1、Designation: D5530 15Standard Test Method forTotal Moisture of Hazardous Waste Fuel by Karl FischerTitrimetry1This standard is issued under the fixed designation D5530; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st 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 or liquidhazardous w
3、aste 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, inks, paints, and pigments. The range of applicabil-ity for this test method is between 1.0 and 100 %; however, thisevaluation was limi
4、ted to samples containing approximately 5to 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 use. It is therespon
5、sibility 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:2D1193 Specification for Reagent WaterD4017 Test Method for Water in Paints and Paint Material
6、sby Karl Fischer MethodE691 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 todryness as explained in 9.1, a
7、nd 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, anextraction using KF
8、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 titration flask may be retained andused for additional analyses. The contents of
9、 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 quality of fuels. Water
10、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. Interferences5.1 A small number of oxi
11、dants such as ferric and chromatesalts can oxidize iodide and may produce artificially lowresults.5.2 Certain reductants oxidized by iodine such asmercaptans, thioacetate, thiosulfate, stannous chloride,sulfides, hydroquinone, and phenylenediamines can consumeiodine and may cause artificially high r
12、esults. Basic materialssuch as hydroxides, oxides, and inorganic carbonates maycause artificially 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. Depending on the nature of t
13、he 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.1This test method is under the juri
14、sdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Sept. 1, 2015. Published September 2015. Originallyapproved in 1994. Last previous edition approved in 2009 as D5530-94(2009). DOI:10.1520/D5530-
15、15.2For 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 Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Bo
16、x C700, West Conshohocken, PA 19428-2959. United States1NOTE 1The Karl Fischer unit used for developing this test methodwas equipped with a twin platinum electrode, 25 to 80-mL capacitytitration flask, magnetic stirrer, electronic piston burette, adjustable delayinterval, LED display, visual and aud
17、ible 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 tes
18、ts. 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 ofsuffi
19、ciently high purity to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type II of Specification D1193.7.3 Karl Fischer SolventThe solvent system must be anon-met
20、hanol 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 Reagen
21、tThe 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 portion for t
22、esting. 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. Calibration and S
23、tandardization9.1 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 theelectrode ti
24、p, 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 reagent.9.1
25、.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 is reac
26、hed.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! 5 water weight mg!/reagent volume mL! (1)9.1.9.2 The replicate values for F should have a relativestandar
27、d 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 theequi
28、pment 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, it
29、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 sample ba
30、sed on the amount of expectedwater content is as given in Table 1.NOTE 2The information given in Table 1 is described in Test MethodD4017.10.6 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 thesensing prob
31、e, or it is observed that the sample is not dissolvedin the KF solvent sufficiently, extract the sample with solventas follows:3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American
32、Chemical Society, 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 Titrant
33、Volumeat 5 mg/mL titre, mL0.51.0 5 51013 25 1020310 12 10201030 0.41.0 152570 0.1 20D5530 15210.7.1 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 andsolvent.10.7.2 Cap the sample mixtur
34、e and shake or mix on avortex-type or orbital mixer for approximately 1 min.10.7.3 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 KF solvent begin
35、ning 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 unextracted samp
36、les, 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 percentagewater as follows:V
37、2 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!1sample mg!sample mg!11. Precision and Bias411.1 PrecisionThe precision
38、 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 E691.11.1.1 Repeatabi
39、lity (Within Laboratory)The coefficientof variation of results (each the average of duplicatedeterminations), obtained by the same analyst on differentdays, has been estimated to be 1.3 % relative at 30 degrees offreedom. Therefore, the results of two properly conductedtests, by the same operator on
40、 the same sample, should notdiffer by more than 3.6 % of their average.11.1.2 Reproducibility (Between Laboratories)The coeffi-cient of variation of results (each the average of duplicatedeterminations), obtained by analysts in different laboratories,has been estimated to be 4.3 % relative at 5 degr
41、ees 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 are no recognize
42、d 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 are expressly ad
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