SIST EN 24049:2000/AC:2000
(Amendment)Dentistry - Resin-based filling materials (ISO 4049:1988 + Technical corrigendum 1:1992)
Dentistry - Resin-based filling materials (ISO 4049:1988 + Technical corrigendum 1:1992)
Zahnheilkunde - Füllungskunststoffe (ISO 4049:1988 + Technische Korrektur 1:1992)
Art dentaire - Produits d'obturation a base de résines synthétiques (ISO 4049:1988 + Rectificatif technique 1:1992)
Dentistry - Resin-based filling materials (ISO 4049:1988 + Technical corrigendum 1:1992)
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Dentistry - Resin-based filling materials (ISO 4049:1988 + Technical corrigendum 1:1992)Zahnheilkunde - Füllungskunststoffe (ISO 4049:1988 + Technische Korrektur 1:1992)Art dentaire - Produits d'obturation a base de résines synthétiques (ISO 4049:1988 + Rectificatif technique 1:1992)Dentistry - Resin-based filling materials (ISO 4049:1988 + Technical corrigendum 1:1992)11.060.10Dental materialsICS:Ta slovenski standard je istoveten z:EN 24049:1993/AC:1994SIST EN 24049:2000/AC:2000en01-januar-2000SIST EN 24049:2000/AC:2000SLOVENSKI
STANDARD
SIST EN 24049:2000/AC:2000
SIST EN 24049:2000/AC:2000
SIST EN 24049:2000/AC:2000
INTERNATIONAL STANDARD INTERNATIONAL ORGANIZATION FOR STANDARDIZATION ORGANISATION INTERNATIONALE DE NORMALISATION MEXAYHAPOJJHAFi OPTAHM3A~MR I-IO CTAH~APTM3A~MM Dentistry - Resin-based filling materials Art dentaire - Produits d’obturation G base de rhsines synthetiques ISO 4049 Deuxikme Edition 1988-12-15 Reference number ISO 4049: 1988 (E) SIST EN 24049:2000/AC:2000
ISO 4049 : 1988 (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. Esch 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, govern- mental 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. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the ISO Council. They are approved in accordance with ISO procedures requiring at least 75 % approval by the member bodies voting. International Standard ISO 4049 was prepared by Technical Committee ISO/TC 106, Den tistry. This second edition cancels and replaces the first edition (ISO 4049 : 19781, of which it constitutes a technical revision (see the Introduction). 0 International Organkation for Standardkation, 1988 Printed in Switzerland ii SIST EN 24049:2000/AC:2000
ISO 4049 : 1988 (El Introduction This second edition sf ISO 4049 takes account of the considerable volume of technical information which has accumulated since the first edition was published in 1978. Some of the tests in the first edition have been omitted and others added for the reasons given below. This International Standard does not cover requirements for materials intended for the restoration of occlusal surfaces or those intended to prevent caries. In Order to make this clear, a classification System has been introduced (see clause 3). This International Standard therefore covers class B materials, i.e. materials other than those intended for occlusal surfaces, and manufacturers are now required to classify their materials ac- cordingly. Furthermore, in Order to assist the purchaser, manufacturers are now also required (see clause 8) to describe the filier particle size range and the principal com- ponent of the resin base. The possibility was considered that materials might be classified by filier loading or its corollary, water uptake, and solubility of the resin Phase. However collaborative testing revealed considerable overlapping of these properties in “‘conventional”’ and “microfine” materials and such a classification was not adopted. Resin-based restorative materials activated by extemal energy are now well established and requirements for these materials are therefore included. As the materials do not have an unlimited working time in the dental surgery, a test for sensitivity to ambient light has been included (sec 7.6). Working and setting times of chemically cured materials cannot be determined ac- curately because of their rapid setting and varying viscosities after mixing. The test in the first edition of this International Standard, using an oscillating rheometer, had poor sensitivity and gave results that could not be correlated with “clinical” working time. In this second edition the test has been replaced by one which is simple and widely ap- plicable. The flexural strength test (sec 7.8) has been aligned with the test used for denture- base polymers by requiring that the specimen be immersed in water during testing. A requirement relating to modulus-dependent flexural strength has been included with the limiting value set to reveal conventional composites with poor filler/resin bonding. Requirements have been included for materials claimed to be radio-opaque (sec 4.5). Although tests are not included in this second edition for determining non-mandatory or optional properties, such as polymerization shrinkage, it is hoped to do so in a later edition. At present more than one test may be used to determine a Single such property which makes true comparisons impossible and confuses the purchaser. The test for depth of eure of external-energy-activated materia revised, if necessa ry, whe n more data become available. Is will be reviewed and Specific qualitative and quantitative requirements for freedom from biological hazard are not included in this International Standard, but it is recommended that reference should be made to ISO/TR 7405 when assessing possible biological or toxicological hazards. SIST EN 24049:2000/AC:2000
