ASTM D2639 D2639M-2016 Standard Test Method for Plastic Properties of Coal by the Constant-Torque Gieseler Plastometer《采用恒转矩基氏塑性计测定煤炭塑性特性的标准试验方法》.pdf

1、Designation: D2639/D2639M 16Standard Test Method forPlastic Properties of Coal by the Constant-Torque GieselerPlastometer1This standard is issued under the fixed designation D2639/D2639M; the number immediately following the designation indicates theyear of original adoption or, in the case of revis

2、ion, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a relative measure of the plasticbehavior of coal when heated under prescribe

3、d conditions. Thistest method may be used to obtain semiquantitative values ofthe plastic properties of coals and blends used in carbonizationand in other situations where determination of plastic behaviorof coals is of practical importance.1.2 The values stated in either SI units or inch-pound unit

4、sare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in non-conformancewith the standard.1.3 This standard does not purport to address

5、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 determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D2013/D2013M Pract

6、ice for Preparing Coal Samples forAnalysisD2234/D2234M Practice for Collection of a Gross Sampleof Coal3. Terminology3.1 Definitions:3.1.1 breaking, vfree spinning behavior of coal, either byan abrupt change to rotating at maximum motor speed or byabrupt changes in rotation, which occurs as a result

7、 of a moltenball of coal forming around the base of the stirrer, and whichmakes reporting of the true maximum fluidity of the coaldifficult.3.1.2 dial division per minute, DDPM, nas used in thistest method, a measure of stirrer rotation rate. There are100 dial divisions for each full 360 rotation of

8、 the stirrer.Stirrer rotation rate is the total dial divisions turned by thestirrer in a one minute time period.3.1.3 initial softening temperature, nas used in this testmethod, the temperature at which the stirrer rotation rate firstreaches 1.0 dial divisions per minute.3.1.4 jamming, vswelling up

9、of coal into the retort tubeduring the test, which may produce lower fluidity results thanexpected and can only be noted after visual inspection of thedisassembled crucible and retort at the conclusion of the test.3.1.5 maximum fluidity, nas used in this test method, themeasured maximum stirrer rota

10、tion rate, in dial divisions perminute.3.1.6 maximum fluidity temperature, nas used in this testmethod, the temperature at which stirrer rotation rate reaches amaximum value.3.1.7 plastic range, ndifference between the solidificationtemperature and the initial softening temperatures.3.1.8 solidifica

11、tion temperature, nas used in this testmethod, the temperature at which the first zero DDPM isreached after the last stirrer rotation.4. Summary of Test Method4.1 The plastometer measures the plastic properties of coalsby the use of a constantly applied torque on a stirrer placed ina crucible into w

12、hich the coal is charged. The crucible isimmersed in a bath and the temperature increased uniformly.The rates of movement of the stirrer are recorded in relation toincrease in temperature.5. Significance and Use5.1 Reliable values of the plastic properties of coals are usedto predict or explain the

13、behavior of a coal or blends duringcarbonization or in other processes such as gasification,liquefaction, and combustion.1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.15 on MetallurgicalProperties of Coal and Co

14、ke.Current edition approved March 1, 2016. Published March 2016. Originallyapproved in 1967. Last previous edition approved in 2013 as D2639/D2639M13.DOI: 10.1520/D2639_D2639M-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org.

15、 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 States16. Apparatus6.1 Gieseler PlastometerThe apparatus shall consist ofth

16、e following:6.1.1 RetortA steel retort consisting of four parts asshown in Fig. 1.6.1.2 Retort Crucible, cylindrical, 21.4 mm 6 0.08 mm0.844 in. 6 0.003 in. in inside diameter and 35.0 mm1.38 in. in depth, with exterior threads for joining the crucibleto the crucible cover. The crucible shall have a

17、 2.38 mm 6FIG. 1 Retort AssemblyD2639/D2639M 1620.02 mm 0.094 in. 6 0.001 in. diameter notch in the center ofits inside base to serve as a seat for the stirrer.6.1.3 Retort Crucible Cover, with interior threads for joiningthe crucible cover to the crucible and exterior threads forjoining the crucibl

18、e cover to the barrel. The inside diameter ofthe hole which accommodates the stirrer is9.53 mm 6 0.08 mm 0.375 in. 6 0.003 in.6.1.4 Barrel, 121 mm 4.75 in. long and having an insidediameter of 9.53 mm 6 0.08 mm 0.375 in. 6 0.003 in. Thetop end of the barrel shall be 12.7 mm 0.500 in. in insidediamet

19、er to a depth sufficient to allow clearance for the axle ofthe plastometer head when the apparatus is assembled. A hole,fitted with a tube, shall be provided at the midpoint of thebarrel so as to afford exit for the volatile products during a test.6.1.5 Steel Stirrer, provided with a straight shaft3

