ASTM D4663-10
(Test Method)Standard Test Method for Polyurethane Raw Materials Determination of Hydrolyzable Chlorine of Isocyanates
Standard Test Method for Polyurethane Raw Materials Determination of Hydrolyzable Chlorine of Isocyanates
SIGNIFICANCE AND USE
This test method can be used for research or for quality control to characterize toluene diisocyanates. Hydrolyzable chlorine correlates with performance in some polyurethane systems.
SCOPE
1.1 This test method determines the hydrolyzable chlorine content of toluene-2,4-diisocyanate, toluene-2,6-diisocyanate, or mixtures of the two. It is acceptable to apply this test method to other isocyanates of suitable solubility. (See Note 1.) The main sources of hydrolyzable chlorine in the isocyanates are carbamoyl chloride and dissolved phosgene. Both of these compounds react with alcohols and water, forming ureas, carbamates, carbon dioxide, and hydrochloric acid. (See Note 2.)
1.2 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—It is possible that this test method is applicable crude polymeric isocyanates. However, the precision with crude polymeric isocyanates has not been established.
Note 2—There is no known ISO equivalent to this standard.
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Designation: D4663 − 10
StandardTest Method for
Polyurethane Raw Materials: Determination of Hydrolyzable
1
Chlorine of Isocyanates
This standard is issued under the fixed designation D4663; 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* 4. Summary of Test Method
1.1 This test method determines the hydrolyzable chlorine 4.1 The hydrolyzable chlorine reacts with methanol, liber-
content of toluene-2,4-diisocyanate, toluene-2,6-diisocyanate, ating hydrochloric acid. The titratable chlorides are then
ormixturesofthetwo.Itisacceptabletoapplythistestmethod determined potentiometrically using a standard silver nitrate
to other isocyanates of suitable solubility. (See Note 1.) The solution.
main sources of hydrolyzable chlorine in the isocyanates are
5. Significance and Use
carbamoyl chloride and dissolved phosgene. Both of these
compounds react with alcohols and water, forming ureas,
5.1 This test method can be used for research or for quality
carbamates, carbon dioxide, and hydrochloric acid. (See Note
control to characterize toluene diisocyanates. Hydrolyzable
2.)
chlorine correlates with performance in some polyurethane
systems.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
6. Interferences
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6.1 Thiocyanate, cyanide, sulfide, bromide, iodide, or other
bility of regulatory limitations prior to use. substances capable of reacting with silver ion, as well as
substances capable of reducing silver ion in acid solution, will
NOTE 1—It is possible that this test method is applicable crude
interfere with the determination.
polymeric isocyanates. However, the precision with crude polymeric
isocyanates has not been established.
7. Apparatus
NOTE 2—There is no known ISO equivalent to this standard.
7.1 Weighing Bottle, or any device capable of weighing a
2. Referenced Document
liquid by difference to the nearest 0.1 g.
2
2.1 ASTM Standards:
7.2 Hot Plate, with magnetic stirrer.
D883 Terminology Relating to Plastics
7.3 Potentiometric Titrator, or pH meter.
D1193 Specification for Reagent Water
7.4 Combination Silver Billet Electrode.
3. Terminology
3.1 Definitions—For definitions of terms used in this test 8. Reagents and Materials
method see Terminology D883.
8.1 Purity of Reagents—Use reagent grade chemicals in all
3.2 Definitions of Terms Specific to This Standard: tests. Unless otherwise indicated, it is intended that all reagents
3.2.1 hydrolyzable chloride—the low level chlorine- conform to the specifications of the Committee on Analytical
containing components of the isocyanate, such as carbamoyl Reagents of the American Chemical Society where such
3
chlorides, which react with water or alcohol to form HCl. specifications are available. Other grades may be used, pro-
vided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
the determination.
and is the direct responsibility of Subcommittee D20.22 on Cellular Materials -
Plastics and Elastomers.
Current edition approved July 1, 2010. Published August 2010. Originally
3
approved in 1987. Last previous edition approved in 2004 as D4663 - 98(2004). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D4663-10. 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 service@astm.org. 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
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D4663 − 10
8.2 Purity of Water—Unless otherwise indicated, references 11.2 Wash the sides of the beaker with water and remove
to water shall be understood to mean reagent water as defined and wash the stirring bar. Cool the beaker in an ice bath to
by Type I of Specification D1193. about 10°C a
...
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:D4663–98 (Reapproved 2004) Designation:D4663–10
Standard Test Method for
Polyurethane Raw Materials: Determination of Hydrolyzable
1
Chlorine of Isocyanates
This standard is issued under the fixed designation D4663; 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 determines the hydrolyzable chlorine content of toluene-2,4-diisocyanate, toluene-2,6-diisocyanate, or
mixtures of the two. This test method may also be appliedIt is acceptable to apply this test method to other isocyanates of suitable
solubility. (See Note 1.) The main sources of hydrolyzable chlorine in the isocyanates are carbamoyl chloride and dissolved
phosgene. Both of these compounds react with alcohols and water, forming ureas, carbamates, carbon dioxide, and hydrochloric
acid. (See Note 2.)
1.2 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.
NOTE1—This 1—It is possible that this test method may be is applicable with crude polymeric isocyanates. However, the precision with crude
polymeric isocyanates has not been established.
NOTE2—There is no equivalent ISO standard. 2—There is no known ISO equivalent to this standard.
2. Referenced Document
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1193 Specification for Reagent Water
3. Terminology
3.1 Definitions—For definitions of terms used in this test method see Terminology D883.
3.2 Description of Term Specific to This Standard.
3.2.1 hydrolyzable chloride—the low level chlorine-containing components of the isocyanate, such as carbamoyl chlorides,
which react with water or alcohol to form HCl.
4. Summary of Test Method
4.1 The hydrolyzable chlorine reacts with methanol, liberating hydrochloric acid. The titratable chlorides are then determined
potentiometrically using a standard silver nitrate solution.
5. Significance and Use
5.1 This test method can be used for research or for quality control to characterize toluene diisocyanates. Hydrolyzable chlorine
correlates with performance in some polyurethane systems.
6. Interferences
6.1 Thiocyanate, cyanide, sulfide, bromide, iodide, or other substances capable of reacting with silver ion, as well as substances
capable of reducing silver ion in acid solution, will interfere with the determination.
7. Apparatus
7.1 Weighing Bottle, or any device capable of weighing a liquid by difference to the nearest 0.1 g.
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular Materials - Plastics
and Elastomers.
Current edition approved MarchJuly 1, 2004.2010. Published June 2004.August 2010. Originally approved in 1987. Last previous edition approved in 19982004 as
D4663 - 98(2004). DOI: 10.1520/D4663-98R04.10.1520/D4663-10.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
*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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D4663–10
7.2 Hot Plate, with magnetic stirrer.
7.3 Potentiometric Titrator, or pH meter.
7.4 Silver-Silver Chloride Electrode.
7.5Silver or Glass Electrode.
7.6Calomel Electrode. Combination Silver Billet Electrode.
2
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D4663–10
8. Reagents and Materials
8.1 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
3
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.
8.2 Purity of Water—Unless otherwise indicated, references to wat
...
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