ASTM D5018-2018 Standard Test Method for Shear Viscosity of Coal-Tar and Petroleum Pitches.pdf

1、Designation: D5018 89 (Reapproved 2015)1D5018 18Standard 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, th

2、e year 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 NOTESI units formatting was corrected editorially in May 2015.1. Scope Scope*1.1 This test method covers the determina

3、tion of the apparent shear viscosity of coal-tar and petroleum-based pitches havinga Mettler softening point (SP) range of approximately 95 C to 120 C.120 C (see Test Method D3104).1.2 This test method is applicable only for rotational viscometers.1.3 Since this test method is based on theoretical g

4、rounds, strict adherence to details of the procedure is necessary to complywith the theoretical requirements.1.4 The values stated in SI units are to be regarded as standard.1.4.1 ExceptionThe values stated in conventional units (centipoise) are to be regarded as the standard for viscositymeasuremen

5、t only. The SI unit is the pascal second (Pas) and one millipascal second (mPas) = one centipoise (cps);(cP);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 responsibilityof the user of this standard to e

6、stablish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.1.6 This international standard was developed in accordance with internationally recognized principle

7、s on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D3104 Test Method for Softening Point

8、of Pitches (Mettler Softening Point Method)D4296 Practice for Sampling PitchE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE1953 Practice for Description of Thermal Analysis and Rheology ApparatusE2975 Test Method for Calibration or Calibration Verif

9、ication of Concentric Cylinder Rotational Viscometers3. Summary of Test Method3.1 The viscosity of a pitch, over the temperature range of about 40 C to 100 C above the SP of the material, is determinedusing a rotational viscometer.3.2 The recommended specifications herein are for measuring the appar

10、ent shear viscosity of binder pitches via a concentriccylinder viscometer. Apparent shear viscosity is the ratio of shear stress to shear rate in a unidirectional simple shear flow fieldat steady state conditions. A concentric cylinder viscometer is useful for measuring the apparent shear viscosity,

11、 provided thesample temperature is adequately controlled, the “end-effects” are negligible, and the gap between rotor/cup is small and remainsconstant during the test. The extrapolated value of apparent shear viscosity at “zero” shear rate is called shear viscosity.1 This test method is under the ju

12、risdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels, Petroleum Coke and Carbon Material.Current edition approved April 1, 2015June 1, 2018. Published May 2015July 2018. Originally approved in

13、 1989. Last previous edition approved in 20092015 asD5018 89 (2009).(2015)1. DOI: 10.1520/D5018-89R15E01.10.1520/D5018-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refe

14、r to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all cha

15、nges accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Ba

16、rr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Significance and Use4.1 This test method is useful as one element in establishing the uniformity of shipments.4.2 Viscosity is also valuable for rheological characterization of binder pitches. Binder pitch imparts consi

17、stency tocarbonaceous mixes and affects their resistance to deformation. Binder pitch viscosity is important for assessing mix consistencyand for evaluating the ease of mix extrusion or molding into artifacts.5. Apparatus5.1 ViscometerArotational viscometer capable of measuring viscosity in the rang

18、e of about 5 cps to 15 000 cps; 5 mPas (cP)to 15 000 mPas (cP); the viscometer should be equipped with the appropriate accessories to allow measurements up to about230 C. Two viscometers meeting these requirements are the LVT, LVF,The essential instrumentation required providing theminimum rotationa

19、l or equivalent, and the RV100, RV20,viscometer analytical capabilities include (see Practice E1953orequivalent.):5.1.1 Drive motor, to apply a unidirectional rotational displacement to the specimen of 0.3 rmin to 60 rmin constant to 61 %.5.1.2 Force sensor, to measure the torque developed by the sp

20、ecimen to within 61 %.5.1.3 Coupling shaft, or other means to transmit the displacement from the motor to the specimen.5.1.4 Rotational element, spindle, or rotor, of the shape shown in Fig. 1, to fix the specimen between the coupling shaft anda stationary position.5.1.5 Specimen container, chamber,

