BS ISO 13779-6-2015 Implants for surgery Hydroxyapatite Powders《外科植入物 羟磷灰石 粉末》.pdf

1、BSI Standards PublicationBS ISO 13779-6:2015Implants for surgery HydroxyapatitePart 6: PowdersBS ISO 13779-6:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 13779-6:2015.The UK participation in its preparation was entrusted to TechnicalCommittee CH/150/1,

2、Materials for surgical implants.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution

3、 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 79882 5ICS 11.040.40Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 January 2015.Amendments issued s

4、ince publicationDate Text affectedBS ISO 13779-6:2015 ISO 2015Implants for surgery Hydroxyapatite Part 6: PowdersImplants chirurgicaux Hydroxyapatite Partie 6: PoudresINTERNATIONAL STANDARDISO13779-6First edition2015-01-15Reference numberISO 13779-6:2015(E)BS ISO 13779-6:2015ISO 13779-6:2015(E)ii IS

5、O 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015All 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

6、, without prior written permission. Permission 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

7、SwitzerlandBS ISO 13779-6:2015ISO 13779-6:2015(E)Contents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Requirements 34.1 General . 34.2 Calcium to phosphorus molar ratio (Ca/P) 34.3 Trace elements 34.4 Qualitative and quantitative determination of fore

8、ign phases 44.5 Powder morphology . 54.6 Granulometry . 54.7 Calcination loss . 55 Manufacturing design requirement . 56 Certificate of compliance . 5Annex A (informative) Other possible characterization tests 7Bibliography 9 ISO 2015 All rights reserved iiiBS ISO 13779-6:2015ISO 13779-6:2015(E)Fore

9、wordISO (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 techni

10、cal 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 e

11、lectrotechnical 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 approval criteria needed for the different types of ISO documents should be noted. This document wa

12、s drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).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 pate

13、nt 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 (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not c

14、onstitute 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 Barriers to Trade (TBT), see the following URL: Foreword Supplementary information .Th

15、e committee responsible for this document is ISO/TC 150, Implants for surgery, Subcommittee SC 1, Materials.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 analy

16、sis and characterization of crystallinity and phase purity Part 4: Determination of coating adhesion strength Part 6: Powdersiv ISO 2015 All rights reservedBS ISO 13779-6:2015ISO 13779-6:2015(E)IntroductionNo known surgical implant material has ever been shown to be completely free of adverse reacti

17、ons in the human body. However, long term clinical experience of the use of the material referred to in this part of ISO 13779 has shown that an acceptable level of biological response can be expected, if the material is used in appropriate applications.This part of ISO 13779 describes specification

18、s for hydroxyapatite raw material powders used to obtain high-quality medical devices. However, the quality of the final device depends on the manufacturing process and it is recognized that a separate performance standard can be necessary for each end-use product. ISO 2015 All rights reserved vBS I

19、SO 13779-6:2015BS ISO 13779-6:2015Implants for surgery Hydroxyapatite Part 6: Powders1 ScopeThis part of ISO 13779 specifies requirements for hydroxyapatite powders used as a raw material for the manufacturing of surgical implants or coating of surgical implants.This part of ISO 13779 does not apply

20、 to hydroxyapatite coatings, ceramic hydroxyapatite, glass ceramics, - and -tricalcium phosphate, or other forms of calcium phosphate.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated r

21、eferences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 2591-1, Test sieving Part 1: Methods using test sieves of woven wire cloth and perforated metal plateISO 13779-3, Implants for surgery Hydroxyapatit

22、e Part 3: Chemical analysis and characterization of crystallinity and phase purityISO 14971, Medical devices Application of risk management to medical devicesISO 24235, Fine ceramics (advanced ceramics, advanced technical ceramics) Determination of particle size distribution of ceramic powders by la

23、ser diffraction methodEuropean Pharmacopoeia 5.0: Tribasic calcium phosphate3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1atomisationprocess for producing more or less spherical agglomerates of powder particles (atomized powders) by spraying a

