ASTM F602-1998a(2003) Standard Criteria for Implantable Thermoset Epoxy Plastics《可植入的热固性环氧塑料标准》.pdf

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1、Designation: F 602 98a (Reapproved 2003)Standard 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.

2、 A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 catalys

3、ts as opposed to thermoplastics 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 withv

4、alues and limits covering 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 resin

5、s, certain curing agents 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 guidan

6、ce for the preparation 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 li

7、st of selectedproperties 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

8、 curedepoxy plastics. 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 ex

9、cess of 30 days.1.8 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

10、.2. Referenced Documents2.1 ASTM Standards:D 149 Test Method for Dielectric Breakdown Voltage andDielectric Strength of Solid Electrical Insulating Materialsat Commercial Power Frequencies2D 150 Test Methods for ac Loss Characteristics and Permit-tivity (Dielectric Constant) of Solid Electrical Insu

11、latingMaterials2D 257 Test Methods for dc Resistance or Conductance ofInsulating Materials2D 570 Test Method for Water Absorption of Plastics3D 621 Test Methods for Deformation of Plastics UnderLoad4D 638 Test Method for Tensile Properties of Plastics3D 785 Test Method for Rockwell Hardness of Plast

12、ics andElectrical Insulating Materials3D 792 Test Methods for Density and Specific Gravity (Rela-tive Density) of Plastics by Displacement3D 883 Terminology Relating to Plastics3D 952 Test Method for Bond or Cohesive Strength of SheetPlastics and Electrical Insulating Materials3D 1042 Test Method fo

13、r Linear Dimensional Changes ofPlastics Under Accelerated Service Conditions3D 1434 Test Method for Determining Gas PermeabilityCharacteristics of Plastic Film and Sheeting5D 1763 Specification for Epoxy Resins3D 2393 Test Method for Viscosity of Epoxy Resins andRelated Components6D 2471 Test Method

14、 for Gel Time and Peak ExothermicTemperature of Reacting Thermosetting Resins7D 2562 Practice for Classifying Visual Defects in Parts1These criteria are under the jurisdiction of ASTM Committee F04 on Medicaland Surgical Materials and Devices and are the direct responsibility of Subcommit-tee F04.11

15、 on Polymeric Materials.Current edition approved Apr. 10, 2003. Published May 2003. Originallyapproved in 1978. Last previous edition approved in 1998 as F 602 98a.2Annual Book of ASTM Standards, Vol 10.01.3Annual Book of ASTM Standards, Vol 08.01.4Discontinued; See 1994 Annual Book of ASTM Standard

16、s, Vol 08.01.5Annual Book of ASTM Standards, Vol 15.09.6Discontinued; See 1995 Annual Book of ASTM Standards, Vol 08.02.7Annual Book of ASTM Standards, Vol 08.02.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Molded from Reinforced

17、Thermosetting Plastics7D 2566 Test Method for Linear Shrinkage of Cured Ther-mosetting Casting Resins During Cure8D 2734 Test Method for Void Content of Reinforced Plas-tics7D 2990 Test Method for Tensile, Compressive, and FlexuralCreep and Creep Rupture of Plastics7D 3013 Specification for Epoxy Mo

18、lding Compounds7D 3137 Test Method for Rubber PropertyHydrolytic Sta-bility9E 96 Test Methods for Water Vapor Transmission of Mate-rials10F 74 Practice for Determining Hydrolytic Stability of Plas-tic Encapsulants for Electronic Devices11F 619 Practice for Extraction of Medical Plastics12F 748 Pract

19、ice for Selecting Generic Biological Test Meth-ods for Materials and Devices122.2 AAM1 Standard:EOS-D 10/75 Standard for Ethylene Oxide Sterilization133. Terminology3.1 Definitions:3.1.1 acceleratoran additive used to increase the rate ofcure. An accelerator may also be a catalyst, or it may actuall

20、ychange 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 orenhance the prope

21、rties 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 containingche

22、mically 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 properties, or oth

23、er 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 order to change i

24、ts 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 relatively very small

25、 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 as “acompound

26、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 lower molecular

27、weight 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 diglycidyl ethers of bi

28、sphenolA 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 additives.3.1.5.2 cu

29、re 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 reactingthermosetting composition

