1、Designation:D317404 (Reapproved 2010) Designation: D3174 11Standard 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
2、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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test me
3、thod covers the determination of the inorganic residue as ash in the analysis sample of coal or coke as preparedin accordance with Practice D2013 or Practice D346. The results obtained can be applied as the ash in the proximate analysis,Practice D3172, and in the ultimate analysis, Practice D3176. F
4、or the determination of the constituents in ash, reference is madeto Test Methods D2795 and D3682. See Terminology D121 for definition of ash.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purpo
5、rt 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 and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D121 T
6、erminology of Coal and CokeD346 Practice for Collection and Preparation of Coke Samples for Laboratory AnalysisD388 Classification of Coals by RankD1756Test Method for Determination as Carbon Dioxide of Carbonate Carbon in CoalD1757 Test Method for Sulfate Sulfur in Ash from Coal and CokeD2013 Pract
7、ice for Preparing Coal Samples for AnalysisD2795 Test Methods for Analysis of Coal and Coke AshD3172 Practice for Proximate Analysis of Coal and CokeD3173 Test Method for Moisture in the Analysis Sample of Coal and CokeD3176 Practice for Ultimate Analysis of Coal and CokeD3180 Practice for Calculati
8、ng Coal and Coke Analyses from As-Determined to Different BasesD3682 Test Method for Major and Minor Elements in Combustion Residues from Coal Utilization ProcessesE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Summary of Test Method3.1 Ash is det
9、ermined by weighing the residue remaining after burning the coal or coke under rigidly controlled conditions ofsample weight, temperature, time, atmosphere, and equipment specifications.4. Significance and Use4.1 Ash, as determined by this test method, is the residue remaining after burning the coal
10、 and coke. Ash obtained differs incomposition from the inorganic constituents present in the original coal. Incineration causes an expulsion of all water, the loss ofcarbon dioxide from carbonates, the conversion of iron pyrites into ferric oxide, and other chemical reactions. Ash, as determinedby t
11、his test method, will differ in amount from ash produced in furnace operations and other firing systems because incinerationconditions influence the chemistry and amount of the ash. References for correcting ash results determined by this test method toa mineral-matter-free basis are listed in Class
12、ification D388, Section 8.1This 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 Dec.April 1, 2010.2011. Published JanuaryApril 2011. Originally approved in 1973. Last
13、previous edition approved in 20042010 asD3174 04(2010). DOI: 10.1520/D3174-04R10.10.1520/D3174-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Doc
14、ument Summary page on the ASTM website.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM
15、 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 document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Appar
16、atus5.1 Electric Muffle Furnace for Coal or CokeFor determination of ash of coal, the furnace shall have an adequate aircirculation and be capable of having its temperature regulated at 700 to 750C. The furnace shall be equipped with a temperatureindicator and means of controlling the temperature wi
17、thin prescribed limits. Means shall be provided for maintaining air flow ata rate of two to four changes per minute (see Fig. 1 and Fig. 2). Combustion gases shall be vented from laboratory. Inlet and outletports shall be located and arranged to distribute the air uniformly throughout the furnace ar
18、ea without the possibility of sweepingsolid particles from the capsules. The temperature over the entire working area of the furnace floor shall be maintained within thespecified temperature limits.5.2 Porcelain Capsules, about 22 mm (78 in.) in depth, and 44 mm (134 in.) in diameter, or similar sha
19、llow dishes or platinumcrucibles.5.3 Balance, sensitive to 0.1 mg.5.4 Crucible Cover, aluminum, porcelain, or similar covers.6. Temperature Calibration6.1 Place a preignited capsule with1gofsand at the center of the working area of the furnace, and by the use of a potentiometerand thermocouple or ot
20、her suitable temperature measuring device, measure the temperature of the sand in the crucible. The crucibleand sand should be at temperature equilibrium with the furnace. There should be two to four air changes per minute movingthroughout the furnace (the air flow may be measured by using a wet-tes
21、t meter or equivalent calibrated at standard conditions forair connected to the ceramic-pipe exhaust). Adjust the furnace temperature until the potentiometer reads 750 6 10C and thenadjust or read the temperature on the indicating pyrometer. Use this reading as the proper setting for controlling the
22、 furnace.7. Procedure7.1 The sample shall be the material pulverized to pass No. 60 (250-mm) sieve in accordance with Practice D2013 or PracticeD346.7.2 Transfer approximately 1 g (weighed to the nearest 0.1 mg) of the thoroughly mixed sample to a weighed capsule and coverquickly. An alternative way
23、 is to use the dried coal from the moisture determination in Test Method D3173. After removing the(Suggested method for inducing regulated air flow through ashing furnace.)FIG. 1 Air AspiratorD3174 112covers, place the capsule containing the sample in a cold furnace and heat gradually at such a rate
24、 that the temperature reaches450 to 500C in 1 h.7.3 Heat coal samples so that a final temperature of 700 to 750C is reached by the end of the second hour. Heat coke samplesso that a final temperature of 950C is reached by the end of the second hour. Continue to heat at the final temperature for addi
25、tional2 h (see Note 1). Remove the capsule from the muffle, place the cover on the capsule, cool under conditions to minimize moisturepickup, and weigh.NOTE 1While the 4-h incineration interval described is sufficient with most coals to reach a condition of complete burn off, certain cokes andnonrea
26、ctive coals may require additional time. If unburned carbon particles are observed, or if duplicate results are suspect, the samples should be returnedto the furnace for sufficient time to reach a constant weight (60.001 g). By this means, pyritic sulfur will be oxidized and expelled before the calc
27、ite isdecomposed. An ample supply of air in the muffle, “two to four changes per minute,” must be assured at all times to ensure complete oxidation of thepyritic sulfur and to remove the SO2formed. The 4-h time limit may be reduced if the sample reaches a constant weight at 700 to 750C in less than4
28、h.NOTE 2Some samples may be encountered that contain a high amount of carbonates (calcite) or pyrites or both. In such cases, sulfur retained assulfates may be both unduly high and nonuniform between duplicate samples. In such cases, sulfate sulfur in the ash can be determined in accordancewith Test
29、 Methods D1757 and the value properly corrected. If such is done, the ash value should be reported and designated both as determined andcorrected.8. Calculation8.1 Calculate the ash percent in the analysis sample as follows:Ash in analysis sample, % 5 A 2 B!/C# 3 100 (1)where:Calibration Flowmeter w
30、ith TubingAmbient AirFor calibration use only, 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.
