ASTM D6304-04e1
(Test Method)Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
SCOPE
1.1 This test method covers the direct determination of water in the range of 10 to 25 000 mg/kg entrained water in petroleum products and hydrocarbons using automated instrumentation. This test method also covers the indirect analysis of water thermally removed from samples and swept with dry inert gas into the Karl Fischer titration cell. Mercaptan, sulfide (S- or H2S), sulfur, and other compounds are known to interfere with this test method (see Section 5).
1.2 This test method is intended for use with commercially available coulometric Karl Fischer reagents and for the determination of water in additives, lube oils, base oils, automatic transmission fluids, hydrocarbon solvents, and other petroleum products. By proper choice of the sample size, this test method may be used for the determination of water from mg/kg to percent level concentrations.
1.3 Values stated in SI units are to be regarded as the standard.
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.
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An American National Standard
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Designation: D 6304 – 04
Standard Test Method for
Determination of Water in Petroleum Products, Lubricating
1
Oils, and Additives by Coulometric Karl Fischer Titration
This standard is issued under the fixed designation D 6304; 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.
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e NOTE—Corrected 6.2.2 editorially in April 2004.
1. Scope* D 4052 Test Method for Density and Relative Density of
Liquids by Digital Density Meter
1.1 This test method covers the direct determination of
D 4057 Practice for Manual Sampling of Petroleum and
water in the range of 10 to 25 000 mg/kg entrained water in
Petroleum Products
petroleum products and hydrocarbons using automated instru-
D 4177 Practice for Automatic Sampling of Petroleum and
mentation. This test method also covers the indirect analysis of
Petroleum Products
water thermally removed from samples and swept with dry
D 5854 Practice for Mixing and Handling of Liquid
inert gas into the Karl Fischer titration cell. Mercaptan, sulfide
−
Samples of Petroleum and Petroleum Products
(S or H S), sulfur, and other compounds are known to
2
E 203 Test Method for Water Using Volumetric Karl Fischer
interfere with this test method (see Section 5).
Titration
1.2 This test method is intended for use with commercially
available coulometric Karl Fischer reagents and for the deter-
3. Summary of Test Method
mination of water in additives, lube oils, base oils, automatic
3.1 An aliquot is injected into the titration vessel of a
transmission fluids, hydrocarbon solvents, and other petroleum
coulometric Karl Fischer apparatus in which iodine for the Karl
products. By proper choice of the sample size, this test method
Fisher reaction is generated coulometrically at the anode.
may be used for the determination of water from mg/kg to
When all of the water has been titrated, excess iodine is
percent level concentrations.
detected by an electrometric end point detector and the titration
1.3 Values stated in SI units are to be regarded as the
is terminated. Based on the stoichiometry of the reaction, 1 mol
standard.
of iodine reacts with 1 mol of water; thus, the quantity of water
1.4 This standard does not purport to address all of the
is proportional to the total integrated current according to
safety concerns, if any, associated with its use. It is the
Faraday’s Law.
responsibility of the user of this standard to establish appro-
3.2 The sample injection can be done either by mass or
priate safety and health practices and determine the applica-
volume.
bility of regulatory limitations prior to use.
3.3 The viscous samples can be analyzed by using a water
2. Referenced Documents vaporizer accessory that heats the sample in the evaporation
2 chamber, and the vaporized water is carried into the Karl
2.1 ASTM Standards:
Fischer titration cell by a dry inert carrier gas.
D 1193 Specification for Reagent Water
D 1298 Test Method for Density, Relative Density (Specific
4. Significance and Use
Gravity), or API Gravity of Crude Petroleum and Liquid
4.1 A knowledge of the water content of lubricating oils,
Petroleum Products by Hydrometer Method
additives, and similar products is important in the manufactur-
ing, purchase, sale, or transfer of such petroleum products to
1
This test method is under the jurisdiction of ASTM Committee D02 on help in predicting their quality and performance characteristics.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
4.2 For lubricating oils, the presence of moisture could lead
D02.02 on Static Petroleum Measurement.
to premature corrosion and wear, an increase in the debris load
Current edition approved Feb. 1, 2004. Published March 2004. Originally
resulting in diminished lubrication and premature plugging of
approved in 1998. Last previous edition approved in 2003 as D 6304–03.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
filters, an impedance in the effect of additives, and undesirable
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
support of deleterious bacterial growth.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
*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.
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D6304–04
TABLE 1 Test Sample Size Based on Expected Water Content
accurate to the nearest 10 μL; 1 mL accurate to the nearest
Exp
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