1、BSI Standards PublicationBS ISO 13179-1:2014Implants for surgery Plasma-sprayed unalloyed titanium coatings on metallic surgical implantsPart 1: General requirementsBS ISO 13179-1:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 13179-1:2014. The UK partici
2、pation in its preparation was entrusted to TechnicalCommittee CH/150/1, Materials for surgical implants.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are
3、 responsible for its correct application. The British Standards Institution 2014.Published by BSI Standards Limited 2014ISBN 978 0 580 69651 0ICS 11.040.40Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the S
4、tandards Policy and Strategy Committee on 30 June 2014.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 13179-1:2014 ISO 2014Implants for surgery Plasma-sprayed unalloyed titanium coatings on metallic surgical implants Part 1: General requirementsImplants chirurgicaux
5、 Revtements en titane non-alli des implants chirurgicaux mtalliques, obtenus par projection plasma Partie 1: Exigences gnralesINTERNATIONAL STANDARDISO13179-1First edition2014-06-01Reference numberISO 13179-1:2014(E)BS ISO 13179-1:2014ISO 13179-1:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTE
6、CTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permi
7、ssion can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 13179-1:2014ISO 13179-1
8、:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 24 Requirements 24.1 Powder for plasma spraying 24.2 Chemical analysis 24.3 Morphology 34.4 Coating mechanical properties . 34.5 Audit control . 44.6 Significan
9、ce of numerical limits . 45 Test report . 4Bibliography 5BS ISO 13179-1:2014ISO 13179-1:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carrie
10、d 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. IS
11、O collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different
12、approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2. www.iso.org/directivesAttention is drawn to the possibility that some of the elements of this document may be the sub
13、ject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received. www.iso.org/patentsAny trade name
14、 used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical
15、 Barriers to Trade (TBT), see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 150, Implants for surgery, Subcommittee SC 1, Materials.ISO 13179 consists of the following parts, under the general title Implants for surgery Plasma-sprayed un
16、alloyed titanium coatings on surgical implants: Part 1: General requirementsiv ISO 2014 All rights reservedBS ISO 13179-1:2014ISO 13179-1:2014(E)IntroductionNo known surgical implant material has ever been found to be completely free of adverse reactions in the human body. However, long term clinica
17、l experience of the use of the material referred to in this Standard has shown that an acceptable level of biological response can be expected, if the material is used in appropriate applications. ISO 2014 All rights reserved vBS ISO 13179-1:2014BS ISO 13179-1:2014Implants for surgery Plasma-sprayed
18、 unalloyed titanium coatings on metallic surgical implants Part 1: General requirements1 ScopeThis part of ISO 13179 specifies general requirements for plasma-sprayed unalloyed titanium coatings on metallic surgical implants.This part of ISO 13179 applies to plasma spraying in air and in vacuum.This
19、 part of ISO 13179 does not apply to coatings made of other materials than unalloyed titanium or coatings realized by another technology than plasma spraying.NOTE 1 A quality management system can be useful, e.g. as described in ISO 13485. Requirements for the competence of testing laboratories can
20、be found in ISO/IEC 17025.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced docu
21、ment (including any amendments) applies.ISO 4287, Geometrical Product Specifications (GPS) Surface texture: Profile method Terms, definitions and surface texture parametersISO 5832-2, Implants for surgery Metallic materials Part 2: Unalloyed titaniumISO 10993-1, Biological evaluation of medical devi
22、ces Part 1: Evaluation and testing within a risk management processISO 14971, Medical devices Application of risk management to medical devicesASTM F1044, Standard Test Method for Shear Testing of Calcium Phosphate Coatings and Metallic CoatingsASTM F1147, Standard Test Method for Tension Testing of
23、 Calcium Phosphate and Metallic CoatingsASTM F1160, Standard Test Method for Shear and Bending Fatigue Testing of Calcium Phosphate and Metallic Medical and Composite Calcium Phosphate/Metallic CoatingsASTM F1580, Standard specification for Titanium and Titanium-6 Aluminium-4 alloy powders for coati
24、ngs of surgical implantsASTM F1854, Standard Test Method for Stereological Evaluation of Porous Coatings on Medical ImplantsASTM F1978, Standard Test Method for measuring abrasion resistance of metallic thermal spray coatings by using the Taber AbraserASTM E2371, Test Method for analysis of Titanium
25、 and Titanium Alloy by Atomic Emission Plasma SpectrometryINTERNATIONAL STANDARD ISO 13179-1:2014(E) ISO 2014 All rights reserved 1BS ISO 13179-1:2014ISO 13179-1:2014(E)3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1plasma sprayingmethod of the
26、rmal spraying that produces coatings using a plasma jet3.2plasma-sprayed unalloyed titanium coatingstitanium which has been deposited onto the surface of a substrate, by means of a plasma spraying process4 Requirements4.1 Powder for plasma sprayingThe powder used for plasma spraying shall comply wit
27、h ASTM F1580.4.2 Chemical analysis4.2.1 Chemical compositionNOTE Although this standard applies to both atmospheric and vacuum plasma spraying coatings the vacuum plasma sprayed coating chemical composition values are likely to be lower than for atmospheric plasma sprayed coatings.The chemical compo
28、sition of the unalloyed titanium plasma sprayed coatings shall be in accordance with Table 1.Table 1 Chemical compositionElementComposition limits(mass fraction)Carbon (C) 0,10 %Hydrogen (H) 0,20 %Iron (Fe) 0,60 %Nitrogen (N) 5,00 %Oxygen (O) 10,00 %Titanium (Ti) BalanceThe sum of the nitrogen, oxyg
