1、Designation: D3174 04 (Reapproved 2010)Standard Test Method forAsh in the Analysis Sample of Coal and Coke from Coal1This standard is issued under the fixed designation D3174; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers the dete
3、rmination of the inor-ganic residue as ash in the analysis sample of coal or coke asprepared in accordance with Practice D2013 or Practice D346.The results obtained can be applied as the ash in the proximateanalysis, Practice D3172, and in the ultimate analysis, PracticeD3176. For the determination
4、of the constituents in ash,reference is made to Test Methods D2795 and D3682. SeeTerminology D121 for definition of ash.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of the
5、safety 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 Terminology of Coal and
6、 CokeD346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD388 Classification of Coals by RankD1756 Test Method for Determination as Carbon Dioxideof Carbonate Carbon in CoalD1757 Test Method for Sulfate Sulfur inAsh from Coal andCoke3D2013 Practice for Preparing Coal S
7、amples for AnalysisD2795 Test Methods for Analysis of Coal and Coke Ash3D3172 Practice for Proximate Analysis of Coal and CokeD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3176 Practice for Ultimate Analysis of Coal and CokeD3180 Practice for Calculating Coal and Coke Analyse
8、sfrom As-Determined to Different BasesD3682 Test Method for Major and Minor Elements inCombustion Residues from Coal Utilization ProcessesE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 Ash is determined by weighing the res
9、idue remainingafter burning the coal or coke under rigidly controlled condi-tions of sample weight, temperature, time, atmosphere, andequipment specifications.4. Significance and Use4.1 Ash, as determined by this test method, is the residueremaining after burning the coal and coke. Ash obtained diff
10、ersin composition from the inorganic constituents present in theoriginal coal. Incineration causes an expulsion of all water, theloss of carbon dioxide from carbonates, the conversion of ironpyrites into ferric oxide, and other chemical reactions. Ash, asdetermined by this test method, will differ i
11、n amount from ashproduced in furnace operations and other firing systems be-cause incineration conditions influence the chemistry andamount of the ash. References for correcting ash resultsdetermined by this test method to a mineral-matter-free basisare listed in Classification D388, Section 8.5. Ap
12、paratus5.1 Electric Muffle Furnace for Coal or CokeFor deter-mination of ash of coal, the furnace shall have an adequate aircirculation and be capable of having its temperature regulatedat 700 to 750C. The furnace shall be equipped with atemperature indicator and means of controlling the temperature
13、within prescribed limits. Means shall be provided for main-taining air flow at a rate of two to four changes per minute (seeFig. 1 and Fig. 2). Combustion gases shall be vented fromlaboratory. Inlet and outlet ports shall be located and arrangedto distribute the air uniformly throughout the furnace
14、area1This 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 Dec. 1, 2010. Published January 2011. Originallyapproved in 1973. Last previous edition approved in 2004 as D31
15、74 04. DOI:10.1520/D3174-04R10.2For 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 Document Summary page onthe ASTM website.3Withdrawn. The last approved
16、version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.without the possibility of sweeping solid particles from thecapsules. The temperature over the entire working area of th
17、efurnace floor shall be maintained within the specified tempera-ture limits.5.2 Porcelain Capsules, about 22 mm (78 in.) in depth, and44 mm (134 in.) in diameter, or similar shallow dishes orplatinum crucibles.5.3 Balance, sensitive to 0.1 mg.5.4 Crucible Cover, aluminum, porcelain, or similar cover
18、s.6. Temperature Calibration6.1 Place a preignited capsule with1gofsand at the centerof the working area of the furnace, and by the use of apotentiometer and thermocouple or other suitable temperaturemeasuring device, measure the temperature of the sand in thecrucible. The crucible and sand should b
19、e at temperatureequilibrium with the furnace. There should be two to four airchanges per minute moving throughout the furnace (the airflow may be measured by using a wet-test meter or equivalentcalibrated at standard conditions for air connected to theceramic-pipe exhaust).Adjust the furnace tempera
20、ture until thepotentiometer reads 750 6 10C and then adjust or read thetemperature on the indicating pyrometer. Use this reading asthe proper setting for controlling the furnace.7. Procedure7.1 The sample shall be the material pulverized to pass No.60 (250-mm) sieve in accordance with Practice D2013
21、 orPractice D346.7.2 Transfer approximately 1 g (weighed to the nearest 0.1mg) of the thoroughly mixed sample to a weighed capsule andcover quickly. An alternative way is to use the dried coal fromthe moisture determination in Test Method D3173. Afterremoving the covers, place the capsule containing
22、 the samplein a cold furnace and heat gradually at such a rate that thetemperature reaches 450 to 500C in 1 h.7.3 Heat coal samples so that a final temperature of 700 to750C is reached by the end of the second hour. Heat cokesamples so that a final temperature of 950C is reached by theend of the sec
23、ond hour. Continue to heat at the final tempera-ture for additional 2 h (see Note 1). Remove the capsule fromthe muffle, place the cover on the capsule, cool under condi-tions to minimize moisture pickup, and weigh.NOTE 1While the 4-h incineration interval described is sufficient withmost coals to r
24、each a condition of complete burn off, certain cokes andnonreactive coals may require additional time. If unburned carbonparticles are observed, or if duplicate results are suspect, the samplesshould be returned to the furnace for sufficient time to reach a constantweight (60.001 g). By this means,
