ASTM F2820-2012 Standard Specification for Polyetherketoneketone (PEKK) 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: F2820 12Standard Specification forPolyetherketoneketone (PEKK) Polymers for SurgicalImplant Applications1This standard is issued under the fixed designation F2820; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye

2、ar 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 virgin polyetherketoneketone(PEKK) polymer resin as supplied by a vendor (for example,

3、 inpellets, powder, and fabricated forms). 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 As with any material, some characteri

4、stics may bealtered by the processing techniques (for example, molding,extrusion, machining, assembly, and sterilization) required forthe production of a specific part or device. Therefore, proper-ties of fabricated forms of these polymers should be evaluatedusing test methods which are appropriate

5、to ensure safety andefficacy as agreed upon by the vendor, purchaser, and regulat-ing bodies. With reduced crystallinity, certain polymers havebeen shown to be more susceptible to environmental stresscracking. Depending upon the implant application, the end usershould characterize the material for e

6、nvironmental stress crack-ing resistance.1.3 The properties included in this specification are thoseapplicable for PEKK polymers only. Indicated properties arefor fabricated forms. Fabricated forms and materials containingcolorants, fillers, processing aids, or other additives, as well aspolymer ble

7、nds which contain PEKK, or reclaimed materialsare not covered by this specification.1.4 This specification is designed to recommend physical,chemical, and biological test methods to establish a reasonablelevel of confidence concerning the performance of virginPEKK polymers for use in medical implant

8、 devices. Theproperties listed should be considered in selecting material(s)in accordance with the specific end-use requirements.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 When evaluating material in accordance with

9、 this speci-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 de

10、termine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D149 Test Method for Dielectric Breakdown Voltage andDielectric Strength of Solid Electrical Insulating Materialsat Commercial Power FrequenciesD256 Test Methods for Determining the Izod Pend

11、ulumImpact Resistance of PlasticsD570 Test Method for Water Absorption of PlasticsD638 Test Method for Tensile Properties of PlasticsD648 Test Method for Deflection Temperature of PlasticsUnder Flexural Load in the Edgewise PositionD695 Test Method for Compressive Properties of RigidPlasticsD696 Tes

12、t Method for Coefficient of Linear Thermal Ex-pansion of Plastics Between 30C and 30C with aVitreous Silica DilatometerD790 Test Methods for Flexural Properties of Unreinforcedand Reinforced Plastics and Electrical Insulating MaterialsD792 Test Methods for Density and Specific Gravity (Rela-tive Den

13、sity) of Plastics by DisplacementD955 Test Method of Measuring Shrinkage from MoldDimensions of ThermoplasticsD1238 Test Method for Melt Flow Rates of Thermoplasticsby Extrusion PlastometerD1505 Test Method for Density of Plastics by the Density-Gradient TechniqueD1898 Practice for Sampling of Plast

14、ics3D3417 Test Method for Enthalpies of Fusion and Crystal-lization of Polymers by Differential Scanning Calorimetry(DSC)31This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is the direct responsibility ofSubcommittee F04.11 on Polymer

15、ic Materials.Current edition approved April 15, 2012. Published May 2012. DOI: 10.1520/F282012.2For 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 Documen

16、t Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.D3418 Test Method for Transition Temperatures and En-tha

17、lpies of Fusion and Crystallization of Polymers byDifferential Scanning CalorimetryD4000 Classification System for Specifying Plastic Materi-alsF748 Practice for Selecting Generic Biological Test Meth-ods for Materials and Devices2.2 ISO Standards:4ISO 178 PlasticsDetermination of Flexural Propertie

18、sISO 180 PlasticsDetermination of Izod Impact StrengthISO 527 PlasticsDetermination of Tensile PropertiesISO 604 PlasticsDetermination of Compressive Proper-tiesISO 1183 PlasticsMethods for Determining the Densityof Non-cellular PlasticsPart 2: Density Gradient Col-umn MethodISO 10993 Biological Eva

19、luation of Medical Devices, Parts1124ISO 9001 Quality Systems ManagementISO 13485 Medical devicesQuality ManagementSystemsRequirements for Regulatory Purposes2.3 Other Documents:5United States Pharmacopeia Vol XXI, or latest edition3. Terminology3.1 Definitions of Terms Specific to This Standard:3.2

20、 fabricated forms, nthose items into which the virginpolymer resin may be converted. These include shapes andforms produced by means of machining, extruding, and com-pression molding virgin polymer resin into a subsequent entity(for example, fibers, tubes, rods, slabs, sheets, film, or complexshaped

21、 parts and devices).3.3 formulated compound, nmaterials, parts, or devicesfabricated from virgin polymer resin in such a way as tocontain intentional or unintentional adjuvant substances.3.4 virgin polymer, nthe initially-delivered form of thepolymer as synthesized from its monomers prior to anyproc

22、essing or fabrication into a medical device. The providedresin is typically in 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 PEKK polymer in the scope of this spec

23、ification isa pure semi-crystalline copolymer consisting of phenylenerings connected by ether (E) and carbonyl (or ketone, K)groups along the polymer chain (see Appendix X2). Itspolymeric structure is defined by the repeating unit EKK. Thisrepeat unit may be of two isomersone where the K-Klinkages a

24、re either of 1,4 arrangement (so-called Para or T)or of 1,3 arrangement (so-called Meta or I). The ratio ofthese isomers defines the types of PEKK. The T/I ratio isdetermined at synthesis and is currently of two types.4.1.1 Type I PEKKThis EKK polymer is made with a T/Iratio of 60/40. The resulting