20、.96 mm 6 0.03 mm 0.156 in. 6 0.001 in. in diameter andequipped with four rabble arms. The lower end of the stirrershall have a 60 included angle. The rabble arms on the stirrershall be 1.59 mm 6 0.03 mm 0.0625 in. 6 0.001 in. indiameter, 6.35 mm 6 0.05 mm 0.250 in. 6 0.002 in. inlength, and shall be

21、 placed perpendicular to the shaft at 90 intervals around the shaft and 3.18 mm 6 0.03 mm0.125 in. 6 0.001 in. apart center to center along the shaft.The middle two rabble arms shall be set at 180 to each other,and likewise, the remaining two arms 180 to each other. Thelowest rabble arm shall be set

22、 in the shaft to give 1.59 mm0.0625 in. clearance between it and the bottom of the cruciblewhen the stirrer is in place. The upper end of the stirrer shall becut to fit into the slot on the lower end of the axle in theplastometer head.6.1.6 Guide Sleeve, provided near the upper end of thestirrer to

23、guide the latter within the barrel, with a clearance ofat least 0.05 mm 0.002 in.6.2 Plastometer HeadThe plastometer head shall consistof a fixed-speed motor connected directly to a hysteresis brakewhich is capable of adjustment from 29gcmto2.90gcm11.4 g in. to 114 g in. torque. Each complete revolu

24、tion, or100-dial division, shall be recorded on a magnetic counteractuated by an electric eye or other suitable method. The torqueshall be checked using a drive pulley, transfer pulley, mono-filament line, and weights as shown in Fig. 2. Adjust thehysteresis brake torque to lift a 38.00 g 6 0.1 g 0.

25、0836 lb 60.00022 lb weight over one full rotation of the slotted axle andnot lift a 42.00 g 6 0.1 g 0.924 lb 6 0.00022 lb weight overone full rotation of the slotted axle. The lifted weights includethe variable weight of the monofilament line between thetransfer pulley and the attached weight. All i

26、nstruments shouldbe checked in this manner at least once each week.6.3 FurnaceAn electrically heated furnace with suitablemanual, or automatic, controls shall be provided so that aheating rate of 3.0 C min 6 0.1 C min 5.4 F min 60.18 F min, on an over-all basis, with not more than 3.0 C6 1.0 C 5.4 F

27、 6 1.8 F for any given minute can bemaintained over a temperature range from 300 C to 550 C572 F to 1022 F. This temperature circuit should bechecked and standardized periodically. The furnace shall con-tain a molten solder bath of approximately 50 % lead and 50 %tin composition. Temperature in the

28、bath shall be measuredwith a suitable thermocouple in a 6.35 mm 0.250 in. outsidediameter protection tube immersed in the bath so that the tubetouches the outside wall of the crucible, and the hot junction ofthe couple is at the same height as the center of the coal charge.A stirrer shall be used to

29、 agitate the solder. A suitable furnaceis illustrated in Fig. 3.6.4 Loading DeviceThe loading device shall be providedso that the coal may be packed uniformly in the crucible undera total packing load of 10 kg 22 lb and designed in such amanner that, after compression, the crucible and its contentsc

30、an easily be removed from the device without disturbing thecontents. A suitable device is shown in Fig. 4. The use of astatic weight of 9 kg 19.8 lb together with a drop-weight of1 kg 2.2 lb dropped twelve times from a height of 114.3 mm4.5 in. is permissible as an alternative method of packing. The

31、drop-weight arrangement is shown in Fig. 5. For coals that aredifficult to pack, it is permissible to add one to three drops ofbenzene or toluene on the shaft of the stirrer near the surface ofthe coal before the weight is added.7. Sample7.1 Collect a representative gross sample of coal in accor-dan

32、ce with Practice D2234/D2234M and prepare in accordancewith Practice D2013/D2013M. The 2.36 mm (No. 8) sievesample from Table 1 in Practice D2013/D2013M shall consti-tute the laboratory sample.8. Preparation of Sample8.1 Air dry the sample prior to preparation. Spread thesample on tared pans, weigh,

33、 and air dry it at room temperatureor at slightly elevated temperatures not exceeding 15 C27 F above room temperature, until the moisture loss is lessthan 0.1 % h. Drying should not be continued beyond thispoint so that the plastic properties of the coal are not altered byoxidation. After air drying

34、, reduce the sample by riffling to noless than 500 g 1.1 lb. Stage crush this 500 g 1.1 lb portionto pass through a 850 m (No. 20) sieve and reduce to 250 g0.55 lb by riffling. Stage crush this 250 g 0.55 lb portion topass through a 425 m (No. 40) sieve and riffle it to 125 g0.275 lb. Mix the coal a

