ASTM F1609-2008 Standard Specification for Calcium Phosphate Coatings for Implantable Materials《可植入材料用磷酸钙涂层的标准规范》.pdf

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1、Designation: F 1609 08Standard Specification forCalcium Phosphate Coatings for Implantable Materials1This standard is issued under the fixed designation F 1609; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis

2、ion. 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 forcalcium phosphate coatings for surgical implant applications.1.2 In parti

3、culate and monolithic form, the calcium phos-phate materials system has been well-characterized regardingbiological response (1,2)2and laboratory characterization (2-4). Several publications (5-10) have documented the in vitroand in vivo properties of selected calcium phosphate coatingsystems.1.3 Th

4、is specification includes hydroxylapatite coatings,tricalcium phosphate coatings, or combinations thereof, with orwithout intentional minor additions of other ceramic or metal-lic,3and applied by methods including, but not limited to, thefollowing: (1) mechanical capture, (2) plasma spray deposition

5、,(3) dipping/sintering, (4) electrophoretic deposition, (5) porce-lainizing, and (6) sputtering.1.4 Substrates may include smooth, porous, textured, andother implantable topographical forms.1.5 This specification excludes organic coatings that maycontain calcium and phosphate ionic species.1.6 Warni

6、ngMercury has been designated by EPA andmany state agencies as a hazardous material that can causecentral nervous 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

7、. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAs website(http:/www.epa.gov/mercury/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.2. Referenced D

8、ocuments2.1 ASTM Standards:4E 376 Practice for Measuring Coating Thickness byMagnetic-Field or Eddy-Current (Electromagnetic) Exami-nation MethodsF 1044 Test Method for Shear Testing of Calcium Phos-phate Coatings and Metallic CoatingsF 1088 Specification for Beta-Tricalcium Phosphate forSurgical Im

9、plantationF 1147 Test Method for Tension Testing of Calcium Phos-phate and Metallic CoatingsF 1160 Test Method for Shear and Bending Fatigue Testingof Calcium Phosphate and Metallic Medical and Compos-ite Calcium Phosphate/Metallic CoatingsF 1185 Specification for Composition of Hydroxylapatitefor S

10、urgical ImplantsF 1854 Test Method for Stereological Evaluation of PorousCoatings on Medical ImplantsF 1926 Test Method for Evaluation of the EnvironmentalStability of Calcium Phosphate CoatingsF 2024 Practice for X-ray Diffraction Determination ofPhase Content of Plasma-Sprayed Hydroxyapatite Coat-

11、ings2.2 Pharmacopeia Convention Documents:5National Formulary XVI, Tribasic Calcium PhosphateUnited States Pharmacopeia:U.S. Pharmacopeia (most current), Chemical Tests: Cal-cium (191), Phosphorous (191), Lead , Mercury, Arsenic , and Heavy Metals Method(1)2.3 Other Documents:U.S. Geological Survey

12、Method, Cadmium61This 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 Materials.Current edition approved May 1, 2008. Published June 2008. Originallyapproved in 1995. Last pre

13、vious edition approved in 2003 as F 1609 031.2The boldface numbers in parentheses refer to the list of references at the end ofthis specification.3The Joint Committee on Powdered Diffraction has established a PowderDiffraction File. The committee operates on an international basis and cooperatesclos

14、ely with the Data Commission of the International Union of Crystallinity andASTM. Hydroxylapatite data can be found on file card No. 9-432; beta tricalciumphosphate data can be found on file card No. 9-169.4For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer

15、Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.5Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,MD 20852-1790, http:/www.usp.org.6Crock, J. G., Felichte, F. E., and Briggs, P. H

16、., “Determination of Elements inNational Bureau of Standards Geological Reference Materials SRM 278 Obsidianand SRM 688 Basalt by Inductively Coupled Argon PlasmaAtomic EmissionSpectrometry,” Geostandards Newsletter, Vol 7, 1983, pp. 335340.1Copyright ASTM International, 100 Barr Harbor Drive, PO Bo

17、x C700, West Conshohocken, PA 19428-2959, United States.U.S. Code of Federal Regulations Title 21 (CFR 21), Part820Quality System Regulation7X-Ray Diffraction Analyses33. Terminology3.1 Definitions:3.1.1 amorphous calcium phosphatea non-crystalline cal-cium phosphate.3.1.2 beta tricalcium phosphatea

18、 calcium phosphate sub-stance of empirical chemical formula, Ca3(PO4)2(see Specifi-cation F 1088).3.1.3 calcium phosphateany one of a number of inorganicchemical compounds containing calcium and phosphate ions asits principal constituents.3.1.4 coatinga layer of mechanically or chemically at-tached

19、material covering a substrate material.3.1.5 hydroxylapatitea calcium phosphate crystallinecompound of empirical chemical formula, Ca5(PO4)3OH (seeSpecification F 1185).4. Chemical or Crystallographic Requirements, or Both4.1 Chemical:4.1.1 Elemental analysis for calcium and phosphorous andintention

