ASTM F1609-2008(2014) 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

1、Designation: F1609 08 (Reapproved 2014)Standard Specification forCalcium Phosphate Coatings for Implantable Materials1This standard is issued under the fixed designation F1609; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye

2、ar 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 forcalcium phosphate coatings for surgical implant applicati

3、ons.1.2 In particulate 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 coati

4、ngsystems.1.3 This specification includes hydroxylapatite coatings,tricalcium phosphate coatings, or combinations thereof, with orwithout intentional minor additions of other ceramic ormetallic,3and applied by methods including, but not limited to,the following: (1) mechanical capture, (2) plasma sp

5、raydeposition, (3) dipping/sintering, (4) electrophoreticdeposition, (5) porcelainizing, 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 speci

6、es.1.6 WarningMercury 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-contain

7、ing products. 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.

8、Referenced Documents2.1 ASTM Standards:4E376 Practice for Measuring Coating Thickness byMagnetic-Field or Eddy-Current (Electromagnetic) Test-ing MethodsF1044 Test Method for Shear Testing of Calcium PhosphateCoatings and Metallic CoatingsF1088 Specification for Beta-Tricalcium Phosphate for Sur-gic

9、al ImplantationF1147 Test Method for Tension Testing of Calcium Phos-phate and Metallic CoatingsF1160 Test Method for Shear and Bending Fatigue Testingof Calcium Phosphate and Metallic Medical and Compos-ite Calcium Phosphate/Metallic CoatingsF1185 Specification for Composition of Hydroxylapatite fo

10、rSurgical ImplantsF1854 Test Method for Stereological Evaluation of PorousCoatings on Medical ImplantsF1926 Test Method for Evaluation of the EnvironmentalStability of Calcium Phosphate CoatingsF2024 Practice for X-ray Diffraction Determination of PhaseContent of Plasma-Sprayed Hydroxyapatite Coatin

11、gs2.2 Pharmacopeia Convention Documents:5National Formulary XVI, Tribasic Calcium PhosphateUnited States Pharmacopeia:U.S. Pharmacopeia (most current), Chemical Tests: Calcium(191), Phosphorous (191), Lead , Mercury ,Arsenic , and Heavy Metals Method (1)2.3 Other Documents:U.S. Geological Survey Met

12、hod, Cadmium6U.S. Code of Federal Regulations Title 21 (CFR 21), Part820Quality System Regulation71This specification is under the jurisdiction of ASTM Committee F04 onMedical and Surgical Materials and Devicesand is the direct responsibility ofSubcommittee F04.13 on Ceramic Materials.Current editio

13、n approved March 1, 2014. Published March 2014. Originallyapproved in 1995. Last previous edition approved in 2008 as F1609 08. DOI:10.1520/F1609-08R14.2The boldface numbers in parentheses refer to the list of references at the end ofthis specification.3The Joint Committee on Powdered Diffraction ha

14、s established a PowderDiffraction File. The committee operates on an international basis and cooperatesclosely 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 ca

15、rd No. 9-169.4For referenced ASTM standards, 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.5Available from U.S. Pharmacopeia (USP), 12601 T

16、winbrook Pkwy., Rockville,MD 20852-1790, http:/www.usp.org.6Crock, 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,” G

17、eostandards Newsletter, Vol 7, 1983, pp. 335340.7Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http:/dodssp.daps.dla.mil.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959

18、. United States1X-Ray Diffraction Analyses33. Terminology3.1 Definitions:3.1.1 amorphous calcium phosphatea non-crystalline cal-cium phosphate.3.1.2 beta tricalcium phosphatea calcium phosphate sub-stance of empirical chemical formula, Ca3(PO4)2(see Specifi-cation F1088).3.1.3 calcium phosphateany o

19、ne 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 material covering a substrate material.3.1.5 hydroxylapatitea calcium phosphate crystallinecompound of empirical chemical form

20、ula, Ca5(PO4)3OH (seeSpecification F1185).4. Chemical or Crystallographic Requirements, or Both4.1 Chemical:4.1.1 Elemental analysis for calcium and phosphorous andintentional additions (other than trace elements) shall beconsistent with the expected stoichiometry of the specificcalcium phosphate co

21、mpound(s).4.1.2 Trace Element Analysis for Hydroxylapatite and BetaTricalcium PhosphateThe concentration of trace elements inthe coating shall be limited as follows:Element ppm, maxAs 3Cd 5Hg 5Pb 30total heavy metals (as lead) 50For reference purposes, the U.S. Pharmacopeia (most cur-rent) and U.S.

