Designation: F641 – 09

Standard Specification for

Implantable Epoxy Electronic Encapsulants1
This standard is issued under the fixed designation F641; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope D149 Test Method for Dielectric Breakdown Voltage and

1.1 This specification covers thermoset plastics based on Dielectric Strength of Solid Electrical Insulating Materials
diglycidyl ethers of bisphenol A and amino functional curing at Commercial Power Frequencies
agents or amine catalysts. D150 Test Methods for AC Loss Characteristics and Per-
1.2 The epoxy encapsulants covered by this specification mittivity (Dielectric Constant) of Solid Electrical Insula-
are intended to provide a tissue-compatible protective covering tion
for implantable medical devices such as pulse generators, D257 Test Methods for DC Resistance or Conductance of
telemetry devices and RF receivers. The biocompatibility of Insulating Materials
epoxy plastics has not been established. Epoxy plastic is a D570 Test Method for Water Absorption of Plastics
generic term relating to the class of polymers formed from D638 Test Method for Tensile Properties of Plastics
epoxy resins, certain curing agents or catalysts and various D790 Test Methods for Flexural Properties of Unreinforced
additives. Since many compositions and formulations fall and Reinforced Plastics and Electrical Insulating Materials
under this category, it is essential that the fabricator assure D1042 Test Method for Linear Dimensional Changes of
safety of implantability of the specific composition or formu- Plastics Under Accelerated Service Conditions
lation for the intended use by current state-of-the-art test D1239 Test Method for Resistance of Plastic Films to
methods. This specification can be used as a basis for stan- Extraction by Chemicals
dardized evaluation of biocompatibility for such implantable D1434 Test Method for Determining Gas Permeability
encapsulants. Characteristics of Plastic Film and Sheeting
1.3 The encapsulants covered by this specification are for D2240 Test Method for Rubber Property—Durometer
use in devices intended as long-term implants. Hardness
1.4 Limitations—This specification covers only the initial D2471 Practice for Gel Time and Peak Exothermic Tem-
qualification of epoxy encapsulants for implantable electronic perature of Reacting Thermosetting Resins3
circuitry. Some of the requirements are not applicable to D2562 Practice for Classifying Visual Defects in Parts
routine lot-to-lot quality control. Molded from Reinforced Thermosetting Plastics
1.5 The values stated in SI units are to be regarded as D2566 Test Method for Linear Shrinkage of Cured Ther-
standard. No other units of measurement are included in this mosetting Casting Resins During Cure3
standard. D2734 Test Methods for Void Content of Reinforced Plas-
1.6 This standard does not purport to address all of the tics
safety concerns, if any, associated with its use. It is the D3137 Test Method for Rubber Property—Hydrolytic Sta-
responsibility of the user of this standard to establish appro- bility
priate safety and health practices and determine the applica- F74 Practice for Determining Hydrolytic Stability of Plastic
bility of regulatory limitations prior to use. Encapsulants for Electronic Devices3
F135 Test Method for Embedment Stress Caused by Cast-
2. Referenced Documents ing Compounds on Glass-Encased Electronic Components3
2.1 ASTM Standards:2 F602 Criteria for Implantable Thermoset Epoxy Plastics
F748 Practice for Selecting Generic Biological Test Meth-
ods for Materials and Devices
1
This specification is under the jurisdiction of ASTM Committee F04 on F895 Test Method for Agar Diffusion Cell Culture Screen-
Medical and Surgical Materials and Devices and is the direct responsibility of
ing for Cytotoxicity
Subcommittee F04.11 on Polymeric Materials.
Current edition approved Aug. 1, 2009. Published September 2009. Originally F981 Practice for Assessment of Compatibility of Biomate-
approved in 1979. Last previous edition approved in 2003 as F641 – 98a(2003). rials for Surgical Implants with Respect to Effect of
DOI: 10.1520/F0641-09. Materials on Muscle and Bone
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
3
the ASTM website. Withdrawn.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 F641 – 09
2.2 AAMI Standard: 5.1.2.2 Foreign Particles—No foreign particles, particulate
EOS-D E-O Sterilization Standard4 matter, or gross contamination shall be observed when checked
2.3 ISO Standard: under 23 wide field magnification.
ISO 10993 Biological Evaluation of Medical Devices5 5.1.2.3 Biocompatibility Testing—While cell culture meth-
