ASTM D3545-95

Standard Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography

SCOPE
1.1 This test method covers the determination by gas chromatography of the ester content and the corresponding alcohol content of acetate esters. This test method has been applied to ethyl,  n-propyl, isopropyl, n-butyl, isobutyl, and 2-ethoxyethyl acetates.
1.2 Water, and in some cases acetic acid, cannot be determined by this test method and must be measured by other appropriate ASTM procedures and the results used to normalize the chromatographic value.
1.3 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.
1.4 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for material listed in this specification.

General Information

• Status: Historical
• Publication Date: 09-Jan-2002
• ICS: 87.060.30 - Solvents
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.35 - Solvents, Plasticizers, and Chemical Intermediates

Relations

• Replaced By: ASTM D3545-02 - Standard Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography
• Effective Date: 10-Jan-2002
• Referred By: ASTM D3131-07(2021) - Standard Specification for Isopropyl Acetate (99 % Grade)
• Effective Date: 10-Jan-2002
• Referred By: ASTM D4615-22 - Standard Specification for <emph type="ital">n</emph>-Butyl Acetate (All Grades)
• Effective Date: 10-Jan-2002
• Referred By: ASTM D3130-11(2019) - Standard Specification for <emph type="bdit">n</emph>-Propyl Acetate (96&#x2009;% Grade)
• Effective Date: 10-Jan-2002
• Referred By: ASTM D1718-09(2023) - Standard Specification for Isobutyl Acetate (95 % Grade)
• Effective Date: 10-Jan-2002
• Referred By: ASTM F2931-19a - Standard Guide for Analytical Testing of Substances of Very High Concern in Materials and Products
• Effective Date: 10-Jan-2002
• Referred By: ASTM D4614-11(2019) - Standard Specification for Ethyl Acetate (All Grades)
• Effective Date: 10-Jan-2002
• Referred By: ASTM D268-22 - Standard Guide for Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material
• Effective Date: 10-Jan-2002
• Referred By: ASTM D4626-95(2019) - Standard Practice for Calculation of Gas Chromatographic Response Factors
• Effective Date: 10-Jan-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3545 – 95
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Alcohol Content and Purity of Acetate Esters by Gas
Chromatography
This standard is issued under the fixed designation D 3545; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope liquid partition column. The acetate is separated from impuri-
ties such as alcohols, other esters, ethers, and several uniden-
1.1 This test method covers the determination by gas
tified compounds while the components are transported
chromatography of the ester content and the corresponding
through the column by an inert carrier gas. The separated
alcohol content of acetate esters. This test method has been
components are measured in the effluent by a detector and
applied to ethyl, n-propyl, isopropyl, n-butyl, isobutyl, and
recorded as a chromatogram. The chromatogram is interpreted
2-ethoxyethyl acetates.
by applying component attenuation and detector response
1.2 Water, and in some cases acetic acid, cannot be deter-
factors to the peak areas, and the relative concentrations are
mined by this test method and must be measured by other
determined by relating the individual peak responses to the
appropriate ASTM procedures and the results used to normal-
total peak response. Water and acidity are measured by Test
ize the chromatographic value.
Methods D 1364 and D 1613, respectively, and the results are
1.3 This standard does not purport to address all of the
used to normalize the values obtained by gas chromatography.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
4.1 This test method is useful for identifying and for
bility of regulatory limitations prior to use.
determining the quantity of various impurities in acetate esters.
1.4 For specific hazard information and guidance, see the
4.2 Total purity of the acetate esters must be determined by
supplier’s Material Safety Data Sheet for material listed in this
use of other appropriate ASTM procedures with this test
specification.
method.
2. Referenced Documents
5. Apparatus
2.1 ASTM Standards:
5.1 Chromatograph—Any gas chromatograph having either
D 1364 Test Method for Water in Volatile Solvents (Karl
a thermal conductivity or flame ionization detector, provided
Fischer Reagent Titration Method)
the system has sufficient sensitivity and stability to obtain for
D 1613 Test Method for Acidity in Volatile Solvents and
0.01 % of the parent alcohol a recorder deflection of at least 20
Chemical Intermediates Used in Paint, Varnish, Lacquer,
2 mm at a signal-to-noise ratio of at least 5 to 1. The specimen
and Related Products
size used in judging the sensitivity must be such that the
D 2593 Test Method for Butadiene Purity and Hydrocarbon
3 column is not overloaded, which would result in peak broad-
Impurities by Gas Chromatography
ening, loss of resolution, shifting retention times and formation
E 180 Practice for Determining the Precision of ASTM
4 of leading peaks. Volumes of 5 μL with thermal conductivity
Methods for Analysis and Testing of Industrial Chemicals
