1、Designation: D8010 16Standard 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 as sodium oxide (Na2O) andpotassium as potassium ox
3、ide (K2O) in the analysis of coalsamples prepared in accordance 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 Thi
4、s standard does not purport 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 Document
5、s2.1 ASTM Standards:3D121 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 CoalD3180 Practice for Calculating Coal and Co
6、ke Analysesfrom As-Determined to Different BasesD7448 Practice for Establishing the Competence of Labora-tories Using ASTM Procedures in the Sampling andAnalysis of Coal and CokeD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisE832 Specification for Labora
7、tory 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 agent. Theconcentrations of sodium and potassium are measur
8、ed 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 boilertube fouling and possible furnace corrosion problem
9、s.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 interferences.7. Apparatus7.1 Analytical balance, with sensitiv
10、ity 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 Bottles, 250 mL capacity with anO-ring seal and screw cap, cap
11、able 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 developed during the digestion.7.3 Filtering Apparatus7.3
12、.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.1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the dir
13、ect responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved Sept. 1, 2016. Published September 2016. Originallyapproved in 2015. Last previous edition approved in 2015 as D801015. DOI:10.1520/D8010-16.2“Coal Fouling and Slagging Parameters.” ASME H-86. Editor E.C.Winegar
14、tner, 1974.3For 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.Copyright ASTM International, 100 Barr Harbor Driv
15、e, PO Box C700, West Conshohocken, PA 19428-2959. United States17.4 SpectrometerBecause of the differences between vari-ous makes and models of satisfactory instruments, no detailedoperating instructions can be provided. Instead, follow theinstructions provided by the manufacturer of the particulari
16、nstrument. Sensitivity, 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
17、are valid.It is the responsibility 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
18、 of ReagentsUse reagent 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 reage
19、nt water asdefined in Specification D1193.8.3 Wetting AgentApproximately 1 to 5 mL of isopropylalcohol, methanol or ethanol may be added to the sample.8.4 Calibration StandardsStandard stock solutions of1000 mg L for each element are needed for preparation ofdilute calibration standards in the nomin
20、al range from 0.1 to100 mg/L. Prepare calibration standard solutions from 99.99 %(mass/mass) purity metals or salts. Alternatively, use commer-cially available standard stock solutions specifically preparedfor the correct spectroscopy method. Dilute calibration stan-dard solutions are also used init
21、ially and periodically to verifythe baseline of the calibration has not changed significantly.8.5 Blank SolutionsTwo types of blank solutions arerequired: a calibration blank of water that is used to establishthe analytical calibration curve and a method blank which isused to evaluate possible conta
22、mination and assess spectralbackground. The calibration blank is also used initially andperiodically to verify the baseline of the calibration has notchanged significantly.8.5.1 Calibration Blankwater.8.5.2 Method BlankProcess the method blank through thesame digestion procedure as the samples, usin
23、g the samevolumes of water and wetting agent as used in preparing thesamples.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
24、, D3302,orD7582 to permitcalculations to other than as-determined bases.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 elemen
25、ts of varying percentsoutside the range of the typical sample. Analysts 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
26、Method A, Hot PlateAccurately weigh5gofsample to the nearest 0.1 mg into a 250 mL Erlenmeyer flask.The sample may be wetted with 1 to 5 mL of wetting agent.Add 100 mL of water to the flask. Place the flask with sampleonto the hot plate and cover. Allow to digest just under boilingfor at least 16 h.
27、Do not allow the sample to go to dryness (arefluxing column may be used to prevent this).Allow to cool toroom temperature. Filter by either gravity filtration or vacuumfiltration into a 250 mL volumetric flask. Once filtration iscomplete, dilute the filtrate to volume (250 mL) with water andmix by i
28、nversion.10.2.2 Method B, Hot BlockAccurately weigh1gofsample to the nearest 0.1 mg into a weighing dish andquantitatively transfer to a polycarbonate bottle. The samplemay be wetted with 1 to 5 mL of wetting agent. Add 25 mL ofwater to the tube. Place the sample on the hot block and digestat 120 6
29、5 C for 16 h. Do not allow the sample to go todryness. Allow to cool to room temperature. Filter by eithergravity filtration or vacuum filtration into a 50 mL centrifugetube. Once filtration is complete, dilute the filtrate to volume(50 mL) with water and mix by inversion.10.3 Determination of Sodiu
30、m and Potassium in the TestSolutionMeasure the concentrations of sodium and potas-sium in the test solution (filtrate 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 metho
31、d assumes that good operatingprocedures are followed. Design differences among instru-ments and different selected analytical wavelengths for indi-vidual spectrometers make it impractical to list detailed con-ditions.11.2 Calibration ProcedureCalibrate the instrument ac-cording to the procedure reco
32、mmended by the manufacturerusing a calibration blank and calibration standards.11.3 Initial Calibration VerificationBefore analyzing testsamples, analyze the method blank and verify the propercalibration of the instrument by analyzing a reference material.Results for the reference material must be w
33、ithin the stateduncertainty limits or the calibration procedure must be re-peated.4Reagent Chemicals, 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 La
34、boratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D8010 16211.4 Periodic Calibration Verification andRecalibrationIn accordance with Guide D7448, analyze acontrol sample on a periodic b
35、asis. Results obtained for thecontrol sample must be within 10 % of the stated value or allresults obtained since the last successful control check for thatelement must be rejected and the calibration procedure re-peated.12. Report12.1 For reporting analyses to other than as-determinedbasis, refer t
36、o Practice D3180.12.2 For instruments that do not have calculation functionsprovided by the manufacturer for converting the concentrationamount of the analyte as analyzed to the appropriate oxide, thefollowing calculations can be used:12.2.1%Na2O as Det!=A 2 B!VCD31.348 31 gNa!1000 mg Na!3100 % (1)w
37、here: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, andD = sample mass, g (as determined basis).Note:MW Na2O!2AW Na!51.348where:MW = molecular weight, andAW = atomic weight.12.2.2%K2O as Det! 5A 2 B!VCD
38、31.205 31 gK!1000 mg K!3100 %(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, if applied, andD = sample mass, g (as determined).Note:MW K2O!2AW K!51.205where:MW = molecular weight, andAW = atomic weight.13. K
39、eywords13.1 alkali; potassium oxide; sodium oxide; water solubleASTM 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 suc
40、h 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 withdrawn. Your comments are invite
41、d 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 received a
42、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 (single or multiple copies) of this
43、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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 163
