ASTM D4661-03

Standard Test Methods for Polyurethane Raw Materials: Determination of Total Chlorine in Isocyanates

SIGNIFICANCE AND USE
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 D 4663) 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 brackets 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.

General Information

• Status: Historical
• Publication Date: 31-Oct-2003
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.22 - Cellular Materials - Plastics and Elastomers

Relations

• Replaces: ASTM D4661-98 - Standard Test Methods for Polyurethane Raw Materials Determination of Total Chlorine in Isocyanates
• Effective Date: 01-Nov-2003
• Replaced By: ASTM D4661-09 - Standard Test Methods for Polyurethane Raw Materials: Determination of Total Chlorine in Isocyanates
• Effective Date: 01-Feb-2009
• Referred By: ASTM D1786-21 - Standard Specification for Toluene Diisocyanate
• Effective Date: 01-Nov-2003

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D 4661–03
Standard Test Methods for
Polyurethane Raw Materials: Determination of Total Chlorine
1
in Isocyanates
This standard is issued under the fixed designation D 4661; 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 (e) 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 D 4663) is a
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.Thevaluesgiveninbracketsareforinformationonly.
aromatic isocyanates. In some instances total chlorine content
1.3 This standard does not purport to address all of the
may correlate with performance in polyurethane systems.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
6. Interferences
priate safety and health practices and determine the applica-
6.1 Bromine and iodine, if present, will react with the silver
bility of regulatory limitations prior to use.
nitrate (AgNO ) solution leading to an erroneously high total
3
NOTE 1—There is no equivalent ISO standard.
chlorine value.
2. Referenced Documents
7. Reagents and Materials
2
2.1 ASTM Standards:
7.1 Purity of Reagents—Use reagent-grade chemicals in all
D 883 Terminology Relating to Plastics
tests. Unless otherwise indicated, it is intended that all reagents
D 1193 Specification for Reagent Water
conform to the specifications of the Committee on Analytical
D 4663 Test Method for Polyurethane Raw Materials: De-
Reagents of the American Chemical Society where such
4
termination of Hydrolyzable Chlorine of Isocyanates
specifications are available. Other grades may be used, pro-
vided it is first ascertained that the reagent is of sufficiently
3. Terminology
high purity to permit its use without lessening the accuracy of
3.1 Definitions—For definitions of terms used in these test
the determination.
methods see Terminology D 883.
7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water as defined
4. Summary of Test Method
by Type I of Specification D 1193.
4.1 In each test method, the organic matter in the sample is
destroyed by combustion with oxygen, the organically com-
1
These test methods are under the jurisdiction of ASTM Committee D20 on
3
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular For information on the Schöniger flask, refer to Microchemie, Springer
Plastics. Publishers, Vienna, Austria, Vol 42, 1955, p. 123, or Vol 43, 1956, p. 869.
4
Current edition approved November 1, 2003. Published January 2004. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1987. Last previous edition approved in 1998 as D 4661 - 98. 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
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM 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

---------------------- Page: 1 ----------------------
D 4661–03
8. Sampling 11.5 Sodium Carbonate Solution (50 g/L)—Dissolve 135 g
of sodium carbonate decahydrate (Na CO · 10H O) in water
2 3 2
8.1 Since organic isocyanates react with atmospheric mois-
and dilute to 1 L.
t
...