1、Designation:D317303 (Reapproved 2008) Designation: D3173 11Standard Test Method forMoisture in the Analysis Sample of Coal and Coke1This standard is issued under the fixed designation D3173; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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. Scope1.1 This test method covers the determination of moisture in the analysis sample of coal or coke. It i
3、s used for calculating otheranalytical results to a dry basis. When used in conjunction with the air drying loss as determined in accordance with Method D2013or Practice D346, each analytical result can be calculated to an as-received basis:1.2 This standard does not purport to address all of the sa
4、fety 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:2D346 Practice for Collection and
5、Preparation of Coke Samples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different BasesD3302 Test Method for Total Moisture in Coal3. Summary of Test Method3.1 Moisture is determined by estab
6、lishing the loss in weight of the sample when heated under rigidly controlled conditions oftemperature, time and atmosphere, sample weight, and equipment specifications.4. Significance and Use4.1 Moisture as determined by this test method is used for calculating other analytical results to a moistur
7、e free basis usingprocedures in Practice D3180. Moisture percent determined by this test method may be used in conjunction with the air-drymoisture loss determined in Method D2013 and Test Method D3302 to determine total moisture in coal. Total moisture is used forcalculating other analytical result
8、s to “as received” basis using Practice D3180. Moisture, ash, volatile matter, and fixed carbonpercents constitute the proximate analysis of coal and coke.5. Analysis Sample5.1 The analysis sample is that sample which has been pulverized to pass 250-m (No. 60) sieve as prepared in accordance withPra
9、ctice D346 or Method D2013.6. Apparatus6.1 Drying Oven, for coal samples:6.1.1 For determining the moisture of coal, the oven shall be so constructed as to have a uniform temperature in all parts, havea minimum of air space, and be capable of temperature regulation between the limits of 104 and 110C
10、. It may be of the formshown in Fig. 1. Provision shall be made for renewing the preheated air in the oven at the rate of two to four times a minute, withthe air dried as defined in 7.1.6.1.2 In the oven shown in Fig. 1, the door should contain a hole of approximately 3.2 mm (18 in.) in diameter nea
11、r the bottomto permit a free flow of air through the oven space.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 Feb. 1, 2008. Published February 2008. Originally
12、 approved in 1973. Last previous edition approved 2003 as D317303. DOI:10.1520/D3173-03R08.Current edition approved April 1, 2011. Published April 2011. Originally approved in 1973. Last previous edition approved 2008 as D3173 03(2008). DOI:10.1520/D3173-11.2An interlaboratory study, designed consis
13、tent with Practice E691, was conducted in 1995. Twelve labs participated. Supporting data have been filed atASTM InternationalHeadquarters and may be obtained by requesting Research Report RR:D05-1020.2For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service
14、 at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document 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
15、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 document.Copyright ASTM Interna
16、tional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Drying Oven, for coke samples. For determining the moisture of coke, an ordinary drying oven with openings for naturalair circulation and capable of temperature regulation between limits of 104 and 110C m
17、ay be used.6.3 Capsules, with covers.Aconvenient form, which allows the ash determination to be made on the same sample, is a porcelaincapsule, 22 mm (78 in.) in depth and 44 mm (134 in. ) in diameter, or a fused silica capsule of similar shape. These capsules shallbe used with a well-fitting flat a
18、luminum cover, illustrated in Fig. 2. Platinum crucibles or glass capsules with ground-glass capsmay also be used. They should be as shallow as possible, consistent with convenient handling.7. Reagents7.1 Dry AirAir used to purge the drying oven should be dried to a moisture content of 1.9 mg/L or l
19、ess. (Dew point 10Cor less.) Any desiccant or drying method capable of achieving this degree of dryness is suitable.7.2 DesiccantsMaterials suitable for use in the desiccator may be chosen from the following:7.2.1 Anhydrous Calcium Sulfate (0.004 mg/L).7.2.2 Silica Gel.7.2.3 Magnesium Perchlorate (0
20、.0005 mg/L).7.2.4 Sulfuric Acid, Concentrated (0.003 mg/L).7.2.5 The desiccant must be kept fresh enough to assure that the air in the desiccator is dry as defined in 7.1. Values inparentheses ( ) are literature values for the residual amount of moisture in air at equilibrium with these desiccants.
