ISO TS 16506-2017 Dentistry - Polymer-based luting materials containing adhesive components.pdf

1、 ISO 2017 Dentistry Polymer-based luting materials containing adhesive components Mdecine bucco-dentaire Produits de scellement base de polymres contenant des composants adhsifs TECHNICAL SPECIFICATION ISO/TS 16506 Reference number ISO/TS 16506:2017(E) First edition 2017-07 ISO/TS 16506:2017(E)ii IS

2、O 2017 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in Switzerland 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 photocopying, or posting on

3、 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 Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22

4、749 09 47 copyrightiso.org www.iso.org ISO/TS 16506:2017(E)Foreword v Introduction vi 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Classification 2 5 Performance issues . 2 5.1 Biocompatibility 2 5.2 Bond strength and physical and chemical performances 2 6 Sampling 3 7 Test me

5、thods . 3 7.1 General . 3 7.2 Test conditions 3 7.3 Inspection 3 7.4 Preparation of test specimens . 3 7.5 Film thickness 4 7.5.1 Apparatus . 4 7.5.2 Test procedure . 4 7.6 Working time 5 7.6.1 Apparatus . 5 7.6.2 Procedure . 5 7.7 Setting time 6 7.7.1 Apparatus . 6 7.7.2 Procedure . 7 7.8 Sensitivi

6、ty to ambient light 8 7.8.1 Apparatus . 8 7.8.2 Procedure . 9 7.9 Depth of cure 9 7.9.1 Apparatus . 9 7.9.2 Procedure . 9 7.10 Flexural strength 10 7.10.1 Apparatus 10 7.10.2 Preparation of test specimens .11 7.10.3 Procedure 12 7.10.4 Treatment of results.12 7.11 Water sorption .12 7.11.1 Apparatus

7、 12 7.11.2 Preparation of test specimens .13 7.11.3 Procedure 14 7.12 Colour stability .15 7.12.1 General.15 7.12.2 Apparatus 15 7.12.3 Preparation of test specimens .16 7.12.4 Procedure 16 7.12.5 Colour comparison 16 7.13 Radio-opacity 16 7.13.1 Preparation of test specimen .16 7.13.2 Test procedur

8、e 16 8 Packaging, marking, instructions and information to be supplied 16 8.1 Packaging 16 8.2 Marking 17 ISO 2017 All rights reserved iii Contents Page ISO/TS 16506:2017(E)8.2.1 Capsule or single-dose container .17 8.2.2 Multi-dose container .17 8.2.3 Outermost package .17 8.3 Manufacturers instruc

9、tions and information for the user 18 Annex A (informative) Test methods to determine shear bond strength to dentine 20 Annex B (informative) C ompact-sized fixing jigs for self-curing pr oc edur e 33 Annex C (informative) Bond strength to dentine and physical and chemical performances .37 Bibliogra

10、phy .41 iv ISO 2017 All rights reserved ISO/TS 16506:2017(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 commi

11、ttees. 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 I

12、nternational 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 approval criteria needed for the

13、 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 (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.

14、 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 (see www .iso .org/ patents). Any trade name used in thi

15、s document is information given for the convenience of users and does not constitute an endorsement. For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World T

16、rade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: w w w . i s o .org/ iso/ foreword .html. This document was prepared by Technical Committee ISO/TC 106, Dentistry, Subcommittee SC 1, Filling and restorative materials. ISO 2017 All rights reserved v IS

17、O/TS 16506:2017(E) Introduction This document provides test methods and information of performances for polymer-based restorative materials for luting which contain adhesive components. Test methods specified in this document used for a group of materials with varying compositions has proved difficu

18、lt to set performance limits. Evidence is needed from using this document to develop it into an International Standard. Specific qualitative and quantitative test methods for demonstrating freedom from unacceptable biological risks are not included in this document but it is recommended that, for as

19、sessment of such biological risks, reference should be made to ISO 10993-1 and ISO 7405.vi ISO 2017 All rights reserved Dentistry Polymer-based luting materials containing adhesive components 1 Scope This document specifies test methods and information of bond strength to dentine and physical and ch

