1、Designation: D5515 97 (Reapproved 2010)1D5515 17Standard Test Method forDetermination of the Swelling Properties of Bituminous CoalUsing a Dilatometer1This standard is issued under the fixed designation D5515; the number immediately following the designation indicates the year oforiginal adoption or
2、, in the case of revision, the 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 NOTEAdded research report information to Section 14 editorially in September 2010.INTRODU
3、CTIONThe principle of this test method is that the final volume of char obtained at the conclusion of astandard dilatation test is dependent on the mass of coal in the coal pencil and on the radius of theretort tube. This test method incorporates a procedure which: determines the mass of air-dried c
4、oal inthe coal pencil; provides a means to measure the average retort tube radii; and employs a means toreport coal expansion on an air dried coal weight basis.Other test methods used to determine the swelling properties of bituminous coals include the Ruhr(ISO 8264) and Audibert-Arnu (ISO 349) Inte
5、rnational Standard Organization (ISO) test methods.However these two ISO test methods provide consistently different values for percent dilatation andpercent contraction. Percent contraction and dilatation values obtained using the Audibert-Arnu testmethod are higher and lower respectively than thos
6、e obtained using the Ruhr test method. Thesedifferences have been attributed to trimming the length of the coal pencil from different ends. TheAudibert-Arnu test method specifies that the wider end of the coal pencil be trimmed while the Ruhrtest method specifies that the narrower end of the coal pe
7、ncil be trimmed.1. Scope1.1 This test method specifies a procedure for the measurement of the swelling of bituminous coal using a dilatometer.1.2 The test method is limited in applicability to those coals which have a free swelling index 1 as determined in accordancewith Test Method D720.1.3 The val
8、ues stated in SI units (IEEE/ASTM SI-10) are to be regarded as standard.1.4 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 establish appropriate safety and health practices and determine t
9、he applicability of regulatorylimitations prior to use.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedb
10、y the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D720 Test Method for Free-Swelling Index of CoalD2013 Practice for Preparing Coal Samples for AnalysisD2234/D2234M Practice for Collection of a Gross Sample of CoalIEEE/ASTM SI-10 St
11、andard for Use of the International System of Units (SI): The Modern Metric System1 This test method is under the jurisdiction ofASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.15 on Metallurgical Propertiesof Coal and Coke.Current edition approved May 1, 201
12、0June 15, 2017. Published May 2010June 15, 2017. Originally approved in 1994. Last previous edition approved in 20042010 asD5515 97 (2004)(2010)21. DOI: 10.1520/D5515-97R10E01.10.1520/D5515-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at ser
13、viceastm.org. For Annual Book of ASTM Standardsvolume information, refer 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.
14、 Becauseit may not be technically possible to adequately depict all changes 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.Copyright ASTM International,
15、100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 International Standardization Organization (ISO) Standards:3ISO 349 Hard Coal-Audibert-Arnu Dilatometer TestISO 8264 Hard CoalDetermination of the Swelling Properties Using a Dilatometer3. Terminology3.1 Abbrevia
16、tions:3.1.1 basement level reference mark height, BLRMht, the char height as measured using the BLRM, after removing thepiston/retort assembly as a unit after completion of the test, expressed in millimetres.3.2 coal pencil, a 60-mm-long test specimen formed by compression in a mold from coal which
17、has been pulverized to passa 250-m (No. 60) sieve.3.3 dry coal pencil mass, Mdry, the calculated mass of the trimmed 60-mm-long coal pencil corrected for added water, expressedin grams.3.4 equivalent percent dilatation for 2.50 g of air dried coal, %D2.50, the calculated percent expansion for a 2.50
18、-g,unmoistened, 60-mm-long, coal pencil corrected for average tube radii, expressed as a percentage.3.5 maximum contraction temperature, T2, the temperature at which the coal pencil starts swelling, expressed in degreesCelsius. For coals which exhibit contraction only, T2 is the temperature at which
19、 the coal pencil reaches its minimum (see Fig.1). For coals that exhibit contraction only and are still contracting at 500C, T2 will be reported as taken at 500C (see Fig. 1d).3.6 maximum dilatation temperature, T3, the temperature at which the coal pencil first reaches a maximum height after swelli