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INTERNATIONAL STANDARD ISO 4049 : 1988 (E) Dentistry - Resin-based filling materials 1 Scope This International Standard specifies requirements for dental resin-based restorative materials supplied in a form suitable for mechanical mixing, hand-mixing, or external energy activation, and intended for use primarily for the direct restoration of class Ill, IV and V cavities in the teeth, i.e. class B materials (sec clause 3). This International Standard does not cover requirements for materials intended for the restoration of occlusal surfaces, i.e. class A materials (see clause 3), or materials intended to pre- vent caries. 2 Normative references The following Standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All Standards are subject to revision, and Parties to agreements based on this International Standard are encour- aged to investigate the possibility of applying the most recent editions of the Standards listed below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 3665 : 1976, Photography - Intra-oral dental radiographic fifm - Specifica tion. I SO /TR 7405 : 1984, Biological evalua tion of dental ma terials. ISO 7491 : 1985, Dental materials - Determination of colour s tabifity o f dental polymeric ma terials. I SO 8601 : 1988, Data elemen ts and in terchange forma ts - ln- formation interchange - Representation of dates and times. 3 Classification For the purposes of this International Standard, dental resin- based restorative materials are classified as follows : Class A : Materials claimed by the manufacturer as suitable for the restoration of cavities involving occlusal surfaces Class B : All other materials Type 1 : Chemically-cured materials, i.e. those materials where setting is effected by mixing an initiator and activator Type 2 : External-energy-activated materials, i.e. those materials where setting is effected by the application of energy, such as blue light 4 Requirements 4.1 Biocompatibility See the Introduction for guidance on biocompatibility. 4.2 Physical and mechanical properties 4.2.1 General If the material is supplied by the manufacturer in pre-coloured Standard shades, each shade shall be capable of satisfying the 1 SIST EN 24049:2000/AC:2000
ISO 4049 : 1988 (El requirements specified in 4.3 appropriate to the material type. If the material is supplied for “tinting” or “blending” to the user’s prescription, the material shall comply with the requirements both when used alone and when used with the maximum recommended Proportion sf tinter or blender [see 8.3 g)]. 4.5 Radio-Opacity If the manufacturer Claims that the material is radio-opaque [see 723.2 b)], the radio-opacity, determined in accordance with 7.11, shall be greater than that of the same thickness of aluminium. 4.2.2 Minimum working time, type 1 materials 5 Sampling The wo rking ti me for type 1 materials, determined in accord- ante wi th 7.4, sha II be not less than 90 S. The test Sample shall consist of retail packages from the same batch containing enough material to carry out the specified tests, plus an allowance for repeat tests, if necessary. 4.2.3 Setting time, type 1 materials NOTE - 50 g should be sufficient, but two further samples batches may be required for the shade test (sec 4.3). of different The setting time for type 1 materials, determined in accordance with 7.5, shall be not more than 5 min. 4.2.4 Sensitivity to ambient light, type 2 materials 6 Preparation of test specimens When tested in accordance with 7.6, there shall be no detect- able Change in the consistency of any of the three samples of type 2 materials after being exposed to the test light for 60 s. NOTE - For the preparation of type 2 materials, reference should be made to the manufacturer’s instructions Isee 8.3 e)l which will state the external energy Source or sources recommended for the materials to be tested. Care should be taken to ensure that the Source is in a satisfactory operating condition. 4.2.5 Depth of eure, type 2 materials Mix or otherwise prepare the man ufacturer’s instructions a in 7. 2. material in accordance with the nd the test conditions speci fied When determined in accordance with 7.7, the depth of eure of type 2 materials shall be not less than 2 mm, and, in any event, no more than 0,5 mm below the value stated by the manufac- turer. 