1、Designation: D5865 12D5865 13Standard Test Method forGross Calorific Value of Coal and Coke1This standard is issued under the fixed designation D5865; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A num
2、ber in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method pertains to the determination of the gross calorific value of coal and coke by either an isoperibol oradiabatic bomb cal
3、orimeter.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 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 es
4、tablish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific hazard statements are given in Section 8.2. Referenced Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD346 Practice for Collection and Preparation of Coke Sa
5、mples for Laboratory AnalysisD388 Classification of Coals by RankD1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample of Coal and CokeD3177 Test Methods for Total Sulfur in the Analysis Sample of Coal and Cok
6、e (Withdrawn 2012)3D3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different BasesD4239 Test Method for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace CombustionD7582 Test Methods for Proximate Analysis of Coal and Coke by Macro Thermog
7、ravimetric AnalysisE144 Practice for Safe Use of Oxygen Combustion BombsE178 Practice for Dealing With Outlying ObservationsE882 Guide for Accountability and Quality Control in the Chemical Analysis LaboratoryE2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids
8、3. Terminology3.1 For additional definitions of terms used in this test method, refer to Terminology D121.3.2 Definitions:3.2.1 adiabatic calorimetera calorimeter that operates in the adiabatic mode and may or may not use a microprocessor. Theinitial temperature before initiating the combustion and
9、the final temperatures are recorded by the operator or the microprocessor.3.2.2 automated calorimetera calorimeter which has a microprocessor that takes the thermometric readings and calculates theCalibration Value and the Heat of Combustion Values.3.2.3 British thermal unit Btuis the amount of heat
10、 required to raise the temperature of one pound - mass lbm of liquidwater at one atmosphere pressure one degree Fahrenheit at a stated temperature. The results of combustion calorimetric tests offuels for steam power plants may be expressed in terms of the 1956 International Steam Table calorie (I.T
11、. cal) which is definedby the relation, 1 I.T. cal = 4.1868 J. The Btu used in modern steam tables is defined by the means of the relation, 1 I.T. cal / g= 1.8 I.T. Btu / lb. Thus, 1 I.T. Btu / lb = 2.326 J / g.1 This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and i
12、s the direct responsibility of Subcommittee D05.21 on Methods of Analysis.Current edition approved Sept. 1, 2012Oct. 1, 2013. Published November 2012October 2013. Originally approved in 1995. Last previous edition approved in 20112012as D5865 11a.D5865 12. DOI: 10.1520/D5865-12.10.1520/D5865-13.2 Fo
13、r referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is refere
14、nced on www.astm.org.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. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that us
15、ers 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.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consh
16、ohocken, PA 19428-2959. United States13.2.4 calorific valuethe heat produced by combustion of a unit quantity of a substance under specified conditions.3.2.5 calorimetera device for measuring calorific value consisting of a bomb, its contents, a vessel for holding the bomb,temperature measuring devi
17、ces, ignition leads, water, stirrer, and a jacket maintained at specified temperature conditions.3.2.6 gross calorific value (gross heat of combustion at constant volume), Qv (gross)the heat produced by completecombustion of a substance at constant volume with all water formed condensed to a liquid.
