1、Designation: D2639/D2639M 13Standard 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, nas used in this testmethod, a measure of stirrer rotation rate. There are 100 dialdivisions for each full 360 rotation of the s
8、tirrer. Stirrerrotation rate is total dial divisions turned by the stirrer in a oneminute 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 of coal in
9、to 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 rotation rate,
10、 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 solidification tempe
11、rature, nas used in this testmethod, the temperature at which the 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 which t
12、he 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 behavi
13、or 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 Coke.Cur
14、rent edition approved Oct. 1, 2013. Published December 2013. Originallyapproved in 1967. Last previous edition approved in 2008 as D263908. DOI:10.1520/D2639_D2639M-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
15、 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 ofthe following
16、:6.1.1 RetortA steel retort consisting of four parts asshown in Fig. 1.FIG. 1 Retort AssemblyD2639/D2639M 1326.1.2 Retort Crucible, cylindrical, 21.4 6 0.08 mm0.844 6 0.003 in. in inside diameter and 35.0 mm 1.38 in.in depth, with exterior threads for joining the crucible to thecrucible cover. The c
17、rucible shall have a 2.38- 6 0.02-mm0.094- 6 0.001-in. diameter notch in the center of its insidebase 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 crucible cover to the barrel.
18、The inside diameter ofthe hole which accommodates the stirrer is 9.53 6 0.08 mm0.375 6 0.003 in.6.1.4 Barrel, 121 mm 4.75 in. long and having an insidediameter of 9.53 6 0.08 mm 0.375 6 0.003 in. The top endof the barrel shall be 12.7 mm 0.500 in. in inside diameter toa depth sufficient to allow cle
19、arance for the axle of theplastometer 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 shaft3.96 6 0.03 mm 0.156 6 0.001 in. in di
20、ameter and equippedwith four rabble arms. The lower end of the stirrer shall havea 60 included angle. The rabble arms on the stirrer shall be1.59 6 0.03 mm 0.0625 6 0.001 in. in diameter, 6.35 6 0.05mm 0.250 6 0.002 in. in length, and shall be placed perpen-dicular to the shaft at 90 intervals aroun
21、d the shaft and3.18 6 0.03 mm 0.125 6 0.001 in. apart center to centeralong the shaft. The middle two rabble arms shall be set at 180to each other, and likewise, the remaining two arms 180 toeach other. The lowest rabble arm shall be set in the shaft togive 1.59-mm 0.0625-in. clearance between it an
22、d the bottomof the crucible when the stirrer is in place. The upper end of thestirrer shall be cut to fit into the slot on the lower end of theaxle in the plastometer head.6.1.6 Guide Sleeve, provided near the upper end of thestirrer to guide the latter within the barrel, with a clearance ofat least
23、 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 29- to 2.90-g cm 11.4-to 114-g in. torque. Each complete revolution, or 100-dialdivision, shall be recorded on a magnetic counter
24、 actuated byan electric eye or other suitable method. The torque shall bechecked using a drive pulley, transfer pulley, monofilamentline, and weights as shown in Fig. 2. Adjust the hysteresisbrake torque to lift a 38.00- 6 0.1-g 0.0836 6 0.00022 lbweight over one full rotation of the slotted axle an
25、d not lift a42.00- 6 0.1-g 0.924 6 0.00022 lb weight over one fullrotation of the slotted axle. The lifted weights include thevariable weight of the monofilament line between the transferpulley and the attached weight. All instruments should bechecked in this manner at least once each week.6.3 Furna
26、ceAn electrically heated furnace with suitablemanual, or automatic, controls shall be provided so that aheating rate of 3.0 6 0.1C/min 5.4 6 0.18F/min, on anover-all basis, with not more than 3.0 6 1.0C 5.4 6 1.8Ffor any given minute can be maintained over a temperaturerange from 300 to 550C 572 to
27、1022F. This temperaturecircuit should be checked and standardized periodically. Thefurnace shall contain a molten solder bath of approximately50 % lead and 50 % tin composition. Temperature in the bathshall be measured with a suitable thermocouple in a 6.35-mm0.250-in. outside diameter protection tu
28、be immersed in thebath so that the tube touches the outside wall of the crucible,and the hot junction of the couple is at the same height as thecenter of the coal charge. A stirrer shall be used to agitate thesolder. A suitable furnace is illustrated in Fig. 3.6.4 Loading DeviceThe loading device sh
29、all 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 contentscan easily be removed from the device without disturbing thecontents. A suitable device is shown in Fig.
