ASTM D1306-88(1996)e1

Standard Test Method for Phthalic Anhydride Content of Alkyd Resins and Esters Containing Other Dibasic Acids (Gravimetric) (Withdrawn 2004)

SCOPE
1.1 This test method covers the gravimetric determination of phthalic anhydride in alkyd resins and esters that contain dibasic acids such as maleic, fumaric, adipic, and sebacic, which would interfere if Test Method D 563 was used.
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.
WITHDRAWN RATIONALE
This test method covers the gravimetric determination of phthalic anhydride in alkyd resins and esters that contain dibasic acids such as maleic, fumaric, adipic, and sebacic, which would interfere if Test Method D 563 was used.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials and Applications, this test method was withdrawn in December 2004 in accordance with section 10.6.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by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

• Status: Withdrawn
• Publication Date: 31-Dec-1995
• Withdrawal Date: 14-Dec-2004
• ICS: 87.060.10 - Pigments and extenders
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.33 - Polymers and Resins

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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Designation:D1306–88(Reapproved 1996)
Standard Test Method for
Phthalic Anhydride Content of Alkyd Resins and Esters
1
Containing Other Dibasic Acids (Gravimetric)
This standard is issued under the fixed designation D 1306; 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.
This standard has been approved for use by agencies of the Department of Defense.
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e NOTE—Keywords were added editorially in October 1996.
1. Scope 5. Apparatus
1.1 This test method covers the gravimetric determination 5.1 Flask and Condenser—A 500-mL Erlenmeyer flask
of phthalic anhydride in alkyd resins and esters that contain fittedwithanair-cooledglassrefluxcondenser30in.(760mm)
dibasic acids such as maleic, fumaric, adipic, and sebacic, in length. The connection between the flask and condenser
which would interfere if Test Method D 563 was used. shall be a standard-taper 24/40 ground-glass joint.
1.2 This standard does not purport to address all of the 5.2 Water Bath.
safety concerns, if any, associated with its use. It is the 5.3 Guard Tube, filled with soda lime.
responsibility of the user of this standard to establish appro- 5.4 Fritted-Glass Filter Crucible, medium porosity, of
priate safety and health practices and determine the applica- 30-mL capacity.
bility of regulatory limitations prior to use. 5.5 Filter Flasks, suction-type.
5.6 Crucible Holder.
2. Referenced Documents
5.7 Oven, of gravity convection type.
2.1 ASTM Standards:
5.8 Desiccator, containing concentrated H SO (sp gr 1.84)
2 4
D 563 Test Method for Phthalic Anhydride Content of as the desiccant.
2
Alkyd Resins and Resin Solutions
5.9 Flash Filtrator.
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D 1193 Specification for Reagent Water 5.10 pH Test Assembly.
5.11 Volumetric Flask, 100-mL.
3. Summary of Test Method
5.12 Erlenmeyer Flask, 250-mL, wide-mouth, with glass
3.1 The specimen is saponified with alcoholic potassium
stopper not smaller than a No. 27.
hydroxide and benzene to precipitate quantitatively the potas-
5.13 Delivery Pipet, 2-mL.
sium salt of phthalic acid as C H (COOH) ·C H OH. Interfer-
6 4 2 2 5
6. Reagents
ing substances are eliminated by dissolving the precipitate in
water, adjusting the pH of the solution to 2.5 with nitric acid,
6.1 Purity of Reagent—Reagent grade chemicals shall be
and filtering. Phthalic acid is then precipitated as nonstoichio- used in all tests. Unless otherwise indicated, it is intended that
metric lead phthalate and calculated to phthalic anhydride,
all reagents shall conform to the specifications of the Commit-
using a factor obtained when compositions of known purity tee onAnalytical Reagents of theAmerican Chemical Society,
4
were analyzed similarly.
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
4. Significance and Use
sufficiently high purity to permit its use without lessening the
4.1 The phthalic anhydride content of alkyd resins controls
accuracy of the determination.
the properties of the final film.
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This test method is under the jurisdiction of ASTM Committee D-1 on Paint
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and Related Coatings, Materials, andApplications, and is the direct responsibility of Reagent Chemicals, American Chemical Society Specifications, American
Subcommittee D01.33 on Polymers and Resins. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved May 27, 1988. Published October 1988. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 1306 –54 T. Last previous edition D 1306 – 80. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
2
Annual Book of ASTM Standards, Vol 06.03. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
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Annual Book of ASTM Standards, Vol 11.01. MD.
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D1306
6.2 Purity of Water—Unless otherwise indicated, references 7.4 Wipe the outer surface of the crucible with a clean cloth
to water shall be understood to mean reagent water as defined and place in a gravity convection oven at 60°C for 1 h. Cool to
by Type II of Specification D 1193. room temperature in a desiccator, and weigh.
6.3 Acetic Acid, Glacial.
NOTE 2—The crucible weighings are for determining aliquot size and
6.4 Alcohol-Benzene Wash Solution—Mix 1 volume of need be weighed to the nearest 10 mg only.
absolute ethyl alcohol (Note 1) with 3 volumes of benzene.
7.5 Dissolve the contents of the crucibl
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