SIST EN ISO 13356:2013

Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2008)

This International Standard specifies the characteristics of, 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 material for surgical implants.

Chirurgische Implantate - Keramische Werkstoffe aus yttriumstabilisiertem tetragonalem Zirkondioxid (Y-TZP) (ISO 13356:2008)

Diese Internationale Norm legt die Eigenschaften und die dazugehörigen Prüfverfahren für ein biokompatibles und biostabiles keramisches Knochenersatzmaterial auf der Grundlage von yttriumstabi¬lisiertem tetragonalem Zirkondioxid (mit Yttrium teilstabi¬lisiertem, polykristallinem, tetragonalem Zirkondioxid, Y TZP) fest, das für chirurgische Implantate verwendet wird.

Implants chirurgicaux - Produits céramiques à base de zircone tétragonal stabilisé à l'oxyde d'yttrium (Y-TZP) (ISO 13356:2008)

L'ISO 13356:2008 spécifie les caractéristiques et les méthodes d'essai correspondantes des matériaux de biosubstitution osseuse, biocompatibles et biostables à base de zirconium tétragonal stabilisé à l'oxyde d'yttrium (polycristaux de zirconium tétragonal stabilisés à l'yttrium, Y-TZP), utilisés dans les matériaux constitutifs des implants chirurgicaux.

Vsadki (implantati) za kirurgijo - Keramični materiali na osnovi tetragonalnega cirkonija, stabiliziranega z itrijem (Y-TZP) (ISO 13356:2008)

Ta mednarodni standard določa lastnosti biozdružljivega in biostabilnega keramičnega materiala za kostne nadomestke na osnovi tetragonalnega cirkonija, stabiliziranega z itrijem, (z itrijem stabilizirani polikristal tetragonalnega cirkonija, Y-TZP) za uporabo kot material za kirurške vsadke ter ustrezne preskusne metode zanj.

General Information

• Status: Withdrawn
• Public Enquiry End Date: 14-Jan-2013
• Publication Date: 20-Aug-2013
• Withdrawal Date: 01-Nov-2015
• ICS: 11.040.40 - Implants for surgery, prosthetics and orthotics
• Technical Committee: VAZ - Healthcare
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 30-Oct-2015
• Due Date: 22-Nov-2015
• Completion Date: 02-Nov-2015
• Directive: 93/42/EEC - Council Directive 93/42/EEC of 14 June 1993 concerning medical devices
• Ref Project: EN ISO 13356:2013 - Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2008)

Relations

• Replaced By: SIST EN ISO 13356:2015 - Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2015)
• Effective Date: 01-Dec-2015
• Replaced By: SIST EN ISO 13356:2015 - Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2015)
• Effective Date: 08-Jun-2022

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 13356:2013
01-september-2013
9VDGNLLPSODQWDWL]DNLUXUJLMR.HUDPLþQLPDWHULDOLQDRVQRYLWHWUDJRQDOQHJD
FLUNRQLMDVWDELOL]LUDQHJD]LWULMHP<7=3,62
Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-
TZP) (ISO 13356:2008)
Chirurgische Implantate - Keramische Werkstoffe aus yttriumstabilisiertem tetragonalem
Zirkondioxid (Y-TZP) (ISO 13356:2008)
Implants chirurgicaux - Produits céramiques à base de zircone tétragonal stabilisé à
l'oxyde d'yttrium (Y-TZP) (ISO 13356:2008)
Ta slovenski standard je istoveten z: EN ISO 13356:2013
ICS:
11.040.40 Implantanti za kirurgijo, Implants for surgery,
protetiko in ortetiko prosthetics and orthotics
SIST EN ISO 13356:2013 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 13356:2013

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SIST EN ISO 13356:2013


EUROPEAN STANDARD
EN ISO 13356

NORME EUROPÉENNE

EUROPÄISCHE NORM
April 2013
ICS 11.040.40
English Version
Implants for surgery - Ceramic materials based on yttria-
stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2008)
Implants chirurgicaux - Produits céramiques à base de Chirurgische Implantate - Keramische Werkstoffe aus
zircone tétragonal stabilisé à l'oxyde d'yttrium (Y-TZP) (ISO yttriumstabilisiertem tetragonalem Zirkondioxid (Y-TZP)
13356:2008) (ISO 13356:2008)
This European Standard was approved by CEN on 28 March 2013.

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

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13356:2013: E
worldwide for CEN national Members.

