1、Designation: F754 08 (Reapproved 2015)Standard Specification forImplantable Polytetrafluoroethylene (PTFE) Sheet, Tube, andRod Shapes Fabricated from Granular Molding Powders1This standard is issued under the fixed designation F754; the number immediately following the designation indicates the year
2、 of originaladoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification describes the physical, chemical, andmech
3、anical performance requirements for polytetrafluoroeth-ylene (PTFE) pre-fabricated by compression molding or extru-sion into sheet, tube, and rod shapes which may be used forimplant products.1.2 PTFE is a high molecular weight straight chain memberof the generic class of perfluorocarbon (containing
4、only theelements fluorine and carbon) polymers.1.3 Perfluorocarbon high polymers exhibit extraordinarythermal and chemical stability and do not require stabilizingadditives of any kind.1.4 This specification applies to primarily void-free moldedor extruded PTFE shapes formed from granular moldingpow
5、ders. This specification does not apply to shapes formedfrom “fine powder” resins by lubricated paste extrusion, whichincludes expanded PTFE.1.5 This specification does not apply to specific surgicalimplant products, including their packaging, sterilization, ormaterial boicompatibility and/or suitab
6、ility for a particularend-use application.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of t
7、he user 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:2D1710 Specification for Extruded Polytetrafluoroethylene(PTFE) Rod, Heavy Walled Tubing and Basic ShapesD3
8、294 Specification for Polytetrafluoroethylene (PTFE)Resin Molded Sheet and Molded Basic ShapesD4894 Specification for Polytetrafluoroethylene (PTFE)Granular Molding and Ram Extrusion MaterialsE1994 Practice for Use of Process Oriented AOQL andLTPD Sampling Plans2.2 AAMI Standards:3AAMI STBK91 Steril
9、izationPart 1: Sterilization inHealth Care FacilitiesAAMI STBK92 SterilizationPart 2: Sterilization Equip-mentAAMI STBK93 SterilizationPart 3: Industrial ProcessControl2.3 ANSI Standards:4ANSI/ISO/ASQ Q9000 Quality Management SystemsFundamentals and VocabularyANSI/ISO/ASQ Q9001 Quality Management Sy
10、stemsRequirements2.4 ISO Standards:4ISO 10993 Biological Evaluation of Medical Devices2.5 U. S. Code of Federal Regulations:521 CFR 820 Quality System Regulation1This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is the direct responsi
11、bility ofSubcommittee F04.11 on Polymeric Materials.Current edition approved March 1, 2015. Published May 2015. Originallyapproved in 1983. Last previous edition approved in 2008 as F754 08. DOI:10.1520/F0754-08R15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM
12、Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Association for the Advancement of Medical Instrumentation(AAMI), 1110 N. Glebe Rd., Suite 220, Arlington, VA 222014795.4Available
13、 from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.5Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.Copyright ASTM Inter
14、national, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.6 U. S. Pharmacopeia (USP) Standards:6USP30/NF25 Sterilization and Sterility Assuranceof Compendial Articles3. Significance and Use3.1 Fabricated PTFE meeting the requirements of this speci-fication can b
15、e expected to exhibit consistent and reproduciblechemical, physical, and biological properties.3.1.1 This specification provides an analytic method toextract organic contaminants from fabricated configurations,which includes a limit to the presence of residual adulterants,additives, or processing ai
16、ds.3.1.2 This specification addresses the characteristics ofvirgin raw granular molding powders obtained from resinmanufacturers and used for producing implant configurations.4. Physical Property Requirements4.1 Molding and Extrusion Powders:4.1.1 PTFE PolymerGranular molding and extrusionpowders us
17、ed for fabrication of implant configurations shall bevirgin product and shall conform to Specification D4894.4.2 PTFE Standard Shapes:4.2.1 Standard shapes, such as molded sheet, rod, and/ortube utilized in implants, shall have been prepared from virginmolding or extrusion materials which meet the p
18、rovisions of4.1.1.4.2.2 PTFE molded sheet shall comply with Type I, Grade I,Class A requirements in Specification D3294.4.2.3 PTFE rod and/or tube in the final implant shape shallcomply with Type I, Grade I, Class D specifications inSpecification D1710. Material purchased for conversion into afinal
19、implant shape may meet Classes A, B, C, or D.4.2.4 The final implant manufacturer shall determine if thespecified dimensions and mechanical properties of thesupplier-provided and/or as-converted sheet, rod, and/or tubeare appropriate for the intended implant application.Additionalmaterial property d
