NOTICE: This standard has either been superceded and replaced by a new version or discontinued.

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Designation: F 602 – 98a

Standard Criteria for

Implantable Thermoset Epoxy Plastics1
This standard is issued under the fixed designation F 602; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope priate safety and health practices and determine the applica-
1.1 These criteria cover thermoset plastics based on digly- bility of regulatory limitations prior to use.
cidyl ethers of bisphenol A (DGEBPA) and appropriate curing 2. Referenced Documents
agents or catalysts as opposed to thermoplastics based on
epoxy structures. 2.1 ASTM Standards:
1.2 These criteria are generic and are intended to provide D 149 Test Method for Dielectric Breakdown Voltage and
definitions and a standard description of epoxy plastics used in Dielectric Strength of Solid Electrical Insulating Materials
implantable devices. It is also intended to serve as a standard at Commercial Power Frequencies2
guide for the preparation of more specific documents with D 150 Test Methods for A-C Loss Characteristics and
values and limits covering specific end uses. Permittivity (Dielectric Constant) of Solid Electrical Insu-
1.3 Compliance with these criteria shall not be construed as lating Materials2
an endorsement of implantability. The biocompatibility of D 257 Test Methods for D-C Resistance or Conductance of
epoxy plastics as a class has not been established. Epoxy Insulating Materials2
plastic is a generic term relating to the class of polymers D 570 Test Method for Water Absorption of Plastics3
formed from epoxy resins, certain curing agents or catalysts, D 621 Test Methods for Deformation of Plastics Under
and various additives. Since many compositions and formula- Load3
tions fall under this class, it is essential that the formulator or D 638 Test Method for Tensile Properties of Plastics3
fabricator ensure biocompatibility of the specific composition D 785 Test Method for Rockwell Hardness of Plastics and
or formulation in its intended end use. Since these criteria Electrical Insulating Materials3
provide guidance for the preparation of more specific docu- D 792 Test Methods for Specific Gravity (Relative Density)
ments covering specific end uses, these documents will provide and Density of Plastics by Displacement3
bases for standardized evaluation of biocompatibility appropri- D 883 Terminology Relating to Plastics3
ate for a specific end use. D 952 Test Method for Bond or Cohesive Strength of Sheet
1.4 Each of the properties listed shall be considered in Plastics and Electrical Insulating Materials3
selecting materials for specific end uses. A list of selected D 1042 Test Method for Linear Dimensional Changes of
properties with limiting values assigned is suggested for Plastics3
separate product specifications. D 1434 Test Method for Determining Gas Permeability
1.5 All of the properties and test methods listed may not be Characteristics of Plastic Film and Sheeting4
pertinent in any specific situation, nor may all of the tests D 1763 Specification for Epoxy Resins3
outlined be required. D 2393 Test Method for Viscosity of Epoxy Resins and
1.6 These criteria are limited to functionally or fully cured Related Components5
epoxy plastics. Uncured or incompletely cured formulations D 2471 Test Method for Gel Time and Peak Exothermic
are specifically excluded. Temperature of Reacting Thermosetting Resins5
1.7 The epoxy plastics covered by this standard are those to D 2562 Practice for Classifying Visual Defects in Parts
be evaluated for use in implantable biomedical devices. The Molded from Reinforced Thermosetting Plastics5
term implantable is herein considered to include devices used D 2566 Test Method for Linear Shrinkage of Cured Ther-
in vivo for time periods in excess of 30 days. mosetting Casting Resins During Cure5
1.8 This standard does not purport to address all of the D 2734 Test Method for Void Content of Reinforced Plas-
safety concerns, if any, associated with its use. It is the tics5
responsibility of the user of this standard to establish appro- D 2990 Test Method for Tensile, Compressive, and Flexural
Creep and Creep Rupture of Plastics5
1
These criteria are under the jurisdiction of ASTM Committee F-4 on Medical
2
and Surgical Materials and Devices and are the direct responsibility of Subcommit- Annual Book of ASTM Standards, Vol 10.01.
3
tee F04.11 on Polymeric Materials. Annual Book of ASTM Standards, Vol 08.01.
4
Current edition approved October 10, 1998. Published December 1998. Origi- Annual Book of ASTM Standards, Vol 15.09.
5
nally published as F 602 – 78. Last previous edition F 602 – 98. Annual Book of ASTM Standards, Vol 08.02.

