ASTM D5530-94(2003)
(Test Method)Standard Test Method for Total Moisture of Hazardous Waste Fuel by Karl Fischer Titrimetry
Standard Test Method for Total Moisture of Hazardous Waste Fuel by Karl Fischer Titrimetry
SIGNIFICANCE AND USE
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, 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 the 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.
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Designation:D5530–94 (Reapproved 2003)
Standard Test Method for
Total Moisture of Hazardous Waste Fuel by Karl Fischer
Titrimetry
This standard is issued under the fixed designation D 5530; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope into the titration flask. The total moisture in the sample is then
determined. The final total moisture percent is an average of
1.1 This test method covers the determination by Karl
two trials for each sample.
Fischer (KF) titrimetry of total moisture in solid or liquid
3.2 The contents of the tiration flask may be retained and
hazardous waste fuels used by industrial furnaces.
used for additional analyses. The contents of the titration flask
1.2 This test method has been used successfully on numer-
will need to be emptied and replaced with new solvent when
ous samples of hazardous waste fuel composed of solvents,
the capacity of the flask is nearly exhausted or when solid
spent oils, paints, and pigments. The expected range of
material affects the sensing by the electrode.
applicability for this test method is between 1.0 and 100 %;
however, this evaluation was limited to samples containing
4. Significance and Use
approximately 5 to 50 % water.
4.1 The determination of total moisture is important for
1.3 The values stated in SI units are to be regarded as the
assessing the quality of fuels. Water content will affect the
standard.
heating value of fuels directly and can contribute to instability
1.4 This standard does not purport to address all of the
in the operation of an industrial furnace. Additionally, high
safety concerns, if any, associated with its use. It is the
water contents can present material handling and storage
responsibility of the user of this standard to establish appro-
problems during winter months or in cold environments.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Interferences
2. Referenced Documents 5.1 Asmall number of oxidants such as ferric and chromate
2 salts can oxidize iodide and may produce artificially low
2.1 ASTM Standards:
results.
D 1193 Specifications for Reagent Water
5.2 Certain reductants oxidized by iodine such as mercap-
D 4017 Test Method forWater in Paints and Paint Materials
tans, thioacetate, thiosulfate, stannous chloride, sulfides, hyd-
by Karl Fischer Method
roquinone, and phenylenediamines can consume iodine and
E 691 Practice for Conducting an Interlaboratory Study to
may cause artificially high results. Basic materials such as
Determine the Precision of a Test Method
hydroxides, oxides, and inorganic carbonates may cause arti-
3. Summary of Test Method ficially high results by water-forming reactions.
5.3 Sometypesofsolidmaterialfoundinwaste-derivedfuel
3.1 An amount of solvent (see 7.3) sufficient to immerse the
may interfere with the electrode by blocking its contact with
electrode in the titration flask fully (see Note 1) is titrated to
the solvent. Depending on the nature of the solid material,
dryness as explained in 9.1, and the Karl Fischer reagent factor
artificially high or low results can occur.
is determined by titration of measured amounts of water. A
weighed portion of the sample is dissolved in KF solvent and
6. Apparatus
titrated with reagent to dryness. If solid material interferes (see
6.1 Karl Fischer Potentiometric Titration Unit, automated
5.3) with the electrode or does not dissolve sufficiently, an
or semi-automated, equipped with a magnetic vessel stirrer.
extraction using KF solvent is performed prior to introduction
The user must follow the manufacturer’s instructions for
installation and use.
This test method is under the jurisdiction of ASTM Committee D34 on Waste
NOTE 1—The Karl Fischer unit used for developing this test method
Management and is the direct responsibility of Subcommittee D34.01.06 on
was equipped with a twin platinum electrode, 25 to 80-mL capacity
Analytical Methods.
Current edition approved April 15, 1994. Published June 1994. titration flask, magnetic stirrer, electronic piston burette, adjustable delay
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
interval, LED display, visual and audible endpoint notification.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.2 Syringe, 100-µL capacity, with needle.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
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D5530–94 (2003)
6.3 Syringe, 1 to 5-mL capacity, without needle. 9.1.6 Dispense the syringe contents into the titration vessel
6.4 Analytical Balance, with minimum capacity of 160 g and replace the sample port stopper immediately. Reweigh the
and capable of weighing to 0.0001 g. syringe and record the water mass.
9.1.7 Titrate with reagent until the endpoint is reached.
7. Reagents and Materials
Record the titrant volume used.
9.1.8 The final value for F should be based on the mean of
7.1 Purity of Reagents—Reagent grade chemicals shall be
a minimum of three replicates.
used in all tests. Unless otherwise indicated, it is intended that
9.1.9 Calculation:
all reagents shall conform to the specifications of the Commit-
9.1.9.1 Calculate F by the following formula:
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
F ~mg/mL!5 water weight ~mg!/reagent volume ~mL! (1)
used, provided it is first ascertained that the reagent is of
9.1.9.2 The replicate values for F should have a relative
sufficiently high purity to permit its use without lessening the
standard deviation of not greater than 5 %.The standardization
accuracy of the determination.
should be repeated if a greater variance is determined.
7.2 Purity of Water— Unless otherwise indicated, refer-
ences to water shall be understood to mean reagent water as
10. Procedure
defined by Type II of Specification D 1193.
10.1 Bring the KF solvent to dryness by titrating with
7.3 Karl Fischer Solvent—The solvent system must be a
reagent to the endpoint. The endpoint is typically indicated
non-methanol formulation for the analysis of aldehydes and
visually or by an audible alarm, or both, depending on the
ketones and for general usage. The use of a strictly general
equipment manufacturer.
purpose solvent is not acceptable because of the potential of
10.2 Refill the burette with reagent.
obtaining artificially high results from water-forming reactions
10.3 Draw a portion of the sample into the 1 to 5-mL
by chemicals with active carbonyl groups.
syringe, and clean any residual sample material from the
7.4
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