ASTM D1364-02

Standard Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)

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 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

• Status: Historical
• Publication Date: 09-Dec-2002
• ICS: 87.060.30 - Solvents
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.35 - Solvents, Plasticizers, and Chemical Intermediates

Relations

• Replaces: ASTM D1364-95(1999) - Standard Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
• Effective Date: 10-Dec-2002
• Replaced By: ASTM D1364-02(2007) - Standard Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
• Effective Date: 01-Jun-2007
• Referred By: ASTM D3548-09(2023) - Standard Specification for Ethyl Acrylate
• Effective Date: 10-Dec-2002
• Referred By: ASTM D4360-11(2019) - Standard Specification for Methyl <emph type="bdit">n</emph>-Amyl Ketone
• Effective Date: 10-Dec-2002
• Referred By: ASTM D3329-03(2023) - Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography
• Effective Date: 10-Dec-2002
• Referred By: ASTM D268-22 - Standard Guide for Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material
• Effective Date: 10-Dec-2002
• Referred By: ASTM D2917-07(2021) - Standard Specification for Methyl Isoamyl Ketone
• Effective Date: 10-Dec-2002
• Referred By: ASTM D3622-11(2019) - Standard Specification for 1-Propanol (<emph type="bdit">n</emph>-Propyl Alcohol)
• Effective Date: 10-Dec-2002
• Referred By: ASTM E203-23 - Standard Test Method for Water Using Volumetric Karl Fischer Titration
• Effective Date: 10-Dec-2002
• Referred By: ASTM D3130-11(2019) - Standard Specification for <emph type="bdit">n</emph>-Propyl Acetate (96&#x2009;% Grade)
• Effective Date: 10-Dec-2002
• Referred By: ASTM D2634-07(2021) - Standard Specification for Methyl Amyl Acetate (95 % Grade)
• Effective Date: 10-Dec-2002
• Referred By: ASTM D1718-09(2023) - Standard Specification for Isobutyl Acetate (95 % Grade)
• Effective Date: 10-Dec-2002
• Referred By: ASTM D4307-17(2021) - Standard Practice for Preparation of Liquid Blends for Use as Analytical Standards
• Effective Date: 10-Dec-2002
• Referred By: ASTM D4615-22 - Standard Specification for <emph type="ital">n</emph>-Butyl Acetate (All Grades)
• Effective Date: 10-Dec-2002
• Referred By: ASTM D329-07(2021) - Standard Specification for Acetone
• Effective Date: 10-Dec-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please
contact ASTM International (www.astm.org) for the latest information.
Designation:D1364–02
Standard Test Method for
Water in Volatile Solvents (Karl Fischer Reagent Titration
1
Method)
This standard is issued under the fixed designation D 1364; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* addition of 0.05 mL of Karl Fischer reagent (6 mg of H O per
2
mL), causing a change of current flow of 10 to 20 µA that
1.1 This test method covers the determination of water in
persists for at least 30 s.
volatile solvents and chemical intermediates used in paint,
varnish, lacquer, and related products.
NOTE 1—Thisendpointissometimesincorrectlycalledthe“deadstop”
1.2 This test method is not applicable in the presence of which is the reverse of the above.
mercaptans, peroxides, or appreciable quantities of aldehydes
3.1.2 color end point—During the titration, the solution first
or amines.
turnsyellow,thenlaterdeepenstowardstheendofthetitration;
1.3 For purposes of determining conformance of an ob-
the end point is indicated by the change from yellow to
served or a calculated value using this test method to relevant
orange-red which is quite sharp and easily repeated. The
specifications, test result(s) shall be rounded off “to the nearest
orange-red color must persist for at least 30 s in order to
unit” in the last right-hand digit used in expressing the
indicate an end point.
specification limit, in accordance with the rounding-off method
NOTE 2—View the color by transmitted daylight or by transmitted light
of Practice E 29.
from an artificial daylight lamp, such as the one that complies with the
1.4 This standard does not purport to address all of the
specifications given in Test Method D 1500.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 This test method is based essentially upon the reduction
bility of regulatory limitations prior to use.
of iodine by sulfur dioxide in the presence of water. This
1.5 For hazard information and guidance, see the supplier’s
reaction can be used quantitatively only when pyridine and an
Material Safety Data sheet.
alcohol are present to react with the sulfur trioxide and
hydriodic acid produced according to the following reactions:
2. Referenced Documents
H O 1 I 1 SO 1 3C H N→ 2C H N·HI 1 C H N·SO
2 2 2 5 5 5 5 5 5 3
2.1 ASTM Standards:
C H N·SO 1 ROH→ C H N·HSO R
5 5 3 5 5 4
D 1500 Test Method for ASTM Color of Petroleum Prod-
(1)
2
ucts (ASTM Color Scale)
4.2 To determine water, Karl Fischer reagent (a solution of
E29 Practice for Using Significant Digits in Test Data to
3
iodine, pyridine, and sulfur dioxide, in the molar ratio of
Determine Conformance with Specifications
1 + 10 + 3) dissolved in anhydrous 2-methoxyethanol is added
3. Terminology
to a solution of the sample in anhydrous pyridine-ethylene
glycol (1 + 4) until all water present has been consumed. This
3.1 Definitions of Terms Specific to This Standard:
is evidenced by the persistence of the orange-red end-point
3.1.1 instrumental end point—that point in the titration
color; or alternatively by an indication on a galvanometer or
when two small platinum electrodes, upon which a potential of
similar current-indicating device which records the depolariza-
20 to 50 mV has been impressed, are depolarized by the
tion of a pair of noble-metal electrodes. The reagent is
standardized by titration of water.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
Current edition approved Dec. 10, 2002. Published February 2003. Originally
approved in 1955. Last previous edition approved in 1999 as D 1364 – 95 (1999).
2
Annual Book of ASTM Standards, Vol 05.01.
3
Annual Book of ASTM Standards, Vol 14.02.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Please
contact ASTM International (www.astm.org) for the latest information.
D1364–02
electrodes and capable of indicating a current flow of 10 to 20
5
µA by means of a galvanometer or radiotuning eye circuit.
6.4 BuretAssembly f
...