ASTM D3362-93(2000)
(Test Method)Standard Test Method for Purity of Acrylate Esters by Gas Chromatography
Standard Test Method for Purity of Acrylate Esters by Gas Chromatography
SCOPE
1.1 This test method covers the determination of the purity of acrylate, ethyl acrylate, n-butyl acrylate, and 2-ethylhexyl acrylate by gas chromatography and, in addition, provides a means for measuring certain impurities such as alcohols and other esters. Water and acidity are measured by other appropriate ASTM procedures and the results are used to normalize the chromatographic values.
1.2 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of whoever uses this standard to consult and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3362–93 (Reapproved 2000)
Standard Test Method for
Purity of Acrylate Esters by Gas Chromatography
This standard is issued under the fixed designation D 3362; 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.
1. Scope 3. Summary of Method
1.1 This test method covers the determination of the purity 3.1 A representative specimen is introduced into a gas
of acrylate, ethyl acrylate, n-butyl acrylate, and 2-ethylhexyl chromatographic column. The acrylate ester is separated from
acrylate by gas chromatography and, in addition, provides a impurities such as alcohols, other esters, ethers, and several
means for measuring certain impurities such as alcohols and unidentified compounds as the components are transported
other esters. Water and acidity are measured by other appro- through the column by an inert carrier gas. The separated
priate ASTM procedures and the results are used to normalize components are measured in the effluent by a detector and
the chromatographic values. recorded as a chromatogram. The chromatogram is interpreted
1.2 For hazard information and guidance, see the supplier’s by applying component attenuation and detector response
Material Safety Data Sheet. factors to the peak areas and the relative concentrations are
1.3 This standard does not purport to address all of the determined by relating the individual peak responses to the
safety problems, if any, associated with its use. It is the total peak response. Water and acidity are measured by the
responsibility of whoever uses this standard to consult and procedures listed in Test Methods D 1364 and D 1613 and the
establish appropriate safety and health practices and deter- results are used to normalize the values obtained by gas
mine the applicability of regulatory limitations prior to use. chromatography.
Specific hazard statements are given in Section 7.
4. Significance and Use
2. Referenced Documents
4.1 This test method provides a measurement of commonly
2.1 ASTM Standards: found impurities in commercially available methyl acrylate,
D 1364 Test Method for Water in Volatile Solvents (Fischer ethyl acrylate, butyl acrylate, and 2-ethylhexyl acrylate. The
Reagent Titration Method) measurement of these impurities and the results thereof can
D 1613 Test Method for Acidity in Volatile Solvents and either individually or when totaled and subtracted from 100
Chemical Intermediates Used in Paint, Varnish, Lacquer, (assay) be used for specification purposes.
and Related Products
5. Apparatus
D 2593 Test Method for Butadiene Purity and Hydrocarbon
Impurities by Gas Chromatography 5.1 Chromatograph—Any gas chromatograph having either
a thermal conductivity or flame ionization detector, provided
E 180 Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial and Spe- the system has sufficient sensitivity and stability to obtain for
0.01 weight % of impurity a recorder deflection of at least 2
cialty Chemicals
E 260 Practice for Packed Column Gas Chromatography mm at a signal-to-noise ratio of at least 5 to 1. The specimen
size used in judging the sensitivity must be such that the
column is not overloaded.
5.2 Column, 6 m (20 ft) of 6.4-mm ( ⁄4 in.).
5.3 Specimen Introduction System—Any system capable of
introducing a representative specimen into the column. Mi-
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
crolitre syringes have been used successfully.
and Related Coatings, Materials, andApplications and is the direct responsibility of
5.4 Recorder—A recording potentiometer, or electronic
Subcommittee D 01.35 on Solvents, Plasticizers, and Chemical Intermediates.
meter with a full-scale deflection of 1 mV, full-scale response
Current edition approved July 15, 1993. Published September 1993. Originally
published as D 3362 – 74. Last previous edition D 3362 – 84 (1987).
Annual Book of ASTM Standards, Vol 06.04.
Annual Book of ASTM Standards, Vol 05.01.
Messner, A. E., et al, Analytical Chemistry, ANCHA, Vol 31, 1959, pp.
Annual Book of ASTM Standards, Vol 15.05.
230–233, Dietz, W. A., Journal of Gas Chromatography, JGCRA, Vol 5, No. 2,
Annual Book of ASTM Standards, Vol 14.02.
February 1967, pp. 68–71.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3362
time of2sor less, and sufficient sensitivity and stability to 9. Calibration and Standardization
meet the requirements of 5.1.
9.1 Using the information in Table 1 as a guide, select the
conditions of column temperature and carrier gas flow that will
6. Reagents and Materials
givethenecessaryresolutionofthecomponents.Determinethe
6.1 Carrier Gas, appropriate to the type of detector used.
retention time of each component by injecting small amounts
Helium or hydrogen may be employed with thermal conduc-
either separately or in known mixtures. Relative component
tivity detectors, and nitrogen, helium, or argon with flame
retention times along with the typical retention times for
ionization detectors. The minimum purity of the carrier gas
methylacrylate,ethylacrylate,butylacrylate,and2-ethylhexyl
used should be 99.95 mol %.
acrylate are given in Table 1.
6.1.1 Warning—If hydrogen is used, take special safety
9.2 Standardization—The area under each peak of the
precautions to ensure that the system is free of leaks and that
chromatogram is considered a quantitative measure of the
the effluent is vented properly.
corresponding compound. The relative area is proportional to
6.2 Column Materials:
7 concentration if the detector responds equally to all the sample
6.2.1 Liquid Phase— lubricant.
8 components. When flame ionization detectors are used the
6.2.2 Solid Support—synthetic polyester wax, acid-
response to different components is generally significantly
washed, 45 to 60 mesh size. Only acid-washed material
different. Differences in detector response may be corrected by
performs satisfactorily.
use of relative response factors obtained by injecting and
6.2.3 Solvent—Methylene chloride, reagent grade.
measuring the response to pure (99 % weight minimum)
6.2.4 Tubing Material—Copper, stainless steel, and alumi-
compounds or known blends. When thermal conductivity
num have been found satisfactory for column tubing. The
detectorsareusedfortheanalysisofhighpurityacrylateesters,
tubing must be nonreactive with the substrate, sample, and
the difference between area percent and weight percent is
carrier gas.
within the precision of the method.
6.3 Standards for Calibration and Identification—Standard
samples of all components present are needed for identification
NOTE 3—Data on thermal conductivity and flame ionization detector
by retention time, and for calibration for quantitative measure-
responses may be found
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.