20、ata (such as fatigue life, wear, and abrasionresistance) may also be necessary to assure suitability, depen-dent on the implant application.4.3 Surface ContaminationThe surface of a fabricatedshape shall not contain particles or residue of a diametergreater than 300 m. The concentration of visible p
21、articlesunder 8 magnification shall not be greater than 10 particlesper 400 cm2.4.4 Physical properties for other than standard shapes arenot encompassed by this specification and must be addressedby appropriate performance standards for given configurations.5. Chemical Property Requirements5.1 Carb
22、on Tetrachloride ExtractionThe supplier-provided or as-converted final PTFE implant shapes shall besampled in accordance with Practice E1994 (or equivalentstandard guidance) and extracted with carbon tetrachloride bythe method described in Annex A1.5.1.1 Extractable HydrocarbonsThe absence of extrac
23、t-able hydrocarbons shall be demonstrated by infrared analysisof the carbon tetrachloride extract using the methodology andacceptance criteria described in Annex A1.5.1.2 AppearanceA sample shall be examined under day-light conditions with the naked eye immediately followingcarbon tetrachloride extr
24、action as described in Annex A1. Thissample while still wet with carbon tetrachloride shall not beapparently changed in size or consistency. When dried for 4 hin a 100C air-circulating oven, the appearance of the extractedpolymer sample shall be unchanged as compared to an unex-tracted specimen.5.2
25、Extraction with Distilled WaterFinal PTFE implantshapes sampled from stock shall be extracted with distilledwater by the methodology described in Annex A2.5.2.1 Extractable ElectrolytesThe resistivity of the wateras measured by a resistivity conductivity meter shall be greaterthan 0.05 Mcm.5.2.2 App
26、earanceWhen examined by unaided vision indaylight, the appearance of PTFE sampled from stock imme-diately following water extraction shall be unchanged exceptfor being obviously wet with water. When dried for 4 h at100C in an air-circulating oven the appearance shall beunchanged from pre-extraction
27、appearance.6. Manufacturing Control, Sterilization, andBiocompatibility6.1 Any final implant product needs to be manufacturedunder an acceptable level of control and provided both insterile form and with a level of biocompatibility suitable for thefinal implant application.6.2 Acceptable levels of m
28、anufacturing control are likely tobe required for commercial distribution. General guidelines forachieving acceptable levels of manufacturing quality controlmay be found in the following standards:6.2.1 United States Code of Federal Regulations (CFR), 21CFR 820.6.2.2 ANSI/ISO/ASQ Q9000Provides funda
29、mentals forquality management systems as described in the ISO 9000family (informative); and specifies quality management termsand their definitions (normative).6.2.3 ANSI/ISO/ASQ Q9001Presents requirements for aquality management system. The application of this guide canbe used by an organization to
30、 demonstrate its capability to meetcustomer requirements for products or services, and for assess-ment of that capability by internal and external parties.6.3 A summary of most common sterilization methods,testing, and quality assurance can be found in USP30/NF25. AAMI maintains a 3-volume set of st
31、erilizationstandards and recommended practices containing 46 differentstandards: AAMI STBK91, AAMI STBK92, and AAMISTBK93.NOTE 1Since many fluoropolymers can be readily damaged and/oraltered by radiation-based sterilization, significant caution should beundertaken when considering such methods.6Avai
32、lable from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,MD 20852-1790, or through http:/www.usp.org/products/USPNF/. The standardswill be listed by appropriate USP citation number. Succeeding USP editionsalternately may be referenced.F754 08 (2015)26.4 Finished device biocompatibility c
33、an be ascertainedthrough evaluation utilizing the guidelines detailed within ISO10993.6.4.1 A brief summary of in vivo particulation concernsspecific to mechanically loaded PTFE may be found inAppendix X2.7. Keywords7.1 perfluorocarbon; polytetrafluoroethylene; PTFE; surgi-cal implantANNEXES(Mandato
34、ry Information)A1. INFRARED ANALYSIS OF HYDROCARBONS EXTRACTABLE IN CARBON TETRACHLORIDEA1.1 Stir at least1gofchopped sample, all of which passesa No. 40 mesh screen, for 30 min with 7-mL of reagent-gradecarbon tetrachloride. When decanted, the carbon tetrachlorideshall be clear and colorless.A1.2 P
