SVENSK STANDARD SS-EN ISO 13356:2015 Fastställd/Approved: 2015-10-04 Publicerad/Published: 2015-10-19 Utgåva/Edition: 2 Språk/Language: engelska/english ICS: 11.040.40; 11.060.15 Kirurgiska implantat Keramiska material Yttriumoxidstabiliserad tetragonal zirkoniumoxid (ISO 13356:2015) Implants for surgery Ceramic materials based on yttriastabilized tetragonal zirconia (Y-TZP) (ISO 13356:2015)
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Europastandarden EN ISO 13356:2015 gäller som svensk standard. Detta dokument innehåller den officiella engelska versionen av EN ISO 13356:2015. Denna standard ersätter SS-EN ISO 13356:2013, utgåva 1. The European Standard EN ISO 13356:2015 has the status of a Swedish Standard. This document contains the official English version of EN ISO 13356:2015. This standard supersedes the Swedish Standard SS-EN ISO 13356:2013, edition 1. Copyright / Upphovsrätten till denna produkt tillhör SIS, Swedish Standards Institute, Stockholm, Sverige. Användningen av denna produkt regleras av slutanvändarlicensen som återfinns i denna produkt, se standardens sista sidor. Copyright SIS, Swedish Standards Institute, Stockholm, Sweden. All rights reserved. The use of this product is governed by the end-user licence for this product. You will find the licence in the end of this document. Upplysningar om sakinnehållet i standarden lämnas av SIS, Swedish Standards Institute, telefon 08-555 520 00. Standarder kan beställas hos SIS Förlag AB som även lämnar allmänna upplysningar om svensk och utländsk standard. Information about the content of the standard is available from the Swedish Standards Institute (SIS), telephone +46 8 555 520 00. Standards may be ordered from SIS Förlag AB, who can also provide general information about Swedish and foreign standards. Denna standard är framtagen av kommittén för Tandvård, SIS / TK 327. Har du synpunkter på innehållet i den här standarden, vill du delta i ett kommande revideringsarbete eller vara med och ta fram andra standarder inom området? Gå in på www.sis.se - där hittar du mer information.
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 13356 September 2015 ICS 11.040.40 Supersedes EN ISO 13356:2013 English Version Implants for surgery - Ceramic materials based on yttriastabilized tetragonal zirconia (Y-TZP) (ISO 13356:2015) Implants chirurgicaux - Produits céramiques à base de zircone tétragonal stabilisée à l'yttrium (Y-TZP) (ISO 13356:2015) Chirurgische Implantate - Keramische Werkstoffe aus yttriumstabilisiertem tetragonalem Zirkonium (Y-TZP) (ISO 13356:2015) This European Standard was approved by CEN on 22 August 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 13356:2015 E
Contents Page European foreword... Introduction...v 1 Scope... 1 2 Normative references... 1 3 Physical and chemical properties... 2 3.1 Test category... 2 3.1.1 General... 2 3.1.2 Category 1... 2 3.1.3 Category 2... 2 4 Test methods... 4 4.1 General... 4 4.2 Bulk density... 4 4.3 Chemical composition... 4 4.4 Microstructure... 4 4.4.1 Principle... 4 4.4.2 Test report... 5 4.4.3 Amount of monoclinic phase... 5 4.5 Biaxial flexural strength... 6 4.5.1 Principle... 6 4.5.2 Apparatus... 6 4.5.3 Preparation of test specimens... 6 4.5.4 Procedure... 7 4.5.5 Calculation of results... 8 4.5.6 Test report... 8 4.6 Four-point bending strength... 8 4.7 Weibull modulus... 9 4.8 Young s modulus... 9 4.9 Hardness... 9 4.10 Cyclic fatigue... 9 4.10.1 Principle... 9 4.10.2 Apparatus... 9 4.10.3 Sample size and preparation of test specimens... 9 4.10.4 Procedure and sample requirement... 9 4.10.5 Test Report...10 4.11 Radioactivity...10 4.11.1 Principle...10 4.11.2 Apparatus...10 4.11.3 Sample preparation...11 4.11.4 Isotope identification - Energy calibration...11 4.11.5 Quantitative analysis...11 4.11.6 Expression of results...12 4.11.7 Test report...12 4.12 Accelerated aging test...12 4.12.1 General...12 4.12.2 Procedure...12 4.12.3 Evaluation of accelerated aging outcome...12 Bibliography...13 iii
European foreword This document (EN ISO 13356:2015) has been prepared by Technical Committee ISO/TC 106 Dentistry in collaboration with Technical Committee CEN/TC 55 Dentistry the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 2016, and conflicting national standards shall be withdrawn at the latest by March 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 13356:2013. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 13356:2015 has been approved by CEN as EN ISO 13356:2015 without any modification. iv
Introduction No known surgical implant material has ever been found to cause absolutely no adverse reactions in the human body. However, long-term clinical experience regarding the use of the material referred to in this International Standard has shown that an acceptable level of biological response can be expected if the material will be used in appropriate applications. v
