ASTM F2102-13
(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 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 PeakFIG. 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).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.
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.
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Designation:F2102 −13
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 E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This guide covers a method for the measurement of the
relative extent of oxidation present in HDPE homopolymers
3. Terminology
and ultra-high-molecular-weight polyethylene (UHMWPE) in-
3.1 Definitions:
tendedforuseinmedicalimplants.Thematerialisanalyzedby
3.1.1 bulk oxidation index (BOI)—asample’sbulkoxidation
infrared spectroscopy. The intensity (area) of the carbonyl
index (BOI) is the average of the oxidation indices collected
-1
absorptions (>C=O) centered near 1720 cm is related to the
over a 500-µm section at the center of the sample.
amount of chemically bound oxygen present in the material.
3.1.1.1 Discussion—Typically, this is a plateau region with
Other forms of chemically bound oxygen (C-O-C, C-O-O-C,
the smallest oxidation indices.
C-O-H, and so forth) are not captured by this guide.
3.1.1.2 Discussion—Forsampleslessthanabout8to10mm
1.2 Although this guide may give the investigator a means
thick, this central region may display the sample’s highest
to compare the relative extent of carbonyl oxidation present in
oxidation indices, depending on its state of oxidation.
variousUHMWPEsamples,itisrecognizedthatotherformsof
3.1.2 depth locator (DL)—a measurement of the distance
chemically bound oxygen may be important contributors to
fromthearticularsurface,orsurfaceofinterest,thataspectrum
these materials’ characteristics.
was collected and a corresponding OI calculated.
1.3 The applicability of the infrared method has been
3.1.3 oxidation index (OI)—an oxidation index (OI) is
demonstrated by many literature reports. This particular
defined as the ratio of the area of the carbonyl absorption
method, using the intensity (area) of the C-H absorption
-1
peak(s) centered near 1720 cm to the area of the absorption
-1
centered near 1370 cm to normalize for the sample’s -1
peak(s) centered near 1370 cm , as shown in Fig. 1. Note that
thickness,hasbeenvalidatedbyanInterlaboratoryStudy(ILS)
the peak areas are computed after subtracting out the appro-
conducted according to Practice E691.
priate baseline, as further discussed in Section 6.
1.4 The following precautionary caveat pertains only to the
3.1.4 oxidation index profile—an oxidation index profile is
test method portion, Section 5, of this specification: This
the graphical representation of variation of the sample’s
standard may involve hazardous materials, operations, and
oxidation index with distance from its articular surface or the
equipment. This standard does not purport to address all of the
surface of interest.This is a plot of an OI versus DL.Typically,
safety concerns, if any, associated with its use. It is the
the graph will show the profile through the entire thickness of
responsibility of the user of this standard to establish appro-
the sample.
priate safety and health practices and determine the applica-
3.1.5 surface oxidation index (SOI)—a sample’s surface
bility of regulatory requirements prior to use.
oxidation index (SOI) is the average of the oxidation indices
2. Referenced Documents fromthesample’sarticularsurface,orthesurfaceofinterest,to
2 a depth of 3-mm subsurface.
2.1 ASTM Standards:
4. Apparatus
1
This guide is under the jurisdiction of ASTM Committee F04 on Medical and
4.1 Infrared Spectrometer:
Surgical Materials and Devices and is the direct responsibility of Subcommittee
4.1.1 A calibrated infrared spectrometer capable of record-
F04.15 on Material Test Methods.
ing a transmission absorption spectrum over the range of about
Current edition approved Nov. 1, 2013. Published December 2013. Originally
-1
ε1
1200 to about 2000 cm using about 200-µsm-thick films at a
approved in 2001. Last previous edition approved in 2006 as F2102 – 06 . DOI:
-1
10.1520/F2102-13.
resolution of 4 cm and an aperture of about 200 by 200 µm.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1.1.1 Othermodesofcollection(thatis,percentreflection,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
attenuated total reflection (ATR), and so forth) and aperture
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. and increment sizes may be used to generate the sample’s
Copyright © ASTM International, 100 Barr
...
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: F2102 − 06 F2102 − 13
Standard Guide for
Evaluating the Extent of Oxidation in Ultra-High-Molecular-
Weight Polyethylene Fabricated Forms Intended for Surgical
1
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
ε NOTE—Paragraphs 7.1.4.2 and 8.1 were editorially corrected in July 2006.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
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 Devicesand is the direct responsibility of Subcommittee F04.15
on Material Test Methods.
Current edition approved May 1, 2006Nov. 1, 2013. Published May 2006December 2013. Originally approved in 2001. Last previous edition approved in 20012006 as
ε1
F2102 – 01F2102 – 06 . DOI: 10.1520/F2102-06E01.10.1520/F2102-13.
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
---------------------- Page: 1 ----------------------
F2102 − 13
FIG. 2 FTIR Spectra Showing the Carbonyl Absorption Bands
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 spectrum was
collected and a corresponding OI calculated.
3.1.3 oxidation index (OI)—an oxidation index (OI) is defined as the ratio of the area of the carbonyl absorption peak(s) centered
-1 -1
near 1720 cm to the area of the absorption peak(s) centered near 1370 cm , as shown in Fig. 1. Note that the peak areas are
computed after subtracting out the appropriate baseline, as further discussed in Section 6.
3.1.4 oxidation index profile—an oxidation index profile is the graphical representation of variation of the sample’s oxidation
index with distance from its articular surface or the surface of interest. This is a plot of an OI versus DL. Typically, the graph will
show the profile throu
...
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