ASTM D3546-05(2019)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3546 − 05 (Reapproved 2019)
Standard Test Method for
Formic Acid in Glacial Acetic Acid
This standard is issued under the fixed designation D3546; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope Determine Conformance with Specifications
E200 Practice for Preparation, Standardization, and Storage
1.1 This test method covers the determination of the formic
of Standard and Reagent Solutions for ChemicalAnalysis
acid (and other reducing substances) content of glacial acetic
acid by oxidation with lead tetraacetate.
3. Summary of Test Method
1.2 For purposes of determining conformance of an ob-
3.1 In an aqueous acetic acid solution, each molecule of
served or a calculated value using this test method to relevant
formic acid is oxidized to one molecule of carbon dioxide by
specifications, test result(s) shall be rounded off “to the nearest
reduction of one molecule of lead tetraacetate. The amount of
unit” in the last right-hand digit used in expressing the
lead tetraacetate remaining is then determined by adding
specification limit, in accordance with the rounding-off method
potassium iodide and titrating the liberated iodine with stan-
of Practice E29.
dard sodium thiosulfate solution to the starch end point.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 4. Significance and Use
standard.
4.1 This test method is useful for determining the formic
1.4 For hazard information and guidance, see the supplier’s acid content of glacial acetic acid by chemical means.
Material Safety Data Sheets.
4.2 Low molecular weight organic acids (such as acetic and
1.5 This standard does not purport to address all of the
propionic), aldehydes (including formaldehyde and
safety concerns, if any, associated with its use. It is the acetaldehyde), ketones, and alcohols (including methyl alco-
responsibility of the user of this standard to establish appro-
hol) do not interfere with the test.
priate safety, health, and environmental practices and deter-
4.3 Formic acid (and other reducing substances) may be
mine the applicability of regulatory limitations prior to use.
present as a result of contamination during storage,
1.6 This international standard was developed in accor-
distribution, and manufacture.This test method may be used in
dance with internationally recognized principles on standard-
assessing compliance with a specification.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5. Reagents
mendations issued by the World Trade Organization Technical
5.1 Purity of Reagents—Reagent-grade chemicals shall be
Barriers to Trade (TBT) Committee.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
2. Referenced Documents
tee onAnalytical Reagents of theAmerican Chemical Society,
2.1 ASTM Standards: 4
where such specifications are available. Other grades may be
D1193 Specification for Reagent Water
used, provided it is first ascertained that the reagent is of
E29 Practice for Using Significant Digits in Test Data to
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
5.2 Purity of Water—Unless otherwise indicated, reference
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
to water shall be understood to mean reagent water conforming
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
to Type IV of Specification D1193.
Current edition approved April 1, 2019. Published April 2019. Originally
approved in 1976. Last previous edition approved in 2011 as D3546 – 05 (2011).
DOI: 10.1520/D3546-05R19.
2 4
Perlin, A. S., “Determination of Formic Acid by Oxidation with Lead Reagent Chemicals, American Chemical Society Specifications, American
Tetraacetate,” Analytical Chemistry, Vol 26, 1954, pp. 1053–1054. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM
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