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ASTM D6304-00

(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 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-Sep-2000
ICS
71.040.50 - Physicochemical methods of analysis
75.080 - Petroleum products in general
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)
Current Stage
Ref Project

Relations

Replaced By
ASTM D6304-03 - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
Effective Date
10-Jul-2003
Referred By
ASTM D6439-23 - Standard Guide for Cleaning, Flushing, and Purification of Steam, Gas, and Hydroelectric Turbine Lubrication Systems
Effective Date
10-Sep-2000
Referred By
ASTM D4868-17 - Standard Test Method for Estimation of Net and Gross Heat of Combustion of Hydrocarbon Burner and Diesel Fuels
Effective Date
10-Sep-2000
Referred By
ASTM D7720-21 - Standard Guide for Statistically Evaluating Measurand Alarm Limits when Using Oil Analysis to Monitor Equipment and Oil for Fitness and Contamination
Effective Date
10-Sep-2000
Referred By
ASTM D8279-23 - Standard Test Method for Determination of Timing-Chain Wear in a Turbocharged, Direct-Injection, Spark-Ignition, Four-Cylinder Engine
Effective Date
10-Sep-2000
Referred By
ASTM D7826-23a - Standard Guide for Evaluation of New Aviation Gasolines and New Aviation Gasoline Additives
Effective Date
10-Sep-2000
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-Sep-2000
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-Sep-2000
Referred By
ASTM D4860-22 - Standard Test Method for Free Water and Particulate Contamination in Middle Distillate Fuels (Clear and Bright Numerical Rating)
Effective Date
10-Sep-2000
Referred By
ASTM D8506-23 - Standard Guide for Microbial Contamination and Biodeterioration in Turbine Oils and Turbine Oil Systems
Effective Date
10-Sep-2000
Referred By
ASTM C1572/C1572M-23 - Standard Guide for Dry Lead Glass and Oil-Filled Lead Glass Radiation Shielding Window Components for Remotely Operated Facilities
Effective Date
10-Sep-2000
Referred By
ASTM D4054-23 - Standard Practice for Evaluation of New Aviation Turbine Fuels and Fuel Additives
Effective Date
10-Sep-2000
Referred By
ASTM D2827-19 - Standard Specification for Styrene Monomer
Effective Date
10-Sep-2000
Referred By
ASTM D1796-22 - Standard Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
Effective Date
10-Sep-2000
Referred By
ASTM D4814-23 - Standard Specification for Automotive Spark-Ignition Engine Fuel
Effective Date
10-Sep-2000

