1、Designation: D8213 18Standard Test Method forDetermination of Boron in Coal1This standard is issued under the fixed designation D8213; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parenthes
2、es indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method describes a procedure for the analysisof total boron in coal.1.2 UnitsThe values stated in SI units are to be regardedas standard. The va
3、lues given in parentheses after SI units areprovided for information only and are not considered standard.1.3 This 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, h
4、ealth, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of Inter
5、national Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD31
6、80 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD5865 Test Method for Gross Calorific Value of Coal andCokeD6349 Test Method for Determination of Major and MinorElements in Coal, Coke, and Solid Residues from Com-bustion of Coal and Coke by Inductively CoupledP
7、lasmaAtomic Emission SpectrometryD6357 Test Methods for Determination of Trace Elements inCoal, Coke, and Combustion Residues from Coal Utiliza-tion Processes by Inductively Coupled Plasma AtomicEmission Spectrometry, Inductively Coupled PlasmaMass Spectrometry, and Graphite Furnace Atomic AbE144 Pr
8、actice for Safe Use of Oxygen Combustion VesselsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 SAI Standard:3AS 1038.10.3 Coal and CokeAnalysis and Testing, Part10.3: Determi
9、nation of Trace ElementsCoal andCokeDetermination of Boron ContentICP-AESMethod3. Terminology3.1 DefinitionsDefinitions applicable to these test meth-ods are listed in Terminology D121.4. Summary of Test Method4.1 Total boron is determined following one of five testpreparation procedures:4.1.1 Proce
10、dure AThe coal or coke to be analyzed iscombusted in a vessel with dilute nitric acid absorbing theboron vapors. The combustion vessel is rinsed into a vesselwith dilute nitric acid.4.1.2 Procedure BThe coal or coke to be analyzed isashed under controlled conditions. The residue is digested byaqua-r
11、egia, and dissolved in 1 % nitric acid.4.1.3 Procedure CThe coal or coke to be analyzed isashed under controlled conditions. The residue is digested in amixture of hydrofluoric, nitric, and hydrochloric acids.4.1.4 Procedure DFollowing AS 1038.10.3, the coal orcoke to be analyzed is ignited at 800 C
12、 with Eschka mixture.The residue is dissolved in dilute hydrochloric acid.4.1.5 Procedure EThe coal or coke to be analyzed isdigested using a microwave system following manufacturersrecommendation for temperatures, power, and time, usingeither the acid mixtures specified in Test Methods D6357 orTest
13、 Method D6349, depending upon instrument capabilities.4.1.6 Combustion residues are digested on an as-receivedbasis.1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.29 on MajorElements in Ash and Trace Elements of
14、Coal.Current edition approved Dec. 1, 2018. Published February 2019. DOI: 10.1520/D8213-18.2For 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 Su
15、mmary page onthe ASTM website.3Available from SAI Global, Level 37, 680 George Street, Sydney NSW 2000,Australia, https:/ ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationall
16、y recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14.1.7 The concentration of boron is determined by eitheri
17、nductively coupled atomic emission spectrometry (ICPAES)or inductively coupled plasma mass spectrometry (ICPMS).Selected elements that occur at concentrations below thedetection limits of ICPAES can be quantitatively analyzed bygraphite furnace atomic absorption spectrometry (GFAAS).5. Significance
18、and Use5.1 The possible emission of boron that may be found incoal from coal combustion is an environmental concern.5.2 When test portions are burned according to thisprocedure, the total boron is quantitatively retained and isrepresentative of concentrations in the whole coal.6. Apparatus6.1 Balanc
