1、Designation: D3175 17Standard Test Method forVolatile Matter in the Analysis Sample of Coal and Coke1This standard is issued under the fixed designation D3175; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 This test method covers the determination
3、of the gas-eous products, exclusive of moisture vapor, as volatile matterin the analysis sample of coal or coke from coal.1.2 The test method for the determination of volatile matteris empirical.1.3 UnitsThe values stated in SI units are to be regardedas standard.1.4 This standard does not purport t
4、o 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. Referenced Documents2.1 ASTM Standards:2D121 Ter
5、minology of Coal and CokeD346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD388 Classification of Coals by RankD2013 Practice for Preparing Coal Samples for AnalysisD3173/D3173M Test Method for Moisture in the AnalysisSample of Coal and CokeD3180 Practice for Calcula
6、ting Coal and Coke Analysesfrom As-Determined to Different BasesD5142 Test Methods for Proximate Analysis of the AnalysisSample of Coal and Coke by Instrumental Procedures(Withdrawn 2010)3D6374 Test Method for Volatile Matter in Green PetroleumCoke Quartz Crucible ProcedureD3173/D3173M Test Method f
7、or Moisture in the AnalysisSample of Coal and CokeD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 poppingunseating of the c
8、rucible cover due to swell-ing of the test sample resulting in mechanical loss of the testmaterial.3.1.1.1 DiscussionThis phenomenon is normally associ-ated with strongly swelling coals.3.1.2 sparkingthe evolution of gaseous products at a ratesufficient to mechanically carry solid particles out of t
9、hecrucible. Those particles escaping at higher temperaturesbecome incandescent when they are emitted, creating sparks.3.1.2.1 DiscussionThis phenomenon is normally associ-ated with non-swelling coals but can also be associated withswelling coals as well as cokes.3.1.3 swellingthe change in volume wh
10、ich takes placewhen coal is heated under conditions allowing the softenedcoal to expand freely in a direction normal to the plane ofheating.3.2 Refer to Terminology D121 for additional definitions ofterms used in this test method.4. Summary of Test Method4.1 Volatile matter is determined by establis
11、hing the massloss resulting from heating a coal or coke under rigidlycontrolled conditions. The measured mass loss, corrected formoisture as determined in Test Method D3173/D3173M estab-lishes the volatile matter content. Two procedures are describedto permit conformity with differences in sample be
12、havior.4.2 In this empirical test method, the use of platinumcrucibles shall be considered the standard reference method forvolatile matter. Platinum crucibles shall be used in determiningthe volatile matter determined for classification of coals byrank. Volatile matter determinations by some labora
13、tories usingalternate nickel-chromium alloy crucibles having the physical1This 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 approved Feb. 1, 2017. Published March 2017. Origin
14、allyapproved in 1973. Last previous edition approved in 2011 as D3175 11. DOI:10.1520/D3175-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Documen
15、t Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis
16、 international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TB
17、T) Committee.1dimensions specified in 6.1 have been shown to differ fromthose obtained using platinum crucibles. A laboratory utilizingnickel-chromium crucibles shall first determine if a relativebias exists between the use of nickel-chromium and platinumcrucibles on the coals being tested using the
18、 test method setforth in Annex A1. Where a relative bias is shown to exist, thevolatile matter determined using nickel-chromium cruciblesshall be corrected by a factor determined through comparisonof volatile matter results from both crucible types on coalsbeing tested or analysis of samples of know
19、n proximateanalysis.5. Significance and Use5.1 Volatile matter, when determined as herein described,can be used to establish the rank of coals, to indicate coke yieldon carbonization process, to provide the basis for purchasingand selling, or to establish burning characteristics.6. Apparatus6.1 Plat
20、inum Crucible, with closely fitting cover, for coal.The crucible shall be of not less than 10 or more than 20 mLcapacity, not less than 25 or more than 35 mm in diameter, andnot less than 30 or more than 35 mm in height.6.2 Platinum Crucible, with closely fitting cover, for coke.The crucible shall b
