1、Designation: F 602 09Standard Criteria forImplantable Thermoset Epoxy Plastics1This standard is issued under the fixed designation F 602; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parent
2、heses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These criteria cover thermoset plastics based on digly-cidyl ethers of bisphenol A (DGEBPA) and appropriate curingagents or catalysts as opposed to the
3、rmoplastics based onepoxy structures.1.2 These criteria are generic and are intended to providedefinitions and a standard description of epoxy plastics used inimplantable devices. It is also intended to serve as a standardguide for the preparation of more specific documents withvalues and limits cov
4、ering specific end uses.1.3 Compliance with these criteria shall not be construed asan endorsement of implantability. The biocompatibility ofepoxy plastics as a class has not been established. Epoxyplastic is a generic term relating to the class of polymersformed from epoxy resins, certain curing ag
5、ents or catalysts,and various additives. Since many compositions and formula-tions fall under this class, it is essential that the formulator orfabricator ensure biocompatibility of the specific compositionor formulation in its intended end use. Since these criteriaprovide guidance for the preparati
6、on of more specific docu-ments covering specific end uses, these documents will providebases for standardized evaluation of biocompatibility appropri-ate for a specific end use.1.4 Each of the properties listed shall be considered inselecting materials for specific end uses. A list of selectedproper
7、ties with limiting values assigned is suggested forseparate product specifications.1.5 All of the properties and test methods listed may not bepertinent in any specific situation, nor may all of the testsoutlined be required.1.6 These criteria are limited to functionally or fully curedepoxy plastics
8、. Uncured or incompletely cured formulationsare specifically excluded.1.7 The epoxy plastics covered by this standard are those tobe evaluated for use in implantable biomedical devices. Theterm implantable is herein considered to include devices usedin vivo for time periods in excess of 30 days.1.8
9、This standard does not purport to address all of thesafety 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 the applica-bility of regulatory limitations prior to use.2. Referenced Docum
10、ents2.1 ASTM Standards:2D 149 Test Method for Dielectric Breakdown Voltage andDielectric Strength of Solid Electrical Insulating Materialsat Commercial Power FrequenciesD 150 Test Methods for AC Loss Characteristics and Per-mittivity (Dielectric Constant) of Solid Electrical Insula-tionD 257 Test Me
11、thods for DC Resistance or Conductance ofInsulating MaterialsD 570 Test Method for Water Absorption of PlasticsD 621 Test Methods for Deformation of Plastics UnderLoad3D 638 Test Method for Tensile Properties of PlasticsD 785 Test Method for Rockwell Hardness of Plastics andElectrical Insulating Mat
12、erialsD 792 Test Methods for Density and Specific Gravity (Rela-tive Density) of Plastics by DisplacementD 952 Test Method for Bond or Cohesive Strength of SheetPlastics and Electrical Insulating MaterialsD 1042 Test Method for Linear Dimensional Changes ofPlastics Under Accelerated Service Conditio
13、nsD 1434 Test Method for Determining Gas PermeabilityCharacteristics of Plastic Film and SheetingD 1763 Specification for Epoxy ResinsD 2393 Test Method for Viscosity of Epoxy Resins andRelated Components3D 2471 Practice for Gel Time and Peak Exothermic Tem-perature of Reacting Thermosetting Resins3
14、D 2562 Practice for Classifying Visual Defects in PartsMolded from Reinforced Thermosetting PlasticsD 2734 Test Methods for Void Content of Reinforced Plas-ticsD 3137 Test Method for Rubber PropertyHydrolytic Sta-bility1These criteria are under the jurisdiction of ASTM Committee F04 on Medicaland Su
15、rgical Materials and Devices and are the direct responsibility of Subcommit-tee F04.11 on Polymeric Materials.Current edition approved Aug. 1, 2009. Published September 2009. Originallyapproved in 1978. Last previous edition approved in 2003 as F 602 98a(2003) .2For referenced ASTM standards, visit
16、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, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
17、 19428-2959, United States.E 96/E 96M Test Methods for Water Vapor Transmission ofMaterialsF74 Practice for Determining Hydrolytic Stability of Plas-tic Encapsulants for Electronic Devices3F 619 Practice for Extraction of Medical PlasticsF 748 Practice for Selecting Generic Biological Test Meth-ods
18、for Materials and Devices2.2 AAM1 Standard:EOS-D 10/75 Standard for Ethylene Oxide Sterilization42.3 ISO Standard:ISO 10993 Biological Evaluation of Medical Devices53. Terminology3.1 Definitions:3.1.1 acceleratoran additive used to increase the rate ofcure. An accelerator may also be a catalyst, or