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ASTM D6304-00 - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher TitrationASTM D6304-00 - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
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ASTM D6304-00 - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
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Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 6304 – 00 An American National Standard
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.
1. Scope D 5854 Practice for Mixing and Handling of Liquid
5
Samples of Petroleum and Petroleum Products
1.1 This test method covers the direct determination of
E 203 Test Method for Water Using Volumetric Karl Fischer
water in the range of 10 to 25 000 mg/kg entrained water in
6
Titration
petroleum products and hydrocarbons using automated instru-
mentation. This test method also covers the indirect analysis of
3. Summary of Test Method
water thermally removed from samples and swept with dry
3.1 An aliquot is injected into the titration vessel of a
inert gas into the Karl Fischer titration cell. Mercaptan, sulfide
−
coulometric Karl Fischer apparatus in which iodine for the Karl
(S or H S), sulfur, and other compounds are known to
2
Fisher reaction is generated coulometrically at the anode.
interfere with this test method (see Section 5).
When all of the water has been titrated, excess iodine is
1.2 This test method is intended for use with commercially
detected by an electrometric end point detector and the titration
available coulometric Karl Fischer reagents and for the deter-
is terminated. Based on the stoichiometry of the reaction, 1 mol
mination of water in additives, lube oils, base oils, automatic
of iodine reacts with 1 mol of water; thus, the quantity of water
transmission fluids, hydrocarbon solvents, and other petroleum
is proportional to the total integrated current according to
products. By proper choice of the sample size, this test method
Faraday’s Law.
may be used for the determination of water from mg/kg to
3.2 The sample injection can be done either by mass or
percent level concentrations.
volume.
1.3 Values stated in SI units are to be regarded as the
3.3 The viscous samples can be analyzed by using a water
standard.
vaporizer accessory that heats the sample in the evaporation
1.4 This standard does not purport to address all of the
chamber, and the vaporized water is carried into the Karl
safety concerns, if any, associated with its use. It is the
Fischer titration cell by a dry inert carrier gas.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use.
4.1 A knowledge of the water content of lubricating oils,
2. Referenced Documents additives, and similar products is important in the manufactur-
ing, purchase, sale, or transfer of such petroleum products to
2.1 ASTM Standards:
2
help in predicting their quality and performance characteristics.
D 1193 Specification for Reagent Water
4.2 For lubricating oils, the presence of moisture could lead
D 1298 Practice for Density, Relative Density (Specific
to premature corrosion and wear, an increase in the debris load
Gravity), or API Gravity of Crude Petroleum and Liquid
3 resulting in diminished lubrication and premature plugging of
Petroleum Products by Hydrometer Method
filters, an impedance in the effect of additives, and undesirable
D 4052 Test Method for Density and Relative Density of
4 support of deleterious bacterial growth.
Liquids by Digital Density Meter
D 4057 Practice for Manual Sampling of Petroleum and
5. Interferences
4
Petroleum Products
5.1 A number of substances and classes of compounds
D 4177 Practice for Automatic Sampling of Petroleum and
associated with condensation or oxidation-reduction reactions
4
Petroleum Products
interferes in the determination of water by Karl Fischer
titration. In petroleum products, the most common interfer-
1
ences are mercaptans and sulfides. At levels of less than 500
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee mg/kg as sulfur, the interference from these compounds is
D2.02 on Static Petroleum Measurement.
insignificant for water concentrations greater than 0.02 mass
Current edition approved Sept. 10, 2000. Published November 2000. Originally
published as D 6304 - 98. L:ast previous edition D 6304 - 98a.
2
Annual Book of ASTM Standards, Vol 11.01.
3 5
Annual Book of ASTM Standards, Vol 5.01. Annual Book of ASTM Standards, Vol 5.03.
4 6
Annual Book of ASTM Standards, Vol 5.02. Annual Book of ASTM Standards, Vol 15.05.
Copyright © ASTM, 100
...

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SIGNIFICANCE AND USE
5.1 A knowledge of the water content is important in the manufacturing, purchase, sale, or transfer of petroleum products to help in predicting their quality and performance characteristics.  
5.2 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.
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1.1 This test method covers the direct determination of 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 6). The precision statement of this method covers the nominal range of 20 mg/kg to 25 000 mg/kg for Procedure A, 30 mg/kg to 2100 mg/kg for Procedure B, and 20 mg/kg to 360 mg/kg for Procedure C.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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5.1 A knowledge of the water content is important in the manufacturing, purchase, sale, or transfer of petroleum products to help in predicting their quality and performance characteristics.  
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This specification covers UNS N06002, UNS N06030, UNS N06035, UNS N06022, UNS N06200, UNS N06230, UNS N06600, UNS N06617, UNS N06625, UNS N08020, UNS N08026, UNS N08024, UNS N08120, UNS N08926, UNS N08367, UNS N10242, UNS N10276, UNS N10665, UNS N10675, UNS N12160, UNS R20033, UNS N06059, UNS N06686, UNS N10629, UNS N08031, UNS N06045, UNS N06025, and UNS R30556 nickel alloy billets and bars for reforging. The products shall be hot worked from ingots by rolling, forging, extruding, hammering, or pressing. The material shall conform to the chemical composition requirements prescribed by the reference material. The chemical composition of the material shall be determined by chemical analysis in accordance with test method E1473.
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