ASTM D5227-01

Standard Test Method for Measurement of Hexane Extractable Content of Polyolefins

SIGNIFICANCE AND USE
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.
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.

General Information

• Status: Historical
• Publication Date: 09-Jun-2001
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Relations

• Replaces: ASTM D5227-95 - Standard Test Method for Measurement of Hexane Extractable Content of Polyolefins
• Effective Date: 10-Jun-2001
• Replaced By: ASTM D5227-01(2008)e1 - Standard Test Method for Measurement of Hexane Extractable Content of Polyolefins
• Effective Date: 01-Nov-2008
• Referred By: ASTM F561-19 - Standard Practice for Retrieval and Analysis of Medical Devices, and Associated Tissues and Fluids
• Effective Date: 10-Jun-2001
• Referred By: ASTM D5577-19 - Standard Guide for Techniques to Separate and Identify Contaminants in Recycled Plastics
• Effective Date: 10-Jun-2001

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: D 5227 – 01
Standard Test Method for
1
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.
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1. Scope* 2.2 Federal Document:
21 CFR 177.1520
1.1 This test method describes an extraction/gravimetric
procedure for determination of the amount of hexane soluble
3. Terminology
low molecular weight material present in polyethylene,
3.1 The definitions given in Terminology D 883, D 1600,
polypropylene, ethylene-propylene copolymers, and ethylene-
and E 131 are applicable to this test method.
vinyl acetate copolymers. This test method is a modification of
3.2 Abbreviations:Abbreviations:
the Food and Drug Administration (FDA) procedure for
3.2.1 EVA—ethylene-vinyl acetate copolymer.
determining hexane extractables of polyolefins. This test
3.2.2 LDPE—low-density polyethylene.
method is based upon the presumption that the weight of the
3.2.3 HDPE—high-density polyethylene.
residue extract present in the solvent is equal to the amount
3.2.4 LLDPE—linear low-density polyethylene.
extracted from the film sample and could therefore be quanti-
3.2.5 FDA—Food and Drug Administration.
fied by measuring the weight loss of the extracted film,
3.2.6 PP—polypropylene.
eliminating the complex and time-consuming evaporation
process described in 21 CFR 177.1520.
4. Summary of Test Method
1.2 This standard does not purport to address all of the
4.1 Film samples are extracted with hexane for 2 h at 49.5
safety concerns, if any, associated with its use. It is the
6 0.5°C, dried, and weighed.
responsibility of the user of this standard to establish appro-
4.2 The loss in weight of the film is presumed to be equal to
priate safety and health practices and determine the applica-
the extractable content determined by solvent evaporation in
bility of regulatory limitations prior to use.
the FDA protocol.
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
5. Significance and Use
test method. Units are in conformance with Federal Code 21
5.1 FDArequirements for maximum extractables are speci-
CFR 177.1520, from which this test method is derived.
fied for resin and uses. This test method provides a means to
NOTE 1—There is no similar or equivalent ISO standard.
determine the amount of hexane-soluble low molecular weight
material present in polyolefins. It is applicable to resins
2. Referenced Documents
containing greater than 0.20 % extractables.
2.1 ASTM Standards:
2
6. Apparatus
D 883 Terminology Relating to Plastics
D 1239 Test Method for Resistance of Plastics Fibers to
6.1 Water Bath, maintained at 49.5 6 0.5°C.
2
6
Extraction by Chemicals
6.2 Resin Kettle, 1500-mL.
D 1600 Terminology for Abbreviated Terms Relating to
6.3 Kettle Head, 3-neck, with one 45/50 and two 24/40
2
7
Plastics
female joints, and appropriate stoppers.
3
8
E 131 Terminology Relating to Molecular Spectroscopy
6.4 Clamp.
E 691 Practice for Conducting an Interlaboratory Study to
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Determine the Precision of a Test Method
1 5
This test method is under the jurisdiction ofASTM Committee D20 on Plastics AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. Robbins Ave., Philadelphia, PA 19111-5094. Attn: NPODS.
6
Current edition approved June 10, 2001. Published August 2001. Originally Ace Glass, Inc., Cat. No. 6476–15, or its equivalent, has been found
published as D 5227 – 92. Last previous edition D 5227 – 95. satisfactory.
7
This edition includes revisions to Section 10, Calculation. Ace Glass, Inc., Cat. No. 6486–40, or its equivalent, has been found
2
Annual Book of ASTM Standards, Vol 08.01. satisfactory.
3 8
Annual Book of ASTM Standards, Vol 03.06. Ace Glass, Inc., Cat. No. 6496–10, or its equivalent, has been found
4
Annual Book of ASTM Standards, Vol 14.02. satisfactory.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5227–01
be discontinued and restarted. The FDA protocol also states the tempera-
ture of the contents must be brought to 49.5 6 0.5°C within 20 to 25 min.
NOTE 3—Thelevelofwaterinthebathmustbekeptatleast2cmabove
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
submersib
...