ASTM D3546-05(2011)
(Test Method)Standard Test Method for Formic Acid in Glacial Acetic Acid
Standard Test Method for Formic Acid in Glacial Acetic Acid
SIGNIFICANCE AND USE
This test method is useful for determining the formic acid content of glacial acetic acid by chemical means.
Low molecular weight organic acids (such as acetic and propionic), aldehydes (including formaldehyde and acetaldehyde), ketones, and alcohols (including methyl alcohol) do not interfere with the test.
Formic acid (and other reducing substances) may be present as a result of contamination during storage, distribution, and manufacture. This test method may be used in assessing compliance with a specification.
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 For purposes of determining conformance of an observed or a calculated value using this test method to relevant specifications, test result(s) shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 For hazard information and guidance, see the supplier's Material Safety Data Sheets.
1.5 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.
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Standards Content (Sample)
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Designation: D3546 − 05 (Reapproved 2011)
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* reduction of one molecule of lead tetraacetate. The amount of
lead tetraacetate remaining is then determined by adding
1.1 This test method covers the determination of the formic
potassium iodide and titrating the liberated iodine with stan-
acid (and other reducing substances) content of glacial acetic
2 dard sodium thiosulfate solution to the starch end point.
acid by oxidation with lead tetraacetate.
1.2 For purposes of determining conformance of an ob-
4. Significance and Use
served or a calculated value using this test method to relevant
4.1 This test method is useful for determining the formic
specifications, test result(s) shall be rounded off “to the nearest
acid content of glacial acetic acid by chemical means.
unit” in the last right-hand digit used in expressing the
4.2 Low molecular weight organic acids (such as acetic and
specification limit, in accordance with the rounding-off method
of Practice E29. propionic), aldehydes (including formaldehyde and
acetaldehyde), ketones, and alcohols (including methyl alco-
1.3 The values stated in SI units are to be regarded as
hol) do not interfere with the test.
standard. No other units of measurement are included in this
4.3 Formic acid (and other reducing substances) may be
standard.
present as a result of contamination during storage,
1.4 For hazard information and guidance, see the supplier’s
distribution, and manufacture.This test method may be used in
Material Safety Data Sheets.
assessing compliance with a specification.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Reagents
responsibility of the user of this standard to establish appro-
5.1 Purity of Reagents—Reagent grade chemicals shall be
priate safety and health practices and determine the applica-
used in all tests. Unless otherwise indicated it is intended that
bility of regulatory limitations prior to use.
all reagents shall conform to the specifications of the Commit-
2. Referenced Documents
tee onAnalytical Reagents of theAmerican Chemical Society,
3 where such specifications are available. Other grades may be
2.1 ASTM Standards:
used, provided it is first ascertained that the reagent is of
D1193 Specification for Reagent Water
sufficiently high purity to permit its use without lessening the
E29 Practice for Using Significant Digits in Test Data to
accuracy of the determination.
Determine Conformance with Specifications
E200 Practice for Preparation, Standardization, and Storage 5.2 Purity of Water—Unless otherwise indicated reference
of Standard and Reagent Solutions for ChemicalAnalysis to water shall be understood to mean reagent water conforming
to Type IV of Specification D1193.
3. Summary of Test Method
5.3 Lead Tetraacetate Solution—Dissolvecompletely40.0g
3.1 In an aqueous acetic acid solution each molecule of
ofsodiumacetatein1Lofglacialaceticacidandthendissolve
formic acid is oxidized to one molecule of carbon dioxide by
40.0 g of lead tetraacetate.
5.4 Sodium Thiosulfate Standard Solution (0.1 N)—Prepare
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and standardize 0.1 N sodium thiosulfate (Na S O)asde-
and Related Coatings, Materials, andApplications and is the direct responsibility of 2 2 3
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
scribed in Practice E200.
Current edition approved Feb. 1, 2011. Published February 2011. Originally
approved in 1976. Last previous edition approved in 2005 as D3546 – 05. DOI:
10.1520/D3546-05R11.
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 website. MD.
*A Summary of Changes section appears at the end of this standard
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