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ASTM D1726-11(2019)

(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
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.
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements see Sections 10 and 16.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
31-May-2019
ICS
83.080.10 - Thermosetting materials
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.33 - Polymers and Resins
Current Stage
Ref Project

Relations

Replaces
ASTM D1726-11 - Standard Test Methods for Hydrolyzable Chloride Content of Liquid Epoxy Resins
Effective Date
01-Jun-2019
Refers
ASTM D841-19 - Standard Specification for Nitration Grade Toluene
Effective Date
15-Nov-2019
Refers
ASTM D6440-10(2018) - Standard Terminology Relating to Hydrocarbon Resins
Effective Date
01-Sep-2018
Refers
ASTM D841-17a - Standard Specification for Nitration Grade Toluene
Effective Date
01-Jul-2017
Refers
ASTM D841-17 - Standard Specification for Nitration Grade Toluene
Effective Date
01-Jun-2017
Refers
ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
Effective Date
01-May-2013
Refers
ASTM D841-13 - Standard Specification for Nitration Grade Toluene
Effective Date
01-Feb-2013
Refers
ASTM D841-12 - Standard Specification for Nitration Grade Toluene
Effective Date
01-Nov-2012
Refers
ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
Effective Date
01-Nov-2011
Refers
ASTM D841-11 - Standard Specification for Nitration Grade Toluene
Effective Date
01-Jul-2011
Refers
ASTM D6440-10 - Standard Terminology Relating to Hydrocarbon Resins
Effective Date
01-Dec-2010
Refers
ASTM D841-10 - Standard Specification for Nitration Grade Toluene
Effective Date
01-Jan-2010
Refers
ASTM D3620-04(2009) - Standard Specification for Glacial Acetic Acid
Effective Date
01-Jun-2009
Refers
ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
Effective Date
01-Oct-2008
Refers
ASTM D841-02(2008)e1 - Standard Specification for Nitration Grade Toluene
Effective Date
01-Jan-2008