5 and 1 to 2 μL with flame ionization detectors have been found
E 260 Practice for Packed Column Gas Chromatography
acceptable.
3. Summary of Test Method 5.1.1 The injection port of the chromatograph must have a
volume of at least 1.2 mL to provide for proper vaporization of
3.1 A representative specimen is introduced into a gas-
the material. The use of a smaller injection port or on-column
injection has been found to cause peak broadening and tailing.
5.2 Column—A 3-m length of 6.4-mm outside diameter
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applicationsand is the direct responsibility of
aluminum or stainless steel tubing packed with 80 to 100-mesh
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. 6
Chromosorb G-HP that has been coated with 9.05 % Dow
Current edition approved Feb. 15, 1995. Published April 1995. Originally
published as D 3545 – 76. Last previous edition D 3545 – 90.
Annual Book of ASTM Standards, Vol 06.04.
Annual Book of ASTM Standards, Vol 05.01.
4 6
Annual Book of ASTM Standards, Vol 15.05. A registered trademark of Manville Products Corp., Lompoc, CA 93436, has
Annual Book of ASTM Standards, Vol 14.02. been found suitable for this purpose.
D 3545
7 8
Corning QF-1 silicone and 0.45 % Igepal CO-990. Any both, are available from several chromatography supply
column, packed or capillary, or any packing material giving sources.
equivalent or superior performance may be used. 7.3 Chromatograph—Install the column in the chromato-
5.3 Recorder—A recording potentiometer with a full-scale graph. Use the information in Table 1 as a guide to establish the
deflection of 1 mV. Full-scale response time should be2sor conditions of column temperature and carrier gas flow that give
less with sufficient sensitivity and stability to meet the require- the necessary resolution of the components in the product
ments of 5.1. being analyzed. Allow sufficient time for the instrument to
5.4 Specimen Introduction System—Any system capable of reach equilibrium as indicated by a stable recorder baseline.
introducing a representative specimen into the column. Mi- Control the detector temperature constant to within 1°C with-
crolitre syringes have been used successfully. out thermostat cycling, which causes an uneven baseline.
Adjust the carrier-gas flow rate to a constant value.
6. Reagents and Materials
NOTE 1—Useful information on column preparation may be found in
6.1 Carrier Gas, appropriate to the type of detector used.
Test Method D 2593 and Practice E 260.
Helium or hydrogen may be employed with thermal conduc-
tivity detectors and nitrogen, helium, or argon with flame
8. Calibration and Standardization
ionization detectors. The minimum purity of the carrier gas
8.1 Identification—Determine the retention time of each
used should be 99.95 mol %.
component by injecting small amounts either separately or in
6.1.1 If hydrogen is used special safety precautions must be
known mixtures. The esters should elute close to the typical
taken to ensure that the system is free of leaks and that the
retention times given in Table 1 and the chromatograms should
effluent is vented properly.
closely approximate those shown in Figs. 1-6.
6.2 Column Materials:
8.2 The area under each peak of the chromatogram is
6.2.1 Liquid Phase, Dow Corning QF-1/FS 1265 silicone
considered a quantitative measure of the corresponding com-
and Igepal CO-990.
pound. The relative area is proportional to concentration if the
6.2.2 Solid Support, Chromosorb G-HP, 80 to 100 mesh
detector responds equally to all the sample components. The
size.
response to different components is generally significantly
6.2.3 Solvents—Methylene chloride and acetone, reagent
different for both flame ionization and thermal conductivity
grade.
detectors and especially for flame ionization detectors. Differ-
6.2.4 Tubing Material—Stainless steel and aluminum have
ence in detector response may be corrected by use of relative
been found satisfactory for column tubing. The tubing must be
response factors obtained by injecting and measuring the
nonreactive with the substrate, sample, and carrier gas and
response to known blends. For precise and accurate determi-
must be of uniform internal diameter.
nation of the parent alcohol, prepare and analyze a known
6.3 Standards for Calibration and Identification—Standard
blend of the acetate and alcohol in which the alcohol content
samples of all components present are needed for identification
approximates the maximum specification limit. Calculate the
by retention time and for calibration for quantitative measure-
alcohol response factor relative to unity for the acetate. With
ments. Most can be obtained from chemical supply houses.
thermal conductivity detectors, the response factor of all
impurities other than the alcohol may be assumed to be one for
7. Preparation of Apparatus
obtaining the purity value. With flame ionization detectors, use
7.1 Column Packing Preparation—Place 100 g of Chro-
experimentally determined response factors.
mosorb G-HP, 80 to 100 mesh, in a large evaporating dish.
NOTE 2—Data on thermal conductivity and fl
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