20、emical performances of dental polymer-based luting materials containing adhesive components. The materials are supplied in a form suitable for mechanical mixing or hand-mixing, including using auto-mixing tips, for self-curing and/or external energy activation, or non-mixing for external energy acti

21、vation. The polymer-based luting materials covered by this document are intended to be used for the cementation or fixation of restorations and appliances such as inlays, onlays, veneers, posts, crowns and bridges. This document does not cover the following polymer-based luting materials: a) those w

22、hich do not have an adhesive component within the structure of the material (see ISO 4049); b) those intended for veneering sub-frames (see ISO 10477). 2 Normative references The following documents are referred to in the text in such a way that some or all of their content constitutes requirements

23、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 1942, Dentistry Vocabulary ISO 3696, Water for analytical laboratory use Specification and test methods ISO 6344-1, Co

24、ated abrasives Grain size analysis Part 1: Grain size distribution test ISO 7491, Dental materials Determination of colour stability ISO 8601, Data elements and interchange formats Information interchange Representation of dates and times ISO 13116, Dentistry Test method for determining radio-opacit

25、y of materials 3 T erms a nd definiti ons For the purposes of this document, the terms and definitions given in ISO 1942 and the following apply. ISO and IEC maintain terminological databases for use in standardization at the following addresses: ISO Online browsing platform: available at h t t p :/

26、 www .iso .org/ obp IEC Electropedia: available at h t t p :/ www .electropedia .org/ 3.1 adhere to be in a state of adherence SOURCE: ISO/TS 11405:2015, 3.1 TECHNICAL SPECIFICATION ISO/TS 16506:2017(E) ISO 2017 All rights reserved 1 ISO/TS 16506:2017(E) 3.2 adherend body that is held or is intended

27、 to be held to another body by an adhesive (3.3) SOURCE: ISO/TS 11405:2015, 3.3 3.3 adhesive substance capable of holding materials together by interfacial forces 3.4 bond strength force per unit area required to break a bonded assembly with failure occurring in or near the adhesive (3.3)/adherend (

28、3.2) interface SOURCE: ISO/TS 11405:2015, 3.6 3.5 opaque luting material intensely pigmented polymer-based luting material intended to mask underlying materials and tooth structure SOURCE: ISO 4049:2009, 3.1 3.6 substrate material upon the surface of which an adhesive (3.3) is spread for any purpose

29、 such as bonding or coating SOURCE: ISO/TS 11405:2015, 3.8 4 Classific ation 4.1 Class 1: materials whose setting is effected by mixing an initiator and activator (self-curing materials). 4.2 Class 2: materials whose setting is effected by the application of energy from an external source, such as

30、visible light external-energy-activated materials, see also 8.3 d). 4.3 Class 3: materials whose setting is effected by the application of external energy and which also have a self-curing mechanism present (dual-cure materials). 5 Performance issues 5.1 Biocompatibility See the Introduction for gui

31、dance on biocompatibility. Further information is available in ISO 10993-1 and ISO 7405. 5.2 Bond strength and physical and chemical performances This document does not specify any limit values of bond strength and physical and chemical performances. When such properties are tested, refer to Annex C

32、2 ISO 2017 All rights reserved ISO/TS 16506:2017(E) 6 Sampling The test sample shall consist of packages prepared for retail sale from the same batch or lot containing enough material to carry out the specified tests, plus an allowance for repeat tests, if necessary. 50 g should be sufficient. 7 Te

33、st methods 7.1 General a) Reagent Water For the tests, use water prepared in accordance with ISO 3696 Grade 2. b) Equipment Validate all test equipment prior to use. 7.2 Test conditions Unless specified otherwise, prepare and test all specimens at (23 2) C. Control the relative humidity to ensure th

34、at it remains (50 20) % at all times. If the material was refrigerated, e.g. for storage, allow it to attain (23 2) C. For Class 3 materials, perform the tests for film thickness (see 7.5), working time (see 7.6) and setting time (see 7.7) in the absence of activating radiation. Ambient light, both

35、natural and artificial, is capable of activating Class 2 and Class 3 materials. For good control, the test should be performed in a darkened room with any artificial light filtered by a yellow filter. 1) 7.3 Inspection Inspect visually to check that requirements specified in Clause 8 have been met.

