ASTM F1538-2003 Standard Specification for Glass and Glass Ceramic Biomaterials for Implantation《植入用玻璃和玻璃陶瓷生物材料标准规范》.pdf

1、Designation: F 1538 03Standard Specification forGlass and Glass Ceramic Biomaterials for Implantation1This standard is issued under the fixed designation F 1538; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revi

2、sion. 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 This specification covers the material requirements andcharacterization techniques for glass and glass-ceramic bioma-terials i

3、ntended for use as bulk porous or powdered surgicalimplants, or as coatings on surgical devices, but not includingdrug delivery systems.1.2 The biological response to glass and glass-ceramicbiomaterials in bone and soft tissue has been demonstrated inclinical use (1-12)2and laboratory studies (13-17

4、).1.3 This specification excludes synthetic hydroxylapatite,hydroxylapatite coatings, aluminum oxide ceramics, alpha- andbeta-tricalcium phosphate, and whitlockite.2. Referenced Documents2.1 ASTM Standards:C 158 Test Methods for Strength of Glass by Flexure(Determination of Modulus of Rupture)3C 169

5、 Test Method for Chemical Analysis of Soda-Limeand Borosilicate Glass3C 373 Test Method for Water Absorption, Bulk Density,Apparent Porosity, and Apparent Specific Gravity of FiredWhiteware Products3C 623 Test Method for Youngs Modulus, Shear Modulus,and Poissons Ratio for Glass and Glass-Ceramics b

6、yResonance3C 633 Test Method for Adhesion or Cohesive Strength ofThermal Sprayed Coatings4C 693 Test Method for Density of Glass by Buoyancy3C 729 Test Method for Density of Glass by the Sink-FloatComparator3C 730 Test Method for Knoop Indentation Hardness ofGlass3C 958 Test Method for Particle Size

7、 Distribution of Alu-mina or Quartz by X-Ray Monitoring of Gravity Sedimen-tation3C 1069 Test Method for Specific Surface Area of Aluminaor Quartz by Nitrogen Adsorption3C 1070 Test Method for Determining Particle Size Distri-bution of Alumina or Quartz by Laser Light Scattering3E 228 Test Method fo

8、r Linear Thermal Expansion of SolidMaterials with a Vitreous Silica Dilatometer5F 748 Practice for Selecting Generic Biological Test Meth-ods for Materials and Devices6F 981 Practice for Assessment of Compatibility of Bioma-terials for Surgical Implants with Respect to Effect ofMaterials on Muscle a

9、nd Bone62.2 Code of Federal Regulations:7Title 21, Part 8202.3 United States Pharmacopoeia:8Lead Mercury Arsenic Heavy Metals Method I2.4 U.S. Geological Survey Method:9Cadmium3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 bioactive glassan amorphous silicate-based solidthat

10、is not intrinsically adhesive and that is capable of forminga cohesive bond with both hard and soft tissue when implanted,and will develop a hydroxycarbonate apatite layer whenexposed to appropriate in vitro environments, such as simu-lated body fluid or tris-hydroxymethylaminomethane buffer.3.1.2 b

11、ioactive glass-ceramican amorphous-derived crys-talline silicate-based solid that is not intrinsically adhesive andthat is capable of forming a cohesive bond with bone and softtissue when implanted, and will develop a hydroxycarbonate1This specification is under the jurisdiction of ASTM Committee F0

12、4 onMedical and Surgical Materials and Devices and is the direct responsibility ofSubcommittee F04.13 on Ceramic Materials.Current edition approved Apr. 10, 2003. Published May 2003. Originallyapproved in 1994. Last previous edition approved in 1994 as F 1538 94.2The boldface numbers in parentheses

13、refer to the list of references at the end ofthis specification.3Annual Book of ASTM Standards, Vol 15.02.4Annual Book of ASTM Standards, Vol 02.05.5Annual Book of ASTM Standards, Vol 14.02.6Annual Book of ASTM Standards, Vol 13.01.7Available from U.S. Government Printing Office, Superintendent of D

14、ocu-ments, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.8Available from United Stated Pharmacopia, 12601 Twinbrook Parkway, Rock-ville, MD 20852.9Crock, J.G., Felichte, F.E., Briggs, P.H., “Determination of Elements inNational Bureau of Standards Geological Reference Materials SRM 27

15、8 Obsidianand SRM 688 Basalt by Inductively Coupled Plasma-Atomic Emission Spectrom-etry,” Geostandards Newsletter, Vol 7, 1983, pp. 335-340.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.apatite layer when exposed to appropriate in

16、 vitro environ-ments, such as simulated body fluid or tris-hydroxymethylaminomethane buffer.3.1.3 bulk materialintended to describe a unit materialused as a load bearing implant.3.1.4 coatingintended to describe a surface layer that isrelatively thin compared to the overall dimensions of theprosthet

17、ic part that has been coated.3.1.5 glass biomaterialany one of a number of composi-tions of amorphous inorganic solids that are used as implantmaterials for various medical or dental uses, or both.3.1.6 glass-ceramic biomaterialsany one of a number ofcompositions of an amorphous-derived crystalline