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SIST EN ISO 13356:2013
EN ISO 13356:2013 (E)
Contents Page
Foreword .3

2

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SIST EN ISO 13356:2013
EN ISO 13356:2013 (E)
Foreword
The text of ISO 13356:2008 has been prepared by Technical Committee ISO/TC 150 “Implants for surgery” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 13356:2013 by
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 October 2013, and conflicting national standards shall be withdrawn at
the latest by October 2013.
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.
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 13356:2008 has been approved by CEN as EN ISO 13356:2013 without any modification.

3

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SIST EN ISO 13356:2013

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SIST EN ISO 13356:2013

INTERNATIONAL ISO
STANDARD 13356
Second edition
2008-06-01

Implants for surgery — Ceramic materials
based on yttria-stabilized tetragonal
zirconia (Y-TZP)
Implants chirurgicaux — Produits céramiques à base de zircone
tétragonal stabilisé à l'oxyde d'yttrium (Y-TZP)




Reference number
ISO 13356:2008(E)
©
ISO 2008

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SIST EN ISO 13356:2013
ISO 13356:2008(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 [e-mail]
Web www.iso.org
Published in Switzerland

ii © ISO 2008 – All rights reserved

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SIST EN ISO 13356:2013
ISO 13356:2008(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope .1
2 Normative references .1
3 Physical and chemical properties.2
4 Test methods.3
4.1 Bulk density.3
4.2 Chemical composition .3
4.3 Microstructure.3
4.4 Biaxial flexural strength .6
4.5 Four-point bending strength .9
4.6 Cyclic fatigue.9
4.7 Radioactivity.10
4.8 Accelerated Aging Test.12
Bibliography .13

© ISO 2008 – All rights reserved iii

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SIST EN ISO 13356:2013
ISO 13356:2008(E)
Foreword
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 13356 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 13356:1997) which has been technically
revised.
iv © ISO 2008 – All rights reserved

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SIST EN ISO 13356:2013
ISO 13356:2008(E)
Introduction
No known surgical implant material has ever been shown to cause absolutely no adverse reactions in the
human body. However, long-term clinical experience of the use of the material referred to in this International
Standard has shown that an acceptable level of biological response can be expected when the material is
used in appropriate applications.

© ISO 2008 – All rights reserved v

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SIST EN ISO 13356:2013

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SIST EN ISO 13356:2013
INTERNATIONAL STANDARD ISO 13356:2008(E)

Implants for surgery — Ceramic materials based on
yttria-stabilized tetragonal zirconia (Y-TZP)
1 Scope
This International Standard specifies the characteristics of, 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 material for surgical implants.
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 3611, Micrometer callipers for external measurement
ISO 7500-1:2004, Metallic materials — Verification of static uniaxial testing machines — Part 1:
Tension/compression testing machines — Verification and calibration of the force-measuring system
ISO 14704, Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for flexural
strength of monolithic ceramics at room temperature
ISO 18754, Fine ceramics (advanced ceramics, advanced technical ceramics) — Determination of density
and apparent porosity
EN 623-2, Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 2:
Determination of density and porosity
EN 623-3, Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 3:
Determination of grain size and size distribution (characterized by the Linear Intercept Method)
ASTM C1499, Standard Test Method for Monotonic Equibiaxial Flexural Strength of Advanced Ceramics at
Ambient Temperature
ASTM E112-96, Standard Test Methods for Determining Average Grain Size
ASTM G136-03, Standard Practice for Determination of Soluble Residual Contaminants in Materials by
Ultrasonic Extraction
1)
ASTM F1873-98 , Standard Specification for High-Purity Dense Yttria Tetragonal Zirconium Oxide
Polycrystal (Y-TZP) for Surgical Implant Applications

1) Standard since withdrawn.
© ISO 2008 – All rights reserved 1

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SIST EN ISO 13356:2013
ISO 13356:2008(E)
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.
Table 1 — Limits for material properties
Test method according to
Property Unit Requirement
subclause
3
Bulk density g/cm W 6,00 4.1
Chemical composition:
ZrO + HfO + Y O W 99,0
2 2 2 3
Y O > 4,5 to u 6,0
2 3
percent mass fraction 4.2
HfO u 5
2
Al O u 0,5
2 3
Other oxides u 0,5
Microstructure:
µm Intercept distance u 0,4 4.3
grain size
Microstructure:
Standard deviation < 0,18
amount of monoclinic 4.3.7
u 20 %
phase
a
Strength :
W 500 4.4
MPa
biaxial flexure or
W 800 4.5
4-point bending
Cyclic fatigue limit stress at
MPa W 320 4.6
6
10 cycles
b
Radioactivity Bq/kg u 200 4.7

