ASTM F1609-2003 Standard Specification for Calcium Phosphate Coatings for Implantable Materials《可植入材料用磷酸钙涂层标准规范》.pdf

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1、Designation: F 1609 03Standard 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 (e) 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 part

3、iculate 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 T

4、his 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 depositio

5、n,(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.2. Refer

6、enced Documents2.1 ASTM Standards:E 376 Practice for Measuring Coating Thickness byMagnetic-Field or Eddy-Current (Electromagnetic) TestMethods4F 1044 Test Method for Shear Testing of Calcium Phos-phate Coatings and Metallic Coatings5F 1088 Specification for Beta-Tricalcium Phosphate forSurgical Imp

7、lantation5F 1147 Test Method for Tension Testing of Calcium Phos-phate Coatings and Metallic Coatings5F 1160 Test Method for Shear and Bending Fatigue Testingof Calcium Phosphate and Metallis Medical and CompositeCalcium Phosphate Metallic Coatings5F 1185 Specification for Composition of Ceramic Hyd

8、roxy-lapatite for Surgical Implants5F 1854 Shear and Bending Fatigue Testing of CalciumPhosphate and Metallis Medical and Composite CalciumPhosphate Metallic Coatings5F 1926 Test Method for Evaluation of the EnvironmentalStability of Calcium Phosphate Coatings5F 2024 Practice for X-Ray Diffraction D

9、etermination ofPhase Content of Plasma-Sprayed Hydroxylapatite Coat-ings52.2 Pharmacopeia Convention Documents:6National Formulary XVI, Tribasic Calcium PhosphateUnited States Pharmacopeia:U.S. Pharmacopeia XXI, Chemical Tests CaP (191), Lead, Mercury , Arsenic , and HeavyMetals Method (1)2.3 Other

10、Documents:U.S. Geological Survey Method, Cadmium7U.S. Code of Federal Regulations Title 21 (CFR 21), Part820Quality System Regulation8X-Ray Diffraction Analyses33. Terminology3.1 Definitions:3.1.1 amorphous calcium phosphatea non-crystalline cal-cium phosphate.3.1.2 beta tricalcium phosphatea calciu

11、m 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.1This specification is under the jurisdiction of ASTM Committee F04

12、onMedical and Surgical Materials and Devices and is the direct responsibility ofSubcommittee F04.13 on Ceramic Materials.Current edition approved Sept. 10, 2003. Published October 2003. Originallyapproved in 1995. Last previous edition approved in 1995 as F 1609 95.2The boldface numbers in parenthes

13、es 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 cooperatesclosely with the Data Commission of the International Union of Crystallinity andAST

14、M. Hydroxylapatite data can be found on file card No. 9-432; beta tricalciumphosphate data can be found on file card No. 9-169.4Annual Book of ASTM Standards, Vol 03.03.5Annual Book of ASTM Standards, Vol 13.01.6Available from U.S. Pharmacopeia Convention, Inc., 12601 Twinbrook Park-way, Rockville,

15、MD 20852.7Crock, J. G., Felichte, F. E., and Briggs, P. H., “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. 335340.8A

16、vailable from Standardization Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5098, Attn: NPODS.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.4 coatinga layer of mechanically or chemically at-ta

17、ched 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 andinte

18、ntional additions (other than trace elements) will be con-sistent with the expected stoichiometry of the specific calciumphosphate compound(s).4.1.2 Trace Element Analysis for Hydroxylapatite and BetaTricalcium PhosphateThe concentration of trace elements inthe coating shall be limited as follows:El

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

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

21、 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 Spectroscopy)

22、 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 Microscopic exa

23、mination 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 will bereported.5.2 ThicknessThe thickness will be measured from crosssections in accordance

24、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 determined in a

25、ccordance 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 bemeasur

26、ed 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 surfacecharacte

27、ristics.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, or coati

28、ng 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 the coat

29、ing 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 evaluated. Th

30、e 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 same equi

31、pment used toapply the coating to actual devices.7.2 For device characterization, all test specimens should besubjected to the same processing and sterilization as thefinished device, if applicable.8. Contact with Calcium Phosphate Coatings8.1 In general, extra precautions should be taken whenhandli

32、ng 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 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

