1、Designation: D 2014 97 (Reapproved 2004)Standard Test Method forExpansion or Contraction of Coal by the Sole-Heated Oven1This standard is issued under the fixed designation D 2014; 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a large-scale laboratory test forobtaining information on the expansion or contract
3、ion of coalor coal blends during carbonization under specified conditions.This test method is applicable in the examination of coals orcoal blends intended for use in the manufacture of coke.1.2 The values stated in SI units shall be regarded asstandard. Inch-pound units shall be accepted on an equi
4、valentbasis.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-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.
5、Referenced Documents2.1 ASTM Standards:2D 2013 Method of Preparing Coal Samples for AnalysisD 2234 Practice for Collection of a Gross Sample of CoalD 3302 Test Method for Total Moisture in CoalE 11 Specification for Wire Cloth and Sieves for TestingPurposes3. Summary of Test Method3.1 During the tes
6、t, a measured thickness of coal about 102mm (4 in.) is heated from the bottom surface while a forcecorresponding to 15.2 kPa (2.20 psi) is applied to the topsurface through a piston. At the end of the test, the thickness ofthe coke is measured by observing the final position of thepiston.4. Signific
7、ance and Use4.1 The values determined in this test method indicate towhat extent a given coal or coal blend will expand or contractduring the carbonization process when evaluated in terms ofpertinent experience with other coals and coal blends andprocessing conditions used in commercial-type coke ov
8、ens.5. Apparatus5.1 Test Oven Assembly, consisting of the following: eithera single-chamber oven having approximately 280-mm (11-in.)width, 610-mm (24-in.) length, and 280-mm depth, or adouble-chambered oven with two chambers each having ap-proximately 280-mm width, length, and depth; a heatingsyste
9、m to heat the charge(s) unidirectionally through the soleaccording to a controlled program; piston(s) arranged so that aconstant load may be applied to the top surface of the charge;and suitable instrumentation so that appropriate temperaturesand the position of the piston(s) may be measured. Theaux
10、iliary equipment includes apparatus facilitating the charg-ing of the oven in a standard manner. The vertical partition ofthe double-chambered oven may be of 2-in. (51-mm) firebricktile or equivalent.5.1.1 Carbonization Chamber:5.1.1.1 The sole shall be of silicon carbide tile, about 40 mm(1.5 in.)
11、thick, 305 mm (12 in.) wide, and extending approxi-mately 75 mm (3 in.) beyond the carbonization chamber at thefront and back. Side, front, and back walls should be 40-mmfirebrick tile or equivalent. It is appropriate to key the sole tothe side and back tiles. The top edges of sidewalls shall be hel
12、din an adjustable steel framework so that the walls may be madeand maintained precisely perpendicular to the sole. Hole(s)6.35 mm (0.25 in.) in diameter shall be provided through theside of the oven to enable the placement of thermocouple(s) onthe top surface of the sole in the center of the oven ch
13、amber(s).5.1.1.2 In constructing the oven, the sides and ends of thecarbonization chamber shall be surrounded with at least 200mm (8 in.) of insulating refractories and the whole assemblyencased in a suitable restraining structure of steel shapes andplates designed to provide dimensional stability.5
14、.1.2 Sole-Heating System:5.1.2.1 The heating system shall consist of a group ofelectrical heating elements mounted under the silicon carbidesole and suitable equipment to provide automatic control.Heating elements may be either silicon carbide-type resistanceelements or coils of heating wire enclose
15、d in silica tubes.Elements shall be arranged to obtain minimum variation oftemperature over the area of the sole. It is desirable to1This 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
16、Coal and Coke.Current edition approved April 1, 2004. Published May 2004. Originallyapproved in 1962. Last previous edition approved in 1997 as D 2014 97.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMS
17、tandards volume information, 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.incorporate a maximum number of supports for the siliconcarbide sole tile. The brickwork and
18、 steelwork beneath theheating flues shall be of appropriate design to maintain rigidityof the oven under the temperature and load stresses ofoperation.5.1.2.2 The thermocouple used for temperature control islocated in a position which enables the sole to be heated inaccordance with the sole temperat
19、ure program shown in Table1. The heating system shall be capable of reachieving the initialset point temperature of 554C within 10 min of charging theoven and of heating the sole in accordance with the soletemperature program shown in Table 1.5.1.2.3 The temperature control thermocouple may be in-st
20、alled in the heating flue or in contact with the sole plate.5.1.3 PistonThe piston assembly shall include a massivebottom plate of metal to which an upper steel assembly isrigidly attached. The bottom plate shall be 19- or 25-mm (0.75-or 1-in.) cast steel or cast iron in one piece with square edges.
