1、BSI Standards Publication PD ISO/TS 11405:2015 Dentistry Testing of adhesion to tooth structurePD ISO/TS 11405:2015 PUBLISHED DOCUMENT National foreword This Published Document is the UK implementation of ISO/TS 11405:2015. The UK participation in its preparation was entrusted to Technical Committee
2、 CH/106/1, Dental restorative and orthodontic materials. 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 responsible for its correct application. The
3、British Standards Institution 2015. Published by BSI Standards Limited 2015 ISBN 978 0 580 81375 7 ICS 11.060.10 Compliance with a British Standard cannot confer immunity from legal obligations. This Published Document was published under the authority of the Standards Policy and Strategy Committee
4、on 31 January 2015. Amendments issued since publication Date Text affectedPD ISO/TS 11405:2015 ISO 2015 Dentistry Testing of adhesion to tooth structure Art dentaire Essais dadhsion la structure de la dent TECHNICAL SPECIFICATION ISO/TS 11405 Reference number ISO/TS 11405:2015(E) Third edition 2015-
5、02-01PD ISO/TS 11405:2015ISO/TS 11405:2015(E)ii ISO 2015 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2015 All 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 pho
6、tocopying, or posting on the internet or an intranet, 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 office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749
7、09 47 E-mail copyrightiso.org Web www.iso.org Published in SwitzerlandPD ISO/TS 11405:2015ISO/TS 11405:2015(E)Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Sampling 2 5 Test methods . 2 5.1 Bond strength tests . 2 5.1.1 General 2 5.1.2 T
8、ooth substrate and storage 3 5.1.3 Treatment of results 4 5.1.4 Tensile bond strength 5 5.2 Gap measurement test for adhesion to dentine . 6 5.2.1 General 6 5.2.2 Tooth substrate and storage 7 5.2.3 Cavity preparation 7 5.2.4 Filling procedure 7 5.2.5 Storage of specimen 7 5.2.6 Gap measurement . 7
9、5.3 Microleakage test 7 5.3.1 General 7 5.3.2 Tooth substrate and storage 8 5.3.3 Cavity preparation 8 5.3.4 Filling procedure 8 5.3.5 Storage of specimens . . 8 5.3.6 Measurement of microleakage. 8 5.3.7 Treatment of results 9 5.4 Clinical usage tests . 9 5.4.1 Introduction . 9 5.4.2 Method 9 5.4.3
10、 Restorations . 9 5.4.4 Study duration . 9 5.4.5 Sample size . 9 5.4.6 Clinical procedures 9 5.4.7 Evaluation 9 5.4.8 Treatment of results.10 Annex A (informative) Examples of test methods for measurement of bond strength.11 Bibliography .12 ISO 2015 All rights reserved iiiPD ISO/TS 11405:2015ISO/TS
11、 11405:2015(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 subjec
12、t 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)
13、 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 approval criteria needed for the different types of ISO documents should be no
14、ted. This document was 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 identifyin
15、g 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 (see www.iso.org/patents). Any trade name used in this document is information given for the convenience
16、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 Barriers to Trade (TBT), see the following URL: Foreword - Sup
17、plementary Information. The committee responsible for this document is ISO/TC 106, Dentistry, Subcommittee SC 1, Filling and restorative materials. This third edition cancels and replaces the second edition (ISO/TS 11405:2003), which has been technically revised.iv ISO 2015 All rights reservedPD ISO
18、/TS 11405:2015ISO/TS 11405:2015(E) Introduction Adhesion in restorative dentistry is an important topic. It is the intention of this Technical Specification to describe different laboratory and clinical procedures whereby the effect or quality of a bond between a dental material and tooth structure
19、may be substantiated. By gaining experience with different testing methods, a correlation between laboratory and clinical performance of the materials may be sought. Adhesive materials are used in many types of restorative and preventive work. Even if the stress on the bond in most circumstances may
20、 be defined as either tensile, shear, or a combination of these, there are no specific laboratory or clinical tests which may be valid for all the various clinical applications of adhesive materials. The relative performance of materials that are claimed to bond to tooth structure has been examined
21、by laboratory assessment of bond strength. While bond strengths may not predict exact clinical behaviour, they could be useful for comparing adhesive materials. ISO 29022 1describes the notched-edge shear bond strength test which is an important publication in the subject. Annex A lists several publ
22、ished laboratory methods for tensile bond strength measurement. Adhesion testing is also common in general materials in science and a publication listing where many systems have been provided with information. 2 ISO 2015 All rights reserved vPD ISO/TS 11405:2015PD ISO/TS 11405:2015Dentistry Testing
23、of adhesion to tooth structure 1 Scope This Technical Specification gives guidance on substrate selection, storage, and handling as well as essential characteristics of different test methods for quality testing of the adhesive bond between restorative dental materials and tooth structure, i.e. enam
24、el and dentine. It includes a tensile bond strength measurement test, a test for measurement of marginal gaps around fillings, a microleakage test, and gives guidance on clinical usage tests for such materials. Some specific test methods for bond strength measurements are given for information in An
25、nex A. This Technical Specification does not include requirements for adhesive materials and their performance. 2 Normative references The following referenced documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references,
26、 only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1942:2009, Dentistry Vocabulary ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 3823-1:1997, Dental rotary instruments
27、Burs Part 1: Steel and carbide burs ISO 6344-1:1998, Coated abrasives Grain size analysis Part 1: Grain size distribution test ISO 14155, Clinical investigation of medical devices for human subjects Good clinical practice 3 T erms a nd definiti ons For the purposes of this document, the terms and de
28、finitions given in ISO 1942 and the following definitions apply. 3.1 adhere to be in a state of adherence (3.2) 3.2 adherence state in which two surfaces are held together by interfacial forces 3.3 adherend body that is held or is intended to be held to another body by an adhesive (3.5) 3.4 adhesion