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ASTM D1726-11(2019) - Standard Test Methods for Hydrolyzable Chloride Content of Liquid Epoxy ResinsASTM D1726-11(2019) - Standard Test Methods for Hydrolyzable Chloride Content of Liquid Epoxy Resins
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ASTM D1726-11(2019) - Standard Test Methods for Hydrolyzable Chloride Content of Liquid Epoxy Resins
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D1726 − 11 (Reapproved 2019)
Standard Test Methods for
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 U.S. Department of Defense.
1. Scope 2. Referenced Documents
1.1 Thesetestmethodscoverthedeterminationoftheeasily 2.1 ASTM Standards:
hydrolyzable chloride content of liquid epoxy resins which are D329Specification for Acetone
defined as the reaction product of a chlorohydrin and a di- or D841Specification for Nitration Grade Toluene
polyfunctional phenolic compound. D1193Specification for Reagent Water
D3620Specification for Glacial Acetic Acid
NOTE 1—There is no known ISO equivalent to this standard.
D6440Terminology Relating to Hydrocarbon Resins
1.1.1 In Test MethodA, the easily hydrolyzable chloride is
E691Practice for Conducting an Interlaboratory Study to
saponified with potassium hydroxide and directly titrated with
Determine the Precision of a Test Method
hydrochloric acid. This test method can be used for concen-
trations of 1 weight % and below. 3. Terminology
1.1.2 In Test Method B, the easily hydrolyzable chloride is
3.1 The terminology in these test methods follows the
again saponified with potassium hydroxide, then titrated po-
standard terminology defined in Terminology D6440.
tentiometrically with silver nitrate. This test method can be
3.2 Definitions:
used for concentrations of 5 to 2500 ppm hydrolyzable
3.3 hydrolyzable chloride, n—the low level chlorine-
chloride.
containing components of the liquid epoxy resin, typically
1.2 The values stated in SI units are to be regarded as the
residualchlorohydrinethers,whichreactwithwateroralcohol
standard. The values given in parentheses are for information
to form hydrochloric acid (HCl).
only.
4. Summary of Test Method
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4.1 The sample is refluxed in the presence of a known
responsibility of the user of this standard to establish appro-
amountof0.1Nalcoholicpotassiumhydroxidetosaponifythe
priate safety, health, and environmental practices and deter- hydrolyzable chlorides.
mine the applicability of regulatory limitations prior to use.
4.2 Test Method A—The amount of potassium hydroxide
For specific hazard statements see Sections 10 and 16.
consumed in the hydrolysis is a measure of the hydrolyzable
1.4 This international standard was developed in accor-
chloride content of the resin.
dance with internationally recognized principles on standard-
4.3 Test Method B—The amount of potassium chloride
ization established in the Decision on Principles for the
detected by direct titration with standard silver nitrate solution
Development of International Standards, Guides and Recom-
is a measure of the hydrolyzable chloride content of the resin.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5. Significance and Use
5.1 Thehydrolyzablechloridecontentofliquidepoxyresins
is an important variable in determining their reactivity and the
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.33 on Polymers and Resins. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2019. Published June 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1960. Last previous edition approved in 2011 as D1726–11. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D1726-11R19. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1726 − 11 (2019)
properties of coatings made from them. These test methods water. Standardize against 0.25 g of sodium carbonate
may be used to determine the hydrolyzable chloride content of (Na CO )accuratelyweighedanddissolvedin75to100mLof
2 3
manufacturedepoxyresinsandconfirmthestatedhydrolyzable water.
chloride content of purchased epoxy resins.
9.2 Methyl Ethyl Ketone (MEK).
9.3 Phenolphthalein Indicator Solution—Dissolve1gof
6. Interferences
phenolphthalein in 100 mL of methanol, ethanol, or isopropa-
6.1 Unless stated otherwise, the following interferences
nol.
apply to both test methods:
9.4 Potassium Hydroxide, Alcohol Solution (0.1 N)—
6.1.1 Test Method A—Alkaline substances easily titratable
Dissolve 5.6 g of potassium hydroxide (KOH) in 1 L of
by HCl, can impact the analysis resulting in lower than
methanol (99%). No standardization of the solution is neces-
expected results. Likewise, acidic species, that may behave as
sary.
the HCl titrant can impact the analysis resulting in higher than
expected results. Liquid epoxy resin samples should be neutral
9.5 Toluene (Warning—See Section 10.), conforming to
when analyzed by this test method.
Specification D841.
6.1.2 Test Method B—Thiocyanate, cyanide, sulfide,
9.6 Boiling Chips.
bromide, 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 and supplier’s Material
than expected results.
SafetyDataSheetsregardingallmaterialsusedinthismethod.
6.1.3 Test Methods A and B (using a visual indicator) may
not be applicable to samples containing heat sensitive
10.2 Hydrochloric acid and potassium hydroxide are corro-
impurities, leading to high color in the reacted solution. sive. Toluene and methyl ethyl ketone are flammable and their
vapors can be harmful. Precautions should be taken to avoid
7. Purity of Reagents
inhalation and skin or eye contact with these chemicals. All
sample preparations should be done in a well ventilated area,
7.1 Purity of Reagents—Reagent grade chemicals shall be
such as a fume hood.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
3 11. Procedure
teeonAnalyticalReagentsoftheAmericanChemicalSociety,
where such specifications are available. Other grades may be 11.1 Weigh to the nearest 0.001 g, 6 to8gof neutral
used, provided it is first ascertained that the reagent is of specimen into a 250-mLglass-stoppered Erlenmeyer flask. By
means of a pipette, transfer 50.0 mL of 0.1 N alcoholic KOH
sufficiently high purity to permit its use without lessening the
accuracy of the determination. solution into the flask and add 15 mL of toluene. Stopper the
flask and swirl to mix.
7.2 Purity of Water—Unless otherwise indicated, references
towatershallbeunderstoodtomeanreagentwaterconforming 11.2 Prepare a blank in a separate 250-Erlenmeyer flask,
adding 15 mL of toluene and 50 mL of 0.1 N alcoholic KOH.
to Type II of Specification D1193.
Swirl to mix.
TEST METHOD A – 1 Weight % and Below of
11.3 Add a few boiling chips and attach each flask to a
Hydrolyzable Chloride
reflux condensers on the hot plate.
8. Apparatus
11.4 Alloweachsolutiontorefluxgentlyfor15 61minon
a hot plate.At the end of the reflux period, remove each flask
8.1 Reflux Apparatus, consisting of a 250-mL Erlenmeyer
from the hot plate and cool to room temperature with the
flask attached to a reflux condenser.
condenser in place.
8.2 Hot Plate, with variable heat control.
11.5 Rinsedowneachcondenserwith20mLoftoulenethen
8.3 Magnetic Stirrer, with polytetrafluorethylene (PTFE)-
remove the condensers from the flasks.
coated stirring bar.
11.6 Add 3 drops of phenolphthalein indicator solution to
8.4 Buret.
eachflask,andtitratewith0.1NHCl.Theendpointisdetected
when 1 drop of 0.1 N HCl changes the solutio
...

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