21、e of 10 mL capacity, with capsule coverhaving thin flexible sides fitting down into crucible. Or thedouble-crucible method can be used, in which the sample isplaced in 10 mL platinum crucible, which is then covered withanother crucible of such a size that it will fit closely to the sidesof the outer
22、 crucible and its bottom will rest 8.5 to 12.7 mm (13to12 in.) above the bottom of the outer crucible.6.3 Alternate Crucible Materials, Nickel-chromium cru-cible with closely fitting cover. The crucible shall not be lessthan 10 or more than 20 mL capacity, not less than 25 or morethan 35 mm in diame
23、ter, and not less than 30 or more than 35mm in height. Nickel-chromium crucibles shall be heat-treatedfor4hat500C to ensure that they are completely oxidizedprior to use.6.3.1 Quartz crucible with closely fitting cover for cokesamples. The crucible shall be the same type as specified foruse with Tes
24、t Method D6374.6.4 Vertical Electric Tube Furnace, for coal or coke. Theelectric furnace shall be a vertical tube furnace. The furnacecan be of the form shown in Fig. 1. It shall be regulated tomaintain a temperature of 950 6 20C in the crucible, asmeasured by a thermocouple positioned in the furnac
25、e. Thefurnace shall accommodate sparking coals and meet thespecifications set forth in 8.3.2.6.5 Balance, sensitive to 0.1 mg.7. Reagents and Materials7.1 DesiccantsUse freshly regenerated self-indicatingdesiccants. Suitable materials are listed as follows.7.1.1 Anhydrous Calcium Sulfate7.1.2 Silica
26、 Gel8. Procedure8.1 The sample shall be the material pulverized to 250 m(No. 60) sieve in accordance with Practice D2013 or PracticeD346.8.1.1 Carry out a moisture determination in accordancewith Test Method D3173/D3173M on a separate portion of theanalysis sample preferably on the same day but not
27、more than24 h apart from the volatile matter determination so thatreliable corrections to other bases can be made.8.2 Procedure for Nonsparking Coals and Cokes:8.2.1 Record the mass of the crucible and cover to thenearest 0.0001 g. For coals place1gofthesample in aplatinum crucible. For coke samples
28、 platinum, nickel-chromium or quartz crucibles are permitted. Close with a coverwhich fits closely enough so that the carbon deposit frombituminous, subbituminous, and lignite coals does not burnaway from the underside. Record the total mass of the crucible,sample and cover to the nearest 0.0001 g.
29、Place the crucible onplatinum or nickel-chromium wire supports and insert directlyinto the furnace chamber, which shall be maintained at atemperature of 950 6 20C, and lower immediately to the950C zone. Regulation of the temperature to within theprescribed limits is critical. After the more rapid di
30、scharge ofvolatile matter has subsided, as shown by the disappearance ofthe luminous flame, or in the case of coke, after 2 or 3 min,inspect the crucible (see Note 1) to verify that the lid is stillproperly sealed. If necessary, reseat the lid to guard against theadmission of air into the crucible.
31、Do this as rapidly as possibleby raising the crucible to the top of the furnace chamber,reposition the lid to more perfectly seal the crucible, then lowerthe crucible immediately back to the 950C zone.After heatingfor a total of exactly 7 min, remove the crucible from thefurnace and without disturbi
32、ng the cover, allow it to cool. Cokeshould be cooled in a desiccator. Weigh as soon as cold. Thepercentage loss of weight minus the percentage moistureequals the volatile matter. With some strongly caking low-volatile and medium-volatile bituminous coals, the coke buttoncan be broken with explosive
33、violence due to the liberation ofvolatile matter within the button. This is usually designated aspopping. Such popping can blow the lid off the crucible andcause mechanical losses of the coked material. When suchpopping is observed, the determination shall be rejected andthe test repeated until popp
34、ing does not occur.NOTE 1Inspection of the crucible can be aided by the use of a mirrorheld above the furnace well.8.3 Modified Procedure for All Sparking Fuels:8.3.1 Fuels that do not cake or cake weakly when volatilematter is determined shall be watched closely for sparkingduring the heating perio
35、d (see 8.3.3); also, at the end of the testthe crucible cover shall be inspected for ash deposits, and thepresence of such deposits shall be considered as evidence ofsparking.8.3.2 All fuels that spark when the volatile matter isdetermined by the methods described in 8.1 shall be treated asfollows:
