ASTM E1064-16

Standard Test Method for Water in Organic Liquids by Coulometric Karl Fischer Titration

SIGNIFICANCE AND USE
4.1 The coulometric technique is especially suited for determining low concentrations of water in organic liquids that would yield small titers by the Karl Fischer volumetric procedure. The precision and accuracy of the coulometric technique decreases for concentrations of water much greater than 2.0 % because of the difficulty in measuring the small size of sample required. The test method assumes 100 % efficiency of coulombs in iodine production. Provision is made for verifying this efficiency. (See Table 1 and Note 5.)
SCOPE
1.1 This test method covers the determination of water from 0 to 2.0 % mass in most liquid organic chemicals, with Karl Fischer reagent, using an automated coulometric titration procedure. Use of this test method is not applicable for liquefied gas products such as Liquid Petroleum Gas (LPG), Butane, Propane, Liquid Natural Gas (LNG), etc.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first-aid procedures, handling, and safety precautions.  
1.4 This standard does not purport to address all of the safety problems, 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. Specific precautionary statements are given in Section 8.

General Information

• Status: Historical
• Publication Date: 31-Mar-2016
• ICS: 71.080.01 - Organic chemicals in general
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.04 - Instrumental Analysis

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E1064 − 16
Standard Test Method for
Water in Organic Liquids by Coulometric Karl Fischer
1
Titration
This standard is issued under the fixed designation E1064; 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.
1. Scope* E180 Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial and Spe-
1.1 This test method covers the determination of water from
3
cialty Chemicals (Withdrawn 2009)
0 to 2.0 % mass in most liquid organic chemicals, with Karl
E203 Test Method for Water Using Volumetric Karl Fischer
Fischer reagent, using an automated coulometric titration
Titration
procedure. Use of this test method is not applicable for
liquefied gas products such as Liquid Petroleum Gas (LPG),
3. Summary of Test Method
Butane, Propane, Liquid Natural Gas (LNG), etc.
3.1 This test method is based on the Karl Fischer reaction
1.2 The values stated in SI units are to be regarded as
for determining water—the reduction of iodine by sulfur
standard. No other units of measurement are included in this
dioxide in the presence of water to form sulfur trioxide and
standard.
hydriodic acid. The reaction becomes quantitative only when
1.3 Review the current Safety Data Sheets (SDS) for de-
pyridine or other organic base and methanol or other alcohol
tailed information concerning toxicity, first-aid procedures,
are present. Unlike the volumetric Karl Fischer reagents that
handling, and safety precautions.
include iodine, the coulometric technique electrolytically gen-
1.4 This standard does not purport to address all of the erates iodine, with 10.71 C of generating current corresponding
safety problems, if any, associated with its use. It is the
to 1 mg of water in accordance with Faraday’s law.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Significance and Use
mine the applicability of regulatory limitations prior to use.
4.1 The coulometric technique is especially suited for de-
Specific precautionary statements are given in Section 8.
termining low concentrations of water in organic liquids that
1.5 This international standard was developed in accor-
would yield small titers by the Karl Fischer volumetric
dance with internationally recognized principles on standard-
procedure. The precision and accuracy of the coulometric
ization established in the Decision on Principles for the
technique decreases for concentrations of water much greater
Development of International Standards, Guides and Recom-
than 2.0 % because of the difficulty in measuring the small size
mendations issued by the World Trade Organization Technical
of sample required. The test method assumes 100 % efficiency
Barriers to Trade (TBT) Committee.
of coulombs in iodine production. Provision is made for
verifying this efficiency. (See Table 1 and Note 5.)
2. Referenced Documents
2
2.1 ASTM Standards:
5. Interferences
D1193 Specification for Reagent Water
5.1 Interfering substances are the same as are encountered
D4672 Test Method for Polyurethane Raw Materials: Deter-
in the volumetric Karl Fischer titration. A detailed discussion
mination of Water Content of Polyols
of interfering substances can be found in the treatise on
4
“Aquametry.”
5.2 Test Method E203 discusses organic compounds in
1
This test method is under the jurisdiction of ASTM Committee D16 on
which water may be determined directly and compounds in
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
bility of Subcommittee D16.04 on Instrumental Analysis.
Current edition approved April 1, 2016. Published May 2016. Originally
approved in 1985. Last previous edition approved in 2012 as E1064 – 12. DOI:
3
10.1520/E1064-16. The last approved version of this historical standard is referenced on
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or www.astm.org.
4
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM J. Mitchell, Jr. and D. M. Smith, “Aquametry”—A Treatise on Methods for the
Standards volume information, refer to the standard’s Document Summary page on Determination of Water, Part III—The Karl Fischer Reagent, 2nd Ed., J. Wiley and
the ASTM website. Sons, Inc., New York, NY 1990.
*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