29、 state in which two surfaces are held together by chemical or physical forces, or both, with the aid of an adhesive (3.5) 3.5 adhesive substance capable of holding materials together TECHNICAL SPECIFICATION ISO/TS 11405:2015(E) ISO 2015 All rights reserved 1PD ISO/TS 11405:2015ISO/TS 11405:2015(E) 3
30、.6 bond strength force per unit area required to break a bonded assembly with failure occurring in or near the adhesive (3.5)/adherend (3.3) interface 3.7 microleakage passage of substances such as saliva, ions, compounds, or bacterial by-products between a cavity wall and the restorative material 3
31、.8 substrate material upon the surface of which an adhesive (3.5) is spread for any purpose such as bonding or coating 4 Sampling The amount of test material should be sufficient for all planned tests and be from the same batch. 5 Test methods This Technical Specification describes essential charact
32、eristics of various types of tests such as: a) tensile bond strength measurement; b) gap measurement tests for adhesion to dentine; c) microleakage tests; d) clinical usage tests. NOTE See Reference 1 for shear bond strength. For substrate selection, storage, and handling, specific characteristics a
33、re described in detail. For the apparatus used for bond strength measurements, general guidelines are given. It is not the intention to recommend the testing of each material by every test as some tests will not be appropriate. However, the quality and sophistication of a laboratory test may not com
34、pensate for the fact that the final evidence of adhesive properties should be a clinical usage test. 5.1 Bond strength tests 5.1.1 General Adhesive materials are used for many different purposes in the mouth. The choice of test should be considered according to the intended use of the material. ISO
35、29022 1describes the ISO standard shear bond strength test for evaluating direct dental restorative materials. This Technical Specification describes a tensile bond strength test. In addition, several variations are described such as application in thin film and bulk, short, or long exposure time to
36、 a wet environment. A set of tests may be necessary to evaluate properly the bond strength of a material. When bond strength is to be measured, the raw data will be in units of force (N). It is necessary to convert this into stress units, i.e. force per unit area (MPa). Hence, control of the area an
37、d smoothness of the surface for application of the adhesive material is important. Several pieces of apparatus are available for measuring the tensile or shear bond strength of an adhesive system. The critical requirements for selection of a suitable instrument for the small and sometimes, fragile s
38、pecimens are the following: the ability to mount the tooth/material specimen in the apparatus and the universal testing machine without application of load (tensile, bending, shear, or torsion) on the specimen;2 ISO 2015 All rights reservedPD ISO/TS 11405:2015ISO/TS 11405:2015(E) a rigid constructio
39、n in order to avoid elastic deformation (or displacement) of the apparatus and the connection to the testing machine; for tensile testing, the ability to apply a slowly increasing and unidirectional tensile load and the ability to align the specimen to avoid an uneven stress distribution during load
40、ing. Large differences in bond strength results between different laboratories are common. Absolute values should therefore be treated with caution and it may be more appropriate to compare the ranking of materials. In some circumstances, bond strength tests are only useful for screening. They may a
41、llow only rough guidance with respect to the clinical performance of an adhesive system. Low values are more likely correlated with poor clinical performance namely retention in adhesive cavities. However, bond strength values above a certain threshold value might not indicate better clinical perfor
42、mance. 5.1.2 Tooth substrate and storage 5.1.2.1 Substrate Use either human permanent premolars/molars or bovine mandibular incisors of animals for the measurement of bond strength. The donor bovine animals should not be more than five years old. When measuring bond strength to human dentine, this T
43、echnical Specification recommends to use the buccal superficial dentine that is as close to enamel as possible in order to reduce variations. It is preferable to use third permanent molars from 16-year-old to 40-year-old individuals, if possible. 5.1.2.2 Time after extraction There is increasing evi
44、dence that changes in dentine occurring after extraction that may influence bond strength measurements. The effect may vary with different types of bonding materials. Ideally, bond strengths should be measured immediately post-extraction, but this is not generally feasible. It appears that most chan
45、ges occur in the initial days or weeks after extraction and therefore, teeth one month, but not more than six months, after extraction should be used. Teeth that have been extracted for longer than six months may undergo degenerative changes in dentinal protein. 5.1.2.3 Condition of teeth Human teet
46、h used for bond strength measurement should be caries-free and preferably unrestored. However, small and superficial restorations not in the adhesion test area may be acceptable. Root filled teeth should not be used. There is some evidence to suggest that different teeth in the dentition may give di
47、fferent results with bonding to dentine and enamel. It is not possible to have complete control of variables such as the age of the donating patient, cultural and dietary history, state of health, or to standardize the composition and structure of the teeth. 5.1.2.4 Storage of teeth Immediately afte
48、r extraction, human teeth should be thoroughly washed in running water and all blood and adherent tissue removed, preferably by the clinician using sharp hand instruments. Bovine teeth should be cleaned as soon as possible after extraction and the soft tissue in the pulp chamber should be removed in
49、 a similar fashion. Teeth should then be placed in distilled water of grade 3 in accordance with ISO 3696:1987 or in a 1,0 % chloramine-T trihydrate bacteriostatic/bacteriocidal solution for a maximum of one week and thereafter, stored in distilled water (ISO 3696:1987, grade 3) in a refrigerator, i.e. nominal 4 C. To minimize deterioration, the storage medium should be replaced at least once every two months. It is essential that no other chemical agents be used as they may be absorbed by tooth substance and alter its
