ASTM F2026-2007e1 Standard Specification for Polyetheretherketone (PEEK) Polymers for Surgical Implant Applications《外科植入物用聚醚醚酮(PEEK)聚合物的标准规范》.pdf

1、Designation: F 2026 07e1Standard Specification forPolyetheretherketone (PEEK) Polymers for Surgical ImplantApplications1This standard is issued under the fixed designation F 2026; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the

2、 year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEThe alignment of Table 2 was editorially corrected in February 2007.1. Scope1.1 This specification covers polyethe

3、retherketone (PEEK)polymer in virgin forms as supplied by a vendor (pellets,powder, and so forth). It provides requirements and associatedtest methods for these thermoplastics when they are to be usedin the manufacture of intracorporeal devices such as surgicalimplants or components of surgical or d

4、ental devices.1.2 As with any material, some characteristics may bealtered by the processing techniques (molding, extrusion,machining, assembly, sterilization, and so forth) required forthe production of a specific part or device. Therefore, proper-ties of fabricated forms of these polymers should b

5、e evaluatedusing test methods which are appropriate to ensure safety andefficacy as agreed upon by the vendor, purchaser, and regulat-ing bodies.1.3 The properties included in this specification are thoseapplicable for PEEK polymers only. Indicated properties arefor injection molded forms. Fabricate

6、d forms, material orforms containing colorants, fillers, processing aids, or otheradditives, as well as polymer blends which contain PEEK, orreclaimed materials, are not covered by this specification.1.4 This specification is designed to recommend physical,chemical, and biological test methods to es

7、tablish a reasonablelevel of confidence concerning the performance of virginPEEK polymers for use in medical implant devices. Theproperties listed should be considered in selecting material(s)in accordance with the specific end-use requirements.1.5 When evaluating material in accordance with this sp

8、eci-fication, hazardous materials, operations, and equipment maybe involved. This standard does not purport to address all ofthe safety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine

9、the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 149 Test Method for Dielectric Breakdown Voltage andDielectric Strength of Solid Electrical Insulating Materialsat Commercial Power FrequenciesD 256 Test Methods for Determining the Izod PendulumIm

10、pact Resistance of PlasticsD 570 Test Method for Water Absorption of PlasticsD 638 Test Method for Tensile Properties of PlasticsD 648 Test Method for Deflection Temperature of PlasticsUnder Flexural Load in the Edgewise PositionD 695 Test Method for Compressive Properties of RigidPlasticsD 696 Test

11、 Method for Coefficient of Linear Thermal Ex-pansion of Plastics Between 30C and 30C with aVitreous Silica DilatometerD 790 Test Methods for Flexural Properties of Unreinforcedand Reinforced Plastics and Electrical Insulating MaterialsD 792 Test Methods for Density and Specific Gravity (Rela-tive De

12、nsity) of Plastics by DisplacementD 955 Test Method of Measuring Shrinkage from MoldDimensions of ThermoplasticsD 1238 Test Method for Melt Flow Rates of Thermoplasticsby Extrusion PlastometerD 1505 Test Method for Density of Plastics by the Density-Gradient TechniqueD 1898 Practice for Sampling of

13、Plastics3D 3417 Test Method for Enthalpies of Fusion and Crystal-lization of Polymers by Differential Scanning Calorimetry(DSC)3D 3418 Test Method for Transition Temperatures of Poly-mers By Differential Scanning CalorimetryD 4000 Classification System for Specifying Plastic Mate-rials1This specific

14、ation is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is the direct responsibility ofSubcommittee F04.11 on Polymeric Materials.Current edition approved Feb. 1, 2007. Published February 2007. Originallyapproved in 2000. Last previous edition approved

15、in 2002 as F 2026 02.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International

16、, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.F 748 Practice for Selecting Generic Biological Test Meth-ods for Materials and DevicesF 1579 Specification for Polyaryletherketone (PAEK) Poly-mers for Surgical Implant Applications2.2 ISO Standards:ISO 1628/1 Pla

17、sticsGuidelines for the Standardization ofMethods for Determination of Viscosity Number andLimiting Viscosity Number of Polymers in DiluteSolutionPart 1: General Conditions4ISO 1133 PlasticsDetermination of the Melt Mass-FlowRate (MFR) and the Melt Volume-Flow Rate (MVR) ofThermoplastics4ISO 10993 B

18、iological Evaluation of Medical Devices, Parts1-1242.3 Other Documents:United States Pharmacopeia, Vol. XXI, or latest edition5Food and Drug Administration, Regulation 21 CFR177.241563. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 fabricated forms, nthose items into which the

19、virginforms 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, nthe PEEK material

20、s, parts,or devices fabricated from virgin forms in such a way as tocontain intentional or unintentional adjuvant substances.3.1.3 virgin forms, nthat form of the PEEK polymer asobtained by the synthesizer. It typically will be in the form ofpellets or powder. It is the material from which fibers, t

