ASTM D1364-22

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D1364 − 22
Standard Test Method for
Water in Volatile Solvents (Karl Fischer Reagent Titration
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 U.S. Department of Defense.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the determination of water in
D1500Test Method forASTM Color of Petroleum Products
volatile solvents and chemical intermediates used in paint,
(ASTM Color Scale)
varnish, lacquer, and related products.
E29Practice for Using Significant Digits in Test Data to
1.2 This test method is not applicable in the presence of
Determine Conformance with Specifications
mercaptans, peroxides, or appreciable quantities of aldehydes
3. Terminology
or amines.
3.1 Definitions of Terms Specific to This Standard:
1.3 For purposes of determining conformance of an ob-
3.1.1 instrumental end point, n—that point in the titration
served or a calculated value using this test method to relevant
whentwosmallplatinumelectrodes,uponwhichapotentialof
specifications, test result(s) shall be rounded off “to the nearest
20 to 50 mV has been impressed, are depolarized by the
unit” in the last right-hand digit used in expressing the
addition of 0.05 mLof Karl Fischer reagent (6 mg of H O per
specificationlimit,inaccordancewiththerounding-offmethod
mL), causing a change of current flow of 10 to 20 µA that
of Practice E29.
persists for at least 30 s.
1.4 The values stated in SI units are to be regarded as
NOTE1—Thisendpointissometimesincorrectlycalledthe“deadstop”
which is the reverse of the above.
standard. No other units of measurement are included in this
standard. 3.1.2 color end point, n—during the titration, the solution
first turns yellow, then later deepens towards the end of the
1.5 For hazard information and guidance, see the supplier’s
titration; the end point is indicated by the change from yellow
Material Safety Data sheet.
to orange-red which is quite sharp and easily repeated; the
orange-red color must persist for at least 30 s in order to
1.6 This standard does not purport to address all of the
indicate an end point.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
NOTE 2—View the color by transmitted daylight or by transmitted light
priate safety, health, and environmental practices and deter- from an artificial daylight lamp, such as the one that complies with the
specifications given in Test Method D1500.
mine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accor-
4. Summary of Test Method
dance with internationally recognized principles on standard-
4.1 This test method is based essentially upon the reduction
ization established in the Decision on Principles for the
of iodine by sulfur dioxide in the presence of water. This
Development of International Standards, Guides and Recom-
reaction can be used quantitatively only when pyridine and an
mendations issued by the World Trade Organization Technical
alcohol are present to react with the sulfur trioxide and
Barriers to Trade (TBT) Committee.
hydriodic acid produced according to the following reactions:
H O1I 1SO 13C H N→2C H N·HI1C H N·SO (1)
2 2 2 5 5 5 5 5 5 3
This test method is under the jurisdiction of ASTM Committee D01 on Paint C H N·SO 1ROH→C H N·HSO R
5 5 3 5 5 4
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
Current edition approved Jan. 1, 2022. Published January 2022. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
approved in 1955. Last previous edition approved in 2012 as D1364–02 (2012) contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
which was withdrawn January 2021 and reinstated in January 2022. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D1364-22. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1364 − 22
mixture.Itisdesirabletohaveameansforcoolingthetitration
vessel to ice temperature.
6.2 Instrument Electrodes—Platinum with a surface equiva-
lent to two No. 26 wires 5 mm long. The wires should be 3 to
8 mm apart and so inserted in the vessel that 25 mL of liquid
will cover them.
6.3 Instrument Depolarization Indicator, having an internal
resistance of less than 5000Ω and consisting of a means of
impressing and showing a voltage of 20 to 50 mV across the
electrodes and capable of indicating a current flow of 10 to
20µAby means of a galvanometer or radiotuning eye circuit.
6.4 Buret Assembly for Karl Fischer reagent, consisting of a
25 or 50-mL buret connected by means of glass (not rubber)
connectors to a source of reagent; several types of automatic
dispensing burets may be used. Since the reagent loses
strengthwhenexposedtomoistair,allventsmustbeprotected
against atmospheric moisture by adequate drying tubes con-
taining indicating calcium sulfate drying agent. All stopcocks
andjointsshouldbelubricatedwithalubricantnotparticularly
reactive with the reagent.
NOTE 1—All dimensions in millimetres.
6.5 Weighing Bottle, of the Lunge or Grethen Type, or
FIG. 1 Titration Flask Assembly
equivalent.
7. Reagents
4.2 To determine water, Karl Fischer reagent (a solution of
iodine, pyridine, and sulfur dioxide, in the molar ratio of
7.1 Purity of Reagents—Reagent grade chemicals shall be
1+10+3) dissolved in anhydrous 2-methoxyethanol is added
used in all tests. Unless otherwise indicated, it is intended that
to a solution of the sample in anhydrous pyridine-ethylene
all reagents shall conform to the specifications of the Commit-
glycol (1+4) until all water present has been consumed. This
tee onAnalytical Reagents of theAmerican Chemical Society,
is evidenced by the persistence of the orange-red end-point
where such specifications are available. Other grades may be
color; or alternatively by an indication on a galvanometer or
used, provided it is first ascertained that the reagent is of
similarcurrent-indicatingdevicewhichrecordsthedepolariza-
sufficiently high purity to permit its use without decreasing the
tion of a pair of noble-metal electrodes. The reagent is
accuracy of the determination.
standardized by titration of water.
7.1.1 Karl Fischer Reagent (equivalent to 6 mg of H O per
mL) —For each liter of solution, dissolve 133 61gofI in
5. Significance and Use
425 6 2 mLof anhydrous (less than 0.1% H O) pyridine in a
dryglass-stopperedbottle.Add425 62mLofanhydrous(less
5.1 Volatile solvents are used in a variety of chemical
than 0.1% H O) 2-methoxyethanol. Cool to below 4°C in an
processes which may be affected by water. Therefore, this test
method provides a test procedure for assessing compliance
with a specification.
The sole source of supply of instrument depolarization indicator known to the
committee at this time is Fisher Scientific Co., www.fishersci.com. If you are aware
6. Apparatus
of alternative suppliers, please provide this information to ASTM International
6.1 Titration Vessel—For color end point titrations, use a Headquarters.Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend.
100 or 250-mLvolumetric flask, which need not be calibrated;
The sole source of supply of automatic dispensing burets, No. J-821, known to
a 250-mLflask fitted with interchangeable electrodes (Fig. 1)
the committee at this time is Scientifice glassApparatus Co., Bloomfield NJ. If you
may also be used for the instrumental end point and is
are aware of alternative suppliers, please provide this information to ASTM
International Headquarters. Your comments will receive careful consideration at a
particularly suitable for titrations at ice temperatures. For
meeting of the responsible technical committee, which you may attend. These
permanently mounted assemblies, the vessel should have a
specifically designed burets present the minimum contact of reagent with stopcock
capacity about equal to that of a 300-mLtall-form beaker; and
lubricant.
be provided with a tight-fitting closure to protect the sample
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
and reagent from atmospheric moisture, a stirrer, and a means
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
of adding sample and reagents and removing spent reaction
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
copeial Convention, Inc. (USPC), Rockville, MD.
3 7
The sole source of supply of flasks known to the committee at this time is the Karl Fischer Reagent is available from various laboratory suppliers. Pyridine-
Rankin Glass Blowing Co., 3920 Franklin Canyon Road, Martinez, CA. If you are freeadaptationsareavailableandmaybeusedifprecisioncanbeestablished.Ifyou
aware of alternative suppliers, please provide this information to ASTM Interna- are aware of alter
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