1、Designation: D3173 11D3173/D3173M 17Standard Test Method forMoisture in the Analysis Sample of Coal and Coke1This standard is issued under the fixed designation D3173;D3173/D3173M; the number immediately following the designation indicatesthe year of original adoption or, in the case of revision, th
2、e year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope Scope*1.1 This test method covers the determination of moisture in the analysis sample of coal or coke. It is u
3、sed 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 The values stated in either SI units or inch-pound units a
4、re to be regarded separately as standard. The values stated in eachsystem may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from thetwo systems may result in non-conformance with the standard.1.3 This standard does not purport to address
5、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 Terminology of
6、Coal and CokeD346 Practice for Collection and 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. Terminology
7、3.1 DefinitionsFor additional definitions of terms used in this test method, refer to Terminology D121.4. Summary of Test Method4.1 Moisture is determined by establishing the loss in weight of the sample when heated under rigidly controlled conditions oftemperature, time and atmosphere, sample weigh
8、t, and equipment specifications.5. Significance and Use5.1 Moisture as determined by this test method is used for calculating other analytical results to a moisture free basis usingprocedures in Practice D3180. Moisture percent determined by this test method may be used in conjunction with the air-d
9、rymoisture loss determined in Method D2013 and Test Method D3302 to determine total moisture in coal. Total moisture is used forcalculating other analytical results to “as received” basis using Practice D3180. Moisture, ash, volatile matter, and fixed carbonpercents constitute the proximate analysis
10、 of coal and coke.6. Analysis Sample6.1 The analysis sample is that sample which has been pulverized to pass 250-m (No. 60) sieve as prepared in accordance withPractice D346 or Method D2013.1 This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and is the direct responsi
11、bility of Subcommittee D05.21 on Methods of Analysis.Current edition approved April 1, 2011Feb. 1, 2017. Published April 2011February 2017. Originally approved in 1973. Last previous edition approved 20082011 asD3173 03D3173 11.(2008). DOI: 10.1520/D3173-11.10.1520/D3173_D3173M-17.2 For referencedAS
12、TM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user
13、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 recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as p
14、ublished by ASTM is to be considered the official document.*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 States17. Apparatus7.1 Drying Oven, for coal samples:7.1.1 For determ
15、ining 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. It may be of the formshown in Fig. 1. Provision shall be made for renewing the preheate
16、d air in the oven at the rate of two to four times a minute, withthe air dried as defined in 7.18.1.7.1.2 In the oven shown in Fig. 1, the door should contain a hole of approximately 3.2 mm (18 in.)in. in diameter near thebottom to permit a free flow of air through the oven space.7.2 Drying Oven, fo
17、r 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 may be used.7.3 Capsules, with covers.Aconvenient form, which allows the ash determination to be made on the sam
18、e sample, is a porcelaincapsule, 22 mm (78 in.)in. in depth and 44 mm (1134 in. ) in. in diameter, or a fused silica capsule of similar shape. Thesecapsules shall be used with a well-fitting flat aluminum cover, illustrated in Fig. 2. Platinum crucibles or glass capsules withground-glass caps may al
19、so be used. They should be as shallow as possible, consistent with convenient handling.8. Reagents8.1 Dry AirAir used to purge the drying oven should be dried to a moisture content of 1.9 mg/L or less. (Dew point 10Cor less.) Any desiccant or drying method capable of achieving this degree of dryness
20、 is suitable.8.2 DesiccantsMaterials suitable for use in the desiccator may be chosen from the following:8.2.1 Anhydrous Calcium Sulfate (0.004 mg/L).8.2.2 Silica Gel.8.2.3 Magnesium Perchlorate (0.0005 mg/L).8.2.4 Sulfuric Acid, Concentrated (0.003 mg/L).8.2.5 The desiccant must be kept fresh enoug
21、h to assure that the air in the desiccator is dry as defined in 7.18.1. Values inparentheses ( ) are literature values for the residual amount of moisture in air at equilibrium with these desiccants. (Warning:Sulfuric acid is corrosive and can cause severe damage to eyes, skin, and clothing. Magnesi
22、um perchlorate is a strong oxidant andcan react violently with organic materials.)9. Procedure for Sample Passing a 250-m (No. 60) Sieve9.1 Heat the empty capsules under the conditions at which the sample is to be dried, place the stopper or cover on the capsule,cool over a desiccant for 15 to 30 mi
