1、Designation: D 5530 94 (Reapproved 2009)Standard Test Method forTotal Moisture of Hazardous Waste Fuel by Karl FischerTitrimetry1This standard is issued under the fixed designation D 5530; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, the year 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 test method covers the determination by KarlFischer (KF) titrimetry of total moisture in solid
3、or liquidhazardous waste fuels used by industrial furnaces.1.2 This test method has been used successfully on numer-ous samples of hazardous waste fuel composed of solvents,spent oils, paints, and pigments. The expected range ofapplicability for this test method is between 1.0 and 100 %;however, thi
4、s evaluation was limited to samples containingapproximately 5 to 50 % water.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its
5、 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:2D 1193 Specification for Reagent WaterD 4017 Test Method for Water in Pa
6、ints and Paint Materialsby Karl Fischer MethodE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Method3.1 An amount of solvent (see 7.3) sufficient to immerse theelectrode in the titration flask fully (see Note 1) is titrated todrynes
7、s as explained in 9.1, and the Karl Fischer reagent factoris determined by titration of measured amounts of water. Aweighed portion of the sample is dissolved in KF solvent andtitrated with reagent to dryness. If solid material interferes (see5.3) with the electrode or does not dissolve sufficiently
8、, anextraction using KF solvent is performed prior to introductioninto the titration flask. The total moisture in the sample is thendetermined. The final total moisture percent is an average oftwo trials for each sample.3.2 The contents of the tiration flask may be retained andused for additional an
9、alyses. The contents of the titration flaskwill need to be emptied and replaced with new solvent whenthe capacity of the flask is nearly exhausted or when solidmaterial affects the sensing by the electrode.4. Significance and Use4.1 The determination of total moisture is important forassessing the q
10、uality of fuels. Water content will affect theheating value of fuels directly and can contribute to instabilityin the operation of an industrial furnace. Additionally, highwater contents can present material handling and storageproblems during winter months or in cold environments.5. Interferences5.
11、1 A small number of oxidants such as ferric and chromatesalts can oxidize iodide and may produce artificially lowresults.5.2 Certain reductants oxidized by iodine such as mercap-tans, thioacetate, thiosulfate, stannous chloride, sulfides, hyd-roquinone, and phenylenediamines can consume iodine andma
12、y cause artificially high results. Basic materials such ashydroxides, oxides, and inorganic carbonates may cause arti-ficially high results by water-forming reactions.5.3 Some types of solid material found in waste-derived fuelmay interfere with the electrode by blocking its contact withthe solvent.
13、 Depending on the nature of the solid material,artificially high or low results can occur.6. Apparatus6.1 Karl Fischer Potentiometric Titration Unit, automatedor semi-automated, equipped with a magnetic vessel stirrer.The user must follow the manufacturers instructions forinstallation and use.NOTE 1
14、The Karl Fischer unit used for developing this test methodwas equipped with a twin platinum electrode, 25 to 80-mL capacity1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edit
15、ion approved Feb. 1, 2009. Published March 2009. Originallyapproved in 1994. Last previous editio approved in 2003 as D 5530-94(2003).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume info
16、rmation, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.titration flask, magnetic stirrer, electronic piston burette, adjustable delayinterval, LED display, visual and
17、audible endpoint notification.6.2 Syringe, 100-L capacity, with needle.6.3 Syringe, 1 to 5-mL capacity, without needle.6.4 Analytical Balance, with minimum capacity of 160 gand capable of weighing to 0.0001 g.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all
18、tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsu
19、fficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Purity of Water Unless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type II of Specification D 1193.7.3 Karl Fischer SolventThe solvent system must be a
20、non-methanol formulation for the analysis of aldehydes andketones and for general usage. The use of a strictly generalpurpose solvent is not acceptable because of the potential ofobtaining artificially high results from water-forming reactionsby chemicals with active carbonyl groups.7.4 Karl Fischer
21、 ReagentThe reagent should have astandard titer value of 5 mg H2O/mL reagent and be listed asbeing compatible with the solvent system.8. Sample8.1 Because stratification or layering of liquid samples ispossible, the laboratory sample should be mixed thoroughly byshaking prior to withdrawing a portio
22、n for testing. Stronglymulti-phasic samples should have each layer analyzed sepa-rately and the total moisture percent of the sample calculated asa weighted average. Solid samples should be mixed thoroughlyby shaking or stirring, depending on the physical characteris-tics of the sample.9. Calibratio
23、n and Standardization9.1 Determination of Karl Fischer reagent factor (F):9.1.1 Determine the mg H2O/mL reagent (F) for each newprocurement of KF solvent and at a minimum of daily on asolvent retained for further titrations (see Section 3).9.1.2 Add a sufficient quantity of solvent to cover theelect
24、rode tip, set the delay interval to 30 s, and engage themagnetic stirrer.9.1.3 Bring the KF solvent to dryness by titrating withreagent to the endpoint. The endpoint is typically indicated bya visual or audible alarm, or both, depending on the equipmentmanufacturer.9.1.4 Refill the burette with reag
