ASTM D1396-92(1998)

Standard Test Methods for Chemical Analysis of Poly(Vinyl Butyral) (Withdrawn 2007)

SCOPE
1.1 These methods cover procedures for the determination of poly(vinyl alcohol), poly(vinyl acetate), and butyraldehyde in poly(vinyl butyral).  
1.2 The procedures appear in the following order:  Sections Poly(vinyl alcohol) 4 Poly(vinyl acetate) 5 Butyraldehyde 6
1.3 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WITHDRAWN RATIONALE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 procedures for the determination of poly(vinyl alcohol), poly(vinyl acetate), and butyraldehyde in poly(vinyl butyral).
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the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in March 2007 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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• Status: Withdrawn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-1991
• Withdrawal Date: 19-Mar-2007
• ICS: 71.040.40 - Chemical analysis
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D1396–92(Reapproved1998)
Standard Test Methods for
Chemical Analysis of Poly(Vinyl Butyral)
This standard is issued under the fixed designation D 1396; 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 4. Poly(Vinyl Alcohol)
1.1 These methods cover procedures for the determination 4.1 Reagents:
of poly(vinyl alcohol), poly(vinyl acetate), and butyraldehyde 4.1.1 Ethylene Dichloride, technical grade.
in poly(vinyl butyral). 4.1.2 Phenolphthalein Indicator Solution (10 g/L)—
1.2 The procedures appear in the following order: Dissolve1gof phenolphthalein in 100 mL of ethanol (95 %),
methanol, or isopropanol.
Sections
Poly(vinyl alcohol) 4
4.1.3 Potassium Hydroxide, Standard Alcoholic Solu-
Poly(vinyl acetate) 5
tion (0.5 N)—Dissolve 33 g of KOH in methanol and dilute to
Butyraldehyde 6
1 L. Standardize against potassium acid phthalate using phe-
1.3 This standard does not purport to address all of the
nolphthalein indicator solution.
safety concerns, if any, associated with its use. It is the
4.1.4 Pyridine Acetic Anhydride Reagent—Mix slowly
responsibility of the user of this standard to establish appro-
1000mLofpyridineand87mLofaceticanhydride.Makeonly
priate safety and health practices and determine the applica-
about a week’s supply, and keep it in a brown bottle.
bility of regulatory limitations prior to use.
4.2 Procedure:
4.2.1 Transfer 2.2 g of the dry sample to a clean, dry,
2. Referenced Documents
500-mL glass-stoppered flask. Add 25.0 mL of pyridine-acetic
2.1 ASTM Standards:
anhydride reagent. Insert the stopper, and heat the flask on a
D 1193 Specification for Reagent Water
sand or steam bath below the boiling point for 5 ⁄2 h. Swirl
gently until the sample is completely dissolved. Vent the flask
3. Reagents
occasionally during the first part of the heating period to
3.1 Purity of Reagents—Reagent grade chemicals shall be
prevent the stopper from blowing out.
used in all tests. Unless otherwise indicated, it is intended that
4.2.2 At the end of the 5 ⁄2-h period, add 25 mL of ethylene
all reagents shall conform to the specifications of the Commit-
dichloride and shake well. Add 100 mL of water, and shake
tee on Analytical Reagents of the American Chemical Society,
vigorously immediately after adding the water. Let the flask
where such specifications are available. Other grades may be
stand for ⁄2 h.
used, provided it is first ascertained that the reagent is of
4.2.3 Add a few drops of phenolphthalein solution and
sufficiently high purity to permit its use without lessening the
titrate with 0.5 N alcoholic KOH solution. Shake vigorously
accuracy of the determination.
during the titration.
3.2 Purity of Water—Unless otherwise indicated, references
4.2.4 Blank—Run a blank determination on the reagents,
to water shall be understood to mean reagent water conforming
following the same procedure as for the sample.
to Specification D 1193.
4.3 Calculation—Calculate the percentage of poly(vinyl
alcohol) as follows:
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD-1onPaint
Poly~vinyl alcohol!,% 5 ~@B 2 V! N 3 4.4]/ S (1)
and Related Coatings, Materials, and Applications and are the direct responsibility
of Subcommittee D01.33 on Polymers and Resins.
where:
Current edition approved May 15, 1992. Published July 1992. Originally
B = KOH solution required for titration of the blank, mL,
e1
published as D 1396 – 56 T. Last previous edition D 1396 – 73 (1987) .
2 V = KOH solution required for titration of the sample, mL,
Annual Book of ASTM Standards, Vol 11.01.
N = normality of the KOH solution, and
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
S = specimen weight, g.
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
5. Poly(Vinyl Acetate)
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
5.1 Apparatus:
MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1396–92 (1998)
5.1.1 Flask, Wide-Mouth, 500-mLcapacity, equipped with a 0.5 NNaOHsolutiontoagreenendpoint(Note2).Runatleast
metal reflux condenser. two blank determinations checking to within 0.5 mL of each
5.2 Reagents: other, titrating to the same end point at 24 6 2°C (Note 3).
5.2.1 Hydrochloric Acid Standard Alcoholic Solution (0.5
NOTE 2—The pH value of the blank and sample vary with temperature;
N).
if the temperature is raised the green end point will turn yellow and if the
5.2.2 Methanol:
temperature is lowered the green end point will turn blue. The pH value
5.2.3 Phenolphthalein Solution (10 g/L)—See 4.1.2.
of the blank changes more quickly than the pH of the sample solution for
a given change in temperature. Therefore, the blank is titrated and kept at
5.2.4 Potassium Hydroxide Alcoholic Solution (28 g KOH/
24 6 2°C and the sample is titrated at the same temperature.
L)—Disso
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