ASTM D5594-98(2004)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5594 – 98 (Reapproved 2004)
Standard Test Method for
Determination of the Vinyl Acetate Content of Ethylene-Vinyl
Acetate (EVA) Copolymers by Fourier Transform Infrared
Spectroscopy (FT-IR)
This standard is issued under the fixed designation D5594; 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* Determine the Precision of a Test Method
2.2 ISO Standard:
1.1 This test method covers infrared procedures for deter-
ISO 8985 Plastics—Ethylene/Vinyl Acetate Copolymer
mining the vinyl acetate content of EVA copolymers using
,
Thermoplastics—Determination of Vinyl Acetate
pressed films (Procedure A) or molded plaques (Procedure B)
and internal corrections for sample thickness.
3. Terminology
1.2 This test method is applicable to the analysis of EVA
3.1 Definitions:
copolymers containing 0.5 to 55% vinyl acetate except as
3.1.1 Units, symbols, and abbreviations used in this test
specified in 1.3.
−1 method appear in Terminology E131 or IEEE/ASTM SI-10.
1.3 Talc interferes with the 1020 cm vinyl acetate band.
3.2 Abbreviations:
Resins containing <5% vinyl acetate and talc are excluded
3.2.1 EVA—ethylene-vinyl acetate copolymer.
from the scope of this test method.
3.2.2 PTFE—tetrafluorethylene polymer.
1.4 The values stated in SI units are to be regarded as the
3.2.3 FT-IR—Fourier transform infrared.
standard. The values given in brackets are provided for
information purposes only.
4. Summary of Test Method
1.5 This standard does not purport to address all of the
4.1 The vinyl acetate content is measured using infrared
safety concerns, if any, associated with its use. It is the
−1
absorption band at 1020 cm (0.5 to 5% vinyl acetate) or 609
responsibility of the user of this standard to establish appro-
−1
cm (5 to 55% vinyl acetate).
priate safety and health practices and determine the applica-
4.2 Sample thickness is measured internally using an ethyl-
bility of regulatory limitations prior to use. Specific precau-
−1
ene infrared absorption band at 720 cm (28 to 55% vinyl
tionary statements are given in Section 8.
−1 −1
acetate),2020cm (0.5to28%vinylacetate),or4250cm (5
NOTE 1—This test method is not equivalent to ISO 8985.
to 28% vinyl acetate).
4.3 Regression analysis is performed on vinyl acetate/
2. Referenced Documents
ethylene ratios versus known vinyl acetate contents for EVA
2.1 ASTM Standards:
copolymer standards. The resulting equation is used to calcu-
E131 Terminology Relating to Molecular Spectroscopy
late the vinyl acetate content for subsequent EVA copolymer
E168 Practices for General Techniques of Infrared Quanti-
samples.
tative Analysis
E177 Practice for Use of the Terms Precision and Bias in 5. Significance and Use
ASTM Test Methods
5.1 Properties of EVA copolymers are affected by the
IEEE/ASTMSI-10 UseoftheInternationalSystemofUnits
amount of vinyl acetate incorporated in the copolymer: This
(SI): The Modem Metric System
test method provides a means to determine the vinyl acetate
E691 Practice for Conducting an Interlaboratory Study to
level in copolymer samples.
5.2 Before proceeding with this test method, reference
shouldbemadetothespecificationofthematerialbeingtested.
Any test specimen preparation, conditioning, dimensions, or
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
CurrenteditionapprovedJuly1,2004.PublishedJuly2004.Originallyapproved
in 1994. Last previous edition approved in 1998 as D5594-98. DOI: 10.1520/ Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
D5594-98R04. 4th Floor, New York, NY 10036.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Nicolet 20 S 3B, available from Nicolet Instrument Corp., Analytical Divi-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM sion, 5225 Verona Rd., Madison, WI 53711-4495, and Perkin Elmer 1760, a
Standards volume information, refer to the standard’s Document Summary page on registered trademark of Perkin-Elmer Corp., 761 Main Ave., Norwalk, CT 06859-
the ASTM website. 0156, or equivalents, have been found suitable for this purpose.
*A Summary of Changes section appears at the end of this standard.
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D5594 – 98 (2004)
testing parameters, or a combination thereof, covered in the 9.1.4 Remove the microscope slide from the hot-plate and
materials specification shall take precedence over those men- quenchthepressedpolymerfilmbydippingthetwoslidesinto
tioned in this test method. If there are no material specifica- a beaker of cold water. Remove the film and blot dry with an
tions, then the default conditions apply. absorbent towel.
9.1.5 Absorption maxima, measured on film produced by
6. Apparatus this procedure, shall not exceed 1.5 absorbance units for either
of the analytical bands used.
6.1 Fourier Transform Infrared (FT-IR) Spectrophotometer,
9.2 Procedure B:
equipped with a detector, which gives a linear response over
the desired concentration range, is capable of 4-cm resolution
NOTE 3—Omit 9.2.1 to 9.2.11 for analysis of blown film.
−1
(nominal), and is able to scan from 4400 to 450 cm .