35、nd scoop 5.0 g 0.011 lb for the test.Seal the excess prepared coal for additional test runs asrequired. Test the coal for plastic properties within eight hoursafter the sample passes through a 425 m (No. 40) sieve.9. Procedure9.1 The hysteresis brake is normally adjusted to101.6gcm6 5.1gcm40.0gin.6

36、2.0 g in. torque.9.2 Mount the crucible, with the stirrer in place, in theloading device as shown in Fig. 4 but with the cage raised.Charge 5.0 g 0.011 lb of the prepared sample of coal into thecrucible. Lower the cage onto the coal and press firmly with thefingers. Rotate the stirrer slightly with

37、the fingers to fill thevoids under the rabble arms. Then lower the cage on the coaland apply the 10 kg 22 lb weight, making sure that the totalweight is transmitted to the coal charge. Compress the chargefor 15 min, after which remove the loading device, takingextreme care not to disturb the positio

38、n of the stirrer in the coal.If an alternative method of packing is used, use the same care.D2639/D2639M 163Screw the barrel on to the plastometer head, making sure thatthe top of the stirrer fits in the slotted end of the axle.9.3 Lower the assembled apparatus into the furnace until thebottom of th

39、e crucible is immersed to a depth of 76.2 mm3 in. in the molten solder bath maintained at a temperature of300 C 572 F. Place the thermocouple in the bath in accor-dance with 6.3. The heating control shall be such that the bathwill reattain the initial temperature in 10 6 2 min afterimmersion of the

40、retort. Thereafter, heat the retort at a rate of3.0 C min 6 0.1 C min 5.4 F 6 0.18 F on the over-allbasis.9.4 Temperature and stirrer rotation measurements shall bemade at 1 min intervals between the initial softening andsolidification temperatures for the analyzed coal test sample.10. Number of Tes

41、ts10.1 All tests shall be made in duplicate, and the averagevalues reported.11. Care of Plastometer11.1 The dimensions of the rabble arms on the stirrer shallmeet the specifications in 6.1.5 and Fig. 1. In addition tothorough cleaning of the stirrer and crucible between tests, it isimportant that th

42、e dimensions of the rabble arms be checked atfrequent intervals. The stirrer is to be discarded when any ofthe rabble arms has a diameter 1.47 mm 0.058 in. or has a6.10 mm 0.24 in. length.12. Calculation12.1 From the measured dial division per minute readings,determine the maximum fluidity of the te

43、st sample.13. Report13.1 Report the following information: initial softeningtemperature; maximum fluidity temperature; solidificationtemperature; plastic range and maximum fluidity.FIG. 2 Pulley Arrangement To Calibrate TorqueD2639/D2639M 16413.2 Report the arithmetic average of the maximum fluidity

44、for individual determinations that meet the requirements of14.1.1 as follows:(a) average maximum fluidity less than 1000 DDPM,report to the nearest 1 DDPM.(b) average maximum fluidity between 1000 DDPM and10 000 DDPM, round and report to the nearest 10 DDPM.(c) average maximum fluidity between 10 00

45、0 DDPM and20 000 DDPM, round and report to the nearest 100 DDPM.(d) average maximum fluidity between 20 000 DDPM and30 000 DDPM, round and report to the nearest 1000 DDPM.(e) average maximum fluidity greater than 30 000 DDPM,report as greater than () 30 000 DDPM.NOTE 1It is recognized that some plas

46、tometers currently in use havethe capability to read and record the fluidity to the nearest 0.1 DDPM. Forcoals which exhibit a maximum fluidity less than 10 DDPM, and whererequired, it is acceptable to round and report the average maximumfluidity to the nearest 0.1 DDPM.13.3 If either breaking or ja

47、mming was observed, a state-ment that maximum fluidity cannot be verified due to thephenomenon should be added to the report.13.4 Example Report:13.4.1 Individual maximum fluidity results for duplicatedeterminations are found as 27 536 DDPM and 22 437 DDPM.The average of the duplicate determinations

48、 is 24 986 DDPM.Repeatability for the two determinations is 62499 DDPM ofthe average. The repeatability statement in 14.1.1 is notsatisfied. A further third determination yields a result of 25 957DDPM. The average of the first and third determinations,respectively, is 26 746 DDPM. Repeatability for

49、these twodeterminations is 62675 DDPM of the average. The repeat-ability statement is now satisfied. Rounding the average of thetwo repeatable determinations to the nearest 1000 DDPMaccording to 13.2(d) provides a reported result of 27 000DDPM.Initial Softening Temperature: 388 CMaximum Fluidity Temperature: 440 CSolidification Temperature: 490 CPlastic Range: 102 CMaximum Fluidity: 27 000 DDPMFIG. 3 Furnace AssemblyFIG. 4 Loading