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

1
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

F 602
D 3013 Specification for Epoxy Molding Compounds5 3.1.4 epoxy—oxirane ring structures.
D 3137 Test Method for Rubber Property—Hydrolytic Sta- O
bility6 R—CH—CH2
E 96 Test Methods for Water Vapor Transmission of Mate- 3.1.4.1 epoxy plastic—thermoplastic or thermosetting plas-
rials7 tics containing ether or hydroxyalkyl repeating units or both,
F 74 Practice for Determining Hydrolytic Stability of Plas- resulting from the ring-opening reactions of lower molecular
tic Encapsulants for Electronic Devices8 weight polyfunctional oxirane resins or compounds, with
F 619 Practice for Extraction of Medical Plastics9 catalysts or with various polyfunctional acidic or basic core-
F 748 Practice for Selecting Generic Biological Test Meth- actants.
ods for Materials and Devices9 3.1.4.2 epoxy resin—generally, any resin (liquid or solid)
2.2 AAM1 Standard: with a chemical structure at least difunctional in oxirane.
EOS-D 10/75 Standard for Ethylene Oxide Sterilization10 Specifically for this standard, the diglycidyl ethers of bisphenol
A or the equivalent. These compounds are defined as Grade 1
3. Terminology in Specification D 1763.
3.1 Definitions: 3.1.5 Terms Relating to Cure:
3.1.1 accelerator—an additive used to increase the rate of 3.1.5.1 cure, v—to change the properties of a polymeric
cure. An accelerator may also be a catalyst, or it may actually system into a final, more stable, usable condition by the use of
change composition and, therefore, not qualify as a catalyst. heat, radiation, or reaction with chemical additives.
3.1.2 additive—a chemical added to epoxy resins or hard- 3.1.5.2 cure cycle—the schedule of time periods at specified
eners to modify the handling characteristics or cured proper- conditions to which a reacting thermosetting material is sub-
ties, or both, of the epoxy-hardener combination. jected to reach a specified property level.
3.1.2.1 diluent—a chemical used in admixture to modify or 3.1.5.3 cure time—the interval of time from the start of
enhance the properties of either or both the uncured or cured reaction to the time at which specified properties of the reacting
formulations. A primary use is to reduce the viscosity of the thermosetting composition are reached. For materials that react
mixed system although other properties such as exotherm rate, under the conditions of mixing, the start of reaction is the time
stiffness, moisture absorption, etc., may be modified or en- of initial exposure to the conditions necessary for reaction to
hanced also. occur.
3.1.2.1.1 nonreactive diluent—a diluent not containing 3.1.5.4 functionally cured—the term used to denote an
chemically reactive functional groups. epoxy plastic that has attained sufficient cure to achieve stable
3.1.2.1.2 reactive diluent—a diluent that reacts chemically properties.
with the epoxy resin or hardener, or both, during cure. 3.1.5.5 fully cured—the term used to denote total disappear-
3.1.2.2 filler—a relatively inert solid particulate material ance of epoxy groups as detected by infrared spectroscopy, or
added to an epoxy formulation to modify its strength, perma- other equally sensitive physicochemical methods.
nence, working properties, or other qualities, or to lower costs. 3.1.5.6 one-component system—a formulation based on an
3.1.3 curing agent or hardener—a compound normally epoxy resin preblended with a heat, moisture, or otherwise
used in a predetermined concentration to react chemically activated curing agent or catalyst. The mixture is storable but
(copolymerize) by means of several different mechanisms (for cures under the appropriate activation conditions.
example, condensation or addition polymerization) with or 3.1.5.7 postcure—the additional and separate curing opera-
without heat or pressure in order to change its form from a tions to which a “hardened” thermosetting plastic composition
liquid or fusible, friable, soluble solid to an infusible, insoluble is subjected in order to enhance one or more properties. Also
solid having useful and desirable application or end-use used to ensure stabilization of physical properties under use
properties. conditions.
3.1.3.1 initiator—an additive used to cause a thermosetting 3.1.5.8 two-component system—a formulation based on an
resin to react with itself (polymerize). Usually, these epoxy resin to which a curing agent or catalyst is added just
additives—used in relatively very small amounts—initiate prior to use.
homo-polymerization of the epoxy resin resulting in ether
4. Chemical Composition
linkages.
4.1 Epoxy Resins—Oxirane-terminated reaction products of
NOTE 1—The term “catalyst” is frequently misused to denote any
epichlorohydrin and bisphenol A (DGEBPA) or the equivalent.
material added to a resin to cause a reaction to occur. This usage should
be discouraged. The Society of Plastics Industries defines a catalyst as “a 4.2 Reactive Diluents—The following are examples of com-
compound which alters the speed of a reaction without changing its pounds that may be included as reactive diluents:
original composition.” 4.2.1 Butyl glycidyl ether (BGE).
4.2.2 Phenyl glycidyl ether (PGE).
4.3 Nonreactive Diluents—The following are examples of
6
Annual Book of ASTM Standards, Vol 09.01. compounds that may be included as nonreactive diluents:
7
8
Annual Book of ASTM Standards, Vol 04.06. 4.3.1 Phthalate esters.
Annual Book of ASTM Standards, Vol 10.04.
9
Annual Book of ASTM Standards, Vol 13.01.
4.3.2 Nonyl phenols.
10
Available from the Association for the Advancement of Medical Instrumen- 4.3.3 Miscible polymers.
tation, 1901 N. Ft. Myer Dr., Suite 602, Arlington, VA 22209. 4.3.4 Flexibilizers.