29、en, hydrogen, carbon and iron, contents shall not be greater than 10 % mass fraction.NOTE If the mechanical properties specified in 4.4 are met and if there are no detrimental effects on the biocompatibility it can be acceptable to have higher limits for Hydrogen and Nitrogen content than those spec
30、ified above.A risk analysis of the plasma spraying process shall be conducted to determine the elements not listed in Table 1 and likely to have a mass fraction greater than 0,5 %. The exact mass fraction shall be determined and the limit shall be specified by the manufacturer of the coating. The in
31、fluence of these impurities on biocompatibility shall be assessed in accordance with ISO 10993-1.2 ISO 2014 All rights reservedBS ISO 13179-1:2014ISO 13179-1:2014(E)4.2.2 SamplingIn order to perform the chemical analysis of the coating, a minimum of 5 g of coating, which has been deposited onto a ti
32、tanium substrate coupon produced in accordance with ISO 5832-2, shall be removed. If the removal of 5 g of coating is not possible or not sensible, the sample weight may be decreased provided that the chemical analysis is not affected. The technique used to remove the coating shall not generate cont
33、amination of the coating. If a cleaning step is performed on the implants after coating, the same cleaning step shall be applied on the sample before analysis.4.2.3 Chemical analysis procedureIron content shall be determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) in acc
34、ordance with ASTM E2371.Nitrogen, oxygen, carbon and hydrogen content, shall be determined by combustion using a recognized validated method.The analysis accuracy with a level of confidence of 95 % shall be taken into account when claiming the conformity of the chemical analysis to the limits specif
35、ied in Table 1.EXAMPLE If the uncertainty for measuring the oxygen content is 1 % with a level of confidence of 95 %, the conformity shall be stated as 9 % for the measured values.4.3 MorphologyFor validation purposes the morphology tests shall be performed on the final device, if possible. If the m
36、orphology tests are not performed on the final device because the requirements of the applied standard cannot be met due to geometry of the device, coupons may be used and their representativeness to the final device shall be justified.The average thickness and the tolerances, in m, shall be determi
37、ned in accordance with ASTM F1854.Roughness (Ra or Rt), in m, shall be determined in accordance with ISO 4287. The evaluation length shall be at least 8 mm.For coatings having an average thickness 300 m, the average volume % void content and mean void intercept length, and/or average void content an
38、d intercept length at distinct levels through the coating thickness (“tissue interface gradient method”) shall be tested in accordance with ASTM F1854.4.4 Coating mechanical properties4.4.1 GeneralAt least 5 test samples, manufactured from the same substrate as the final implant, shall be used for t
39、he tests specified in 4.4.2 to 4.4.4. The same pre-treatments (e.g. cleaning, sand-blasting) and post-treatments (e.g. cleaning, sterilization) shall be applied to the test samples and the final implant.4.4.2 Static shear strengthWhen tested in accordance with ASTM F1044, the mean static shear stren
40、gth of the coating shall be greater than 20 MPa.4.4.3 Shear fatigue strengthWhen tested in accordance with ASTM F1160 with a shear fatigue maximum strain of at least 10 MPa, the coating shall withstand at least 107cycles without any failure. ISO 2014 All rights reserved 3BS ISO 13179-1:2014ISO 13179
41、-1:2014(E)4.4.4 Static tensile strengthWhen tested in accordance with ASTM F1147, the mean static tensile strength of the surface coating shall be greater than 22 MPa.4.4.5 Abrasion resistanceWhen tested in accordance with ASTM F1978, the abrasion loss of the surface coating shall be less than 65 mg
42、 after 100 cycles.4.5 Audit controlThe chemical composition, morphology and tensile strength of the coating shall be controlled periodically with a periodicity determined during the risk analysis in accordance with ISO 14971.Routine control procedures of the coating shall specify the type and time i
43、nterval of each control test.4.6 Significance of numerical limitsFor determination of compliance to all limits specified in any condition, the calculated or observed values shall be rounded to the nearest two significant digits after the decimal sign expressing the specified limit.NOTE For rounding
44、of numbers see ISO 80000-1:2009, Annex B.5 Test reportThe test report shall include at least the following information:a) identification of the test sample including source, date of receipt, form;b) number of test samples used for each test;c) the reference to the test method used;d) deviations from
45、 the test method used, if relevant;e) any unusual features observed during the tests;f) justification for any results removed from the data;g) chemical analysis results (see 4.2);h) morphology analysis results (see 4.3);i) mean static shear strength (see 4.4.2);j) shear fatigue strength (see 4.4.3);
46、k) mean static tensile strength (see 4.4.4);l) abrasion loss (see 4.4.5);m) dates of tests;n) identification of the laboratory carrying out the test;o) signature of the laboratory manager and operator.4 ISO 2014 All rights reservedBS ISO 13179-1:2014ISO 13179-1:2014(E)Bibliography1 ISO 5961, Water q
47、uality Determination of cadmium by atomic absorption spectrometry2 ISO 13485, Medical devices Quality management systems Requirements for regulatory purposes3 ISO 16429, Implants for surgery Measurements of open-circuit potential to assess corrosion behaviour of metallic implantable materials and me
48、dical devices over extended time periods4 ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories5 ISO 80000-1, Quantities and units Part 1: General6 ASTM F67, Standard Specification for Unalloyed Titanium for Surgical Implant Applications7 ASTM E1409, Standard
49、 Test Method for Determination of Oxygen and Nitrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Technique8 ASTM E1447, Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by Inert Gas Fusion Thermal Conductivity/Infrared Detection Method9 ASTM E1941, Standard Test Method for Determination of Carbon in Refractory and Reactive Metals and Their Alloys by Combustion Analysis ISO 2014 All rights reserved 5BS ISO 13179-1:2014ISO 13179-1:201