9.2.1 Select a brass or paper mold with a thickness appro-
NOTE 2—ADTGSdetectorhasbeenfoundsuitableforthisapplication.
priatetothevinylacetatecontentofthesample.Theabsorption
6.2 Hot Plate, (Sample Preparation Procedure A only).
maxima of the vinyl acetate and ethylene bands measured on
6.3 Microscope Slides, (Sample Preparation Procedure A the plaque are not to exceed 1.5 absorbance units.
only).
NOTE 4—To meet the absorbance requirement specified in 9.2.1 it will
6.4 Laboratory Press, capable of at least 9000 kg [20000
be necessary to vary the mold thickness as the vinyl acetate content
lb] 150°C [300°F], (Sample Preparation Procedure B only).
changes. The mold thickness required typically will be between 50 and
6.5 Backing Plates, steel or aluminum (Sample Preparation
150 µm [2 to 6 mil].
Procedure B only).
9.2.2 Place a polyester sheet (or fiberglass impregnated
6.6 Brass Shim Stock (Roll),50 to 150 µm [2 to 6 mil] thick
PTFE cloth) followed by a brass or paper mold on a backing
and 150 mm [6 in.] wide (Sample Preparation Procedure B
plate. For resins with vinyl acetate content $40%, a PTFE
only).
film should be placed on top of the brass mold, or, if using a
6.7 Polyester Sheet, or fiberglass impregnated PTFE cloth
paper mold, under the paper.
(Sample Preparation Procedure B only).
9.2.3 Place a quantity of sample, appropriate to the thick-
6.8 PTFE Film (Sample Preparation Procedure B, resins
ness of the mold used, in the center of each opening in the
containing$40% vinyl acetate only).
mold.Donotoverfillthemoldopenings.Ifflashingoccurs,the
6.9 Templates, (mold) with 150 3150 mm [6 36 in.]
brass mold and backing plates can be cleaned with a nylon
pieces of paper or brass shim stock (item 6.6) containing
scrubbing pad.
cavities of a size and shape appropriate for the sample holders
9.2.4 Place another piece of polyester sheet (or fiberglass
used, and, if applicable, sheets of items 6.7 and 6.8 (Sample
impregnated PTFE cloth) and a backing plate on top of the
Preparation Procedure B only).
sample. For resins with vinyl acetate content$40%, a PTFE
6.10 Cooling Block, steel or aluminum, at least 150 3150
film should be placed over the sample before the polyester
mm [6 36 in.], approximately 25 mm [1 in.] thick, channeled
sheet (or fiberglass impregnated PTFE cloth).
for cooling water (Sample Preparation Procedure B only).
9.2.5 Place the resulting “sandwich” in the press with the
platens heated at 150 to 175°C.
7. Materials
9.2.6 Close the press until the top platen barely touches the
7.1 EVA copolymer standards containing nominal vinyl
top plate and leave for sufficient time to permit the sample to
acetate concentrations of 0.5 to 55%, by weight.
soften and outgas.
7.2 Dry ice (Sample Preparation B Procedure A only).
NOTE 5—Acceptable plaques, free of gas bubbles, have been obtained
when the sample is allowed to soften for 3 min.
8. Hazards
8.1 Care should be taken to avoid burns when handling
9.2.7 Closethepresscompletelyandapplyatleast9000kg
microscope slides on the hot-plate (Sample Preparation Proce-
[20000 lb] force for approximately 1 min.
dureA),andglovesshouldbewornwhenplaquesareprepared
9.2.8 Cool the “sandwich” to room temperature, release the
using a heated press (Sample Preparation Procedure B).
pressure, and remove the “sandwich” from the press.
8.2 Care also should be taken to avoid breaking the micro-
9.2.9 In cases where the press does not have cooling
scope slides while removing the pressed polymer film.
capability or where sample throughput needs to be increased,
8.3 Care should be taken to avoid burns when handling dry
thefollowingalternativeto9.2.8maybeused.The“sandwich”
ice.
is removed from the press hot and placed on a metal cooling
blockthroughwhichcoldwateriscirculated.Amassofatleast
9. Specimen Preparation
4 kg [9 lb] is placed on top to the “sandwich” while it cools to
room temperature.
9.1 Procedure A:
9.2.10 Forresinswithvinylacetatecontent<40%,separate
9.1.1 Control the hot-plate temperature at 250 610°C.
9.1.2 Place a microscope slide, containing a fraction of the the backing plates and remove the plaques from the mold.
sample pellet, on the hot-plate. 9.2.11 For resins with vinyl acetate content$40%, place
9.1.3 Cover the sample with another slide and press with a the“sandwich”ondryiceforatleast15sbeforeseparatingthe
wooden pestle. Use film circular motions to press a uniform backingplate,polyestersheet(orfiberglassimpregnatedPTFE
film. cloth), and the PTFE film from the plaque.
D5594 – 98 (2004)
10.9 A minimum of five standards shall be used for the
linear regression of the 0.5 to 5.0% vinyl acetate r
...