20、al additions (other than trace elements) shall beconsistent with the expected stoichiometry of the specificcalcium phosphate compound(s).4.1.2 Trace Element Analysis for Hydroxylapatite and BetaTricalcium PhosphateThe concentration of trace elements inthe coating shall be limited as follows:Element

21、ppm, maxAs 3Cd 5Hg 5Pb 30total heavy metals (as lead) 50For reference purposes, the U.S. Pharmacopeia (most cur-rent) and U.S. Geological Survey Method, Cadmium, shall beused.4.1.3 The analysis of other trace elements may be required,based on the conditions, apparatus, or environments specific tothe

22、 coating application technique used.4.1.4 The analysis of intentional additional elements orcompounds such as fluorine, manganese, magnesium, carbon-ate, and so forth shall be specified for calcium phosphatecoatings.4.1.5 Calcium to Phosphorus ratio (Ca/P) shall be per-formed on both the powder and

23、coating forms using a suitablemethod.4.2 Crystallographic Characterization:4.2.1 Crystallographic characterization shall be in accor-dance with Practice F 2024.4.2.2 Testing shall include quantitative phase analysis andamorphous calcium phosphate content.4.2.3 FTIR (Fourier Transform Infrared Spectr

24、oscopy) shallbe performed to identify functional groups.4.3 Environmental StabilityEnvironmental stability test-ing shall be performed in accordance with Test Method F 1926to access the relative dissolution behavior of the material.5. Physical Characterization5.1 Coverage of Substrate:5.1.1 Microsco

25、pic examination of the surface will be madeat 103 magnification; “bare” areas, “pinholes,” cracking,foreign debris, unmelts, chips, delamination and the appear-ance at the coating/substrate interface, and so forth shall bereported.5.2 ThicknessThe thickness shall be measured from crosssections in ac

26、cordance with Test Method F 1854. If distinctlayers exist, they should be reported.5.2.1 Alternatively, a magnetic field or eddy current tech-nique may be used if it has been shown to be equivalent to TestMethod F 1854.5.3 PorosityThe microporosity and macroporosity char-acterization shall be determ

27、ined in accordance with TestMethod F 1854.5.4 ColorA macroscopic examination of color should beperformed to guarantee a uniform and consistent appearance,in consideration of the specific process, substrate material andgeometry, and coating thickness.5.5 Surface TopographyThe surface topography shall

28、 bemeasured using equipment designed to determine surfaceroughness. Characterization of the surface topography of theunderlying substrate may be required, if applicable, for thespecific coating method. Scanning electron microscopy shallbe used to provide a visual representation of the coating surfac

29、echaracteristics.5.6 DensityDensity of both the powder and coated formsshall be performed using a suitable method.6. Mechanical Characterization6.1 The following mechanical characterizations may beapplicable to a coating, depending on the substrate material orgeometry, coating thickness or location,

30、 or coating method(s).Characterization reports shall contain sufficient informationregarding the test techniques, procedures, and standards usedand details such as specimen orientation and proportional depthof thickness in order to represent the analysis accurately.6.1.1 The tensile bond strength of

31、 the coating to the sub-strate shall be determined using Test Method F 1147.6.1.2 The shear strength shall be determined using TestMethod F 1044.6.1.3 The fatigue strength shall be determined using TestMethod F 1160. Both the coating/substrate interface, and theeffect on the substrate should be eval

32、uated. The effect of thecoating on the resulting fatigue strength of an actual deviceshould also be considered.7. Test Specimen Fabrication7.1 All test specimens for coating characterizations shall beprepared from coating lots and samples from the same produc-tion feedstock lots and prepared on the

33、same equipment used toapply the coating to actual devices.7Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5098, Attn: NPODS.F16090827.2 For device characterization, all test specimens should besubjected to the same processing and steri

34、lization as thefinished device, if applicable.8. Contact with Calcium Phosphate Coatings8.1 In general, extra precautions should be taken whenhandling calcium phosphate coatings.8.1.1 Contact with the coatings should be limited to soft,biocompatible polymers.8.1.2 The only liquids to come in contact

35、 with the coatingshall be distilled water, acetone, and isopropyl alcohol.8.1.2.1 pH is critical, and should measure 7.0 or higher inany liquid that comes in contact with the coating.8.1.3 Powder-free latex or nitrile gloves shall be the onlygloves used for handling coatings.9. Quality Program Requi

36、rements9.1 The manufacture of calcium phosphate coatings shallconform to the applicable FDA and ISO quality standards.10. Keywords10.1 bone implant; calcium phosphate; coating; dental im-plant materials; hydroxylapatite; mechanical tests; orthopedicmedical devices; physical characterizations; trical

