1、Designation: D8010 16D8010 18Standard Practice Test Method 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
2、 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 practice describes a procedure for the determination of water soluble sodium as sodium oxide (Na2O) and potas
3、siumas potassium oxide (K2O) in the analysis of coal samples prepared in accordance with Practice D2013.1.2 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 practice is derived in part from the ASME procedure water sol
4、uble alkalis.21.4 This standard does not purport 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.
5、Referenced Documents2.1 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 of Coal and CokeD3302 Test Method for Total Moisture in CoalD3180 Practice for Cal
6、culating Coal and Coke Analyses from As-Determined to Different BasesD7448 Practice for Establishing the Competence of Laboratories UsingASTM Procedures in the Sampling andAnalysis of Coaland CokeD7582 Test Methods for Proximate Analysis of Coal and Coke by Macro Thermogravimetric AnalysisE832 Speci
7、fication for Laboratory Filter Papers3. Terminology3.1 For definitions of terms used in this practice, refer to Terminology D121.4. Summary of Practice4.1 Sodium and potassium salts are leached from the sample during a lengthy digestion with water and a wetting agent. Theconcentrations of sodium and
8、 potassium are measured in the filtered 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 a number of interests, including the indication of possible boiler tubefouling and possible fu
9、rnace corrosion problems.6. Interferences6.1 Several types of interference effects may contribute to inaccuracies in the determination of sodium and potassium. Followthe manufacturers operating guide to develop and apply correction factors to compensate for the interferences.1 This test method is un
10、der 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 Sept. 1, 2016Sept. 1, 2018. Published September 2016October 2018. Originally approved in 2015. Last previous edition approved in 2015201
11、6as D8010D8010 16.15. DOI: 10.1520/D8010-16.10.1520/D8010-18.2 “Coal Fouling and Slagging Parameters.” ASME H-86. Editor E.C. Winegartner, 1974.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvo
12、lume 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 of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to ade
13、quately 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshoho
14、cken, PA 19428-2959. United States17. Apparatus7.1 Analytical balance, with sensitivity of 0.1 mg.7.2 Digestion Apparatus7.2.1 Stirring Hotplate and Bars, with operating temperature 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
15、.2.2.1 Polycarbonate Bottles, 250 mL capacity with an O-ring seal and screw cap, capable of withstanding temperatures up to130 C, the pressure that is developed during the digestion, and resistant to oxidation. Other types of bottles or vials may be usedprovided they are capable of withstanding the
16、temperatures and pressures developed during the digestion.7.3 Filtering Apparatus7.3.1 Filter Paper or 0.45 micron filter. The paper used must be 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 Spectro
17、meterBecause of the differences between various makes and models of satisfactory instruments, no detailedoperating instructions can be provided. Instead, follow the instructions provided by the manufacturer of the particular instrument.Sensitivity, instrumental detection limit, precision, linear dyn
18、amic range, and interference effects must be investigated andestablished for each individual analyte line on that particular instrument. All measurements must be within the instruments linearrange in which correction factors are valid. It is the responsibility of the analyst to verify that the instr
19、ument configuration andoperating conditions used satisfy the analytical requirements of this method and to maintain quality control data confirminginstrument performance and analytical results.8. Reagents and Materials8.1 Purity of ReagentsUse reagent grade chemicals in all tests that conform to the
20、 specifications of the Committee onAnalytical Reagents of the American Chemical Society,4 where such specifications are available.8.2 Purity of WaterUnless otherwise indicated, references to water are understood to mean Type II reagent water as definedin Specification D1193.8.3 Wetting AgentApproxim
21、ately 1 to 5 mL of isopropyl alcohol, methanol or ethanol may be added to the sample.8.4 Calibration StandardsStandard stock solutions of 1000 mgL for each element are needed for preparation of dilutecalibration standards in the nominal range from 0.1 to 100 mg/L. Prepare calibration standard soluti
22、ons from 99.99 %(mass/mass) purity metals or salts. Alternatively, use commercially available standard stock solutions specifically prepared for thecorrect spectroscopy method. Dilute calibration standard solutions are also used initially and periodically to verify the baseline ofthe calibration has
23、 not changed significantly.8.5 Blank SolutionsTwo types of blank solutions are required: a calibration blank of water that is used to establish theanalytical calibration curve and a method blank which is used to evaluate possible contamination and assess spectral background.The calibration blank is
24、also used initially and periodically to verify the baseline of the calibration has not changed significantly.8.5.1 Calibration Blankwater.8.5.2 Method BlankProcess the method blank through the same digestion procedure as the samples, using the same volumesof water and wetting agent as used in prepar
