ASTM D4672-18
(Test Method)Standard Test Method for Polyurethane Raw Materials: Determination of Water Content of Polyols
Standard Test Method for Polyurethane Raw Materials: Determination of Water Content of Polyols
SIGNIFICANCE AND USE
5.1 This test method is suitable for quality control, as a specification test, and for research. The water content of a polyol is important since isocyanates react with water.
SCOPE
1.1 This test method measures water content of polyols and many other organic compounds.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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.
Note 1: This test method is equivalent to ISO 14897.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4672 − 18
Standard Test Method for
Polyurethane Raw Materials: Determination of Water
1
Content of Polyols
This standard is issued under the fixed designation D4672; 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* 3. Terminology
1.1 This test method measures water content of polyols and 3.1 Definitions:
many other organic compounds. 3.1.1 polyurethane, n—a polymer prepared by the reaction
of an organic diisocyanate with compounds containing hy-
1.2 The values stated in SI units are to be regarded as the
droxyl groups.
standard. The values given in parentheses are for information
3.1.1.1 Discussion—Polyurethanes,orurethanes,astheyare
only.
sometimes called, can be thermosetting, thermoplastic, rigid or
1.3 This standard does not purport to address all of the
soft and flexible, cellular or solid. (See Terminology D883.)
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Methods
priate safety, health, and environmental practices and deter-
4.1 This method is based essentially on volumetric or
mine the applicability of regulatory limitations prior to use.
coulometric titrations that follow the reduction of iodine by
NOTE 1—This test method is equivalent to ISO 14897.
sulfur dioxide in the presence of water. This reaction proceeds
1.4 This international standard was developed in accor-
quantitatively when methanol or another alcohol (ROH) and
dance with internationally recognized principles on standard-
pyridine (C H N) or a similar amine (R'N) are present to react
5 5
ization established in the Decision on Principles for the
withthesulfurtrioxide(SO )andhydriodicacid(HI)produced
3
Development of International Standards, Guides and Recom-
according to the following reactions:
mendations issued by the World Trade Organization Technical ROH+SO + R'N→ [R'NH]SO R
2 3
Barriers to Trade (TBT) Committee.
HO+I + [R'NH]SO R + 2R'N→ [R'NH]SO R + 2[R'NH]I
2 2 3 4
4.2 To determine water, Karl Fischer reagent (a solution of
2. Referenced Documents
iodine, sulfur dioxide, imidazole, and pyridine or a pyridine
2
2.1 ASTM Standards:
substitute) is added to a solution of the sample in methanol or
D1193 Specification for Reagent Water
other alcohol until all of the water present has been consumed.
D883 Terminology Relating to Plastics
The titrant is either added by buret (volumetry) or generated
E203 Test Method for Water Using Volumetric Karl Fischer
electrochemically in the titration cell (coulometry). Coulomet-
Titration
ric titrations eliminate the need for standardizing the reagent.
E691 Practice for Conducting an Interlaboratory Study to
Pyridine is less commonly used recently due to its toxicity. If
Determine the Precision of a Test Method
pyridine is to be used, refer to the SDS for proper precautions.
3
2.2 ISO Standards:
4.3 This method provides details specific to water determi-
ISO 14897 Plastics—Polyols for use in the production of
nations in polyols. General guidance to the use of Karl-Fischer
polyurethane—Determination of water content
analysis, including a list of interferences, can be found in Test
Method E203.
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
and are the direct responsibility of Subcommittee D20.22 on Cellular Materials -
5. Significance and Use
Plastics and Elastomers.
Current edition approved April 1, 2018. Published April 2018. Originally 5.1 This test method is suitable for quality control, as a
approved in 1991. Last previous edition approved in 2012 as D4672 - 12. DOI:
specification test, and for research. The water content of a
10.1520/D4672-18.
polyol is important since isocyanates react with water.
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 6. Apparatus
the ASTM website.
3
6.1 Several commercial Karl Fischer autotitrators are avail-
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org. able that employ volumetric or coulometric titrations. These
*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
-----
...
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: D4672 − 12 D4672 − 18
Standard Test Method for
Polyurethane Raw Materials: Determination of Water
1
Content of Polyols
This standard is issued under the fixed designation D4672; 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 measures water content of polyols and many other organic compounds.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
NOTE 1—This test method is equivalent to ISO 14897.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D883 Terminology Relating to Plastics
E203 Test Method for Water Using Volumetric Karl Fischer Titration
E180E691 Practice for Determining Conducting an Interlaboratory Study to Determine the Precision of ASTM Methods for
Analysis and Testing of Industrial and Specialty Chemicalsa Test Method (Withdrawn 2009)
3
2.2 ISO Standards:
ISO 14897 Plastics—Polyols for use in the production of polyurethane—Determination of water content
3. Terminology
3.1 Definitions:
3.1.1 polyurethane, n—a polymer prepared by the reaction of an organic diisocyanate with compounds containing hydroxyl
groups.
3.1.1.1 Discussion—
Polyurethanes, or urethanes, as they are sometimes called, maycan be thermosetting, thermoplastic, rigid or soft and flexible,
cellular or solid. (See Terminology D883.)
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular Materials - Plastics
and Elastomers.