2
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

F 602
4.4 Fillers—The following are examples of fillers that may 5.2.4 USP Biological Tests11 —The material shall pass the
be incorporated in the formulations: biological tests for plastic containers, as is appropriate for the
4.4.1 Silicas: intended end use:
4.4.1.1 Fumed silica. 5.2.4.1 Short-term implantation test.
4.4.1.2 Precipitated hydrated silica. 5.2.4.2 Saline extract test.
4.4.1.3 Diatomaceous earth. 5.2.4.3 Cottonseed oil extract test.
4.4.2 Carbons. 5.2.4.4 Alcohol extract test.
4.4.3 Certain radiopaque materials: 5.2.5 Sterilant Residues—Testing regarding applicable
4.4.3.1 Certain inorganic nonmetallic particles. methods of sterilization should be documented. In addition to
4.4.3.2 Certain metallic particles. degassing time necessary for EtO sterilization, the stability of
4.4.4 Certain pigments. the epoxy under steam and radiation sterilization should be
4.4.5 Glass fibers. specified if these types of sterilization are called for.
4.4.6 Glass ceramic particles. 5.2.5.1 Sterilant residues shall be tested according to appro-
priate methods, such as AAMI EOS-D. The concentration of
4.4.7 Glass or plastic microballoons.
ethylene oxide, ethylene chlorohydrin, ethylene glycol, and
4.5 Other Additives—The following are examples of addi-
dichlorodifluoromethane (or the equivalents) at the time of
tives that may be used in the formulation:
implant shall be shown to be within safe limits prescribed by
4.5.1 Slip agents.
the device manufacturer. Cell culture tests can be used to show
4.5.2 Optical brighteners. absence of sterilant residues. When materials are sterilized by
4.5.3 Surfactants. radiation, materials subjected to maximum radiation dose shall
4.6 Curing Agents—The following are examples of curing be qualified by performance tests.
agents for epoxy resins: 5.2.6 Water Absorption—Test Method D 570.
4.6.1 Amines (primary, secondary, and tertiary) such as 5.3 Cured Properties (Optional)—The following test meth-
triethylenetetramine (TETA). ods shall be conducted on the fully cured and properly
4.6.2 Anhydrides, such as phthalic anhydride. conditioned material as is appropriate for the end use:
4.6.3 Acids such as phthalic acid. 5.3.1 Adhesion—Test Method D 952.
4.6.4 Amine-terminated polyamides. 5.3.2 Bacteriostasis and Fungistasis—Sterility Tests.12
4.6.5 Acid or amine-terminated telomers. 5.3.3 Compression Set—Test Methods D 621.
4.6.6 Schiff’s bases. 5.3.4 Dielectric Constant—Test Methods D 150.
4.7 Catalysts: 5.3.5 Dielectric Strength—Test Method D 149.
4.7.1 Lewis bases such as tertiary amines. 5.3.6 Dissipation Factor—Test Methods D 150.
4.7.2 Lewis acids such as BF3. 5.3.7 Elongation—Test Method D 638.
4.8 Accelerators: 5.3.8 Flexural Strength—Test Method D 1434.
4.8.1 Tertiary amines. 5.3.9 Gas Permeation—Test Method D 1434.
4.8.2 Phenols. 5.3.10 Hardness—Test Method D 785.
5.3.11 Hemolysis—The material shall be tested for
NOTE 2—Since some curing agents and catalysts may be toxic by hemolytic properties by appropriate methods.
themselves, it may be necessary in specific end-use standards to require
tests to limit their presence in the final product.
5.3.12 Implantability—The encapsulant shall be shown to
be safe and effective for long-term implant by appropriate
5. Physical Requirements state-of-the-art tests.
5.3.12.1 Biological test procedures appropriate to determine
5.1 Uncured Properties—The following test methods may
biological safety and tissue reactions are described in Practice
be conducted on the uncured mixed formulation or appropriate
F 748 which recommends generic biological test methods for
components:
materials and devices according to end use applications.
5.1.1 Peak Exotherm Temperature—Test Method D 2471.
5.3.13 Moisture Vapor Transmission—Test Methods E 96.
5.1.2 Gel Time—Test Method D 2471. 5.3.14 Prothrombin Time—The effect of the material on
5.1.3 Mix Ratio—The mix ratio shall be calculated and Prothrombin time shall be tested by appropriate methods.13
maintained at the ratio recommended by the manufacturer of 5.3.15 Specific Gravity—Test Methods D 792.
the formulation. 5.3.16 Stability (dimensional)—Test Method D 1042.
5.1.4 Viscosity—Test Method D 2393. 5.3.17 Stypven Time—The effect of the material on Stypven
5.2 Cured Properties (Required)—The following test meth- time shall be tested by appropriate methods.12
ods shall be conducted on the fully cured and properly 5.3.18 Surface Resistivity—Test Methods D 257.
conditioned material. 5.3.19 Tangent Modulus—Test Method D 638.
5.2.1 Extraction—Practice F 619. 5.3.20 Tensile Strength—Test Method D 638.
5.2.2 Foreign Particles—Upon careful visual examination,
the epoxy plastic shall be free of any extraneous debris that
11
may adversely affect its safety, efficacy, or reliability. United States Pharmacopeia, XXIII, 1995, pp. 1783–1786.
12
Ibid, XXIII, 1995, pp. 1686–1690.
5.2.3 Hydrolytic Stability—Practice F 74 or Test Method 13
Human Blood Coagulation, Haemostasis, and Thrombosis, Rosemary Biggs,
D 3137. ed., Blackwell Scientific Publications, 1972.

