Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fischer Titration

SIGNIFICANCE AND USE
4.1 A knowledge of the water content of lubricating oils, additives, and similar products is important in the manufacturing, purchase, sale, or transfer of such petroleum products to help in predicting their quality and performance characteristics.  
4.2 For lubricating oils, the presence of moisture could lead to premature corrosion and wear, an increase in the debris load resulting in diminished lubrication and premature plugging of filters, an impedance in the effect of additives, and undesirable support of deleterious bacterial growth.
SCOPE
1.1 This test method covers the direct determination of water in the range of 10 mg/kg 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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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Historical
Publication Date
30-Jun-2016
Current Stage
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ASTM D6304-16 - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fischer Titration
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D6304 − 16
StandardTest 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 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 (´) 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 ucts by Hydrometer Method
D4052Test Method for Density, Relative Density, and API
1.1 This test method covers the direct determination of
Gravity of Liquids by Digital Density Meter
water in the range of 10mg⁄kg to 25000mg⁄kg entrained
D4057Practice for Manual Sampling of Petroleum and
water in petroleum products and hydrocarbons using auto-
Petroleum Products
mated instrumentation. This test method also covers the
D4177Practice for Automatic Sampling of Petroleum and
indirectanalysisofwaterthermallyremovedfromsamplesand
Petroleum Products
swept with dry inert gas into the Karl Fischer titration cell.
− D5854Practice for Mixing and Handling of Liquid Samples
Mercaptan, sulfide (S or H S), sulfur, and other compounds
2
of Petroleum and Petroleum Products
are known to interfere with this test method (see Section 5).
E203Test Method for Water Using Volumetric Karl Fischer
1.2 This test method is intended for use with commercially
Titration
available coulometric Karl Fischer reagents and for the deter-
mination of water in additives, lube oils, base oils, automatic
3. Summary of Test Method
transmissionfluids,hydrocarbonsolvents,andotherpetroleum
3.1 An aliquot is injected into the titration vessel of a
products.Byproperchoiceofthesamplesize,thistestmethod
coulometricKarlFischerapparatusinwhichiodinefortheKarl
may be used for the determination of water from mg/kg to
Fisher reaction is generated coulometrically at the anode.
percent level concentrations.
When all of the water has been titrated, excess iodine is
1.3 The values stated in SI units are to be regarded as
detectedbyanelectrometricendpointdetectorandthetitration
standard. No other units of measurement are included in this
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
vaporizer accessory that heats the sample in the evaporation
2. Referenced Documents
chamber, and the vaporized water is carried into the Karl
2
2.1 ASTM Standards:
Fischer titration cell by a dry inert carrier gas.
D1193Specification for Reagent Water
D1298Test Method for Density, Relative Density, or API
4. Significance and Use
Gravity of Crude Petroleum and Liquid Petroleum Prod-
4.1 A knowledge of the water content of lubricating oils,
additives, and similar products is important in the
manufacturing, purchase, sale, or transfer of such petroleum
1
This test method is under the jurisdiction of ASTM Committee D02 on
products to help in predicting their quality and performance
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
characteristics.
CurrenteditionapprovedJuly1,2016.PublishedJuly2016.Originallyapproved
4.2 For lubricating oils, the presence of moisture could lead
in 1998. Last previous edition approved in 2007 as D6304–07, which was
withdrawn in April 2016 and reinstated in July 2016. DOI: 10.1520/D6304-16.
toprematurecorrosionandwear,anincreaseinthedebrisload
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
resulting in diminished lubrication and premature plugging of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
filters, an impedance in the effect of additives, and undesirable
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. support of deleterious bacterial growth.
*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 − 16
TABLE 1 Test Sample Size Based on Expected Water Content
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