ods as described in Test Method F895 may be appropriate for
3. Classification the lot-to-lot screening of fully cured specimens, the basic
3.1 Encapsulants shall be classified as follows: recipe used should have been qualified for its overall tissue
3.1.1 Type I—Those encapsulants which contact the tissue response by methods such as those suggested in Practice F748
directly or indirectly. or ISO 10993 for the intended application, including testing
3.1.2 Type II—Those encapsulants used only within her- according to Practice F981.
metically sealed containers. The epoxy encapsulant has no (1) Biocompatibility testing should be performed on speci-
contact with tissues or physiological fluids. mens that have been processed and sterilized per the methods
intended for the final device.
4. Chemical Composition
5.1.2.4 USP Bacterial Endotoxin Test6 or other Pyrogen
4.1 Additives (Type I Encapsulants Only): methods which have been demonstrated to be of equal or
4.1.1 Reactive Diluents—The following compounds when greater sensitivity—Pass.
used as reactive diluents shall not be used in concentrations 5.1.2.5 Sterilant Residues (AAMI EOS-D)—Where appli-
greater than 12 parts per hundred resin (phr). cable, the concentration of ethylene oxide, ethylene chlorohy-
4.1.1.1 Butyl glycidyl ether (BGE). drin, ethylene glycol, and dichlorodifluoromethane (or the
4.1.1.2 Phenyl glycidyl ether (PGE). equivalents) at the time of implantation shall be shown to be
4.1.2 Other Additives (see Note 1)—Other additives shall be within safe limits prescribed by the device manufacturer.
shown to be nonextractable in 37°C physiological saline for the 5.1.2.6 The cure shrinkage (Test Method D2566) or embed-
device design life in concentrations sufficient to significantly ment stress (Test Method F135) shall be #2%. The stress shall
affect the properties of the encapsulant or to produce a not exceed the limits of the most pressure-sensitive compo-
significant biological reaction. nents.
NOTE 1—Other additives, as indicated in Criteria F602, include com- 5.1.2.7 Tissue Culture Test (Agar Overlay)7 or Test Method
pounds such as nonreactive diluents, fillers, release agents, and the like. F895—Pass.
4.1.3 Phthalate Esters—Phthalate esters such as dibutyl 5.1.3 Required Cured Properties Measured in Long-Term
phthalate shall not be used in concentrations $10 phr. Immersion Tests for Type I Encapsulants—The property values
4.2 Mix Ratios (Type I and Type II Encapsulants): prescribed in Table 1 shall be obtained at 22 6 3°C and 50 6
4.2.1 Amines—The mix ratio shall be maintained at 65 10 % relative humidity on specimens conditioned as in 6.3.
equivalent % of stoichiometry. Samples shall be wiped dry prior to test with a lint-free tissue,
4.2.2 Catalysts—The mix ratio shall be maintained within as appropriate.
the ranges recommended by the formulator. 5.1.4 Optional cured properties measured after accelerated
4.3 Carbonates (Type I and Type II Encapsulants)—The immersion for Type I encapsulants may be determined for
encapsulant shall be poured under conditions such that the screening purposes after conditioning as in 6.2.
formation of amine carbonates is minimized. The device 5.2 Type II Encapsulants:
manufacturer may specify maximum limits for carbon dioxide 5.2.1 Peak Exotherm Temperature (Test Method D2471)—
or water vapor, or both, in the atmosphere in which the The peak exotherm temperature during cure shall be kept
encapsulant is being mixed or poured. below the maximum acceptable value for the lowest tempera-
ture rated component of the device.
5. Physical Properties 5.2.2 The property values prescribed in Table 2 shall be
5.1 Type I Encapsulants: determined at 22 6 3°C and 50 6 10 % relative humidity on
5.1.1 Peak Exotherm Temperature (Test Method D2471)— fully cured samples conditioned as in 6.1.
The peak exotherm temperature during cure shall be kept
below the maximum acceptable value for the lowest tempera- 6. Specimen Preparation
ture rated component of the device. 6.1 Preparation—Prepare specimens used for evaluation of
5.1.2 Fully Cured Specimens—The required properties properties of the cured material in the same manner as the
measured on fully cured specimens conditioned as in 6.1 are as intended product. Such conditioning shall include all specified
follows: relevant variables for the product prior to implantation, includ-
5.1.2.1 Transparency—In cases where no fillers or rein- ing specimen size or shape, cure time, cure temperature,
forcements are used, the encapsulant shall have sufficient post-cure, cleaning, packaging, sterilization, and aeration.
transparency so that the circuitry may be visually inspected 6.2 Accelerated Immersion:
after encapsulation.

