ISO 13779-2-2008

Reference numberISO 13779-2:2008(E)©ISO 2008INTERNATIONAL STANDARD ISO13779-2Second edition2008-10-01Implants for surgery — Hydroxyapatite —Part 2: Coatings of hydroxyapatite Implants chirurgicaux — Hydroxyapatite — Partie 2: Revêtements à base d hydroxyapatite Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 13779-2:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe s licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe s licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT © ISO 2008 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO s member body in the country of the requester. ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyright@iso.org Web www.iso.org Published in Switzerland ii © ISO 2008 – All rights reservedCopyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 13779-2:2008(E) © ISO 2008 – All rights reserved iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 13779-2 was prepared by Technical Committee ISO/TC 150, Implants for surgery, Subcommittee SC 1, Materials. This second edition cancels and replaces the first edition (ISO 13779-2:2000), which has been technically revised. ISO 13779 consists of the following parts, under the general title Implants for surgery — Hydroxyapatite: ⎯ Part 1: Ceramic hydroxyapatite ⎯ Part 2: Coatings of hydroxyapatite ⎯ Part 3: Chemical analysis and characterization of crystallinity and phase purity ⎯ Part 4: Determination of coating adhesion strength Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 13779-2:2008(E) iv © ISO 2008 – All rights reservedIntroduction No known surgical implant material has ever been shown to be completely free of adverse reactions in the human body. However, long-term clinical experience of the use of the material referred to in ISO 13779 has shown that an acceptable level of biological response can be expected, if the material is used in appropriate applications. The biological response to hydroxyapatite coatings has been demonstrated by a history of clinical use and by laboratory studies. See Bibliography. Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---INTERNATIONAL STANDARD ISO 13779-2:2008(E)© ISO 2008 – All rights reserved 1Implants for surgery — Hydroxyapatite — Part 2: Coatings of hydroxyapatite 1 Scope This part of ISO 13779 specifies requirements for ceramic hydroxyapatite coatings applied to metallic or non-metallic surgical implants. This part of ISO 13779 does not cover coatings made from glasses, glass ceramics, alpha- and beta-calcium orthophosphate or other forms of calcium phosphate, nor does it cover coatings in which the hydroxyapatite is present in a powder form. This part of ISO 13779 does not apply to nanoparticle-type materials. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 10993-17, Biological evaluation of medical devices — Part 17: Establishment of allowable limits for leachable substances ISO 13779-1, Implants for surgery — Hydroxyapatite — Part 1: Ceramic hydroxyapatite ISO 13779-3, Implants for surgery — Hydroxyapatite — Part 3: Chemical analysis and characterization of crystallinity and phase purity ISO 13779-4; Implants for surgery — Hydroxyapatite — Part 4: Determination of coating adhesion strength 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 13779-1 and the following apply. 3.1 coating hydroxyapatite that has been deposited on to the surface of a metallic or non-metallic substrate either by means of a thermal spray process, which produces a ceramic-type coating or by means of a solution-based technique, which can deposit hydroxyapatite directly or might require thermal or other treatment to convert it into a crystalline form Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 13779-2:2008(E) 2 © ISO 2008 – All rights reserved4 Coating preparation The coating to be tested shall be representative of the final product i.e. produced in the same way as the coating for the implant and subjected to any other final process like cleaning and sterilization. 5 Requirements 5.1 Chemical analysis The content of calcium and phosphorus of the hydroxyapatite ceramic coating shall be determined in accordance with ISO 13779-3. The calcium to phosphorus ratio, Ca:P, shall have a value in the range of 1,67 to 1,76 for the atomic ratio. This shall be determined as specified in ISO 13779-3. 5.2 Elements The limits of specific trace elements for ceramic hydroxyapatite are given in Table 1. The maximum allowable limit for metals having adverse biological reactions shall be a total of 50 mg/kg. The trace element levels shall be determined as specified in ISO 13779-3. Assessment of the risk posed by other chemical impurities shall be in accordance with ISO 10993-17. Table 1 — Limits of specific trace elements Trace element Maximum limit mg/kg Arsenic 3 Cadmium 5 Mercury 5 Lead 30 5.3 Crystalline phase compositions Allowed % mass fraction of crystalline phases: ⎯ hydroxyapatite shall be 50 % mass fraction or greater; ⎯ α-tricalcium phosphate (α-TCP), β-tricalcium phosphate (β-TCP), tetracalcium phosphate (TTCP) and calcium oxide (CaO) shall each be equal to or less than 5 % mass fraction. 5.4 Crystallinity value The hydroxyapatite phase (50 % mass fraction or higher) shall have a crystallinity value not less than 45 % of the 100 % crystalline hydroxyapatite standard value as determined by ISO 13779-3. 