Accelerated aging:

maximum amount of
u 25 %
 monoclinic phase

 after accelerated

 aging
4.8
W 500 MPa, and decrease
residual biaxial flexure
not more than 20 %
 strength

residual 4-point
W 800 MPa, and decrease
 bending strength
not more than 20 %
a
Measured on a minimum of 10 samples.
b 238 226 232
The radioactivity, defined as the sum of the mass activity of U, Ra, Th 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.
2 © ISO 2008 – All rights reserved

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SIST EN ISO 13356:2013
ISO 13356:2008(E)
4 Test methods
4.1 Bulk density
The bulk density shall be determined in accordance with ISO 18754 or EN 623-2.
4.2 Chemical composition
The chemical compositions should be determined by ICP-OES (Inductively Coupled Plasma — Optical
Emission Spectrometry), fluorescent X-ray, or atomic absorption spectrum analysis methods.
[1]
NOTE ISO 12677 can be used.
4.3 Microstructure
4.3.1 Principle
For describing the microstructure, the average grain size is determined by measuring the linear intercept size
in accordance with EN 623-3 or ASTM E112.
4.3.2 Apparatus
The apparatus shall consist of the following items:
4.3.2.1 Grinding and polishing devices, for preparing plane and smooth surfaces.
4.3.2.2 Furnace, capable of maintaining a temperature of 1 400 °C.
4.3.2.3 Scanning electron microscope.
4.3.3 Preparation of test piece
Test pieces shall be prepared in accordance with EN 623-3 and the following instructions.
a) Prepare test pieces of the zirconia ceramic using methods representative of the method of production of
parts for surgery, using the same precursor powder, pressing technique, pressure and firing conditions.
b) Grind one surface plane, polish it until the percentage of interpretable area is at least 90 % and thermally
etch in air at a low temperature of less than 200 °C from sintering temperature. The etching conditions
shall be specifically determined for each zirconia material.
c) Coat the polished surface by sputtering with a thin conductive layer, for example, gold or carbon.
NOTE A gold or a gold-platinum alloy can be used.
d) Five extra test pieces shall be made from the chosen flexure test sample. These test pieces shall be
made in the same way as described for each according to 4.4.3 for the biaxial test and 4.4.5 for the 4-
point bend test. The samples for microstructural analysis shall be chosen randomly from the flexure test
samples.
e) Each microstructure test sample shall be cut in half. If it is a disc it shall be cut diametrically, if a bar it
shall be cut lengthwise through the centre as shown in Figure 1. The piece may be sectioned further to
permit it to fit into the microscope (4.3.2.3), the positions for the micrographs being those determined for
the full section.
f) The surface shall then be thermally etched to produce appropriate grain relief, using typically
temperatures in the range 1 300 °C to 1 400 °C for 30 min to 60 min.
© ISO 2008 – All rights reserved 3

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SIST EN ISO 13356:2013
ISO 13356:2008(E)
g) Use
⎯ either a low vacuum electron microscope with optics capable of discerning the microstructure on a
sufficiently fine scale or
⎯ sputter a thin conducting coating of Au, Au-Pd or C sufficient to allow for conductivity of the beam
from the site
while retaining adequate feature resolution on the sample to allow analysis.
4.3.4 Procedure
Carry out the test in accordance with EN 623-3 or ASTM E112 and the following instructions.
a) Observe the microstructure using the scanning electron microscope (4.3.2.3) at a magnification sufficient
to clearly delineate grain boundaries. Using either lines drawn on photomicrographs or stage movement,
follow the general procedure described in EN 623-3 or ASTM E112 to measure the linear intercept sizes
of at least 250 grains in total over at least three fields of view on lines sufficiently long to encompass at
least 20 gra
...

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.WHWUDJRQDOQHJDChirurgische Implantate - Keramische Werkstoffe aus yttriumstabilisiertem tetragonalem Zirkondioxid (Y-TZP) (ISO 13356:2008)Implants chirurgicaux - Produits céramiques à base de zircone tétragonal stabilisé à l'oxyde d'yttrium (Y-TZP) (ISO 13356:2008)Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2008)11.040.40Implantanti za kirurgijo, protetiko in ortetikoImplants for surgery, prosthetics and orthoticsICS:Ta slovenski standard je istoveten z:FprEN ISO 13356kSIST FprEN ISO 13356:2013en01-februar-2013kSIST FprEN ISO 13356:2013SLOVENSKI
STANDARD



kSIST FprEN ISO 13356:2013



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
FINAL DRAFT
FprEN ISO 13356
September 2012 ICS 11.040.40 English Version
Implants for surgery - Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) (ISO 13356:2008)
Implants chirurgicaux - Produits céramiques à base de zircone tétragonal stabilisé à l'oxyde d'yttrium (Y-TZP) (ISO 13356:2008)
Chirurgische Implantate - Keramische Werkstoffe aus yttriumstabilisiertem tetragonalem Zirkondioxid (Y-TZP) (ISO 13356:2008) This draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical Committee CEN/TC 55.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. FprEN ISO 13356:2012: EkSIST FprEN ISO 13356:2013



