1、Designation: D3175 17D3175 18Standard 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 las
2、t revision. 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 determ
3、ination of the gaseous products, exclusive of moisture vapor, as volatile matter in theanalysis sample of coal or coke from coal.1.2 The test method for the determination of volatile matter is empirical.1.3 UnitsThe values stated in SI units are to be regarded as standard. The values given in parent
4、heses after SI units areprovided for information only and are not considered 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 safety, health, and he
5、althenvironmental practices and determine theapplicability of regulatory limitations 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 St
6、andards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD346 Practice for Collection and Preparation of Coke Samples for Laboratory AnalysisD388 Classification of
7、 Coals by RankD2013 Practice for Preparing Coal Samples for AnalysisD3173/D3173M Test Method for Moisture in the Analysis Sample of Coal and CokeD3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different BasesD5142 Test Methods for Proximate Analysis of the Analysis Sample
8、 of Coal and Coke by Instrumental Procedures (Withdrawn2010)3D6374 Test Method for Volatile Matter in Green Petroleum Coke Quartz Crucible ProcedureD3173/D3173M Test Method for Moisture in the Analysis Sample of Coal and CokeD7582 Test Methods for Proximate Analysis of Coal and Coke by Macro Thermog
9、ravimetric AnalysisE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Definitions:3.1.1 poppingunseating of the crucible cover due to swelling of the test sample resulting in mechanical loss of the testmaterial.3.1.1.1 DiscussionThis ph
10、enomenon is normally associated with strongly swelling coals.1 This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.21 on Methods of Analysis.Current edition approved Feb. 1, 2017Dec. 1, 2018. Published March 2017Janua
11、ry 2019. Originally approved in 1973. Last previous edition approved in 20112017 asD3175 11.D3175 17. DOI: 10.1520/D3175-17.10.1520/D3175-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolum
12、e information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced 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
13、been made to the previous version. 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 docum
14、ent.*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 States13.1.2 sparkingthe evolution of gaseous products at a rate sufficient to mechanically carry solid particles out of the
15、 crucible.Thosecrucible; those particles escaping at higher temperatures become incandescent when they are emitted, creating sparks.3.1.2.1 DiscussionThis phenomenon is normally associated with non-swelling coals but can also be associated with swelling coals as well as cokes.3.1.3 swellingthe chang
16、e in volume which takes place when coal is heated under conditions allowing the softened coal toexpand freely in a direction normal to the plane of heating.3.2 Refer to Terminology D121 for additional definitions of terms used in this test method.4. Summary of Test Method4.1 Volatile matter is deter
17、mined by establishing the mass loss resulting from heating a coal or coke under rigidly controlledconditions. The measured mass loss, corrected for moisture as determined in Test Method D3173/D3173M or Test Methods D7582establishes the volatile matter content. Two procedures are described to permit
18、conformity with differences in sample behavior.4.2 In this empirical test method, the use of platinum crucibles shall be considered the standard reference method for volatilematter. Platinum crucibles shall be used in determining the volatile matter determined for classification of coals by rank. Vo
19、latilematter determinations by some laboratories using alternate nickel-chromium alloy crucibles having the physical dimensionsspecified in 6.1 have been shown to differ from those obtained using platinum crucibles. A laboratory utilizing nickel-chromiumcrucibles shall first determine if a relative
20、bias exists between the use of nickel-chromium and platinum crucibles on the coals beingtested using the test method set forth in Annex A1. Where a relative bias is shown to exist, the volatile matter determined usingnickel-chromium crucibles shall be corrected by a factor determined through compari
