ASTM D3546-05
(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 tetraacetate².
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 E 29.
1.4This 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.
1.5 For hazard information and guidance, see the supplier's Material Safety Data Sheets.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3546–05
Standard Test Method for
1
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* lead tetraacetate remaining is then determined by adding
potassium iodide and titrating the liberated iodine with stan-
1.1 This test method covers the determination of the formic
dard sodium thiosulfate solution to the starch end point.
acid (and other reducing substances) content of glacial acetic
2
acid by oxidation with lead tetraacetate.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as
4.1 This test method is useful for determining the formic
standard. No other units of measurement are included in this
acid content of glacial acetic acid by chemical means.
standard.
4.2 Low molecular weight organic acids (such as acetic and
1.3 For purposes of determining conformance of an ob-
propionic), aldehydes (including formaldehyde and acetalde-
served or a calculated value using this test method to relevant
hyde), ketones, and alcohols (including methyl alcohol) do not
specifications, test result(s) shall be rounded off “to the nearest
interfere with the test.
unit” in the last right-hand digit used in expressing the
4.3 Formic acid (and other reducing substances) may be
specification limit, in accordance with the rounding-off method
present as a result of contamination during storage, distribu-
of Practice E29.
tion, and manufacture. This test method may be used in
1.4 This standard does not purport to address all of the
assessing compliance with a specification.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Reagents
priate safety and health practices and determine the applica-
5.1 Purity of Reagents—Reagent grade chemicals shall be
bility of regulatory limitations prior to use.
used in all tests. Unless otherwise indicated it is intended that
1.5 For hazard information and guidance, see the supplier’s
all reagents shall conform to the specifications of the Commit-
Material Safety Data Sheets.
tee onAnalytical Reagents of theAmerican Chemical Society,
4
where such specifications are available. Other grades may be
2. Referenced Documents
3
used, provided it is first ascertained that the reagent is of
2.1 ASTM Standards:
sufficiently high purity to permit its use without lessening the
D1193 Specification for Reagent Water
accuracy of the determination.
E29 Practice for Using Significant Digits in Test Data to
5.2 Purity of Water—Unless otherwise indicated reference
Determine Conformance with Specifications
to water shall be understood to mean reagent water conforming
E200 Practice for Preparation, Standardization, and Storage
to Type IV of Specification D1193.
of Standard and Reagent Solutions for Chemical Analysis
5.3 Lead Tetraacetate Solution—Dissolve completely 40.0
3. Summary of Test Method g of sodium acetate in 1 L of glacial acetic acid and then
dissolve 40.0 g of lead tetraacetate.
3.1 In an aqueous acetic acid solution each molecule of
5.4 Sodium Thiosulfate Standard Solution (0.1 N)—Prepare
formic acid is oxidized to one molecule of carbon dioxide by
and standardize 0.1 N sodium thiosulfate (Na S O)as
reduction of one molecule of lead tetraacetate. The amount of 2 2 3
described in Practice E200.
5.5 Starch Indicator Solution—Prepare the starch indicator
solution as described in Practice E200.
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
5.6 Stopping Solution—Dissolve 100 g of potassium iodide
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
and 500 g of sodium acetate in 1 L of water.
Current edition approved May 15, 2005. Published June 2005. Originally
approved in 1976. Last previous edition approved in 1999 as D3546 – 90 (1999).
DOI: 10.1520/D3546-05.
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
3
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 informa
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.