000 cps to 50 cps. Based on this study, thecriteria in 15.1.1 and 15.1.2 shall be used for judging theacceptability of results (95 % probability
47、) obtained in theaforementioned temperature ranges and in the viscosity rangeof 50 cps to 12 000 cps:15.1.1 Repeatability LimitsDuplicate values (cps) by thesame operator shall not be considered suspect unless thedetermined viscosities, at a given temperature, differ by morethan 12 % of the average
48、of the duplicate determinations.15.1.2 Reproducibility LimitsThe values reported by eachof two laboratories, representing the arithmetic average ofduplicate determinations at a given temperature, shall not beconsidered suspect unless the reported values (cps) differ bymore than 36 % of the average o
49、f the four values.15.2 BiasThis test method has no bias with any otherstandard.16. Keywords16.1 coal tar pitch; petroleum pitch; pitch; viscosityASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the respons
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