ASTM D1726-11
(Test Method)Standard Test Methods for Hydrolyzable Chloride Content of Liquid Epoxy Resins
Standard Test Methods for Hydrolyzable Chloride Content of Liquid Epoxy Resins
SIGNIFICANCE AND USE
The hydrolyzable chloride content of liquid 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 hydrolyzable chloride content of manufactured epoxy resins and confirm the stated hydrolyzable chloride content of purchased epoxy resins.
SCOPE
1.1 These test methods cover the determination of the easily hydrolyzable chloride content of liquid epoxy resins which are defined as the reaction product of a chlorohydrin and a di- or polyfunctional phenolic compound.
Note 1—There is no known ISO equivalent to this standard.
1.1.1 In Test Method A, the easily hydrolyzable chloride is saponified with potassium hydroxide and directly titrated with hydrochloric acid. This test method can be used for concentrations of 1 weight % and below.
1.1.2 In Test Method B, the easily hydrolyzable chloride is again saponified with potassium hydroxide, then titrated potentiometrically with silver nitrate. This test method can be used for concentrations of 5 to 2500 ppm hydrolyzable chloride.
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 Sections 10 and 16.
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Designation: D1726 − 11
Standard Test Methods for
1
Hydrolyzable Chloride Content of Liquid Epoxy Resins
This standard is issued under the fixed designation D1726; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D6440Terminology Relating to Hydrocarbon Resins
E691Practice for Conducting an Interlaboratory Study to
1.1 Thesetestmethodscoverthedeterminationoftheeasily
Determine the Precision of a Test Method
hydrolyzable chloride content of liquid epoxy resins which are
defined as the reaction product of a chlorohydrin and a di- or
3. Terminology
polyfunctional phenolic compound.
3.1 The terminology in these test methods follows the
NOTE 1—There is no known ISO equivalent to this standard.
standard terminology defined in Terminology D6440.
1.1.1 In Test MethodA, the easily hydrolyzable chloride is
3.2 Definitions:
saponified with potassium hydroxide and directly titrated with
3.3 hydrolyzable chloride, n—the low level chlorine-
hydrochloric acid. This test method can be used for concen-
containing components of the liquid epoxy resin, typically
trations of 1 weight % and below.
residualchlorohydrinethers,whichreactwithwateroralcohol
1.1.2 In Test Method B, the easily hydrolyzable chloride is
to form hydrochloric acid (HCl).
again saponified with potassium hydroxide, then titrated po-
tentiometrically with silver nitrate. This test method can be
4. Summary of Test Method
used for concentrations of 5 to 2500 ppm hydrolyzable
4.1 The sample is refluxed in the presence of a known
chloride.
amountof0.1Nalcoholicpotassiumhydroxidetosaponifythe
1.2 The values stated in SI units are to be regarded as the
hydrolyzable chlorides.
standard. The values given in parentheses are for information
4.2 Test Method A—The amount of potassium hydroxide
only.
consumed in the hydrolysis is a measure of the hydrolyzable
1.3 This standard does not purport to address all of the
chloride content of the resin.
safety concerns, if any, associated with its use. It is the
4.3 Test Method B—The amount of potassium chloride
responsibility of the user of this standard to establish appro-
detected by direct titration with standard silver nitrate solution
priate safety and health practices and determine the applica-
is a measure of the hydrolyzable chloride content of the resin.
bility of regulatory limitations prior to use. For specific hazard
statements see Sections 10 and 16.
5. Significance and Use
2. Referenced Documents
5.1 Thehydrolyzablechloridecontentofliquidepoxyresins
2
is an important variable in determining their reactivity and the
2.1 ASTM Standards:
properties of coatings made from them. These test methods
D329Specification for Acetone
may be used to determine the hydrolyzable chloride content of
D841Specification for Nitration Grade Toluene
manufacturedepoxyresinsandconfirmthestatedhydrolyzable
D1193Specification for Reagent Water
chloride content of purchased epoxy resins.
