1、Designation: D 7582 10Standard Test Methods forProximate Analysis of Coal and Coke by MacroThermogravimetric Analysis1This standard is issued under the fixed designation D 7582; 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These instrumental test methods cover the determinationof moisture, volatile matter, and ash, and the calculati
3、on offixed carbon in the analysis of coal and coke samples preparedin accordance with Practice D2013 and Practice D346.1.2 These instrumental test methods are not applicable tothermogravimetric analyzers using microgram size samples.1.3 Test Methods D3173, D3174, and D3175 shall beconsidered the ref
4、eree test methods.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 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
5、 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:2D121 Terminology of Coal and CokeD346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice
6、 for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3174 Test Method for Ash in the Analysis Sample of Coaland Coke from CoalD3175 Test Method for Volatile Matter in the AnalysisSample of Coal and CokeD3176 Practice for Ultimate Analysis of C
7、oal and CokeD3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD3302 Test Method for Total Moisture in CoalD5016 Test Method for Total Sulfur in Coal and CokeCombustion Residues Using a High-Temperature TubeFurnace Combustion Method with Infrared AbsorptionE691
8、 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology D121.4. Summary of Test Method4.1 In thermogravimetric analysis the mass of a sample in acontrolled atmosphere is recor
9、ded repeatedly as a function oftemperature or time, or both. In macro thermogravimetricanalysis a sample size of approximately 1 g is used. All massmeasurements are conducted by the system. In a typicalanalysis, the temperature is normally ramped from ambient toa specific temperature and held at tha
10、t temperature for aprescribed length of time. The mass change is recordedrepeatedly during the entire procedure. For the thermogravi-metric analysis of coal and coke samples the moisture and ashanalyses are complete when the sample reaches a constantmass as defined in the instrumental operating para
11、meters.Alternatively, the measurement of moisture and ash can beconsidered complete after heating the sample for a fixed periodof time. In the volatile matter analysis, the samples are weighedafter heating to 950C and held at this temperature for 7 min.4.2 Moisture is determined by measuring the los
12、s in mass ofthe analysis specimen of coal or coke when heated underspecified conditions of temperature, time, atmosphere, speci-men mass, and equipment specifications.4.3 Volatile matter is determined by measuring the loss inmass of the analysis specimen of coal or coke when heatedunder rigidly cont
13、rolled conditions. The measured mass loss isused to calculate the volatile matter after correcting for themoisture content.1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition a
14、pproved June 1, 2010. Published July 2010. Originally approvedin 2009. Last previous edition approved in 2009 as D7582-09. DOI: 10.1520/D758210.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards v
15、olume 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.4.4 Ash is determined by measuring the mass of the residueremaining after burning the coal or coke spe
16、cimen underspecified conditions of specimen mass, temperature, time,atmosphere, and equipment specifications.4.5 In these test methods, moisture, volatile matter, and ashcan be determined sequentially in a single instrumental proce-dure. Another procedure allows the moisture and ash to bedetermined
17、sequentially. Moisture and ash can also be deter-mined in separate determinations. Ruggedness testing and pastexperiences have shown the volatile matter values determinedon samples without first determining the moisture (drying thesample) are always higher than those of the dried samples.4.6 Good la
18、boratory practice requires checking for biasesbetween analytical methods for contractual compliance. Whenonly a few coal types will be routinely tested, the instrumentused in these test methods must be shown to yield results, forthe coal(s) to be tested, that are equivalent to those obtainedusing Te
19、st Methods D3173, D3174, and D3175. If they arefound to be not equivalent, either the instrument used iscalibrated or the instrumental results are adjusted to establishand maintain equivalence. Alternatively, when a broad spec-trum of coal types will be tested, the instrument used in thesetest metho
