ASTM D1652-11
(Test Method)Standard Test Method for Epoxy Content of Epoxy Resins
Standard Test Method for Epoxy Content of Epoxy Resins
SIGNIFICANCE AND USE
The epoxy content of epoxy resins is an important variable in determining their reactivity and the properties of coatings made from them. These test methods may be used to determine the epoxy content of manufactured epoxy resins and confirm the stated epoxy content of purchased epoxy resins.
SCOPE
1.1 This test method covers the procedure for manual and automatic titration of epoxy resins for the quantitative determination of the percent epoxide content from 0.1 – 26 % epoxide.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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. For specific hazard statements, see Section 6.
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Designation:D1652–11
Standard Test Method for
1
Epoxy Content of Epoxy Resins
This standard is issued under the fixed designation D1652; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* 3.1.1 In the Manual Titration Method, the titration is with
standard perchloric acid in the presence of an excess of
1.1 This test method covers the procedure for manual and
tetraethylammonium bromide. Hydrogen bromide generated in
automatic titration of epoxy resins for the quantitative deter-
situ by the addition of perchloric acid to the quaternary
mination of the percent epoxide content from 0.1 – 26 %
ammonium halide rapidly opens the oxirane ring.
epoxide.
3.1.2 In the Automatic Titration Method, the reaction is
1.2 The values stated in SI units are to be regarded as the
measuring the millivolt (MV) potential as perchloric acid is
standard. The values given in parentheses are for information
added, which combines with the bromide to form the hydro-
only.
bromic acid, which reacts with the epoxide group. As the
1.3 This standard does not purport to address all of the
reaction progresses, the potential will gradually increase until
safety concerns, if any, associated with its use. It is the
the reaction nears completion at which point the potential
responsibility of the user of this standard to establish appro-
increases very quickly. The titrator measures the rate of the
priate safety and health practices and determine the applica-
reaction by calculating the change in potential between per-
bility of regulatory limitations prior to use. For specific hazard
chloric acid addition increments. When the change in potential
statements, see Section 6.
begins to decrease, the titrator determines that the titration is
2. Referenced Documents complete. The epoxide content is calculated using the reagent
2
factor entered by the user during standardization, the weight of
2.1 ASTM Standards:
the sample, and the volume of perchloric acid added during
D1193 Specification for Reagent Water
titration.
2.2 Other Documents:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and
4. Significance and Use
3
1910.1200
4.1 The epoxy content of epoxy resins is an important
3. Summary of Test Method
variable in determining their reactivity and the properties of
coatings made from them. These test methods may be used to
3.1 The resin is dissolved in a suitable solvent and the
determine the epoxy content of manufactured epoxy resins and
resulting solution is titrated with hydrogen bromide either
confirm the stated epoxy content of purchased epoxy resins.
directly or in situ. The hydrogen bromide reacts stoichiometri-
cally with epoxy groups to form bromohydrins; therefore, the
5. Reagents
quantity of acid consumed is a measure of the epoxy content.
5.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
all reagents shall conform to the specifications of the Commit-
and Related Coatings, Materials, andApplications and is the direct responsibility of
tee onAnalytical Reagents of theAmerican Chemical Society,
Subcommittee D01.33 on Polymers and Resins.
4
where such specifications are available. Other grades may be
Current edition approved Nov. 1, 2011. Published January 2012. Originally
approved in 1969. Last previous edition approved in 2004 as D1652 – 04. DOI: used, provided it is first ascertained that the reagent is of
10.1520/D1652-11.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Reagent Chemicals, American Chemical Society Specifications, American
Standards volume information, refer to the standard’s Document Summary page on Chemical Society, Washington, DC. For suggestions on the testing of reagents not
the ASTM website. listed by the American Chemical Society, see Analar Standards for Laboratory
3
AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments, Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:// and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
www.access.gpo.gov. 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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...
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:D1652–04 Designation:D1652–11
Standard Test Method for
1
Epoxy Content of Epoxy Resins
This standard is issued under the fixed designation D1652; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope*
1.1 This test method covers the procedure for manual and automatic titration of epoxy resins for the quantitative determination
of the percent epoxide content from 0.1 – 26 % epoxide.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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. For specific hazard statements, see Section 6.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
2.2 Other Documents:
3
OSHA Regulations, 29 CFR,CFR paragraphs 1910.1000 and 1910.1200
3. Summary of Test Method
3.1 The resin is dissolved in a suitable solvent and the resulting solution is titrated with hydrogen bromide either directly or in
situ. The hydrogen bromide reacts stoichiometrically with epoxy groups to form bromohydrins; therefore, the quantity of acid
consumed is a measure of the epoxy content.
3.1.1 In the Manual Titration Method, the titration is with standard perchloric acid in the presence of an excess of
tetraethylammonium bromide. Hydrogen bromide generated in situ by the addition of perchloric acid to the quaternary ammonium
halide rapidly opens the oxirane ring.
3.1.2 In the Automatic Titration Method, the reaction is measuring the millivolt (MV) potential as perchloric acid is added,
which combines with the bromide to form the hydrobromic acid, which reacts with the epoxide group.As the reaction progresses,
the potential will gradually increase until the reaction nears completion at which point the potential increases very quickly. The
titrator measures the rate of the reaction by calculating the change in potential between perchloric acid addition increments. When
the change in potential begins to decrease, the titrator determines that the titration is complete. The epoxide content is calculated
using the reagent factor entered by the user during standardization, the weight of the sample, and the volume of perchloric acid
added during titration.
4. Significance and Use
4.1 The epoxy content of epoxy resins is an important variable in determining their reactivity and the properties of coatings
made from them. These test methods may be used to determine the epoxy content of manufactured epoxy resins and confirm the
stated epoxy content of purchased epoxy resins.
5. Reagents
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.33 on Polymers and Resins.
CurrenteditionapprovedNovemberNov.1,2004.2011.PublishedDecember2004.January2012.Originallyapprovedin1969.Lastpreviouseditionapprovedin19972004
as D1652–97.D1652 – 04. DOI: 10.1520/D1652-04.10.1520/D1652-11.
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 U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
*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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D1652–11
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such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficien
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