1、Designation: D 5018 89 (Reapproved 2009)Standard Test Method forShear Viscosity of Coal-Tar and Petroleum Pitches1This standard is issued under the fixed designation D 5018; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the appar-ent shear viscosity of coal-tar and petroleum-based pitchesh
3、aving a Mettler softening point (SP) range of approximately95 to 120C.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 procedure is necessary tocomply with the theoretical requirements.1.
4、4 The values stated in conventional units (centipoise) areto be regarded as the standard. The SI unit is the pascal second(Pas) and one millipascal second (mPas) = one centipoise(cps); centipoise is in cgs units.1.5 This standard does not purport to address all of thesafety concerns, if any, associa
5、ted with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardstatements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:2D 4296 Pra
6、ctice for Sampling PitchE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 The viscosity of a pitch, over the temperature range ofabout 40 to 100C above the SP of the material, is determinedusing a rotational viscometer.3.2 T
7、he recommended specifications herein are for measur-ing the apparent shear viscosity of binder pitches via aconcentric cylinder viscometer. Apparent shear viscosity is theratio of shear stress to shear rate in a unidirectional simpleshear flow field at steady state conditions. A concentriccylinder v
8、iscometer is useful for measuring the apparent shearviscosity, provided the sample temperature is adequately con-trolled, the “end-effects” are negligible, and the gap betweenrotor/cup is small and remains constant during the test. Theextrapolated value of apparent shear viscosity at “zero” shearrat
9、e is called shear viscosity.4. Significance and Use4.1 This test method is useful as one element in establishingthe uniformity of shipments.4.2 Viscosity is also valuable for rheological characteriza-tion of binder pitches. Binder pitch imparts consistency tocarbonaceous mixes and affects their resi
10、stance 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 to 15 000 cps; theviscometer should
11、be equipped with the appropriate accesso-ries to allow measurements up to about 230C. 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 maintaining the sample test temperature wi
12、thin limitsof 61.0C while allowing viscosity measurements. Examplesare the Thermosel System3and the TP 245with heater.5.3 ThermometerASTM precision thermometer 2C, hav-ing a range of 5 to 300C.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and i
13、s the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved April 15, 2009. Published July 2009. Originallyapproved in 1989. Last previous edition approved in 2004 as D 501889(2004).2For referenced ASTM standards, visit the AS
14、TM website, www.astm.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.3The sole source of supply of the apparatus known to the committee at this timeis available from Brookfie
15、ld Engineering Laboratories, 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 att
16、end.4The sole source of 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
17、comments will receivecareful consideration at a meeting of the responsible technical committee1, whichyou may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.4 Hot Plate5Any hot plate with adjustable temperaturecontrol and s
18、urface temperature indication (to prevent sampleoverheating).5.5 Calibration Fluids6A series of calibrated fluids thatcover the viscosity range of approximately 100 to 15 000 cps attemperatures up to 150C.6. Reagents and Materials6.1 Cleaning SolventAny solvent capable of dissolvingpitch, (suitable
19、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 spar
20、ks 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 D 4296. Samples shall be free of foreign substances.Thoroughly mix the sample immediately
21、 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 50C in a forced-air or vacuum oven until dry, butno longer than 2 h. (Experience has shown that drying attemperatures in excess o
22、f 50C increases the SP and viscosityof the pitch.)9.2 Crush dry lumps of pitch to a size of 6 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. (Maximumt
23、emperature should not exceed 50C above SP. As a guide, thesurface temperature of the hot plate surface should not exceed200C.)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 the manuf
24、acturer.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 agreement
25、 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 consideredto
26、 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 Determinatio
27、n12.1 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 prolonged rotatio
28、n ofrotor at high rpm).12.2 Select the proper rotor/cup combination that covers theanticipated viscosity range. A typical viscosity-temperaturecurve for various coal-tar pitches is given in Fig. 1, and atypical spindle number and rpm relationship for a LV seriesBrookfield viscometer4is given in Tabl
29、e 1. If there is overlapin rotor/cup selection, select the combination that best meetsthe 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 rpm during heat-up (after sample ismelted) and when changing test temperatu
30、res.12.5 Stabilize temperature for a minimum of 5 min 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 and90 % of the maximum
31、scale reading.12.7 Increase temperature controller 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 Pi
32、tch is generally regarded as a Newtonian liquid (theviscosity is independent of shear rate (rotational velocity orrpm). To ensure that the pitch sample is in fact Newtonian,determine the viscosity at different rpm at a given temperature.If viscosities at different rpm are different (at same tempera-
33、ture), but are within 10 % of the average of the readings, reportthe average value. If the viscosities, at different rpm but thesame temperature, differ by more than 10 % from the average,the material is non-Newtonian and the viscosity for each shearrate (rpm) should be reported.5The sole source of
34、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, PA 15238. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarte
35、rs. Your comments will receive careful consideration at a meeting of theresponsible technical committee1, which you may attend.6Fluids available from Brookfield Engineering Laboratories; Cannon InstrumentCo., P.O. Box 16, State College, PA 16804, have been found suitable for thispurpose. If you are
36、aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee1, which you may attend.D 5018 89 (2009)212.10 Occasionally, the pitch volume in the cup can de-crea
37、se 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. Also, theviscosity at lower temperatures will be inaccurate due tofoaming. To ensu
38、re that this did not occur, check the level inthe cup after the test is completed and the temperature is about150C. If the rotor is not completely immersed, repeat the testtaking care to expel any moisture or entrapped air prior tocharging the cup. Moisture can be eliminated by drying at50C, see 9.1
39、. 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 pitchparticles; use 6 3 12-mm sized particles, see 9.2.13. Cleaning13.1 After complet
40、ion of test, cool to about 40C 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 out pitch; clean with quinoline,or other appropriate solvent, and toluene.13.3 After th
41、e 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 orplotted on suitable graph paper. (Usually a plot of log viscosityversus 1/T
42、 (Celsius) gives a straight-line relationship.)15. Precision and Bias15.1 The precision was determined by an interlaboratorystudy conducted in accordance with Practice E 691. Fourteenlaboratories tested four materials (three coal-tar pitches andone petroleum pitch) in the temperature range of 150 to
43、 210C(150 to 230C for the petroleum pitch); the viscosities rangedfrom 12 000 to 50 cps. Based on this study, the criteria in15.1.1 and 15.1.2 shall be used for judging the acceptability ofresults (95 % probability) obtained in the aforementionedtemperature ranges and in the viscosity range of 50 to
44、 12 000cps: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 of the duplicate determinations.15.1.2 Reproducibility LimitsThe values reported by eachof
45、 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 of the four values.15.2 BiasThis test method has no bias with any otherstandard.16. Keyword
46、s16.1 coal tar pitch; petroleum pitch; pitch; viscosityFIG. 1 Viscosity of Coal-Tar Pitch as a Function of TemperatureTABLE 1 Brookfield Thermosel Spindle Factors LV SeriesViscometersASpeed, rpmSpindle Number18 31 3460 0.5 5 1030 1 10 2012 2.5 25 506 5 50 1003 10 100 2001.5 20 200 4000.6 50 500 1000
47、0.3 100 1000 2000AViscosity (centipoise) is determined by multiplying the scale reading (0 to 100)by the 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, and 100 to 180 000 c
48、entipoise, respectively.D 5018 89 (2009)3ASTM 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 th
49、e riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments
