ASTM D5227-13

Standard Test Method for Measurement of Hexane Extractable Content of Polyolefins

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.
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 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.

General Information

• Status: Historical
• Publication Date: 31-May-2013
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5227 −13
Standard Test Method for
1
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* Determine the Precision of a Test Method
3
2.2 Federal Document:
1.1 This test method describes an extraction/gravimetric
21 CFR 177.1520
procedure for determination of the amount of hexane soluble
low molecular weight material present in polyethylene,
3. Terminology
polypropylene, ethylene-propylene copolymers, and ethylene-
3.1 The definitions given inTerminology D883, D1600, and
vinyl acetate copolymers. This test method is a modification of
E131 are applicable to this test method.
the Food and Drug Administration (FDA) procedure for
determining hexane extractables of polyolefins. This test
3.2 Abbreviations:
method is based upon the presumption that the weight of the
3.2.1 EVA—ethylene-vinyl acetate copolymer.
residue extract present in the solvent is equal to the amount
3.2.2 LDPE—low-density polyethylene.
extracted from the film sample and could therefore be quanti-
3.2.3 HDPE—high-density polyethylene.
fied by measuring the weight loss of the extracted film,
eliminating the complex and time-consuming evaporation 3.2.4 LLDPE—linear low-density polyethylene.
process described in 21 CFR 177.1520.
3.2.5 FDA—Food and Drug Administration.
1.2 This standard does not purport to address all of the
3.2.6 PP—polypropylene.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 Film samples are extracted with hexane for 2 h at 49.5
bility of regulatory limitations prior to use.
6 0.5°C, dried, and weighed.
1.3 The values stated in SI units are to be regarded as the
4.2 The loss in weight of the film is presumed to be equal to
standard. Units used in 21 CFR 177.1520 are also used in this
the extractable content determined by solvent evaporation in
test method. Units are in conformance with Federal Code 21
the FDA protocol.
CFR 177.1520, from which this test method is derived.
NOTE 1—There is no known ISO equivalent to this standard.
5. Significance and Use
5.1 FDArequirements for maximum extractables are speci-
2. Referenced Documents
fied for resin and uses. This test method provides a means to
2
2.1 ASTM Standards:
determine the amount of hexane-soluble low molecular weight
D883 Terminology Relating to Plastics
material present in polyolefins. It is applicable to resins
D1239 Test Method for Resistance of Plastic Films to
containing greater than 0.20 % extractables.
Extraction by Chemicals
D1600 Terminology forAbbreviatedTerms Relating to Plas-
6. Apparatus
tics
6.1 Water Bath, maintained at 49.5 6 0.5°C.
E131 Terminology Relating to Molecular Spectroscopy
6.2 Resin Kettle, 1500-mL.
E691 Practice for Conducting an Interlaboratory Study to
6.3 Kettle Head, 3-neck, with one 45/50 and two 24/40
female joints, and appropriate stoppers.
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
6.4 Clamp.
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
CurrenteditionapprovedJune1,2013.PublishedJuly2013.Originallyapproved
ε1 6.5 Allihn Condenser, Size C, with 45/50 male joint.
in 1992. Last previous edition approved in 2008 as D5227 - 01(2008) . DOI:
10.1520/D5227-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Standards volume information, refer to the standard’s Document Summary page on Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
the ASTM website. www.dodssp.daps.mil.
*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
1

---------------------- Page: 1 ----------------------
D5227−13
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 Weigh2.5 60.05goffilmsquaresandrecordtheinitial
film weight to the nearest 0
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D5227 − 01 (Reapproved 2008) D5227 − 13
Standard Test Method for
1
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
ε NOTE—Reapproved with editorial changes in November 2008.
1. Scope 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 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 ISO to this test method.standard.
2. Referenced Documents
2
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
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3
2.2 Federal Document:
21 CFR 177.1520
3. Terminology
3.1 The definitions given in Terminology D883, D1600, and E131 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.
1
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 Nov. 1, 2008June 1, 2013. Published March 2009July 2013. Originally approved in 1992. Last previous edition approved in 20012008 as
ε1
D5227 - 01.D5227 - 01(2008) . DOI: 10.1520/D5227-01R08E01.10.1520/D5227-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://www.dodssp.daps.mil.
*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
1

---------------------- Page: 1 ----------------------
D5227 − 13
FIG. 1 Resin Kettle Setup
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
...