ASTM D6304-16e1
(Test Method)Standard Test Method for Determination of Water in Petroleum Products, Lubricating Oils, and Additives by Coulometric Karl Fischer Titration
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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´1
Designation: D6304 − 16
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 (´) 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
ε NOTE—Reference to a Summary of Changes was removed editorially in September 2016.
1. Scope D1298Test Method for Density, Relative Density, or API
Gravity of Crude Petroleum and Liquid Petroleum Prod-
1.1 This test method covers the direct determination of
ucts by Hydrometer Method
water in the range of 10mg⁄kg to 25000mg⁄kg entrained
D4052Test Method for Density, Relative Density, and API
water in petroleum products and hydrocarbons using auto-
Gravity of Liquids by Digital Density Meter
mated instrumentation. This test method also covers the
D4057Practice for Manual Sampling of Petroleum and
indirectanalysisofwaterthermallyremovedfromsamplesand
Petroleum Products
swept with dry inert gas into the Karl Fischer titration cell.
− D4177Practice for Automatic Sampling of Petroleum and
Mercaptan, sulfide (S or H S), sulfur, and other compounds
2
Petroleum Products
are known to interfere with this test method (see Section 5).
D5854Practice for Mixing and Handling of Liquid Samples
1.2 This test method is intended for use with commercially
of Petroleum and Petroleum Products
available coulometric Karl Fischer reagents and for the deter-
E203Test Method for Water Using Volumetric Karl Fischer
mination of water in additives, lube oils, base oils, automatic
Titration
transmissionfluids,hydrocarbonsolvents,andotherpetroleum
3. Summary of Test Method
products.Byproperchoiceofthesamplesize,thistestmethod
may be used for the determination of water from mg/kg to
3.1 An aliquot is injected into the titration vessel of a
percent level concentrations.
coulometricKarlFischerapparatusinwhichiodinefortheKarl
Fisher reaction is generated coulometrically at the anode.
1.3 The values stated in SI units are to be regarded as
When all of the water has been titrated, excess iodine is
standard. No other units of measurement are included in this
detectedbyanelectrometricendpointdetectorandthetitration
standard.
isterminated.Basedonthestoichiometryofthereaction,1mol
1.4 This standard does not purport to address all of the
ofiodinereactswith1molofwater;thus,thequantityofwater
safety concerns, if any, associated with its use. It is the
is proportional to the total integrated current according to
responsibility of the user of this standard to establish appro-
Faraday’s Law.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 3.2 The sample injection can be done either by mass or
volume.
2. Referenced Documents
3.3 The viscous samples can be analyzed by using a water
2
2.1 ASTM Standards: vaporizer accessory that heats the sample in the evaporation
D1193Specification for Reagent Water chamber, and the vaporized water is carried into the Karl
Fischer titration cell by a dry inert carrier gas.
4. Significance and Use
1
This test method is under the jurisdiction of ASTM Committee D02 on
4.1 A knowledge of the water content of lubricating oils,
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
additives, and similar products is important in the
CurrenteditionapprovedJuly1,2016.PublishedJuly2016.Originallyapproved
manufacturing, purchase, sale, or transfer of such petroleum
in 1998. Last previous edition approved in 2007 as D6304–07, which was
products to help in predicting their quality and performance
withdrawn in April 2016 and reinstated in July 2016. DOI: 10.1520/D6304-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or characteristics.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4.2 For lubricating oils, the presence of moisture could lead
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. toprematurecorrosionandwear,anincreaseinthedebrisload
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
resulting in diminished lubrication and premature plugging of
filters, an impedance in the effect of additives, and undesirable Expected Water
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D6304 − 16 D6304 − 16
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. A number 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
ε NOTE—Reference to a Summary of Changes was removed editorially in September 2016.
1. 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 H S),
2
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products by
Hydrometer Method
D4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density Meter
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products
E203 Test Method for Water Using Volumetric Karl Fischer Titration
3. Summary of Test Method
3.1 An aliquot is injected into the titration vessel of a coulometric Karl Fischer apparatus in which iodine for the Karl Fisher
reaction is generated coulometrically at the anode. When all of the water has been titrated, excess iodine is detected by an
electrometric end point detector and the titration is terminated. Based on the stoichiometry of the reaction, 1 mol of iodine reacts
with 1 mol of water; thus, the quantity of water is proportional to the total integrated current according to Faraday’s Law.
3.2 The sample injection can be done either by mass or volume.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.06 on Analysis of Liquid Fuels and Lubricants.
Current edition approved July 1, 2016. Published July 2016. Originally approved 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.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 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
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
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D6304 − 16
TABLE 1 Test Sample Size Based on Expected Water Content
Expected Water Sample Size μg Water
Concentration g or mL Titrated
10 mg ⁄kg to 100 mg/kg or μg/mL 3.0 30 to 300
10 mg ⁄kg to 500 mg/kg or μg/mL 2.0 200 to 1000
0.02 % to 0.1 % 1.0 200 to 1000
0.1 % to 0.5 % 0.5 500 to 2500
0.5 % to 2.5 % 0.25 1250 to 6250
3.3 The viscous samples can be analyzed by using a water vapo
...
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