ASTM D5227-95
(Test Method)Standard Test Method for Measurement of Hexane Extractable Content of Polyolefins
Standard Test Method for Measurement of Hexane Extractable Content of Polyolefins
SCOPE
1.1 This test method describes an extraction/gravimetric procedure for determination of the amount of hexane soluble low molecular weight material present in polyethylene, polypropylene, ethylene-propylene copolymers, and ethylene-vinyl acetate copolymers. This test method is a modification of the Food and Drug Administration (FDA) procedure for determining hexane extractables of polyolefins. This test method is based upon the presumption that the weight of the residue extract present in the solvent is equal to the amount extracted from the film sample and could therefore be quantified by measuring the weight loss of the extracted film, eliminating the complex and time-consuming evaporation process described in 21 CFR 177.1520.
1.2 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.
1.3 The values stated in SI units are to be regarded as the standard. Units used in 21 CFR 177.1520 are aslo used in this test methhod. Units are in conformance with Federal Code 21 CFR 177.1520, from which this test method is derived.
Note 1--There is no similar or equivalent ISO standard.
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5227 – 95 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Measurement of Hexane Extractable Content of Polyolefins
This standard is issued under the fixed designation D 5227; 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. Terminology
1.1 This test method describes an extraction/gravimetric 3.1 Units, symbols, and abbreviations used in this test
procedure for determination of the amount of hexane soluble method are in accordance with the definitions given in Termi-
low molecular weight material present in polyethylene, nology 883, and Terminology E 131 or Practice E 380.
ethylene-propylene copolymers, and ethylene-vinyl acetate 3.2 Abbreviations:
copolymers. This test method is a modification of the Food and 3.2.1 EVA—ethylene-vinyl acetate copolymer.
Drug Administration (FDA) procedure for determining hexane 3.2.2 LDPE—low-density polyethylene.
extractables of polyolefins. This test method is based upon the 3.2.3 HDPE—high-density polyethylene.
presumption that the weight of the residue extract present in the 3.2.4 LLDPE—linear low-density polyethylene.
solvent is equal to the amount extracted from the film sample 3.2.5 FDA—Food and Drug Administration.
and could therefore be quantified by measuring the weight loss
4. Summary of Test Method
of the extracted film, eliminating the complex and time-
4.1 Film samples are extracted with hexane for2hat 49.5
consuming evaporation process described in 21 CFR 177.1520.
1.2 This standard does not purport to address all of the 6 0.5°C, dried, and weighed.
4.2 The loss in weight of the film is presumed to be equal to
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- the extractable content determined by solvent evaporation in
the FDA protocol.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents
5.1 FDA requirements for maximum extractables are speci-
2.1 ASTM Standards: fied for resin and uses. This test method provides a means to
determine the amount of hexane-soluble low molecular weight
D 883 Terminology Relating to Plastics
D 1239 Test Method for Resistance of Plastics Fibers to material present in polyolefins. It is applicable to resins
containing greater than 0.20 % extractables.
Extraction by Chemicals
D 1600 Terminology for Abbreviated Terms Relating to
2 6. Apparatus
Plastics
6.1 Water Bath, maintained at 49.5 6 0.5°C.
E 131 Terminology Relating to Molecular Spectroscopy
6.2 Resin Kettle, 1500-mL.
E 380 Practice for Use of the International System of Units
6.3 Kettle Head, 3-neck, with one 45/50 and two 24/40
(SI) (the Modernized Metric System)
female joints, and appropriate stoppers.
E 691 Practice for Conducting an Interlaboratory Study to
6.4 Clamp.
Determine the Precision of a Test Method
6.5 Allihn Condenser, Size C, with 45/50 male joint.
2.2 Federal Document:
6.6 Plastic Sleeves, tetrafluoroethylene (TFE), to fit Allihn
21 CFR 177.1520
condenser 45/50 male joint.
6.7 Vacuum Oven, capable of maintaining 80 6 5°C and a
minimum of 25-in. Hg pressure.
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved June 15, 1995. Published August 1995. Originally Ace Glass, Inc., Cat. No. 6476, Code 15, or its equivalent, has been found
published as D 5227 – 92. Last previous edition D 5227 – 92. satisfactory.
This edition includes revisions to Section 10, Calculation. Ace Glass, Inc., Cat. No. 6486, Code 50, or its equivalent, has been found
Annual Book of ASTM Standards, Vol 08.01. satisfactory.
3 8
Annual Book of ASTM Standards, Vol 14.01. Ace Glass, Inc., Cat. No. 6496, Code 10, or its equivalent, has been found
Annual Book of ASTM Standards, Vol 14.02. satisfactory.
5 9
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 Ace Glass, Inc., Cat. No. 6740, Code 06, or its equivalent, has been found
Robbins Ave., Philadelphia, PA 19111-5094. Attn: NPODS. satisfactory.
D 5227
mil or less in thickness) into about 1-in. squares using clean
sharp scissors.
NOTE 3—Care must be exercised when cutting the samples to avoid
ragged edges on the specimen. Small shards of film or contamination
present at initial weighing can easily be lost during the test, adversely
affecting the test results.
9.5 Weigh 2.5 6 0.05 g of film squares and record the initial
film weight to the nearest 0.1 mg. Also record the number of
film pieces.
NOTE 4—Forty or more squares will be obtained depending on the film
thickness. Some laboratories have found that a basket assembly, as shown
in Appendix X1, eliminates the need to count the film pieces before and
after the solvent extraction step.
9.6 Add the film sample to the hexane making sure all
squares become immersed in the solvent. (Use tweezers.)
Replace the kettle head with condenser column. Extract for 2 h.
9.7 After the extraction period:
FIG. 1 Resin Kettle Setup
9.7.1 Filter the contents of the resin kettle through the fritted
porcelain funnel.
6.8 Magnetic Stirring Bar, egg-shaped, TFE-coated, 1 ⁄2 by
9.7.2 Transfer the film squares, using tweezers, to a 200-mL
⁄8 in.
Berzelius beaker and recount the film pieces to verify that none
6.9 Submersible Magnetic Stirring Motor, with power sup-
were lost during transfer.
ply.
9.7.3 Cover the beaker with a watchglass and place it in a
6.10 Analytical Balance, capable of weighing to 0.1 mg.
vacuum oven at 80 6 5°C for 2 h.
9.7.4 After 2 h, remove the covered beaker from the vacuum
7. Reagents and Materials
oven and place it in a desiccator to cool to room temperature
7.1 n-Hexane, aromatic free (<1 mg/L), minimum 85 %
(about 1 h).
n-Hexane-reagent grade or equivalent. The solvent must
...
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