18、solid that isused as an implantable biomaterial for medical or dental use, orboth.3.1.7 particulate materialintended to describe severalpieces (usually small size) used together within an implantconstruct.4. Chemical Requirements4.1 Bulk compositions shall be tested using Test MethodC 169.4.2 The co

19、ncentration of trace element levels in the bioac-tive glass and glass-ceramics shall be limited as follows:Element ppm, maxArsenic (As) 3Cadmium (Cd) 5Mercury (Hg) 5Lead (Pb) 30total heavy metals (as lead) 50Either inductively-coupled plasma/mass spectroscopy (ICP/MS) (18), atomic absoprtion (AAS),

20、or the methods listed in2.3 and 2.4 shall be used.5. Physical Characterization5.1 The following physical and mechanical characteriza-tions may be applicable to various bioactive glass and glass-ceramics products and should be used whenever possible toverify the material.5.1.1 DensityThe densities of

21、 glass and glass ceramicmaterials are related directly to the processing history andcomposition of the material. The density of the bulk materialshall be measured using Test Methods C 373 or C 729 and shallbe consistent for the specific materials.NOTE 1This test should use a non-aqueous liquid for b

22、ioactive glassand glass ceramic materials, which are known to react in an aqueousenvironment and could thereby affect the measurement.5.1.2 Flexural StrengthWhen used as bulk materials inload bearing applications, the flexural strength of the bulkmaterial shall be measured using Test Methods C 158.5

23、.1.3 Youngs ModulusWhen used as a bulk material,Youngs Modulus of glass and glass ceramic biomaterials shallbe determined following Test Method C 623.5.1.4 HardnessWhere applicable, for characterization ofthe material, the hardness of bulk samples shall be determinedusing Test Method C 730. The Knoo

24、p indentation hardness isone of many properties that is used to characterize glasses.Attempts have been made to relate Knoop hardness to tensilestrength, but no generally accepted methods are available. Suchconversion is limited in scope and should be used with caution,except for special cases in wh

25、ich a reliable basis for conversionhas been obtained by conversion tests.5.1.5 Surface AreaThe surface area of a particulate maybe important in determining the reliability of the bioactivity ofthe material. Whenever the specific surface area of the materialrelates to function, the surface area of pa

26、rticulate glass andglass ceramic biomaterials shall be measured using TestMethod C 1069.5.1.6 Bond Strength of Glass or Glass Ceramic CoatingWhen used as a coating on a metallic or ceramic substrate, thebond strength of the coating shall be measured following TestMethod C 633.5.1.7 CrystallinityFor

27、glass-ceramic biomaterials, thepercent crystallinity and crystal phases present in glass ceramicbiomaterials shall be determined by means of X-ray diffractionanalysis. While there is no single standard method for deter-mining the crystallinity and crystal phases of glass ceramicmaterials, techniques

28、 such as those detailed in Refs (19) and(20) should be followed to standardize methods as much aspossible.5.1.8 Thermal ExpansionThermal expansion shall bemeasured using Test Method E 228, when materials are to beused for coatings (raw materials are to be measured), or onfinished product as a qualit

29、y control test.5.1.9 Particle SizeWhen used as a particulate, the particlesize shall be measured in accordance with Test Methods C 958or C 1070.6. Biocompatibility6.1 Glass and glass-ceramic biomaterials should be evalu-ated thoroughly for biocompatibility before human use. Bio-active glass and glas

30、s-ceramic materials are unique in theirmode of action when implanted in the body due to the releasedionic species and the mechanisms by which these materialsbond with bony tissue. These materials have been found toexhibit an excellent tissue response in laboratory studies(13-17) and clinical usage (

31、1-12). Before any new formulationsare used clinically, the tissue response should be characterizedby the methods recommended in Practice F 748 and F 981 asappropriate.7. Test Specimen Fabrication7.1 Test specimens should be prepared concurrent withimplant devices, as well as from the same batch of m

32、aterial andby the same processes as those used in fabricating the glass andglass-ceramic implant device.8. Quality Program Requirement8.1 The manufacturer shall conform to Quality Systemsrequirements (2.2) or equivalent.9. Keywords9.1 bioactive glass; bioactive glass-ceramics; glass bioma-terials; g

33、lass-ceramic biomaterial; surgical implantsF1538032APPENDIXES(Nonmandatory Information)X1. RATIONALEX1.1 A number of glass-ceramic materials are availablecommercially. Bioactive glass and glass-ceramic materials areavailable commercially as synthetic graft materials for main-tenance of the alveolar

34、ridge; as devices for spinal fusion; asimplants for replacement of the vertebral body, iliac crest, andossicular chain of the middle ear; as bone filler to substitute forbone defects remaining after the excision of bone tumors andextraction of loosened joint prostheses; and as coatings ondental and

35、orthopedic implants. As with any implant material,the bioresponse is critically dependent on the material proper-ties. To achieve reliable biocompatibility, these properties mustbe known and consistent. This specification provides specifi-cations for biocompatible grades of bioactive glass and glass

36、-ceramics.X1.2 In order to be called bioactive, the materials mustdemonstrate that living tissue is bonding to a significantlyhigher level than non-bonding implant control, as well asdemonstrate that ionic species are released from the materialinto solution in a controlled and reproducible manner.X1

