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ASTM D1397-93(1998)

(Test Method)

Standard Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions (Withdrawn 2007)

Standard Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions (Withdrawn 2007)

SCOPE
1.1 This test method covers the determination of unsaponifiable matter in alkyd resins and resin solutions. This test method is not applicable to alkyd resins containing modifying agents such as urea, melamine, phenols, rosin, and styrene.
1.2 This standard does not purport to address all of the safety problems, 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 Note 4.
WITHDRAWN RATIONALE
This test method covers the determination of unsaponifiable matter in alkyd resins and resin solutions. This test method is not applicable to alkyd resins containing modifying agents such as urea, melamine, phenols, rosin, and styrene.
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the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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

Status
Withdrawn
Publication Date
31-Dec-1992
Withdrawal Date
19-Mar-2007
ICS
87.060.20 - Binders
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.33 - Polymers and Resins
Current Stage
Ref Project

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ASTM D1397-93(1998) - Standard Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions (Withdrawn 2007)ASTM D1397-93(1998) - Standard Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions (Withdrawn 2007)
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ASTM D1397-93(1998) - Standard Test Method for Unsaponifiable Matter in Alkyd Resins and Resin Solutions (Withdrawn 2007)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 1397 – 93 (Reapproved 1998)
Standard Test Method for
Unsaponifiable Matter in Alkyd Resins and Resin Solutions
This standard is issued under the fixed designation D 1397; 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.
1. Scope 4.4 Steam Bath.
4.5 Vacuum Drying Oven—Asmall,laboratory-sizevacuum
1.1 This test method covers the determination of unsaponi-
oven, thermostatically controlled to operate at 80 6 5°C. A
fiable matter in alkyd resins and resin solutions. This test
water aspirator vacuum source is satisfactory.
method is not applicable to alkyd resins containing modifying
agents such as urea, melamine, phenols, rosin, and styrene.
5. Reagents and Materials
1.2 This standard does not purport to address all of the
5.1 Reagent grade chemicals shall be used in all tests.
safety concerns, if any, associated with its use. It is the
Unless otherwise indicated, it is intended that all reagents shall
responsibility of the user of this standard to establish appro-
conform to the specifications of the Committee on Analytical
priate safety and health practices and determine the applica-
Reagents of the American Chemical Society, where such
bility of regulatory limitations prior to use. For a specific
specifications are available. Other grades may be used, pro-
hazard statement, see Note 4.
vided it is first ascertained that the reagent is of sufficiently
2. Referenced Documents high purity to permit its use without lessening the accuracy of
the determination.
2.1 ASTM Standards:
5.2 Unless otherwise indicated references to water shall be
D 1193 Specification for Reagent Water
understood to mean reagent water as defined by Type II of
3. Significance and Use Specification D 1193.
5.3 Benzene.
3.1 The unsaponifiable matter in alkyd resins controls the
5.4 Benzene–Alcohol Mixture—Mix equal volumes of ben-
properties of the final film.
zene and ethyl alcohol, add 2 drops of phenolphthalein
4. Apparatus
indicator solution, and neutralize with 0.02 N sodium hydrox-
ide (NaOH) solution to a persistent faint pink color.
4.1 Aluminum Beaker, having a capacity of 125 mL.
5.5 Ethyl Alcohol (95 volume %)—Pure ethyl alcohol or
4.2 Flask and Condenser—A 200-mL Erlenmeyer flask
denatured alcohol conforming to Formula No. 2B of the U. S.
fitted with a water-cooled glass reflux condenser. The connec-
Bureau of Internal Revenue.
tion between the flask and condenser shall be a standard 24/40
5.6 Ethyl Ether.
taper ground-glass joint.
5.7 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
4.3 Separatory Funnels—Three500-mLcapacityfittedwith
1gofphenolphthaleininethylalcohol(95 %)anddiluteto100
standard-taper, ground-glass stoppers and stopcocks. Stop-
mL with ethyl alcohol.
cocks should be lubricated sparingly with ether-insoluble
5.8 pH Indicator Paper, universal type.
stopcock grease. Alternatively, funnels fitted with tetrafluoro-
5.9 Sodium Hydroxide Solution (50 %)—Dissolve sodium
ethylene (TFE-fluorocarbon) stopcocks may be used.
hydroxide (NaOH) in an equal weight of water.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.33 on Polymers and Resins.
Current edition approved April 15, 1993. Published June 1993. Originally Reagent Chemicals, American Chemical Society Specifications, American
published as D 1397 – 56 T. Last previous edition D 1397 – 88. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 11.01. listed by the American Chemical Society, see Analar Standards for Laboratory
Aluminum beakers, Catalog No. 2100, manufactured by theA. H.Thomas Co., Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
W. Washington Square, Philadelphia, PA 19105, have been found satisfactory for and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
this purpose. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 1397 – 93 (1998)
NOTE 4—Precaution: In addition to other precautions, be sure to use a
5.10 Sodium Hydroxide, Standard Solution (0.02 N)—
hood.
Prepare and accurately standardize a 0.02 N aqueous NaOH
solution. 6.6 Evaporate the final portion of ether; then transfer the
beaker and its contents to the vacuum oven, previously heated
to 80°C. Heat to constant weight, allowing to cool to room
6. Procedure
temperature in a desiccator before weighing.
6.1 Weigh by difference, from a closed container into the
6.7 After weighing, take up the residue in 50 mL of warm
200-mL Erlenmeyer flask, a portion of resin or resin solution
(approximately 50°C) benzene-alcohol mixture. Titrate with
containing from 0.05 to 0.2 g of unsaponifiable matter (Note 1)
0.02 NNaOHsolutiontothesamepersistentfaintpinkcoloras
(8 to 10 g of resin solution usually is sufficient).
in
...

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