21、ubes,rods, slabs, sheets, films, or specific parts and devices arefabricated.4. Classification4.1 The PEEK polymer in the scope of this specification isa pure semicrystalline homopolymer consisting of phenylenerings connected by ether (E) and carbonyl (or ketone, K)groups along the polymer chain (se

22、e 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 D 4000.5. Properties5.1 The infrared spectrum7of these materials is character-istic of their molecular repeating units. A repres

23、entative spec-trum is listed in Appendix X3. The PEEK polymer shall yieldan infrared spectrum, which exhibits major bands only at thewavelengths listed for a standard reference spectrum of thatmaterial.5.1.1 The infrared spectrum, as used in this specification, isto identify the specific type of pol

24、y aryl ether ketone (PAEK)present (see Specification F 1579) and does not necessarilyindicate an acceptable degree of material purity.5.1.2 The presence of additional bands in the samplesinfrared spectrum compared to that of the reference materialmay indicate a different PAEK or impurities, or both.

25、5.2 The physical and chemical property requirements for thevirgin polymer are listed in Table 1. If additional characteristicsare necessary because of a specific application, the proceduresreferenced in 5.6 are recommended, or as agreed upon betweenthe vendor and the purchaser.5.3 The viscosity requ

26、irements will vary depending uponthe grade and test method. The method and requirements shallbe agreed upon between the vendor and the purchaser.5.4 The chemical, physical, and mechanical properties offabricated forms are related to the processes utilized inproducing the fabricated form (for example

27、, molding, machin-ing, sterilization, and so forth). Additionally, the propertiesnecessary for a particular device to perform properly will varyfrom one device type to another. Table 2 lists some typicalproperties of non-sterilized fabricated forms.5.5 Test specimens shall be fabricated (machined, i

28、njectionmolded, and so forth) from the virgin polymer, or finished part,in such a way as to effectively represent the material charac-teristics of the non-sterilized finished part.5.6 Tests and test procedures shall be such as to ensure ahigh level of control and characterization of the virgin polym

29、eras received from the supplier. The following are some testmethods that may be appropriate: Test Method D 149, TestMethod D 256, Test Method D 570, Test Method D 638, TestMethod D 648, Test Method D 695, Test method D 696, TestMethods D 790, Test Methods D 792, Test Method D 955, TestMethod D 1238,

30、 Test Method D 1505, Test Method D 3417,Test Method D 3418, and Classification System D 4000.6. Sampling6.1 The material should be sampled in accordance with thestandard sampling procedures, such as those described inPractice D 1898, or other sampling techniques unless otherwiseagreed upon between t

31、he consumer and the supplier.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.5Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,MD 20852-1790, http:/www.usp.org.6Available from Food and Drug Adminis

32、tration (FDA), 5600 Fishers Ln.,Rockville, MD 20857, http:/www.fda.gov.7Silverstein, R. M., Bassler, G. C., and Morrill, T. C., “Spectroscopic Identifi-cation of Organic Compounds,” 5th ed., John Wiley polyetheretherketoneAPPENDIXES(Nonmandatory Information)X1. RATIONALEX1.1 The PEEK polymers may be

33、 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, and irradiation. Repeatedsterilization may weaken parts fabricated of an

34、y 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 function, and method of steriliza-tion of the device. Therefore, it is imperat

35、ive 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 crys-tallinity is an important characteristic of these materials.Performance characteristics are related

36、to the percent crystal-linity. Certain additives and processes (for example, excessivecross linking) can limit these materials ability to crystallize.Therefore, this feature of the polymer and its fabricated formshould be evaluated, using appropriate test methods, to ensureefficacy.X1.3 A formulated

37、 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 compounds, parts, and devices shall be established inaccordance with Practice

38、F 748 or the ISO 10993 series.X2. CHEMICAL STRUCTURE OF PEEKTABLE 2 Typical Properties of Fabricated FormsParameter ISO Methods and Requirements ASTM Methods and RequirementsDensity, kg/m3ISO 1183 1280 - 1320 ASTM D 1505 1280 - 1320Tensile Strengthat Yield (Zero Slope), min, MPaat Break, min, MPAISO

39、 527, Type 1B,50 mm/min 9070ASTM D 638,Type IV, 5.08 cm/min 9070Percent elongation at break,min, %ISO 527, Type 1B,50 mm/min5 ASTM D 638,Type IV, 5.08 cm/min5Flexural Strength, min, MPa ISO 178 110 ASTM D 790 110Flexural Modulus, min, GPa ISO 178 3 ASTM D 790 3Impact Strength, Notched Izod,minISO 18

40、0 4(kJ/m2)ASTM D 256,0.254 cm depth, 0.025 cm radius50(J/m)F202607e13X3. 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. 53.Autian, J., “The New

41、 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 Science Chemistry,VolA4

42、, 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. 43.ASTM International

43、 takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their ow

44、n responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be ad

45、dressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, a

46、t the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).F202607e14