30、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 stableproperties.3

31、.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 otherwiseactivated curing agent

32、 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 stabilization o

33、f 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) or the equiv

34、alent.8Discontinued; See 1993 Annual Book of ASTM Standards, Vol 08.02.9Annual Book of ASTM Standards, Vol 09.01.10Annual Book of ASTM Standards, Vol 04.06.11Discontinued; See 1994 Annual Book of ASTM Standards, Vol 10.04.12Annual Book of ASTM Standards, Vol 13.01.13Available from the Association fo

35、r the Advancement of Medical Instrumen-tation, 1901 N. Ft. Myer Dr., Suite 602, Arlington, VA 22209.F 602 98a (2003)24.2 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 Nonreact

36、ive DiluentsThe following are examples ofcompounds that may be included as nonreactive diluents:4.3.1 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:4.4.1.1 Fu

37、med silica.4.4.1.2 Precipitated hydrated silica.4.4.1.3 Diatomaceous earth.4.4.2 Carbons.4.4.3 Certain radiopaque materials:4.4.3.1 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 plasti

38、c microballoons.4.5 Other AdditivesThe following are examples of addi-tives that may be used in the formulation:4.5.1 Slip agents.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) s

39、uch astriethylenetetramine (TETA).4.6.2 Anhydrides, such as phthalic anhydride.4.6.3 Acids such as phthalic acid.4.6.4 Amine-terminated 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 Acc

40、elerators:4.8.1 Tertiary amines.4.8.2 Phenols.NOTE 2Since some curing agents and catalysts may be toxic bythemselves, it may be necessary in specific end-use standards to requiretests to limit their presence in the final product.5. Physical Requirements5.1 Uncured PropertiesThe following test method

41、s maybe conducted on the uncured mixed formulation or appropriatecomponents:5.1.1 Peak Exotherm TemperatureTest Method D 2471.5.1.2 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 Viscosity

42、Test Method D 2393.5.2 Cured Properties (Required)The following test meth-ods shall be conducted on the fully cured and properlyconditioned 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

43、adversely affect its safety, efficacy, or reliability.5.2.3 Hydrolytic StabilityPractice F 74 or Test MethodD 3137.5.2.4 USP Biological Tests14The material shall pass thebiological tests for plastic containers, as is appropriate for theintended end use:5.2.4.1 Short-term implantation test.5.2.4.2 Sa

44、line extract test.5.2.4.3 Cottonseed oil extract test.5.2.4.4 Alcohol extract test.5.2.5 Sterilant ResiduesTesting regarding applicablemethods of sterilization should be documented. In addition todegassing time necessary for EtO sterilization, the stability ofthe epoxy under steam and radiation ster

45、ilization should bespecified if these types of sterilization are called for.5.2.5.1 Sterilant residues shall be tested according to appro-priate methods, such as AAMI EOS-D. The concentration ofethylene oxide, ethylene chlorohydrin, ethylene glycol, anddichlorodifluoromethane (or the equivalents) at

46、 the time ofimplant shall be shown to be within safe limits prescribed bythe device manufacturer. Cell culture tests can be used to showabsence of sterilant residues. When materials are sterilized byradiation, materials subjected to maximum radiation dose shallbe qualified by performance tests.5.2.6

47、 Water AbsorptionTest Method D 570.5.3 Cured Properties (Optional)The following test meth-ods shall be conducted on the fully cured and properlyconditioned material as is appropriate for the end use:5.3.1 AdhesionTest Method D 952.5.3.2 Bacteriostasis and FungistasisSterility Tests.155.3.3 Compressi

48、on SetTest Methods D 621.5.3.4 Dielectric ConstantTest Methods D 150.5.3.5 Dielectric StrengthTest Method D 149.5.3.6 Dissipation FactorTest 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 7

49、85.5.3.11 HemolysisThe material shall be tested forhemolytic properties by appropriate methods.5.3.12 ImplantabilityThe encapsulant shall be shown tobe safe and effective for long-term implant by appropriatestate-of-the-art tests.5.3.12.1 Biological test procedures appropriate to determinebiological safety and tissue reactions are described in PracticeF 748 which recommends generic biological test methods formaterials and devices according to end use applications.5.3.13 Moisture Vapor TransmissionTest Methods E 96.14United Stat