19、ecapable of weighing the analysis sample tothe nearest 0.1 mg.6.2 Procedure A:6.2.1 Combustion Vessel, constructed of materials that arenot affected by the combustion process or products. The vesselmust be designed so that all liquid combustion products can bequantitatively recovered by washing the
20、inner surfaces. Theremust be no gas leakage during the test. The vessel must becapable of withstanding a hydrostatic-pressure test to approxi-mately 20 MPa at room temperature without stressing any partbeyond its elastic limit.6.2.2 Water BathA container large enough to hold thecombustion vessel and
21、 enough cooling water to dissipate theheat generated during the combustion process. The containershall be designed to allow a constant flow of water around thecombustion vessel.6.2.3 Combustion CruciblesSamples shall be burned in anopen crucible of platinum, quartz, or acceptable base-metalalloy.6.2
22、.4 Firing Wire, 100 mm, nickel-chromium alloy, No. 34Bthe details are given in ASTM Research Report No.D05-1050.413.1.1 Repeatability Limit (r)The difference between re-petitive results obtained by the same operator in a givenlaboratory applying the same test method with the sameapparatus under cons
23、tant operating conditions on identical testmaterial within short intervals of time would in the long run, inthe normal and correct operation of the test method, exceed thefollowing values only in 1 case in 20.13.1.1.1 Repeatability can be interpreted as the maximumdifference between two results, obt
24、ained under repeatabilityconditions, that is accepted as plausible due to random causesunder normal and correct operation of the test method.13.1.1.2 Repeatability limits for the combined Procedures Dand E are listed in Table 2. Estimates for the moisture in theanalysis samples, individual procedure
25、s, and the combinedprocedures are listed in Tables A1.1-A1.7.13.1.2 Reproducibility Limit (R)The difference betweentwo single and independent results obtained by differentoperators applying the same test method in different laborato-ries using different apparatus on identical test material would,in
26、the long run, in the normal and correct operation of the testmethod, exceed the following values only in 1 case in 20.13.1.2.1 Reproducibility can be interpreted as the maximumdifference between two results, obtained under reproducibilityconditions, that is accepted as plausible due to random causes
27、under normal and correct operation of the test method.13.1.2.2 Reproducibility estimates for the combined Proce-dures D and E are listed in Table 2. Estimates for the moisturein the analysis samples, individual procedures, and the com-bined procedures are listed in Tables A1.1-A1.7.13.1.3 The above
28、terms (repeatability limit and reproduc-ibility limit) are used as specified in Practice E177.13.1.4 Any judgment in accordance with statements 10.1.1and 10.1.2 would normally have an approximate 95 % prob-ability of being correct, however the precision statistics ob-tained in this ILS must not be t
29、reated as exact mathematicalquantities which are applicable to all circumstances and uses.The limited number of laboratories reporting results guaranteesthat there will be times when differences greater than predictedby the ILS results will arise, sometimes with considerablygreater or smaller freque
30、ncy than the 95 % probability limitwould imply. The repeatability limit and the reproducibility4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D05-1050. ContactASTM CustomerService at serviceastm.org.TABLE 1 Example Microwave Pa
31、rametersTemperature(C)Ramp Time(min)Hold Time(min)Pressure(PSI)Power(W)Example 1 210 5:00 3:00 400 300Example 2 250 20:00 20:00 N/A 500 to 1800Example 3 210 25:00 20:00 N/A 1000Example 4 160 5:00 10:00 435 1350Example 5 250 5:00 35:00 500 1500D8213 184limit should be considered as general guides, an
32、d the associ-ated probability of 95 % as only a rough indicator of what canbe expected.13.2 BiasAt the time of the study, there was no accepted,certified reference material suitable for determining the bias forthis test method available, therefore no statement on bias isbeing made.13.3 The precision
