1、Designation: F2026 12Standard Specification forPolyetheretherketone (PEEK) Polymers for Surgical ImplantApplications1This standard is issued under the fixed designation F2026; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification covers polyetheretherketone (PEEK)polymer in virgin forms as supplied by a vendor (pellets,pow
3、der, fabricated forms, and so forth). It provides require-ments and associated test methods for these thermoplasticswhen they are to be used in the manufacture of intracorporealdevices such as surgical implants or components of surgical ordental devices.1.2 The properties included in this specificat
4、ion are thoseapplicable for PEEK polymers only. Indicated properties arefor fabricated forms. Materials or forms containing colorants,fillers, processing aids, or other additives, as well as polymerblends which contain PEEK, or reclaimed materials, are notcovered by this specification.1.3 This speci
5、fication is designed to recommend physical,chemical, and biological test methods to establish a reasonablelevel of confidence concerning the performance of virginPEEK polymers for use in medical implant devices.1.4 The values stated in SI units are to be regarded asstandard. No other units of measur
6、ement are included in thisstandard.1.5 When evaluating material in accordance with thisspecification, hazardous materials, operations, and equipmentmay be involved. This standard does not purport to address allof the safety concerns, if any, associated with its use. It is theresponsibility of the us
7、er of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D256 Test Methods for Determining the Izod PendulumImpact Resistance of PlasticsD638 Test Method for Tensile Pr
8、operties of PlasticsD648 Test Method for Deflection Temperature of PlasticsUnder Flexural Load in the Edgewise PositionD695 Test Method for Compressive Properties of RigidPlasticsD790 Test Methods for Flexural Properties of Unreinforcedand Reinforced Plastics and Electrical Insulating Materi-alsD150
9、5 Test Method for Density of Plastics by the Density-Gradient TechniqueD1898 Practice for Sampling of Plastics (Withdrawn 1998)3D3418 Test Method for Transition Temperatures and En-thalpies of Fusion and Crystallization of Polymers byDifferential Scanning CalorimetryD4000 Classification System for S
10、pecifying Plastic Materi-alsF748 Practice for Selecting Generic Biological Test Methodsfor Materials and Devices2.2 ISO Standards:4ISO 178 PlasticsDetermination of Flexural PropertiesISO 180 PlasticsDetermination of Izod Impact StrengthISO 527 PlasticsDetermination of Tensile PropertiesPart 1: Gener
11、al PrinciplesISO 1183 PlasticsMethods for Determining the Density ofNon-cellular PlasticsPart 2: Density Gradient ColumnMethodISO 10993 Biological Evaluation of Medical Devices, Parts1-12ISO 13485 Medical DevicesQuality ManagementSystemsRequirements for Regulatory Purposes2.3 Other Documents:United
12、States Pharmacopeia, Vol. XXI, or latest edition53. Terminology3.1 Definitions of Terms Specific to This Standard:1This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is the direct responsibility ofSubcommittee F04.11 on Polymeric Mater
13、ials.Current edition approved Oct. 1, 2012. Published October 2012. Originallyapproved in 2000. Last previous edition approved in 2010 as F2026 10. DOI:10.1520/F2026-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annua
14、l Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036,
15、http:/www.ansi.org.5Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,MD 20852-1790, http:/www.usp.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1 fabricated forms, nthose items into which the virginfo
16、rms may be converted. These include shapes and formsproduced by means of machining, extruding, and compressionmolding virgin forms into a subsequent entity (for example,fibers, tubes, rods, slabs, sheets, film, or complex shaped partsand devices).3.1.2 formulated compound, nmaterials, parts, or devi
17、cesfabricated from virgin forms in such a way as to containintentional or unintentional adjuvant substances.3.1.3 virgin forms, nthe initially delivered form of thepolymer as synthesized from its monomers prior to anyprocessing or fabrication into a medical device. The providedresin is typically in
18、the form of pellets, granules, or powder andis the material from which fibers, tubes, rods, slabs, sheets,films, or specific parts and devices are fabricated.4. Classification4.1 The PEEK polymer in the scope of this specification isa pure semicrystalline homopolymer consisting of phenylenerings con
19、nected by ether (E) and carbonyl (or ketone, K)groups along the polymer chain (see Appendix X1). Itspolymeric structure is defined by the repeating unit EEK.4.2 Types of PEEK plastics, molding, and extrusion gradesare described in Classification System D4000.5. Properties5.1 The properties listed be
20、low shall be considered inselecting material(s) in accordance with the specific end-userequirements.5.2 The infrared spectrum6of these materials is character-istic of their molecular repeating units. A representative spec-trum is listed in Appendix X3. The PEEK polymer shall yieldan infrared spectru
21、m, which exhibits major bands only at thewavelengths listed for a standard reference spectrum of thatmaterial.5.2.1 The infrared spectrum, as used in this specification, isto identify the specific type of poly aryl ether ketone (PAEK)present and does not necessarily indicate an acceptable degreeof m
22、aterial purity.5.2.2 The presence of additional bands in the samplesinfrared spectrum compared to that of the reference materialmay indicate a different PAEK or impurities, or both.5.3 The physical and chemical property requirements for thevirgin polymer are listed in Table 1. If additional characte