23、n, and weigh. Dip out with a spoon or spatula from the sample bottle approximately 1 g ofthe sample. Put this quickly into the capsule, close, and weigh at once to the nearest 60.1 mg.NOTE 1Details in U.S. Bureau of Mines Bulletin No. 492, 1951, p 6.FIG. 1 Moisture OvenD3173/D3173M 1729.2 An alterna
24、tive 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 exactly 1 g in weight (60.5 mg) by quickly removing the excess weight of the samplewith a spatula. The utmost dispatch must be used to minimize
25、the exposure of the sample until the weight is determined.9.3 After removing the covers, quickly place the capsules in a preheated oven (at 104 to 110C) through which passes 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 ove
26、n, cover thecapsules quickly, cool in a desiccator over desiccant, and weigh as soon as the capsules have reached room temperature.9.4 Use the percentage of moisture in the sample passing a 250-m (No. 60) sieve to calculate the results of the other analysesto a dry basis.10. Calculations10.1 Calcula
27、te the percent moisture in the analysis sample as follows:Moisture in analysis sample,%5A 2B!/A# 3100 (1)where:A = grams of sample used andB = grams of sample after heating.11. Report11.1 Report the following information:11.1.1 Moisture in the analysis sample, %, to the nearest 0.01 percentage point
28、.12. Precision and Bias312.1 PrecisionThe precision of this method for the determination of moisture in the analysis sample of coal and coke is shownin Table 1 and Table A1.2. The precision characterized by repeatability (Sr,r) and reproducibility (SR,R) is described in Table A1.1in Annex A1.12.1.1
29、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 quantity
30、of homogenous material, may be expected to occur with a probabilityof approximately 95%.12.1.2 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 that
31、is as nearly homogenous as possible,may be expected to occur with a probability of approximately 95%.12.2 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 first ro
32、w of information in Table 1. The average moisture3 An 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 add
33、ition, information for coke was calculated per Practice 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 give
34、n in Research Report RR:D05-1039 .FIG. 2 Capsule for Use in Determining MoistureTABLE 1 PrecisionRange RepeatabilityLimit(r)ReproducibilityLimit(R)Coal 1.0 21.9 % 0.09 + 0.01xA 0.23 + 0.02xACoke 0.181.87% 0.08 0.24AWhere x is the average of two single test results.D3173/D3173M 173of the coke sample
35、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 sample is 0.053.ANNEX(Mandatory Information)A1. PRECISION STATISTICSA1.1 The p
36、recision of this test method, characterized by repeatability (Sr,r) and reproducibility (SR,R) has been determined for thefollowing materials as listed in Table A1.1 and Table A1.2.A1.2 Repeatability Standard Deviation (Sr)The standardTABLE A1.1 Repeatability (Sr,r) and Reproducibility (SR,R)Paramet
37、ers Used for Calculation of Precision Statement for CoalSamplesNOTE 1The R-Squared statistic for both the repeatability (r) andreproducibility (R) indicates that the model as fitted explains 62% of thevariability in the two variables.Material Average Sr SR r R91-2Ivb 0.9683 0.0479 0.0853 0.1341 0.23
38、8891-1 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 0.3505 0.61489-7 subA 12.4556 0.0798 0.1188 0.2234 0.332691-6 subA 15.1753 0.0577 0.1737 0.16
39、15 0.486589-6 subC 21.9461 0.1949 0.2843 0.5456 0.796D3173/D3173M 174deviation of test results obtained under repeatability conditions.A1.3 Reproducibility Standard Deviation (SR)The standard deviation of test results obtained under reproducibility conditions.TABLE A1.2 Repeatability (Sr,r) and Repr
40、oducibility (SR,R)Parameters Used for Calculation of Precision Statement for CokeSamplesMaterial Average Sr SR r 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 -
41、 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 0.06 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 0.4
42、6 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 0.24CK0101 - 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.
43、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 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
44、 - 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 0.08 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.
45、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 0.26CK0801 - 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
46、 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/D3173M 1
47、75SUMMARY OF CHANGESCommittee D05 has identified the location of selected changes to this standard since the last issue (D3173-11)that may impact the use of this standard.(1) Added sections 3 and 11.(2) Note 3 of subsection 12.2 was deleted.(3) Section A1.1 was revised.(4) Designation was corrected
48、to D3173/D3173M.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 determination of the validity of any such patent rights, and the riskof infringement of
49、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 withdrawn.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 your comments have not r