22、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 coating application technique used.4.1.4 The analysis of intentional additional elements orcompounds such as fluorine, mangane

23、se, magnesium,carbonate, 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 coating forms using a suitablemethod.4.2 Crystallographic Characterization:4.2.1 Crystallographic characterization shall be in ac

24、cor-dance with Practice F2024.4.2.2 Testing shall include quantitative phase analysis andamorphous calcium phosphate content.4.2.3 FTIR (Fourier Transform Infrared Spectroscopy) shallbe performed to identify functional groups.4.3 Environmental StabilityEnvironmental stability test-ing shall be perfo

25、rmed in accordance with Test Method F1926to access the relative dissolution behavior of the material.5. Physical Characterization5.1 Coverage of Substrate:5.1.1 Microscopic examination of the surface will be madeat 10 magnification; “bare” areas, “pinholes,” cracking, for-eign debris, unmelts, chips

26、, delamination and the appearance atthe coating/substrate interface, and so forth shall be reported.5.2 ThicknessThe thickness shall be measured from crosssections in accordance with Test Method F1854. If distinctlayers exist, they should be reported.5.2.1 Alternatively, a magnetic field or eddy cur

27、rent tech-nique may be used if it has been shown to be equivalent to TestMethod F1854.5.3 PorosityThe microporosity and macroporosity charac-terization shall be determined in accordance with Test MethodF1854.5.4 ColorA macroscopic examination of color should beperformed to guarantee a uniform and co

28、nsistent appearance,in consideration of the specific process, substrate material andgeometry, and coating thickness.5.5 Surface TopographyThe surface topography shall bemeasured using equipment designed to determine surfaceroughness. Characterization of the surface topography of theunderlying substr

29、ate may be required, if applicable, for thespecific coating method. Scanning electron microscopy shallbe used to provide a visual representation of the coating surfacecharacteristics.5.6 DensityDensity of both the powder and coated formsshall be performed using a suitable method.6. Mechanical Charac

30、terization6.1 The following mechanical characterizations may beapplicable to a coating, depending on the substrate material orgeometry, coating thickness or location, or coating method(s).Characterization reports shall contain sufficient informationregarding the test techniques, procedures, and stan

31、dards 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 coating to the sub-strate shall be determined using Test Method F1147.6.1.2 The shear strength shall be determined using TestMeth

32、od F1044.6.1.3 The fatigue strength shall be determined using TestMethod F1160. Both the coating/substrate interface, and theeffect on the substrate should be evaluated. The effect of thecoating on the resulting fatigue strength of an actual deviceshould also be considered.7. Test Specimen Fabricati

33、on7.1 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 equipment used toapply the coating to actual devices.7.2 For device characterization, all test specimens should besubjected to the s

34、ame processing and sterilization as thefinished device, if applicable.F1609 08 (2014)28. 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

35、.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 comes in contact with the coating.8.1.3 Powder-free latex or nitrile gloves shall be the onlygloves used for ha

36、ndling coatings.9. Quality Program Requirements9.1 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 dev

37、ices; physical characterizations; tricalcium phos-phateAPPENDIX(Nonmandatory Information)X1. RATIONALEX1.1 Ceramic hydroxylapatite and beta-tricalcium phos-phate are commercially available in many forms as syntheticbone grafting materials. Specifications F1088 and F1185 havebeen established for thes

38、e substances as particulates. For mostimplant 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 re

39、sults and reliable biocompatibility. Thisspecification 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 ama

40、jor 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 eachseparate coating as designated by the major crystalline phase.The physical and mechanical property assessments are nots

41、pecific 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 bemade to result in useful characterization data for the mainte-nance of individual coating consistency. The sources

42、 of generaltest methods for these coatings are listed in Section 2.REFERENCESF1609 08 (2014)3(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.

43、 7992.(2) Jarcho, M., “Calcium Phosphate Ceramics as Hard TissueProsthetics,” 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., Bo

44、len, 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. 20272035.(5) “Bioceramics: Material Characteristics Versus In-Vivo Behavior,” P.Ducheyne and J. Lemons,

45、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 Implant Applications,” International Journal ofOral Maxillofac Implants, Vol 2, 1987, pp. 1522.(7) Cook,

46、 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., Golec, T. S., and Riley, R. L., “Hydroxylapatite-CoatedSubperiosteal Dental Implants: Design Rationa

47、le and ClinicalExperience,” 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 of OralMaxillofac Surg, Vol 45, 1987, pp. 601607.(10) Thomas, K. A., Kay, J. F., and Cook, S. D., “

48、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. 13951414.(11) Cullity, B. D., Elements of X-Ray Diffraction, Addison Wesley,Reading, MA, 1967.(12) Handbook

49、 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 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-RayDiffraction,” Journal of Applied Biomaterials, Vol 2, 1991, pp.3740.(15) Sendax, V., “Hydroxylapatite C