33、 statement was determined through sta-tistical examination of 843 results, from as many as 7laboratories, on 13 different coal samples.13.4 To judge the equivalency of two test results, it isrecommended to choose the coal material closest in character-istics to the test coal.14. Keywords14.1 boron;
34、coal; inductively coupled plasma mass spec-trometer; trace elementsANNEX(Mandatory Information)A1. PRECISION STATISTICSA1.1 Repeatability Standard Deviation (Sr)A1.1.1 The standard deviation of test results obtained underrepeatability conditions.A1.2 Reproducibility Standard Deviation (SR)A1.2.1 The
35、 standard deviation of test results obtained underreproducibility conditions.TABLE 2 Mass Fraction Ranges and Limits for Repeatability andReproducibility for Determination of Boron in CoalAProcedure Mass FractionRange, g/mLRepeatabilityLimitrReproducibilityLimitRD and E 16 to 236 0.03x + 5.8 0.12x+
36、21.1AWhere x is the average of two single test results.TABLE A1.1 Repeatability (Sr,r) and Reproducibility (SR,R) Parameters, Moisture in the Analysis SampleMaterial Number ofLabsAveragex(%)RepeatabilityStandard DeviationSrReproducibilityStandard DeviationSRRepeatability Limitr(%)Reproducibility Lim
37、itR(%)Subbit 2 18.05 0.04 0.04 0.11 0.11Lignite 2 28.59 0.00 1.00 0.00 2.81hvCb, IL 2 4.25 0.04 0.04 0.11 0.12hvAb, WV 2 1.52 0.00 0.02 0.00 0.06hcAB, KY 2 3.38 0.04 0.07 0.11 0.20hvCb, IN 2 5.55 0.04 0.04 0.11 0.12Subbit, WY 2 9.38 0.07 0.18 0.20 0.50mv, RUS 2 2.21 0.00 0.29 0.00 0.81Bit, CO 2 3.88
38、 0.04 0.31 0.11 0.86Bit, UT 2 3.82 0.04 0.04 0.11 0.11SRM 1632d 2 2.24 0.00 0.06 0.00 0.16SRM 1635a 2 14.49 0.04 0.82 0.11 2.29SARM 18 2 3.34 0.07 0.66 0.20 1.85D8213 185TABLE A1.2 Repeatability (Sr,r) and Reproducibility (SR,R) Parameters, Procedure AMaterial Number ofLabsAveragex(g/g)Repeatability
39、Standard DeviationSrReproducibilityStandard DeviationSRRepeatability Limitr(g/g)Reproducibility LimitR(g/g)Subbit 2 28.48 3.41 6.54 9.55 18.31Lignite 2 34.88 2.31 10.56 6.46 29.58hvCb, IL 2 161.87 2.48 3.29 6.96 9.22hvAb, WV 2 72.00 1.37 4.89 3.84 13.70hcAB, KY 2 47.23 1.46 7.54 4.10 21.12hvCb, IN 2
40、 109.77 2.60 2.72 7.27 7.61Subbit, WY 2 22.43 1.38 2.45 3.88 6.85mv, RUS 2 13.38 0.48 0.79 1.33 2.20Bit, CO 2 153.37 5.36 14.08 15.00 39.44Bit, UT 2 43.20 0.60 3.43 1.69 9.60SRM 1632d 2 45.70 0.54 3.47 1.52 9.71SRM 1635a 2 26.45 0.80 4.41 2.23 12.34SARM 18 2 23.47 0.90 0.90 2.53 2.53TABLE A1.3 Repea
41、tability (Sr,r) and Reproducibility (SR,R) Parameters, Procedure BMaterial Number ofLabsAveragex(g/g)RepeatabilityStandard DeviationSrReproducibilityStandard DeviationSRRepeatability Limitr(g/g)Reproducibility LimitR(g/g)Subbit 3 32.50 3.22 9.29 9.00 26.02Lignite 3 38.65 1.31 1.88 3.67 5.27hvCb, IL
42、3 154.11 7.70 35.48 21.56 99.34hvAb, WV 3 56.72 5.75 5.75 16.09 16.09hcAB, KY 3 40.55 3.80 4.29 10.65 12.02hvCb, IN 3 91.11 2.32 12.97 6.51 36.31Subbit, WY 3 23.41 0.40 0.62 1.11 1.74mv, RUS 3 10.99 1.10 2.28 3.08 6.38Bit, CO 3 170.16 5.36 15.88 15.02 44.47Bit, UT 3 53.65 1.16 4.50 3.24 12.61SRM 163
43、2d 3 42.54 1.77 14.32 4.95 40.10SRM 1635a 3 34.80 0.79 4.08 2.20 11.41SARM 18 1 24.40 0.70 0.70 1.96 1.96TABLE A1.4 Repeatability (Sr,r) and Reproducibility (SR,R) Parameters, Procedure CMaterial Number ofLabsAveragex(g/g)RepeatabilityStandard DeviationSrReproducibilityStandard DeviationSRRepeatabil
44、ity Limitr(g/g)Reproducibility LimitR(g/g)Subbit 2 39.33 0.92 9.79 2.57 27.41Lignite 2 41.37 0.71 12.27 2.00 34.36hvCb, IL 2 171.35 4.04 8.91 11.32 24.94hvAb, WV 2 68.44 1.67 17.15 4.67 48.02hcAB, KY 2 49.01 2.84 15.90 7.96 44.53hvCb, IN 2 102.14 4.27 16.30 11.95 45.63Subbit, WY 2 23.91 0.16 5.40 0.
45、44 15.13mv, RUS 2 13.47 0.40 3.88 1.11 10.87Bit, CO 2 160.85 2.70 24.64 7.57 68.98Bit, UT 2 51.30 0.97 10.78 2.71 30.18SRM 1632d 55.12 0.85 11.93 2.37 33.41SRM 1635a 1 37.30 0.66 0.66 1.84 1.84SARM 18 1 30.30 0.75 0.75 2.11 2.11D8213 186ASTM International takes no position respecting the validity of
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