ASTM F1538-2003(2017) Standard Specification for Glass and Glass Ceramic Biomaterials for Implantation《玻璃和玻璃瓷质植入人体生物材料的标准规格》.pdf

1、Designation: F1538 03 (Reapproved 2017)Standard Specification forGlass and Glass Ceramic Biomaterials for Implantation1This standard is issued under the fixed designation F1538; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y

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

3、bioma-terials intended 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

4、 studies (13-17).1.3 This specification excludes synthetic hydroxylapatite,hydroxylapatite coatings, aluminum oxide ceramics, alpha- andbeta-tricalcium phosphate, and whitlockite.1.4 WarningMercury has been designated by EPA andmany state agencies as a hazardous material that can causecentral nervou

5、s system, kidney, and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury-containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAs website(http:/www.epa.gov/m

6、ercury/faq.htm) for additional informa-tion. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited bystate law.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization est

7、ablished in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3C158 Test Methods for Strength of Glass by Flexure (De-termin

8、ation of Modulus of Rupture)C169 Test Methods for Chemical Analysis of Soda-Limeand Borosilicate GlassC373 Test Methods for Determination of Water Absorptionand Associated Properties by Vacuum Method for PressedCeramic Tiles and Glass Tiles and Boil Method forExtruded Ceramic Tiles and Non-tile Fire

9、d CeramicWhiteware ProductsC623 Test Method for Youngs Modulus, Shear Modulus,and Poissons Ratio for Glass and Glass-Ceramics byResonanceC633 Test Method for Adhesion or Cohesion Strength ofThermal Spray CoatingsC693 Test Method for Density of Glass by BuoyancyC729 Test Method for Density of Glass b

10、y the Sink-FloatComparatorC730 Test Method for Knoop Indentation Hardness of GlassC958 Test Method for Particle Size Distribution of Aluminaor Quartz by X-Ray Monitoring of Gravity SedimentationC1069 Test Method for Specific Surface Area of Alumina orQuartz by Nitrogen AdsorptionC1070 Test Method fo

11、r Determining Particle Size Distribu-tion of Alumina or Quartz by Laser Light ScatteringE228 Test Method for Linear Thermal Expansion of SolidMaterials With a Push-Rod DilatometerF748 Practice for Selecting Generic Biological Test Methodsfor Materials and DevicesF981 Practice for Assessment of Compa

12、tibility of Biomate-rials for Surgical Implants with Respect to Effect ofMaterials on Muscle and Insertion into Bone1This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devices and is the direct responsibility ofSubcommittee F04.13 on Ceramic Mater

13、ials.Current edition approved May 1, 2017. Published June 2017. Originallyapproved in 1994. Last previous edition approved in 2009 as F1538 03 (2009).DOI: 10.1520/F1538-03R17.2The boldface numbers in parentheses refer to the list of references at the end ofthis specification.3For referenced ASTM sta

14、ndards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,

15、PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization

16、 Technical Barriers to Trade (TBT) Committee.12.2 Code of Federal Regulations:4Title 21, Part 8202.3 United States Pharmacopoeia:5Lead Mercury Arsenic Heavy Metals Method I2.4 U.S. Geological Survey Method:6Cadmium3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 bioactive glass

17、an amorphous silicate-based solidthat 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-hy

18、droxymethylaminomethane buffer.3.1.2 bioactive 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 hydroxycarbonateapatite layer when exposed t

19、o appropriate in vitroenvironments, 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

20、of theprosthetic 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-derive

21、d crystalline 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 MethodC1

22、69.4.2 The concentration 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 absop

23、rtion (AAS), 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

24、 densities of 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 C373 or C729 and shallbe consistent for the specific materials.NOTE 1This test should use a non-aqueous l

25、iquid for bioactive 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 Meth

26、ods C158.5.1.3 Youngs ModulusWhen used as a bulk material,Youngs Modulus of glass and glass ceramic biomaterials shallbe determined following Test Method C623.5.1.4 HardnessWhere applicable, for characterization ofthe material, the hardness of bulk samples shall be determinedusing Test Method C730.

27、The Knoop 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 cas

28、es in which 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 ar

29、ea of particulate glass andglass ceramic biomaterials shall be measured using TestMethod C1069.5.1.6 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 C633.5.1.7 Crystallini

30、tyFor glass-ceramic biomaterials, the per-cent 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, te

31、chniques 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 E228, when materials are to be4Available from U.S. Government Printing Office Superintendent of Documents,732

32、N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.5Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,MD 20852-1790, http:/www.usp.org.6Crock, J.G., Felichte, F.E., Briggs, P.H., “Determination of Elements inNational Bureau of Standards Geologic

33、al Reference Materials SRM 278 Obsidianand SRM 688 Basalt by Inductively Coupled Plasma-Atomic EmissionSpectrometry,” Geostandards NewsletterVol 7, 1983pp. 335340.F1538 03 (2017)2used for coatings (raw materials are to be measured), or onfinished product as a quality control test.5.1.9 Particle Size

34、When used as a particulate, the particlesize shall be measured in accordance with Test Methods C958or C1070.6. Biocompatibility6.1 Glass and glass-ceramic biomaterials should be evalu-ated thoroughly for biocompatibility before human use. Bio-active glass and glass-ceramic materials are unique in th

35、eirmode 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 (1-12). Before any new formulationsar

36、e used clinically, the tissue response should be characterizedby the methods recommended in Practice F748 and F981 asappropriate.7. Test Specimen Fabrication7.1 Test specimens should be prepared concurrent withimplant devices, as well as from the same batch of material andby the same processes as th

37、ose 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; glass-ceramic biomaterial; surgical imp

38、lantsAPPENDIXES(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 ridge; as devices for spinal fusion; asimplant

39、s 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 orthopedic implants. As with any implant mater

40、ial,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-ceramics.X1.2 In order to be called bioactive

41、, 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.X1.3 Bioactive glass and glass-ceramic materials

42、 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 specific examples of the bioactive glass andgl

43、ass-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 end-use product. Physical andmechanical properti

44、es 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 %)45S5 Bioglass 52S4.6 Bioglass S53P4 Bioactive G

45、lass 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 23.0F1538 03 (2017)3X2. BIOCOMPATIBILITYX2.1 No known surgical implant material has ever beenshown to be completely free of adverse reactions in the humanbody. However, long-term clinical experience wi

46、th 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,”Clin. Otolaryngol, Vol 6, 1981, pp. 5963

47、.(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, BocaRaton, Florida, 1990, pp. 323328.(3) Douek, E., “Otological Applications of Bioglass Implants,” Pro-ceed

48、ings Fourth International Symposium on Bioceramics inMedicine, Ed. W. Bonfield, London, United Kingdom, September 10and 11, 1990.(4) Stanley, H. R., et al., “Residual Alveolar Ridge Maintenance with aNew Endosseous Implant Material,” J. Pros. Dent., Vol 58, No. 5,November 1987.(5) Nakamura, T., et a

49、l., “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 Characteristics Versusin Vivo 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 CeramicsProsthesis, Eds. T. Yamamuro, L. L. Hench, and J. Wilson, Vol 1,CRC Press, Boca Raton