7 Test methods NOTE - This test is considered to represent about twice the optimal conve rsion of monomer to polymer. 7.1 General reagent and apparatus 4.2.6 Flexural strength 7.1.1 Water The flexura! strength of type 1 and type 2 materials, determined in accordance with 7.8, shall be not lower than the value of iV = [(flexural modulus x 0,002 5) + 401 MPa, and, in any event, not lower than 50 MPa. Water prepared by - multiple distillation, or - distillation followed by de-ionization, or 4.2.7 Water mater ‘ials absorption and solubility, types 1 and 2 - distillation followed by reverse osmosis. When determined in accordance with 7.9, the water absorption of type 1 and type 2 materials shall not be greater than 50 (Ig/mm3 and the solubility shall not be greater than 5 pglmm3. 7.1.2 Glass slides/plates Quartz glass plates, 2 mm thick, are required for use with type 2 materials being cured by ultraviolet light only. For type 1 materials and type 2 cured by blue light, Standard glass microscope slides may be used. 4.3 Wade When the material is assessed in accordance with 7.10 by three observers, the shade of the set material shall match closely that of the manufacturer’s shade guide. If a shade guide is not sup- plied by the manufacturer, samples from two further batches shall be taken for comparative purposes; all three samples shall show no more than a slight Change in colour. 7.2 Test conditions Unless specified otherwise by the manufacturer, prepare and test all specimens at (23 + 1) OC. Control the relative humidity to ensure that it remains greater than 30 % at all times. If the material was refrigerated for storage, allow sufficient time for it to attain (23 AI 1) OC. 4.4 Colour stability 7.3 Inspection When the material is assessed in accordance with 7.10, none of the three observers shall observe more than a slight Change in colour. Visually inspect have been met. to check that requirements specified in clause 8 2 SIST EN 24049:2000/AC:2000
ISO 4049 : 1988 (El 7.4 Working time, type 1 materials Dimensions in millimetres 7.4.1 Apparatus Thermocouple apparatus, as shown in figure 1. The apparatus consists of a piece of polyethylene tubing, 0 A , located on a block of Polyamide or similar material, @ , which has a hole into which is inserted a stainless steel tube, @ , containing a stabilized thermocouple @ . The tube @ is 8 mm long, 4 mm in internal diameter and - has a wall thickness of 1 mm. The locating part of block (B) is 4 mm in diameter and 2 mm high. When assembled the two components form a specimen well 6 mm high x 4 mm in diameter. In Order to facilitate removal of the specimen after testing, the thermocouple @ has a conical tip which pro- trudes 1 mm into the base of the specimen weil. The tolerantes on the above-mentioned dimensions are + 0,2 mm. The thermocouple consists of wires (0,2 + 0,051 mm in diameter, made of a material (e.g. copper/constantan) capable of registering temperature changes in a specimen of setting material to an accuracy of 0,l OC. The thermocouple is con- nected to an instrument (e.g. Voltmeter or Chart recorder) capable of recording the temperature to that accuracy. 7.4.2 Procedure Prepare the test material in accordance with the manufacturer’s instructions (see 8.3) and Start timing from the moment mixing is begun. Maintain the mould at (23 + 1) OC and, 30 s after the Start of mixing, place the mixed material in the mould and record the temperature, l,, of the material. Maintain the ap- paratus at (23 ?Z 1) OC and continuously record the tempera- ture of the material until the peak temperature is passed. NOTE - A typical recording trace is shown in figure 2. As soon as the material is inserted into the mould, the temperature falls slightly until it becomes steady at /o and then star-% to increase. The Point at which the temperature begins to increase denotes the Start of the setting reaction and, therefore, the end of the working time. This Point should be determined by drawing a proof line at ‘0 31 0,Ol OC and recording TW at the Point of intersection with the trace. The results are extremely temperafure-dependent and slight variations within the permitted temperature range will Cause variations of several seconds. Record the time, T,, from the Start of mixing until the temperature Starts to increase. Carry out five determinations. 7.4.3 Interpretation of results If at least four of the times obtained are longer than 90 s, the material is deemed to have complied with the requirement of 4.2.2. If three or more of the times are shorter than 90 s, the material is deemed to have failed. If only three times are longer than 90 s, repeat the whole test. If three or fewer times are longer than 90 s on the second oc- casion, the material is deemed to have failed the whole test. o- C Key (sec also 7.4.1) 0 A Polyethylene tu bing 0 B Polyamide block 0 C Stainless steel tu be 0 D Thermocouple-cone of solder NOTE - Dimensional tolerantes shall be + 0,2 mm. Figure 1 - Apparatus for determination of working and setting times SIST EN 24049:2000/AC:2000