25、ing the samples.9. Analysis Sample9.1 Prepare the analysis sample in accordance with Practice D2013 for coal by pulverizing the material to pass a 250 m (No.60) U.S.A. standard sieve. Determine moisture in accordance with Test Method D3173, D3302, or D7582 to permit calculationsto other than as-dete
26、rmined bases.10. Procedure10.1 The solutions and proportions described below are the typical samples as represented by American coals. Therefore,stronger or weaker dilutions may be required to establish suitable concentrations for those elements of varying percents outsidethe range of the typical sa
27、mple.Analysts must determine the sensitivity and linear range of calibration of their own equipment andchoose concentration ranges for standards compatible with the samples and instrument specific to their own work.5 Reagent Chemicals, American Chemical Society Specifications, American Chemical Soci
28、ety, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, M
29、D.D8010 18210.2 Sample Digestion10.2.1 Method A, Hot PlateAccurately weigh 5 g of sample to the nearest 0.1 mg into a 250 mLErlenmeyer flask. The samplemay be wetted with 1 to 5 mL of wetting agent. Add 100 mL of water to the flask. Place the flask with sample onto the hot plateand cover. Allow to d
30、igest just under boiling for at least 16 h. Do not allow the sample to go to dryness (a refluxing column maybe used to prevent this). Allow to cool to room temperature. Filter by either gravity filtration or vacuum filtration into a 250 mLvolumetric flask. Once filtration is complete, dilute the fil
31、trate to volume (250 mL) with water and mix by inversion.10.2.2 Method B, Hot BlockAccurately weigh 1 g of sample to the nearest 0.1 mg into a weighing dish and quantitativelytransfer to a polycarbonate bottle. The sample may be wetted with 1 to 5 mL of wetting agent. Add 25 mL of water to the tube.
32、Place the sample on the hot block and digest at 120 6 5 C for 16 h. Do not allow the sample to go to dryness. Allow to coolto room temperature. Filter by either gravity filtration or vacuum filtration into a 50 mLcentrifuge tube. Once filtration is complete,dilute the filtrate to volume (50 mL) with
33、 water and mix by inversion.10.3 Determination of Sodium and Potassium in the Test SolutionMeasure the concentrations of sodium and potassium in thetest solution (filtrate from 10.2.1 or 10.2.2) according to the selected spectrometric method.11. Instrument Operation11.1 Consult the manufacturers ins
34、tructions for the chosen spectrometer. The present method assumes that good operatingprocedures are followed. Design differences among instruments and different selected analytical wavelengths for individualspectrometers make it impractical to list detailed conditions.11.2 Calibration ProcedureCalib
35、rate the instrument according to the procedure recommended by the manufacturer using acalibration blank and calibration standards.11.3 Initial Calibration VerificationBefore analyzing test samples, analyze the method blank and verify the proper calibrationof the instrument by analyzing a reference m
36、aterial. Results for the reference material must be within the stated uncertainty limitsor the calibration procedure must be repeated.11.4 Periodic Calibration Verification and RecalibrationIn accordance with Guide D7448, analyze a control sample on aperiodic basis. Results obtained for the control
37、sample must be within 10 % of the stated value or all results obtained since thelast successful control check for that element must be rejected and the calibration procedure repeated.12. Report12.1 For reporting analyses to other than as-determined basis, refer to Practice D3180.12.2 For instruments
38、 that do not have calculation functions provided by the manufacturer for converting the concentrationamount of the analyte as analyzed to the appropriate oxide, the following calculations can be used:12.2.1%Na2O as Det!=A 2 B!VCD 31.3483 1 g N a!1000 mg Na! 3100 % (1)where:A = as measured concentrat
39、ion 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 Na2 O!2AW Na! 51.348where:MW = molecular weight, andAW = atomic weight.D8010 18312.2.2%K2O as Det! 5A 2 B!VCD 31.2053 1 g K!1000
40、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:M W K2 O!2A W K! 51.205where:MW = molecular weight, andAW = atomic weight.13. Keywords13.1
41、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 such patent rig
42、hts, 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 invited either for
43、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 fair hearing
44、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 standard may
45、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,
46、MA 01923, Tel: (978) 646-2600; http:/ Scope1.1 This test method describes a procedure for the determination of water soluble sodium as sodium oxide (Na2O) andpotassium as potassium oxide (K2O) in the analysis of coal samples prepared in accordance with Practice D2013.1.2 The values stated in SI unit
47、s are to be regarded as standard. The values given in parentheses after SI units are provided forinformation only and are not considered standard.1.3 This test method is derived in part from the ASME procedure water soluble alkalis.21.4 This standard does not purport to address all of the safety con
48、cerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability ofregulatory limitations prior to use.1.5 This international standard was developed in accordance with int
49、ernationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 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 of Coal and CokeD3302 Test Method for Total Moisture in