21、 or cup, to contain the test specimen during testing.NOTE 1Rotor and cup are matched in size so that shear rate is fixed and known.5.1.6 Data collection device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.The minimum output signals required for ro

22、tational visocity are torque, rotational speed, temperature, and time.5.1.7 Auxiliary instrumentation considered useful in conducting this test method includes:5.1.7.1 Data analysis capability, to provide viscosity, stress, or other useful parameters derived from measured signals.5.1.7.2 Stand, to s

23、upport, level, and adjust the height of the drive motor, shaft, and rotor.5.1.7.3 Level, to indicate the vertical plumb of the drive motor, shaft, and rotor.5.2 Sample Temperature Control SystemAny device capable of maintaining the sample test temperature within limits of61.0 C while allowing viscos

24、ity measurements. Examples are the Thermosel System and the TP 245 with heater.5.3 ThermometerASTM precision thermometer 2C, having a range of 5 C to 300 C.5.4 Hot Plate3Any hot plate with adjustable temperature control and surface temperature indication (to prevent sampleoverheating).5.5 Calibratio

25、n FluidsFluidsA series of calibrated fluids that cover the viscosity range of approximately 100 cps to15 000 cps 100 mPas (cP) to 15 000 mPas (cP) at temperatures up to 150 C.NOTE 2Calibration fluids are available from the rotational viscometer supplier.6. Reagents and Materials6.1 Cleaning SolventA

26、ny solvent capable of dissolving pitch, (suitable solvents are quinoline or creosote oils).6.2 Rinsing SolventsToluene and acetone are used for final rinsing after initial cleaning.7. Safety Hazards7.1 Fumes of hot pitch or solvents, or both, should be removed from all working areas by means of prop

27、er hoods. The workingarea should be kept free of sparks and flames. Quinoline fumes should not be inhaled, and prolonged contact with skin should beavoided. Toluene is toxic and flammable.8. Bulk Sampling8.1 Take samples from shipments in accordance with Practice D4296. Samples shall be free of fore

28、ign substances. Thoroughlymix the sample immediately before removing a representative portion for the determination or for dehydration.3 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., Stough

29、ton,MA 02072. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful considerationat a meeting of the responsible technical committee 1, which you may attend.4 The sole source of supply of the apparatus known

30、to the committee at this time is available from Haake Buchler Instruments, Inc., 244 Saddle River Road, Saddle Brook,NJ 07662-6001. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive carefulconsideration at a meet

31、ing of the responsible technical committee 1, which you may attend.3 The sole source of supply of the apparatus known to the committee at this time is the Hot plate Model 11-496-3 with 11-496-4 dial thermometer, available from FisherScientific, 585 Alpha Drive, Pittsburgh, PA 15238. If you are aware

32、 of alternative suppliers, please provide this information to ASTM International Headquarters. Yourcomments will receive careful consideration at a meeting of the responsible technical committee 1, which you may attend.D5018 1829. Sample Preparation9.1 Ensure sample is dry; if there is visible moist

33、ure, dehydrate at 50 C in a forced-air or vacuum oven until dry, but no longerthan 2 h. (Experience has shown that drying at temperatures in excess of 50 C increases the SP and viscosity of the pitch.)9.2 Crush dry lumps of pitch to a size of 6 mm to 12 mm.A Viscosity (centipoise) is determined by m

34、ultiplying the scale reading (0 to 100) by the appropriate spindle factor. If the usable scale readings are 10 % to 90 % of maximum(see 12.6), then the viscosity range for spindles 18, 31, and 34 are 5 to 9000, 50 to 90 000, and 100 to 180 000 centipoise, respectively.FIG. 1 Rotor ConfigurationD5018

35、 18310. Charging Sample Cup10.1 In a suitable container, or the sample cup, melt pitch with occasional stirring. Overheating of sample must be avoided asloss of volatiles may affect viscosity. (Maximum temperature should not exceed 50 C above SP. As a guide, the surfacetemperature of the hot plate s