31、2 Air AspiratorD3174 113A = 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 reporting analyses to other than as-determined basis, refer to Practice D3180.10. Precision and Bias10.1 Precision10.1.1 250 m
32、(No. 60) SamplesThe precision of this test method for the determination of ash in the analysis sample of coaland coke is shown in Table 1. The precision characterized by repeatability (Sr,r)and reproducibility (SR,R)is described in TableA1.1 and Table A1.2 in Annex A1.10.1.1.1 Repeatability Limit (r
33、)The value below which the absolute difference between two test results calculated to a drybasis (Practice D3180) of separate and consecutive test determinations, carried out on the same sample of 250 m (No. 60) coaland coke in the same laboratory, by the same operator, using the same apparatus on s
34、amples taken at random from a single quantityof homogeneous material, may be expected to occur with a probability of approximately 95 %.10.1.1.2 Reproducibility Limit (R)The value below which the absolute difference between two test results calculated to a drybasis (Practice D3180), carried out in d
35、ifferent laboratories, using samples of 250 m (No. 60) coal and coke taken at random froma single quantity of material that is as homogeneous as possible, may be expected to occur with a probability of approximately95 %.10.1.2 2.36 mm (No. 8) Samples3The precision of this test method for the determi
36、nation of ash in the analysis sample of coaland coke is shown in Table 2.10.1.2.1 Repeatability Limit (r)The value below which the absolute difference between two test results calculated to a drybasis (Practice D3180) of separate and consecutive test determinations, carried out on the same sample, u
37、sing the same riffle,determined on a single test specimen of two separate 2.36 mm (No. 8) test units of coal reduced entirely to 250 m (No. 60) andprepared from the same bulk sample coal in the same laboratory, by the same operator, using the same apparatus on samples takenat random from a single qu
38、antity of homogeneous material, may be expected to occur with a probability of approximately 95 %.10.1.2.2 Reproducibility Limit (R)The value below which the absolute difference between two test results calculated to a drybasis (Practice D3180), carried out in different laboratories, using samples o
39、f 2.36 mm (No. 8) coal reduced entirely to 250 m(No. 60), taken at random from a single quantity of material that is as homogeneous as possible, may be expected to occur witha probability of approximately 95 %.10.2 BiasSince this is an empirical test method, the degree of absolute bias cannot be det
40、ermined.11. Keywords11.1 ash; coal; coke3An interlaboratory study, designed consistent with Practice E691, was conducted in 1989. Eight laboratories participated in this study. Supporting data are available fromASTM Headquarters. Request Report RR:D05-1015., was conducted in 1989. Eight laboratories
41、 participated in this study. Supporting data are available from ASTMHeadquarters. Request Report RR:D05-1015. In addition, information for coke was calculated per Practice E691 using 48 sets of data for 24 coke samples for a commerciallyavailable interlaboratory proficiency test program. The cokes u
42、sed in this study included furnace coke, foundry coke and coke breeze. Details and supporting information aregiven in RR:D05-1039TABLE 1 Determination of Ash in the Analysis Sample of Coaland CokeRange RepeatabilityLimit,rReproducibilityLimit,R2.68 to 17.86 % 0.22 0.32Coal 2.68 to 17.86 % 0.22 0.32C
43、oke 5.73 to 11.75 % 0.10 0.20D3174 114ANNEX(Mandatory Information)A1. PRECISION STATISTICS 250 m (No. 60) SAMPLESA1.1 The precision of this test method, characterized by repeatability (Sr,r) and reproducibility (SR,R) has been determined forthe following materials as listed in Table A1.1 and Table A
44、1.2.A1.2 Repeatability Standard Deviation (Sr)The standard deviation of test results obtained under repeatability conditions.A1.3 Reproducibility Standard Deviation (SR)The standard deviation of test results obtained under reproducibility conditions.ASTM International takes no position respecting th
45、e validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard i
46、s subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International He
47、adquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This s
48、tandard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or
49、 serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 2 Range and Limits for Repeatability and Reproducabilityfor the Detrmination of Ash in Coal and CokeCoal Range RepeatabilityLimit,rReproducibilityLimit,RBituminous 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 Statement for CoalS
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