ASTM D3594-93(2013)
(Test Method)Standard Test Method for Copolymerized Ethyl Acrylate In Ethylene-Ethyl Acrylate Copolymers (Withdrawn 2019)
Standard Test Method for Copolymerized Ethyl Acrylate In Ethylene-Ethyl Acrylate Copolymers (Withdrawn 2019)
SIGNIFICANCE AND USE
5.1 Ethyl acrylate is copolymerized with ethylene to produce film, molding, and wire coating resins with improved physical properties. Ethyl acrylate comonomer increases flexibility, stress cracking resistance, toughness, and clarity. A rapid quantitative technique is needed for the evaluation of the amount of ethyl acrylate in a resin for specification purposes because physical properties change rapidly with increasing comonomer content.
5.2 Infrared spectrophotometric analysis, when suitably calibrated, can be used for the measurement of the concentration of comonomer present. Calibration is performed with samples that have been analyzed for oxygen content by fast neutron activation analysis. Oxygen content is converted to ethyl acrylate comonomer content by a simple calculation.
5.3 A purpose of the infrared method of analysis is to provide a procedure for use in quality control analysis. It is a rapid, secondary method of analysis as contrasted with the more expensive and time-consuming fast neutron activation analysis which is the primary, calibrating method.
SCOPE
1.1 This test method covers ethylene-ethyl acrylate copolymers containing from 1 to 25 % ethyl acrylate comonomer.
1.2 The values stated in SI units are to be regarded as standard. (See IEEE/ASTM SI-10.)
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 the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Note 1—There is no known ISO equivalent to this standard.
WITHDRAWN RATIONALE
This test method covers ethylene-ethyl acrylate copolymers containing from 1 to 25 % ethyl acrylate comonomer.
Formerly under the jurisdiction of Committee D20 on Plastics, this test method was withdrawn in August 2019. This standard is being withdrawn without replacement due to its limited use by industry.
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D3594 − 93 (Reapproved 2013)
Standard Test Method for
Copolymerized Ethyl Acrylate In Ethylene-Ethyl Acrylate
Copolymers
This standard is issued under the fixed designation D3594; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Summary of Test Method
4.1 The infrared absorption band at 11.60 µm responds to
1.1 This test method covers ethylene-ethyl acrylate copoly-
increases in comonomer content.There is no absorption at this
mers containing from 1 to 25% ethyl acrylate comonomer.
wavelengthwhenthereisnocomonomerpresent.Itapparently
1.2 The values stated in SI units are to be regarded as
is unique and characteristic of the copolymer. There is no
standard. (See IEEE/ASTM SI-10.)
interference from the monomer at this wavelength.
1.3 This standard does not purport to address all of the
4.2 The infrared absorption band at 11.60 µm is of medium
safety problems, if any, associated with its use. It is the
intensity;consequently,fairlythickfilmsareemployed.Thisis
responsibility of the user of this standard to establish appro-
an advantage in that errors in measurements of the thicknesses
priate safety and health practices and determine the applica-
of films have minimal influence on the analytical result. Film
bility of regulatory limitations prior to use.
thicknessisselectedsothatnotmorethan80%oftheinfrared
energy is absorbed at the analytical wavelength. The approxi-
NOTE 1—There is no known ISO equivalent to this standard.
mate thicknesses found to be satisfactory for different concen-
trationsofcomonomerareasfollows:(1)lessthan5weight%
2. Referenced Documents
ethyl acrylate=0.5 mm, (2) 5 to 15 weight% ethyl acry-
2.1 ASTM Standards:
late=0.25 mm, and (3) 15 to 25 weight% ethyl acry-
D883Terminology Relating to Plastics
late=0.18 mm. It is necessary first to press a film approxi-
D1898Practice for Sampling of Plastics (Withdrawn 1998)
mately 0.25 mm in thickness and scan it to observe the
E131Terminology Relating to Molecular Spectroscopy
absorption intensity unless the approximate ethyl acrylate
E168Practices for General Techniques of Infrared Quanti-
content is known.
tative Analysis
4.3 For the highest precision, the test method requires that
E177Practice for Use of the Terms Precision and Bias in
the thickness of the sample film be determined accurately.