D3620Specification for Glacial Acetic Acid
6. Interferences
1
These test methods are under the jurisdiction of ASTM Committee D01 on
6.1 Unless stated otherwise, the following interferences
Paint and Related Coatings, Materials, and Applications and are the direct
apply to both test methods:
responsibility of Subcommittee D01.33 on Polymers and Resins.
6.1.1 Test Method A—Alkaline substances easily titratable
Current edition approved June 1, 2011. Published June 2011. Originally
by HCl, can impact the analysis resulting in lower than
approved in 1960. Last previous edition approved in 2003 as D1726–03. DOI:
10.1520/D1726-11.
expected results. Likewise, acidic species, that may behave as
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the HCl titrant can impact the analysis resulting in higher than
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
expected results. Liquid epoxy resin samples should be neutral
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. when analyzed by this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D1726 − 11
6.1.2 Test Method B—Thiocyanate, cyanide, sulfide, bro- 9.6 Boiling Chips.
mide, iodide, or other substances capable of reacting with
silver ion, as well as substances capable of reducing silver ion
10. Hazards
in acidic solutions will impact the analysis resulting in higher
10.1 Consult the latest regulations
...
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:D1726–03 Designation:D1726–11
Standard Test Methods for
1
Hydrolyzable Chloride Content of Liquid Epoxy Resins
This standard is issued under the fixed designation D1726; 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 These test methods cover the determination of the easily hydrolyzable chloride content of liquid epoxy resins which are
defined as the reaction product of a chlorohydrin and a di- or polyfunctional phenolic compound.
NOTE 1—There is no known ISO equivalent to this standard.
1.1.1 In Test Method A, the easily hydrolyzable chloride is saponified with potassium hydroxide and directly titrated with
hydrochloric acid. This test method can be used for concentrations of 1 weight % and below.
1.1.2 In Test Method B, the easily hydrolyzable chloride is again saponified with potassium hydroxide, then titrated
potentiometrically with silver nitrate. This test method can be used for concentrations of 5 to 2500 ppm hydrolyzable chloride.
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 Sections 9 10 and 1516.
2. Referenced Documents
2
2.1 ASTM Standards:
D329 Specification for Acetone
D841 Specification for Nitration Grade Toluene
D1193 Specification for Reagent Water
D3620 Specification for Glacial Acetic Acid
D6440 Terminology Relating to Hydrocarbon Resins
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Documents:
OSHA Regulations, 29 CFR,paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1For definitions relating to hydrocarbon resins see Terminology
3.1 The terminology in these test methods follows the standard terminology defined in Terminology D6440.
3.2 Definitions:
3.3 hydrolyzable chloride, n—the low level chlorine-containing components of the liquid epoxy resin, typically residual
chlorohydrin ethers, which react with water or alcohol to form hydrochloric acid (HCl).
4. Summary of Test Method
4.1 Thesampleisrefluxedinthepresenceofaknownamountof0.1Nalcoholicpotassiumhydroxide.Theamountofpotassium
hydroxideconsumedinthehydrolysisisameasureofthehydrolyzablechloridecontentoftheresin.alcoholicpotassiumhydroxide
to saponify the hydrolyzable chlorides.
4.2 Test Method A—The amount of potassium hydroxide consumed in the hydrolysis is a measure of the hydrolyzable chloride
content of the resin.
4.3 Test Method B—The amount of potassium chloride detected by direct titration with standard silver nitrate solution is a
1
ThisThese test method ismethods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and isare the direct
responsibility of Subcommittee D01.33 on Polymers and Resins.
Current edition approved Dec.June 1, 2003.2011. Published January 2004.June 2011. Originally approved in 1960. Last previous edition approved in 19902003 as
D1726–90(1996).D1726 – 03. DOI: 10.1520/D1726-03. 10.1520/D1726-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book ofASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D1726–11
measure of the hydrolyzable chloride content of the resin.
5. Significance and Use
5.1 The hydrolyzable chloride content of liquid 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 hydrolyzable chloride content of
manufactured epoxy resins and confirm the stated hydrolyzable chloride content of purchased epoxy resins.
6. Apparatus
6.1Reflux Apparatus, consisting of a 250-mL Erlenmeyer flask attache
...
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