ASTM D4661-23
(Test Method)Standard Test Methods for Polyurethane Raw Materials: Determination of Total Chlorine in Isocyanates
Standard Test Methods for Polyurethane Raw Materials: Determination of Total Chlorine in Isocyanates
SIGNIFICANCE AND USE
5.1 These test methods are suitable for use for research or for quality control to determine the total chlorine content of aromatic isocyanates. In some instances total chlorine content may correlate with performance in polyurethane systems.
SCOPE
1.1 These test methods determine the total chlorine content of aromatic isocyanates used as polyurethane raw materials. The difference between the total chlorine content and the hydrolyzable chlorine content (see Test Method D4663) is a measure of the amount of chlorobenzene, o-dichlorobenzene, and other ring-substituted chlorinated products that are present. Both procedures are applicable to a variety of organic compounds but the amount of sample used is varied. (See Note 1.)
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 standard is identical to ISO 26603.
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.
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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: D4661 − 23
Standard Test Methods for
Polyurethane Raw Materials: Determination of Total Chlorine
1
in Isocyanates
This standard is issued under the fixed designation D4661; 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.
3
1. Scope* 2.2 ISO Standard:
ISO 26603 Plastics—Aromatic isocyanates for use in the
1.1 These test methods determine the total chlorine content
production of polyurethanes—Determination of total
of aromatic isocyanates used as polyurethane raw materials.
chlorine
The difference between the total chlorine content and the
hydrolyzable chlorine content (see Test Method D4663) is a
3. Terminology
measure of the amount of chlorobenzene, o-dichlorobenzene,
3.1 Definitions—For definitions of terms used in these test
and other ring-substituted chlorinated products that are present.
Both procedures are applicable to a variety of organic com- methods see Terminology D883.
pounds but the amount of sample used is varied. (See Note 1.)
4. Summary of Test Method
1.2 The values stated in SI units are to be regarded as the
4.1 In each test method, the organic matter in the sample is
standard. The values given in parentheses are for information
destroyed by combustion with oxygen, the organically com-
only.
bined chlorine being converted to ionic chloride. The chloride
1.3 This standard does not purport to address all of the
is determined potentiometrically by titration with silver nitrate
safety concerns, if any, associated with its use. It is the
(AgNO ) solution.
3
responsibility of the user of this standard to establish appro-
4.1.1 Test Method A—The sample is combusted in a pres-
priate safety, health, and environmental practices and deter-
surized ignition vessel.
mine the applicability of regulatory limitations prior to use.
4.1.2 Test Method B—The sample is combusted at atmo-
4
NOTE 1—This standard is identical to ISO 26603.
spheric pressure in a Schöniger oxygen flask.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard- 5. Significance and Use
ization established in the Decision on Principles for the
5.1 These test methods are suitable for use for research or
Development of International Standards, Guides and Recom-
for quality control to determine the total chlorine content of
mendations issued by the World Trade Organization Technical
aromatic isocyanates. In some instances total chlorine content
Barriers to Trade (TBT) Committee.
may correlate with performance in polyurethane systems.
2. Referenced Documents
6. Interferences
2
2.1 ASTM Standards:
6.1 Bromine and iodine, if present, will react with the silver
D883 Terminology Relating to Plastics
nitrate (AgNO ) solution leading to an erroneously high total
3
D1193 Specification for Reagent Water
chlorine value.
D4663 Test Method for Polyurethane Raw Materials: Deter-
mination of Hydrolyzable Chlorine of Isocyanates
7. Reagents and Materials
7.1 Purity of Reagents—Use reagent-grade chemicals in all
tests. Unless otherwise indicated, it is intended that all reagents
1
These test methods are under the jurisdiction of ASTM Committee D20 on
conform to the specifications of the Committee on Analytical
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular
Materials - Plastics and Elastomers.
Reagents of the American Chemical Society where such
Current edition approved March 1, 2023. Published March 2023. Originally
approved in 1987. Last previous edition approved in 2018 as D4661 - 18. DOI:
10.1520/D4661-23.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 4th Floor, New York, NY 10036, http://www.ansi.org.
4
Standards volume information, refer to the standard’s Document Summary page on For information on the Schöniger flask, refer to Microchemie, Springer
the ASTM website. Publishers, Vienna, Austria, Vol 42, 1955, p. 123, or Vol 43, 1956, p. 869.
*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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D4661 − 23
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specifications are available. Other grades are acceptable, nitric acid (HNO , sp gr 1.42) have been added. Any turbidity
3
...
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: D4661 − 18 D4661 − 23
Standard Test Methods for
Polyurethane Raw Materials: Determination of Total Chlorine
1
in Isocyanates
This standard is issued under the fixed designation D4661; 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 These test methods determine the total chlorine content of aromatic isocyanates used as polyurethane raw materials. The
difference between the total chlorine content and the hydrolyzable chlorine content (see Test Method D4663) is a measure of the
amount of chlorobenzene, o-dichlorobenzene-dichlorobenzene, and other ring-substituted chlorinated products that are present.
Both procedures are applicable to a variety of organic compounds but the amount of sample used may have to be is varied. (See
Note 1.)
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 standard is identical to ISO 26603.
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:
D883 Terminology Relating to Plastics
D1193 Specification for Reagent Water
D4663 Test Method for Polyurethane Raw Materials: Determination of Hydrolyzable Chlorine of Isocyanates
3
2.2 ISO Standard:
ISO 26603 Plastics—Aromatic isocyanates for use in the production of polyurethanes—Determination of total chlorine
3. Terminology
3.1 Definitions—For definitions of terms used in these test methods see Terminology D883.
1
These test methods are 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, 2018March 1, 2023. Published August 2018March 2023. Originally approved in 1987. Last previous edition approved in 20132018 as
D4661 - 13.D4661 - 18. DOI: 10.1520/D4661-18.10.1520/D4661-23.
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
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.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
---------------------- Page: 1 ----------------------
D4661 − 23
4. Summary of Test Method
4.1 In each test method, the organic matter in the sample is destroyed by combustion with oxygen, the organically combined
chlorine being converted to ionic chloride. The chloride is determined potentiometrically by titration with silver nitrate (AgNO )
3
solution.
4.1.1 Test Method A—The sample is combusted in a pressurized ignition vessel.
4
4.1.2 Test Method B—The sample is combusted at atmospheric pressure in a Schöniger oxygen flask.
5. Significance and Use
5.1 These test methods can be used are suitable for use for research or for quality control to determine the total chlorine content
of aromatic isocyanates. In some instances total chlorine content may correlate with performance in polyurethane systems.
6. Interferences
6.1 Bromine and iodine, if present, will react with the silver nitrate (AgNO ) solution leading to an erroneously high total chlorine
3
value.
7. Reagents and Materials
7.1 Purity of Reagents—Use reagent-grade chemicals in all tests. Unless otherwise indicated, it is intended that all reagents
conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
5
specifications are available. Other grades are acceptable, p
...
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