35、erform infrared analysis of the carbon tetrachlorideafter placement within a 10 by 10 mm silica quartz UV cuvette(for example, Beckman-Coulter Part No. 580012).A1.2.1 The requirements of this analysis shall be satisfiedwhen transmission between 3 and 4 m is essentially 100 % forthe reagent grade con
36、trol and at least 95 % of that of the controlscan for carbon tetrachloride in which the chopped sample wasstored.A2. EXTRACTION WITH WATER FOR ELECTROLYTESA2.1 The specimens shall be cubes or rectangles with noedge dimension greater than 1 cm. The total specimen weightshall be 10 6 1g.A2.2 Place the
37、 specimens in a suitable container, such as a100-cm3suction flask, along with 50 mL of distilled water.Store the flask 48 h at ambient temperature.A2.3 After 48 h, decant the water. The water shall remainclear and colorless. The extractable electrolyte requirementsshall be satisfied when the resisti
38、vity of the water is greaterthan 0.05 Mcm.APPENDIXES(Nonmandatory Information)X1. STATEMENT OF RATIONALEX1.1 This specification was established to provide guidancein the testing of polytetrafluorethylene intended for use inmedical device applications. It recommends test methods forthe measurement of
39、 chemical, physical and mechanical prop-erties of unfabricated and fabricated forms. Tests should beselected according to end-use applications. It is intended thatbiocompatibility be established on the finished product by theappropriate procedures, after it has gone through all processingsteps.X1.2
40、The scope section of this document defines the term“PTFE” and limits the specific scope of the document tofabricated sheet, tube, and rod shapes. It further makes clearthat the specification does not apply to specific surgical implantproducts that would be subject to appropriate specific end-useperf
41、ormance standards. This section emphasizes the extraordi-nary chemical and thermal stability and inherent absence ofadditives in PTFE; these factors are no doubt responsible forthe large bibliography of successful implant use for thispolymer in the absence of any previous implant grade specifi-catio
42、n guidance.X1.3 The significance section sets out the capability of thisstandard by ensuring consistent and reproducible behavior.X2.1 explains the caution against construing this specificationfor applications where particulate debris may be anticipated.X1.4 In 4.1, the specific raw polymer properti
43、es consistentwith the scope and intent of this specification are defined inF754 08 (2015)3terms of existingASTM specifications so that the raw polymerswill be virgin products providing the highest purity availableunder current manufacturing technology. Similarly, 4.2 relatesthe finished shape physic
44、al properties consistent with the scopeand objectives of this standard specification to existing ASTMspecifications for such standard shapes. These requirementswould provide the superior properties for such shapes availablewith current fabrication technology.X1.5 Section 5 provides appearance and ex
45、tractable criteriafor PTFE-fabricated shapes sampled from stock to establish theabsence of extractable organic or electrolytic contaminants thatmay have contaminated the product during its preparation. Afailure would then signal the need for review of the manufac-turing process to determine the natu
46、re, source, and significanceof the contamination.X2. BIOCOMPATIBILITYX2.1 PTFE configurations were first used for implantationin the early 1950s and, in numerous applications, have servedas compatible implants in large numbers of patients, with someimplant durations beyond 20 years (1, 2, 3).7Howeve
47、r, use ofPTFE in in vivo applications with load bearing outside of thepressure-velocity (PV) limits for the polymer may result insignificant particulation and extensive adverse effects (4, 5).Abrief summary of adverse effects from the historical use ofPTFE in the temporomandibular joint application
48、can be foundin the document entitled TMJ ImplantsA Consumer Infor-mational Update.8X2.2 No known surgical implant material has ever beenshown to be completely free of adverse reactions in the humanbody. However, long term clinical experience of use of specificcompositions and formations of this mate
49、rial referred to in thisstandard has shown that an acceptable level of biologicalresponse can be expected, if the material is used in appropriateapplications.REFERENCES(1) Homsy, C. A., “Biocompatibility of Perfluorinated Polymers andComposites of These Polymers,” Biocompatibility of Clinical ImplantMaterials, O.F. Williams, ed., Chap. 3, Vol II, Boca Raton, FL, C.R.C.Press, Inc., 1982, pp 59 77.(2) Sanchez, L. A., Snuggs, W. D., Veith, F. J., Marin, M. L., Wengerter,K. R., Panetta, T. F., “Is Surveillance to Detect Failing Polytetrafluo-roethy