24、 suspension of particles followed by immediate drying3.2 tricalcium phosphate-TCPchemical compound with a crystallographic structure characterized by ICDD PDF 09-0348 (see Bibliography)Note 1 to entry: The chemical formula is Ca3(PO4)2.Note 2 to entry: International Centre for Diffraction Data Powde

25、r Diffraction File (ICDD PDF).INTERNATIONAL STANDARD ISO 13779-6:2015(E) ISO 2015 All rights reserved 1BS ISO 13779-6:2015ISO 13779-6:2015(E)3.3 tricalcium phosphate-TCPchemical compound with a crystallographic structure characterized by ICDD PDF 09-0169 (see Bibliography)Note 1 to entry: The chemic

26、al formula is Ca3(PO4)2.Note 2 to entry: International Centre for Diffraction Data Powder Diffraction File (ICDD PDF).3.4calcinationthermal treatment of the powder in order to remove volatile impurities or to change the density or specific surface area of the powder3.5calcium oxideCaOchemical compou

27、nd with a crystallographic structure characterized by ICDD PDF 4-0777 or 82-1690 (see Bibliography)Note 1 to entry: International Centre for Diffraction Data Powder Diffraction File (ICDD PDF).3.6crystallinity ratioratio between the mass fraction of crystalline hydroxyapatite and the total mass frac

28、tion of hydroxyapatite (crystalline and amorphous)3.7D50particle diameter corresponding to 50 % of the cumulative undersize volume distributionNote 1 to entry: On a volumetric basis size distribution, 50 % of the particles is smaller than D50.3.8D10particle diameter corresponding to 10 % of the cumu

29、lative undersize volume distributionNote 1 to entry: On a volumetric basis size distribution, 10 % of the particles is smaller than D10.3.9D90particle diameter corresponding to 90 % of the cumulative undersize volume distributionNote 1 to entry: On a volumetric basis size distribution, 90 % of the p

30、articles is smaller than D90.3.10foreign phasecrystalline phase other than hydroxyapatite3.11grindingprocess for reducing the size of the raw powder particles3.12hydroxyapatiteHAchemical compound with a crystallographic structure characterized by ICDD PDF 09-0432 or 72-1243 (see Bibliography)Note 1

31、to entry: The chemical formula is Ca10(PO4)6(OH)2.2 ISO 2015 All rights reservedBS ISO 13779-6:2015ISO 13779-6:2015(E)Note 2 to entry: International Centre for Diffraction Data Powder Diffraction File (ICDD PDF).3.13hydroxyapatite ceramichydroxyapatite which has been sintered into a body of high cry

32、stallinity3.14hydroxyapatite coatinghydroxyapatite which has been deposited onto the surface of a metallic or non-metallic substrateNote 1 to entry: Material deposition can be obtained either by means of a thermal spray process which produces a ceramic-type coating or by means of a solution-based te

33、chnique which may deposit hydroxyapatite directly or may require thermal or other treatment to convert it into a crystalline form.3.15pressingprocess for producing green (before sintering) ceramics under pressure causing the consolidation of powders to the shape of the die used3.16sinteringprocess f

34、or production of ceramics in which the application of heat promotes the coalescence of ceramic grains and causes a significant reduction of particle surface area and bulk volume to achieve densification and consequent increase in mechanical properties3.17specific surface areatotal surface area of th

35、e powder particles per unit of mass, m2g-13.18tetracalcium phosphateTTCPchemical compound with a crystallographic structure characterized by ICDD PDF 25-1137 or 70-1379 (see Bibliography)Note 1 to entry: The chemical formula is Ca4(PO4)2O.Note 2 to entry: International Centre for Diffraction Data Po

36、wder Diffraction File (ICDD PDF).4 Requirements4.1 GeneralThe minimum requirements for the hydroxyapatite powder are established in 4.2 to 4.7.According to the use of the hydroxyapatite powder, other characterization tests can be useful and should be conducted (see Annex A).4.2 Calcium to phosphorus