33、 comes in contact with the coating.8.1.3 Powder-free latex gloves shall be the only glovematerial for handling coatings.9. Quality Program Requirements9.1 The manufacture of calcium phosphate coatings willconform to the applicable FDA and ISO quality standards.F160903210. Keywords10.1 bone implant;

34、calcium phosphate; coating; dental im-plant materials; hydroxylapatite; mechanical tests; orthopedicmedical devices; physical characterizations; tricalcium phos-phateAPPENDIX(Nonmandatory Information)X1. RATIONALEX1.1 Ceramic hydroxylapatite and beta-tricalcium phos-phate are commercially available

35、in many forms as syntheticbone grafting materials. Specifications F 1088 and F 1185 havebeen established for these substances as particulates. For mostimplant materials, the biological performance is criticallydependent on the materials properties, including chemical andmechanical properties and phy

36、sical form. These propertiesmust be well-characterized and consistent in order to achievereproducible clinical results and reliable biocompatibility. Thisspecification shall cover biocompatible grades of calciumphosphate coatings only.X1.2 Powder X-ray diffraction analysis provides differen-tiation

37、between crystalline forms of these various calciumphosphate crystalline species, one or more of which will be amajor phase in coatings covered by this specification, whileothers may occur as second or minor phases. It is anticipatedthat a separate performance standard may be necessary for eachsepara

38、te coating as designated by the major crystalline phase.The physical and mechanical property assessments are notspecific to any one type of coating for this reason, but ratherthey are listed generically as guidelines for analysis. Minor orsignificant modifications to these procedures may have to bem

39、ade to result in useful characterization data for the mainte-nance of individual coating consistency. The sources of generaltest methods for these coatings 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 Subcellula

40、r Events at a Bone-CeramicHydroxylapatite Interface,” Journal of Bioengineering, Vol 1, 1977,pp. 7992.(2) Jarcho, M., “Calcium Phosphate Ceramics as Hard Tissue Prosthet-ics,” Clin Orthop, Vol 157, 1981, pp. 259.(3) de Groot, K., “Ceramics of Calcium Phosphates: Preparation andProperties,” Biocerami

41、cs 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., andDoremus, R. H., “Hydroxylapatite Synthesis and Characterization inDense Polycrystalline Form,” Journal of Materials Science, Vol 11,1976, pp. 202720

42、35.(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. D., Kay, J. F., Thomas, K. A., and Jarcho, M., “InterfaceMechanics and Histology of Titanium and Hydroxylapatite-CoatedTitanium for Dental Implan

43、t Applications,” International Journal ofOral Maxillofac Implants, Vol 2, 1987, pp. 1522.(7) Cook, S. D., Kay, J. F., Thomas, K. A., and Jarcho, M.,“Hydroxylapatite-Coated Porous Titanium for Use as an OrthopaedicBiological Attachment System,” Clin Orthop, Vol 230, 1988, pp.303312.(8) Kay, J. F., Go

44、lec, T. S., and Riley, R. L., “Hydroxylapatite-CoatedSubperiosteal Dental Implants: Design Rationale and Clinical Experi-ence,” Journal of Prosthet Dent, 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

45、 of OralMaxillofac Surg, Vol 45, 1987, pp. 601607.(10) Thomas, K. A., Kay, J. F., and Cook, S. D., “The Effect of SurfaceMacrostructure and Hydroxylapatite Coating on the MechanicalStrengths and Histologic Profiles of Titanium Implant Materials,”Journal of Biomed Mater Res, Vol 21, 1987, pp. 1395141

46、4.(11) Cullity, B. D., Elements of X-Ray Diffraction, Addison Wesley,Reading, MA, 1967.(12) Handbook of Bioactive Ceramics, II: Calcium Phosphate andHydroxylapatite Ceramics, Yamamuro, Hench, Wilson, eds., CRCPress, Boca Raton, FL, 1990.(13) Balmain, N., Legros, R., and Bonel, G., “X-Ray Diffraction

47、 ofCalcified Bone Tissue: A Reliable Method for the Determination ofBone Ca/P Molar Ratio,” Calc Tiss Res, Vol 34, 1982, pp. 9398.(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

48、, Vol 2, 1991, pp. 3740.(15) Sendax, V., “Hydroxylapatite Coated Implants,” Dent Clin N Am,Vol 36, 1992.F1609033ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advis

49、ed that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical com