ASTM D4662-08
(Test Method)Standard Test Methods for Polyurethane Raw Materials: Determination of Acid and Alkalinity Numbers of Polyols
Standard Test Methods for Polyurethane Raw Materials: Determination of Acid and Alkalinity Numbers of Polyols
SIGNIFICANCE AND USE
These test methods are suitable for quality control, as specification tests, and for research. The acid and alkalinity numbers indicate the extent of a reaction with acids. The results are measures of batch-to-batch uniformity and may be used as correction factors in calculating hydroxyl number.
SCOPE
1.1 These test methods measure the acidic and basic constituents in polyols and other materials of high acidity or alkalinity that are soluble in mixtures of toluene and ethyl alcohol. These test methods do not apply to polyethers. (See Note 1.)
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—There is no known ISO equivalent to this standard.
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Designation:D4662–08
Standard Test Methods for
Polyurethane Raw Materials: Determination of Acid and
1
Alkalinity Numbers of Polyols
This standard is issued under the fixed designation D4662; 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 phenolphthalein. Alkalinity numbers are determined by back-
titration after adding excess hydrochloric acid.The endpoint of
1.1 These test methods measure the acidic and basic con-
these titrations also can be determined potentiometrically.
stituents in polyols and other materials of high acidity or
alkalinity that are soluble in mixtures of toluene and ethyl
5. Significance and Use
alcohol. These test methods do not apply to polyethers. (See
5.1 These test methods are suitable for quality control, as
Note 1.)
specification tests, and for research. The acid and alkalinity
1.2 This standard does not purport to address all of the
numbersindicatetheextentofareactionwithacids.Theresults
safety concerns, if any, associated with its use. It is the
are measures of batch-to-batch uniformity and may be used as
responsibility of the user of this standard to establish appro-
correction factors in calculating hydroxyl number.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
6. Reagents and Materials
NOTE 1—There is no known ISO equivalent to this standard.
6.1 Purity of Reagents—Use reagent-grade chemicals in all
tests. Unless otherwise indicated, it is intended that all reagents
2. Referenced Documents
conform to the specifications of the Committee on Analytical
2
2.1 ASTM Standards:
Reagents of the American Chemical Society where such
D883 Terminology Relating to Plastics 3
specifications are available. Other grades may be used pro-
D1193 Specification for Reagent Water
vided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
3. Terminology
the determination.
3.1 Definitions—For definitions of terms used in these test
6.2 Purity of Water—Unless otherwise indicated, references
methods see Terminology D883.
to water shall be understood to mean reagent water as defined
3.2 Descriptions of Terms Specific to This Standard:
by Type I of Specification D1193.
3.2.1 acid number—the quantity of base, expressed in
6.3 Ethyl Alcohol, 95 %.
milligrams of potassium hydroxide, that is required to titrate
6.4 Hydrochloric Acid (0.1 N)—Prepare a 0.1 N solution of
acidic constituents present in1gof sample.
hydrochloric acid (HCl). Standardization is unnecessary.
3.2.2 alkalinity number—the quantity of base, expressed as
6.5 Phenolphthalein Indicator Solution—Dissolve 0.5 g of
milligrams of potassium hydroxide, present in1gof sample.
phenolphthalein in 100 mL of a mixture of equal volumes of
water and ethyl alcohol. Add a slight excess of 0.1 N NaOH
4. Summary of Test Method
solution (pink color) and then just neutralize (colorless) with
4.1 The sample is dissolved in a mixture of toluene and
0.1 N HCl.
ethyl alcohol. The resulting single-phase solution is titrated at
6.6 Potassium Hydroxide, Standard Alcoholic Solution (0.1
room temperature with alcoholic potassium hydroxide solu-
N)—Dissolve 5.61 g of potassium hydroxide (KOH) in 10 mL
tion,totheendpointindicatedbythecolorchangeoftheadded
of carbon dioxide-free water and dilute to 1 L with ethyl
alcohol. Store the solution in a chemical-resistant dispensing
bottle protected by a guard tube containing soda-lime or
1
These test methods are under the jurisdiction of ASTM Committee D20 on
ascarite. Standardize frequently enough to detect changes of
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular
Materials - Plastics and Elastomers.
Current edition approved Aug. 1, 2008. Published September 2008. Originally
3
approved in 1987. Last previous edition approved in 2003 as D4662 - 03. DOI: Reagent Chemicals, American Chemical Society Specifications, American
10.1520/D4662-08. 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. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C7
...
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:D 4662–03 Designation:D 4662–08
Standard Test Methods for
Polyurethane Raw Materials: Determination of Acid and
1
Alkalinity Numbers of Polyols
This standard is issued under the fixed designation D 4662; 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 *
1.1These1.1 These test methods measure the acidic and basic constituents in polyols and other materials of high acidity or
alkalinity that are soluble in mixtures of toluene and ethyl alcohol. These test methods do not apply to polyethers. (See Note 1.)
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—There is no equivalent ISO standard. 1—There is no known ISO equivalent to this standard.
2. Referenced Documents
2
2.1 ASTM Standards:
D 883 Terminology Relating to Plastics
D 1193 Specification for Reagent Water
3. Terminology
3.1 Definitions—For definitions of terms used in these test methods see Terminology D 883.
3.2 Descriptions of Terms Specific to This Standard:
3.2.1 acid number—the quantity of base, expressed in milligrams of potassium hydroxide, that is required to titrate acidic
constituents present in1gof sample.
3.2.2 alkalinity number—the quantity of base, expressed as milligrams of potassium hydroxide, present in1gof sample.
4. Summary of Test Method
4.1The4.1 The sample is dissolved in a mixture of toluene and ethyl alcohol. The resulting single-phase solution is titrated at
room temperature with alcoholic potassium hydroxide solution, to the end point indicated by the color change of the added
phenolphthalein.Alkalinity numbers are determined by back-titration after adding excess hydrochloric acid. The endpoint of these
titrations also can be determined potentiometrically.
5. Significance and Use
5.1These5.1 These test methods are suitable for quality control, as specification tests, and for research. The acid and alkalinity
numbers indicate the extent of a reaction with acids. The results are measures of batch-to-batch uniformity and may be used as
correction factors in calculating hydroxyl number.
6. Reagents and Materials
6.1 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.
1
These test methods are under the jurisdiction of ASTM Committee D20 on Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular Materials -
Plastics and Elastomers.
CurrenteditionapprovedNovemberAug.1,2003.2008.PublishedJanuary2004.September2008.Originallyapprovedin1987.Lastpreviouseditionapprovedin19982003
as D4662-98.D 4662 - 03.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, 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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D 4662–08
6.2 Purity of Water— Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type I of Specification D 1193.
6.3 Ethyl Alcohol, 95 %.
6.4 Hydrochloric Acid (0.1 N)—Prepare a 0.1 N solution of hydrochloric acid (HCl). Standardization is unnecessary.
6.5 Phenolphthalein Indicator Solution —Dissolve 0.5 g o
...
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