ASTM D5530-15

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

SIGNIFICANCE AND USE
4.1 The determination of total moisture is important for assessing the quality of fuels. Water content will affect the heating value of fuels directly and can contribute to instability in the operation of an industrial furnace. Additionally, high water contents 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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-Aug-2015
• ICS: 13.030.30 - Special wastes
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5530 − 15
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 weighed portion of the sample is dissolved in KF solvent and
titrated with reagent to dryness. If solid material interferes (see
1.1 This test method covers the determination by Karl
5.3) with the electrode or does not dissolve sufficiently, an
Fischer (KF) titrimetry of total moisture in solid or liquid
extraction using KF solvent is performed prior to introduction
hazardous waste fuels used by industrial furnaces.
into the titration flask. The total moisture in the sample is then
1.2 This test method has been used successfully on numer-
determined. The final total moisture percent is an average of
ous samples of hazardous waste fuel composed of solvents,
two trials for each sample.
spent oils, inks, paints, and pigments. The range of applicabil-
3.2 The contents of the titration flask may be retained and
ityforthistestmethodisbetween1.0and100 %;however,this
used for additional analyses. The contents of the titration flask
evaluation was limited to samples containing approximately 5
will need to be emptied and replaced with new solvent when
to 50 % water.
the capacity of the flask is nearly exhausted or when solid
1.3 The values stated in SI units are to be regarded as
material affects the sensing by the electrode.
standard. No other units of measurement are included in this
standard.
4. Significance and Use
1.4 This standard does not purport to address all of the
4.1 The determination of total moisture is important for
safety concerns, if any, associated with its use. It is the
assessing the quality of fuels. Water content will affect the
responsibility of the user of this standard to establish appro-
heating value of fuels directly and can contribute to instability
priate safety and health practices and determine the applica-
in the operation of an industrial furnace. Additionally, high
bility of regulatory limitations prior to use.
water contents can present material handling and storage
problems during winter months or in cold environments.
2. Referenced Documents
2
2.1 ASTM Standards:
5. Interferences
D1193 Specification for Reagent Water
5.1 Asmall number of oxidants such as ferric and chromate
D4017 Test Method for Water in Paints and Paint Materials
salts can oxidize iodide and may produce artificially low
by Karl Fischer Method
results.
E691 Practice for Conducting an Interlaboratory Study to
5.2 Certain reductants oxidized by iodine such as
Determine the Precision of a Test Method
mercaptans, thioacetate, thiosulfate, stannous chloride,
3. Summary of Test Method
sulfides, hydroquinone, and phenylenediamines can consume
iodine and may cause artificially high results. Basic materials
3.1 An amount of solvent (see 7.3) sufficient to immerse the
such as hydroxides, oxides, and inorganic carbonates may
electrode in the titration flask fully (see Note 1) is titrated to
cause artificially high results by water-forming reactions.
dryness as explained in 9.1, and the Karl Fischer reagent factor
is determined by titration of measured amounts of water. A
5.3 Sometypesofsolidmaterialfoundinwaste-derivedfuel
may interfere with the electrode by blocking its contact with
the solvent. Depending on the nature of the solid material,
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 artificially high or low results can occur.
Analytical Methods.
Current edition approved Sept. 1, 2015. Published September 2015. Originally
6. Apparatus
approvedin1994.Lastpreviouseditionapprovedin2009asD5530-94(2009).DOI:
10.1520/D5530-15.
6.1 Karl Fischer Potentiometric Titration Unit, automated
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
or semi-automated, equipped with a magnetic vessel stirrer.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
The user must follow the manufacturer’s instructions for
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. installation and use.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5530 − 15
NOTE 1—The Karl Fischer unit used for developing this test method
9.1.3 Bring the KF solvent to dryness by titrating with
was equipped with a twin platinum elec
...

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 − 94 (Reapproved 2009) D5530 − 15
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 expected 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 and health practices and determine the applicability of regulatory
limitations prior to use.
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
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Test Method
3.1 An amount of solvent (see 7.3) sufficient to immerse the electrode in the titration flask fully (see Note 1) is titrated to dryness
as explained in 9.1, 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 5.3) 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 for each sample.
3.2 The contents of the tirationtitration 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.
4. Significance and Use
4.1 The determination of total moisture is important for assessing the quality of fuels. Water content will affect the heating value
of fuels directly and can contribute to instability in the operation of an industrial furnace. Additionally, high water contents can
present material handling and storage problems during winter months or in cold environments.
5. Interferences
5.1 A small number of oxidants such as ferric and chromate salts can oxidize iodide and may produce artificially low results.
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 Feb. 1, 2009Sept. 1, 2015. Published March 2009September 2015. Originally approved in 1994. Last previous editioedition approved in
20032009 as D5530-94(2003).D5530-94(2009). DOI: 10.1520/D5530-94R09.10.1520/D5530-15.
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 − 15
5.2 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.
5.3 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 materi
...