ASTM Test Methods
E275PracticeforDescribingandMeasuringPerformanceof
4.4 The general procedure is to scan the absorption band
Ultraviolet and Visible Spectrophotometers
from 10.50 to 12.50 µm, although a single-point measurement
IEEE/ASTM SI-10Standard for Use of the International
may also be used.This test method describes the use of a scan
System of Units (SI): The Modern Metric System
and employs the base-line method as outlined in 7.2 and the
figure illustrating the Base-Line Method for MeasuringAbsor-
3. Terminology
bance of Practices E168. A calibration curve is prepared by
plotting absorbance per millimetre values versus weight per-
3.1 See Terminology D883.
cent ethyl acrylate for several copolymers which have had
ethyl acrylate contents established by a fast neutron activation
analysis of oxygen content. The ethyl acrylate content of an
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
unknown sample is then obtained by referring the absorbance
and is the direct responsibility of Subcommittee D20.70 on Analytical Meth-
per millimetre value to the calibration curve.
ods.70.08).
Current edition approved April 1, 2013. Published April 2013. Originally
approved in 1977. Last previous edition approved in 2006 as D3594-93(2006).
5. Significance and Use
DOI: 10.1520/D3594-93R13.
5.1 Ethyl acrylate is copolymerized with ethylene to pro-
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
duce film, molding, and wire coating resins with improved
Standards volume information, refer to the standard’s Document Summary page on
physical properties. Ethyl acrylate comonomer increases
the ASTM website.
flexibility, stress cracking resistance, toughness, and clarity.A
The last approved version of this historical standard is referenced on
www.astm.org. rapid quantitative technique is needed for the evaluation of the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3594 − 93 (2013)
amount of ethyl acrylate in a resin for specification purposes independentmethod.Thesamplesshouldvaryinethylacrylate
because physical properties change rapidly with increasing contentovertherangefromnearzerotoabout25%.Amethod
comonomer content. that has been found to give high precision and accuracy for
oxygen content is fast neutron activation analysis. The ethyl
5.2 Infrared spectrophotometric analysis, when suitably
acrylate comonomer content, E, is calculated from the oxygen
calibrated, can be used for the measurement of the concentra-
analysis, assuming that all oxygen present is due to ethyl
tion of comonomer present. Calibration is performed with
acrylate, as follows:
samples that have been analyzed for oxygen content by fast
100 3X
neutron activation analysis. Oxygen content is converted to
E, wt% 5 (1)
ethyl acrylate comonomer content by a simple calculation. 31.5
5.3 A purpose of the infrared method of analysis is to
where:
provide a procedure for use in quality control analysis. It is a
X = oxygen content of unknown copolymers, weight%.
rapid, secondary method of analysis as contrasted with the
10.2 Set the controls of the infrared spectrometer for quan-
more expensive and time-consuming fast neutron activation
titative conditions with a good signal-to-noise ratio and satis-
analysis which is the primary, calibrating method.
factory reproducibility. Use a sufficiently expanded chart scale
6. Apparatus such that line width can be measured accurately. Use a
4 scanningspeedsufficientlyslowtogivegoodreproducibilityof
6.1 Infrared Spectrophotometer, capable of spectral resolu-
band shape. Set the slit width narrow enough that there is little
tion equivalent to that defined by Practice E275 and exhibited
distortion of the true band shape. Record the instrument
in Fig. 7 of that practice. The instrument should be capable of
conditions used.
scale expansion along the wavelength (or wave number) axis.
6.1.1 Fourier Transform Infrared Spectrophotometer (FT-
NOTE 2—For the Perkin-Elmer Model 221 Spectrophotometer the
−1
followingsettingsaresatisfactory:PrismNaCl,slits2×,slitprogram927,
IR), with nominal 4 cm resolution.
attenuator speed 600, amplifier gain adjusted to give good response, chart
6.2 Compression-Molding Press, small, with platens ca-
scale 0.01 µm/mm, chart speed 0.5 µm/min, electrical balance and
pable of being heated to 150°C.
suppression adjusted to specifications in instrument manual. Comparable
operating conditions should be used when other instruments are em-
6.3 Metal Plates, two, 150 by 150 mm or larger, of 0.5-mm
ployed.
thickness with smooth surfaces, chromium plated preferably.
10.3 Scan the films from 10.50 to 12.50 µm.
6.4 Brass Shi
...
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