ASTM D4274-11
(Test Method)Standard Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols
Standard Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols
SIGNIFICANCE AND USE
These test methods are suitable for research and as quality control and specification tests. It is necessary to know the hydroxyl contents of polyols in order to formulate polyurethane systems.
SCOPE
1.1 These test methods measure the hydroxyl groups in polyester and polyether polyols containing primary and secondary hydroxyl groups. They also apply to many other hydroxyl-containing substances.
1.1.1 Test Method AAcetic Anhydride Pressure Bottle, recommended for polyesters.
1.1.2 Test Method BPhthalic Anhydride Pressure Bottle, recommended for polyethers and polyesters.
1.1.3 Test Method CPhthalic Anhydride Reflux, recommended for polyethers and polyesters.
1.1.4 Test Method DImidazole–Catalyzed Phthalic Anhydride Pressure Bottle, recommended for polyethers, polyesters, polymer polyols, and amine-initiated polyols.
1.1.5 Test Method E—Imidazole-Catalyzed Pyromellitic Dianhydride Esterification, recommended for polyols used for flexible and rigid polyurethane foams and urethane elastomers. It is recommended for polyester polyols, polyether polyols, amine-started polyols, and polymer polyols (polyacrylonitrile/copolystyrene-based).
1.2 Another ASTM test method for measuring hydroxyl groups is Test Method E222.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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—This standard and ISO 6796 address the same subject matter, but differ in technical content.
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Designation: D4274 − 11
StandardTest Methods for Testing
Polyurethane Raw Materials: Determination of Hydroxyl
1
Numbers of Polyols
This standard is issued under the fixed designation D4274; 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* 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 These test methods measure the hydroxyl groups in
D883 Terminology Relating to Plastics
polyester and polyether polyols containing primary and sec-
D1193 Specification for Reagent Water
ondary hydroxyl groups. They also apply to many other
E180 Practice for Determining the Precision of ASTM
hydroxyl-containing substances.
Methods for Analysis and Testing of Industrial and Spe-
1.1.1 Test Method A—Acetic Anhydride Pressure Bottle,
3
cialty Chemicals (Withdrawn 2009)
recommended for polyesters.
E200 Practice for Preparation, Standardization, and Storage
1.1.2 Test Method B—Phthalic Anhydride Pressure Bottle,
of Standard and Reagent Solutions for ChemicalAnalysis
recommended for polyethers and polyesters. E203 Test Method for Water Using Volumetric Karl Fischer
Titration
1.1.3 Test Method C—Phthalic Anhydride Reflux, recom-
E222 Test Methods for Hydroxyl Groups Using Acetic
mended for polyethers and polyesters.
Anhydride Acetylation
1.1.4 Test Method D—Imidazole–Catalyzed Phthalic Anhy-
E691 Practice for Conducting an Interlaboratory Study to
dride Pressure Bottle,recommendedforpolyethers,polyesters,
Determine the Precision of a Test Method
polymer polyols, and amine-initiated polyols.
4
2.2 ISO Standard:
1.1.5 Test Method E—Imidazole-Catalyzed Pyromellitic Di-
ISO 6796 Polyglycols for Industrial Use—Determination of
anhydride Esterification, recommended for polyols used for
Hydroxyl Number—Phthalic Anhydride Esterification
flexible and rigid polyurethane foams and urethane elastomers.
Method
It is recommended for polyester polyols, polyether polyols,
3. Terminology
amine-started polyols, and polymer polyols (polyacrylonitrile/
copolystyrene-based).
3.1 Definitions—The terminology in these test methods
follows the standard terminology defined in Terminology
1.2 Another ASTM test method for measuring hydroxyl
D883.
groups is Test Method E222.
3.2 Definitions of Terms Specific to This Standard—There
1.3 The values stated in SI units are to be regarded as the
are no terms in these test methods that require new or other
standard.
than dictionary definitions.
