ASTM D5530-22

Standard Test Method for Total Moisture of Hazardous Waste Fuel by Karl Fischer Titrimetry

SIGNIFICANCE AND USE
5.1 The determination of total moisture is important for assessing the fuel quality. Water content will affect the heating value of fuels directly and can contribute to instability in the operation of an industrial furnace or adversely impact performance in other applications. Additionally, high water content can present material handling and storage problems during winter months or in cold environments.
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, health, and environmental 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.

General Information

• Status: Published
• Publication Date: 30-Sep-2022
• ICS: 13.030.30 - Special wastes
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Standards Content (Sample)

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.
Designation: D5530 − 22
Standard Test Method for
Total Moisture of Hazardous Waste Fuel by Karl Fischer
1
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 E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method covers the determination by Karl
Fischer (KF) titrimetry of total moisture in solid or liquid
3. Terminology
hazardous waste fuels used by industrial furnaces.
3.1 For definitions of terms used in this test method, refer to
1.2 This test method has been used successfully on numer-
Terminology D5681.
ous samples of hazardous waste fuel composed of solvents,
spent oils, inks, paints, and pigments. The range of applicabil- 4. Summary of Test Method
ityforthistestmethodisbetween1.0and100 %;however,this
4.1 Karl Fischer reagent contains iodine, sulfur dioxide in
evaluation was limited to samples containing approximately 5
pyridine (nonpyridine-containing reagents are currently avail-
to 50 % water.
able). The iodine in the presence of water is reduced to
1.3 The values stated in SI units are to be regarded as colorless hydrogen iodide, with the endpoint being the pres-
standard. No other units of measurement are included in this
ence of free I .The basic reaction of the KF reagent with water
2
standard. is:
1.4 This standard does not purport to address all of the
H O1SO 1I→2HI1SO (1)
2 2 2 3
safety concerns, if any, associated with its use. It is the
SO 1R 2 OH→HSO 2R (2)
3 4
responsibility of the user of this standard to establish appro-
4.1.1 The methanol in the solution drives the equation to the
priate safety, health, and environmental practices and deter-
right, removing sulfur trioxide.
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
4.2 An amount of solvent (see 8.3) sufficient to immerse the
dance with internationally recognized principles on standard-
electrode fully in the titration flask (see Note 1) is titrated to
ization established in the Decision on Principles for the
dryness as explained in 10.1, and the Karl Fischer reagent
Development of International Standards, Guides and Recom-
factor is determined by titration of measured amounts of water.
mendations issued by the World Trade Organization Technical
AweighedportionofthesampleisdissolvedinKFsolventand
Barriers to Trade (TBT) Committee.
titrated with reagent to dryness. If solid material interferes (see
6.3) with the electrode or does not dissolve sufficiently, an
2. Referenced Documents
extraction using KF solvent is performed prior to introduction
2
into the titration flask. The total moisture in the sample is then
2.1 ASTM Standards:
determined. The final total moisture percent is an average of
D1193 Specification for Reagent Water
two trials meeting the repeatability as stated in 12.1.1 or
D4017 Test Method for Water in Paints and Paint Materials
repeatability criteria agreed upon between involved parties for
by Karl Fischer Method
each sample. The measurement can be repeated to obtain
D5681 Terminology for Waste and Waste Management
results that meet repeatability criteria.
4.3 The contents of the titration flask may be retained and
1
This test method is under the jurisdiction of ASTM Committee D34 on Waste used for additional analyses. The contents of the titration flask
Management and is the direct responsibility of Subcommittee D34.01.06 on
will need to be emptied and replaced with new solvent when
Analytical Methods.
the capacity of the flask is nearly exhausted or when solid
Current edition approved Oct. 1, 2022. Published October 2022. Originally
material affects the sensing by the electrode.
approved 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, or 5. Significance and Use
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
5.1 The determination of total moisture is important for
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. assessing the fuel quality. Water content will affect the heating
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5530 − 22
value of f
...

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
1
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
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.
1
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.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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
1

---------------------- Page: 1 ----------------------
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
2
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 near
...