ASTM F1538-03(2009)
(Specification)Standard Specification for Glass and Glass Ceramic Biomaterials for Implantation
Standard Specification for Glass and Glass Ceramic Biomaterials for Implantation
ABSTRACT
This specification covers the material requirements and characterization techniques for glass and glass-ceramic biomaterials intended for use as bulk porous or powdered surgical implants, or as coatings on surgical devices, but not including drug delivery systems. Glass and glass-ceramic biomaterials should be evaluated thoroughly for biocompatibility before human use. Tests shall be performed to determine the properties of the biomaterials, in accordance with the following test methods: bulk composition; density; flexural strength; Young's modulus; hardness; surface area; bond strength of glass or glass ceramic coating; crystallinity; thermal expansion; and particle size.
SCOPE
D
1.1 This specification covers the material requirements and characterization techniques for glass and glass-ceramic biomaterials intended for use as bulk porous or powdered surgical implants, or as coatings on surgical devices, but not including drug delivery systems.
1.2 The biological response to glass and glass-ceramic biomaterials in bone and soft tissue has been demonstrated in clinical use (1-12) and laboratory studies (13-17).
1.3 This specification excludes synthetic hydroxylapatite, hydroxylapatite coatings, aluminum oxide ceramics, alpha- and beta-tricalcium phosphate, and whitlockite.
1.4 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central nervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.
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Designation:F1538 −03 (Reapproved 2009)
Standard Specification for
Glass and Glass Ceramic Biomaterials for Implantation
This standard is issued under the fixed designation F1538; 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 Apparent Porosity, andApparent Specific Gravity of Fired
Whiteware Products
1.1 This specification covers the material requirements and
C623 Test Method for Young’s Modulus, Shear Modulus,
characterization techniques for glass and glass-ceramic bioma-
and Poisson’s Ratio for Glass and Glass-Ceramics by
terials intended for use as bulk porous or powdered surgical
Resonance
implants, or as coatings on surgical devices, but not including
C633 Test Method for Adhesion or Cohesion Strength of
drug delivery systems.
Thermal Spray Coatings
1.2 The biological response to glass and glass-ceramic
C693 Test Method for Density of Glass by Buoyancy
biomaterials in bone and soft tissue has been demonstrated in
C729 Test Method for Density of Glass by the Sink-Float
clinical use (1-12) and laboratory studies (13-17).
Comparator
1.3 This specification excludes synthetic hydroxylapatite, C730 Test Method for Knoop Indentation Hardness of Glass
C958 Test Method for Particle Size Distribution ofAlumina
hydroxylapatitecoatings,aluminumoxideceramics,alpha-and
beta-tricalcium phosphate, and whitlockite. or Quartz by X-Ray Monitoring of Gravity Sedimentation
C1069 Test Method for Specific SurfaceArea ofAlumina or
1.4 Warning—Mercury has been designated by EPA and
Quartz by Nitrogen Adsorption
many state agencies as a hazardous material that can cause
C1070 Test Method for Determining Particle Size Distribu-
central nervous system, kidney, and liver damage. Mercury, or
tion of Alumina or Quartz by Laser Light Scattering
its vapor, may be hazardous to health and corrosive to
E228 Test Method for Linear Thermal Expansion of Solid
materials.Cautionshouldbetakenwhenhandlingmercuryand
Materials With a Push-Rod Dilatometer
mercury-containing products. See the applicable product Ma-
F748 PracticeforSelectingGenericBiologicalTestMethods
terial Safety Data Sheet (MSDS) for details and EPA’s website
for Materials and Devices
(http://www.epa.gov/mercury/faq.htm) for additional informa-
F981 Practice for Assessment of Compatibility of Biomate-
tion. Users should be aware that selling mercury or mercury-
rials for Surgical Implants with Respect to Effect of
containingproducts,orboth,inyourstatemaybeprohibitedby
Materials on Muscle and Bone
state law.
2.2 Code of Federal Regulations:
Title 21, Part 820
2. Referenced Documents
2.3 United States Pharmacopoeia:
2.1 ASTM Standards:
Lead <252>
C158 Test Methods for Strength of Glass by Flexure (De-
Mercury <261>
termination of Modulus of Rupture)
Arsenic <211>
C169 Test Methods for Chemical Analysis of Soda-Lime
Heavy Metals <231> Method I
and Borosilicate Glass 6
2.4 U.S. Geological Survey Method:
C373 Test Method for Water Absorption, Bulk Density,
Cadmium
3. Terminology
This specification is under the jurisdiction of ASTM Committee F04 on
3.1 Definitions of Terms Specific to This Standard:
Medical and Surgical Materials and Devices and is the direct responsibility of
Subcommittee F04.13 on Ceramic Materials.