20、ds shall be calibrated using certified referencematerials of known composition covering the range of param-eters being determined. The certified values shall be estab-lished using Test Methods D3173, D3174, and D3175. Section16.2 lists a number of biases that have been shown to existbetween instrume
21、ntal results. Other biases, of unknown mag-nitude and sign, may exist for other coals.5. Significance and Use5.1 Moisture, as determined by this instrumental testmethod, is used for calculating other analytical results to a drybasis using procedures in Practice D3180.5.2 Moisture can be used in conj
22、unction with the air-drymoisture loss determined by Test Method D3302 to determinetotal moisture in coal. Total moisture is used for calculatingother analytical results to an as-received basis using PracticeD3180.5.3 Ash yield is the residue remaining after heating the coaland coke samples (see Note
23、 1).NOTE 1The ash obtained differs in composition and amount from themineral constituents present in the original coal. Combustion causes anexpulsion of all water, the loss of carbon dioxide from carbonates, theconversion of iron pyrite into iron oxides and sulfur oxides, and otherchemical reactions
24、. Ash yield, as determined by this test method, candiffer from the amount of ash produced in furnace operations or othercombustion systems because combustion conditions influence the chem-istry and amount of ash.5.4 Ash yield is used, (1) as a parameter for evaluatingsampling procedures and coal cle
25、aning processes, (2) in theultimate analysis calculation of oxygen by difference usingPractice D3176, (3) in calculations including material balance,reactivity and yields of products relevant to coal conversionprocesses such as gasification and liquefaction, (4) in calcula-tions to estimate the load
26、ing on electrostatic precipitators andon the fly ash and bottom ash disposal systems as well aserosion rates on boiler systems.5.5 Volatile matter yield, when determined as herein de-scribed, may be used to (1) indicate coke yield on carboniza-tion, (2) provide the basis for purchasing and selling,
27、or (3)establish combustion characteristics.5.6 Fixed carbon is a calculated value. It is the differencebetween 100 and the sum of the percent moisture, ash, andvolatile matter. All percents shall be on the same moisturereference base.5.7 Moisture, ash, and volatile matter are three of theprincipal p
28、arameters used for assessing the quality of coal.6. Interferences6.1 There are no known interferences for these test methods.7. Apparatus7.1 Macro Thermogravimetric Analyzer (Macro TGA)Acomputer controlled apparatus consisting of a furnace with acavity large enough to accept crucibles containing tes
29、t speci-mens that meet the minimum mass requirements of theprocedure. The macro TGA system can accommodate multiplecrucibles, allowing for continuous analysis with one cruciblereserved for the blank or reference crucible. The furnace isconstructed so the cavity is surrounded by a suitable refractory
30、and insulated so as to develop a uniform temperature in allparts of the cavity, but with a minimum free space. The furnaceshall be capable of being heated rapidly (30-45C/min fromambient to 950C. The temperature shall be monitored andmaintained at values specified for each determination. Thesystem s
31、hall have an integrated balance capable of weighingthe crucibles and test specimens repeatedly throughout theanalysis. All mass measurements are conducted and recordedby the system. The sensitivity of the balance shall be at least0.1 mg. Provision shall be made to introduce gases specifiedfor this s
32、tandard and to remove products of drying, devolatil-ization, and combustion. The macro TGA system shall have aventing fan, tolerant of hot product gases, to efficiently removethe exhaust gases.7.2 Crucibleswith covers of composition and dimensionsspecified for the instrument by the instrument manufa
33、cturer.The covers shall fit closely enough so that the carbon depositfrom bituminous, subbituminous, and lignitic coals does notburn away from the underside of the cover during the deter-mination of the volatile matter8. Reagents and Materials8.1 Drying GasNitrogen (99.5% purity), Argon (99.5%purity
34、) or air, dried to a moisture content of 1.9 mg/L or less(dew point 10C or less).8.2 Inert GasNitrogen (99.5% purity) or Argon (99.5%purity).8.3 Oxidizing GasOxygen (99.5% purity) or air.8.4 Certified Reference MaterialsCoal or coke material(s)meeting the requirements of 10.1, with a certificate of
35、analysisspecifying the reference value and the uncertainty of thereference value. Reference material(s) can be employed tocalibrate the instrument for the determination of volatilematter. Certified reference values shall have been establishedusing Test Methods D3173, D3174, and D3175. ReferenceD7582