23、risticsare necessary because of a specific application, the proceduresreferenced in Section 2 are recommended, or as agreed uponbetween the vendor and the purchaser.5.4 The viscosity requirements will vary depending uponthe grade and test method. The method and requirements shallbe agreed upon betwe
24、en the vendor and the purchaser.5.5 The chemical, physical, and mechanical properties offabricated forms are related to the processes utilized inproducing the fabricated form (for example, molding,machining, sterilization, and so forth). Additionally, the prop-erties necessary for a particular devic
25、e to perform properly willvary from one device type to another. Table 2 lists some typicalproperties of non-sterilized fabricated forms.5.6 Test specimens shall be fabricated (machined, injectionmolded, and so forth) from the virgin polymer, or finished part,in such a way as to effectively represent
26、 the material charac-teristics of the non-sterilized finished part.5.6.1 As with any material, some characteristics may bealtered by the processing techniques (for example, molding,extrusion, machining, assembly, and sterilization) required forthe production of a specific part or device. Therefore,
27、proper-ties of fabricated forms of these polymers should be evaluatedusing test methods which are appropriate to ensure safety andefficacy as agreed upon by the vendor, purchaser, and regulat-ing bodies.5.7 Tests and test procedures shall be such as to ensure ahigh level of control and characterizat
28、ion of the virgin polymeras received from the supplier. The test methods referenced inSection 2 may be appropriate (Test Methods D648 and D695).6Silverstein, R. M., Bassler, G. C., and Morrill, T. C., Spectroscopic Identifica-tion of Organic Compounds, 5th ed., John Wiley polyetheretherketoneAPPENDI
29、XES(Nonmandatory Information)X1. RATIONALEX1.1 The PEEK polymers may be processed by mosttechniques available for thermoplastic polymers. Medical de-vices and components of medical devices made of PEEKpolymers may be sterilized. Sterilization methods successfullyused include steam, ethylene oxide, a
30、nd irradiation. Repeatedsterilization may weaken parts fabricated of any plastic mate-rial. The number of times a given part may be sterilized safelywithout fear of subsequent failure depends on a number offactors including the molecular weight of the polymer anddesign, fabrication, intended functio
31、n, and method of steriliza-tion of the device. Therefore, it is imperative that the manu-facturer test the device in order to determine the maximumnumber of sterilization cycles to which it can be safelysubjected.X1.2 The potential to develop a significant level of crystal-linity is an important cha
32、racteristic of these materials. Perfor-mance characteristics are related to the percent crystallinity.Certain additives and processes (for example, excessive crosslinking) can limit these materials ability to crystallize.Therefore, this feature of the polymer and its fabricated formshould be evaluat
33、ed, using appropriate test methods, to ensureefficacy.X1.3 A formulated compound or fabricated part or devicemay contain optional adjuvant substances required for thefabrication or intended use of the end product. The biocom-patibility of these adjuvant substances, and subsequent formu-lated compoun
34、ds, parts, and devices shall be established inaccordance with Practice F748 or the ISO 10993 series.7Hay, J. N., and Kemmish, D. J., “Environmental Stress Crack Resistance andAbsorption of Low-Molecular-Weight Penetrants by Poly(Aryl Ether EtherKetone),” Polymer, Vol 29, April 1988, pp. 613618.8Sriv
35、astava, A. P., Depke, N., and Wolf, C. J., “Environmental Stress Deforma-tion of Poly(ether ether ketone),” J. Applied Polymer Science, Vol 66, 1997, pp.725731.9Kurtz, S.M. and Devine, J.N., “PEEK Biomaterials in Trauma, Orthopedic, andSpinal Implants,” Biomaterials, Vol 28, No. 32, 2007, pp. 4845-4
36、869.TABLE 2 Required Properties of Fabricated FormsParameter ISO Methods and Requirements ASTM Methods and RequirementsDensity, kg/m3ISO 1183 1280 - 1320 ASTM D1505 1280 - 1320Tensile Strength ISO 527, Type 1B, ASTM D638,50 mm/min Type IV, 5.08 cm/minat Yield (Zero Slope), MPaat break, MPa90709070Pe
37、rcent elongation at break,A%ISO 527, Type 1B,50 mm/min5 ASTM D638,Type IV, 5.08 cm/min5Flexural Strength, MPa ISO 178 110 ASTM D790 110Flexural Modulus, GPa ISO 178 3 ASTM D790 3Impact Strength, Notched Izod ISO 180 4 (kJ/m2) ASTM D256,0.254 cm depth, 0.025 cm radius50 (J/m)AUse an extensometer for
38、measuring strain and calculating percent elongation.F2026 123X2. CHEMICAL STRUCTURE OF PEEKX3. REPRESENTATIVE INFRARED SPECTRA OF PEEKRELATED MATERIALAutian, J., “Toxicological Evaluation of Biomaterials: Primary AcuteToxicity Screening Program,” Journal of Artificial Organs, Vol 1, No.1, 1977, p. 5
39、3.Autian, J., “The New Field of Plastic Toxicological Methods and Results,”CRC Critics Review in Toxicology, 1973, p. 18.Homsy, C. A., Ansevin, K. D., OBrannon, W., Thompson, S. H., Hodge,R., and Estrella, M. E., “Rapid In Vitro Screening of Polymers forBiocompatibility,” Journal of Macromolecular S
40、cience Chemistry,VolA4, No. 3, May 1970, pp. 615-634.Rice, R. M., Hegyeli, A. F., Gourlay, S. J., Wade, C. W. R., Dillon, J. G.,Jaffe, H., and Kulkarni, R. K., “Biocompatibility Testing for Polymers:In Vitro Studies With In Vivo Correlation,” Journal of BiomedicalMaterials Research, Vol 12, 1978, p.
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