ASTM D1364-02(2007)
(Test Method)Standard Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
Standard Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
SIGNIFICANCE AND USE
Volatile solvents are used in a variety of chemical processes which may be affected by water. Therefore, this test method provides a test procedure for assessing compliance with a specification.
SCOPE
1.1 This test method covers the determination of water in volatile solvents and chemical intermediates used in paint, varnish, lacquer, and related products.
1.2 This test method is not applicable in the presence of mercaptans, peroxides, or appreciable quantities of aldehydes or amines.
1.3 For purposes of determining conformance of an observed or a calculated value using this test method to relevant specifications, test result(s) shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.
1.5 For hazard information and guidance, see the supplier's Material Safety Data sheet.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D1364 − 02 (Reapproved 2007)
StandardTest Method for
Water in Volatile Solvents (Karl Fischer Reagent Titration
1
Method)
This standard is issued under the fixed designation D1364; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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* 3. Terminology
1.1 This test method covers the determination of water in
3.1 Definitions of Terms Specific to This Standard:
volatile solvents and chemical intermediates used in paint,
3.1.1 instrumental end point, n—that point in the titration
varnish, lacquer, and related products.
whentwosmallplatinumelectrodes,uponwhichapotentialof
20 to 50 mV has been impressed, are depolarized by the
1.2 This test method is not applicable in the presence of
addition of 0.05 mLof Karl Fischer reagent (6 mg of H O per
mercaptans, peroxides, or appreciable quantities of aldehydes
2
mL), causing a change of current flow of 10 to 20 µA that
or amines.
persists for at least 30 s.
1.3 For purposes of determining conformance of an ob-
served or a calculated value using this test method to relevant
NOTE1—Thisendpointissometimesincorrectlycalledthe“deadstop”
specifications, test result(s) shall be rounded off “to the nearest which is the reverse of the above.
unit” in the last right-hand digit used in expressing the
3.1.2 color end point, n—During the titration, the solution
specificationlimit,inaccordancewiththerounding-offmethod
first turns yellow, then later deepens towards the end of the
of Practice E29.
titration; the end point is indicated by the change from yellow
1.4 The values stated in SI units are to be regarded as to orange-red which is quite sharp and easily repeated. The
orange-red color must persist for at least 30 s in order to
standard. No other units of measurement are included in this
standard. indicate an end point.
1.5 This standard does not purport to address all of the
NOTE 2—View the color by transmitted daylight or by transmitted light
safety concerns, if any, associated with its use. It is the
from an artificial daylight lamp, such as the one that complies with the
responsibility of the user of this standard to establish appro- specifications given in Test Method D1500.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 4. Summary of Test Method
1.6 For hazard information and guidance, see the supplier’s
4.1 This test method is based essentially upon the reduction
Material Safety Data sheet.
of iodine by sulfur dioxide in the presence of water. This
reaction can be used quantitatively only when pyridine and an
2. Referenced Documents
alcohol are present to react with the sulfur trioxide and
2
2.1 ASTM Standards:
hydriodic acid produced according to the following reactions:
D1500Test Method forASTM Color of Petroleum Products
H O1I 1SO 13C H N→2C H N·HI1C H N·SO (1)
2 2 2 5 5 5 5 5 5 3
(ASTM Color Scale)
E29Practice for Using Significant Digits in Test Data to
C H N·SO 1ROH→C H N·HSO R
5 5 3 5 5 4
Determine Conformance with Specifications
4.2 To determine water, Karl Fischer reagent (a solution of
iodine, pyridine, and sulfur dioxide, in the molar ratio of
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
1+10+3) dissolved in anhydrous 2-methoxyethanol is added
and Related Coatings, Materials, andApplications and is the direct responsibility of
to a solution of the sample in anhydrous pyridine-ethylene
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
glycol (1+4) until all water present has been consumed. This
Current edition approved June 1, 2007. Published June 2007. Originally
is evidenced by the persistence of the orange-red end-point
approved in 1955. Last previous edition approved in 2002 as D1364–02. DOI:
10.1520/D1364-02R07.
color; or alternatively by an indication on a galvanometer or
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
similarcurrent-indicatingdevicewhichrecordsthedepolariza-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
tion of a pair of noble-metal electrodes. The reagent is
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. standardized by titration of water.
*A Summary of Changes section appears at the end of this standard
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D1364 − 02 (Reapproved 2007)
electrodes and capable
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