20、ng,expressed in degrees Celsius (see Fig. 1).3.7 percent contraction, %C, the minimum recorded height of char expressed as a percentage, based on an initial coal pencilheight of 60 mm (see Fig. 1).3.8 percent dilatation, %D, the maximum recorded height of char expressed as a percentage, based on an
21、initial coal pencilheight of 60 mm (see Fig. 1).3.9 softening temperature, T1, the temperature at which the height of the coal pencil contracts 1.0 % (0.6 mm) from the highestrecorded initial pencil height, expressed in degrees Celsius (see Fig. 1).3.10 wet coal pencil mass, Mwet, the measured mass
22、of a trimmed 60-mm-long coal pencil weight, expressed in grams.3 Available from International Organization for Standardization (ISO), 1, ch. de la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.FIG. 1 Types of Dilatation CurvesD5515 1724. Summary of Test Method4.1 Th
23、e test involves preparing a coal pencil and determining the changes of the coal pencil height in a retort tube during aprescribed heating cycle.5. Significance and Use5.1 Values of the dilatation properties of coals may be used to predict or explain the behavior of a coal or blends duringcarbonizati
24、on or in other processes such as gasification, liquefaction, and combustion.6. Apparatus6.1 Dilatometer apparatus, a typical arrangement of the dilatometer apparatus is shown in Fig. 2. The apparatus consists of thefollowing:6.1.1 Electric FurnaceThe dilatometer furnace has a core consisting of a 65
25、-mm-diameter cylindrical block of aluminumbronze, resistant to oxidation, and having a sufficiently high melting point. The length of the furnace core can vary from 400 to460 mm depending on the length of the retort tubes used. The block has three symmetrically placed 15-mm-diameter bored holescapab
26、le of accepting three retort tubes. The core is heated electrically by insulated resistance windings capable of being controlledat a temperature ramp rate of 3.0 6 0.1C per minute from within 7 min of the time a test is started to a final temperature of 520C.The furnace shall perform in accordance w
27、ith the specifications outlined in 8.2. The thermocouple used for temperature controlis situated in a retort tube placed in the third role of the core. The thermocouple tip is placed in contact with the retort tube wall60 mm above the bottom of the retort tube plug.6.1.2 System for Measuring Piston
28、Movement and TemperatureThe system shall be capable of measuring the lineardisplacement of the piston to the nearest 1.0 mm and providing a correlation of displacement with temperature.6.1.3 Retort Tube and PistonsThe retort tube consists of a seamless tube of steel, with an internal diameter of 8.0
29、0 6 0.05mm and an external diameter of 14.50 6 0.05 mm. It shall have a support collar at the top and be threaded to accept a gastight,threaded plug at its base. The retort tube shall have a minimum length of 345 mm and be supported only by its collar when placedin the furnace. The retort tube shall
30、 be discarded when its internal diameter exceeds 8.15 mm.6.1.3.1 The piston shall be machined from a steel rod to a finished diameter of 7.80 6 0.05 mm. The piston shall be of sufficientlength to permit the mechanical recording or transducer assembly to record a coal pencil height of 30 mm. The pist
31、on andmechanical recording or transducer assembly shall weigh 150 6 10 g. The piston shall be discarded when its diameter is less than7.65 mm.FIG. 2 Typical Dilatometer ApparatusD5515 1736.1.3.2 The piston and retort tube shall be marked and used as a matched set and require identification imprinted
32、 on both theretort tube and its matched piston. A line, called the Basement Level Reference Mark (BLRM), shall be imprinted on the piston,so when assembled with its matched retort tube, with plug in place, the BLRM is even with the top of the retort tube. The lengthfrom the bottom of the piston to t
33、he BLRM is the length of the retort tube bore with plug in place.6.2 Mold and AccessoriesThe mold and accessories shall be capable of producing a 60.0 6 0.5-mm-long coal pencil. Themold shall have a 70.0 6 0.1-mm inside bore length with a taper of 1:50. The narrow end of the bore shall have a diamet
34、er of6.00 6 0.01 mm. Use a trimming block to facilitate the trimming of the coal pencil to length and the subsequent weighing of thetrimmed pencil (see Note 1). The portion of the trimming block holding the pencil shall not weigh more than 155 g.NOTE 1The coal pencil may be trimmed to length from ei