19、it may actuallychange composition and, therefore, not qualify as a catalyst.3.1.2 additivea chemical added to epoxy resins or hard-eners to modify the handling characteristics or cured proper-ties, or both, of the epoxy-hardener combination.3.1.2.1 diluenta chemical used in admixture to modify orenh
20、ance the properties of either or both the uncured or curedformulations. A primary use is to reduce the viscosity of themixed system although other properties such as exotherm rate,stiffness, moisture absorption, and so forth, may be modified orenhanced also.3.1.2.1.1 nonreactive diluenta diluent not
21、 containingchemically reactive functional groups.3.1.2.1.2 reactive diluenta diluent that reacts chemicallywith the epoxy resin or hardener, or both, during cure.3.1.2.2 fillera relatively inert solid particulate materialadded to an epoxy formulation to modify its strength, perma-nence, working prop
22、erties, or other qualities, or to lower costs.3.1.3 curing agent or hardenera compound normallyused in a predetermined concentration to react chemically(copolymerize) by means of several different mechanisms (forexample, condensation or addition polymerization) with orwithout heat or pressure in ord
23、er to change its form from aliquid or fusible, friable, soluble solid to an infusible, insolublesolid having useful and desirable application or end-useproperties.3.1.3.1 initiatoran additive used to cause a thermosettingresin to react with itself (polymerize). Usually, theseadditivesused in relativ
24、ely very small amountsinitiatehomo-polymerization of the epoxy resin resulting in etherlinkages.NOTE 1The term “catalyst” is frequently misused to denote anymaterial added to a resin to cause a reaction to occur. This usage shouldbe discouraged. The Society of Plastics Industries defines a catalyst
25、as “acompound which alters the speed of a reaction without changing itsoriginal composition.”3.1.4 epoxyoxirane ring structures.ORCHCH23.1.4.1 epoxy plasticthermoplastic or thermosetting plas-tics containing ether or hydroxyalkyl repeating units or both,resulting from the ring-opening reactions of l
26、ower molecularweight polyfunctional oxirane resins or compounds, withcatalysts or with various polyfunctional acidic or basic core-actants.3.1.4.2 epoxy resingenerally, any resin (liquid or solid)with a chemical structure at least difunctional in oxirane.Specifically for this standard, the diglycidy
27、l ethers of bisphenolA or the equivalent. These compounds are defined as Grade 1in Specification D 1763.3.1.5 Terms Relating to Cure:3.1.5.1 cure, vto change the properties of a polymericsystem into a final, more stable, usable condition by the use ofheat, radiation, or reaction with chemical additi
28、ves.3.1.5.2 cure cyclethe schedule of time periods at specifiedconditions to which a reacting thermosetting material is sub-jected to reach a specified property level.3.1.5.3 cure timethe interval of time from the start ofreaction to the time at which specified properties of the reactingthermosettin
29、g composition are reached. For materials that reactunder the conditions of mixing, the start of reaction is the timeof initial exposure to the conditions necessary for reaction tooccur.3.1.5.4 functionally curedthe term used to denote anepoxy plastic that has attained sufficient cure to achieve stab
30、leproperties.3.1.5.5 fully curedthe term used to denote total disappear-ance of epoxy groups as detected by infrared spectroscopy, orother equally sensitive physicochemical methods.3.1.5.6 one-component systema formulation based on anepoxy resin preblended with a heat, moisture, or otherwiseactivate
31、d curing agent or catalyst. The mixture is storable butcures under the appropriate activation conditions.3.1.5.7 postcurethe additional and separate curing opera-tions to which a “hardened” thermosetting plastic compositionis subjected in order to enhance one or more properties. Alsoused to ensure s
32、tabilization of physical properties under useconditions.3.1.5.8 two-component systema formulation based on anepoxy resin to which a curing agent or catalyst is added justprior to use.4. Chemical Composition4.1 Epoxy ResinsOxirane-terminated reaction products ofepichlorohydrin and bisphenol A (DGEBPA
33、) or the equivalent.4.2 Reactive DiluentsThe following are examples of com-pounds that may be included as reactive diluents:4.2.1 Butyl glycidyl ether (BGE).4.2.2 Phenyl glycidyl ether (PGE).4.3 Nonreactive DiluentsThe following are examples ofcompounds that may be included as nonreactive diluents:4
34、.3.1 Phthalate esters.4.3.2 Nonyl phenols.4.3.3 Miscible polymers.4.3.4 Flexibilizers.4.4 FillersThe following are examples of fillers that maybe incorporated in the formulations:4.4.1 Silicas:4Available from the Association for the Advancement of Medical Instrumenta-tion, 1901 N. Ft. Myer Dr., Suit
