ASTM D4274-16

Standard Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols

SIGNIFICANCE AND USE
5.1 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 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).  
1.2 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, ISO 14900 and ISO 6796 address the same subject matter, but differ in technical content.

General Information

• Status: Historical
• Publication Date: 31-Mar-2016
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.22 - Cellular Materials - Plastics and Elastomers

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4274 − 16
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* 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,
ISO 14900 Plastics—Polyols for Use in the Production of
amine-started polyols, and polymer polyols (polyacrylonitrile/
Polyurethane—Determination of Hydroxyl Number
copolystyrene-based).
3. Terminology
1.2 Another ASTM test method for measuring hydroxyl
3.1 Definitions—The terminology in these test methods
groups is Test Method E222.
follows the standard terminology defined in Terminology
1.3 The values stated in SI units are to be regarded as the D883.
standard.
3.2 Definitions of Terms Specific to This Standard—There
are no terms in these test methods that require new or other
1.4 This standard does not purport to address all of the
than dictionary definitions.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Methods
priate safety and health practices and determine the applica-
4.1 Test Method A—Thesampleisacetylatedwithasolution
bility of regulatory limitations prior to use.
ofaceticanhydrideinpyridineinapressurebottleat98°C.The
NOTE 1—This standard, ISO 14900 and ISO 6796 address the same
excess reagent is hydrolyzed with water and the acetic acid is
subject matter, but differ in technical content.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. 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 April 1, 2016. Published April 2016. Originally www.astm.org.
4
approved in 1988. Last previous edition approved in 2011 as D4274 - 11. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D4274-16. 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 − 16
titratedwithstandardsodiumhydroxidesolution.Thehydroxyl 7. Sampling
content is calculated from the difference in titration of the
7.1 Polyesters and polyethers usually contain molecules
blank and sample solutions. (Warning—Acetic anhydride and
covering an appreciable range of molecular weights. These
pyridine are toxic and flammable. In addition, acetic anhydride
have a tendency to fractionate during solidification. Unless the
is c
...

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: D4274 − 11 D4274 − 16
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).
1.2 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 standard, ISO 14900 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
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
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
4
2.2 ISO Standard:
ISO 6796 Polyglycols for Industrial Use—Determination of Hydroxyl Number—Phthalic Anhydride Esterification Method
ISO 14900 Plastics—Polyols for Use in the Production of Polyurethane—Determination of Hydroxyl Number
3. Terminology
3.1 Definitions—The terminology in these test methods follows the standard terminology defined in Terminology D883.
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 Feb. 1, 2011April 1, 2016. Published March 2011April 2016. Originally approved in 1988. Last previous edition approved in 20052011 as
D4274 - 05.D4274 - 11. DOI: 10.1520/D4274-11.10.1520/D4274-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
4
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 − 16
3.2 Definitions of Terms Specific to This Standard—There are no terms in these test methods that require new or other than
dictionary definitions.
4. Summary of Test Methods
4.1 Test Method A—The sample is acetylated with a solution of acetic anhydride in pyridine in a pressure bottle at 98°C. The
excess reagent is hydrolyzed with water and the acetic acid is titrated with standard sodium hydroxide solution. The hydroxyl
content i
...