FprEN ISO 13356:2012 (E) 2 Contents Page Foreword .3 kSIST FprEN ISO 13356:2013



FprEN ISO 13356:2012 (E) 3 Foreword The text of ISO 13356:2008 has been prepared by Technical Committee ISO/TC 150 “Implants for surgery” of the International Organization for Standardization (ISO) and has been taken over as FprEN ISO 13356:2012 by Technical Committee CEN/TC 55 “Dentistry” the secretariat of which is held by DIN. This document is currently submitted to the Unique Acceptance Procedure. Endorsement notice The text of ISO 13356:2008 has been approved by CEN as a FprEN ISO 13356:2012 without any modification.
kSIST FprEN ISO 13356:2013



kSIST FprEN ISO 13356:2013



Reference numberISO 13356:2008(E)© ISO 2008
INTERNATIONAL STANDARD ISO13356Second edition2008-06-01Implants for surgery —Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) Implants chirurgicaux — Produits céramiques à base de zircone tétragonal stabilisé à l'oxyde d'yttrium (Y-TZP)
kSIST FprEN ISO 13356:2013



ISO 13356:2008(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
[e-mail] Web
www.iso.org Published in Switzerland
ii © ISO 2008 – All rights reserved
kSIST FprEN ISO 13356:2013



ISO 13356:2008(E) © ISO 2008 – All rights reserved iiiContents Page Foreword.iv Introduction.v 1 Scope.1 2 Normative references.1 3 Physical and chemical properties.2 4 Test methods.3 4.1 Bulk density.3 4.2 Chemical composition.3 4.3 Microstructure.3 4.4 Biaxial flexural strength.6 4.5 Four-point bending strength.9 4.6 Cyclic fatigue.9 4.7 Radioactivity.10 4.8 Accelerated Aging Test.12 Bibliography.13
kSIST FprEN ISO 13356:2013



ISO 13356:2008(E) iv © ISO 2008 – All rights reserved Foreword 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 13356 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 13356:1997) which has been technically revised. kSIST FprEN ISO 13356:2013



ISO 13356:2008(E) © ISO 2008 – All rights reserved vIntroduction No known surgical implant material has ever been shown to cause absolutely no adverse reactions in the human body. However, long-term clinical experience of the use of the material referred to in this International Standard has shown that an acceptable level of biological response can be expected when the material is used in appropriate applications.
kSIST FprEN ISO 13356:2013



kSIST FprEN ISO 13356:2013



INTERNATIONAL STANDARD ISO 13356:2008(E) © ISO 2008 – All rights reserved 1Implants for surgery — Ceramic materials based on yttria-stabilized tetragonal zirconia (Y-TZP) 1 Scope This International Standard specifies the characteristics of, 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 material for surgical implants. 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 3611, Micrometer callipers for external measurement ISO 7500-1:2004, Metallic materials — Verification of static uniaxial testing machines — Part 1: Tension/compression testing machines — Verification and calibration of the force-measuring system ISO 14704, Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for flexural strength of monolithic ceramics at room temperature ISO 18754, Fine ceramics (advanced ceramics, advanced technical ceramics) — Determination of density and apparent porosity EN 623-2, Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 2: Determination of density and porosity EN 623-3, Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 3: Determination of grain size and size distribution (characterized by the Linear Intercept Method) ASTM C1499, Standard Test Method for Monotonic Equibiaxial Flexural Strength of Advanced Ceramics at Ambient Temperature ASTM E112-96, Standard Test Methods for Determining Average Grain Size ASTM G136-03, Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction ASTM F1873-98 1), Standard Specification for High-Purity Dense Yttria Tetragonal Zirconium Oxide Polycrystal (Y-TZP) for Surgical Implant Applications
1) Standard since withdrawn. kSIST FprEN ISO 13356:2013