36、urface should not exceed 200 C.)10.2 Place rotor in cup and preheat both to approximately the first test temperature.10.3 Remove rotor and transfer required amount of pitch to the level specified by the manufacturer.10.4 Re-insert rotor, check that rotor is immersed to specified depth, and install i

37、nsulating cover.11. Viscometer Calibration11.1 This step, required only occasionally, is designed to establish that the temperature and viscosity indicated by theappropriate measuring devices are in agreement with known standards.11.2 Equipment is to be properly leveled and installed in accordance w

38、ith manufacturers instructions.11.3 Use the ASTM thermometer (applying the appropriate stem correction) to correlate pitch temperature (in cup) totemperature controller/indicator. Test temperature is considered to be the actual pitch temperature and not the temperature indicatedon the controller.11.

39、4 Calibrate viscometer using calibration fluids. fluids (see Test Method E2975).11.4.1 Use high- and low-temperature fluids; see 5.5.11.4.2 Calibrate each rotor/cup combination and use them as a paired set.12. Procedure for Viscosity Determination12.1 The following general principles apply to all vi

40、scosity measurements 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 rotation of rotor at high revolutions per minute).12.2 Selec

41、t the proper rotor/cup combination that covers the anticipated viscosity range. A typical viscosity-temperature curvefor various coal-tar pitches is given in Fig. 12, and a typical spindle number and revolutions per minute relationship for a LV seriesBrookfield viscometer is given in Table 1. If the

42、re is overlap in rotor/cup selection, select the combination that best meets thecriteria set forth in 12.1.1 to 12.1.4.12.3 Determine viscosity from the lowest to the highest test temperatures.12.4 Turn rotor at low revolutions per minute rotational speed during heat-up (after sample is melted) and

43、when changing testtemperatures.12.5 Stabilize temperature for a minimum of 5 min but not more than 15 min before measuring viscosity.12.6 Determine viscosity following manufacturers procedure. Ensure that the scale reading has stabilized before recording thevalue; only record values that are between

44、 10 % and 90 % of the maximum torque scale reading.12.7 Increase temperature controller to next higher test temperature and repeat 12.4 through 12.7.12.8 Record test temperature and corresponding scale readings and convert scale readings to viscosity using appropriate factorssupplied by manufacturer

45、 or determined by calibration.12.9 Pitch is generally regarded as a Newtonian liquid (the viscosity is independent of shear rate (rotational velocity orrevolutions per minute). speed). To ensure that the pitch sample is in fact Newtonian, determine the viscosity at differentrevolutions per minute ro

46、tational speeds at a given temperature. If viscosities at different revolutions per minute rotational speedsare different (at same temperature), but are within 10 % of the average of the readings, report the average value. If the viscosities,at different revolutions per minute rotational speeds but

47、the same temperature, differ by more than 10 % from the average, thematerial is non-Newtonian and the viscosity for each shear rate (revolutions per minute) (rotational speed) should be reported.12.10 Occasionally, the pitch volume in the cup can decrease when heated to higher temperatures due to lo

48、ss of moisture orentrapped air. Consequently, the rotor will not be completely immersed in pitch and the viscosity at higher temperatures will belower than the true value. Also, the viscosity at lower temperatures will be inaccurate due to foaming. To ensure that this did notoccur, check the level i

49、n the cup after the test is completed and the temperature is about 150 C. If the rotor is not completelyimmersed, repeat the test taking care to expel any moisture or entrapped air prior to charging the cup. Moisture can be eliminatedby drying at 50 C, see 9.1. Entrapped air can be removed by carefully melting the pitch and stirring gently until no foaming isobserved; avoid overheating the pitch, see 10.1. Also, entrapped air can be minimized by avoiding the use of fine pitch particles;use 6 mm 12 mm sized particles, see 9.2.D5018 1