1、Designation: D8010 15Standard Practice forDetermination of Water Soluble Alkali Content in Coal1This standard is issued under the fixed designation D8010; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、 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 practice describes a procedure for the determina-tion of water soluble sodium oxide (Na2O) and potassiumoxide (K2O) in the analys
3、is of coal samples prepared inaccordance with Practice D2013.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This practice is derived in part from the ASME proce-dure water soluble alkalis.21.4 This standard does not pur
4、port to address all of thesafety 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:3D1
5、21 Terminology of Coal and CokeD1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3302 Test Method for Total Moisture in CoalD7582 Test Methods for Proximate Analysis of Coal andCoke by Macr
6、o Thermogravimetric AnalysisE832 Specification for Laboratory Filter Papers3. Terminology3.1 For definitions of terms used in this practice, refer toTerminology D121.4. Summary of Practice4.1 Sodium and potassium salts are leached from the sampleduring a lengthy digestion with water and a wetting ag
7、ent. Theconcentrations of sodium and potassium are measured in thefiltered liquid by an appropriate spectrometric technique for theelements sodium and potassium.5. Significance and Use5.1 Results obtained from the practice are used to serve anumber of interests, including the indication of possible
8、boilertube fouling and possible furnace corrosion problems.6. Interferences6.1 Several types of interference effects may contribute toinaccuracies in the determination of sodium and potassium.Follow the manufacturers operating guide to develop andapply correction factors to compensate for the interf
9、erences.7. Apparatus7.1 Analytical balance, with sensitivity of 0.1 mg.7.2 Digestion Apparatus7.2.1 Stirring Hotplate and Bars, with operating tempera-ture up to 200 C.7.2.1.1 Erlenmeyer flask with cover, 250 mL.7.2.1.2 Refluxing column (optional).7.2.2 Hot Block Digestion7.2.2.1 Polycarbonate Bottl
10、es, 250 mL capacity with anO-ring seal and screw cap, capable of withstanding tempera-tures up to 130 C, the pressure that is developed during thedigestion, and resistant to oxidation. Other types of bottles orvials may be used provided they are capable of withstandingthe temperatures and pressures
11、developed during the digestion.7.3 Filtering Apparatus7.3.1 Filter Paper or 0.45 micron filter. The paper used mustbe ash-free, quantitative Type II filter paper, as described inSpecification E832.7.3.2 Filter (gravity or vacuum).7.3.3 Volumetric flask, 250 mL.7.4 SpectrometerBecause of the differen
12、ces between vari-ous makes and models of satisfactory instruments, no detailedoperating instructions can be provided. Instead, follow theinstructions provided by the manufacturer of the particular1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct resp
13、onsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved Nov. 1, 2015. Published December 2015. DOI:10.1520/D8010-15.2“Coal Fouling and Slagging Parameters.” ASME H-86. Editor E.C.Winegartner, 1974.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontac
14、t ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1instrument. Sensitivity,
15、instrumental detection limit, precision,linear dynamic range, and interference effects must be inves-tigated and established for each individual analyte line on thatparticular instrument. All measurements must be within theinstruments linear range in which correction factors are valid.It is the resp
16、onsibility of the analyst to verify that theinstrument configuration and operating conditions used satisfythe analytical requirements of this method and to maintainquality control data confirming instrument performance andanalytical results.8. Reagents and Materials8.1 Purity of ReagentsUse reagent
17、grade chemicals in alltests that conform to the specifications of the Committee onAnalytical Reagents of theAmerican Chemical Society,4wheresuch specifications are available.8.2 Purity of WaterUnless otherwise indicated, referencesto water are understood to mean Type II reagent water asdefined in Sp
18、ecification D1193.8.3 Wetting AgentApproximately 1 to 5 mL of isopropylalcohol, methanol or ethanol may be added to the sample.8.4 Standard Stock SolutionsStock solutions of1000 mg L for each element are needed for preparation ofdilute standards in the range from 0.1 to 100 mg/L. Preparestandard sto
19、ck solutions from 99.999 % (mass/mass) puritymetals or salts. Alternatively, use commercially available stocksolutions specifically prepared for the correct spectroscopymethod. Dilute standard solutions are also used initially andperiodically to verify the baseline of the calibration has notchanged
