ASTM D2690-98
(Test Method)Standard Test Method for Isophthalic Acid in Alkyd and Polyester Resins (Withdrawn 2007)
Standard Test Method for Isophthalic Acid in Alkyd and Polyester Resins (Withdrawn 2007)
SCOPE
1.1 This test method covers the gravimetric determination of the isophthalic acid content of alkyd resins and polyesters. There is no interference from styrene monomer or polymer or from other dicarboxylic acids except terephthalic acid.
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. For a specific hazard statement, see section 7.
WITHDRAWN RATIONALE
This test method covers the gravimetric determination of the isophthalic acid content of alkyd resins and polyesters. There is no interference from styrene monomer or polymer or from other dicarboxylic acids except terephthalic acid.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D2690–98
Standard Test Method for
Isophthalic Acid in Alkyd and Polyester Resins
This standard is issued under the fixed designation D 2690; 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 in length. The connection between the flask and condenser
should be a standard-taper 24/40 ground joint.
1.1 This test method covers the gravimetric determination
5.2 Heat Source:
of the isophthalic acid content of alkyd resins and polyesters.
5.2.1 Combination Hot Plate and Magnetic Stirrer,or
There is no interference from styrene monomer or polymer or
5.2.2 Heating Mantle and Magnetic Stirrer Base and Bar.
from other dicarboxylic acids except terephthalic acid.
5.3 Büchner Funnel,frittedglass,mediumporosity,150-mL
1.2 This standard does not purport to address all of the
capacity.
safety concerns, if any, associated with its use. It is the
5.4 Volumetric Flask, 100-mL volume.
responsibility of the user of this standard to establish appro-
5.5 Fritted-Glass Filter Crucible, medium porosity, 30-mL
priate safety and health practices and determine the applica-
capacity.
bility of regulatory limitations prior to use. For a specific
hazard statement, see Section 7.
6. Reagents
2. Referenced Documents 6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
2.1 ASTM Standards:
all reagents shall conform to the specifications of the Commit-
D 1193 Specification for Reagent Water
tee onAnalytical Reagents of theAmerican Chemical Society,
3. Summary of Test Method where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
3.1 Theresinissaponifiedwithalcoholicpotassiumhydrox-
sufficiently high purity to permit its use without lessening the
ide and benzene to precipitate entirely the potassium salt of the
accuracy of the determination.
phthalic acid isomer. Since the salt contains entrained impuri-
6.2 Purity of Water—Unless otherwise indicated, references
ties, it is dissolved in water and diluted to volume. An aliquot
to water shall be understood to mean reagent water as defined
portion is acidified under conditions that release the insoluble
by Type II of Specification D 1193.
acid in filterable form. It is then isolated, weighed, and
6.3 Alcohol-Benzene Wash Solution (2 + 3)—Mix absolute
corrected for its slight solubility in water.
ethyl alcohol (Note 1) with benzene in the proportion of 2
4. Significance and Use
volumes of alcohol to 3 volumes of benzene.
4.1 This test method is used to determine the amount of
NOTE 1—The alcohol may be denatured Formula 2-B, but must be
isophthalic acid contained in alkyd and polyester resins. Use of
anhydrous.
this test method provides a means whereby the relative
6.4 Alcoholic Potassium Hydroxide Solution (0.5 N)—
applicabilityofthealkydorpolyesterresintotheparticularend
Dissolve 33 g of KOH in 1 L of absolute ethyl alcohol (Note
use may be estimated by the buyer and the seller.
1) by reflux or by standing overnight. Protect against carbon
dioxide absorption. Filter just before use.
5. Apparatus
6.5 Benzene (anhydrous).
5.1 Flask and Condenser—A 250-mL Erlenmeyer flask
6.6 Ether (anhydrous).
fittedwithanair-cooledglassrefluxcondenser30in.(760mm)
1 3
This test method is under the jurisdiction of ASTM Committee D-1 on Paint Reagent Chemicals, American Chemical Society Specifications, American
and Related Coatings, Materials, andApplications and is the direct responsibility of Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Subcommittee D01.33 on Polymers and Resins. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved June 10, 1998. Published August 1998. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
{1
published as D 2690 – 68. Last previous edition D 2690 – 89 (l996) . and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2690
6.7 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro- water. Dry the crucible in an oven at 105°C for 1 h, cool in a
chloric acid (HCl). desiccator, and weigh. If the collected isophthalic sample
6.8 Methyl Purple Indicator Solution. exceeds 200 mg, withdraw a smaller aliquot from the remain-
ing solution, dilute to 50 mL with water and repeat the
7. Hazards
precipitation procedure. If less than 50
...
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