ASTM D2191-97(2001)
(Test Method)Standard Test Method for Acetaldehyde Content of Vinyl Acetate
Standard Test Method for Acetaldehyde Content of Vinyl Acetate
SCOPE
1.1 This test method covers the determination of trace quantities of acetaldehyde, in the range from 0.00 to 0.05%, contained in 99% grade vinyl acetate.
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. For specific hazard statements see Section 8.
1.3 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
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Designation:D2191–97 (Reapproved 2001)
Standard Test Method for
Acetaldehyde Content of Vinyl Acetate
This standard is issued under the fixed designation D 2191; 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 6.4 Pipet, 100-mL capacity.
1.1 This test method covers the determination of trace
7. Reagents
quantities of acetaldehyde, in the range from 0.00 to 0.05 %,
7.1 Purity of Reagents—Unless otherwise indicated, it is
contained in 99 % grade vinyl acetate.
intended that all reagents shall conform to the specifications of
1.2 This standard does not purport to address all of the
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
safety concerns, if any, associated with its use. It is the
cal Society, where such specifications are available. Other
responsibility of the user of this standard to establish appro-
grades may be used provided that it is first ascertained that the
priate safety and health practices and determine the applica-
reagent is of sufficiently high purity to permit its use without
bility of regulatory limitations prior to use. For specific hazard
lessening the accuracy of the determination.
statements see Section 8.
7.2 Purity of Water—Unless otherwise indicated, references
1.3 For hazard information and guidance, see the supplier’s
to water shall be understood to mean reagent water as defined
Material Safety Data Sheet.
by Type IV of Specification D 1193.
2. Referenced Documents 7.3 Iodine, Standard Solution (0.1 N)—Dissolve 35.0 g of
potassiumiodide(KI)and13.0gofresublimediodineinwater,
2.1 ASTM Standards:
and dilute to 1 Lwith water. Store this solution in a dark bottle
D 1193 Specification for Reagent Water
and standardize each day, as required, against a standard 0.1 N
3. Summary of Test Method
sodium thiosulfate (Na S O ) solution. (See standardization
2 2 3
procedure, 9.3 and 9.4.)
3.1 The acetaldehyde present in the specimen is reacted
7.4 Potassium Iodate (KIO ), primary standard.
with a measured excess of sodium bisulfite. The amount of 3
7.5 Sodium Bisulfite Solution (0.44 %)—Dissolve 4.4 g of
sodium bisulfite consumed, determined by titrating the excess
sodium metabisulfite (Na S O ) in 1 L of water. This solution
with a standard iodine solution, is a measure of the acetalde- 2 2 5
should be prepared fresh daily or just before using.
hyde present in the vinyl acetate.
7.6 Sodium Thiosulfate, Standard Solution (0.1 N)—Weigh
4. Significance and Use
to 0.1 g 24.8 g of sodium thiosulfate (Na S O ·5H O) crystals
2 2 3 2
and dissolve in 500 mL of water. Dilute this solution to 1 L
4.1 This test method provides a measurement of acetalde-
with water. Add 0.5 mL of chloroform per litre of solution as
hyde content in vinyl acetate. The results of these measure-
a preservative, and store in a clean dark bottle. This solution
ments can be used for specification acceptance.
should be standardized weekly, as required, against potassium
5. Interference
iodate (KIO ). (See standardization procedure, 9.1 and 9.2.)
7.7 Starch Indicator—Make a paste of6gof powdered
5.1 Ketones and other aldehydes, if present, cause a positive
soluble starch in water, and dilute to 1 L with water, stirring to
interference.
produce a suspension. While stirring, add 20 g of potassium
6. Apparatus
hydroxide (KOH) pellets, and continue stirring until the KOH
is dissolved. Let stand for 2 h and add 27.5 mLof hydrochloric
6.1 Buret, 50-mL capacity, graduated in 0.1-mL subdivi-
acid (HCl).Adjust the mixture to a pH of 6.0 6 0.1 by adding
sions, with a funnel or flared top and a ground-glass stopcock.
small increments of HCl or KOH as required. Add 6 mL of
6.2 Erlenmeyer Flask, 500-mL capacity, glass-stoppered.
glacial acetic acid as a preservative.
6.3 Pipet, 50-mL capacity.
1 3
This test method is under the jurisdiction of ASTM Committee D01 on Paint Reagent Chemicals, American Chemical Society Specifications, American
and Related Coatings, Materials, andApplications and is the direct responsibility of Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved June 10, 1997. Published September 1997. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
e1
published as D 2191 – 63 T. Last previous edition D 2191 – 89 (1993) . and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2191
7.8 Sulfuric Acid (1 N)—Place approximately 700 to 800 10. Procedure
mL of water in a 1-L volumetric flask. Add slowly and with
10.1 Pipet50mLofNa S O solution(7.5)intoeachoftwo
2 2 5
constant stirring 27.2 mLof concentrated sulfuric acid (H SO ,
2 4
glass-stoppered500-mLErlenmeyerflasks.Addapproximately
sp gr 1.84). Allow the solution to cool to room temperature,
25gofcleanchippedicetoeachflaskandintooneoftheflasks
and adjust the volume to the 1-L mark with additional water.
pipet 100 mL of the sample. Grease the stoppers and place the
flasksonamechanicalshaker,allowingthe
...
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