35、e 602, Arlington, VA 22209.5Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.F6020924.4.1.1 Fumed silica.4.4.1.2 Precipitated hydrated silica.4.4.1.3 Diatomaceous earth.4.4.2 Carbons.4.4.3 Certain radiopaque materials:4.4.3
36、.1 Certain inorganic nonmetallic particles.4.4.3.2 Certain metallic particles.4.4.4 Certain pigments.4.4.5 Glass fibers.4.4.6 Glass ceramic particles.4.4.7 Glass or plastic microballoons.4.5 Other AdditivesThe following are examples of addi-tives that may be used in the formulation:4.5.1 Slip agents
37、.4.5.2 Optical brighteners.4.5.3 Surfactants.4.6 Curing AgentsThe following are examples of curingagents for epoxy resins:4.6.1 Amines (primary, secondary, and tertiary) such astriethylenetetramine (TETA).4.6.2 Anhydrides, such as phthalic anhydride.4.6.3 Acids such as phthalic acid.4.6.4 Amine-term
38、inated polyamides.4.6.5 Acid or amine-terminated telomers.4.6.6 Schiffs bases.4.7 Catalysts:4.7.1 Lewis bases such as tertiary amines.4.7.2 Lewis acids such as BF3.4.8 Accelerators:4.8.1 Tertiary amines.4.8.2 Phenols.NOTE 2Since some curing agents and catalysts may be toxic bythemselves, it may be n
39、ecessary in specific end-use standards to requiretests to limit their presence in the final product.5. Physical Requirements5.1 Uncured PropertiesThe following test methods maybe conducted on the uncured mixed formulation or appropriatecomponents:5.1.1 Peak Exotherm TemperatureTest Method D 2471.5.1
40、.2 Gel TimeTest Method D 2471.5.1.3 Mix RatioThe mix ratio shall be calculated andmaintained at the ratio recommended by the manufacturer ofthe formulation.5.1.4 ViscosityTest Method D 2393.5.2 Cured Properties (Required)The following test meth-ods shall be conducted on the fully cured and properlyc
41、onditioned material.5.2.1 ExtractionPractice F 619.5.2.2 Foreign ParticlesUpon careful visual examination,the epoxy plastic shall be free of any extraneous debris thatmay adversely affect its safety, efficacy, or reliability.5.2.3 Hydrolytic StabilityPractice F74 or Test MethodD 3137.5.2.4 Biocompat
42、ibility TestingBiocompatibility of poly-mers and implant devices made using these materials shall bedetermined in accordance with Practice F 748 or theISO 10993 series, unless otherwise agreed upon between thesupplier and the consumer and regulating bodies. These stan-dards recommend specific biocom
43、patibility testing, dependingon the intended use of the device.5.2.4.1 Biocompatibility testing should be performed onspecimens that have been processed and sterilized using themethods intended for the final device.5.2.5 Sterilant Residues and Sterilization EffectsTestingregarding applicable methods
44、 of sterilization should be docu-mented. In addition to degassing time necessary for EtOsterilization, the stability of the epoxy under steam andradiation sterilization should be specified if these types ofsterilization are called for.5.2.5.1 Sterilant residues shall be tested according to appro-pri
45、ate methods, such as AAMI EOS-D. The concentration ofethylene oxide, ethylene chlorohydrin, ethylene glycol, anddichlorodifluoromethane (or the equivalents) at the time ofimplantation shall be shown to be within safe limits prescribedby the device manufacturer. Cell culture tests can be used toshow
46、the absence of sterilant residues. When materials aresterilized by radiation, materials subjected to maximum radia-tion dose shall be qualified by performance tests.5.2.6 Water AbsorptionTest Method D 570.5.3 Cured Properties (Optional)The following test meth-ods shall be conducted on the fully cure
47、d and properlyconditioned material as is appropriate for the end use:5.3.1 AdhesionTest Method D 952.5.3.2 Bacteriostasis and FungistasisSterility Tests.65.3.3 Compression SetTest Methods D 621.5.3.4 Dielectric ConstantTest Methods D 150.5.3.5 Dielectric StrengthTest Method D 149.5.3.6 Dissipation F
48、actorTest Methods D 150.5.3.7 ElongationTest Method D 638.5.3.8 Flexural StrengthTest Method D 1434.5.3.9 Gas PermeationTest Method D 1434.5.3.10 HardnessTest Method D 785.5.3.11 Moisture Vapor TransmissionTest Methods E 96/E 96M.5.3.12 Prothrombin TimeThe effect of the material on theProthrombin ti
49、me shall be tested by appropriate methods.75.3.13 Specific GravityTest Methods D 792.5.3.14 Stability (dimensional)Test Method D 1042.5.3.15 Stypven TimeThe effect of the material on theStypven time shall be tested by appropriate methods.65.3.16 Surface ResistivityTest Methods D 257.5.3.17 Tangent ModulusTest Method D 638.5.3.18 Tensile StrengthTest Method D 638.5.3.19 Visual DefectsPractice D 2562.5.3.20 VoidsTest Method D 2734.5.3.21 Volume ResistivityTest Method D 257.6. Identification6.1 The following analytical