5.5 Adhesion to substrate The adhesion to the substrate shall be determined in accordance with the method described in ISO 13779-4. At least 6 specimens shall be tested. Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 13779-2:2008(E) © ISO 2008 – All rights reserved 3The mean coating adhesion strength shall be W 15 MPa unless a lower value can be justified based on the intended application. NOTE In some applications, a higher value can be recommended. Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 13779-2:2008(E) 4 © ISO 2008 – All rights reservedBibliography [1] ISO 5961:1994, Water quality — Determination of cadmium by atomic absorption spectrometry [2] ISO 8288, 1986, Water quality — Determination of cobalt, nickel, copper, zinc, cadmium and lead — Flame atomic absorption spectrometric methods [3] ASTM F 1147-05, Standard Test Method for Tension Testing of Calcium Phosphate and Metal Coatings [4] ASTM F 1609-03, Standard Specification for Calcium Phosphate Coatings for Implantable Materials [5] ASTM F 1185-03, Standard Specification for Composition of Hydroxyapatite for Surgical Implants [6] ASTM C 633-79, 2001, Standard Test Method for Adhesion or Cohesion Strength of Thermal Spray Coatings [7] NF S 94-065, Materials for surgical implants — Determination of arsenic, mercury, cadmium and lead on coatings based on phosphate of calcium [8] NF S 94-066, Materials for surgical implants — Quantitative determination of the Ca/P ratio of calcium phosphate [9] NF S 94-067, Materials for surgical implants — Qualitative and quantitative determination of the foreign phases present in calcium phosphate based powders, deposits and ceramics [10] NF S 94-068, Materials for surgical implants — Determination of the crystallinity and apparent size of the apatite crystallites of hydroxyapatite based powders, deposits and ceramics [11] NF S 94-072, Materials for surgical implants — determination of tensile adherence of phosphocalcic materials for biomedical applications [12] NF S 94-071, Materials for surgical implants — determination of the surface finish of coatings used for biomedical applications [13] BS 5350 part C15:1990, Methods of test for adhesives. Adhesively bonded joints: mechanical tests. Determination of bond strength in compressive shear [14] JIS H 8666, Test methods for Ceramic Sprayed Coatings [15] ICDD cards 9-432, 9-348, 9-169, 25-1137, 37-1497, 9-80, 9-77, 14-1475, 5-586 X-ray diffraction standards for hydroxyapatite, α-tri-calciumorthophosphate, β-tri-calciumorthophosphate, tetra-calciumphosphate, calcium oxide, monetite, brushite, aragonite, calcite [16] Hydroxyapatite Ceramic — A Decade of Experience in Hip Arthroplasty, Symposium at Royal College of Surgeons, London, November 1995 [17] DE GROOT, K. et al., J. Biomed. Mater. Res., 21, 1375 ff, 1987 [18] MORONI, A. et al., Bone Ingrowth Analysis and Interface Evaluation of Hydroxyapatite Coated Versus Uncoated Titanium Porous Bone Implants in Bioceramics, Yamamuro, T Kokubo, T Nakamura Editors, Bioceramics 5, Kobunshi Kankokai, Kyoto, pp. 299-305, 1992 [19] KLEIN, C.P.A.T. et al., Stability of calcium phosphate ceramics and plasma sprayed coating in Larry Hench & June Wilson (Eds), An Introduction to Bioceramics, World Scientific, pp. 199-221, 1993 Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 13779-2:2008(E) © ISO 2008 – All rights reserved 5[20] COOK, S.D. et al., Hydroxylapatite Coated Titanium for Orthopaedic Implant Applications, Clin. Orthop. Rel. Res., 232, pp. 225-243, 1988 [21] HASTINGS, G.W. et al., Hydroxyapatite coatings for biomaterials — A report of a multi-centre investigation in Ö H Andersson, R-P Happonen, A Yli-Urpo, (Eds), Bioceramics 7, Butterworth-Heinemann, Oxford, pp. 207-213, 1994 [22] TUDOR, A.M. et al., The analysis of biomedical hydroxyapatite powders and hydroxyapatite coatings on metallic implants by near IR Fourier Transform Raman Spectroscopy, Spectrochim. Acta, 49A, 4/6, pp. 675-680, 1993 [23] MEROLLI, A. TRANQUILLI, P., Crystallinity of the coating directs the in vivo response to hydroxyapatite in the rabbit in Ö H Andersson, R-P Happonen, A Yli-Urpo, (Eds), Bioceramics 7, Butterworth-Heinemann, Oxford, pp. 223-228, 1994 [24] Hydroxylapatite coatings in orthopaedic surgery, R.G.T. Geesink and M.T. Manley (Eds), Raven Press, New York, 1993 [25] Hideki Aoki, Medical Applications of Hydroxyapatite. Ishiyaku EuroAmerica, Tokyo, 1994 [26] BERNDT, C.C., Tensile Adhesion testing methodology for thermally sprayed coatings, J. Mater Eng. 12, pp. 151-158, 1990 [27] BERNDT, C.C. and LIN, C.K., Measurement of adhesion for thermally sprayed materials, Adhesion Sci Technol, 7, No. 12, pp. 1235-1264, 1993 [28] BERNDT, C.C. Instrumented tensile adhesion tests on plasma sprayed thermal barrier coating, J. Mater Eng, 11, pp. 275-282, 1989 [29] BERNDT, C.C. and MCPHERSON, R., The adhesion of flame and plasma sprayed coatings — A literature review, Australian Welding Research, January 1979 [30] Determining the adhesive/cohesive strength of thin thermal spray coatings, AWS Welding Journal, 1978 Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 13779-2:2008(E) ICS 11.040.40 Price based on 5 pages © ISO 2008 – All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---