ASTM D3546-90(1999)

Standard Test Method for Formic Acid in Glacial Acetic Acid

SCOPE
1.1 This test method covers the determination of the formic acid (and other reducing substances) content of glacial acetic acid by oxidation with lead tetraacetate.  
1.2 This standard does not purport to address the safety problems 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.  
1.3 For hazard information and guidance, see the supplier's Material Safety Data Sheets.

General Information

• Status: Historical
• Publication Date: 09-Dec-1999
• ICS: 71.080.40 - Organic acids
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.35 - Solvents, Plasticizers, and Chemical Intermediates

Relations

• Replaced By: ASTM D3546-05 - Standard Test Method for Formic Acid in Glacial Acetic Acid
• Effective Date: 15-May-2005
• Referred By: ASTM D3620-04(2023) - Standard Specification for Glacial Acetic Acid
• Effective Date: 10-Dec-1999

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3546–90(Reapproved 1999)
Standard Test Method for
Formic Acid in Glacial Acetic Acid
This standard is issued under the fixed designation D 3546; 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 tion, and manufacture. This test method may be used in
assessing compliance with a specification.
1.1 This test method covers the determination of the formic
acid (and other reducing substances) content of glacial acetic
5. Reagents
acid by oxidation with lead tetraacetate.
5.1 Purity of Reagents—Reagent grade chemicals shall be
1.2 This standard does not purport to address all of the
used in all tests. Unless otherwise indicated it is intended that
safety concerns, if any, associated with its use. It is the
all reagents shall conform to the specifications of the Commit-
responsibility of the user of this standard to establish appro-
tee onAnalytical Reagents of theAmerican Chemical Society,
priate safety and health practices and determine the applica-
where such specifications are available. Other grades may be
bility of regulatory limitations prior to use.
used, provided it is first ascertained that the reagent is of
1.3 For hazard information and guidance, see the supplier’s
sufficiently high purity to permit its use without lessening the
Material Safety Data Sheets.
accuracy of the determination.
2. Referenced Documents 5.2 Purity of Water—Unless otherwise indicated reference
to water shall be understood to mean reagent water conforming
2.1 ASTM Standards:
to Type IV of Specification D 1193.
D 1193 Specification for Reagent Water
5.3 Lead Tetraacetate Solution—Dissolve completely 40.0
E 200 Practice for Preparation, Standardization, and Stor-
g of sodium acetate in 1 L of glacial acetic acid and then
age of Standard Solutions for Chemical Analysis
dissolve 40.0 g of lead tetraacetate.
3. Summary of Test Method 5.4 Sodium Thiosulfate Standard Solution (0.1 N)—Prepare
and standardize 0.1 N sodium thiosulfate (Na S O)as
3.1 In an aqueous acetic acid solution each molecule of 2 2 3
described in Practice E 200.
formic acid is oxidized to one molecule of carbon dioxide by
5.5 Starch Indicator Solution—Prepare the starch indicator
reduction of one molecule of lead tetraacetate. The amount of
solution as described in Practice E 200.
lead tetraacetate remaining is then determined by adding
5.6 Stopping Solution—Dissolve 100 g of potassium iodide
potassium iodide and titrating the liberated iodine with stan-
and 500 g of sodium acetate in 1 L of water.
dard sodium thiosulfate solution to the starch end point.
6. Procedure
4. Significance and Use
6.1 Pipet 25 mLof the lead tetraacetate solution into each of
4.1 This test method is useful for determining the formic
two 500-mL Erlenmeyer flasks. Pipet the specimen (Note 1)
acid content of glacial acetic acid by chemical means.
into one of the flasks, swirl, and allow to stand for 20 to 30
4.2 Low molecular weight organic acids (such as acetic and
min. The second flask is the blank.
propionic), aldehydes (including formaldehyde and acetalde-
hyde), ketones, and alcohols (including methyl alcohol) do not
NOTE 1—The following are suggested specimen sizes for varying
interfere with the test.
concentrations of formic acid:
4.3 Formic acid (and other reducing substances) may be
Formic Acid, % Specimen Size, mL
0.0 to 0.10 25
present as a result of contamination during storage, distribu-
0.10 to 0.30 10
0.30 to 0.60 5
0.60 to 1.00 3
1.00 to 2.00 2
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 D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
Current edition approved May 25, 1990. Published July 1990. Originally Reagent Chemicals, American Chemical Society Specifications, American
published as D 3546 – 76. Last previous edition D 3546 – 86. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Perlin, A. S., “
...