Current edition approved April 1, 2009. Published April 2009. Originally AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
´1
approved in 1994. Last previous edition approved in 2003 as F1538 – 03 . DOI: 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
10.1520/F1538-03R09. www.access.gpo.gov.
2 5
The boldface numbers in parentheses refer to the list of references at the end of Available from U.S. Pharmacopeia (USP), 12601Twinbrook Pkwy., Rockville,
this specification. MD 20852-1790, http://www.usp.org.
3 6
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Crock, J.G., Felichte, F.E., Briggs, P.H., “Determination of Elements in
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM National Bureau of Standards Geological Reference Materials SRM 278 Obsidian
Standards volume information, refer to the standard’s Document Summary page on and SRM 688 Basalt by Inductively Coupled Plasma-Atomic Emission
the ASTM website. Spectrometry,” Geostandards Newsletter, Vol 7, 1983, pp. 335–340.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1538−03 (2009)
3.1.1 bioactive glass—an amorphous silicate-based solid 5.1.2 Flexural Strength—When used as bulk materials in
that is not intrinsically adhesive and that is capable of forming load bearing applications, the flexural strength of the bulk
acohesivebondwithbothhardandsofttissuewhenimplanted, material shall be measured using Test Methods C158.
and will develop a hydroxycarbonate apatite layer when 5.1.3 Young’s Modulus—When used as a bulk material,
exposed to appropriate in vitro environments, such as simu- Young’s Modulus of glass and glass ceramic biomaterials shall
lated body fluid or tris-hydroxymethylaminomethane buffer. be determined following Test Method C623.
5.1.4 Hardness—Where applicable, for characterization of
3.1.2 bioactive glass-ceramic—an amorphous-derived crys-
the material, the hardness of bulk samples shall be determined
talline silicate-based solid that is not intrinsically adhesive and
using Test Method C730. The Knoop indentation hardness is
that is capable of forming a cohesive bond with bone and soft
one of many properties that is used to characterize glasses.
tissue when implanted, and will develop a hydroxycarbonate
Attempts have been made to relate Knoop hardness to tensile
apatite layer when exposed to appropriate in vitro
strength,butnogenerallyacceptedmethodsareavailable.Such
environments, such as simulated body fluid or tris-
conversionislimitedinscopeandshouldbeusedwithcaution,
hydroxymethylaminomethane buffer.
exceptforspecialcasesinwhichareliablebasisforconversion
3.1.3 bulk material—intended to describe a unit material
has been obtained by conversion tests.
used as a load bearing implant.
5.1.5 Surface Area—The surface area of a particulate may
3.1.4 coating—intended to describe a surface layer that is
be important in determining the reliability of the bioactivity of
relatively thin compared to the overall dimensions of the
the material.Whenever the specific surface area of the material
prosthetic part that has been coated.
relates to function, the surface area of particulate glass and
glass ceramic biomaterials shall be measured using Test
3.1.5 glass biomaterial—any one of a number of composi-
tions of amorphous inorganic solids that are used as implant Method C1069.
5.1.6 Bond Strength of Glass or Glass Ceramic Coating—
materials for various medical or dental uses, or both.
When used as a coating on a metallic or ceramic substrate, the
3.1.6 glass-ceramic biomaterials—any one of a number of
bond strength of the coating shall be measured following Test
compositions of an amorphous-derived crystalline solid that is
Method C633.
usedasanimplantablebiomaterialformedicalordentaluse,or
5.1.7 Crystallinity—For glass-ceramic biomaterials, the per-
both.
cent crystallinity and crystal phases present in glass ceramic
3.1.7 particulate material—intended to describe several
biomaterials shall be determined by means of X-ray diffraction
pieces (usually small size) used together within an implant
analysis. While there is no single standard method for deter-
construct.
mining the crystallinity and crystal phases of glass ceramic
materials, techniques such as those detailed in Refs (19) and
4. Chemical Requirements
(20) should be followed to standardize methods as much as
4.1 Bulk compositions shall be tested using Test Method
possible.
C169. 5.1.8 Thermal Expansion—Thermal expansion shall be
measured using Test Method E228, when materials are to be
4.2 The concentration of trace element levels in the bioac-
used for coatings (raw materials are to be measured), or on
tive glass and glass-ceramics shall be limited as follows:
finished product as a quality control test.
