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Designation: D5530 − 15Standard Test Method forTotal Moisture of Hazardous Waste Fuel by Karl FischerTitrimetry 1This standard is issued under the f i xed designation D5530; 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 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 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, inks, paints, and pigments. The range of applicabil-ity for this test method is between 1.0 and 100 %; however, thisevaluation was limited 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 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: 2D1193 Specif i cation for Reagent WaterD4017 Test Method for Water in Paints and Paint Materialsby 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 f l ask fully (see Note 1) is titrated todryness 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, anextraction using KF solvent is performed prior to introductioninto the titration f l ask. The total moisture in the sample is thendetermined. The f i nal total moisture percent is an average oftwo trials for each sample.3.2 The contents of the titration f l ask may be retained andused for additional analyses. The contents of the titration f l askwill need to be emptied and replaced with new solvent whenthe capacity of the f l ask is nearly exhausted or when solidmaterial affects the sensing by the electrode.4. Signif i cance and Use4.1 The determination of total moisture is important forassessing the quality 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. Interferences5.1 A small number of oxidants such as ferric and chromatesalts can oxidize iodide and may produce artif i cially lowresults.5.2 Certain reductants oxidized by iodine such asmercaptans, thioacetate, thiosulfate, stannous chloride,sulf i des, hydroquinone, and phenylenediamines can consumeiodine and may cause artif i cially high results. Basic materialssuch as hydroxides, oxides, and inorganic carbonates maycause artif i cially 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 the solid material,artif i cially 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 manufacturer’s instructions forinstallation and use.1 This 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 edition approved Sept. 1, 2015. Published September 2015. Originallyapproved in 1994. Last previous edition approved in 2009 as D5530-94(2009). DOI:10.1520/D5530-15.2 For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at service@astm.org. For Annual Book of ASTMStandards volume information, refer to the standard’s Document Summary page onthe ASTM website.Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1