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ASTM D4274-05

(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 A-Acetic Anhydride Pressure Bottlerecommended for polyesters.
1.1.2 Test Method B-Phthalic Anhydride Pressure Bottlerecommended for polyethers and polyesters.
1.1.3 Test Method C-Phthalic Anhydride Refluxrecommended for polyethers and polyesters.
1.1.4 Test Method D-Imidazole-Catalyzed Phthalic Anhydride Pressure Bottlerecommended for polyethers, polyesters, polymer polyols, and amine-initiated polyols.
1.1.5 Test Method EImidazole-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 Other ASTM test methods for measuring hydroxyl groups are Test Methods D 1957 and E 222 (see Note 0).
Note 1—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.

General Information

Status
Historical
Publication Date
30-Jun-2005
ICS
83.080.20 - Thermoplastic materials
Technical Committee
D20 - Plastics
Drafting Committee
D20.22 - Cellular Materials - Plastics and Elastomers
Current Stage
Ref Project

Relations

Replaces
ASTM D4274-99 - Standard Test Methods for Testing Polyurethane Raw Materials Determination of Hydroxyl Numbers of Polyols
Effective Date
01-Jul-2005
Replaced By
ASTM D4274-11 - Standard Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols
Effective Date
01-Feb-2011
Referred By
ASTM D6342-22 - Standard Practice for Polyurethane Raw Materials: Determining Hydroxyl Number of Polyols by Near Infrared (NIR) Spectroscopy
Effective Date
01-Jul-2005
Referred By
ASTM E1899-23 - Standard Test Method for Hydroxyl Groups Using Reaction with <emph type="ital">p</emph >-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium Hydroxide
Effective Date
01-Jul-2005

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ASTM D4274-05 - Standard Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of PolyolsASTM D4274-05 - Standard Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols
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ASTM D4274-05 - Standard Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols
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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:D4274–05
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.Anumber 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
polyester and polyether polyols containing primary and sec- D883 Terminology Relating to Plastics
ondary hydroxyl groups. They also apply to many other D1193 Specification for Reagent Water
hydroxyl-containing substances. D1957 Test Method for Hydroxyl Value of Fatty Oils and
3
1.1.1 Test Method A—Acetic Anhydride Pressure Bottle, Acids
recommended for polyesters. E180 Practice for Determining the Precision of ASTM
1.1.2 Test Method B—Phthalic Anhydride Pressure Bottle, Methods for Analysis and Testing of Industrial and Spe-
recommended for polyethers and polyesters. cialty Chemicals
1.1.3 Test Method C—Phthalic Anhydride Reflux, recom- E200 Practice for Preparation, Standardization, and Storage
mended for polyethers and polyesters. of Standard and Reagent Solutions for Chemical Analysis
1.1.4 Test Method D—Imidazole–Catalyzed Phthalic Anhy- E203 TestMethodforWaterUsingVolumetricKarlFischer
dride Pressure Bottle,recommendedforpolyethers,polyesters, Titration
polymer polyols, and amine-initiated polyols. E222 Test Methods for Hydroxyl Groups Using Acetic
2
1.1.5 Test Method E —Imidazole-Catalyzed Pyromellitic Anhydride Acetylation
Dianhydride Esterification, recommended for polyols used for E691 Practice for Conducting an Interlaboratory Study to
flexibleandrigidpolyurethanefoamsandurethaneelastomers. Determine the Precision of a Test Method
4
It is recommended for polyester polyols, polyether polyols, 2.2 ISO Standard:
amine-started polyols, and polymer polyols (polyacrylonitrile/ ISO 6796-1981 Polyglycols for Industrial Use—
copolystyrene-based). Determination of Hydroxyl Number—PhthalicAnhydride
1.2 Other ASTM test methods for measuring hydroxyl Esterification Method
groups are Test Methods D1957 and E222 (see Note 1).
3. Terminology
NOTE 1—Test Method C is essentially similar to ISO6796-1981, but
3.1 Definitions—The terminology in these test methods
therearesomedifferencesintheconcentrationsusedandsomeprocedural
follows the standard terminology defined in Terminology
details. There are currently no data available for comparing the results of
D883.
Test Method C to those of ISO6796-1981.
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
safety concerns, if any, associated with its use. It is the
4. Summary of Test Methods
responsibility of the user of this standard to establish appro-
4.1 Test Method A—The sample is acetylated with a solu-
priate safety and health practices and determine the applica-
tionofaceticanhydrideinpyridineinapressurebottleat98°C.
bility of regulatory limitations prior to use.
Theexcessreagentishydrolyzedwithwaterandtheaceticacid
is titrated with standard sodium hydroxide solution. The
hydroxylcontentiscalculatedfromthedifferenceintitrationof
1
These test methods are under the jurisdiction of ASTM Committee D20 on
the blank and sample solutions. (Warning—Acetic anhydride
Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular
Materials—Plastics and Elastomers.
and pyridine are toxic and flammable. In addition, acetic
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.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Withdrawn. The last approved version of this historical standard is referenced
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM on www.astm.org.
4
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036.
*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 ----------------------
D4274–05
anhydride is corrosive. Proper precautions must be taken in TEST METHOD A—ACETYLATION
handling these reagents.)
8. Interferences
4.2 Te
...

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