ASTM D1398-93(1998)

Standard Test Method for Fatty Acid Content of Alkyd Resins and Alkyd Resin Solutions (Withdrawn 2007)

SCOPE
1.1 This test method covers the gravimetric determination of the total fatty acids in alkyd resins and alkyd resin solutions. The 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 whoever uses this standard to consult and 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WITHDRAWN RATIONALE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 the total fatty acids in alkyd resins and alkyd resin solutions. The 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the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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• Status: Withdrawn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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D1398–93(Reapproved1998)
Standard Test Method for
Fatty Acid Content of Alkyd Resins and Alkyd Resin
Solutions
This standard is issued under the fixed designation D 1398; 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 Filtering Funnel, 75-mm diameter, long-stem.
4.5 Flask, 250-mL, flat-bottom, with standard taper open-
1.1 This test method covers the gravimetric determination
ing.
of the total fatty acids in alkyd resins and alkyd resin solutions.
4.6 Nitrogen Gas Supply.
The test method is not applicable to alkyd resins containing
4.7 Separatory Funnels, three 500-mL capacity glass-
modifying agents such as urea, melamine, phenols, rosin, and
stoppered, fitted with standard-taper ground-glass stoppers and
styrene.
stopcocks.
1.2 This standard does not purport to address all of the
4.8 Steam Bath.
safety concerns, if any, associated with its use. It is the
4.9 Water Bath.
responsibility of whoever uses this standard to consult and
4.10 Vacuum Drying Oven, small, laboratory-size, thermo-
establish appropriate safety and health practices and deter-
statically controlled to operate at 606 2°C. A water-aspirator
mine the applicability of regulatory limitations prior to use.
vacuum source is satisfactory.
2. Referenced Documents
4.11 Cotton, absorbent, USP.
2.1 ASTM Standards:
5. Reagents and Materials
D 563 Test Method for Phthalic Anhydride Content of
5.1 Purity of Reagents—Reagent grade chemicals shall be
Alkyd Resins and Resin Solutions
used in all tests. Unless otherwise indicated, it is intended that
D 1193 Specification for Reagent Water
all reagents shall conform to the specifications of the Commit-
D 1615 Test Methods for Glycerol, Ethylene Glycol, and
tee onAnalytical Reagents of theAmerican Chemical Society,
Pentaerythritol in Alkyd Resins
where such specifications are available. Other grades may be
D 2245 Test Method for Identification of Oils and OilAcids
used, provided it is first ascertained that the reagent is of
in Solvent-Reducible Paints
sufficiently high purity to permit its use without lessening the
3. Significance
accuracy of the determination.
5.2 Purity of Water—Unless otherwise indicated, references
3.1 This test method is used to determine total fatty acid
to water shall be understood to mean reagent water conforming
content of alkyl resins and this solution, in the absence of
to Type IV of Specification D 1193.
interfering compounds, as a means whereby the relative
5.3 Ether, anhydrous.
applicability of the alkyd resin to the particular end use may be
5.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
estimated by buyer and seller.
chloric acid (HCl).
4. Apparatus
5.5 Indicator Paper, universal-type.
5.6 Sodium Sulfate (Na SO ), anhydrous.
4.1 Beakers, having capacities of 150 and 400 mL. 2 4
4.2 Desiccator,
6. Procedure
4.3 Filter Paper, rapid, low-ash filter paper, to fit the
6.1 Saponify a portion of resin or resin solution in accor-
filtering funnel.
dance with Test Method D 563. After filtering the potassium
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. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved April 15, 1993. Published June 1993. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as D 1398 – 56. Last previous edition D 1398 – 84. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 06.03. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 06.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1398–93 (1998)
phthalate alcoholate (6.3), transfer the combined filtrate and contents.Swaboutthestemofthefunnelwithapieceofcotton
washings to the 400-mLbeaker with the aid of 25 mLof water attached to a stiff wire.
from a wash bottle. Concentrate to a volume of approximately
NOTE 4—A small brass screw soldered to the end of a stiff brass wire
25 mLon the steam bath under a blanket of nitrogen to prevent
will serve for this purpose.
oxidation of the fatty acids. (Caution—Be sure to use a hood.)
6.7.3 Insert a clean plug of cotton moistened with ether into
Transfer to a 500-mL separatory funnel with the aid of water
the funnel stem and filter the ether solution through the cotton
fromawashbottle,dilutewithwatertoapproximately300mL,
plug into the appropriate receiver.
and add 10 mL of alcohol.
6.2 Extract the unsaponifiable and volatile thinners with
NOTE 5—Experience will show how tightly packed the cotton must be
to hold back the Na SO and still allow a sufficient flow of ether extract.
successive 50-mLportions of ether (not less than three, or until
2 4
a colorless ether extract is obtained), combining the ether
6.8 Evaporate the ether portionwise from the beaker or
extracts in the first separatory funnel and using the other two
distill it from the flask on the steam bath, in a hood. Apply a
funnels fo
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