25、polymer system has a crystalkinetic behavior that makes processing in either amorphous orsemi-crystalline forms practical.4.1.2 Type II PEKKThis EKK polymer is made with a T/Iratio of 80/20. The resulting polymer system is used in asemi-crystalline state.4.2 Types of PEKK plastics, molding and extru

26、sion gradesare described in Classification D4000.5. Properties5.1 The infrared spectrum6of these materials is character-istic of their molecular repeating units. A representative spec-trum is listed in Appendix X3. The PEKK polymer shall yieldan infrared spectrum, which exhibits major bands only at

27、thewavelengths listed for a standard reference spectrum of thatmaterial.5.1.1 The infrared spectrum, as used in this specification, isto identify the material as polyetherketoneketone (PEKK) butdoes not necessarily indicate an acceptable degree of materialpurity.5.1.2 The presence of additional band

28、s in the samplesinfrared spectrum compared to that of the reference materialmay indicate a different polyaryletherketone (PAEK) material(for example, PEEK, PEKEKK, PEK) or impurities, or both.5.2 The physical and chemical property requirements for thevirgin polymer are listed in Table 1. If addition

29、al characteristicsare necessary because of a specific application, the proceduresreferenced in Section 2 are recommended, or as agreed uponbetween the vendor and the purchaser.5.3 The viscosity requirements shall be agreed upon be-tween the vendor and the purchaser4Available from American National S

30、tandards 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.6Silverstein, R. M., Bassler, G. C., and Morrill, T. C., “Spectroscopic Identifi-cation of Organic Co

31、mpounds,” 5th ed., John Wiley polyetherketoneketoneF2820 123APPENDIXES(Nonmandatory Information)X1. RATIONALEX1.1 The PEKK polymers may be processed by mosttechniques available for thermoplastic polymers. Medical de-vices and components of medical devices made of PEKKpolymers may be sterilized. Ster

32、ilization methods successfullyused include steam, ethylene oxide, and 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 molec

33、ular weight of the polymer anddesign, fabrication, intended function, 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 t

34、o develop a significant level of crys-tallinity is an important characteristic of these materials.Performance characteristics are related to the percent crystal-linity. Certain additives and processes (for example, excessivecross linking) can limit these materials ability to crystallize.Therefore, t

35、his feature of the polymer and its fabricated formshould be evaluated, 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-patibili

36、ty of these adjuvant substances, and subsequent formu-lated compounds, parts, and devices shall be established inaccordance with Practice F748 or the ISO 10993 series.TABLE 2 Typical PropertiesAof Fabricated FormsPEKK Type IParameter ISO Methods and Values ASTM Methods and ValuesDensity, kg/m3ISO 11

37、83 1270 D1505 1270Tensile Strength:At Break, MPaISO 527, Type 1B,50 mm/min 90 D638, Type I, 5.08 cm/min 90Tensile Modulus:GPaISO 527, Type 1B,50 mm/min 3.4 D638, Type I, 5.08 cm/min 3.4Percent elongation:at breakB,%ISO 527, Type 1B,50 mm/min 80 D638, Type I, 5.08 cm/min 80Flexural Strength: MPa ISO

38、178 138 D790 138Flexural Modulus: GPa ISO 178 3.3 D790 3.3Compressive Strength: MPa ISO 604 103 D695 103Impact Strength: Notched Izod, J/m ISO 180 6 (kJ/m2) D256, 0.254 cm depth, 0.025 cm radius 50 (J/m)AProperties provided by Oxford Performance Materials, IncBUse an extensometer for measuring strai

39、n and calculating percent elongation.PEKK Type IIParameter ISO Methods and Values ASTM Methods and ValuesDensity, kg/m3ISO 1183 1310 D1505 1310Tensile Strength:At Break, MPaISO 527, Type 1B,50 mm/min 110 D638, Type I, 5.08 cm/min 110Tensile Modulus:GPaISO 527, Type 1B,50 mm/min 4.5 D638, Type I, 5.0

40、8 cm/min 4.5Percent elongation:at breakA,%ISO 527, Type 1B,50 mm/min 10 D638, Type I, 5.08 cm/min 10Flexural Strength: MPa ISO 178 193 D790 193Flexural Modulus: GPa ISO 178 4.6 D790 4.6Compressive Strength: MPa ISO 604 207 D695 207Impact Strength: Notched Izod, J/m ISO 180 3 (kJK/m2) D256, 0.254 cm

41、depth, 0.025 cm radius 50 (Jm)AUse an extensometer for measuring strain and calculating percent elongation.F2820 124X2. CHEMICAL STRUCTURE OF PEKKX3. REPRESENTATIVE INFRARED SPECTRA OF PEKKFIG. X2.1 Chemical Structure of PEKKFIG. X3.1 Representative Infrared Spectra of PEKKF2820 125RELATED MATERIALA

42、utian, J., “Toxicological Evaluation of Biomaterials: Primary AcuteToxicity Screening Program,” Journal of Artificial Organs, Vol 1, No.1, 1977, p. 53.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.,

43、 OBrannon, W., Thompson, S. H., Hodge,R., and Estrella, M. E., “Rapid In Vitro Screening of Polymers forBiocompatibility,” Journal of Macromolecular Science Chemistry,VolA4, No. 3, May 1970, pp. 615634.Rice, R. M., Hegyeli, A. F., Gourlay, S. J., Wade, C. W. R., Dillon, J. G.,Jaffe, H., and Kulkarni

44、, R. K., “Biocompatibility Testing for Polymers:In Vitro Studies With In Vivo Correlation,” Journal of BiomedicalMaterials Research, Vol 12, 1978, p. 43.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. U

45、sers 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 own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed eve

46、ry 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 addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible techn

47、ical 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, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohock

48、en, 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).F2820 126