ASTM D1312-93(1998)

Standard Test Methods for Apparent Free Phenols in Synthetic Phenolic Resins or Solutions Used for Coating Purposes (Withdrawn 2007)

SCOPE
1.1 These test methods cover the determination of the amount of apparent free phenol in synthetic phenolic resins or solutions used for coating purposes. The test method for isolation of the free phenol applies to all the commonly used resins except those containing p-phenyl-phenol. Test Method A applies to the simpler phenols up to and including the xylenols; Test Method B applies to the common alkylated phenols. >
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. >
WITHDRAWN RATIONALE
These test methods cover the determination of the amount of apparent free phenol in synthetic phenolic resins or solutions used for coating purposes. The test method for isolation of the free phenol applies to all the commonly used resins except those containing p-phenyl-phenol. Test Method A applies to the simpler phenols up to and including the xylenols; Test Method B applies to the common alkylated phenols.
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the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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• Status: Withdrawn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: 87.060.30 - Solvents
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D1312–93(Reapproved1998)
Standard Test Methods for
Apparent Free Phenols in Synthetic Phenolic Resins or
Solutions Used for Coating Purposes
This standard is issued under the fixed designation D 1312; 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 ISOLATION OF FREE PHENOLS
1.1 These test methods cover the determination of the
4. Apparatus
amount of apparent free phenol in synthetic phenolic resins or
4.1 Steam Generator.
solutions used for coating purposes. The test method for
4.2 Distillation Flask—A 500-mL Kjeldahl flask.
isolation of the free phenol applies to all the commonly used
4.3 Condenser.
resins except those containing p-phenyl-phenol.Test MethodA
applies to the simpler phenols up to and including the xylenols;
5. Reagents
Test Method B applies to the common alkylated phenols.
5.1 Sodium Hydroxide Solution (100 g NaOH/L)—
1.2 This standard does not purport to address all of the
Dissolve 100 g of NaOH [Caution] in water and dilute to 1 L.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
6. Procedure
priate safety and health practices and determine the applica-
6.1 Transfer 1 to2gofthe sample, weighed to the nearest
bility of regulatory limitations prior to use.
0.01 g, to a 500-mL Kjeldahl flask.Add 50 mL of water. Lead
steam from a steam generator through a T-trap and then
2. Referenced Documents
throughatubeextendingtothebottomoftheflask.Takeoffthe
2.1 ASTM Standards:
2 distillate through a second bent tube that extends just through
D 1193 Specification for Reagent Water
the stopper of the flask and is attached to the top of an inclined
long condenser. Using a 1000-mL volumetric flask as a
3. Purity of Reagents
receiver, collect 900 mLof the distillate.Asmall flame may be
3.1 Reagent grade chemicals shall be used in all tests.
applied to the bottom of the Kjeldahl flask during distillation to
Unless otherwise indicated, it is intended that all reagents shall
maintain the volume of water constant. If the distillate is clear,
conform to the specifications of the Committee on Analytical
dilute to 1000 mL; if not, add several millilitres of NaOH
Reagents of the American Chemical Society, where such
3 solution to dissolve the insoluble phenols. Determine the
specifications are available. Other grades may be used, pro-
apparent free phenol in accordance with Method A or B,as
vided it is first ascertained that the reagent is of sufficiently
required.
high purity to permit its use without lessening the accuracy of
the determination.
NOTE 1—p-Phenylphenol is not completely isolated by this procedure.
3.2 Unless otherwise indicated, references to water shall be
TEST METHODA—SIMPLER PHENOLS
understood to mean reagent water conforming to Type III of
Specification D 1193.
7. Summary of Test Method
7.1 Free phenols are isolated by steam distillation, reacted
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD-1onPaint with a measured excess of bromine, and the excess back-
and Related Coatings, Materials, and Applications and are the direct responsibility
titrated with standard sodium thiosulfate solution.
of Subcommittee D01.33 on Polymers and Resins.
Current edition approved April 15, 1993. Published June 1993. Originally
8. Apparatus
e1
published as D 1312 – 54. Last previous edition D 1312 – 56 (1987) .
Annual Book of ASTM Standards, Vol 11.01.
8.1 Iodine Flasks, 500-mL, glass-stoppered.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
9. Reagents
listed by the American Chemical Society, see Analar Standards for Laboratory
9.1 Bromide-BromateSolution—Dissolve2.784gofKBrO
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
and 10 g of KBr in 1 L of water.
MD.
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D1312–93 (1998)
9.2 Potassium Iodide Solution (100 g KI/L)—Dissolve 100 15. Reagents
g of KI in water and dilute to 1 L.
15.1 Iodine Solution—Dissolve 4.2 g of iodine in 15 g of a
9.3 Sodium Thiosulfate, Standard Solution (0.1 N)— Dis-
saturated aqueous KI solution and dilute to 1 L.
solve 25 g of Na S O ·5H O in 1 L of water. Standardize
2 2 3 2
15.2 Sodium Bicarbonate Solution (84 g NaHCO /L)—
against iodine.
Dissolve 84 g of NaHCO in water and dilute to 1 L.
9.4 Starch Indicator Solution—Dissolve1gof soluble
15.3 Sodium Hydroxide Solution (100 g NaOH/L)—
starch in 100 mL of boiling water and cool.
Dissolve 100 g
...