Element ppm, max
5.1.9 Particle Size—When used as a particulate, the particle
Arsenic (As) 3
Cadmium (Cd) 5 size shall be measured in accordance with Test Methods C958
Mercury (Hg) 5
or C1070.
Lead (Pb) 30
total heavy metals (as lead) 50
6. Biocompatibility
Either inductively-coupled plasma/mass spectroscopy (ICP/
6.1 Glass and glass-ceramic biomaterials should be evalu-
MS) (18), atomic absoprtion (AAS), or the methods listed in
ated thoroughly for biocompatibility before human use. Bio-
2.3 and 2.4 shall be used.
active glass and glass-ceramic materials are unique in their
mode of action when implanted in the body due to the released
5. Physical Characterization
ionic species and the mechanisms by which these materials
5.1 The following physical and mechanical characteriza-
bond w
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:F1538–94 Designation: F 1538 – 03 (Reapproved 2009)
Standard Specification for
Glass and Glass Ceramic Biomaterials for Implantation
This standard is issued under the fixed designation F 1538; 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
1.1 This specification covers the material requirements and characterization techniques for glass and glass-ceramic biomaterials
intended for use as bulk porous or powdered surgical implants, or as coatings on surgical devices, but not including drug delivery
systems.
1.2 The biological response to glass and glass-ceramic biomaterials in bone and soft tissue has been demonstrated in clinical
use (1-91-12) and laboratory studies 10-14. and laboratory studies (13-17).
1.3 This specification excludes synthetic hydroxylapatite, hydroxylapatite coatings, aluminum oxide ceramics, alpha- and
beta-tricalcium phosphate, and whitlockite.
1.4 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central
nervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution
should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet
(MSDS) for details and EPA’s website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware
that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.
2. Referenced Documents
2.1 ASTM Standards:
C 158 Method for Flexural Testing of Glass (Determination of Modulus of Rupture) Test Methods for Strength of Glass by
Flexure (Determination of Modulus of Rupture)
C 169 Test Methods for Chemical Analysis of Soda-Lime and Borosilicate Glass
C 373 Test Method for WaterAbsorption, Bulk Density,Apparent Porosity, andApparent Specific Gravity of Fired Whiteware
Products
C 623 Test Method for Young’s Modulus, Shear Modulus, and Poisson’s Ratio for Glass and Glass-Ceramics by Resonance
C 633 Test Method for Adhesion or CohesiveCohesion Strength of Flame-Sprayed Thermal Spray Coatings
C 693 Test Method for Density of Glass by Buoyancy
C 729 Test Method for Density of Glass by the Sink-Float Comparator
C 730 Test Method for Knoop Indentation Hardness of Glass
C958Method for Determination of Particle Size Distribution of Alumina or Quartz by X-Ray Monitoring of Gravity
Sedimentation Test Method for Knoop Indentation Hardness of Glass
C 958 Test Method for Particle Size Distribution of Alumina or Quartz by X-Ray Monitoring of Gravity Sedimentation
C 1069 Method for Specific Surface Area of Alumina or Quartz by Nitrogen Adsorption
C1070Test Method for Determining Particle Size Distribution ofAlumina or Quartz by Laser Light Scattering Test Method for
Specific Surface Area of Alumina or Quartz by Nitrogen Adsorption
C 1070 Test Method for Determining Particle Size Distribution of Alumina or Quartz by Laser Light Scattering
E 228 Test Method for Linear Thermal Expansion of Solid Materials withWith a Vitreous Silica Push-Rod Dilatometer
F 748 Practice for Selecting Generic Biological Test Methods for Materials and Devices Practice for Selecting Generic
Biological Test Methods for Materials and Devices
F 981 Practice for Assessment of Compatibility of Biomaterials for Surgical Implants with Respect to Effect of Materials on
Muscle and Bone
This specification is under the jurisdiction ofASTM Committee F-4 F04 on Medical and Surgical Materials and Devices and is the direct responsibility of Subcommittee
F04.13 on Ceramic Materials.
Current edition approved Dec. 15, 1994. Published February 1995.
´1
Current edition approved April 1, 2009. Published April 2009. Originally approved in 1994. Last previous edition approved in 2003 as F 1538 – 03 .