35、ther end.6.3 Cleaning Implements (Recommended)The cleaning implements for the retort tube consist of an approximately7.95-mm-diameter reamer and a 9-mm bronze wire rifle brush with suitable attachments to permit cleaning of the full length ofthe retort tube. A circular wire brush, attached to a benc
36、h top mounted grinder, is recommended for the cleaning of the pistons.6.4 BalanceThe balance shall have a weighing range of 160.00 g with 0.01-g readability.7. Preparation of Sample7.1 Collect a gross sample in accordance with the requirements of Test Method D2234/D2234M.7.2 The analysis sample shal
37、l consist of a minimum of 50 g of coal pulverized to 250-m (No. 60) sieve in accordance withTest Method D2013. Perform the dilatation analysis on the coal sample passing 250-m (No. 60) sieve within five days afterreduction to 250-m (No. 60) sieve.8. Calibration8.1 For all systems not using a mechani
38、cal pen/chart, calibrate the recorder of piston height when there is a difference of 3.0mm or more between the final char heights as calculated from the chart readout and those directly measured using the BLRM fortwo consecutive determinations.8.2 The furnace, while being ramped at 3C per minute, mu
39、st meet the following temperature criteria with the empty retort tubesplaced in Bores 1 and 2 of the furnace and all temperature measurements made with the thermocouple(s) in contact with the retorttube wall(s): temperatures measured in Bores 1 and 2 must be 63.0C measured at the same height for 45-
40、mm intervalsencompassing the bottom 180 mm; temperatures between the control thermocouple placed in its usual position and those of Bores1 and 2 measured at 45-mm intervals shall be 63.0C for the bottom 135 mm and 66C for the next 45 mm. The furnacetemperature profile shall be calibrated every twelv
41、e months.8.3 The dilatometer temperature readout of the measuring thermocouple shall be checked every four months by comparison witha digital thermometer which is calibrated for the same type of thermocouple. If the temperature difference is greater than 3C, thenthe dilatometer furnace temperature r
42、eadout requires recalibration using a temperature calibrator.8.4 Calibrate the retort tubes, as described in Annex A1, every four months.prior to initial use and after every 50 tests.9. Preparation of the Coal Pencil9.1 All weights shall be recorded to the nearest 0.01 g. Care must be taken to avoid
43、 sample loss and the following steps mustbe performed without a break.9.1.1 Preparation of Homogeneous Coal Sample and Water MixThe amount of water in the mix shall be 11 % on a weightbasis.9.1.1.1 Weigh a mixing vessel. Record the mass as M1.9.1.1.2 Add approximately 2 g of coal to the pre-weighed
44、mixing vessel; distribute the coal evenly over the bottom of the mixingvessel. Record the mass as M2.9.1.1.3 Add approximately 1 mL of distilled water to the coal. Record the mass as M3.9.1.1.4 Mix the coal and water together using a metal spatula to form a homogeneous paste. Care must be taken to a
45、void lossof sample.9.1.1.5 Add another increment of approximately 8 g of coal. Record the mass as M4. Mix to homogeneity using a metal spatula.9.2 Construction of the Coal Pencil:9.2.1 If a mold release agent has been applied to the bore of the pencil mold, then excess release agent must be removed
46、byforcing a wad of tissue through the bore of the mold before adding the moistened coal.9.2.2 Add not less than ten increments of the moistened coal to a mold and compact.9.2.3 Press the coal pencil out of the mold using equipment provided. Gently place the pencil into a trimming block and trimthe p
47、encil to a 60-mm length. Discard the trimmed off portion of the pencil. Record the mass of the trimmed coal pencil andtrimming block as M5.D5515 1749.3 Transfer the trimmed coal pencil into the top of the horizontally placed retort tube. The coal pencil is gently pushed to thebottom of the retort tu
48、be with the matched piston. Check that the matched piston slides freely inside the retort tube. Record themass of the trimming block and any fragments of the trimmed pencil not transferred into the retort tube as M6. To determine theaccurate mass of coal in the coal pencil, it is essential that any
49、untransferred fragments of the coal pencil are weighed along withthe trimming block.10. Procedure10.1 Clean the dilatometer retort and piston assembly. Firmly attach the retort tube plugs to the retort tubes. Check that thematched piston slides freely in the retort tube.10.2 Prepare the coal pencils and load them into the retort tubes as described in Section 9.10.3 Load both retort tube and piston assemblies, charged with trimmed coal pencils, into the dilatometer furnace which isthermally stabilized at its 315C setpoint. Start the temperature co