37、 molar ratio (Ca/P)The content of calcium and phosphorus of the hydroxyapatite powder shall be determined in accordance with ISO 13779-3.A calcium to phosphorus molar ratio, Ca/P, of 1,66 Ca/P 1,71 is suitable to fit the requirements of ISO 13175-3, ISO 13779-1, and ISO 13779-2.4.3 Trace elementsThe

38、 limits of specific trace elements for hydroxyapatite powders are given in Table 1. ISO 2015 All rights reserved 3BS ISO 13779-6:2015ISO 13779-6:2015(E)Either inductively coupled plasma/atomic emission spectrometry (ICP/AES), inductively coupled plasma/mass spectroscopy (ICP/MS), atomic absorption s

39、pectroscopy (AAS), or the method specified in ISO 13779-3 shall be used to quantify trace elements. The method used shall be specified and validated.The maximum allowable limit of the sum of all heavy metals shall be 30 mg/kg. Method A ( 2.4.8.) described in European Pharmacopoeia for tribasic calci

40、um phosphate shall be used to quantify heavy metals. It is also possible to use one of the methods described above for the quantification of trace elements considering that the total amount of heavy metals is the sum of the following elements: lead; mercury; bismuth; arsenic; antimony; tin; cadmium;

41、 silver; copper; molybdenum.The method used shall be specified.Any chemical element except for calcium, phosphorus, hydrogen, and oxygen likely to be present with a mass fraction more than 500 mg/kg shall be identified. Identification of these elements shall be based on a risk analysis of the proces

42、s of the manufacturer of the powder, performed according to ISO 14971. These elements shall be quantified and if present with a mass fraction more than 500 mg/kg, the element content shall be indicated on the certificate of compliance of the batch.Table 1 Limits of specific trace elementsElementMaxi

43、mum limit mg/kgArsenic 3Cadmium 5Mercury 5Lead 30Total heavy metals 30Total heavy metals specified in Table 1 is more restrictive than in other parts of ISO 13779 or ISO 13175-3 as it is considered that a raw material shall have a higher purity than the finished product to take into account possible

44、 pollution by the process.4.4 Qualitative and quantitative determination of foreign phasesCrystallinity ratio determination shall be performed in accordance with ISO 13779-3.Quantification of foreign phases shall be performed in accordance with ISO 13779-3. If the crystallinity ratio of the raw powd

45、er is 95 %, it is not necessary to perform calcination of the sample before the quantification of foreign phases. Otherwise, the sample shall be calcined for 15 h at (1 000 25) C before the quantification of foreign phases.4 ISO 2015 All rights reservedBS ISO 13779-6:2015ISO 13779-6:2015(E)The CaO c

46、ontent shall be not more than 1 %. The sum of -TCP, -TCP, TTCP, and CaO content shall be not more than 5 % (-TCP, -TCP, TTCP, or CaO content shall be considered as zero if their value is below the detection threshold). The detection threshold for each phase (-TCP, -TCP, TTCP, and CaO) shall be not m

47、ore than 1 %.Some crystalline foreign phases such as carbonated apatite and hydrogenophosphate phases may be present in the hydroxyapatite powder and will not be detected by X-ray diffraction as per ISO 13779-3 after calcination at 1 000C. For qualitative determination of the foreign phases includin

48、g carbonated apatite and hydrogenophosphate phases, a method is proposed in A.3.4.5 Powder morphologyThe nature of the powder (ground or atomized) shall be specified.The powder morphology shall be described and documented by optical microscopy (OM) or scanning electron microscopy (SEM) pictures at d

49、ifferent scales.4.6 GranulometryD10, D50, and D90shall be specified.If laser diffraction is used, it shall be in accordance with ISO 24235.If a sieving method is used, it shall be in accordance with ISO 2591-1. If another method is used, it shall be specified and justified.4.7 Calcination lossDefine the calcination loss only for powders which have a crystallinity ratio 95 % when tested in accordance with ISO 13779-3.Calcination loss shall be specified for a treatment of 1 h at (1 000 25) C.