ASTM D6304-03

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 Fisher 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.

General Information

• Status: Historical
• Publication Date: 09-Jul-2003
• ICS: 71.040.50 - Physicochemical methods of analysis
• ICS: 75.080 - Petroleum products in general
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.02.08 - Sampling (API MPMS Chapter 8.0)

Relations

• Replaces: ASTM D6304-00 - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
• Effective Date: 10-Jul-2003
• Replaced By: ASTM D6304-04 - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
• Effective Date: 01-Feb-2004
• Referred By: ASTM D4054-23 - Standard Practice for Evaluation of New Aviation Turbine Fuels and Fuel Additives
• Effective Date: 10-Jul-2003
• Referred By: ASTM D2827-19 - Standard Specification for Styrene Monomer
• Effective Date: 10-Jul-2003
• Referred By: ASTM E1417/E1417M-21e1 - Standard Practice for Liquid Penetrant Testing
• Effective Date: 10-Jul-2003
• Referred By: ASTM D8046-21 - Standard Guide for Pumpability of Heat Transfer Fluids
• Effective Date: 10-Jul-2003
• Referred By: ASTM D4378-22 - Standard Practice for In-Service Monitoring of Mineral Turbine Oils for Steam, Gas, and Combined Cycle Turbines
• Effective Date: 10-Jul-2003
• Referred By: ASTM D7754-19 - Standard Test Method for Determination of Trace Oxygenates in Automotive Spark-Ignition Engine Fuel by Multidimensional Gas Chromatography
• Effective Date: 10-Jul-2003
• Referred By: ASTM D4293-22 - Standard Specification for Phosphate Ester-Based Fluids for Turbine Lubrication and Steam Turbine Electro-Hydraulic Control (EHC) Applications
• Effective Date: 10-Jul-2003
• Referred By: ASTM D6710-21 - Standard Guide for Evaluation of Hydrocarbon-Based Quench Oil
• Effective Date: 10-Jul-2003
• Referred By: ASTM D1796-22 - Standard Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
• Effective Date: 10-Jul-2003
• Referred By: ASTM D8506-23 - Standard Guide for Microbial Contamination and Biodeterioration in Turbine Oils and Turbine Oil Systems
• Effective Date: 10-Jul-2003
• Referred By: ASTM D7044-15 - Standard Specification for Biodegradable Fire Resistant Hydraulic Fluids
• Effective Date: 10-Jul-2003
• Referred By: ASTM D8324-21 - Standard Guide for Selection of Environmentally Acceptable Lubricants for the U.S. Environmental Protection Agency (EPA) Vessel General Permit
• Effective Date: 10-Jul-2003
• Referred By: ASTM D7596-23 - Standard Test Method for Automatic Particle Counting and Particle Shape Classification of Oils Using a Direct Imaging Integrated Tester
• Effective Date: 10-Jul-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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An American National Standard
Designation: D 6304 – 03
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.
4
1. Scope* Petroleum Products
D 5854 Practice for Mixing and Handling of Liquid
1.1 This test method covers the direct determination of
5
Samples of Petroleum and Petroleum Products
water in the range of 10 to 25 000 mg/kg entrained water in
E 203 Test Method for Water Using Volumetric Karl Fischer
petroleum products and hydrocarbons using automated instru-
6
Titration
mentation. This test method also covers the indirect analysis of
water thermally removed from samples and swept with dry
3. Summary of Test Method
inert gas into the Karl Fischer titration cell. Mercaptan, sulfide
−
3.1 An aliquot is injected into the titration vessel of a
(S or H S), sulfur, and other compounds are known to
2
coulometric Karl Fischer apparatus in which iodine for the Karl
interfere with this test method (see Section 5).
Fisher reaction is generated coulometrically at the anode.
1.2 This test method is intended for use with commercially
When all of the water has been titrated, excess iodine is
available coulometric Karl Fischer reagents and for the deter-
detected by an electrometric end point detector and the titration
mination of water in additives, lube oils, base oils, automatic
is terminated. Based on the stoichiometry of the reaction, 1 mol
transmission fluids, hydrocarbon solvents, and other petroleum
of iodine reacts with 1 mol of water; thus, the quantity of water
products. By proper choice of the sample size, this test method
is proportional to the total integrated current according to
may be used for the determination of water from mg/kg to
Faraday’s Law.
percent level concentrations.
3.2 The sample injection can be done either by mass or
1.3 Values stated in SI units are to be regarded as the
volume.
standard.
3.3 The viscous samples can be analyzed by using a water
1.4 This standard does not purport to address all of the
vaporizer accessory that heats the sample in the evaporation
safety concerns, if any, associated with its use. It is the
chamber, and the vaporized water is carried into the Karl
responsibility of the user of this standard to establish appro-
Fischer titration cell by a dry inert carrier gas.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Significance and Use
4.1 A knowledge of the water content of lubricating oils,
2. Referenced Documents
additives, and similar products is important in the manufactur-
2.1 ASTM Standards:
2 ing, purchase, sale, or transfer of such petroleum products to
D 1193 Specification for Reagent Water
help in predicting their quality and performance characteristics.
D 1298 Practice for Density, Relative Density (Specific
4.2 For lubricating oils, the presence of moisture could lead
Gravity), or API Gravity of Crude Petroleum and Liquid
3 to premature corrosion and wear, an increase in the debris load
Petroleum Products by Hydrometer Method
resulting in diminished lubrication and premature plugging of
D 4052 Test Method for Density and Relative Density of
4 filters, an impedance in the effect of additives, and undesirable
Liquids by Digital Density Meter
support of deleterious bacterial growth.
D 4057 Practice for Manual Sampling of Petroleum and
4
Petroleum Products
5. Interferences
D 4177 Practice for Automatic Sampling of Petroleum and
5.1 A number of substances and classes of compounds
associated with condensation or oxidation-reduction reactions
1 interferes in the determination of water by Karl Fischer
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee titration. In petroleum products, the most common interfer-
D02.02 on Static Petroleum Measurement.
ences are mercaptans and sulfides. At levels of less than 500
Current edition approved July 10, 2003. Published September 2003. Originally
approved in 1998. Last previous edition approved in 2000 as D 6304–00.
2
Annual Book of ASTM Standards, Vol 11.01.
3 5
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 05.03.
4 6
Annual Book of ASTM Standards, Vol 05.02. Annual Book of ASTM Standards, Vol 15.05.
*A Summary of Changes section appears at the end of this standard.
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