20、significantly.8.5 Blank SolutionsTwo types of blank solutions arerequired: a calibration blank of DI water that is used toestablish the analytical calibration curve and a method blankwhich is used to evaluate possible contamination and assessspectral background. The calibration blank is also used in
21、itiallyand periodically to verify the baseline of the calibration has notchanged significantly.8.5.1 Calibration BlankDI water.8.5.2 Method BlankProcess the method blank through thesame digestion procedure as the samples, using the samevolumes of DI water and wetting agent as used in preparing thesa
22、mples.9. Analysis Sample9.1 Prepare the analysis sample in accordance with PracticeD2013 for coal by pulverizing the material to pass a 250 m(No. 60) U.S.A. standard sieve. Determine moisture in accor-dance with Test Method D3173, D3302,orD7582 to permitcalculations to other than as-determined bases
23、.10. Procedure10.1 The solutions and proportions described below are thetypical samples as represented by American coals. Therefore,stronger or weaker dilutions may be required to establishsuitable concentrations for those elements of varying percentsoutside the range of the typical sample. Analysts
24、 must deter-mine the sensitivity and linear range of calibration of their ownequipment and choose concentration ranges for standardscompatible with the samples and instrument specific to theirown work.10.2 Sample Digestion10.2.1 Method A, Hot PlateAccurately weigh5gofsample to the nearest 0.1 mg int
25、o a 250 mL Erlenmeyer flask.The sample may be wetted with 1 to 5 mL of wetting agent.Add 100 mL of DI water to the flask. Place the flask withsample onto the hot plate and cover. Allow to digest just underboiling for at least 16 h. Do not allow the sample to go todryness (a refluxing column may be u
26、sed to prevent this).Allow to cool to room temperature. Filter by either gravityfiltration or vacuum filtration into a 250 mL volumetric flask.Once filtration is complete, dilute the filtrate to volume (250mL) with DI water and mix by inversion.10.2.2 Method B, Hot BlockAccurately weigh1gofsample to
27、 the nearest 0.1 mg into a weighing dish andquantitatively transfer to a polycarbonate bottle. Add 25 mL ofDI water to the tube. Place the sample on the hot block anddigest at 120 6 5 C for 16 h. Do not allow the sample to goto dryness. Allow to cool to room temperature. Filter by eithergravity filt
28、ration or vacuum filtration into a 50 mL centrifugetube. Once filtration is complete, dilute the filtrate to volume(50 mL) with DI water and mix by inversion.10.3 Determination of Sodium and Potassium in the TestSolutionMeasure the concentrations of sodium and potas-sium in the test solution (filtra
29、te from 10.2.1 or 10.2.2)according to the selected spectrometric method.11. Instrument Operation11.1 Consult the manufacturers instructions for the chosenspectrometer. The present method assumes that good operatingprocedures are followed. Design differences among instru-ments and different selected
30、analytical wavelengths for indi-vidual spectrometers make it impractical to list detailed con-ditions.11.2 To ensure the validity of the data obtained from aspectrometer analysis, implement appropriate QC elements foreach analyte wavelength.12. Report12.1 For instruments that do not have calculation
31、 functionsprovided by the manufacturer for converting the concentrationamount of the analyte as analyzed to the appropriate oxide, thefollowing calculations can be used:12.1.1%Na2O, dry basis =A 2 B!VCD3MW Na2O!2 MW Na!3mass of solute, g!mass of solution, g!3 100 % 3S100100 2 MadD(1)4Reagent Chemica
32、ls, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National F
33、ormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D8010 152where:A = as measured concentration of Na, mg/L,B = as measured concentration of blank, mg/L,V = volume of solution, LC = dilution factor, if applied,D = sample mass, g, andMad= residual moisture, %.Note:MW Na2O!2MW Na!51.34
34、8mass of solute, g!mass of solution , g!3100 % 50.112.1.2%K2O, dry basis 5A 2 B!VCD3MW K2O!2MW K!3mass of solute , g!mass of solution , g!3100 %3S100100 2 MadD(2)where:A = as measured concentration of K, mg/L,B = as measured concentration of blank, mg/L,V = volume of solution, LC = dilution factor,
35、if applied,D = sample mass, g, andMad= residual moisture, %.Note:MW K2O!2MW K!51.205mass of solute, g!mass of solution , g!3100 % 50.113. Keywords13.1 alkali; potassium oxide; sodium oxide; water solubleASTM International takes no position respecting the validity of any patent rights asserted in con
36、nection 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 is subject to revision at any time by the respon
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