37、ciumphosphateAPPENDIX(Nonmandatory Information)X1. RATIONALEX1.1 Ceramic hydroxylapatite and beta-tricalcium phos-phate are commercially available in many forms as syntheticbone grafting materials. Specifications F 1088 and F 1185 havebeen established for these substances as particulates. For mostim

38、plant materials, the biological performance is criticallydependent on the materials properties, including chemical andmechanical properties and physical form. These propertiesmust be well-characterized and consistent in order to achievereproducible clinical results and reliable biocompatibility. Thi

39、sspecification shall cover biocompatible grades of calciumphosphate coatings only.X1.2 Powder X-ray diffraction analysis provides differen-tiation between crystalline forms of these various calciumphosphate crystalline species, one or more of which will be amajor phase in coatings covered by this sp

40、ecification, whileothers may occur as second or minor phases. It is anticipatedthat a separate performance standard may be necessary for eachseparate coating as designated by the major crystalline phase.The physical and mechanical property assessments are notspecific to any one type of coating for t

41、his reason, but ratherthey are listed generically as guidelines for analysis. Minor orsignificant modifications to these procedures may have to bemade to result in useful characterization data for the mainte-nance of individual coating consistency. The sources of generaltest methods for these coatin

42、gs are listed in Section 2.REFERENCES(1) Jarcho, M., Kay, J. F., Gumaer, K. I., Doremus, R. H., and Drobeck, H.P., “Tissue, Cellular and Subcellular Events at a Bone-CeramicHydroxylapatite Interface,” Journal of Bioengineering, Vol 1, 1977,pp. 7992.(2) Jarcho, M., “Calcium Phosphate Ceramics as Hard

43、 Tissue Prosthet-ics,” Clin Orthop, Vol 157, 1981, pp. 259.(3) de Groot, K., “Ceramics of Calcium Phosphates: Preparation andProperties,” Bioceramics of Calcium Phosphate, K. de Groot, ed.,CRC Press, Inc., Boca Raton, FL, 1982.(4) Jarcho, M., Bolen, C. H., Thomas, M. B., Bobick, J., Kay, J. F., andD

44、oremus, R. H., “Hydroxylapatite Synthesis and Characterization inDense Polycrystalline Form,” Journal of Materials Science, Vol 11,1976, pp. 20272035.(5) “Bioceramics: Material Characteristics Versus In-Vivo Behavior,” P.Ducheyne and J. Lemons, eds., N.Y. Academy of Science, Vol 523,1988.(6) Cook, S

45、. D., Kay, J. F., Thomas, K. A., and Jarcho, M., “InterfaceMechanics and Histology of Titanium and Hydroxylapatite-CoatedTitanium for Dental Implant Applications,” International Journal ofOral Maxillofac Implants, Vol 2, 1987, pp. 1522.(7) Cook, S. D., Kay, J. F., Thomas, K. A., and Jarcho, M.,“Hydr

46、oxylapatite-Coated Porous Titanium for Use as an OrthopaedicBiological Attachment System,” Clin Orthop, Vol 230, 1988, pp.303312.(8) Kay, J. F., Golec, T. S., and Riley, R. L., “Hydroxylapatite-CoatedSubperiosteal Dental Implants: Design Rationale and Clinical Experi-ence,” Journal of Prosthet Dent,

47、 Vol 58, 1987, pp. 339343.(9) Block, M. S., Kent, J. N., and Kay, J. F., “The Evaluation ofHydroxylapatite-Coated Dental Implants in Dogs,” Journal of OralMaxillofac Surg, Vol 45, 1987, pp. 601607.(10) Thomas, K. A., Kay, J. F., and Cook, S. D., “The Effect of SurfaceMacrostructure and Hydroxylapati

48、te Coating on the MechanicalStrengths and Histologic Profiles of Titanium Implant Materials,”Journal of Biomed Mater Res, Vol 21, 1987, pp. 13951414.(11) Cullity, B. D., Elements of X-Ray Diffraction, Addison Wesley,Reading, MA, 1967.(12) Handbook of Bioactive Ceramics, II: Calcium Phosphate and Hy-

49、droxylapatite Ceramics,Yamamuro, Hench, Wilson, eds., CRC Press,Boca Raton, FL, 1990.(13) Balmain, N., Legros, R., and Bonel, G., “X-Ray Diffraction ofCalcified Bone Tissue: A Reliable Method for the Determination ofBone Ca/P Molar Ratio,” Calc Tiss Res, Vol 34, 1982, pp. 9398.F1609083(14) Toth, J., Hirthe, W., Hubbard, W., Brantley, W., and Lynch, K.,“Determination of the Ratio of HA/TCP Mixtures by X-Ray Diffrac-tion,” Journal of Applied Biomaterials, Vol 2, 1991, pp. 3740.(15) Sendax, V., “Hydroxylapatite Coated Implants,” Dent Clin N Am,Vol 36, 1992