21、(Warning:Sulfuric acid is corrosive and can cause severe damage to eyes, skin, and clothing. Magnesium perchlorate is a strong oxidant andcan react violently with organic materials.)8. Procedure for Sample Passing a 250-m (No. 60) Sieve8.1 Heat the empty capsules under the conditions at which the sa
22、mple is to be dried, place the stopper or cover on the capsule,cool over a desiccant for 15 to 30 min, and weigh. Dip out with a spoon or spatula from the sample bottle approximately1gofthe sample. Put this quickly into the capsule, close, and weigh at once to the nearest 60.1 mg.NOTE 1Details in U.
23、S. Bureau of Mines Bulletin No. 492, 1951, p 6.FIG. 1 Moisture OvenFIG. 2 Capsule for Use in Determining MoistureD3173 1128.2 An alternative procedure for weighing the sample (more subject to error) is as follows: After transferring an amount of thesample slightly in excess of 1 g, bring to exactly1
24、ginweight (60.5 mg) by quickly removing the excess weight of the samplewith a spatula. The utmost dispatch must be used to minimize the exposure of the sample until the weight is determined.8.3 After removing the covers, quickly place the capsules in a preheated oven (at 104 to 110C) through which p
25、asses a currentof dry air. (The current of dry air is not necessary for coke.) Close the oven at once and heat for 1 h. Open the oven, cover thecapsules quickly, cool in a desiccator over desiccant, and weigh as soon as the capsules have reached room temperature.8.4 Use the percentage of moisture in
26、 the sample passing a 250-m (No. 60) sieve to calculate the results of the other analysesto a dry basis.9. Calculations9.1 Calculate the percent moisture in the analysis sample as follows:Moisture in analysis sample, % 5 A 2 B!/A 3 100 (1)where:A = grams of sample used andB = grams of sample after h
27、eating.10. Precision and Bias310.1 PrecisionThe precision of this method for the determination of moisture in the analysis sample of coal and coke is shownin Table 1 and TableA1.2. The precision characterized by repeatability (Sr, r) and reproducibility (SR, R) is described in TableA1.1in Annex A1.1
28、0.1.1 Repeatability Limit (r)The value below which the absolute difference between two test results calculated to separateconsecutive 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 qua
29、ntity of homogenous material, may be expected to occur with a probabilityof approximately 95%.10.1.2 Reproducibility Limit (R)The value below which the absolute difference between two test results, carried out indifferent laboratories, using samples taken at random from a single quantity of material
30、 that is as nearly homogenous as possible,may be expected to occur with a probability of approximately 95%.10.2 BiasCertified Reference Materials are not available for the determination of bias by this test method.NOTE 1One coke sample was analyzed in the interlaboratory study which generated the fi
31、rst row of information in Table 1. The average moistureof the coke sample was 0.36 %. The repeatability limit for this sample is 0.10. The reproducibility limit for this sample is 0.15. The repeatability standarddeviation for this sample is 0.036. The reproducibility standard deviation for this samp
32、le is 0.053.ANNEX(Mandatory Information)A1. PRECISION STATISTICSA1.1 The precision of this test method, characterized by repeatability (Sr, r) and reproducibility (SR, R) has been determinedfor the following materials as listed in Table A1.1.A1.2 Repeatability Standard Deviation (Sr)The standard3An
33、interlaboratory study, designed consistent with Practice E691, was conducted in 1995. Twelve labs participated. Supporting data have been filed atASTM InternationalHeadquarters and may be obtained by requesting Research Report RR:D05-1020. In addition, information for coke was calculated per Practic
34、e E 691 using 48 sets of datafor 24 coke samples from a commercially available inter-laboratory proficiency test program. The cokes used in this study included furnace coke, foundry coke and cokebreeze. Details and supporting information are given in Research Report RR:D05-1039 .TABLE 1 PrecisionRan
