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ASTM D6304-04a

(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.

General Information

Status
Historical
Publication Date
30-Apr-2004
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

Replaces
ASTM D6304-04e1 - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
Effective Date
01-May-2004
Referred By
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Effective Date
01-May-2004
Referred By
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Effective Date
01-May-2004
Referred By
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Effective Date
01-May-2004
Referred By
ASTM D6074-15(2022) - Standard Guide for Characterizing Hydrocarbon Lubricant Base Oils
Effective Date
01-May-2004
Referred By
ASTM D7826-23a - Standard Guide for Evaluation of New Aviation Gasolines and New Aviation Gasoline Additives
Effective Date
01-May-2004
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
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ASTM D6710-21 - Standard Guide for Evaluation of Hydrocarbon-Based Quench Oil
Effective Date
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Effective Date
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Effective Date
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ASTM D7796-21 - Standard Test Method for Analysis of Ethyl tert-Butyl Ether (ETBE) by Gas Chromatography
Effective Date
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Effective Date
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ASTM D7155-20 - Standard Practice for Evaluating Compatibility of Mixtures of Turbine Lubricating Oils
Effective Date
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ASTM D8350-22 - Standard Test Method for Evaluation of Automotive Engine Oils in the Sequence IVB Spark-Ignition Engine
Effective Date
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Referred By
ASTM D1796-22 - Standard Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
Effective Date
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ASTM D6304-04a - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher TitrationASTM D6304-04a - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher Titration
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ASTM D6304-04a - Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fisher 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
An American National Standard
Designation:D6304–04a
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 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope* D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the direct determination of
D 5854 Practice for Mixing and Handling of Liquid
water in the range of 10 to 25 000 mg/kg entrained water in
Samples of Petroleum and Petroleum Products
petroleum products and hydrocarbons using automated instru-
E203 TestMethodforWaterUsingVolumetricKarlFischer
mentation.Thistestmethodalsocoverstheindirectanalysisof
Titration
water thermally removed from samples and swept with dry
inert gas into the Karl Fischer titration cell. Mercaptan, sulfide
3. Summary of Test Method
−
(S or H S), sulfur, and other compounds are known to
2
3.1 An aliquot is injected into the titration vessel of a
interfere with this test method (see Section 5).
coulometricKarlFischerapparatusinwhichiodinefortheKarl
1.2 This test method is intended for use with commercially
Fisher reaction is generated coulometrically at the anode.
available coulometric Karl Fischer reagents and for the deter-
When all of the water has been titrated, excess iodine is
mination of water in additives, lube oils, base oils, automatic
detectedbyanelectrometricendpointdetectorandthetitration
transmissionfluids,hydrocarbonsolvents,andotherpetroleum
isterminated.Basedonthestoichiometryofthereaction,1mol
products.Byproperchoiceofthesamplesize,thistestmethod
ofiodinereactswith1molofwater;thus,thequantityofwater
may be used for the determination of water from mg/kg to
is proportional to the total integrated current according to
percent level concentrations.
Faraday’s Law.
1.3 Values stated in SI units are to be regarded as the
3.2 The sample injection can be done either by mass or
standard.
volume.
1.4 This standard does not purport to address all of the
3.3 The viscous samples can be analyzed by using a water
safety concerns, if any, associated with its use. It is the
vaporizer accessory that heats the sample in the evaporation
responsibility of the user of this standard to establish appro-
chamber, and the vaporized water is carried into the Karl
priate safety and health practices and determine the applica-
Fischer titration cell by a dry inert carrier gas.
bility of regulatory limitations prior to use.
4. Significance and Use
2. Referenced Documents
2 4.1 A knowledge of the water content of lubricating oils,
2.1 ASTM Standards:
additives, and similar products is important in the manufactur-
D1193 Specification for Reagent Water
ing, purchase, sale, or transfer of such petroleum products to
D1298 TestMethodforDensity,RelativeDensity(Specific
helpinpredictingtheirqualityandperformancecharacteristics.
Gravity), or API Gravity of Crude Petroleum and Liquid
4.2 For lubricating oils, the presence of moisture could lead
Petroleum Products by Hydrometer Method
toprematurecorrosionandwear,anincreaseinthedebrisload
D4052 Test Method for Density and Relative Density of
resulting in diminished lubrication and premature plugging of
Liquids by Digital Density Meter
filters, an impedance in the effect of additives, and undesirable
D4057 Practice for Manual Sampling of Petroleum and
support of deleterious bacterial growth.
Petroleum Products
5. Interferences
1
This test method is under the jurisdiction of ASTM Committee D02 on
5.1 A number of substances and classes of compounds
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
associated with condensation or oxidation-reduction reactions
D02.02 on Static Petroleum Measurement.
interferes in the determination of water by Karl Fischer
Current edition approved May 1, 2004. Published June 2004. Originally
e1
approved in 1998. Last previous edition approved in 2004 as D6304–04 . titration. In petroleum products, the most common interfer-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ences are mercaptans and sulfides. At levels of less than 500
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
mg/kg as sulfur, the interference from these compounds is
Standards volume information, refer to the standard’s Document Summary page on
insignificant for water concentrations greater than 0.02 mass
the ASTM website.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive
...

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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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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.  
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5.1 This test method can be used to determine whether the amount of draindown measured for a given asphalt mixture is within specified acceptable levels. The test provides an evaluation of the draindown potential of an asphalt mixture during mixture design and/or during field production. This test is primarily used for mixtures with high coarse aggregate content such as porous asphalt (open-graded friction course) and stone matrix asphalt (SMA).
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1.1 This test method covers the determination of the amount of draindown in an uncompacted asphalt mixture sample when the sample is held at elevated temperatures comparable to those encountered during the production, storage, transport, and placement of the mixture. The test is particularly applicable to mixtures such as porous asphalt (open-graded friction course) and stone matrix asphalt (SMA).  
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SCOPE
1.1 These test methods cover the physical properties associated with preformed expansion joint fillers. The test methods include:    
Property  
Section  
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7.1  
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7.2  
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7.3  
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7.4  
Asphalt Content  
7.5  
Water Absorption  
7.6  
Density  
7.7
Note 1: Specific test methods are applicable only to certain types of joint fillers, as stated herein.  
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
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This specification covers asphalt plank used for bridge decks as well as for industrial floors. Asphalt planks shall be classified according to usage: Type Ia; Type Ib; and Type II. Asphalt plank shall be formed from a mixture of asphalt, fibers, modifiers, or a combination thereof, and mineral filler in such a manner as to produce a uniformly dense mass. The following test methods shall be intended to measure those attributes necessary to measure the ability of asphalt plank to provide a reasonably long and satisfactory service: absorption; brittleness; dimensions; and hardness.
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