21、son of volatile matter results from bothcrucible types on coals being tested or analysis of samples of known proximate analysis.5. Significance and Use5.1 Volatile matter, when determined as herein described, can be used to establish the rank of coals, to indicate coke yield oncarbonization process,
22、 to provide the basis for purchasing and selling, or to establish burning characteristics.6. Apparatus6.1 Platinum Crucible, with closely fitting cover, for coal. The crucible shall be of not less than 1010 mL or more than 20 mL20 mL capacity, not less than 2525 mm or more than 35 mm 35 mm in diamet
23、er, and not less than 3030 mm or more than 35 mm35 mm in height.6.2 Platinum Crucible, with closely fitting cover, for coke. The crucible shall be of 10 mL capacity, with capsule cover havingthin flexible sides fitting down into crucible. Or the double-crucible method can be used, in which the sampl
24、e is placed in 10 mLplatinum crucible, which is then covered with another crucible of such a size that it will fit closely to the sides of the outer crucibleand its bottom will rest 8.58.5 mm to 12.7 mm 12.7 mm (13 in. to 12 in.) in.) above the bottom of the outer crucible.6.3 Alternate Crucible Mat
25、erials, Nickel-chromiumnickel-chromium crucible with closely fitting cover. The crucible shall notbe less than 1010 mL or more than 20 mL 20 mL capacity, not less than 2525 mm or more than 35 mm 35 mm in diameter, andnot less than 3030 mm or more than 35 mm 35 mm in height. Nickel-chromium crucibles
26、 shall be heat-treated for 4 h at500C500 C to ensure that they are completely oxidized prior to use.6.3.1 Quartz crucible with closely fitting cover for coke samples. The crucible shall be the same type as specified for use withTest Method D6374.6.4 Vertical Electric Tube Furnace, for coal or coke.
27、The electric furnace shall be a vertical tube furnace. The furnace can beof the form shown in Fig. 1. It shall be regulated to maintain a temperature of 950950 C 6 20C20 C in the crucible, as measuredby a thermocouple positioned in the furnace. The furnace shall accommodate sparking coals and meet t
28、he specifications set forthin 8.3.2.6.5 Balance, sensitive to 0.1 mg.7. Reagents and Materials7.1 DesiccantsUse freshly regenerated self-indicating desiccants. Suitable materials are listed as follows.7.1.1 Anhydrous Calcium Sulfate7.1.2 Silica Gel8. Procedure8.1 The sample shall be the material pul
29、verized to 250 m (No. 60) sieve in accordance with Practice D2013 or Practice D346.D3175 1828.1.1 Carry out a moisture determination in accordance with Test Method D3173/D3173M or Test Methods D7582 on aseparate portion of the analysis sample preferably on the same day but not more than 24 h apart f
30、rom the volatile matterdetermination so that reliable 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 the nearest 0.0001 g. For coals place 1 g of the sample in a platinum crucible.For coke samples platinum, nick
31、el-chromiumnickel-chromium, or quartz crucibles are permitted. Close with a cover which fitsclosely enough so that the carbon deposit from bituminous, subbituminous, and lignite coals does not burn away from theunderside. Record the total mass of the crucible, sample, and cover to the nearest 0.0001
32、 g. 0.0001 g. Place the crucible on platinumor nickel-chromium wire supports and insert directly into the furnace chamber, which shall be maintained at a temperature of950950 C 6 20C,20 C, and lower immediately to the 950C950 C zone. Regulation of the temperature to within the prescribedFIG. 1 Elect
33、ric Furnace for Determining Volatile MatterD3175 183limits is critical. After the more rapid discharge of volatile matter has subsided, as shown by the disappearance of the luminousflame, or in the case of coke, after 22 min or 3 min, 3 min, inspect the crucible (see Note 1) to verify that the lid i
34、s still properlysealed. If necessary, reseat the lid to guard against the admission of air into the crucible. Do this as rapidly as possible by raisingthe crucible to the top of the furnace chamber, reposition the lid to more perfectly seal the crucible, then lower the crucibleimmediately back to th
35、e 950C950 C zone. After heating for a total of exactly 7 min, remove the crucible from the furnace andwithout disturbing the cover, allow it to cool. Coke should be cooled in a desiccator. Weigh as soon as cold. The percentage lossof weight minus the percentage moisture equals the volatile matter. W