The boldface numbers in parentheses refer to the list of references at the end of this specification.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 15.02.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
F 1538 – 03 (2009)
2.2 Code of Federal Regulations:
Title 21, Part 820
2.3 United States Pharmacopoeia:
Lead <252>
Mercury <261>
Arsenic <211>
Heavy Metals <231>Method found in Annual Book of ASTM Standards, vol 13.01.
2.4 U.S. Geological Survey Method:
(7) Cadmium
Heavy Metals <231> Method I
2.4 U.S. Geological Survey Method:
Cadmium
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 bioactive glass—an amorphous solid that is not intrinsically adhesive and that is capable of forming a cohesive bond with
both hard and soft tissue when exposed to appropriate in vivo or in vitro environments, such as simulated body fluid or
tris-hydroxymethylaminomethane buffer, by developing a surface layer of hydroxycarbonate apatite by release of ionic species
from the bulk material. —an amorphous silicate-based solid that is not intrinsically adhesive and that is capable of forming a
cohesive bond with both hard and soft tissue when implanted, and will develop a hydroxycarbonate apatite layer when exposed
to appropriate in vitro environments, such as simulated body fluid or tris-hydroxymethylaminomethane buffer.
3.1.2 bioactive glass-ceramic—an amorphous-derived crystalline solid that is not intrinsically adhesive and that is capable of
formingacohesivebondwithboneandsofttissuewhenexposedtoappropriateinvivoorinvitroenvironments,suchassimulated
body fluid or tris-hydroxymethylaminomethane buffer, by developing a surface layer of hydroxycarbonate apatite by release of
ionic species from the bulk material. —an amorphous-derived crystalline silicate-based solid that is not intrinsically adhesive and
that is capable of forming a cohesive bond with bone and soft tissue when implanted, and will develop a hydroxycarbonate apatite
layer when exposed to appropriate in vitro environments, such as simulated body fluid or tris-hydroxymethylaminomethane buffer.
3.1.3 bulk material—intended to describe a unit material used as a load bearing implant.
3.1.4 coating—intended to describe a surface layer that is relatively thin compared to the overall dimensions of the prosthetic
part that has been coated.
3.1.5 glass biomaterial—any one of a number of compositions of amorphous inorganic solids that are used as implant materials
for various medical or dental uses, or both.
3.1.6 glass-ceramic biomaterials—any one of a number of compositions of an amorphous-derived crystalline solid that is used
as an implantable biomaterial for medical or dental use, or both.
3.1.7 particulate material—intended to describe several pieces (usually small size) used together within an implant construct.
4. Chemical Requirements
4.1 Bulk compositions shall be tested using Test Method C 169.
4.2 The concentration of heavy metalstrace element levels in the bioactive glass and glass-ceramics shall be limited as follows:
Element ppm, max
As 3
Arsenic (As) 3
Cd 5
Cadmium (Cd) 5
Hg 5
Mercury (Hg) 5
Pb 30
Lead (Pb) 30
total heavy metals (as lead) 50
For referee purposes, the methods listed in 2.2 and
Either inductively-coupled plasma/mass spectroscopy (ICP/MS) (18), atomic absoprtion (AAS), or the methods listed in 2.3 and
2.4 shall be used.
Annual Book of ASTM Standards, Vol 02.05.
Available 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.
Annual Book of ASTM Standards, Vols 03.01 and 14.02.
Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville, MD 20852-1790, http://www.usp.org.
Annual Book of ASTM Standards, Vol 13.01.
Crock, J.G., Felichte, F.E., Briggs, P.H., “Determination of Elements in National Bureau of Standards Geological Reference Materials SRM 278 Obsidian and SRM 688
Basalt by Inductively Coupled Plasma-Atomic Emission Spectrometry,” Geostandards Newsletter, Vol 7, 1983, pp. 335–340.
F 1538 – 03 (2009)
5. Physical Characterization
5.1 The following physical and mechanical characterizations may be applicable to various bioactive glass and glass-ceramics
products and should be used whenever possible to verify the material.
5.1.1 Density—The densities of glass and glass ceramic materials are related directly to the processing history and composition
of the material. The density of the bulk material shall be measured using Test Methods C 373 or C 729and shall be consistent for
the specific materials.
NOTE 1—Thistestshoulduseanon-aqueousliquidforbioactiveglassandglassceramicmaterials,whichareknowntoreactinanaqueousenvironment
and could thereby affect the measurement.
5.1.2 Flexural Strength—When used as bulk materials in load bearing applications, the flexural strength of the bulk material
shall be measured using Test Methods C 158.