Implants for surgery Ceramic materials based on yttriastabilized tetragonal zirconia (Y-TZP) 1 Scope This International Standard specifies the requirements and corresponding test methods for a biocompatible and biostable ceramic bone-substitute material based on yttria-stabilized tetragonal zirconia (yttria tetragonal zirconia polycrystal, Y-TZP) for use as a material for surgical implants. 2 Normative references The 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 document (including any amendments) applies. ISO 3310 1, Test sieves Technical requirements and testing Part 1: Test sieves of metal wire cloth ISO 3611, Geometrical product specifications (GPS) Dimensional measuring equipment: Micrometers for external measurements Design and metrological characteristics ISO 7500 1, Metallic materials Verification of static uniaxial testing machines Part 1: Tension/compression testing machines Verification and calibration of the force-measuring system ISO 13383 1, Fine ceramics (advanced ceramics, advanced technical ceramics) Microstructural characterization Part 1: Determination of grain size and size distribution ISO 14704, Fine ceramics (advanced ceramics, advanced technical ceramics) Test method for flexural strength of monolithic ceramics at room temperature ISO 14705, Fine ceramics (advanced ceramics, advanced technical ceramics) Test method for hardness of monolithic ceramics at room temperature ISO 17561, Fine ceramics (advanced ceramics, advanced technical ceramics) - Test method for elastic moduli of monolithic ceramics at room temperature by sonic resonance ISO 18754, Fine ceramics (advanced ceramics, advanced technical ceramics) Determination of density and apparent porosity ISO 20501, Fine ceramics (advanced ceramics, advanced technical ceramics) Weibull statistics for strength data ISO 22214, Fine ceramics (advanced ceramics, advanced technical ceramics) Test method for cyclic bending fatigue of monolithic ceramics at room temperature EN 623 2, Advanced technical ceramics Monolithic ceramics General and textural properties Part 2: Determination of density and porosity EN 843 2, Advanced technical ceramics Mechanical properties of monolithic ceramics at room temperature Part 2: Determination of Young s modulus, shear modulus and Poisson s ratio EN 843 4, Advanced technical ceramics Mechanical properties of monolithic ceramics at room temperature Part 4: Vickers, Knoop and Rockwell superficial hardness EN 843 5, Advanced technical ceramics Mechanical properties of monolithic ceramics at room temperature Part 5: Statistical analysis 1
ASTM C1161, Standard Test Method for Flexural Strength of Advanced Ceramics at Ambient Temperature ASTM C1198, Standard Test Method for Dynamic Young s Modulus, Shear Modulus, and Poisson s Ratio for Advanced Ceramics by Sonic Resonance ASTM C1239, Standard Practice for Reporting Uniaxial Strength Data and Estimating Weibull Distribution Parameters for Advanced Ceramics ASTM C1259, Standard Test method for Dynamic Young s Modulus. Shear Modulus, and Poisson s Ratio for Advanced Ceramics by Impulse Excitation of Vibration ASTM C1327, Standard Test Method for Vickers Indentation Hardness of Advanced Ceramics ASTM C1331, Standard Test Method for Measuring Ultrasonic Velocity in Advanced Ceramics with Broadband Pulse-Echo Cross-Correlation Method ASTM E112, Standard Test Method for Determining Average Grain Size 3 Physical and chemical properties The physical and chemical properties, when tested as specified in Clause 4, shall comply with the values specified in Table 1. 3.1 Test category 3.1.1 General The required tests are divided into two categories. 3.1.2 Category 1 The following test shall be performed for periodical production control: a) bulk density; b) chemical composition; c) microstructure; d) strength (including Weibull modulus); e) accelerated aging (monoclinic fraction). 3.1.3 Category 2 The manufacturer shall define the general materials specification. In addition to all tests in 3.1.2, the following tests shall be performed to demonstrate compliance with the material specification: a) hardness; b) Young s modulus; c) fatigue strength; d) accelerated aging (strength); e) quantity of monoclinic phase; f) radioactivity. 2
Table 1 Limits for material properties Property Unit Test category Requirement Reference Subclause Bulk density g/cm3 1 6,00 ISO 18754 EN 623 2 4.2 Chemical composition 4.3 ZrO 2 +HfO 2 +Y 2 O 3 a 99,0 Y 2 O 3 > 4,5 to 6,0 HfO 2 % mass fraction 1 5 Al 2 O 3 0,5 Other oxides 0,5 Microstructure 4.4 Grain size μm 1 Intercept distance 0,4 ISO 13383 1 Standard deviation < 0,2 ASTM E112 Amount of monoclinic phase % molar fraction 2 20 See 4.4.3 Strength: alternative of 1) or 2) 1a) Biaxial flexurea 1 500 ASTM C1499 4.5 ISO 20501 1b) Weibull modulus 1 8 EN 843 5 4.7 ASTM C1239 MPa 2a) 4-point bendinga 1 800 2b) Weibull modulus 1 8 Young s modulus GPa 2 200 Hardness GPa 2 11,8 Cyclic fatigue limit stress at 106 cycles ISO 14704 EN 843 1 ASTM C1161 ISO 20501 EN 843 5 ASTM C 1239 ISO 17561 EN 843 2 ASTM C1198 ASTM C1259 ASTM C1331 ISO 14705 EN 843 4 ASTM C1327 MPa 2 320 ISO 22214 4.10 Radioactivityb Bq/kg 2 200 4.11 Accelerated aging 4.12 NOTE The number of fractional digits given for each limit value in this table indicates the appropriate number of fractional digits which should be given for the respective measured values. a Measured on a minimum of 10 test specimens. b The radioactivity, defined as the sum of the mass activity of U 238, Ra 226, Th 232, and determined by gamma spectroscopy on the ready-to-use powder should be equal or less than 200 Bq/kg. This value will be reviewed at the next revision of this International Standard and will be based upon the radioactivity data from implant ceramic manufacturers. All naturally occurring gamma emitters are to be analysed. 4.6 4.7 4.8 4.9 3