25、ent.9.1.5 Fill the 100-L syringe with approximately 10 L ofwater and weigh to the nearest 0.0001 g.9.1.6 Dispense the syringe contents into the titration vesseland replace the sample port stopper immediately. Reweigh thesyringe and record the water mass.9.1.7 Titrate with reagent until the endpoint
26、is reached.Record the titrant volume used.9.1.8 The final value for F should be based on the mean ofa minimum of three replicates.9.1.9 Calculation:9.1.9.1 Calculate F by the following formula:F mg/mL!5water weight mg!/reagent volume mL! (1)9.1.9.2 The replicate values for F should have a relativest
27、andard deviation of not greater than 5 %. The standardizationshould be repeated if a greater variance is determined.10. Procedure10.1 Bring the KF solvent to dryness by titrating withreagent to the endpoint. The endpoint is typically indicatedvisually or by an audible alarm, or both, depending on th
28、eequipment manufacturer.10.2 Refill the burette with reagent.10.3 Draw a portion of the sample into the 1 to 5-mLsyringe, and clean any residual sample material from thesyringe tip. If the sample contains a large amount of solids orits viscosity is such that it cannot be drawn into the syringeeasily
29、, it may be necessary to weigh the sample and introduceit using a laboratory spatula or suitable device.10.4 Weigh the syringe with sample to the nearest 0.0001 g.10.5 Add the sample to the titration vessel and allowsufficient time for the material to dissolve adequately. Thesuggested amount of samp
30、le based on the amount of expectedwater content is as given in Table 1.NOTE 2The information given in Table 1 is described in Test MethodD 4017.10.6 Reweigh the syringe and record the sample mass addedto the vessel to the nearest 0.0001 g.10.7 If solid material is observed interfering with thesensin
31、g probe, or it is observed that the sample is not dissolvedin the KF solvent sufficiently, extract the sample with solventas follows:10.7.1 Beginning again with a new sample, combine thesample and solvent gravimetrically at an approximate 1:1 ratioin a large test tube. Record the mass of both sample
32、 andsolvent.10.7.2 Cap the sample mixture and shake or mix on avortex-type or orbital mixer for approximately 1 min.3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical S
33、ociety, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Specimen GuidelinesExpected water, %Approximate SpecimenMass, gApproximate TitrantVolumeat 5
34、 mg/mL titre, mL0.51.0 5 51013 25 1020310 12 10201030 0.41.0 152570 0.1 20D 5530 94 (2009)210.7.3 Centrifuge the sample mixture to separate theundissolved/leached solids.10.7.4 Analyze the supernatant beginning with 10.1.10.7.5 In addition to the extracted sample, analyze a blanksolution of virgin K
35、F solvent beginning with 10.1. The KFsolvent blank (mL of titrant used) is subtracted in 10.9.3.10.8 Titrate with reagent until the endpoint is reached.Record the volume.10.9 The final percentage of water should be based on themean of a minimum of two determinations.10.9.1 Calculation:10.9.1.1 For u
36、nextracted samples, calculate the percentagewater as follows:V!F! 5 WW/S! 100 5 water, weight% (2)where:V = reagent volume (mL),F = Karl Fischer reagent factor (mg/mL),W = mass of water contained in the sample (mg), andS = sample mass (mg).10.9.1.2 For extracted samples, calculate the percentagewate
37、r as follows:V solvent blank!F! 5 WW/S!dilution factor! 5 % water (3)where:V = reagent volume (mL),F = Karl Fischer reagent factor (mg/mL),W = mass of water contained in the sample (mg),S = sample mass (mg), anddilution factor 5KF solvent mg!1 sample mg!sample mg!11. Precision and Bias411.1 Precisio
38、nThe precision estimates are based on aninterlaboratory study in which operators in six different labo-ratories analyzed in duplicate, on separate days, five samples ofhazardous waste fuel containing between 13 and 32 % water.The results were analyzed statistically in accordance withPractice E 691.1
39、1.1.1 Repeatability (Within Laboratory)The coefficientof variation of results (each the average of duplicate determi-nations), obtained by the same analyst on different days, hasbeen estimated to be 1.3 % relative at 30 degrees of freedom.Therefore, the results of two properly conducted tests, by th
40、esame operator on the same sample, should not differ by morethan 3.6 % of their average.11.1.2 Reproducibility (Between Laboratories)The coef-ficient of variation of results (each the average of duplicatedeterminations), obtained by analysts in different laboratories,has been estimated to be 4.3 % r
41、elative at 5 degrees offreedom. Therefore, the results of properly conducted tests, onidentical samples of the same material, by two differentlaboratories, should not differ from each other by more than11.9 % of their average.11.2 BiasThe bias of this test method has not beendetermined because there
42、 are no recognized reference stan-dards.12. Keywords12.1 hazardous waste fuel; Karl Fischer titrimetry; percentwater; total moistureASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard
43、 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 responsible technical committee and must be reviewed every five years andif n
44、ot 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
45、 you may attend. If you feel that your comments have not received a 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,Uni
46、ted States. Individual reprints (single or multiple copies) of this 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).4A copy of the research report used to develop the precision statement isavailable from ASTM headquarters. Request RR:D 34-1009.D 5530 94 (2009)3
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