ASTM F2102-17
(Guide)Standard Guide for Evaluating the Extent of Oxidation in Polyethylene Fabricated Forms Intended for Surgical Implants
Standard Guide for Evaluating the Extent of Oxidation in Polyethylene Fabricated Forms Intended for Surgical Implants
ABSTRACT
This guide covers method for evaluating the relative extent of oxidation in ultra-high-molecular-weight polyethylene fabricated forms intended for surgical implants. Equipments for this method shall include an infrared spectrometer, specimen holder, and microtome. Specimen shall be tested with infrared spectrometer in accordance to the procedure of test specimen preparation, spectrometer setup, and test specimen configuration. Oxidation peak area, normalization peak area, oxidation index, oxidation index depth locator, oxidation index profile, surface oxidation index, bulk oxidation index, and maximum oxidation index shall be calculated from the spectra. Report shall include material information, sample information, spectrometer information, and data analysis information.
SCOPE
1.1 This guide covers a method for the measurement of the relative extent of oxidation present in HDPE homopolymers and ultra-high-molecular-weight polyethylene (UHMWPE) intended for use in medical implants. The material is analyzed by infrared spectroscopy. The intensity (area) of the carbonyl absorptions (>C=O) centered near 1720 cm-1 is related to the amount of chemically bound oxygen present in the material. Other forms of chemically bound oxygen (C-O-C, C-O-O-C, C-O-H, and so forth) are not captured by this guide.
1.2 Although this guide may give the investigator a means to compare the relative extent of carbonyl oxidation present in various UHMWPE samples, it is recognized that other forms of chemically bound oxygen may be important contributors to these materials' characteristics.
1.3 The applicability of the infrared method has been demonstrated by many literature reports. This particular method, using the intensity (area) of the C-H absorption centered near 1370 cm-1 to normalize for the sample’s thickness, has been validated by an Interlaboratory Study (ILS) conducted according to Practice E691.
FIG. 1 Typical FTIR Spectra of Oxidized UHMWPE, Showing the Definition of an Area-Based Oxidation Index Based on Normalization Using the 1370-cm-1 Peak
FIG. 2 FTIR Spectra Showing the Carbonyl Absorption Bands
Note 1: Note that both reagents effectively extracted the lipids (the lipid absorption peak is centered at approximately 1740 cm-1). The tibial insert was fabricated from highly crosslinked and remelted UHMWPE followed by terminal sterilization in EtO gas (Ref. 1).
1.4 The following precautionary caveat pertains only to the test method portion, Section 5, of this specification: This standard may involve hazardous materials, operations, and equipment. 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 requirements prior to use.
1.5 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.
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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.
Designation:F2102 −17
Standard Guide for
Evaluating the Extent of Oxidation in Polyethylene
1
Fabricated Forms Intended for Surgical Implants
This standard is issued under the fixed designation F2102; 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 2. Referenced Documents
2
1.1 This guide covers a method for the measurement of the
2.1 ASTM Standards:
relative extent of oxidation present in HDPE homopolymers
E691 Practice for Conducting an Interlaboratory Study to
and ultra-high-molecular-weight polyethylene (UHMWPE) in-
Determine the Precision of a Test Method
tendedforuseinmedicalimplants.Thematerialisanalyzedby
E2857 Guide for Validating Analytical Methods
infrared spectroscopy. The intensity (area) of the carbonyl
-1
absorptions (>C=O) centered near 1720 cm is related to the
3. Terminology
amount of chemically bound oxygen present in the material.
3.1 Definitions:
Other forms of chemically bound oxygen (C-O-C, C-O-O-C,
3.1.1 bulkoxidationindex(BOI)—asample’sbulkoxidation
C-O-H, and so forth) are not captured by this guide.
index (BOI) is the average of the oxidation indices collected
1.2 Although this guide may give the investigator a means
over a 500-µm section at the center of the sample.
to compare the relative extent of carbonyl oxidation present in
3.1.1.1 Discussion—Typically, this is a plateau region with
variousUHMWPEsamples,itisrecognizedthatotherformsof
the smallest oxidation indices.
chemically bound oxygen may be important contributors to
3.1.1.2 Discussion—Forsampleslessthanabout8to10mm
these materials’ characteristics.
thick, this central region may display the sample’s highest
oxidation indices, depending on its state of oxidation.