Current edition approved Aug. 1, 2012April 1, 2018. Published August 2012April 2018. Originally approved in 1991. Last previous edition approved in 20002012 as
ε1
D4672 - 00D4672 - 12.(2006) . DOI: 10.1520/D4672-12.10.1520/D4672-18.
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.
3
The last approved version of this historical standard is referenced on www.astm.org.Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th
Floor, New York, NY 10036, http://www.ansi.org.
4
Instruments similar to and including the following types have been found suitable for determining water content of polyols, based on round-robin studies: Metrohm
models 633, 652, 658, 665, 684, 701, 720, 737, and 758 (available from Brinkmann Instruments, Inc. at www.brinkmann.com) and Mettler Toledo models DL 18, 31, 37,
and 38 (www.mt.com).
*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 ----------------------
D4672 − 18
4. Summary of Test Methods
4.1 This method is based essentially on volumetric or coulometric titrations that follow the reduction of iodine by sulfur dioxide
in the presence of water. This reaction proceeds quantitatively when methanol or another alcohol (ROH) and pyridine (C H N) or
5 5
a similar amine (R'N) are present to react with the sulfur trioxide (SO ) and hydriodic acid (HI) produced according to the
3
following reactions:
ROH + SO + R'N → [R'NH]SO R
2 3
H O + I + [R'NH]SO R + 2R'N → [R'NH]SO R + 2[R'NH]I
2 2 3 4
4.2 To determine water, Karl Fischer reagent (a solution of iodine, sulfur dioxide, imidazole, and pyridine or a pyridine
substitute) is added to a solution of the sample in methanol or other alcohol until all of the water present has been consumed. The
titrant is either added b
...
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: D4672 − 18
Standard Test Method for
Polyurethane Raw Materials: Determination of Water
1
Content of Polyols
This standard is issued under the fixed designation D4672; 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* 3. Terminology
1.1 This test method measures water content of polyols and 3.1 Definitions:
many other organic compounds. 3.1.1 polyurethane, n—a polymer prepared by the reaction
of an organic diisocyanate with compounds containing hy-
1.2 The values stated in SI units are to be regarded as the
droxyl groups.
standard. The values given in parentheses are for information
3.1.1.1 Discussion—Polyurethanes, or urethanes, as they are
only.
sometimes called, can be thermosetting, thermoplastic, rigid or
1.3 This standard does not purport to address all of the
soft and flexible, cellular or solid. (See Terminology D883.)
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Methods
priate safety, health, and environmental practices and deter-
4.1 This method is based essentially on volumetric or
mine the applicability of regulatory limitations prior to use.
coulometric titrations that follow the reduction of iodine by
NOTE 1—This test method is equivalent to ISO 14897.
sulfur dioxide in the presence of water. This reaction proceeds
1.4 This international standard was developed in accor-
quantitatively when methanol or another alcohol (ROH) and
dance with internationally recognized principles on standard-
pyridine (C H N) or a similar amine (R'N) are present to react
5 5
ization established in the Decision on Principles for the
with the sulfur trioxide (SO ) and hydriodic acid (HI) produced
3
Development of International Standards, Guides and Recom- according to the following reactions:
mendations issued by the World Trade Organization Technical
ROH + SO + R'N → [R'NH]SO R
2 3
Barriers to Trade (TBT) Committee. H O + I + [R'NH]SO R + 2R'N → [R'NH]SO R + 2[R'NH]I
2 2 3 4
4.2 To determine water, Karl Fischer reagent (a solution of
2. Referenced Documents
iodine, sulfur dioxide, imidazole, and pyridine or a pyridine
2
2.1 ASTM Standards:
substitute) is added to a solution of the sample in methanol or
D1193 Specification for Reagent Water
other alcohol until all of the water present has been consumed.
D883 Terminology Relating to Plastics
The titrant is either added by buret (volumetry) or generated
E203 Test Method for Water Using Volumetric Karl Fischer
electrochemically in the titration cell (coulometry). Coulomet-
Titration
ric titrations eliminate the need for standardizing the reagent.
E691 Practice for Conducting an Interlaboratory Study to
Pyridine is less commonly used recently due to its toxicity. If
Determine the Precision of a Test Method
pyridine is to be used, refer to the SDS for proper precautions.
3
2.2 ISO Standards:
4.3 This method provides details specific to water determi-
ISO 14897 Plastics—Polyols for use in the production of
nations in polyols. General guidance to the use of Karl-Fischer
polyurethane—Determination of water content
analysis, including a list of interferences, can be found in Test
Method E203.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and are the direct responsibility of Subcommittee D20.22 on Cellular Materials -
5. Significance and Use
Plastics and Elastomers.
5.1 This test method is suitable for quality control, as a
Current edition approved April 1, 2018. Published April 2018. Originally
approved in 1991. Last previous edition approved in 2012 as D4672 - 12. DOI:
specification test, and for research. The water content of a
10.1520/D4672-18.
polyol is important since isocyanates react with water.
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 6. Apparatus
the ASTM website.
3 6.1 Several commercial Karl Fischer autotitrators are avail-
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org. able that employ volumetric or coulometric titrations. These
*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 ----------------------
D4672 − 18
are available, use the guidelines listed in Table 1 and Table 2.
...
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