ASTM D5227-21

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Designation: D5227 − 13 D5227 − 21
Standard Test Method for
Measurement of Hexane Extractable Content of Polyolefins
This standard is issued under the fixed designation D5227; 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 (´) indicates an editorial change since the last revision or reapproval.
1. 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 safety, health, and healthenvironmental 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 also used in this test
method. Units are in conformance with Federal Code 21 CFR 177.1520, from which this test method is derived.
NOTE 1—There is no known ISO equivalent to this standard.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1239 Test Method for Resistance of Plastic Films to Extraction by Chemicals
D1600 Terminology for Abbreviated Terms Relating to Plastics
E131 Terminology Relating to Molecular Spectroscopy
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E2935 Practice for Evaluating Equivalence of Two Testing Processes
2.2 Federal Document:
21 CFR 177.1520 CFR 177.1520Olefin Polymers
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved June 1, 2013July 1, 2021. Published July 2013July 2021. Originally approved in 1992. Last previous edition approved in 20082013 as
ε1
D5227 - 01D5227 - 13.(2008) . DOI: 10.1520/D5227-13.10.1520/D5227-21.
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*A Summary of Changes section appears at the end of this standard
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D5227 − 21
3. Terminology
3.1 The definitions given in Terminology D883, D1600, E131and, E131and E456 are applicable to this test method.
3.2 Abbreviations:
3.2.1 EVA—ethylene-vinyl acetate copolymer.
3.2.2 LDPE—low-density polyethylene.
3.2.3 HDPE—high-density polyethylene.
3.2.4 LLDPE—linear low-density polyethylene.
3.2.5 FDA—Food and Drug Administration.
3.2.6 PP—polypropylene.
4. Summary of Test Method
4.1 Film samples are extracted with hexane for 2 h at 49.5 6 0.5°C, dried, and weighed.
4.2 The loss in weight of the film is presumed to be equal to the extractable content determined by solvent evaporation in the FDA
protocol.
5. Significance and Use
5.1 FDA requirements for maximum extractables are specified for resin and uses. This test method provides a means to determine
the amount of hexane-soluble low molecular weight material present in polyolefins. It is applicable to resins containing greater than
0.20 % extractables.
6. Apparatus
6.1 Water Bath, maintained at 49.5 6 0.5°C.
6.2 Resin Kettle, 1500-mL.
6.3 Kettle Head, 3-neck, with one 45/50 and two 24/40 female joints, and appropriate stoppers.
6.4 Clamp.
6.5 Allihn Condenser, Size C, with 45/50 male joint.
6.6 Plastic Sleeves, tetrafluoroethylene (TFE), to fit Allihn condenser 45/50 male joint.
6.7 Vacuum Oven, capable of maintaining 80 6 5°C and a minimum of 25-in. Hg pressure.
1 5
6.8 Magnetic Stirring Bar, egg-shaped, TFE-coated, 1 ⁄2 by ⁄8 in.
6.9 Submersible Magnetic Stirring Motor, with power supply.
6.10 Analytical Balance, capable of weighing to 0.1 mg.
D5227 − 21
FIG. 1 Resin Kettle Setup
7. Reagents and Materials
7.1 n-Hexane, aromatic free (<1 mg/L), minimum 85 % n-Hexane-reagent grade or equivalent. The solvent must be free of
aromatic compounds that would significantly increase the solubility of the resin. The solvent grade specified represents the
minimum required purity.
8. Materials
8.1 Blown Film, compression molded films, or cast films are suitable for testing.
8.2 Film, approximately 2.5 g, with a thickness not exceeding 4 mil is required for a single determination.
9. Procedure
9.1 Assemble the resin kettle setup with glass stopper, clamp, and magnetic stirring bar. (See Fig. 1.)
9.2 Add 1000 mL of n-Hexane to the kettle assembly.
9.3 Stopper the kettle and clamp the assembly into the water bath set at 49.5 6 0.5°C.
NOTE 2—Temperature is a critical factor in this analysis and must not vary more than 1°C. If the temperature exceeds these limits, the test must be
discontinued and restarted. The FDA protocol also states the temperature of the contents must be brought to 49.5 6 0.5°C within 20 to 25 min.
NOTE 3—The level of water in the bath must be kept at least 2 cm above the level of the solvent in the kettle to ensure the temperature equilibrium. Position
the kettle so that the center bottle of the kettle is sitting on a submersible stirrer. Start stirring and allow the hexane to heat for 1 h.
9.4 Using gloves and metal tweezers to avoid sample contamination, cut 2.7 g of the prepared film sample (4 mil or less in
thickness) into 1-in. squares using clean sharp scissors.
NOTE 4—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 t
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