21、Dimensions are to be so chosen that the clearances betweenpiston edges and chamber walls, ends, and sides, at theconclusion of a test (upper surface of coal at 500C) are at least3.2 mm (0.125 in.) but not as much as 9.5 mm (0.375 in.). A10-to 130-mm (4.5- to 5-in.) layer of insulating refractory sha
22、ll beformed upon the steel plate, the sides being recessed somewhatwithin the piston edges. The upper steel assembly shall berigidly fastened to the corners of the lower plate with steelsupports. The upper steel assembly and corner supports shallbe of adequate strength to permit application of the d
23、esiredload and shall be fitted with appropriate hardware to permitready placement into or removal from the carbonizationchamber. A vertical hole, 13 mm (0.5 in.) in diameter, piercingthe piston assembly, including lower plate shall be provided onthe longitudinal center line for a thermocouple, about
24、 200 mm(8 in.) from either the front or rear edge of the piston.5.1.4 Apparatus for Loading PistonApparatus shall beprovided so that a constant load of 15.17 6 0.35 kPa (2.20 60.05 psi) calculated over the measured area of the piston plate,may be applied to the piston during the test. The manner ofa
25、pplying this load is not critical. Examples of suitable proce-dures are (1) use of a hydraulic piston as shown in Fig. 1, (2)use of a hinged lever-arm system bearing on a fulcrummounted on the upper steelwork of the piston structure, and (3)placement of sufficient additional dead weights on the pist
26、onitself. Whatever system is chosen should be characterized byrapid assembly for the prompt application of force aftercharging.6. Instrumentation6.1 Piston MovementThe excursion of the piston from aninitial reference position may be measured either manually, byobserving the movement of an indicator,
27、 or automatically bymeans of an appropriate transducer and recording system. Apreferred form of indicator is a witness point on a silica rodmounted on the upper surface of the lower piston plate and notconnected in any way to the remaining piston structure. Whenusing this design of indicator, no cor
28、rections need be made forexpansion of the piston structure itself. Alternatively, the basicindicator may be mounted on the upper steel structure of thepiston. In this event, any correction for piston expansion duringa test, if necessary, shall be determined by appropriate prelimi-nary calibration. M
29、easurements of the position of the indicatormay be made by directly observing the witness point with acathetometer or by using a suitable mechanical or electricalsystem of magnifying movement. Apparatus of the latter typeshould be calibrated with an accurate cathetometer. Whatevertype of indicator i
30、s used it shall be placed as close to thegeometric center of the piston as possible.6.1.1 Thermocouples shall be provided for measuring boththe temperature of the top surface of the sole (maximum ofabout 950C) and the temperature of the top surface of the coal(maximum about 500C) (Note 2). The therm
31、owell containingthe sole couple shall be placed horizontally through the hole inthe sidewall or endwall tile so that the thermowell lies flat withits tip near the geometric center of the sole. The thermowellcontaining the top surface thermocouple shall be placed in thevertical hole in the piston and
32、 adjusted so that its lowest pointis flush with the lower surface of the piston plate.NOTE 1Type K Chromel-Alumel thermocouples have proven satis-factory in these applications. Quartz or porcelain is a satisfactory materialfor thermocouple protection tubing. Mild steel or stainless tubing may alsobe
33、 used but will require frequent replacement.7. Accessory Equipment7.1 Auxiliary ApparatusNecessary auxiliary apparatus in-cludes a sole cover plate, a charging hopper, and an adjustableleveling device:7.1.1 Sole Cover Plate, conforming to the dimensions of thepiston plate and consisting of a suitabl
34、e metal frameworkcontaining either a layer of insulating brick or an equivalentlayer of insulating refractory. It shall be placed on the soleovernight and during other short periods of nonoperation toreduce heat losses and facilitate maintenance of proper soletemperature before the start of a test.7
35、.1.2 Hopper and Leveling DeviceFunctionally adequatedesigns of hopper and leveling devices are shown in Fig. 2. Theleveling device should be constructed so as to be quicklyadjustable.7.1.3 The provision of a permanently installed crane forhandling the piston in and out of the carbonization chamberfa