ISO 13356:2008(E) 2 © ISO 2008 – All rights reserved 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. Table 1 — Limits for material properties Property Unit Requirement Test method according to subclause Bulk density g/cm3 W 6,00 4.1 Chemical composition: ZrO2 + HfO2 + Y2O3 Y2O3 HfO2 Al2O3 Other oxides percent mass fraction
W 99,0 > 4,5 to u 6,0 u 5 u 0,5 u 0,5 4.2 Microstructure:
grain size µm Intercept distance u 0,4 4.3 Microstructure:
amount of monoclinic
phase
Standard deviation < 0,18 u 20 % 4.3.7 Strength a:
biaxial flexure or
4-point bending MPa W 500 W 800 4.4 4.5 Cyclic fatigue limit stress at
106 cycles MPa W 320 4.6 Radioactivity b Bq/kg u 200 4.7 Accelerated aging:
maximum amount of
monoclinic phase
after accelerated
aging
residual biaxial flexure
strength
residual 4-point
bending strength
u 25 %
W 500 MPa, and decrease not more than 20 %
W 800 MPa, and decrease not more than 20 % 4.8 a Measured on a minimum of 10 samples. b The radioactivity, defined as the sum of the mass activity of 238U, 226Ra, 232Th 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. kSIST FprEN ISO 13356:2013



ISO 13356:2008(E) © ISO 2008 – All rights reserved 34 Test methods 4.1 Bulk density The bulk density shall be determined in accordance with ISO 18754 or EN 623-2. 4.2 Chemical composition The chemical compositions should be determined by ICP-OES (Inductively Coupled Plasma — Optical Emission Spectrometry), fluorescent X-ray, or atomic absorption spectrum analysis methods. NOTE ISO 12677[1] can be used. 4.3 Microstructure 4.3.1 Principle For describing the microstructure, the average grain size is determined by measuring the linear intercept size in accordance with EN 623-3 or ASTM E112. 4.3.2 Apparatus The apparatus shall consist of the following items: 4.3.2.1 Grinding and polishing devices, for preparing plane and smooth surfaces. 4.3.2.2 Furnace, capable of maintaining a temperature of 1 400 °C. 4.3.2.3 Scanning electron microscope. 4.3.3 Preparation of test piece Test pieces shall be prepared in accordance with EN 623-3 and the following instructions. a) Prepare test pieces of the zirconia ceramic using methods representative of the method of production of parts for surgery, using the same precursor powder, pressing technique, pressure and firing conditions. b) Grind one surface plane, polish it until the percentage of interpretable area is at least 90 % and thermally etch in air at a low temperature of less than 200 °C from sintering temperature. The etching conditions shall be specifically determined for each zirconia material. c) Coat the polished surface by sputtering with a thin conductive layer, for example, gold or carbon. NOTE A gold or a gold-platinum alloy can be used. d) Five extra test pieces shall be made from the chosen flexure test sample. These test pieces shall be made in the same way as described for each according to 4.4.3 for the biaxial test and 4.4.5 for the 4-point bend test. The samples for microstructural analysis shall be chosen randomly from the flexure test samples. e) Each microstructure test sample shall be cut in half. If it is a disc it shall be cut diametrically, if a bar it shall be cut lengthwise through the centre as shown in Figure 1. The piece may be sectioned further to permit it to fit into the microscope (4.3.2.3), the positions for the micrographs being those determined for the full section. f) The surface shall then be thermally etched to produce appropriate grain relief, using typically temperatures in the range 1 300 °C to 1 400 °C for 30 min to 60 min. kSIST FprEN ISO 13356:2013



ISO 13356:2008(E) 4 © ISO 2008 – All rights reserved g) Use ⎯ either a low vacuum electron microscope with optics capable of discerning the microstructure on a sufficiently fine scale or ⎯ sputter a thin conducting coating of Au, Au-Pd or C sufficient to allow for conductivity of the beam from the site while retaining adequate feature resolution on the sample to allow analysis. 4.3.4 Procedure Carry out the test in accordance with EN 623-3 or ASTM E112 and the following instructions. a) Observe the microstructure using the scanning electron microscope (4.3.2.3) at a magnification sufficient to clearly delineate grain boundaries. Using either lines drawn on photomicrographs or stage movement, follow the general procedure described in EN 623-3 or ASTM E112 to measure the linear intercept sizes of at least 250 grains in total over at least three fields of view on lines sufficiently long to encompass at least 20 grains, taking random orientations of measurement. Calibrate the magnification employed using a certified graticule or grid. The micrographs should be of sufficient magnification, approximately 10 000 ×. NOTE Alternatively a calibrated stage micrometer can be used. b) Align the cross section or cut fraction thereof so that the side of the bottom of the part when firing is at the bottom of the micrograph. c) Take micrographs for each of the five positions shown on the appropriate cross-section below. The micrographs should be of sufficient magnification, approximatel
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