ASTM D4661-13
(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 can be used 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 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 may have to be 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 and health practices and determine the applicability of regulatory limitations prior to use.Note 1—There is no known ISO equivalent to this standard.
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Designation: D4661 − 13
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* bined chlorine being converted to ionic chloride. The chloride
is determined potentiometrically by titration with silver nitrate
1.1 These test methods determine the total chlorine content
(AgNO ) solution.
3
of aromatic isocyanates used as polyurethane raw materials.
4.1.1 Test Method A—The sample is combusted in a pres-
The difference between the total chlorine content and the
surized oxygen bomb.
hydrolyzable chlorine content (see Test Method D4663)isa
4.1.2 Test Method B—The sample is combusted at atmo-
measure of the amount of o-dichlorobenzene and other ring-
3
spheric pressure in a Schöniger oxygen flask.
substituted chlorinated products that are present. Both proce-
dures are applicable to a variety of organic compounds but the
5. Significance and Use
amount of sample used may have to be varied. (See Note 1.)
5.1 These test methods can be used for research or for
1.2 The values stated in SI units are to be regarded as the
quality control to determine the total chlorine content of
standard. The values given in parentheses are for information
aromatic isocyanates. In some instances total chlorine content
only.
may correlate with performance in polyurethane systems.
1.3 This standard does not purport to address all of the
6. Interferences
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 6.1 Bromine and iodine, if present, will react with the silver
priate safety and health practices and determine the applica- nitrate (AgNO ) solution leading to an erroneously high total
3
bility of regulatory limitations prior to use. chlorine value.
NOTE 1—There is no known ISO equivalent to this standard.
7. Reagents and Materials
2. Referenced Documents
7.1 Purity of Reagents—Use reagent-grade chemicals in all
2
tests. Unless otherwise indicated, it is intended that all reagents
2.1 ASTM Standards:
conform to the specifications of the Committee on Analytical
D883 Terminology Relating to Plastics
Reagents of the American Chemical Society where such
D1193 Specification for Reagent Water
4
specifications are available. Other grades may be used, pro-
D4663 Test Method for Polyurethane Raw Materials: Deter-
vided it is first ascertained that the reagent is of sufficiently
mination of Hydrolyzable Chlorine of Isocyanates
high purity to permit its use without lessening the accuracy of
3. Terminology
the determination.
3.1 Definitions—For definitions of terms used in these test
7.2 Purity of Water—Unless otherwise indicated, references
methods see Terminology D883.
to water shall be understood to mean reagent water as defined
by Type I of Specification D1193.
4. Summary of Test Method
4.1 In each test method, the organic matter in the sample is 8. Sampling
destroyed by combustion with oxygen, the organically com-
8.1 Since organic isocyanates react with atmospheric
moisture, take special precautions in sampling. Usual sampling
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
3
Materials - Plastics and Elastomers. For information on the Schöniger flask, refer to Microchemie, Springer
Current edition approved Nov. 1, 2013. Published November 2013. Originally Publishers, Vienna, Austria, Vol 42, 1955, p. 123, or Vol 43, 1956, p. 869.
4
approved in 1987. Last previous edition approved in 2009 as D4661 - 09. DOI: Reagent Chemicals, American Chemical Society Specifications, American
10.1520/D4661-13. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contactASTM Customer Service at service@astm.org. ForAnnual Book ofASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
*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 − 13
methods, even when c
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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 − 09 D4661 − 13
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 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 may have to be 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 and health practices and determine the applicability of regulatory
limitations prior to use.
NOTE 1—There is no equivalent ISO standard. known ISO equivalent to this standard.
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. Terminology
3.1 Definitions—For definitions of terms used in these test methods see Terminology D883.
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 oxygen bomb.
3
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 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
3
chlorine value.
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 Feb. 1, 2009Nov. 1, 2013. Published March 2009November 2013. Originally approved in 1987. Last previous edition approved in 20032009 as
D4661 - 03.D4661 - 09. DOI: 10.1520/D4661-09.10.1520/D4661-13.
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
For information on the Schöniger flask, refer to Microchemie, Springer 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
---------------------- Page: 1 ----------------------
D4661 − 13
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
4
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type I of Specification D1193.
8. Sampling
8.1 Since organic isocyanates react with atmospheric moisture, take special precautions in sampling. (Warning—Organic
isocyanates are toxic when they are absorbed throug
...
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