1、Designation: D6316 09b1D6316 17Standard Test Method forDetermination of Total, Combustible and Carbonate Carbonin Solid Residues from Coal and Coke1This standard is issued under the fixed designation D6316; the number immediately following the designation indicates the year oforiginal adoption or, i
2、n 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 NOTETable A1.1 was editorially corrected in June 2013.1. Scope1.1 This test method covers th
3、e determination of total, combustible, and carbonate carbon remaining in the solid byproducts ofcombustion from boiler furnaces and similar reactors, including ash, flyash, char, slag, and similar materials.1.2 This test method is intended for the use of industry to determine the performance of boil
4、er furnaces and similar combustionreactors and aid in determining the quality of the solid residue from combustion.1.3 This test method comprises the use of any of several methods to determine total carbon content combined with any ofseveral methods to determine carbonate carbon, and the calculation
5、, by difference, of the combustible carbon remaining in asample.1.4 Alternatively, this test method applies to the determination of total carbon remaining in a material after acidification withstrong acid to evolve carbonate carbon. In this case, the combustible carbon is the total carbon measured i
6、n the sample afteracidification.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in thisstandard.Non-SI units, if provided, are for information only and are contained within parentheses.1.6 This standard does not purport to address all of t
7、he safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and to determine theapplicability of regulatory limitations prior to use.1.7 This international standard was dev
8、eloped in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Docum
9、ents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD513 Test Methods for Total and Dissolved Carbon Dioxide in WaterD1756 Test Method for Determination as Carbon Dioxide of Carbonate Carbon in Coal (Withdrawn 2013)3D3178 Test Methods for Carbon and Hydrogen in the Analysis Sample of Coal and C
10、oke (Withdrawn 2007)3D3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different BasesD5373 Test Methods for Determination of Carbon, Hydrogen and Nitrogen inAnalysis Samples of Coal and Carbon inAnalysisSamples of Coal and CokeE691 Practice for Conducting an Interlaborator
11、y Study to Determine the Precision of a Test Method1 This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.29 on Major Elements inAsh and Trace Elements of Coal.Current edition approved May 1, 2009Dec. 1, 2017. Publishe
12、d June 2009December 2017. Originally approved in 1998. Last previous edition approved in 2009 asD6316 - 09a.D6316 - 09b1. DOI: 10.1520/D6316-09BE01.10.1520/D6316-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Boo
13、k 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 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 indicati
14、on 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 users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be consi
15、dered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 Other Standards:ANSI/ASME Standard, PTC 38-1980 Determining the Concentration of Particulate Matter in A Gas Stream and US EPAStandard CFR 60 Appendix A,
16、Method 174ISO 57256:0994 Accuracy of Measurement Methods and ResultsPart 6: Use in Practice of Accuracy Values3. Terminology3.1 Definitions:3.1.1 For additional definitions of terms used in this test method, refer to Terminology D121.3.1.2 carbonate carbon, nthe carbon content present in the solid p
17、roducts derived from the combustion or reaction of coal,coal byproducts, or coke as carbonates and which is non-combustible in standard industry practice.3.1.3 combustible carbon, ncarbon content remaining in the solid products derived from the combustion or reaction of coal,coal byproducts, or coke
18、, exclusive of carbonate in any form.3.1.4 total carbon, ncarbon content remaining in the solid products derived from the combustion or reaction of coal, coalbyproducts, or coke, inclusive of carbonate in any form.4. Summary of Test Method4.1 Total CarbonThe determination of total carbon is made by
19、the oxidative thermal decomposition of a weighed quantity ofsample in a closed system and, after complete oxidation and purification of the resulting gaseous products, measurement of thecarbon dioxide produced by one of several methods.4.1.1 Absorptive Determination of Total CarbonThe evolved carbon
20、 dioxide is fixed on an absorption train and is measuredquantitatively by weighing the absorbent (see Test Methods D3178).4.1.2 Instrumental Determination of Total CarbonThe carbon dioxide is measured quantitatively by an electronic detectionsystem calibrated against an appropriate reference standar
21、d (see Test Methods D5373).4.2 Carbonate CarbonThe determination of carbonate carbon is made by decomposing a weighed quantity of the sample witha dilute mineral acid, and after the purification of the evolved gases, measuring quantitatively the evolved carbon dioxide.4.2.1 Absorptive Determination
22、of Carbonate CarbonThe carbon dioxide is liberated by acidification and heating. Theevolved gases are passed through a purification train and the CO2 is fixed as Na2CO3 on a preweighed absorption unit and ismeasured gravimetrically (see Test Method D1756).4.2.2 Coulometric Determination of Carbonate
23、 CarbonThe carbon dioxide is liberated by acidification and heating. Theevolved gas is swept through a scrubber and into an absorption cell where it is coulometrically titrated (see Part B of Test MethodsD513).4.2.3 Instrumental Determination of Carbonate CarbonThe carbon dioxide is liberated by aci
24、dification and heating. Theevolved gases are purified and measured quantitatively by an electronic detection system against an appropriate reference stream.This test method resembles that for the instrumental determination of total carbon, with the provision for sample combustionreplaced by a provis
25、ion for acidification. In practice, this test method uses an adaptation to instruments designed to measure totalcarbon content.4.3 Combustible Carbon by Prior AcidificationThe determination of combustible carbon is made directly by first acidifyingand heating to dryness a weighed sample. All carbona
26、te carbon present is evolved as carbon dioxide. The dried sample is thenanalyzed for total carbon content as above. No determination of carbonate carbon is made and the carbon content measured as totalcarbon is the combustible carbon.5. Significance and Use5.1 The combustible carbon content of solid
