ASTM D3401-97(2006)
(Test Method)Standard Test Methods for Water in Halogenated Organic Solvents and Their Admixtures
Standard Test Methods for Water in Halogenated Organic Solvents and Their Admixtures
SIGNIFICANCE AND USE
High water concentrations can have a detrimental effect on many uses of halogenated solvents.
4.1.1 Water can cause corrosion and spotting when solvents are used for metal cleaning.
4.1.2 Water can reduce the shelf life of aerosol formulations.
4.1.3 Water can inhibit desired reactions when solvents are used in formulations.
SCOPE
1.1 These test methods describe the use of the Karl Fischer (KF) titration for determination of water in halogenated organic solvents and mixtures thereof. Water concentrations from 2 to 1000 ppm can be determined in these solvents. Two test methods are covered as follows:
1.1.1 Test Method A, Water Determination Using a Coulometric KF TitratorThe coulometric test method is known for its high degree of sensitivity (typically 10 g H 2O) and should be the test method of choice if water concentrations are typically below 50 ppm or if only small amounts of sample are available for water determinations. This test method requires the use of equipment specifically designed for coulometric titrations.
1.1.2 Test Method B, Water Determination Using a Volumetric KF TitratorThe volumetric test method is a more traditional approach to KF water determinations. Although titrators are specifically designed for KF volumetric determinations, many automatic titrators on the market can be adapted to perform KF titrations.
1.2 Either of these test methods can be used to determine typical water concentrations (15 to 500 ppm) found in halogenated solvents.
1.3 These test methods recommend the use of commercially available Karl Fischer titrators and reagents.
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. For specific precautionary statements, see Sections 11 and 15.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D3401–97(Reapproved 2006)
Standard Test Methods for
Water in Halogenated Organic Solvents and Their
1
Admixtures
This standard is issued under the fixed designation D3401; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 2. Referenced Documents
2
1.1 These test methods describe the use of the Karl Fischer 2.1 ASTM Standards:
(KF) titration for determination of water in halogenated or- E203 Test Method forWater UsingVolumetric Karl Fischer
ganicsolventsandmixturesthereof.Waterconcentrationsfrom Titration
2 to 1000 ppm can be determined in these solvents. Two test
3. Summary of Test Methods
methods are covered as follows:
3.1 In the Karl Fischer reaction, water will react with iodine
1.1.1 Test Method A, Water Determination Using a Coulo-
metricKFTitrator—The coulometric test method is known for in the presence of sulfur dioxide, alcohol, and an organic base
according to the following equation:
its high degree of sensitivity (typically < 10 µg H O) and
2
should be the test method of choice if water concentrations are
H O 1 I 1 SO 1 CH OH 1 3RN→ ~RNH!SO CH 1 2~RNH!I
2 2 2 3 4 3
typically below 50 ppm or if only small amounts of sample are
(1)
available for water determinations. This test method requires
the use of equipment specifically designed for coulometric
where RN = organic base.
titrations.
3.2 When the volumetric titration test method is used for
1.1.2 TestMethodB,WaterDeterminationUsingaVolumet-
this determination, the halogenated sample is added to a KF
ric KF Titrator—The volumetric test method is a more
solvent that usually consists of sulfur dioxide and an amine
traditional approach to KF water determinations. Although
dissolved in anhydrous methanol. This solution is titrated with
titrators are specifically designed for KF volumetric determi-
an anhydrous solvent containing iodine. The iodine titrant is
nations, many automatic titrators on the market can be adapted
first standardized by titrating a known amount of water.
to perform KF titrations.
3.3 In the coulometric titration test method, the sample is
1.2 Either of these test methods can be used to determine
injected into an electrolytic cell where the iodine required for
typical water concentrations (15 to 500 ppm) found in haloge-
the reaction with water is produced by anodic oxidation of
nated solvents.
iodide. With this technique, no standardization of reagents is
1.3 These test methods recommend the use of commercially
required.
available Karl Fischer titrators and reagents.
3.4 In both test methods, the end point is determined
1.4 This standard does not purport to address all of the
amperometrically with a platinum electrode that senses a sharp
safety concerns, if any, associated with its use. It is the
change in cell resistance when the iodine has reacted with all
responsibility of the user of this standard to establish appro-
of the water in the sample.
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use. For specific
precautionary statements, see Sections 11 and 15.
4.1 High water concentrations can have a detrimental effect
on many uses of halogenated solvents.
1
These test methods are under the jurisdiction of ASTM Committee D26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and are the direct
2
responsibility of Subcommittee D26.04 on Test Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2006. Published June 2006. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1975. Last previous edition approved in 2001 as D3401 – 97(2001). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D3401-97R06. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D3401–97 (2006)
equipment. Pyridine-free reagents are said to be less toxic, less odorous,
4.1.1 Water can cause corrosion and spotting when solvents
and more stable than pyridine types.
are used for metal cleaning.
4.1.2 Water can reduce the shelf life of aerosol formula-
8. Sampling
tions.
4.1.3 Water can inhibit desired reactions when solvents are 8.1 Since halogenated solvents normally contain low con-
centrations of water, care must be taken to eliminate the
used in formulations.
introduction of wate
...
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