25、pyritic sulfur will be oxidized and(Suggested method for inducing regulated air flow through ashing furnace.)FIG. 1 Air AspiratorD3174 04 (2010)2expelled before the calcite is decomposed. An ample supply of air in themuffle, “two to four changes per minute,” must be assured at all times toensure com
26、plete oxidation of the pyritic sulfur and to remove the SO2formed. The 4-h time limit may be reduced if the sample reaches aconstant weight at 700 to 750C in less than 4 h.NOTE 2Some samples may be encountered that contain a highamount of carbonates (calcite) or pyrites or both. In such cases, sulfu
27、rretained as sulfates may be both unduly high and nonuniform betweenduplicate samples. In such cases, sulfate sulfur in the ash can bedetermined in accordance with Test Methods D1757 and the valueproperly corrected. If such is done, the ash value should be reported anddesignated both as determined a
28、nd corrected.8. Calculation8.1 Calculate the ash percent in the analysis sample asfollows:Ash in analysis sample, % 5 A 2 B!/C# 3 100 (1)where:A = weight of capsule, cover, and ash residue, g,B = weight of empty capsule and cover, g, andC = weight of analysis sample used, g.9. Report9.1 For reportin
29、g analyses to other than as-determined basis,refer to Practice D3180.10. Precision and Bias10.1 Precision10.1.1 250 m (No. 60) SamplesThe precision of this testmethod for the determination of ash in the analysis sample ofcoal and coke is shown in Table 1. The precision characterizedby repeatability
30、(Sr,r)and reproducibility (SR,R)is describedin Table A1.1 in Annex A1.10.1.1.1 Repeatability Limit (r)The value below whichthe absolute difference between two test results calculated to adry basis (Practice D3180) of separate and consecutive testdeterminations, carried out on the same sample of 250
31、m (No.60) coal and coke in the same laboratory, by the same operator,using the same apparatus on samples taken at random from asingle quantity of homogeneous material, may be expected tooccur with a probability of approximately 95 %.Calibration Flowmeter with TubingAmbient AirFor calibration use onl
32、y, adjust forced air valve to deliver two to four furnace volume changes per minute (at standardtemperature-pressure conditions.)NOTE 1Flowmeters are usually calibrated for one atmosphere at 70F (760-mm Hg at 21.1C).(Suggested layout for calibration.)FIG. 2 Air AspiratorD3174 04 (2010)310.1.1.2 Repr
33、oducibility Limit (R)The value below whichthe absolute difference between two test results calculated to adry basis (Practice D3180), carried out in different laboratories,using samples of 250 m (No. 60) coal and coke taken atrandom from a single quantity of material that is as homoge-neous as possi
34、ble, may be expected to occur with a probabilityof approximately 95 %.10.1.2 2.36 mm (No. 8) Samples4The precision of this testmethod for the determination of ash in the analysis sample ofcoal and coke is shown in Table 2.10.1.2.1 Repeatability Limit (r)The value below whichthe absolute difference b
35、etween two test results calculated to adry basis (Practice D3180) of separate and consecutive testdeterminations, carried out on the same sample, using the sameriffle, determined on a single test specimen of two separate 2.36mm (No. 8) test units of coal reduced entirely to 250 m (No.60) and prepare
36、d from the same bulk sample coal in the samelaboratory, by the same operator, using the same apparatus onsamples taken at random from a single quantity of homoge-neous material, may be expected to occur with a probability ofapproximately 95 %.10.1.2.2 Reproducibility Limit (R)The value below whichth
37、e absolute difference between two test results calculated to adry basis (Practice D3180), carried out in different laboratories,using samples of 2.36 mm (No. 8) coal reduced entirely to 250m (No. 60), taken at random from a single quantity of materialthat is as homogeneous as possible, may be expect
38、ed to occurwith a probability of approximately 95 %.10.2 BiasSince this is an empirical test method, thedegree of absolute bias cannot be determined.11. Keywords11.1 ash; coal; cokeANNEX(Mandatory Information)A1. PRECISION STATISTICS 250 m (No. 60) SAMPLESA1.1 The precision of this test method, char
39、acterized byrepeatability (Sr,r) and reproducibility (SR,R) has been deter-mined for the following materials as listed in Table A1.1.A1.2 Repeatability Standard Deviation (Sr)The standarddeviation of test results obtained under repeatability condi-tions.A1.3 Reproducibility Standard Deviation (SR)Th
40、e stan-dard deviation of test results obtained under reproducibilityconditions.4An interlaboratory study, designed consistent with Practice E691, was con-ducted in 1989. Eight laboratories participated in this study. Supporting data areavailable from ASTM Headquarters. Request Report RR:D05-1015.TAB
41、LE 1 Determination of Ash in the Analysis Sample of Coaland CokeRange RepeatabilityLimit,rReproducibilityLimit,R2.68 to 17.86 % 0.22 0.32TABLE 2 Range and Limits for Repeatability and Reproducabilityfor the Detrmination of Ash in Coal and CokeCoal Range RepeatabilityLimit,rReproducibilityLimit,RBitu
42、minous 5.0 to 15.0 % 0.30 % 0.49 %Subbituminous-Lignite 4.5 to 30.0 % 0.33 % 0.47 %TABLE A1.1 Repeatability (Sr,r) and Reproducibility (SR,R)Parameters Used for Calculation of Precision StatementMaterial Average SrSRrR912 lvb 6.86364 0.049024 0.072788 0.13717 0.20366911 hvAb 2.68068 0.047123 0.05563
43、3 0.13185 0.15566915 hvAb 10.0873 0.065132 0.080675 0.18224 0.22573894 hvCb 10.475 0.075743 0.121383 0.21193 0.33963914 hvCb 12.515 0.071347 0.082831 0.19963 0.23176901 subB 16.7593 0.07752 0.1306 0.2169 0.36542897 subA 8.81705 0.06302 0.10659 0.17633 0.29824916 subA 11.0723 0.061279 0.083981 0.1714
44、6 0.23498896 subC 13.5182 0.127066 0.194514 0.35553 0.54425Lignite 17.865 0.103367 0.163095 0.28922 0.45634D3174 04 (2010)4ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expr
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