36、7.4 Preparation of test specimens For the preparation of Class 2 and Class 3 materials, refer to the manufacturers instructions for use see 8.3 d) that states the external energy source or sources recommended for the materials to be tested. Ensure that the source is in a satisfactory operating condi

37、tion. NOTE ISO 10650 gives guidance on this. Mix or otherwise prepare the material in accordance with the manufacturers instructions for use and the test conditions specified in 7.2. When fully cured specimens are required for testing (7.10 to 7.12), ensure that the specimens are homogeneous after r

38、emoval from the mould. Discard any specimens containing clefts, voids, discontinuities or air inclusions when inspected visually without magnification. 1) Polyester filter 101, Lee Filters, Andover, Hants, UK is an example of a suitable product available commercially. This information is given for t

39、he convenience of the users of this document and does not constitute an endorsement of this product by ISO. ISO 2017 All rights reserved 3 ISO/TS 16506:2017(E) 7.5 Film thickness 7.5.1 Apparatus 7.5.1.1 Two glass plates, optically flat, square or circular, each having a contact surface area of (200

40、25) mm 2and a uniform thickness not less than 5 mm. 7.5.1.2 Loading device, of the type illustrated in Figure 1 or an equivalent means, whereby a force of (150 2) N can be applied vertically to the specimen via the upper glass plate. In Figure 1, the anvil that is attached to the bottom of the rod i

41、s horizontal and parallel to the base, such that the load can be applied smoothly and without rotation of the specimen. NOTE A holder can be used to assist in the positioning of the plates. Such a device consists of a base-plate with three vertical pins to align circular plates or four pins to align

42、 square plates. 7.5.1.3 External energy source (for Class 2 and Class 3 materials), as recommended by the manufacturer for use with the test material. 7.5.1.4 Micrometer, accurate to at least 0,5 m. Key 1 specimen 2 glass plates (7.5.1.1) F i g u r e 1 L o a d i n g d e v i c e f o r u s e i n t h e

43、 f i l m t h i c k n e s s t e s t 7.5.2 Test procedure 7.5.2.1 Preliminary steps Measure with the micrometer (7.5.1.4), to an accuracy of 1,0 m, the combined thickness of the two optically flat glass plates (7.5.1.1) stacked in contact (reading A). Remove the upper plate and place between 0,02 ml a

44、nd 0,10 ml of the test material prepared in accordance with the manufacturers instructions for use in the centre of the lower plate and centre the plate below the loading device (7.5.1.2) on its lower plate. Centre the second glass plate on the test specimen in the same orientation as in the origina

45、l measurement.4 ISO 2017 All rights reserved ISO/TS 16506:2017(E) 7.5.2.2 Class 1 materials At (60 2) s after the completion of mixing Class 1 materials, apply a force of (150 2) N vertically and centrally to the specimen via the top plate smoothly and in such a manner that no rotation occurs for (1

46、80 10) s. Ensure that the cement has completely filled the space between the glass plates. At least 10 min after the commencement of mixing, remove the plates from the loading device and measure the combined thickness of the two glass plates and the specimen film, again taking the reading in the cen

47、tre of the plates (reading B). Record the difference between reading A and reading B, to the nearest micrometre, as the film thickness of the material. Carry out five determinations. 7.5.2.3 Class 2 and Class 3 materials Immediately after dispensing Class 2 materials or at (60 2) s after the complet

48、ion of mixing Class 3 materials, apply a force of (150 2) N vertically and centrally to the specimen via the top plate smoothly and in such a manner that no rotation occurs for (180 10) s. Ensure that the specimen has completely filled the space between the glass plates. After (180 10) s, release th

49、e load and irradiate the specimen through the centre of the upper glass plate for twice the exposure time recommended by the manufacturer. NOTE This irradiation is not intended to cure the material totally, but to stabilize the specimen for measurement. After the irradiation of Class 2 and Class 3 materials, remove the plates from the loading device and measure the combined thickness of the two glass plates and the specimen film, again taking the reading in the centre of