1、Designation: D 2639 04e1Standard Test Method forPlastic Properties of Coal by the Constant-Torque GieselerPlastometer1This standard is issued under the fixed designation D 2639; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEEditorial changes were made throughout in January 2005.1. Scope1.1 This test method covers a relative measure of the
3、 plasticbehavior of coal when heated under prescribed 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
4、 values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 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-pria
5、te safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 2013 Practice of Preparing Coal Samples for AnalysisD 2234 Practice for Collection of a Gross Sample of Coal3. Terminology3.1 Definitions:3.1.1 dial div
6、ision per minute, nas used in this testmethod, a measure of stirrer rotation rate. There are 100 dialdivisions for each full 360 rotation of the stirrer. Stirrerrotation rate is total dial divisions turned by the stirrer in a oneminute time period.3.1.2 initial softening temperature, nas used in thi
7、s testmethod, the temperature at which the stirrer rotation rate firstreaches 1.0 dial divisions per minute.3.1.3 maximum fluidity, nas used in this test method, themeasured maximum stirrer rotation rate, in dial divisions perminute.3.1.4 maximum fluidity temperature, nas used in this testmethod, th
8、e temperature at which stirrer rotation rate reaches amaximum value.3.1.5 plastic range, ndifference between the solidificationtemperature and the initial softening temperatures.3.1.6 solidification temperature, nas used in this testmethod, the temperature at which the the first zero ddpm isreached
9、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 the coal is charged. The crucible isimmersed in a bath and the temperature increased uniformly.Th
10、e 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 behavior of a coal or blends duringcarbonization or in other processes such as gasification, lique-fac
11、tion, and combustion.6. Apparatus6.1 Gieseler PlastometerThe apparatus shall consist ofthe following:6.1.1 RetortA steel retort consisting of four parts asshown in Fig. 1.6.1.2 Retort Crucible, cylindrical, 21.4 6 0.08 mm(0.844 6 0.003 in.) in inside diameter and 35.0 mm (1.38 in.)in depth, with ext
12、erior threads for joining the crucible to thecrucible cover. The crucible shall have a 2.38- 6 0.02-mm1This 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.Current edition
13、approved Nov. 1, 2004. Published November 2004. Originallyapproved in 1967. Last previous edition approved in 1998 as D 263998e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informati
14、on, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.FIG. 1 Retort AssemblyD 2639 04e12(0.094- 6 0.001-in.) diameter notch in the center of its insidebase to serve as a s
15、eat for the stirrer.6.1.3 Retort Crucible Cover, with interior threads for join-ing the crucible cover to the crucible and exterior threads forjoining the crucible cover to the barrel. The inside diameter ofthe hole which accommodates the stirrer is 9.53 6 0.08 mm(0.375 6 0.003 in.).6.1.4 Barrel, 12
16、1 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 clearance for the axle of theplastometer head when the apparatus is assembled. A hole,fitted with a tube, sh
17、all 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 diameter and equippedwith four rabble arms. The lower end of the stirrer shall havea 60 included angle. T
18、he 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 around the shaft and3.18 6 0.03 mm (0.125 6 0.001 in.) apart center to centeralong the shaft. The middle
19、 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 and the bottomof the crucible when the stirrer is in place. The upper end of thestirrer shall be
20、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 0.05 mm (0.002 in.).6.2 Plastometer HeadThe plastometer head shall consistof a fixed-speed mot
21、or 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 actuated byan electric eye or other suitable method. The torque shall bechecked using a d
22、rive pulley, transfer pulley, monofilamentline, and weights as shown in Fig. 2. Adjust the hysteresisbrake torque to lift a 38.00- 6 0.1-g weight over one fullrotation of the slotted axle and not lift a 42.00- 6 0.1-g weightover one full rotation of the slotted axle. The lifted weightsinclude the va
23、riable weight of the monofilament line betweenthe transfer pulley and the attached weight. All instrumentsshould be 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 6 0.