18、3.2.7 heat of formationthe change in heat content resulting from the formation of 1 mole of a substance from its elements atconstant pressure.3.2.8 isoperibol calorimetera calorimeter that operates in the isoperibol mode and uses a microprocssor to record the initialand final temperatures and make t
19、he appropiate heat leak corrections during the temperature rise. It determines when thecalorimeter is in equilibrium and ignites the sample and determines when the calorimeter has reached equilibrium after ignition.3.2.9 net calorific value (net heat of combustion at constant pressure), Qp (net)the
20、heat produced by combustion of a substanceat a constant pressure of 0.1 MPa (1 atm), with any water formed remaining as vapor.3.3 Definitions of Terms Specific to This Standard:3.3.1 corrected temperature risethe calorimeter temperature change caused by the process that occurs inside the bombcorrect
21、ed for various effects.3.3.2 heat capacitythe energy required to raise the temperature of the calorimeter one arbitrary unit.3.3.2.1 DiscussionThe heat capacity can also be referred to as the energy equivalent or water equivalent of the calorimeter.4. Summary of Test Method4.1 The heat capacity of t
22、he calorimeter is determined by burning a specified mass of benzoic acid in oxygen. A comparableamount of the analysis sample is burned under the same conditions in the calorimeter. The calorific value of the analysis sampleis computed by multiplying the corrected temperature rise, adjusted for extr
23、aneous heat effects, by the heat capacity and dividingby the mass of the sample.4.2 Oxidation of coal after sampling can result in a reduction of calorific value. In particular, lignite and sub-bituminous rankcoal samples may experience greater oxidation effects than samples of higher rank coals. Un
24、necessary exposure of the samples tothe air for the time of sampling or delay in analysis shall be avoided. (See X2.1.)5. Significance and Use5.1 The gross calorific value can be used to compute the total calorific content of the quantity of coal or coke represented bythe sample for payment purposes
25、.5.2 The gross calorific value can be used for computing the calorific value versus sulfur content to determine whether the coalmeets regulatory requirements for industrial fuels.5.3 The gross calorific value can be used to evaluate the effectiveness of beneficiation processes.5.4 The gross calorifi
26、c value can be required to classify coals according to Classification D388.6. Apparatus and Facilities6.1 Test AreaAn area free from drafts, shielded from direct sunlight and other radiation sources. Thermostatic control of roomtemperature and controlled relative humidity are desirable.6.2 Combustio
27、n BombConstructed of materials that are not affected by the combustion process or the products formed tointroduce measurable heat input or alteration of end products. The bomb shall be designed so that all liquid combustion productscan be completely recovered by washing the inner surfaces. There sha
28、ll be no gas leakage. The bomb shall be capable ofwithstanding a hydrostatic pressure test to 20 MPa (3000 psig) at room temperature without stressing any part beyond its specifiedelastic limit.6.3 BalanceA laboratory balance capable of weighing the analysis sample to the nearest 0.0001 g. The balan
29、ce shall bechecked weekly, at a minimum, for accuracy.6.4 Calorimeter VesselMade of metal with a tarnish-resistant coating, with all outer surfaces highly polished. Its size shall besuch that the bomb is completely immersed in water during a determination. A stirrer shall be provided for uniform mix
30、ing of thewater. The immersed portion of the stirrer shall be accessible to the outside through a coupler of low thermal conductivity. Thestirrer speed shall remain constant to minimize any temperature variations due to stirring. Continuous stirring for 10 min shall notraise the calorimeter temperat
31、ure more than 0.01C when starting with identical temperatures in the calorimeter, test area andD5865 132jacket. For calorimeters having a bucket it can be a separate component or integral component of the bomb. The vessel shall beof such construction that the environment of the calorimeters entire o
32、uter boundaries can be maintained at a uniform temperature.6.5 JacketA container with the inner perimeter maintained at constant temperature 60.1C (isoperibol) or at the sametemperature 60.1C as the calorimeter vessel (adiabatic) during the test. To minimize convection, the sides, top and bottom of
33、thecalorimeter vessel shall not be more than 10 mm from the inner surface of the jacket. Mechanical supports for the calorimetervessel shall be of low thermal conductivity.6.6 Thermometers:6.6.1 Platinum resistance or thermistor thermometersshall be capable of measuring to the nearest 0.0001C. These