ISO 4049 : 1988 (El t 1 T W Time 4 e T - 1 NOTE - The typical recording trace illustrated Shows the temperature at the time of insertion, Q, the slight temperature drop immediately after inser- tion, ~0, and the initial time of temperature increase, Tw, which denotes the Start of the setting reaction and, therefore, the end of the working time. At (37 + 1) OC, the peak temperature t2 is noted to measure Ts, the setting time. Figure 2 - Typical recording trace showing temperature changes with time for determination of working and setting times 7.5 Setting time, type 1 materials 7.5.1 Apparatus Thermocouple apparatus, as specified in 7.4.1. 7.5.2 Procedure Repeat the procedure specified in 7.4.2, but maintain the ap- paratus at (37 + 1) OC. Measure the time from the Start of mixing until the maximum temperature is reached. Record this time, TS, as the setting time (sec figure 2). 7.5.3 Interpretation of results 16 at least four of the times obtained are shorter than 5 min, the material is deemed to have complied with the requirement of 4.2.3. If three or more of the times are longer than 5 min, the material is deemed to have failed. If only three of the times are shorter than 5 min, repeat the whole test. If one or more times are longer than 5 min on the second occasion, the material is deemed to have failed the whole test. 7.6 Sensitivity to ambient light, type 2 materials 7.6.1 Apparatus 7.6.1.1 Xenon lamp or radiation Source of equivalent Performance, with colour conversion and ultraviolet filters in- serted. The colour conversion filter shall be 3 mm thick hardened glass and shall have an internal transmittance which matches within L- 10 % that shown in figure 3.‘) 1) A suitable filter which corresponds to the internal transmittance shown in figure 3 and which is available commercially is the FG 15, hardened, rough-polished, 3 mm thick (supplied by Schott Glaswerke, Postbox 2480, D-6500, Mainz 1, Germany, F.R. 1. This information is given for the con- venience of the users of this International Standard and does not constitute an endorsement of this product by ISO. 4 SIST EN 24049:2000/AC:2000
0,99 0,98 0,97 0,96 0,95 09 I .- bJ . E .- % 08 1 .- E z 07 I Co l= T 06 I z 05 I E 04 - I 03 I 02 0’10 0'05 0’01 l 10 -3 10-4 10 -5 200 600 700 800 Wavelength, nm Figure 3 - lnternal transmittance for colour conversion filter (see 7.6.1 .l) SIST EN 24049:2000/AC:2000
Iso 4049 : 1988 (El The ultraviolet filter shall be made of borosilicate glass with a transmittance of less than 1 % below 300 nm and greater than 90 % above 370 nm. 7.7.1.4 Film, transparent to the activating radiation, (50 & 30) Fm thick, e.g. Polyester. 7.7.1.5 Externa I energy so urce , as recommended manufacturer for use with the test material [see 8.3 e) by the NOTE - The purpose of the filter is to convert the Xenon, or equivalent, spectrum to that approxima ting to a dental operating lig ht. 1. 7.7.1.6 Micrometer, accurate to 0,Ol mm. 7.6.1.2 Two glass slides/plates (sec 7.12). 7.7.1.7 Plastics spatula. 7.6.1.3 Illuminance-measuring device e.g. Iuxmeter, capable of measuring illuminance of (10 000 + 2 000) IX. 7.7.2 Procedure 7.6.1.4 Adjustable table. Place the mould (7.7.1 .l) on a Strip of the transparent film (7.7.1.4) covering the filter Paper (7.7.1.3) and fill it with the test material, prepared in accordance with the manufacturer’s instructions. Take care to exclude air bubbles. Slightly overfill the mould and put a second Strip of the transparent film on top. Press the mould and Strip of film between the glass slides (7.7.1.2) to exude excess material. Remove the microscope slide covering the Strips of film and gently place the exit win- dow of the external energy Source (7.7.1.5) against the Strip of film. Irradiate the material for the time recommended by the manufacturer to achieve a depth of eure of at least 2 mm. 7.6.2 Procedure In a dark room, Position the illuminance-measuring device cell (7.6.1.3) under the Xenon lamp with colour conversion and ultraviolet filters inserted (7.6.1.1) at such a height as to provide an illuminance of (10 000 & 2 000) IX. [The adjustable table (7.6.1.4) is required to do this efficiently.] Place approximately 30 mg of material on a glass slide (7.6.1.2), Position the slide on top of the cell and expose it to the light for (60 * 5) s. Remove the slide with the Sample from the irradiated area and press the second microscope slide against the material to produce a thin layer , Remove the specimen from the mould (180 + 20) s after com- pletion of exposure and gently remove the uncured material with the plastics spatula (7.7.1.7). M
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