ASTM D5530-94(1998)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5530 – 94 (Reapproved 1998)
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 determined. The final total moisture percent is an average of
two trials for each sample.
1.1 This test method covers the determination by Karl
3.2 The contents of the tiration flask may be retained and
Fischer (KF) titrimetry of total moisture in solid or liquid
used for additional analyses. The contents of the titration flask
hazardous waste fuels used by industrial furnaces.
will need to be emptied and replaced with new solvent when
1.2 This test method has been used successfully on numer-
the capacity of the flask is nearly exhausted or when solid
ous samples of hazardous waste fuel composed of solvents,
material affects the sensing by the electrode.
spent oils, paints, and pigments. The expected range of
applicability for this test method is between 1.0 and 100 %;
4. Significance and Use
however, this evaluation was limited to samples containing
4.1 The determination of total moisture is important for
approximately 5 to 50 % water.
assessing the quality of fuels. Water content will affect the
1.3 The values stated in SI units are to be regarded as the
heating value of fuels directly and can contribute to instability
standard.
in the operation of an industrial furnace. Additionally, high
1.4 This standard does not purport to address all of the
water contents can present material handling and storage
safety concerns, if any, associated with its use. It is the
problems during winter months or in cold environments.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Interferences
bility of regulatory limitations prior to use.
5.1 A small number of oxidants such as ferric and chromate
salts can oxidize iodide and may produce artificially low
2. Referenced Documents
results.
2.1 ASTM Standards:
2 5.2 Certain reductants oxidized by iodine such as mercap-
D 1193 Specifications for Reagent Water
tans, thioacetate, thiosulfate, stannous chloride, sulfides, hyd-
D 4017 Test Method for Water in Paints and Paint Materials
3 roquinone, and phenylenediamines can consume iodine and
by Karl Fischer Method
may cause artificially high results. Basic materials such as
E 691 Practice for Conducting an Interlaboratory Study to
4 hydroxides, oxides, and inorganic carbonates may cause arti-
Determine the Precision of a Test Method
ficially high results by water-forming reactions.
3. Summary of Test Method 5.3 Some types of solid material found in waste-derived fuel
may interfere with the electrode by blocking its contact with
3.1 An amount of solvent (see 7.3) sufficient to immerse the
the solvent. Depending on the nature of the solid material,
electrode in the titration flask fully (see Note 1) is titrated to
artificially high or low results can occur.
dryness as explained in 9.1, and the Karl Fischer reagent factor
is determined by titration of measured amounts of water. A
6. Apparatus
weighed portion of the sample is dissolved in KF solvent and
6.1 Karl Fischer Potentiometric Titration Unit, automated
titrated with reagent to dryness. If solid material interferes (see
or semi-automated, equipped with a magnetic vessel stirrer.
5.3) with the electrode or does not dissolve sufficiently, an
The user must follow the manufacturer’s instructions for
extraction using KF solvent is performed prior to introduction
installation and use.
into the titration flask. The total moisture in the sample is then
NOTE 1—The Karl Fischer unit used for developing this test method
was equipped with a twin platinum electrode, 25 to 80-mL capacity
titration flask, magnetic stirrer, electronic piston burette, adjustable delay
This test method is under the jurisdiction of ASTM Committee D34 on Waste
interval, LED display, visual and audible endpoint notification.
Management and is the direct responsibility of Subcommittee D34.01.06 on
Analytical Methods.
6.2 Syringe, 100-μL capacity, with needle.
Current edition approved April 15, 1994. Published June 1994.
Annual Book of ASTM Standards, Vol 11.01. 6.3 Syringe, 1 to 5-mL capacity, without needle.
Annual Book of ASTM Standards, Vol 06.01.
6.4 Analytical Balance, with minimum capacity of 160 g
Annual Book of ASTM Standards, Vol 14.02.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5530
and capable of weighing to 0.0001 g. 9.1.7 Titrate with reagent until the endpoint is reached.
Record the titrant volume used.
7. Reagents and Materials
9.1.8 The final value for F should be based on the mean of
a minimum of three replicates.
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that 9.1.9 Calculation:
9.1.9.1 Calculate F by the following formula:
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
F ~mg/mL!5 water weight ~mg!/reagent volume ~mL! (1)
where such specifications are available. Other grades may be
9.1.9.2 The replicate values for F should have a relative
used, provided it is first ascertained that the reagent is of
standard deviation of not greater than 5 %. The standardization
sufficiently high purity to permit its use without lessening the
should be repeated if a greater variance is determined.
accuracy of the determination.
7.2 Purity of Water— Unless otherwise indicated, refer-
10. Procedure
ences to water shall be understood to mean reagent water as
10.1 Bring the KF solvent to dryness by titrating with
defined by Type II of Specification D 1193.
reagent to the endpoint. The endpoint is typically indicated
7.3 Karl Fischer Solvent—The solvent system must be a
visually or by an audible alarm, or both, depending on the
non-methanol formulation for the analysis of aldehydes and
equipment manufacturer.
ketones and for general usage. The use of a strictly general
10.2 Refill the burette with reagent.
purpose solvent is not acceptable because of the potential of
10.3 Draw a portion of the sample into the 1 to 5-mL
obtaining artificially high results from water-forming reactions
syringe, and clean any residual sample material from the
by chemicals with active carbonyl groups.
syringe tip. If the sample contains a large amount of solids or
7.4 Karl Fischer Reagent—The reagent should have a
its viscosity is such that it cannot be drawn into the syringe
standard titer value of 5 mg H O/mL reagent and be listed as
ea
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