34、 types ofthermometers consist of two major subsystems. The first and most obvious is the temperature sensing probe itself. The second andequally important aspect is the measurement subsystem. For both subsystems, the relationship between the thermometer resistanceand temperature shall be well charac
35、terized. The absolute temperature shall be known to 6 0.1 C at the temperature of thecalorimetric measurement.6.6.2 Assessing the valid working range of the calorimeter, as outlined in 10.9, is sufficient to demonstrate that all importantaspects of the calorimeter functionality, including the thermo
36、metry, are in good working order. The traceability of the heat ofcombustion measurement is governed by the traceability of the heat of combustion of the benzoic acid calibrant in addition tomeeting the aforementioned criteria.6.6.3 Liquid-in-Glass ThermometersConforming to the requirements for therm
37、ometers S56C, S116C, or S117C as prescribedin Specification E2251.6.6.3.1 Thermometer AccessoriesAmagnifier is required for reading liquid-in-glass thermometers to one tenth of the smallestscale division. The magnifier shall have a lens and holder designed so as to minimize errors as a result of par
38、allax.6.7 Sample HolderAn open crucible of platinum, quartz, or base metal alloy. Before use in the calorimeter, heat treat basemetal crucibles for a minimum of 4 h at 500C to ensure the crucible surface is completely oxidized. Base metal alloy cruciblesare acceptable, if after three preliminary fir
39、ings, the weight does not change by more than 0.0001 g.6.8 Ignition FuseIgnition fuse of 100-mm length and 0.16-mm (No. 34 B filling the calorimeter vessel; firing the ignitioncircuit; recording calorimeter temperatures before, during, and after the test; recording the balance weights; and carrying
40、out allnecessary corrections and calculations.6.11 Crucible LinerQuartz fiber or alundum for lining the crucible to promote complete combustion of samples that do notburn completely during the determination of the calorific value.47. Reagents7.1 Reagent WaterConforming to conductivity requirements f
41、or Type II of Specification D1193 for preparation of reagentsand washing of the bomb interior.7.2 Purity of ReagentsUse reagent grade chemicals conforming to the specification of the Committee on Analytical Reagentsof the American Chemical Society in all tests.57.3 Benzoic AcidStandard (C6H5COOH)Pel
42、lets made from benzoic acid available from the National Institute of Standardsand Technology (NIST) or benzoic acid calibrated against NIST standard material. The calorific value of benzoic acid, for use inthe calibration calculations, shall be traceable to a recognized certificate value.7.4 OxygenM
43、anufactured from liquid air, guaranteed to be greater than 99.5 % pure, and free of combustible matter. Oxygenmade by the electrolytic process contains small amounts of hydrogen rendering it unfit unless purified by passage over copperoxide at 500C.7.5 Titration IndicatorMethyl orange, methyl red, o
44、r methyl purple for indicating the end point when titrating the acid formedduring combustion. The same indicator shall be used for both calibration and calorific value determinations.4 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Repor
45、t RR:D05-1025.5 Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United
46、 States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D5865 1337.6 Standard SolutionSodium carbonate (Na2CO3) or other suitable standard solution.Aconvenient standard solution may beprepared as follows. Dissolve 3.706 g of sodium carbonate, dried for 2
47、4 h at 105C, in water and dilute to 1 L. The resultingconcentration (0.0699 N) assumes the energy of formation of HNO3 under bomb conditions is -59.7 kJ/mol (-14.3 kcal/mole)(seeX1.1). One milliliter of this solution is equivalent to 4.2 J (1.0 cal) in the acid titration. Alternatively, 1.0 ml of a
48、0.1000 Nbase solution is equivalent to 6.0 J (1.4 cal) in the acid titration. In general, one milliliter of an arbitrary standard titrant solutionis equivalent to its concentration (equivalents / liter or normality N) times 59.7 J (14.3 cal).8. Hazards8.1 The following precautions are recommended fo
49、r safe calorimeter operation. Additional precautions are noted in PracticeE144. Also consult the calorimeter equipment manufacturers installation and operating instructions before using the calorimeter.8.1.1 The mass of sample and any combustion aid as well as the pressure of the oxygen admitted to the bomb shall not exceedthe bomb manufacturers specifications.8.1.2 Inspect the bomb parts carefully after each use. Replace cracked or significantly worn parts. Replace O-rings and valveseats in accordance with manufacturers instructi
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