ASTM D1726-90(1996)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 1726 – 90 (Reapproved 1996)
Standard Test Methods for
Hydrolyzable Chloride Content of Liquid Epoxy Resins
This standard is issued under the fixed designation D 1726; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope manufactured epoxy resins and confirm the stated hydrolyzable
chloride content of purchased epoxy resins.
1.1 These test methods cover the determination of the easily
hydrolyzable chloride content of liquid epoxy resins which are
5. Apparatus
defined as the reaction product of a chlorohydrin and a di- or
5.1 Reflux Apparatus, consisting of a 250-mL Erlenmeyer
polyfunctional phenolic compound.
flask attached to a reflux condenser and a hot plate with
1.1.1 In Test Method A, the easily hydrolyzable chloride is
variable heat control.
saponified with potassium hydroxide and directly titrated with
hydrochloric acid. This test method can be used for concen-
6. Purity of Reagents
trations of 1 weight % and below.
6.1 Purity of Reagents—Reagent grade chemicals shall be
1.1.2 In Test Method B, the easily hydrolyzable chloride is
used in all tests. Unless otherwise indicated, it is intended that
again saponified with potassium hydroxide, then titrated po-
all reagents shall conform to the specifications of the Commit-
tentiometrically with silver nitrate. This test method can be
tee on Analytical Reagents of the American Chemical Society,
used for concentrations of 5 to 2500 ppm hydrolyzable
where such specifications are available. Other grades may be
chloride.
used, provided it is first ascertained that the reagent is of
1.2 This standard does not purport to address all of the
sufficiently high purity to permit its use without lessening the
safety concerns, if any, associated with its use. It is the
accuracy of the determination.
responsibility of the user of this standard to establish appro-
6.2 Purity of Water—Unless otherwise indicated, references
priate safety and health practices and determine the applica-
to water shall be understood to mean reagent water conforming
bility of regulatory limitations prior to use. For specific hazard
to Type II of Specification D 1193.
statements see Sections 8 and 14.
TEST METHOD A
2. Referenced Documents
2.1 ASTM Standards:
7. Reagents and Materials
D 841 Specification for Nitration Grade Toluene
7.1 Hydrochloric Acid, Standard (0.1 N)—Dilute 9 mL of
D 1193 Specification for Reagent Water
concentrated hydrochloric acid (HCl, sp gr 1.19) to 1 L with
water. Standardize against 0.25 g of sodium carbonate
3. Summary of Test Method
(Na CO ) accurately weighed and dissolved in 75 to 100 mL of
2 3
3.1 The sample is refluxed in the presence of a known
water.
amount of 0.1 N alcoholic potassium hydroxide. The amount of
7.2 Methyl Ethyl Ketone.
potassium hydroxide consumed in the hydrolysis is a measure
7.3 Phenolphthalein Indicator Solution—Dissolve1gof
of the hydrolyzable chloride content of the resin.
phenolphthalein in 100 mL of methanol, ethanol, or isopro-
panol.
4. Significance and Use
7.4 Potassium Hydroxide, Alcohol Solution (0.1 N)—
4.1 The hydrolyzable chloride content of liquid epoxy resins
Dissolve 5.5 to 6.0 g of potassium hydroxide (KOH) in 1 L of
is an important variable in determining their reactivity and the
methanol (99 %) or ethanol conforming to Formula No. SD-30
properties of coatings made from them. These test methods
of the U.S. Bureau of Internal Revenue. No standardization of
may be used to determine the hydrolyzable chloride content of
the solution is necessary.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applicationsand is the direct responsibility of Reagent Chemicals, American Chemical Society Specifications, American
Subcommittee D01.33on Polymers and Resins. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved May 25, 1990. Published July 1990. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 1726 – 60. Last previous edition D 1726 – 87. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 06.04. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
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D 1726
7.5 Toluene (Warning—See Section 8.), conforming to 12.2 Hot Plate, with variable heat control.
Specification D 841. 12.3 Magnetic Stirrer, with polytetrafluoroethylene (PTFE)-
coated stirring bar.
8. Hazards
12.4 Buret or Automatic Titrator.
8.1 Hydrochloric acid and potassium hydroxide are corro-
12.5 Silver Electrode or equivalent.
sive. Toluene and methyl ethyl ketone are flammable and their
12.6 Boiling Chips.
vapors can be harmful. Precautions should be taken to avoid
inhalation and skin or eye contact with these chemicals. All
13. Reagents and Material
sample preparations should be done in a well ventilated area,
13.1 Acetone.
such as a fume hood.
13.2 Bromcresol Green Indicator Solution (0.1 %)—
Dissolve 0.1 g of bromcresol green in 100 mL of water.
9. Procedure
13.3 Nitric acid, (HNO ) (1 + 1), diluted with water.
9.1 Weigh to the nearest 1 mg, 6 to8gof neutral specimen
13.4 Potassium Hydroxide, alcohol solution (0.1 N)—
into a 250-mL glass-stoppered Erlenmeyer flask. By means of
Dissolve 5.6 g of potassium hydroxide (KOH) in 1 mL of
a pipet, transfer 50.0 mL of 0.1 N alcoholic KOH solution into
methanol (99 %) or ethanol conforming to Formu
...