5.1.3 Young’s Modulus— When used as a bulk material, Young’s Modulus of glass and glass ceramic biomaterials shall be
determined following Test Method C 623.
5.1.4 Hardness—Where applicable, for characterization of the material, the hardness of bulk samples shall be determined using
Test Method C 730.The knoopKnoop indentation hardness is one of many properties that is used to characterize glasses.Attempts
have been made to relate knoopKnoop hardness to tensile strength, but no generally accepted methods are available. Such
conversion is limited in scope and should be used with caution, except for special cases in which a reliable basis for conversion
has been obtained by conversion tests.
5.1.5 Surface Area— The surface area of a particulate may be important in determining the reliability of the bioactivity of the
material. Whenever the specific surface area of the material relates to function, the surface area of particulate glass and glass
ceramic biomaterials shall be measured using Test Method C 1069.
5.1.6 Bond Strength of Glass or Glass Ceramic Coating—When used as a coating on a metallic or ceramic substrate, the bond
strength of the coating shall be measured following Test Method C 633.
5.1.7 Crystallinity— For glass-ceramic biomaterials, the percent crystallinity and crystal phases present in glass ceramic
biomaterials shall be determined by means of X-ray diffraction analysis. While there is no single standard method for determining
the crystallinity and crystal phases of glass ceramic materials, techniques such as those detailed in reference 10.16Refs (19) and
10.17(20) should be followed to standardize methods as much as possible.
5.1.8 Thermal Expansion—Thermal expansion shall be measured using Test Method E 228, when materials are to be used for
coatings (raw materials are to be measured), or on finished product as a quality control test.
5.1.9 Particle Size— When used as a particulate, the particle size shall be measured in accordance with Test Methods C 958
or C 1070.
6. Biocompatibility
6.1 Glassandglass-ceramicbiomaterialsshouldbeevaluatedthoroughlyforbiocompatibilitybeforehumanuse.Bioactiveglass
and glass-ceramic materials are unique in their mode of action when implanted in the body due to the released ionic species and
the mechanisms by which these materials bond with bony tissue. These materials have been found to exhibit an excellent tissue
response in laboratory studies (10-1413-17) and clinical usage (1-71-12). Before any new formulations are used clinically, the
tissue response should be characterized by the methods recommended in Practice F 748. and F 981 as appropriate.
7. Test Specimen Fabrication
7.1 Test specimens should be prepared concurrent with implant devices, as well as from the same batch of material and by the
same processes as those used in fabricating the glass and glass-ceramic implant device.
8. Quality Program Requirement
8.1The manufacturer shall conform to good manufacturing practices (2.1) or its equivalent.
8.1 The manufacturer shall conform to Quality Systems requirements (2.2) or equivalent.
9. Keywords
9.1 bioactive glass; bioactive glass-ceramics; glass biomaterials; glass-ceramic biomaterial; —surgicalsurgical implants
APPENDIXES
(Nonmandatory Information)
X1. RATIONALE
X1.1 Anumberofglass-ceramicmaterialsareavailablecommercially.Bioactiveglassandglass-ceramicmaterialsareavailable
commercially as synthetic graft materials for maintenance of the alveolar ridge; as devices for spinal fushion;fusion; as implants
for replacement of the vertebral body, iliac crest, and ossicular chain of the middle ear; as bone filler to substitute for bone defects
F 1538 – 03 (2009)
remaining after the excision of bone tumors and extraction of loosened joint prostheses; and as coatings on dental and orthopedic
implants. As with any implant material, the bioresponse is critically dependent on the material properties. To achieve reliable
biocompatibility, these properties must be known and consistent. This specification provides specifications for biocompatible
grades of bioactive glass and glass-ceramics.
X1.2 In order to be called bioactive, the materials must demonstrate that living tissue is bonding to a significantly higher level
than non-bonding implant control, as well as demonstrate that ionic species are released from the material into solution in a
controlled and reproducible manner.
X1.3 Bioactive glass and glass-ceramic materials are generally silicate-based materials, with additions of oxides of calcium,
phosphorous, and various alkalis. They may be phosphate-based materials as well. These materials may also include fluoride and
other alkaline earth metals. Table X1.1 gives a few specific examples of the bioactive glass and glass-ceramic materials produced.
Since the compositions of these materials may vary greatly from product to product, it is not possible to specify their exact
compositions.
X1.4 It is recognized that separate performance standards may be necessary for each end-use product. Physical and mechanical
properties were not specified for this reason. A source of
...
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