36、cilitates convenience of operation. A hood over the wholeassembly is desirable for the removal and venting of carbon-ization gases.8. Sampling8.1 The gross sample shall be collected in accordance withPractice D 2234.TABLE 1 Sole Temperatures ProgramTime, (h) After InitialSetpoint of 554C AchievedTem
37、perature,C0.00 5541.00 6852.00 7773.00 8404.00 8895.00 9216.00 9437.00 950from then on 950D 2014 97 (2004)28.2 About 30 kg (66 lbs) of sample (sufficient for perform-ing duplicate sole-heated oven tests) shall be prepared. Thesample shall pass a 4.75-mm (No. 4) sieve and shall havebetween 2 and 4 %
38、total moisture content. Only oversized coalis to be stage crushed to prepare the sample to pass a 4.75-mm(No. 4) sieve. If required, moisture content may be reduced byair drying. Heating the air is permitted provided that the heatedair is #10C above ambient conditions and never exceeds35C. The prepa
39、red sample is to be placed in a sealed containeruntil ready for testing. If required, moisture content of the coalmay be increased by sprinkling water over the coal andthoroughly mixing the coal and applied water together to forma homogeneous mixture.9. Procedure9.1 Maintain overnight heating levels
40、 so that the tempera-ture of a thermocouple placed on the sole, under the sole coverplate, is near 554C. As a preliminary to a test, adjust theFIG. 1 Sole-Heated OvenFIG. 2 Auxiliary EquipmentD 2014 97 (2004)3automatic controller, if necessary, to maintain this temperatureand begin the test as soon
41、as this temperature has beenachieved.9.2 For a single-chamber oven, weigh 13.1 6 0.02 kg(28.88 6 0.05 lb) of the prepared sample and transfer com-pletely to a charging hopper. For each chamber of a double-chambered oven, weigh 6.0 6 0.02 kg (13.23 6 0.05 lb) of theprepared sample and transfer comple
42、tely to a charging hopper.Shortly before loading the hopper, collect a small sample of theprepared coal for a moisture determination and place in anairtight container.9.3 With the sole thermocouple in position and indicating554C, remove the sole cover plate, place the hopper contain-ing the weighed
43、quantity of charge over the oven, and allow thecoal to fall into the carbonization chamber. Place the automatictemperature program controller into operation at the instant ofcharging. Use the leveling device, which has been preadjusted,to produce a level coal surface quickly without excess at either
44、end. A further quick adjustment of the leveling device may benecessary at this time.9.4 Lower the piston onto the surface of the coal charge,taking care to guide it so that desired clearances are maintainedon all sides. Then adjust the piston loading apparatus to give atotal loading, calculated over
45、 the actual area of the piston plate,of 15.17 6 0.35 kPa (2.20 6 0.05 psi). Take the reading,defining the initial height of the piston precisely 3 min after thedischarge of the coal or blend from the hopper. Place athermocouple in a thermowell in the vertical hole in the pistonand adjust so that the
46、 lowest point of the thermowell justtouches the top surface of the charge.9.5 It is informative to have a record of the excursion of thepiston during the test. A continuous record with automaticinstrumentation is convenient; manual readings every12 h willusually also be quite adequate. The test is c
47、onsidered to beended when the thermocouple on the top surface of the coalindicates 500C. Measure the position of the piston at thismoment and consider it as the definitive datum for thecalculation of total expansion or contraction. Record the timeinterval to this point.9.6 At the end of the test, re
48、move the piston and withdrawthe coke. Wirebrush the piston and piston plate and scrape thechamber walls to remove any accumulated carbon or tar.Replace the refractory cover plate and adjust the temperaturecontroller setting for the standby condition.NOTE 2At times, with very fluid coals, this fluid
49、coal exudes betweenthe ovenwall and the piston. If this exudate cokes or becomes solid, it maybind the piston to the ovenwall. Should this exuding occur, a knife bladeor similar tool should be used to break such bonds so that the movementof the piston is not impaired.10. Determination of Oven Constants10.1 In order that the experimental data may be interpretedproperly, determine two oven constants. One constant is theaverage area A of the carbonization chamber, expressed insquare metres (square feet). The second constant is the refer-ence height of the top surfac
