ASTM E1616-08

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E1616 − 08
Standard Test Method for
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Analysis of Acetic Anhydride Using Gas Chromatography
This standard is issued under the fixed designation E1616; 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* an intermediate in many chemical processes. Its relative
concentration affects the efficiency of these processes.This test
1.1 This test method describes the determination of assay
method provides a test procedure for assay and impurity
and impurities in acetic anhydride by gas chromatography.The
specification acceptance as well as manufacturing control.
acetic anhydride should be at least 95 % pure.
1.2 The values stated in SI units are to be regarded as
6. Interferences
standard. The values given in parentheses are for information
6.1 This test method describes the chromatographic separa-
only.
tionofpossibleimpuritiesinaceticanhydride.Otherimpurities
1.3 This standard does not purport to address all of the
could coelute with the known components and cause an
safety concerns, if any, associated with its use. It is the
interference. Therefore, an efficient gas chromatographic col-
responsibility of the user of this standard to establish appro-
umn in good condition should be used in order to ensure the
priate safety and health practices and determine the applica-
necessarychromatographicseparationsandproperpeakshapes
bilityofregulatorylimitationspriortouse.Forspecifichazards
so that good quantitative data may be obtained.
statements see Section 9.
6.2 This analysis is based upon the assumption that all
2. Referenced Documents components are eluted from the gas chromatographic column.
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2.1 ASTM Standards:
7. Apparatus
E355 Practice for Gas ChromatographyTerms and Relation-
ships 7.1 Gas Chromatograph—Any gas chromatograph
equipped with a flame ionization detector and a split injection
3. Terminology
system for use with capillary columns that can be operated at
the conditions given in Table 1.
3.1 Definitions—For definitions of terms used in this test
method, see Practice E355.
7.2 Column—The column must give satisfactory resolution
and proper peak shapes for the components listed in Fig. 1.
4. Summary of Test Method
Table 1 contains a description of a column that has been found
4.1 The sample is injected onto a gas chromatographic
satisfactory.
column. The components are separated as they pass through
7.3 Recorder/Integrator—Electronic integration is recom-
the column with helium carrier gas, their presence in the
mended for this analysis.
effluent is detected by a flame ionization detector, and recorded
as a chromatogram. The concentrations of sample components 7.4 Syringe, 10-µL capacity.
are calculated as weight percentages using area normalization.
8. Reagents
5. Significance and Use
8.1 Purity of Reagents—Reagent grade chemicals shall be
5.1 This test method provides for the determination of assay
used in all tests. Unless otherwise indicated, it is intended that
and impurities in acetic anhydride.Acetic anhydride is used as
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
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This test method is under the jurisdiction of ASTM Committee D16 on such specifications are available. Other grades may be used,
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.16 on Industrial and Specialty Product Standards.
Current edition approved April 1, 2008. Published May 2008. Originally
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approved in 1994. Last previous edition approved in 2002 as E1616– 94 (2002) . Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/E1616-08. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
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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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E1616 − 08
TABLE 1 Instrument Conditions for Acetic Anhydride Analysis
9.3 Acetic anhydride is combustible. Its vapor is flammable
Colu
...