ASTM D6304-04ae1

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An American National Standard
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Designation:D6304–04a
Standard Test Method for
Determination of Water in Petroleum Products, Lubricating
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Oils, and Additives by Coulometric Karl Fischer Titration
This standard is issued under the fixed designation D6304; 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 (ε) indicates an editorial change since the last revision or reapproval.
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ε NOTE—Editorial changes were made throughout in March 2005.
1. Scope* D4052 Test Method for Density and Relative Density of
Liquids by Digital Density Meter
1.1 This test method covers the direct determination of
D4057 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-
D4177 Practice for Automatic Sampling of Petroleum and
mentation.Thistestmethodalsocoverstheindirectanalysisof
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
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E203 TestMethodforWaterUsingVolumetricKarlFischer
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
transmissionfluids,hydrocarbonsolvents,andotherpetroleum
coulometricKarlFischerapparatusinwhichiodinefortheKarl
products.Byproperchoiceofthesamplesize,thistestmethod
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.
detectedbyanelectrometricendpointdetectorandthetitration
1.3 Values stated in SI units are to be regarded as the
isterminated.Basedonthestoichiometryofthereaction,1mol
standard.
ofiodinereactswith1molofwater;thus,thequantityofwater
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.
D1193 Specification for Reagent Water
D1298 TestMethodforDensity,RelativeDensity(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
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This test method is under the jurisdiction of ASTM Committee D02 on helpinpredictingtheirqualityandperformancecharacteristics.
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
4.2 For lubricating oils, the presence of moisture could lead
D02.02 on Static Petroleum Measurement.
toprematurecorrosionandwear,anincreaseinthedebrisload
Current edition approved May 1, 2004. Published June 2004. Originally
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resulting in diminished lubrication and premature plugging of
approved in 1998. Last previous edition approved in 2004 as D6304–04 .
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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.
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D6304–04a
TABLE 1 Test Sample Size Based on Expected Water Content
accurate to the nearest 10 µL; 1 mL accurate to the nearest
Expected Water Sample Size µg Water 0.01mL; 2 mL accurate to the nearest 0.01 mL; and 3 mL
Concentration g o
...