1.3 The applicability of the infrared method has been
demonstrated by many literature reports. This particular
3.1.2 depth locator (DL)—a measurement of the distance
method, using the intensity (area) of the C-H absorption
fromthearticularsurface,orsurfaceofinterest,thataspectrum
-1
centered near 1370 cm to normalize for the sample’s
was collected and a corresponding OI calculated.
thickness,hasbeenvalidatedbyanInterlaboratoryStudy(ILS)
3.1.3 oxidation index (OI)—an oxidation index (OI) is
conducted according to Practice E691.
defined as the ratio of the area of the carbonyl absorption
-1
1.4 The following precautionary caveat pertains only to the
peak(s) centered near 1720 cm to the area of the absorption
-1
test method portion, Section 5, of this specification: This
peak(s) centered near 1370 cm , as shown in Fig. 1. Note that
standard may involve hazardous materials, operations, and
the peak areas are computed after subtracting out the appro-
equipment. This standard does not purport to address all of the
priate baseline, as further discussed in Section 6.
safety concerns, if any, associated with its use. It is the
3.1.4 oxidation index profile—an oxidation index profile is
responsibility of the user of this standard to establish appro-
the graphical representation of variation of the sample’s
priate safety and health practices and determine the applica-
oxidation index with distance from its articular surface or the
bility of regulatory requirements prior to use.
surface of interest.This is a plot of an OI versus DL.Typically,
1.5 This international standard was developed in accor-
the graph will show the profile through the entire thickness of
dance with internationally recognized principles on standard-
the sample.
ization established in the Decision on Principles for the
3.1.5 surface oxidation index (SOI)—a sample’s surface
Development of International Standards, Guides and Recom-
oxidation index (SOI) is the average of the oxidation indices
mendations issued by the World Trade Organization Technical
fromthesample’sarticularsurface,orthesurfaceofinterest,to
Barriers to Trade (TBT) Committee.
a depth of 3-mm subsurface.
1
This guide is under the jurisdiction of ASTM Committee F04 on Medical and
Surgical Materials and Devices and is the direct responsibility of Subcommittee
2
F04.15 on Material Test Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2017. Published September 2017. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2001. Last previous edition approved in 2013 as F2102 – 13. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/F
...
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.
Designation: F2102 − 13 F2102 − 17
Standard Guide for
Evaluating the Extent of Oxidation in Polyethylene
1
Fabricated Forms Intended for Surgical Implants
This standard is issued under the fixed designation F2102; 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 guide covers a method for the measurement of the relative extent of oxidation present in HDPE homopolymers and
ultra-high-molecular-weight polyethylene (UHMWPE) intended for use in medical implants. The material is analyzed by infrared
-1
spectroscopy. The intensity (area) of the carbonyl absorptions (>C=O) centered near 1720 cm is related to the amount of
chemically bound oxygen present in the material. Other forms of chemically bound oxygen (C-O-C, C-O-O-C, C-O-H, and so
forth) are not captured by this guide.
1.2 Although this guide may give the investigator a means to compare the relative extent of carbonyl oxidation present in
various UHMWPE samples, it is recognized that other forms of chemically bound oxygen may be important contributors to these
materials’ characteristics.
1.3 The applicability of the infrared method has been demonstrated by many literature reports. This particular method, using
-1
the intensity (area) of the C-H absorption centered near 1370 cm to normalize for the sample’s thickness, has been validated by
an Interlaboratory Study (ILS) conducted according to Practice E691.
1.4 The following precautionary caveat pertains only to the test method portion, Section 5, of this specification: This standard
may involve hazardous materials, operations, and equipment. 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 requirements prior to use.
1.5 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
2.1 ASTM Standards:
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E2857 Guide for Validating Analytical Methods
3. Terminology
3.1 Definitions:
3.1.1 bulk oxidation index (BOI)—a sample’s bulk oxidation index (BOI) is the average of the oxidation indices collected over
a 500-μm section at the center of the sample.
1
This guide is under the jurisdiction of ASTM Committee F04 on Medical and Surgical Materials and Devices and is the direct responsibility of Subcommittee F04.15
on Material Test Methods.
Current edition approved Nov. 1, 2013Sept. 1, 2017. Published December 2013September 2017. Originally approved in 2001. Last previous edition approved in 20062013
ε1
as F2102 – 06F2102 – 13. . DOI: 10.1520/F2102-13.10.1520/F2102-17.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3.1.1.1 Discussion—
Typically, this is a plateau region with the smallest oxidation indices.
3.1.1.2 Discussion—
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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F2102 − 17
FIG. 1 Typical FTIR Spectra of Oxidized UHMWPE, Showing the Definition of an Area-Based Oxidation Index Based on Normalization
-1
Using the 1370-cm Peak
FIG. 2 FTIR Spectra Showing the Carbonyl Absorption Bands
-1
NOTE 1—Note that both reagents effectively extracted the lipids (the lipid absorption peak is centered at approximately 1740 cm ). The tibial insert
was fabricated from highly crosslinked and remelted UHMWPE followed by terminal sterilization in EtO gas (Ref. 1).
For samples less than about 8 to 10 mm thick, this central region may display the sample’s highest oxidation indices, depending
on its state of oxidation.
3.1.2 depth locator (DL)—a measurement of the distance from the articular surface, or surface of interest, that a spectru
...
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