36、102materials used for the calibration of volatile matter shallinclude information on the certificate of analysis detailing themethod(s) employed to determine volatile matter of the refer-ence material.9. Hazards9.1 The user shall insure acceptable documented safetyprocedures are in place for the han
37、dling of all reagents and testmaterials and for the operation of laboratory equipment speci-fied for these test methods.9.2 Venting EquipmentInstall equipment in the vicinity ofthe apparatus to vent combustion and volatile gases evolvedduring the test procedures from the laboratory.10. Analysis Samp
38、le10.1 The analysis sample shall be the material pulverized topass a 250-m (No. 60) sieve in accordance with PracticeD2013 or Practice D346.11. Preparation of Apparatus11.1 Verify the instrument can meet all specifications in thestandard with respect to gas flows, heating rates, and balancesensitivi
39、ty prior to use. Condition the instrument after initialsetup, or repairs, by conducting a run through a complete cyclewithout samples.11.2 Condition new crucibles and covers for use in these testmethods by heating under the same conditions of the test andcool before use.11.3 The macro TGA system can
40、 be programmed to termi-nate the measurement process when the test specimens andcrucibles have reached a constant mass. Crucibles are weighedby the instrument at specified intervals. The analysis iscomplete when the sample reaches constant mass. Constantmass is defined as a point where the mass chan
41、ge is or = to0.05% over a nine-minute period, either by using not less thanthree successive weighings or a fixed nine-minute period ofsuccessive weighings. This mass change of 0.05% is equivalentto 0.0005 g for a 1.0000 g sample. Alternately, the instrumentcan be programmed to allow for moisture and
42、 ash determina-tion by heating the test specimens for the time periods, heatingrates and soak temperatures specified in Test Methods D3173and D3174. The mass measured at the end of the time periodis used for calculations.12. Calibration and Standardization12.1 The instrument shall be calibrated for
43、the determina-tion of volatile matter employing certified reference materials.The calibration shall be performed at the same furnace ramptemperature as that used for the analysis. Do not use coalreference materials(s) for coke volatile matter calibration. Donot use coke reference material(s) for coa
44、l volatile mattercalibration. Use coal reference material(s) with a certifiedreference value and uncertainty based on measurements madeemploying Test Methods D3173, D3174, and D3175 to cali-brate this test method.13. Procedure13.1 The determination of moisture, followed by volatilematter followed by
45、 ash can be carried out in sequence using thesame test specimen. Alternatively, the determination of mois-ture, volatile matter, or ash can be carried out separately on testspecimens of coal or coke.13.2 Sequential Determination of Moisture, Volatile Matterand Ash:13.2.1 After verifying instrument s
46、etup according to Section11 on the preparation of apparatus, load and tare the crucibles.Add1g6 0.1 g of coal or coke to the crucible in the balanceposition and weigh immediately before advancing the nextcrucible. Transfer the test specimen from the sample bottle tothe crucible quickly to minimize t
47、he exposure of the testspecimen to the atmosphere during the initial weighing pro-cess.13.2.2 For moisture determinations, heat the weighed testspecimens in crucibles without the covers at 107 6 3 C. Usea drying gas flow rate of 0.4 to 1.4 furnace volume changes perminute (see 8.1). Program the inst
48、rument to terminate the testwhen the test specimens and crucibles have reached a constantmass (see 11.3). Alternatively, program the instrument to allowfor moisture determination by heating the test specimens for 1h.13.2.3 For volatile matter determinations following themoisture analysis, place cove
49、rs on the crucibles in the TGAcarousel (the crucibles are placed automatically in somesystems and manually in others). Program the instrument toreweigh the crucibles, with specimens inside, and covers inplace before initiating the volatile matter part of the cycle.13.2.3.1 To provide an inert atmosphere, use nitrogen orargon with a flow rate of 0.7 to 1.4 furnace volume changes perminute to sweep away the volatile components. Raise thefurnace temperature at a rate such that the temperature is raisedfrom 107C to 950 6 10C in a 26-30 min time period (SeeNote 2). Program
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