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E1064 − 16
which water cannot be determined directly, but in which 7.2
...

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.
Designation: E1064 − 12 E1064 − 16
Standard Test Method for
Water in Organic Liquids by Coulometric Karl Fischer
1
Titration
This standard is issued under the fixed designation E1064; 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.
1. Scope*
1.1 This test method covers the determination of water from 0 to 2.0 % mass in most liquid organic chemicals, with Karl Fischer
reagent, using an automated coulometric titration procedure. Use of this test method is not applicable for liquefied gas products
such as Liquid Petroleum Gas (LPG), Butane, Propane, Liquid Natural Gas (LNG), etc.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Review the current material safety data sheets (MSDS) Safety Data Sheets (SDS) for detailed information concerning
toxicity, first-aid procedures, handling, and safety precautions.
1.4 This standard does not purport to address all of the safety problems, 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. Specific precautionary statements are given in Section 8.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D4672 Test Method for Polyurethane Raw Materials: Determination of Water Content of Polyols
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E203 Test Method for Water Using Volumetric Karl Fischer Titration
3. Summary of Test Method
3.1 This test method is based on the Karl Fischer reaction for determining water—the reduction of iodine by sulfur dioxide in
the presence of water to form sulfur trioxide and hydriodic acid. The reaction becomes quantitative only when pyridine or other
organic base and methanol or other alcohol are present. Unlike the volumetric Karl Fischer reagents that include iodine, the
coulometric technique electrolytically generates iodine, with 10.71 C of generating current corresponding to 1 mg of water in
accordance with Faraday’s law.
4. Significance and Use
4.1 The coulometric technique is especially suited for determining low concentrations of water in organic liquids that would
yield small titers by the Karl Fischer volumetric procedure. The precision and accuracy of the coulometric technique decreases for
concentrations of water much greater than 2.0 % because of the difficulty in measuring the small size of sample required. The test
method assumes 100 % efficiency of coulombs in iodine production. Provision is made for verifying this efficiency. (See Table
1Table 1 and Note 6.)5.)
1
This test method is under the jurisdiction of ASTM Committee E15 on Industrial and Specialty Chemicals and is the direct responsibility of Subcommittee E15.01 on
General Standards.
Current edition approved April 1, 2012April 1, 2016. Published May 2012May 2016. Originally approved in 1985. Last previous edition approved in 20082012 as
E1064 – 08.E1064 – 12. DOI: 10.1520/E1064-12.10.1520/E1064-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
*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

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E1064 − 16
TABLE 1 Sample Size Estimation
Expected Water Content Sample Size, mL
0 to 500 mg/kg 5
500 to 1000 mg/kg 2
1000 to 2000 mg/kg 1
0.2 to 0.5 % mass 0.5
0.5 to 2.0 % mass 0.1
5. Interferences
5.1 Interfering substances are the same as are encountered in the volumetric Karl Fischer titration. A detailed discussion of
4
interfering substances can be found in the treatise on “Aquametry.”
5.2 Test Method E203 discusses organic compounds in which water may be determined directly and compounds in which water
cannot be determined directly, but in which interferences may be el
...