ASTM D5530-94(2009)
(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 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.
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Standards Content (Sample)
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Designation: D5530 − 94(Reapproved 2009)
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 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, paints, and pigments. The expected range of
3.2 The contents of the tiration flask may be retained and
applicability for this test method is between 1.0 and 100 %;
used for additional analyses. The contents of the titration flask
however, this evaluation was limited to samples containing
will need to be emptied and replaced with new solvent when
approximately 5 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
2.1 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,
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 Feb. 1, 2009. Published March 2009. Originally
6. Apparatus
approved in 1994. Last previous editio approved in 2003 as D5530-94(2003). DOI:
10.1520/D5530-94R09.
6.1 Karl Fischer Potentiometric Titration Unit, automated
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 service@astm.org. 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.
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D5530 − 94 (2009)
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 electrode, 25 to 80-mL capacity
reagent to the endpoint. The endpoint is typically indicated by
titration flask, magnetic stirrer, electronic piston burette, adjustable delay
a visual or audible alarm, or both, depending on the equipment
interval, LED display, visual and audible endpoint notification.
manufacturer.
6.2 Syringe, 100-µL capacity, with needle.
9.1.4 Refill the burette with reagent.
6.3 Syringe, 1 to 5-mL capacity, without needle. 9.1.5 Fill the 100-µL syringe with approximately 10 µL of
water and weigh to the nearest 0.0001 g.
6.4 Analytical Balance, with minimum capacity of 160 g
9.1.6 Dispense the syringe contents into the titration vessel
and capable of weighing to 0.0001 g.
and replace the sample port stopper immediately. Reweigh the
syringe and record the water mass.
7. Reagents and Materials
9.1.7 Titrate with reagent until the endpoint is reached.
7.1 Purity of Reagents—Reagent grade chemicals shall be
Record the titrant volume used.
used in all tests. Unless otherwise indicated, it is intended that
9.1.8 The final value for F should be based on the mean of
all reagents shall conform to the specifications of the Commit-
a minimum of three replicates.
tee onAnalytical Reagents of theAmerican Chemical Society,
9.1.9 Calculation:
where such specifications are available. Other grades may be
9.1.9.1 Calculate F by the following formula:
used, provided it is first ascertained that the reagent is of
F ~mg/mL! 5 water weight ~mg!/reagent volume ~mL! (1)
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
9.1.9.2 The replicate values for F should have a relative
standard deviation of not greater than 5 %.The standardization
7.2 Purity of Water—Unless otherwise indicated, references
should be repeated if a greater variance is determined.
to water shall be understood to mean reagent water as defined
by Type II of Specification D1193.
10. Procedure
7.3 Karl Fischer Solvent—The solvent system must be a
10.1 Bring the KF solvent to dryness by titrating with
non-methanol formulation for the analysis of aldehydes and
reagent to the endpoint. The endpoint is typically indicated
ketones and for general usage. The use of a strictly general
visually or by an audible alarm, or both, depen
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