ASTM D1744-13
(Test Method)Standard Test Method for Determination of Water in Liquid Petroleum Products by Karl Fischer Reagent (Withdrawn 2016)
Standard Test Method for Determination of Water in Liquid Petroleum Products by Karl Fischer Reagent (Withdrawn 2016)
SIGNIFICANCE AND USE
4.1 Knowledge of the water content of petroleum products can be useful to predict quality and performance characteristics of the product.
SCOPE
1.1 This test method covers the determination of water in the concentration from 50 to 1000 mg/kg in liquid petroleum products.
1.2 Values stated in SI units are to be regarded as the standard. Inch-pound units are provided for information only.
1.3 This standard does not purport to address all of the safety problems, 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 Section 7.
WITHDRAWN RATIONALE
This test method covers the determination of water in the concentration from 50 to 1000 mg/kg in liquid petroleum products.
Formerly under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, this test method was withdrawn in April 2016 because it is out of date and has not been revised.
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D1744 − 13 AnAmerican National Standard
Standard Test Method for
Determination of Water in Liquid Petroleum Products by
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Karl Fischer Reagent
This standard is issued under the fixed designation D1744; 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 react with iodine, interfere. One part per million of sulfur as
mercaptan causes an error in the titration, equivalent to
1.1 This test method covers the determination of water in
approximately 0.2 mg/kg of water.
the concentration from 50 to 1000 mg/kg in liquid petroleum
products.
6. Apparatus
1.2 Values stated in SI units are to be regarded as the
6.1 Assemble the apparatus as described in the Annex A1.
standard. Inch-pound units are provided for information only.
(See Note 1.)
1.3 This standard does not purport to address all of the
NOTE 1—Any apparatus that will give equal or better precision is
safety problems, if any, associated with its use. It is the
acceptable.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
7. Reagents and Materials
bility of regulatory limitations prior to use. For specific
7.1 Purity of Reagents—Reagent grade chemicals shall be
precautionary statements see Section 7.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
2. Referenced Documents
tee onAnalytical Reagents of theAmerican Chemical Society,
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2.1 ASTM Standards:
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where such specifications are available. Other grades can be
D4057Practice for Manual Sampling of Petroleum and
used, provided it is first ascertained that the reagent is of
Petroleum Products
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
3. Summary of Test Method
7.2 Purity of Water—Unless otherwise indicated, references
3.1 The material to be analyzed is titrated with standard
towatershallbeunderstoodtomeandistilledwaterorwaterof
Karl Fischer reagent to an electrometric end point.
equal purity. The solvents used must have low-water content,
4. Significance and Use
for example, less than 500 mg/kg mass.
4.1 Knowledge of the water content of petroleum products
7.3 Karl Fischer Reagent, Solution (Note 2), Stock—
canbeusefultopredictqualityandperformancecharacteristics
(Warning—Toxic.) For each litre of solution, dissolve 85 6 1
of the product.
gofiodinein270 62mLofpyridineinadry,glass-stoppered
bottle. Add 670 6 2 mL of methanol (99.9%) (Note 3). Cool
5. Interferences
the mixture in an ice bath to below 3.9°C. Bubble gaseous
5.1 Free alkali, oxidizing and reducing agents, mercaptans,
sulfur dioxide (SO)(Note 4) through concentrated sulfuric
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certain basic nitrogenous substances, or other materials that
acid (H SO , rel dens 1.84) (see warning information below)
2 4
into the cooled mixture. Continue the addition of SO until the
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This test method is under the jurisdiction of ASTM Committee D02 on
volume is increased 50 6 1 mL.Alternatively, add 50 61mL
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
of freshly drawn liquid SO in small increments to the
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Subcommittee D02.02 on Hydrocarbon Measurement for Custody Transfer (Joint
precooled mixture in an ice bath. Mix well and set aside for at
ASTM-API).
Current edition approved Dec. 1, 2013. Published December 2013. Originally
approved in 1960. Last previous edition approved in 1992 as D1744–92, which
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was withdrawn in January 2000 and reinstated in December 2013. DOI: 10.1520/ Reagent Chemicals, American Chemical Society Specifications, American
D1743-13. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
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D1744 − 13
least 12 h before using. (Warning—Poison. Corrosive. Strong 9.1.5 Fromataredweighingbottle,bymeansofaclean,dry
oxidizer. Conta
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