4 6
Available from Association for Advancement of Medical Instrumentation, 1500 U.S. Pharmacopeia, USP-NF, <85>, available from U.S. Pharmacopeia (USP),
Wilson Blvd., Suite 417, Arlington, VA 22209. 12601 Twinbrook Pkwy., Rockville, MD 20852-1790, http://www.usp.org.
5 7
Available from American National Standards Institute (ANSI), 25 W. 43rd St., Guess, W. L., et al., Journal of Pharmaceutical Sciences , Vol 54, 1965, pp.
4th Floor, New York, NY 10036, http://www.ansi.org. 1545–1547.

2
 F641 – 09
TABLE 1 Cure Requirements for Long-Term Immersion Tests for Type I Encapsulants
Property Requirement ASTM Method
Extraction <1 % in water D1239
Water absorption #4 % D570
Dielectric strength >11.8 kV/mm D149
Dielectric constant >2.0 D150
Dissipation factor <0.05 D150
Elongation >1.5 % D638
Flexural strength $1380 MPa D790
A
Gas permeation D1434
Hardness $60 Shore D D2240
Dimensional stability <0.5 % change D1042
Tangent modulus $1380 MPa D638
Tensile strength (with outgassing power $55 MPa D638
sources)
Tensile strength (without outgassing power $7 MPa D638
sources)
Visual defects none that adversely affect the safety, efficacy, or reliability of D2562
the device
Voids none that adversely affect the safety, efficacy, or reliability of D2734
the device
Volume resistivity 1010V· cm D257
A
For those devices containing gas-evolving power sources, the hydrogen permeation coefficient shall be 1.18 3 10 [(STP)(cm )(mm)/(atm)(day)(cm2)]; or the
−3 3

encapsulant shall allow the escape of 0.06 cm3 of hydrogen per cell day; or provision shall be made to ensure that gaseous material evolving from the power sources will
be adequately disposed of in such a manner that the encapsulant is not comprised.

TABLE 2 Cure Requirements for Long-Term Immersion Tests for Type II Encapsulants
Property Requirement ASTM Method
Foreign particles none visible ...
Cure shrinkage or embedment #2 % D2566 or F135,
stress respectively
Dielectric constant >2.0 D150
Dielectric strength >11.8 kV/mm D149
Dissipation factor <0.05 D150
Dimensional stability <0.5 % change D1042
Visual defects none that adversely affect the safety, efficacy, or reliability of D2562
the device
Voids none that adversely affect the safety, efficacy, or reliability of D2734
the device
Volume resistivity 1010V·cm D257

6.2.1 For screening purposes, immerse specimens prepared device’s projected service life before one can claim compliance
as in 6.1 in refluxing physiological saline of pH 7.4 6 0.2 for with the specification. One shall be considered in compliance
7 days. with this section of the specification, therefore, if specimens
6.2.2 Prior to evaluation, allow the specimens to equilibrate meet the requirements of 5.4 after 1 year’s immersion.
to the test temperature of 22 6 3°C in physiological saline of 6.3.3 Store controls at 22 6 3°C and 50 6 10 % relative
pH 7.4 6 0.2. humidity.
6.2.3 Condition one set of controls at 100 6 3°C and
another set at 22 6 3°C for 7 days at 50 6 10 % relative 7. Inspection
humidity. 7.1 As a minimum, the following methods shall be used to
6.2.4 Since two variables, heat and moisture, are inherent in characterize the formulation prior to mixing:
this test, data from specimens refluxed 7 days in saline may be 7.1.1 Infrared spectroscopy on each component.
compared to controls conditioned dry at 100°C and at 22°C.
7.1.2 Amine number on curing agent.
Thus, one may estimate the long-term effects of moisture as
7.1.3 Epoxide equivalent weight on resin.
opposed to the effects of moisture and heat or heat alone.
7.2 As a minimum, the following methods shall be used to
6.3 Long-Term Immersion (Test Method D3137 or Practice
characterize the “mixed” or “hardened” polymer:
F74):
7.2.1 Infrared spectroscopy.
6.3.1 Prepare the specimens in accordance with 6.1.
6.3.2 During initial qualification of the formulation, im- 7.2.2 Spectrographic analysis.
merse specimens in 37 6 3°C aerated physiological saline of 7.2.3 Total nitrogen.
pH 7.4 6 0.2 with periodic sampling for evaluation as is
appropriate for a period of time consistent with projected 8. Packaging and Package Marking
service life. Immersion shall continue for the projected service 8.1 Packaging shall bear appropriate lot numbers that di-
life of the device. For devices intended for long-term implant, rectly relate to the identification of the homogeneous batches
however, it may not be practical to complete tank tests over the which are the source of the encapsulant.

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 F641 – 09
8.2 Packaging shall provide appropriate protection for the
epoxy components of the device.
9. Keywords
9.1 encapsulants; evaluation of biocompatibility; implant-
able medical devices

APPENDIXES

(Nonmandatory Information)

X1. RATIONALE

X1.1 Epoxies as a general class of thermoset polymers may ever changes are made in the formulation of an encapsulant,
exhibit a wide range of properties, depending upon the formu- the possibility exists that there may be changes in the tissue
lation. This specification is intended to describe minimum response. This specification therefore calls for requalification
requirements for materials for use as encapsulants in implant- of different formulations to assure no adverse effects on the
able electronic components. It remains the responsibility of the tissue response while allowing for cell culture screening
device manufacturer to determine whether the particular for- batch-to-batch. This specification does not attempt to address
mulation utilized meets other specific requirements of the the amount of change in formulation which would necessitate
particular end-use application. re-testing. The material and device manufacturers will need to
make that determination based upon their own experience,
X1.2 Epoxy encapsulants have been used in the manufac-
published data, and consultations with experts experienced in
ture of implantable electronic components for many years and
this area.
have been found to exhibit acceptable tissue response. When-

X2. BIOCOMPATIBILITY

X2.1 The suitability of these materials from a human shown to be completely free of adverse reactions in the human
implant perspective is dependent on the specific application. body. However, long-term clinical experience of use of specific
The biologic tests appropriate for the specific site, such as compositions and formulations of this material class referred to
recommended in Practice F748 or ISO 10993 should be used as in this standard has shown that an acceptable level of biological
a guideline. response can be expected, if the material is used in appropriate
X2.2 No known surgical implant material has ever been applications.

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