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Designation: D5530 − 22Standard 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, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards: 2D1193 Specif i cation for Reagent WaterD4017 Test Method for Water in Paints and Paint Materialsby Karl Fischer MethodD5681 Terminology for Waste and Waste ManagementE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 For def i nitions of terms used in this test method, refer toTerminology D5681.4. Summary of Test Method4.1 Karl Fischer reagent contains iodine, sulfur dioxide inpyridine (nonpyridine-containing reagents are currently avail-able). The iodine in the presence of water is reduced tocolorless hydrogen iodide, with the endpoint being the pres-ence of free I 2 . The basic reaction of the KF reagent with wateris:H 2 O1SO 2 1I 2 →2HI1SO 3 (1)SO 3 1R 2 OH→HSO 4 2 R (2)4.1.1 The methanol in the solution drives the equation to theright, removing sulfur trioxide.4.2 An amount of solvent (see 8.3) sufficient to immerse theelectrode fully in the titration f l ask (see Note 1) is titrated todryness as explained in 10.1, and the Karl Fischer reagentfactor is 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 (see6.3) 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 meeting the repeatability as stated in 12.1.1 orrepeatability criteria agreed upon between involved parties foreach sample. The measurement can be repeated to obtainresults that meet repeatability criteria.4.3 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.5. Signif i cance and Use5.1 The determination of total moisture is important forassessing the fuel quality. Water content will affect the heating1 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 Oct. 1, 2022. Published October 2022. Originallyapproved in 1994. Last previous edition approved in 2015 as D5530 – 15. DOI:10.1520/D5530-22.2 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 StatesThis international standard was developed in accordance with internationally 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.1