27、 residues is used to calculate efficiency of fuel combustion in boiler furnaces andsimilar combustors.5.2 Combustible carbon values are also used to determine the residual fuel value of incompletely combusted/reacted coal andcoke in other reactors that consume carbonaceous fuels (examples include fl
28、uidized bed furnaces and liquefaction, gasification andpyrolysis reactors).5.3 The combustible carbon content of flyash is an important parameter in the use of flyash as a cement additive.6. Interferences6.1 The interferences for the determination of total carbon content are those specified in the r
29、eferenced standard methods, TestMethods D3178 and Test Methods D5373, with the following added stipulation.4 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.D6316 1726.1.1 The temperature and conditions of combustion that
30、 ensure complete conversion of a residue samples total carbon contentto carbon dioxide may be different than those required for conversion in coal samples. It is absolutely imperative that theinstrumental conditions used will ensure complete conversion of mineral carbonate in any amount or form.6.2
31、The interferences for the determination of carbonate carbon are those specified in the referenced methods, Test MethodD1756 and Part B of Test Methods D513 with the following stipulation6.2.1 Some coal combustion residues contain significant amounts of reactive elements such as CaO which will absorb
32、 carbondioxide on exposure to open air and form mineral carbonates. This absorption will influence the calculated amount of combustiblecarbon in the sample only if there was carbon dioxide chemisorption from the air between the time of the carbonate determinationand the total carbon determination. T
33、herefore, it is necessary that the sample be protected from air exposure.6.3 The mineral acid and temperature required for prior acidification of the analytical sample shall not interfere with the amountof combustible carbon present in the sample or the analytical determination of carbon. The use of
34、 oxidizing acids such asconcentrated nitric acid may oxidize a portion of the combustible carbon. Other acids such as hydrochloric acid may beincompatible with the reagents used to purify the gas stream in the instrumental determination of carbon. Sulfuric acid has arelatively high boiling point and
35、 is difficult to remove from the sample by drying. A solution of 10 % nitric acid is suggested foruse in this procedure.7. Apparatus7.1 The apparatus used is specified in the respective referenced method.7.2 Total Carbon Content:7.2.1 Absorptive Determination of Total CarbonThe apparatus consists of
36、 an oxygen-purifying train, combustion unit, andabsorption train of the type and configuration specified in Test Methods D3178.7.2.2 Instrumental Determination of Total CarbonBecause a variety of instrumental components and configurations can beused satisfactorily for these test methods, no specific
37、ations are presented here with respect to overall system design. However, theapparatus shall be capable of completely converting the carbon content to carbon dioxide, and the detection system shall determinethe carbon dioxide individually and without interference.7.3 Carbonate Carbon Content:7.3.1 A
38、bsorptive Determination of Carbonate CarbonThe apparatus shall consist of an air purifying train, reaction unit, andabsorption unit of the type and configuration specified in Test Method D1756.7.3.2 Coulometric Determination of Carbonate CarbonThe apparatus shall consist of an evolution unit, a carb
39、on dioxidecoulometer, scrubber, and pH meter of the type and configuration specified in Part B of Test Methods D513.7.3.3 Instrumental Determination of Carbonate CarbonThe apparatus shall consist of a heated acidification unit that isinstalled by bypassing the combustion system in a device designed
40、for the determination of total carbon content. The gas-purifyingsystem of such instrument shall be capable of completely removing the water content and acid gases produced as byproducts ofthe carbon dioxide evolution. The detection system shall measure the evolved carbon dioxide as an individual spe
41、cies and withoutinterference.7.4 Combustible Carbon by Prior AcidificationThe crucibles used for this method must be free of carbonate, inert to themineral acid used, and compatible with the instrument used for measuring total carbon. The acidified sample is heated to drynessusing a laboratory hotpl
42、ate capable of maintaining the fine temperature control required to dry the sample without material lossof sample as a result of spattering or boilover. The instrument used shall meet the requirements of Test Methods D5373 and becapable of removing the additional acid gases that result from the mine
43、ral acid used for evolving the carbon dioxide beforedetermining carbon content.8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents
44、of the American Chemical Society, wheresuch specifications are available.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.9. Standards9.1 There are currently no standard r
45、eference materials of coal or coke residues that are certified for combustible carbon orcarbonate carbon content. However, other types of standard materials can be used for both method validation and instrumentcalibration. These include:9.1.1 Buffalo River Sediment (NIST 2704)Total RM 8704)Total car
46、bon = 3.3483.351 6 0.016 %.0.017 %.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., Pool, Dorset,
47、U.K., and the United States Pharmacopoeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D6316 1739.1.2 Carbonate Primary Standard GradeFor example, CaCO3 total carbonate carbon = 12.00 %.nominally 12 %.9.1.3 CoalTrace Elements in Coal Bituminous (NIST 1632b)1632d)
48、total carbon = 76.8676.88 6 0.26 %.0.15 %.NOTE 1NIST SRM 1632d is scheduled to be replaced by SRM 1632e in 2018.9.1.4 EDTA Primary Standard GradeTotal carbon = 41.07 %.nominally 41 %.10. Sample Preparation10.1 Analysis samples are intended to originate by collection according to appropriate standard
49、 industry practice suitable forthe intended purpose. In the case of combustion boilers, it may be necessary to collect bottom ash, fly ash, and slag samples foranalysis. The type and location of sample collection therefore depends on the ultimate use of the data and the current industrypractice. In the special case of calculating combustor efficiency, the standard industry sampling practice is prescribed in ANSIASME PTC 38-1980 or EPA CRF 60 Appendix A, Method 17, or both.10.2 If moist or wet, the combustion residue sample will be predried at 107 C