30、 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. Thedrop-weight arrangement is shown in Fig. 5. For coals that aredifficult to pack, it is permissible to a
31、dd 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-dance with Practice D2234/D2234M and prepare in accordancewith Practice D2013/D2013M. The 2.36 mm (No. 8)
32、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, and air dry it at room temperatureor at slightly elevated temperatures not exceeding 15C 27Fabove room
33、 temperature, until the moisture loss is less than0.1 %/h. Drying should not be continued beyond this point sothat the plastic properties of the coal are not altered byoxidation. After air drying, reduce the sample by riffling to noless than 500 g 1.1 lb. Stage crush this 500 g 1.1 lb portionto pass
34、 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 and scoop 5.0 g 0.011 lb for the test.Seal the excess prepared coal for additional test runs asrequired. T
35、est 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 to101.6- 6 5.1-g cm 40.0- 6 2.0-g in. torque.9.2 Mount the crucible, with the stirrer in place, in theloading device as shown in Fig.
36、 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 the fingers to fill thevoids under the rabble arms. Then lower the cage on the coaland apply the 10-kg 22
37、-lb weight, making sure that the totalweight is transmitted to the coal charge. Compress the chargefor 15 min, after which remove the loading device, takingD2639/D2639M 133extreme care not to disturb the position of the stirrer in the coal.If an alternative method of packing is used, use the same ca
38、re.Screw 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 the crucible is immersed to a depth of 76.2 mm 3in. in the molten solder bath maintained at a temperature o
39、f300C 572F. 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 retort. Thereafter, heat the retort at a rate of3.0 6 0.1C/min 5.4 6 0.18F on the over-all basis.9.4 Temper
40、ature 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 Tests10.1 All tests shall be made in duplicate, and the averagevalues reported.11. Care of Plastometer11.1 The dimensio
41、ns 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 isFIG. 2 Pulley Arrangement To Calibrate TorqueD2639/D2639M 134important that the dimensions of the rabble arms be checked atfrequent i
42、ntervals. 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 test sample.13. Report13.1 Report the following informati
43、on: initial softeningtemperature; maximum fluidity temperature; solidificationtemperature; plastic range and maximum fluidity.13.2 Report the maximum fluidity to the nearest 1 ddpm.Maximum fluidities greater than 30,000 ddpm should bereported as greater than () 30,000 ddpm.13.3 If either breaking or
44、 jamming was observed, a state-ment that maximum fluidity cannot be verified due to thephenomenon should be added to the report.14. Precision and Bias14.1 Precision:14.1.1 RepeatabilityFor duplicate tests carried out at dif-ferent times in the same laboratory, by the same operator, withthe same appa
45、ratus, on representative portions taken from thesame sample after the last stage of the reduction process, allcharacteristic temperature points should agree within 5C9F. Likewise, maximum rates of drum dial movement ofduplicate tests should agree within 610 % of the arithmeticaverage of the two test
46、s. If these criteria are not met, a third testshould be run. If there is agreement between two of the threetests, use their arithmetic average for reporting. If agreementbetween the three tests is unsatisfactory, the average of thethree individual tests should be reported.14.1.2 ReproducibilityIt is
47、 not practical to specify thereproducibility of this test method because numerous round-robin experiments have demonstrated inherent variance of testequipment.NOTE 1Round-robin experiments have included both coal and syn-thetic standards.FIG. 3 Furnace AssemblyFIG. 4 Loading DeviceFIG. 5 Loading Dev
48、iceD2639/D2639M 13514.1.2.1 It has been determined there are no valid statisticaldata for the establishment of a reproducibility statement for thistest method. This test method should, therefore, be used only asan indicator of the plastic properties of coal.14.2 BiasThis test method, including calib
49、ration, is anempirical procedure. Therefore, the degree of absolute biascannot be determined.15. Keywords15.1 carbonization; contraction; dial divisions; expansion;fluidity; gieseler; plasticity; rheologyASTM 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 rig
