ASTM D4663-15
(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
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.
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 to crude polymeric isocyanates. However, the precision with crude polymeric isocyanates has not been established.
Note 2: This standard is identical to ISO 15028.
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Designation: D4663 − 15
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* 3. Terminology
1.1 This test method determines the hydrolyzable chlorine 3.1 Definitions—For definitions of terms used in this test
content of toluene-2,4-diisocyanate, toluene-2,6-diisocyanate, method see Terminology D883.
ormixturesofthetwo.Itisacceptabletoapplythistestmethod
3.2 Definitions of Terms Specific to This Standard:
to other isocyanates of suitable solubility. (See Note 1.) The
3.2.1 hydrolyzable chloride—the low level chlorine-
main sources of hydrolyzable chlorine in the isocyanates are
containing components of the isocyanate, such as carbamoyl
carbamoyl chloride and dissolved phosgene. Both of these
chlorides, which react with water or alcohol to form HCl.
compounds react with alcohols and water, forming ureas,
4. Summary of Test Method
carbamates, carbon dioxide, and hydrochloric acid. (See Note
2.)
4.1 The hydrolyzable chlorine reacts with methanol, liber-
ating hydrochloric acid. The titratable chlorides are then
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the determined potentiometrically using a standard silver nitrate
solution.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use.
5.1 This test method can be used for research or for quality
NOTE 1—It is possible that this test method is applicable to crude
control to characterize toluene diisocyanates. Hydrolyzable
polymeric isocyanates. However, the precision with crude polymeric
chlorine correlates with performance in some polyurethane
isocyanates has not been established.
NOTE 2—This standard is identical to ISO 15028.
systems.
2. Referenced Document
6. Interferences
2
2.1 ASTM Standards: 6.1 Thiocyanate, cyanide, sulfide, bromide, iodide, or other
D883 Terminology Relating to Plastics
substances capable of reacting with silver ions, as well as
D1193 Specification for Reagent Water
substances capable of reducing silver ions in acid solution, will
2.2 ISO Standards: interfere with the determination.
ISO 15028 Plastics—Aromatic Isocyanates for Use in the
7. Apparatus
Production of Polyurethanes—Determination of Hydroly-
3
sable Chlorine
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 7.2 Hot Plate, with magnetic stirrer.
and is the direct responsibility of Subcommittee D20.22 on Cellular Materials -
7.3 Potentiometric Titrator, or pH meter.
Plastics and Elastomers.
Current edition approved May 1, 2015. Published June 2015. Originally
7.4 Combination Silver Billet Electrode.
approved in 1987. Last previous edition approved in 2010 as D4663 - 10. DOI:
10.1520/D4663-15.
8. Reagents and Materials
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
8.1 Purity of Reagents—Use reagent grade chemicals in all
Standards volume information, refer to the standard’s Document Summary page on
tests. Unless otherwise indicated, it is intended that all reagents
the ASTM website.
3 conform to the specifications of the Committee on Analytical
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org. Reagents of the American Chemical Society where such
*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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---------------------- Page: 1 ----------------------
D4663 − 15
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NOTE3—Ifthehydrolyzablechlorinecontentisexpectedtobelessthan
specifications are available. Other grades may be used, pro-
0.01 %, use 18 to 22 g of sample.
vided it is first ascertained that the reagent is of sufficiently
NOTE 4—Some isocyanates will not react readily and slight warming
high purity to permit its use without lessening the accuracy of
may be necessary to initiate reaction. Other isocyanates may react, as
the determination.
indicated by warming of reactants, but may not form crystals.
NOTE 5—Add the water quickly to keep the reactants from solidifying
8.2 Purity of Water—Unless otherwise indicated,
...
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 − 10 D4663 − 15
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. 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 to 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.This standard is identical to ISO 15028.
2. Referenced Document
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1193 Specification for Reagent Water
2.2 ISO Standards:
ISO 15028 Plastics—Aromatic Isocyanates for Use in the Production of Polyurethanes—Determination of Hydrolysable
3
Chlorine
3. Terminology
3.1 Definitions—For definitions of terms used in this test method see Terminology D883.
3.2 Definitions of Terms 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.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular Materials - Plastics
and Elastomers.
Current edition approved July 1, 2010May 1, 2015. Published August 2010June 2015. Originally approved in 1987. Last previous edition approved in 20042010 as
D4663 - 98D4663 - 10.(2004). DOI: 10.1520/D4663-10.10.1520/D4663-15.
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 ----------------------
D4663 − 15
6. Interferences
6.1 Thiocyanate, cyanide, sulfide, bromide, iodide, or other substances capable of reacting with silver ion,ions, as well as
substances capable of reducing silver ionions 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.
7.2 Hot Plate, with magnetic stirrer.
7.3 Potentiometric Titrator, or pH meter.
7.4 Combination Silver Billet Electrode.
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
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.
...
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