36、ith some strongly caking low-volatile and medium-volatilebituminous coals, the coke button can be broken with explosive violence due to the liberation of volatile matter within the button.This is usually designated as popping. Such popping can blow the lid off the crucible and cause mechanical losse
37、s of the cokedmaterial. When such popping is observed, the determination shall be rejected and the test repeated until popping does not occur.NOTE 1Inspection of the crucible can be aided by the use of a mirror held above the furnace well.8.3 Modified Procedure for All Sparking Fuels:8.3.1 Fuels tha
38、t do not cake or cake weakly when volatile matter is determined shall be watched closely for sparking duringthe heating period (see 8.3.3); also, at the end of the test the crucible cover shall be inspected for ash deposits, and the presenceof such deposits shall be considered as evidence of sparkin
39、g.8.3.2 All fuels that spark when the volatile matter is determined by the methods described in 8.18.2 shall be treated as follows:The sample shall be given a preliminary gradual heating such that a temperature of 600600 C 6 50C50 C is reached in 6 min6 min (8.3.3). After this preliminary heating th
40、e sample shall be heated for exactly 6 min 6 min at 950950 C 6 20C.20 C. Ifsparking is then observed, the determination shall be rejected and the test repeated until no sparking occurs either during thepreliminary heating or during the 6 min 6 min period at 950C.950 C. Remove the crucible from the f
41、urnace, cool on a metalcooling block, and weigh. To ensure uniformity of results, keep the cooling period constant and do not prolong beyond 15 min.15 min. The percentage loss in weight minus the percent moisture in accordance with Test Method D3173/D3173M or TestMethods D7582, is the volatile matte
42、r. All analyses by this test method shall be so marked when reported to indicate that themodified procedure was used.8.3.3 If a tubular furnace of the Fieldner type (Fig. 1) is used for the determination of volatile matter, the preliminary gradualheating can be accomplished by moving the crucible to
43、 predetermined positions in the cooler top zone of the furnace. Due tovariations in the heating characteristics of the furnace, the operator shall predetermine by thermocouple the proper positions tomeet a preliminary heating rate as specified in 8.3.2. A mechanical device to lower the crucible into
44、 the furnace can be used tofacilitate control of the lowering operation.9. Calculation9.1 Calculate the percent mass loss on heating as follows:mass loss %, D51003B 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 c
45、rucible and cover and contents after heating, g.9.2 Calculate the percent volatile matter in the analysis samples as follows:Volatile matter in analysis sample,%5D 2E (2)where:D = mass loss, %, andE = moisture in analysis sample, %, as determined by Test Methods D3173/D3173M and D7582.9.3 The calcul
46、ated volatile matter in the analysis sample is the as-determined volatile matter.10. Report10.1 Report the volatile matter in the analysis sample along with the sample moisture from 8.1.1.10.2 Report the procedure employed for the determination of volatile matter. Report as the D3175 Procedure for N
47、onsparkingFuels or the D3175 Procedure for Sparking Fuels.10.3 The volatile matter result can be reported in any of a number of bases differing in the manner in which the moisture istreated. Procedures for converting the test result obtained on an analysis sample to other bases are described in Prac
48、tice D3180.10.4 Use Classification D388 for reporting volatile matter on a dry mineral matter free basis.D3175 18411. Precision and Bias11.1 The precision of this test method for the determination ofVolatile Matter in Coal areis shown in Table 1. Coal Repeatabilityand Reproducibility limits for this
49、 test method were determined using only platinum crucibles. Coal Repeatability andReproducibility limits for nickel-chromium crucibles have not been determined.11.1.1 Repeatability Limit (r)The value below which the absolute difference between two test results of separate andconsecutive test determinations, carried out on the same sample, in the same laboratory, by the same operator, using the sameapparatus on samples taken at random from a single quantity of homogeneous material, can be expected to occur with a probabilityof approximatel