1.4 This standard does not purport to address all of the
4. Summary of Test Methods
safety concerns, if any, associated with its use. It is the
4.1 Test Method A—Thesampleisacetylatedwithasolution
responsibility of the user of this standard to establish appro-
ofaceticanhydrideinpyridineinapressurebottleat98°C.The
priate safety and health practices and determine the applica-
excess reagent is hydrolyzed with water and the acetic acid is
bility of regulatory limitations prior to use.
titratedwithstandardsodiumhydroxidesolution.Thehydroxyl
NOTE 1—This standard and ISO 6796 address the same subject matter,
content is calculated from the difference in titration of the
but differ in technical content.
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
1
These test methods are under the jurisdiction of ASTM Committee D20 on Standards volume information, refer to the standard’s Document Summary page on
Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular the ASTM website.
3
Materials - Plastics and Elastomers. The last approved version of this historical standard is referenced on
Current edition approved Feb. 1, 2011. Published March 2011. Originally www.astm.org.
4
approved in 1988. Last previous edition approved in 2005 as D4274 - 05. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D4274-11. 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 ----------------------
D4274 − 11
blank and sample solutions. (Warning—Acetic anhydride and TEST METHOD A—ACETYLATION
pyridine are toxic and flammable. In addition, acetic anhydride
is corrosive. Proper precautions must be taken in handling 8. Interferences
these reagents. ).
8.1 Dry the sample if it contains more than 0.2 % water.
4.2 Test Method B—The hydroxyl group is esterified with a More than that will interfere by destroying the esterification
reagents.
so
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D4274–05 Designation:D4274–11
Standard Test Methods for Testing
Polyurethane Raw Materials: Determination of Hydroxyl
1
Numbers of Polyols
This standard is issued under the fixed designation D4274; 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 measure the hydroxyl groups in polyester and polyether polyols containing primary and secondary
hydroxyl groups. They also apply to many other hydroxyl-containing substances.
1.1.1 Test Method A—Acetic Anhydride Pressure Bottle, recommended for polyesters.
1.1.2 Test Method B—Phthalic Anhydride Pressure Bottle, recommended for polyethers and polyesters.
1.1.3 Test Method C—Phthalic Anhydride Reflux, recommended for polyethers and polyesters.
1.1.4 Test Method D—Imidazole–Catalyzed Phthalic Anhydride Pressure Bottle, recommended for polyethers, polyesters,
polymer polyols, and amine-initiated polyols.
1.1.5 Test Method E—Imidazole-Catalyzed Pyromellitic Dianhydride Esterification, recommended for polyols used for flexible
and rigid polyurethane foams and urethane elastomers. It is recommended for polyester polyols, polyether polyols, amine-started
polyols, and polymer polyols (polyacrylonitrile/copolystyrene-based).
1.2Other ASTM test methods for measuring hydroxyl groups are Test Methods D1957 and
1.2 Another ASTM test method for measuring hydroxyl groups is Test Method E222(see Note 1).
NOTE1—Test Method C is essentially similar to ISO 6796-1981, but there are some differences in the concentrations used and some procedural details.
There are currently no data available for comparing the results of Test Method C to those of ISO 6796-1981.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 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—This standard and ISO 6796 address the same subject matter, but differ in technical content.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1193 Specification for Reagent Water D1957Test Method for Hydroxyl Value of Fatty Oils and Acids
E180 Practice for Determining the Precision ofASTM Methods forAnalysis and Testing of Industrial and Specialty Chemicals
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
E203 Test Method for Water Using Volumetric Karl Fischer Titration
E222 Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 ISO Standard:
ISO 6796-1981ISO 6796 Polyglycols for Industrial Use—Determination of Hydroxyl Number—Phthalic Anhydride Esterifi-
cation Method
1
These test methods are 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, 2005. Published August 2005. Originally approved in 1988. Last previous edition approved in 1999 as D4274-99. DOI:
10.1520/D4274-05.on Cellular Materials - Plastics and Elastomers.
Current edition approved Feb. 1, 2011. Published March 2011. Originally approved in 1988. Last previous edition approved in 2005 as D4274 - 05. DOI:
10.1520/D4274-11.
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.
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 ----------------------
D4274–11
3. Terminology
3.1 Definitions—The terminology in these test methods follows the standard terminology defined in Terminology D883.
3.2 Definitions of Terms Specific to This Standard—There are no terms in thes
...
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