36、The sample shall be given a preliminary gradualheating such that a temperature of 600 6 50C is reached in 6min (8.3.3). After this preliminary heating the sample shall beD3175 172heated for exactly 6 min at 950 6 20C. If sparking is thenobserved, the determination shall be rejected and the testrepea
37、ted until no sparking occurs either during the preliminaryheating or during the 6 min period at 950C. Remove thecrucible from the furnace, cool on a metal cooling block, andweigh. To ensure uniformity of results, keep the cooling periodconstant and do not prolong beyond 15 min. The percentageloss in
38、 weight minus the percent moisture in accordance withTest Method D3173/D3173M, is the volatile matter. All analy-ses by this test method shall be so marked when reported toindicate that the modified procedure was used.8.3.3 If a tubular furnace of the Fieldner type (Fig. 1) is usedfor the determinat
39、ion of volatile matter, the preliminary gradualheating can be accomplished by moving the crucible topredetermined positions in the cooler top zone of the furnace.Due to variations in the heating characteristics of the furnace,the operator shall predetermine by thermocouple the properpositions to mee
40、t a preliminary heating rate as specified inFIG. 1 Electric Furnace for Determining Volatile MatterD3175 1738.3.2. A mechanical device to lower the crucible into thefurnace can be used to facilitate control of the loweringoperation.9. Calculation9.1 Calculate the percent mass loss on heating as foll
41、ows:mass loss %, D 5 100 3 B 2 C! B 2 A!# (1)where:A = mass of crucible and cover, g,B = mass of crucible and cover and contents before heating,g, andC = mass of crucible and cover and contents after heating, g.9.2 Calculate the percent volatile matter in the analysissamples as follows:Volatile matt
42、er in analysis sample, % 5 D 2 E (2)where:D = mass loss, %, andE = moisture in analysis sample, %, as determined by TestMethods D3173/D3173M and D7582.9.3 The calculated volatile matter in the analysis sample isthe as-determined volatile matter.10. Report10.1 Report the volatile matter in the analys
43、is sample alongwith the sample moisture from 8.1.1.10.2 Report the procedure employed for the determinationof volatile matter. Report as the D3175 Procedure for Nonspar-king Fuels or the D3175 Procedure for Sparking Fuels.10.3 The volatile matter result can be reported in any of anumber of bases dif
44、fering in the manner in which the moistureis treated. Procedures for converting the test result obtained onan analysis sample to other bases are described in PracticeD3180.10.4 Use Classification D388 for reporting volatile matteron a dry mineral matter free basis.11. Precision and Bias11.1 The prec
45、ision of this test method for the determinationof Volatile Matter in Coal are shown in Table 1. CoalRepeatability and Reproducibility limits for this test methodwere determined using only platinum crucibles. Coal Repeat-ability and Reproducibility limits for nickel-chromium cru-cibles have not been
46、determined.11.1.1 Repeatability Limit (r)The value below which theabsolute difference between two test results of separate andconsecutive test determinations, carried out on the samesample, in the same laboratory, by the same operator, using thesame apparatus on samples taken at random from a single
47、quantity of homogeneous material, can be expected to occurwith a probability of approximately 95 %.11.1.2 Reproducibility Limit (R)The value below whichthe absolute difference between two test results carried out indifferent laboratories, using samples taken at random from asingle quantity of materi
48、al that is as homogeneous as possible,can be expected to occur with a probability of approximately95 %.11.2 The precision of this test method for the determinationof Volatile Matter in Coke are shown in Table 2. The precisioncharacterized by repeatability (Sr, r) and reproducibility (SR,R)is describ
49、ed in Table A2.1 in Annex A2.11.2.1 The inter-laboratory proficiency test data employedto derive the r and R values for cokes include 48 samplescovering a period of 11 years. Some of the samples weredistributed as many as three separate times. All crucible typeswere included for the derivation of the precision statement forcoke offered in this test method. There are a number of reasonsfor this. Of the 20 to 22 participants taking part in theproficiency testing program only 10 to 12 reported volatilematter by D3175. The remaining participants employed Test