3
 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

F 602
5.3.21 Visual Defects—Practice D 2562. and handling precautions for each component and shall bear
5.3.22 Voids—Test Method D 2734. appropriate lot numbers.
5.3.23 Volume Resistivity—Test Method D 257.
8. Packaging
6. Identification
6.1 The following analytical methods may be used to 8.1 Packaging shall provide appropriate protection for the
characterize the materials: compound(s).
6.1.1 Infrared spectroscopy.
6.1.2 Spectrographic analysis. 9. Keywords
6.1.3 X-ray emission or diffraction. 9.1 epoxy (EP) plastics-surgical implants; plastics (thermo-
7. Marking setting); plastic surgical devices/applications; polymers-
surgical applications; resins-epoxy
7.1 The labels shall bear appropriate statements as to safety

APPENDIXES

(Nonmandatory Information)

X1. RATIONALE

X1.1 This document provides definitions and a standard developing more specific specifications for implantable devices
description for thermoset epoxy plastics based on diglycidyl containing epoxy resins with values and limits covering
ethers of bisphenol A and appropriate curing agents and end-use applications. This document should also help the
catalysts, compositions which are used in the manufacture of fabricator to select ingredients for the medical device that
implantable devices. The guide enumerates relevant test meth- ensure its biocompatibility.
ods and describes generic criteria which should assist in

X2. BIOCOMPATIBILITY

X2.1 The suitability of these materials from a human body. However, long-term clinical experience of use of specific
implant perspective is dependent on the specific application. compositions and formulations of this material class referred to
The biologic tests appropriate for the specific site, such as in this standard has shown that an acceptable level of biological
recommended in Practice F 748 should be used as a guideline. response can be expected, if the material is used in appropriate
applications.
X2.2 No known surgical implant material has ever been
shown to be completely free of adverse reactions in the human

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