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ASTM D3545-06

(Test Method)

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

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 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.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for material listed in this specification.
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.

General Information

Status
Historical
Publication Date
31-May-2006
ICS
87.060.30 - Solvents
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.35 - Solvents, Plasticizers, and Chemical Intermediates
Current Stage
Ref Project

Relations

Replaces
ASTM D3545-02 - Standard Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography
Effective Date
01-Jun-2006
Referred By
ASTM D4626-95(2019) - Standard Practice for Calculation of Gas Chromatographic Response Factors
Effective Date
01-Jun-2006
Referred By
ASTM D4614-11(2019) - Standard Specification for Ethyl Acetate (All Grades)
Effective Date
01-Jun-2006
Referred By
ASTM D4615-22 - Standard Specification for <emph type="ital">n</emph>-Butyl Acetate (All Grades)
Effective Date
01-Jun-2006
Referred By
ASTM D3130-11(2019) - Standard Specification for <emph type="bdit">n</emph>-Propyl Acetate (96&#x2009;% Grade)
Effective Date
01-Jun-2006
Referred By
ASTM D1718-09(2023) - Standard Specification for Isobutyl Acetate (95 % Grade)
Effective Date
01-Jun-2006
Referred By
ASTM D3131-07(2021) - Standard Specification for Isopropyl Acetate (99 % Grade)
Effective Date
01-Jun-2006
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
01-Jun-2006
Referred By
ASTM F2931-19a - Standard Guide for Analytical Testing of Substances of Very High Concern in Materials and Products
Effective Date
01-Jun-2006

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ASTM D3545-06 - Standard Test Method for Alcohol Content and Purity of Acetate Esters by Gas ChromatographyASTM D3545-06 - Standard Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography
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ASTM D3545-06 - Standard Test Method for Alcohol Content and Purity of Acetate Esters by Gas Chromatography
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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: D3545 − 06
StandardTest Method for
Alcohol Content and Purity of Acetate Esters by Gas
1
Chromatography
This standard is issued under the fixed designation D3545; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope* D1364 Test Method for Water in Volatile Solvents (Karl
Fischer Reagent Titration Method)
1.1 This test method covers the determination by gas
D1613 Test Method for Acidity in Volatile Solvents and
chromatography of the ester content and the corresponding
Chemical Intermediates Used in Paint, Varnish, Lacquer,
alcohol content of acetate esters. This test method has been
and Related Products
applied to ethyl, n-propyl, isopropyl, n-butyl, isobutyl, and
D2593 Test Method for Butadiene Purity and Hydrocarbon
2-ethoxyethyl acetates.
Impurities by Gas Chromatography
1.2 Water, and in some cases acetic acid, cannot be deter-
E29 Practice for Using Significant Digits in Test Data to
mined by this test method and must be measured by other
Determine Conformance with Specifications
appropriate ASTM procedures and the results used to normal-
E180 Practice for Determining the Precision of ASTM
ize the chromatographic value.
Methods for Analysis and Testing of Industrial and Spe-
3
cialty Chemicals (Withdrawn 2009)
1.3 For purposes of determining conformance of an ob-
served or a calculated value using this test method to relevant E260 Practice for Packed Column Gas Chromatography
specifications, test result(s) shall be rounded off “to the nearest
3. Summary of Test Method
unit” in the last right-hand digit used in expressing the
3.1 A representative specimen is introduced into a gas-
specificationlimit,inaccordancewiththerounding-offmethod
liquid partition column. The acetate is separated from impuri-
of Practice E29.
ties such as alcohols, other esters, ethers, and several uniden-
1.4 The values stated in SI units are to be regarded as
tified compounds while the components are transported
standard. No other units of measurement are included in this
through the column by an inert carrier gas. The separated
standard.
components are measured in the effluent by a detector and
1.5 For specific hazard information and guidance, see the
recorded as a chromatogram. The chromatogram is interpreted
supplier’s Material Safety Data Sheet for material listed in this
by applying component attenuation and detector response
specification.
factors to the peak areas, and the relative concentrations are
determined by relating the individual peak responses to the
1.6 This standard does not purport to address all of the
total peak response. Water and acidity are measured by Test
safety concerns, if any, associated with its use. It is the
Methods D1364 and D1613, respectively, and the results are
responsibility of the user of this standard to establish appro-
used to normalize the values obtained by gas chromatography.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Significance and Use
2. Referenced Documents 4.1 This test method is useful for identifying and for
2 determining the quantity of various impurities in acetate esters.
2.1 ASTM Standards:
4.2 Total purity of the acetate esters must be determined by
use of other appropriate ASTM procedures with this test
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
method.
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
5. Apparatus
Current edition approved June 1, 2006. Published June 2006. Originally
approved in 1976. Last previous edition approved in 2002 as D3545 – 02. DOI:
5.1 Chromatograph—Any gas chromatograph having either
10.1520/D3545-06.
a thermal conductivity or flame ionization detector, provided
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D3545 − 06
the system has sufficient sensitivity and stability to obtain for 6.2.4 Tubing Material—Stainless stee
...