35、ge RepeatabilityLimit(r)ReproducibilityLimit(R)1.0 21.9 %0.09 + 0.01xA0.23 + 0.02xACoal 1.0 21.9 %0.09 + 0.01xA0.23 + 0.02xACoke 0.181.87% 0.08 0.24AWhere xis the average of two single test results.D3173 113deviation of test results obtained under repeatability conditions.A1.3 Reproducibility Standa
36、rd Deviation (SR)The standard deviation of test results obtained under reproducibility conditions.ASTM 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 expressly advised that determ
37、ination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or w
38、ithdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that
39、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 standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (s
40、ingle 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 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 webs
41、ite (www.astm.org/COPYRIGHT/).TABLE A1.1 Repeatability (Sr, r) and Reproducibility (SR, R)Parameters Used for Calculation of Precision Statement for CoalSamplesNOTEThe R-Squared statistic for both the repeatability (r) andreproducibility (R) indicates that the model as fitted explains 62% of thevari
42、ability in the two variables.Material Average SrSRrR91-2Ivb 0.9683 0.0479 0.0853 0.1341 0.238891-1 hvAb 1.5689 0.0569 0.1387 0.1593 0.388491-5 hvAb 3.1178 0.0559 0.0977 0.1564 0.273689-4 hvCb 5.4428 0.0601 0.1408 0.1682 0.394391-4 hvCb 9.6392 0.0636 0.1004 0.1781 0.281190-1 subB 11.9 0.1252 0.2193 0
43、.3505 0.61489-7 subA 12.4556 0.0798 0.1188 0.2234 0.332691-6 subA 15.1753 0.0577 0.1737 0.1615 0.486589-6 subC 21.9461 0.1949 0.2843 0.5456 0.796D3173 114TABLE A1.2 Repeatability (Sr, r) and Reproducibility (SR, R)Parameters Used for Calculation of Precision Statement for CokeSamplesMaterial Average
44、 SrSRr RCK980108 - Furnace 0.19 0.04 0.08 0.12 0.22CK980312 - Furnace 0.30 0.05 0.15 0.13 0.41CK980716 - Foundry 0.27 0.03 0.10 0.08 0.29CKReference2 - Furnace 0.18 0.03 0.11 0.09 0.30CKNIST01 - Foundry 0.57 0.04 0.09 0.13 0.24CKNIST02 - Furnace 0.30 0.03 0.06 0.09 0.18CK0303 - Foundry 0.75 0.03 0.0
45、6 0.09 0.16CK9903 - Foundry 0.50 0.04 0.10 0.10 0.29CK9904 - Furnace 0.65 0.03 0.10 0.08 0.27CK0001 - Furnace 0.44 0.03 0.07 0.09 0.21CK0401 - Furnace 0.58 0.03 0.10 0.07 0.30CK0002 - Breeze 0.46 0.02 0.15 0.04 0.42CK0302 - Breeze 0.55 0.04 0.05 0.10 0.13CK0003 - Foundry 0.31 0.02 0.08 0.07 0.24CK01
46、01 - Furnace 0.19 0.02 0.08 0.04 0.23CK0504 - Furnace 0.28 0.04 0.08 0.10 0.23CK0701 - Furnace 0.29 0.02 0.08 0.06 0.24CK0102 - Furnace 0.33 0.04 0.10 0.10 0.29CK0301 - Furnace 0.34 0.01 0.08 0.04 0.23CK0404 - Furnace 0.50 0.02 0.07 0.06 0.21CK0103 - Furnace 1.04 0.03 0.30 0.07 0.84CK0304 - Furnace
47、1.49 0.02 0.10 0.06 0.27CK0601 - Furnace 1.54 0.03 0.05 0.08 0.14CK0903 - Furnace 1.87 0.07 0.08 0.18 0.23CK0104 - Furnace 0.20 0.01 0.08 0.04 0.23CK0503 - Furnace 0.35 0.02 0.06 0.06 0.17CK0201 - Furnace 0.51 0.03 0.08 0.08 0.22CK0501 - Furnace 0.59 0.03 0.13 0.08 0.36CK0802 - Furnace 0.72 0.02 0.0
48、8 0.05 0.23CK0904 - Furnace 0.77 0.03 0.08 0.08 0.24CK0202 - Furnace 0.35 0.02 0.13 0.06 0.36CK0502 - Furnace 0.46 0.02 0.11 0.06 0.32CK0603 - Furnace 0.53 0.04 0.08 0.10 0.23CK0203 - Furnace 0.21 0.02 0.08 0.05 0.24CK0403 - Furnace 0.24 0.02 0.07 0.06 0.20CK0604 - Furnace 0.23 0.03 0.09 0.07 0.26CK
49、0801 - Furnace 0.18 0.02 0.05 0.06 0.14CK0204 - Breeze 0.60 0.04 0.19 0.10 0.54CK0402 - Breeze 0.72 0.04 0.10 0.12 0.27CK0602 - Breeze 0.72 0.03 0.14 0.07 0.40CK0704 - Breeze 0.81 0.02 0.08 0.05 0.22CK0702 - Furnace 0.64 0.06 0.24 0.18 0.67CK0902 - Furnace 0.91 0.04 0.18 0.11 0.50CK0703 - Coke 1.68 0.04 0.11 0.11 0.30CK0803 - Furnace 0.43 0.02 0.10 0.06 0.28CK0804 - Furnace 0.44 0.02 0.06 0.06 0.17CK0901 - Coke 0.27 0.03 0.06 0.09 0.18CK1001 - Furnace 0.29 0.03 0.11 0.09 0.30D3173 115
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