ASTM D4662-15
(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
5.1 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 are typically 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 − 15
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* room temperature with alcoholic potassium hydroxide
solution, to the end point indicated by the color change of
1.1 These test methods measure the acidic and basic con-
added phenolphthalein. Alkalinity numbers are determined by
stituents in polyols and other materials of high acidity or
back-titration after adding excess hydrochloric acid. The end-
alkalinity that are soluble in mixtures of toluene and ethyl
point of these titrations also can be determined potentiometri-
alcohol. These test methods do not apply to polyethers. (See
cally.
Note 1.)
1.2 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 These test methods are suitable for quality control, as
responsibility of the user of this standard to establish appro-
specification tests, and for research. The acid and alkalinity
priate safety and health practices and determine the applica-
numbersindicatetheextentofareactionwithacids.Theresults
bility of regulatory limitations prior to use.
are measures of batch-to-batch uniformity and are typically
NOTE 1—There is no known ISO equivalent to this standard.
used as correction factors in calculating hydroxyl number.
2. Referenced Documents
6. Reagents and Materials
2
2.1 ASTM Standards:
6.1 Purity of Reagents—Use reagent-grade chemicals in all
D883 Terminology Relating to Plastics
tests. Unless otherwise indicated, it is intended that all reagents
D1193 Specification for Reagent Water
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society where such
3. Terminology
3
specifications are available. Other grades are allowed, pro-
3.1 Definitions—For definitions of terms used in these test
vided it is first ascertained that the reagent is of sufficiently
methods see Terminology D883.
high purity to permit its use without lessening the accuracy of
the determination.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 acid number—the quantity of base, expressed in mil-
6.2 Purity of Water—Unless otherwise indicated, references
ligramsofpotassiumhydroxide,thatisrequiredtotitrateacidic
to water shall be understood to mean reagent water as defined
constituents present in1gof sample.
by Type I of Specification D1193.
3.2.2 alkalinity number—the quantity of base, expressed as
6.3 Ethyl Alcohol, 95 %.
milligrams of potassium hydroxide, present in1gof sample.
6.4 Hydrochloric Acid (0.1 N)—Prepare a 0.1 N solution of
hydrochloric acid (HCl). Standardization is unnecessary.
4. Summary of Test Method
6.5 Phenolphthalein Indicator Solution—Dissolve 0.5 g of
4.1 The sample is dissolved in a mixture of toluene and
phenolphthalein in 100 mL of a mixture of equal volumes of
ethyl alcohol. The resulting single-phase solution is titrated at
water and ethyl alcohol. Add a slight excess of 0.1 N NaOH
solution (pink color) and then just neutralize (colorless) with
1
These test methods are under the jurisdiction of ASTM Committee D20 on
0.1 N HCl.
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular
Materials - Plastics and Elastomers.
Current edition approved Sept. 1, 2015. Published September 2015. Originally
ε1
3
approved in 1987. Last previous edition approved in 2011 as D4662 - 08(2011) . Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D4662-15. 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.
*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
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D4662 − 15
6.6 Potassium Hydroxide, Standard Alcoholic Solution (0.1
B = KOH solution required for titration of the blank, mL,
N)—Dissolve 5.61 g of pot
...
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.
´1
Designation: D4662 − 08 (Reapproved 2011) D4662 − 15
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
ε NOTE—Editorially added Report and Precision and Bias information following Test Method A in February 2011.
1. Scope 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1193 Specification for Reagent Water
3. Terminology
3.1 Definitions—For definitions of terms used in these test methods see Terminology D883.
3.2 Definitions 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 in 1 g of sample.
3.2.2 alkalinity number—the quantity of base, expressed as milligrams of potassium hydroxide, present in 1 g of sample.
4. Summary of Test Method
4.1 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
5.1 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 beare typically 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
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.
Current edition approved Feb. 1, 2011Sept. 1, 2015. Published March 2011September 2015. Originally approved in 1987. Last previous edition approved in 20082011
ε1
as D4662 - 08.D4662 - 08(2011) . DOI: 10.1520/D4662-08R11E01.10.1520/D4662-15.
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.
*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 ----------------------
D4662 − 15
3
specifications are available. Other grades may be used are allowed, provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of the determination.
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 D1193.
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 of phenolphthalein in 100 mL of a mixture of equal volumes of water
and ethyl alcohol. Add a slight excess of 0.1 N NaOH solution (pink color) and then just neutralize (colorless) with 0.1 N HCl.
6.6 Potas
...
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