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5.1 Earlier methods for characterizing turpentine and related terpene products were based on physical properties, such as those in Specification D13 and Test Methods D801 and D802, and packed column gas chromatography for the major constituents (for example, α-pinene, β-pinene) as in Test Method D3009. As terpene products became widely used as chemical raw material, the separation and quantitation of compounds present at lower concentrations in the product became more important. The capillary gas chromatographic technique described in these test methods is a rapid and convenient means to perform these analyses.
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Standard Test Method for Odor of Volatile Solvents and Diluents

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3.1 Many pine chemical products contain water as a result of the processes used for their production. Typically refined products such as terpenes, pine oil, tall oil fatty acids, and distilled tall oil contain only traces of water, but crude tall oil might contain 0.5 % to 2.5 % of water. Although the Karl Fischer and coulometric methods are most applicable to low levels of moisture, these can be and are used at higher levels. The azeotropic distillation method is generally used at higher levels.
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1.1 These test methods cover the quantitative determination of dissolved or occluded water present in any proportion in liquid pine chemicals, such as turpentine, pinene, dipentene, pine oil, tall oil, and tall oil fatty acids. Three methods of moisture testing are included. The Karl Fisher titration method is the preferred method for testing tall oil, Test Methods D803.  
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ASTM D804-12(2022)(Terminology)
Standard Terminology Relating to Pine Chemicals, Including Tall Oil and Related Products

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1.1 Although the pine chemical industry has been a continuing producer of chemical products for many centuries, the nature of the industry, its products, and its terminology have changed. In particular, the original practice of recovering pine chemical through the processing of the exudate from pine trees has been supplemented by their extraction by solvent products of the wood pulping industry. For many years the industry was known as the Naval Stores industry but that term has gradually been replaced by the more descriptive and meaningful term, Pine Chemicals Industry. Thus, this terminology contains some old terms now mostly of historic value, together with the terms of the modern pine chemical industry.2  
1.2 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.

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ASTM D6438-05(2022)(Test Method)
Standard Test Method for Acetone, Methyl Acetate, and Parachlorobenzotrifluoride Content of Paints, and Coatings by Solid Phase Microextraction-Gas Chromatography

SIGNIFICANCE AND USE
5.1 In order to calculate the volatile organic content (VOC) of paints containing EPA exempt solvents, it is necessary to know the acetone, methyl acetate, or parachlorobenzotrifluoride content. This gas chromatographic test method provides a simple and direct way for measuring these solvents. Each analyte is measured with respect to a unique internal standard. For acetone, the internal standard used is acetone-d6, for methyl acetate it is methyl acetate-d3, and for PCBTF it is metachlorobenzotrifluoride (MCBTF). These unique analyte/internal standard pairs behave very nearly as single solvents with respect to evaporation rate and adsorption rate onto a coated silica fiber (SPME) but are separable on a gas chromatograph (GC) capillary column. The only critical analytical technique required for successfully performing this test method is the ability of an analyst to weigh a paint sample and internal standard, corresponding to the analyte of interest, into a septum capped vial. After weighing, solvent evaporation has no effect on the final value of the determination. Since whole paint is not injected into the gas chromatograph, the analytical system is never compromised.
SCOPE
1.1 This test method is for the determination of acetone, methyl acetate, or parachlorobenzotrifluoride (PCBTF), or combination of any of the three, in paints and coatings, by solid phase microextraction (SPME) headspace sampling, and subsequent injection into a gas chromatograph. It has been evaluated for cellulose nitrate, acrylic, and urethane solvent-borne systems. The established working range of this test method is: acetone, 28 to 90 %; methyl acetate, 12 to 22 %; parachlorobenzotrifluoride, 10 to 17 %. There is no reason to believe that it will not work outside these ranges. A minor modification of this test method would make it suitable for the analysis of the same analytes in water-borne coatings (see Note 1).
Note 1: Water-borne paints are internally standardized and diluted with water followed by addition of solid sodium chloride.  
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 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

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