24、1C/min, on an over-all basis, with notmore than 3.0 6 1.0C for any given minute can be maintainedover a temperature range from 300 to 550C. This temperaturecircuit should be checked and standardized periodically. Thefurnace shall contain a molten solder bath of approximately50 % lead and 50 % tin co
25、mposition. Temperature in the bathshall be measured with a suitable thermocouple in a 6.35-mm(0.250-in.) outside diameter protection tube 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 ch
26、arge. A stirrer shall be used to agitate thesolder. A suitable furnace is 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 and designed in such a mannerthat, after compression, the
27、crucible and its contents can easilybe removed from the device without disturbing the contents. Asuitable device is shown in Fig. 4. The use of a static weight of9 kg together with a drop-weight of 1 kg dropped twelve timesfrom a height of 114.3 mm (4.5 in.) is permissible as analternative method of
28、 packing. The drop-weight arrangement isshown in Fig. 5. For coals that are difficult to pack, it ispermissible to add one to three drops of benzene or toluene onthe shaft of the stirrer near the surface of the coal before theweight is added.7. Sample7.1 Collect a representative gross sample of coal
29、 in accor-dance with Test Methods D 2234 and prepare in accordancewith Practice D 2013. Approximately 4 kg of coal crushed topass a 4.75-mm (No. 4) sieve shall constitute the laboratorysample.8. Preparation of Sample8.1 Air dry the sample prior to preparation. Spread thesample on tared pans, weigh,
30、and air dry it at room temperatureor at slightly elevated temperatures not exceeding 15C aboveroom temperature, until the moisture loss is less than 0.1 %/h.Drying should not be continued beyond this point so that theplastic properties of the coal are not altered by oxidation. Afterair drying, grind
31、 the 4-kg sample to pass a 2.36 mm (No. 8)sieve and reduce it by riffling to no less than 500 g. Grind this500 g portion to pass through a 850-m (No. 20) sieve andreduce to 250 g by riffling. Stage crush this 250 g portion topass through a 425-m (No. 40) sieve and riffle it to 125 g. Mixthe coal and
32、 scoop 5.0 g for the test. Seal the excess preparedcoal for additional test runs as required. Test the coal for plasticproperties within eight hours after the sample passes through a425-m (No. 40) sieve.9. Procedure9.1 The hysteresis brake is normally adjusted to 101.6-6 5.1-g cm (40.0- 6 2.0-g in.)
33、 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 of the prepared sample of coal into the crucible.Lower the cage onto the coal and press firmly with the fingers.Rotate the stirrer slightly with the fingers to fil
34、l the voids underthe rabble arms. Then lower the cage on the coal and apply the10-kg weight, making sure that the total weight is transmittedto the coal charge. Compress the charge for 15 min, after whichremove the loading device, taking extreme care not to disturbthe position of the stirrer in the
35、coal. If an alternative methodof packing is used, use the same care. Screw the barrel on to theplastometer head, making sure that the top of the stirrer fits inthe 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.
36、2 mm (3D 2639 04e13in.) in the molten solder bath maintained at a temperature of300C. Place the thermocouple in the bath in accordance with6.3. The heating control shall be such that the bath will reattainthe initial temperature in 10 6 2 min after immersion of theretort. Thereafter, heat the retort
37、 at a rate of 3.0 6 0.1C/minon the over-all basis.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 Tests10.1 All tests shall be made in duplicate, and the ave
38、ragevalues 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 the dimensions of the rabble arms be checked atfrequent in
39、tervals. The stirrer is to be discarded when any ofthe rabble arms has a diameter #1.47 mm (0.058 in.) or has a#6.10-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 info
40、rmation: initial softeningtemperature; maximum fluidity temperature; solidificationtemperature; plastic range and maximum fluidity.14. Precision and Bias14.1 Precision:FIG. 2 Pulley Arrangement To Calibrate TorqueD 2639 04e1414.1.1 RepeatabilityFor duplicate tests carried out atdifferent times in th
41、e same laboratory, by the same operator,with the same apparatus, on representative portions taken fromthe same sample after the last stage of the reduction process, allcharacteristic temperature points should agree within 5C.Likewise, maximum rates of drum dial movement of duplicatetests should agre
42、e within 610 % of the arithmetic average ofthe two tests. If these criteria are not met, a third test should berun. If there is agreement between two of the three tests, usetheir arithmetic average for reporting. If agreement betweenthe three tests is unsatisfactory, the average of the threeindividu
43、al tests should be reported.14.1.2 ReproducibilityIt is 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.14.1.2.
44、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 calibration, is anempirical pro
45、cedure. Therefore, the degree of absolute biascannot be determined.15. Keywords15.1 carbonization; contraction; dial divisions; expansion;fluidity; gieseler; plasticity; rheologyFIG. 3 Furnace AssemblyFIG. 4 Loading DeviceFIG. 5 Loading DeviceD 2639 04e15ASTM International takes no position respecti
46、ng 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 stand
47、ard 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 Internation
48、al Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.T
49、his standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 2639 04e16
