ASTM D5530-22

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5530 − 15 D5530 − 22
Standard Test Method for
Total Moisture of Hazardous Waste Fuel by Karl Fischer
Titrimetry
This standard is issued under the fixed designation D5530; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the determination by Karl Fischer (KF) titrimetry of total moisture in solid or liquid hazardous waste
fuels used by industrial furnaces.
1.2 This test method has been used successfully on numerous samples of hazardous waste fuel composed of solvents, spent oils,
inks, paints, and pigments. The range of applicability for this test method is between 1.0 and 100 %; however, this evaluation was
limited to samples containing approximately 5 to 50 % water.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D4017 Test Method for Water in Paints and Paint Materials by Karl Fischer Method
D5681 Terminology for Waste and Waste Management
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 For definitions of terms used in this test method, refer to Terminology D5681.
This test method is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.06 on Analytical
Methods.
Current edition approved Sept. 1, 2015Oct. 1, 2022. Published September 2015October 2022. Originally approved in 1994. Last previous edition approved in 20092015
as D5530-94(2009).D5530 – 15. DOI: 10.1520/D5530-15.10.1520/D5530-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5530 − 22
4. Summary of Test Method
4.1 Karl Fischer reagent contains iodine, sulfur dioxide in pyridine (nonpyridine-containing reagents are currently available). The
iodine in the presence of water is reduced to colorless hydrogen iodide, with the endpoint being the presence of free I . The basic
reaction of the KF reagent with water is:
H O1SO 1I →2HI1SO (1)
2 2 2 3
SO 1R2 OH→HSO 2 R (2)
3 4
4.1.1 The methanol in the solution drives the equation to the right, removing sulfur trioxide.
4.2 An amount of solvent (see 7.38.3) sufficient to immerse the electrode fully in the titration flask fully (see Note 1) is titrated
to dryness as explained in 9.110.1, and the Karl Fischer reagent factor is determined by titration of measured amounts of water.
A weighed portion of the sample is dissolved in KF solvent and titrated with reagent to dryness. If solid material interferes (see
5.36.3) with the electrode or does not dissolve sufficiently, an extraction using KF solvent is performed prior to introduction into
the titration flask. The total moisture in the sample is then determined. The final total moisture percent is an average of two trials
meeting the repeatability as stated in 12.1.1 or repeatability criteria agreed upon between involved parties for each sample. The
measurement can be repeated to obtain results that meet repeatability criteria.
4.3 The contents of the titration flask may be retained and used for additional analyses. The contents of the titration flask will need
to be emptied and replaced with new solvent when the capacity of the flask is nearly exhausted or when solid material affects the
sensing by the electrode.
5. Significance and Use
5.1 The determination of total moisture is important for assessing the quality of fuels. fuel quality. Water content will affect the
heating value of fuels directly and can contribute to instability in the operation of an industrial furnace. furnace or adversely impact
performance in other applications. Additionally, high water contentscontent can present material handling and storage problems
during winter months or in cold environments.
6. Interferences
6.1 A small number of oxidants such as ferric and chromate salts can oxidize iodide and may produce artificially low results.
6.2 Certain reductants oxidized by iodine such as mercaptans, thioacetate, thiosulfate, stannous chloride, sulfides, hydroquinone,
and phenylenediamines can consume iodine and may cause artificially high results. Basic materials such as hydroxides, oxides, and
inorganic carbonates may cause artificially high results by water-forming reactions.
6.3 Some types of solid material found in waste-derived fuel may interfere with the electrode by blocking its contact with the
solvent. Depending on the nature of the solid material, artificially high or low results can occur.
7. Apparatus
7.1 Karl Fischer Potentiometric Titration Unit, automated or semi-automated, equipped with a magnetic vessel stirrer. The user
must follow the manufacturer’s instructions for installation and use.
NOTE 1—The Karl Fischer unit used for developing this test method was equipped with a twin platinum electrode, 25 to 80-mL 80 mL capacity titration
flask, magnetic stirrer, electronic piston burette, adjustable delay interval, LED display, visual and audible endpoint notification.
7.2 Syringe, 100-μL 100 μL capacity, with needle.
7.3 Syringe, 1 to 5-mL 5 mL capacity, without needle.
7.4 Analytical Balance, with minimum capacity of 160 g and capable of weighing to 0.0001 g.
D5530 − 22
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used,used provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of the determination.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by Type
II of Specification D1193.
8.3 Karl Fischer Solvent—The solvent system must be a non-methanol formulation for the analysis of aldehydes and ketones and
for general usage. The use of a strictly general purpose solvent is not acceptable because of the potential of obtaining artificially
high results from water-forming reactions by chemicals with active carbonyl groups.
8.4 Karl Fischer Reagent—The reagent should have a standard titer value of 5 mg H O/mL reagent and be listed as being
compatible with the solvent system.
9. Sample
9.1 Because stratification or layering of liquid samples is possible, the laboratory sample should be mixed thoroughly by shaking
prior to withdrawing a portion for testing. Strongly multi-phasic samples should have each layer analyzed separately and the total
moistur
...