ASTM D3594-93(2000)
(Test Method)Standard Test Method for Copolymerized Ethyl Acrylate In Ethylene-Ethyl Acrylate Copolymers
Standard Test Method for Copolymerized Ethyl Acrylate In Ethylene-Ethyl Acrylate Copolymers
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 the standard. (See Practice E380.)
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 similar or equivalent ISO standard.
General Information
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 3594 – 93 (Reapproved 2000)
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope wavelengthwhenthereisnocomonomerpresent.Itapparently
is unique and characteristic of the copolymer. There is no
1.1 This test method covers ethylene-ethyl acrylate copoly-
interference from the monomer at this wavelength.
mers containing from 1 to 25% ethyl acrylate comonomer.
4.2 The infrared absorption band at 11.60 µm is of medium
1.2 The values stated in SI units are to be regarded as the
intensity;consequently,fairlythickfilmsareemployed.Thisis
standard. (See Practice E380.)
an advantage in that errors in measurements of the thicknesses
1.3 This standard does not purport to address all of the
of films have minimal influence on the analytical result. Film
safety problems, if any, associated with its use. It is the
thicknessisselectedsothatnotmorethan80%oftheinfrared
responsibility of the user of this standard to establish appro-
energy is absorbed at the analytical wavelength. The approxi-
priate safety and health practices and determine the applica-
mate thicknesses found to be satisfactory for different concen-
bility of regulatory limitations prior to use.
trationsofcomonomerareasfollows:(1)lessthan5weight%
NOTE 1—There is no similar or equivalent ISO standard.
ethyl acrylate=0.5 mm, ( 2) 5 to 15 weight% ethyl acry-
late=0.25 mm, and (3) 15 to 25 weight% ethyl acry-
2. Referenced Documents
late=0.18 mm. It is necessary first to press a film approxi-
2.1 ASTM Standards:
mately 0.25 mm in thickness and scan it to observe the
B883 Terminology Relating to Plastics
absorption intensity unless the approximate ethyl acrylate
D1898 Practice for Sampling of Plastics
content is known.
E131 Terminology Relating to Molecular Spectroscopy
4.3 For the highest precision, the test method requires that
E168 Practices for General Techniques of Infrared Quanti-
the thickness of the sample film be determined accurately.
tative Analysis
4.4 The general procedure is to scan the absorption band
E177 Practice for Use of the Terms Precision and Bias in
from 10.50 to 12.50 µm, although a single-point measurement
ASTM Test Methods
may also be used.This test method describes the use of a scan
E275 Practice for Describing and Measuring Performance
and employs the base-line method as outlined in 7.2 and the
of Ultraviolet, Visible, and Near Infrared Spectrophotom-
figure illustrating the Base-Line Method for MeasuringAbsor-
eters
bance of Practices E168. A calibration curve is prepared by
E380 Practice for Use of the International System of Units
plotting absorbance per millimetre values versus weight per-
(SI)
cent ethyl acrylate for several copolymers which have had
ethyl acrylate contents established by a fast neutron activation
3. Terminology
analysis of oxygen content. The ethyl acrylate content of an
3.1 See Terminology D883.
unknown sample is then obtained by referring the absorbance
per millimetre value to the calibration curve.
4. Summary of Test Method
4.1 The infrared absorption band at 11.60 µm responds to
5. Significance and Use
increases in comonomer content.There is no absorption at this
5.1 Ethyl acrylate is copolymerized with ethylene to pro-
duce film, molding, and wire coating resins with improved
1 physical properties. Ethyl acrylate comonomer increases flex-
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods ibility, stress cracking resistance, toughness, and clarity. A
(Section D20.70.08).
rapid quantitative technique is needed for the evaluation of the
Current edition approved Feb. 15, 1993. Published April 1993. Originally
amount of ethyl acrylate in a resin for specification purposes
published as D3594–77. Last previous edition D3594–77 (1987).
because physical properties change rapidly with increasing
Annual Book of ASTM Standards, Vol 08.01.
Annual Book of ASTM Standards, Vol 08.02. comonomer content.
Annual Book of ASTM Standards, Vol 14.01.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3594
5.2 Infrared spectrophotometric analysis, when suitably oxygen content is fast neutron activation analysis. The ethyl
calibrated, can be used for the measurement of the concentra- acrylate comonomer content, E, is calculated from the oxygen
tion of comonomer present. Calibration is performed with analysis, assuming that all oxygen present is due to ethyl
samples that have been analyzed for oxygen content by fast acrylate, as follows:
neutron activation analysis. Oxygen content is converted to
100 3 X
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
such that line width can be measured accurately. Use a
6. Apparatus
scanningspeedsufficientlyslowtogivegoodreproducibilityof
6.1 Infrared Spectrophotometer, capable of spectral resolu-
band shape. Set the slit width narrow enough that there is little
tion equivalenttothatdefinedbyPracticeE275andexhibited
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.
NOTE 2—For the Perkin-Elmer Model 221 Spectrophotometer the
6.1.1 Fourier Transform Infrared Spectrophotometer (FT-
−1
followingsettingsaresatisfactory:PrismNaCl,slits2X,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
6.3 Metal Plates, two, 150 by 150 mm or larger, of 0.5-mm
operating conditions should be used when other instruments are em-
thickness with smooth surfaces, chromium plated preferably.
ployed.
6.4 Brass Shims, three, approximately 75 by 75 mm and
10.3 Scan the films from 10.50 to 12.50 µm.
thicknesses of 0.50 mm, 0.25 mm, and 0.18 mm, with an
NOTE 3—Films having high gloss may exhibit interference fringes in
apert
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