37、.3 Bioactive glass and glass-ceramic materials are gen-erally silicate-based materials, with additions of oxides ofcalcium, phosphorous, and various alkalis. They may bephosphate-based materials as well. These materials may alsoinclude fluoride and other alkaline earth metals. Table X1.1gives a few

38、specific examples of the bioactive glass andglass-ceramic materials produced. Since the compositions ofthese materials may vary greatly from product to product, it isnot possible to specify their exact compositions.X1.4 It is recognized that separate performance standardsmay be necessary for each en

39、d-use product. Physical andmechanical properties were not specified for this reason. Asource of general test methods for glass and ceramic materialsmay be found in the Annual Book of ASTM Standards,Vol15.02.TABLE X1.1 Typical Bioactive Glass and Glass-Ceramic Compositions (Compositions in Weight %)4

40、5S5 BioglassT 52S4.6 BioglassT S53P4 Bioactive Glass A-W-GC (21)SiO245 52 53.0 34.2P2O56 6 4.0 16.3CaO 24.5 21 20.0 44.9CaF20.5MgO 4.6Na2O 24.5 21 23.0F1538033X2. BIOCOMPATIBILITYX2.1 No known surgical implant material has ever beenshown to be completely free of adverse reactions in the humanbody. H

41、owever, long-term clinical experience with the compo-sitions referred to in this specification has shown that anacceptable level of biological response can be expected if thematerials are used in appropriate applications.REFERENCES(1) Reck, R., “Tissue Reactions to Glass Ceramics in the Middle Ear,”

42、Clin. Otolaryngol, Vol 6, 1981, pp. 5963.(2) Merwin, G. E., “Review of Bioactive Materials for Otological andMaxillofacial Applications,” Handbook of Bioactive Ceramics, Vol 1,Ed. T. Yamamuro, L. L. Hench, and J. Wilson, CRC Press, Boca Raton,Florida, 1990, pp. 323328.(3) Douek, E., “Otological Appl

43、ications of Bioglasst Implants,” Pro-ceedings Fourth International Symposium on Bioceramics in Medi-cine, Ed. W. Bonfield, London, United Kingdom, September 10 and11, 1990.(4) Stanley, H. R., et al., “Residual Alveolar Ridge Maintenance with aNew Endosseous Implant Material,” J. Pros. Dent., Vol 58,

44、 No. 5,November 1987.(5) Nakamura, T., et al., “A New Glass-Ceramic for Bone Replacement:Evaluation of its Bonding to Bond Tissue,” Journal of BiomedicalMaterial Research, Vol 19, 1985.(6) Yamamuro, T., et al., “Novel Methods for Clinical Application ofBioactive Ceramics,” Bioceramics: Material Char

45、acteristics Versus inVivo Behavior, Ann. New York Acad. Sci., Vol 523, 1988, pp. 107114.(7) Yamamuro, T., “Reconstruction of the Iliac Crest with BioactiveGlass-Ceramic Prosthesis,” Handbook of Bioactive Ceramics Prosthe-sis, Eds. T. Yamamuro, L. L. Hench, and J. Wilson, Vol 1, CRC Press,Boca Raton,

46、 FL, 1990, pp. 335342.(8) Yamamuro, T., “Replacement of the Spine with Bioactive Glass-Ceramic Prosthesis,” pp. 343352, idem.(9) Taguchi, T., “A Bioactive Glass Powder-Ammonium HydrogenPhosphate Composite for Repairing Bone Defects,” Journal of Appl.Biomater., Vol 1, pp. 217223.(10) Froum, S.J., et

47、al., “Comparison of Bioglasst Synthetic Bone GraftParticles and Open Debridement on the Treatment of Human Peri-odontal Disease,” J. Periodontal., Vol 69, 1998, pp. 698-709.(11) Lovelace, T.B., et al, “Clinical Evaluations of Bioactive Glass in theTreatment of Periodontal Osseous Defects,” J. Period

48、ontal., Vol 69,1998, pp. 1027-1035.(12) Stoor, P., et al., “Bioactive Glass S53P4 in Repair of SeptalPerformations and Its Interactions with the Respiratory Infection-Associated Microorganisms Heamophilus influenzae and Streptococ-cus pneumoniae,” J. Biomed. Mater. Res, (Appl. Biomater.), Vol 58,200

49、1, pp. 113-120.(13) Hench, L. L., and Paschall, H. A., “Histo-Chemical Responses at aBiomaterials Interface,” Journal of Biomedical Material Research,Vol 5, 1974, p. 1.(14) Kitsugi, T., et al., “Bonding Behavior of a Glass-Ceramic Contain-ing Apatite and Wollastonite in Segmental Replacement of the RatTibia Under Load-Bearing Conditions,” Journal of Bone St. Surg.,Vol 71A, 1989.(15) Gross, U., et al., “The Response of Bone to Surface ActiveGlasses/Glass-Ceramics,” CRC Critical Reviews in Biocompatibility,Vol 4, No. 2, 1988, pp. 155179.(16) Piotrowski, G., et