EN ISO 4049:2000
(Main)Dentistry - Polymer-based filling, restorative and luting materials (ISO 4049:2000)
Dentistry - Polymer-based filling, restorative and luting materials (ISO 4049:2000)
Zahnheilkunde - Füllungs-, restaurative und Befestigungskunststoffe (ISO 4049:2000)
Art dentaire - Produits d'obturation, de restauration et de scellement à base de polymères (ISO 4049:2000)
Dentistry - Polymer-based filling, restorative and luting materials (ISO 4049:2000)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 4049:2000
01-november-2000
1DGRPHãþD
SIST EN 24049:2000
SIST EN 24049:2000/AC:2000
Dentistry - Polymer-based filling, restorative and luting materials (ISO 4049:2000)
Dentistry - Polymer-based filling, restorative and luting materials (ISO 4049:2000)
Zahnheilkunde - Füllungs-, restaurative und Befestigungskunststoffe (ISO 4049:2000)
Art dentaire - Produits d'obturation, de restauration et de scellement a base de
polymeres (ISO 4049:2000)
Ta slovenski standard je istoveten z: EN ISO 4049:2000
ICS:
11.060.10 =RERWHKQLþQLPDWHULDOL Dental materials
SIST EN ISO 4049:2000 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 4049:2000
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SIST EN ISO 4049:2000
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SIST EN ISO 4049:2000
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SIST EN ISO 4049:2000
INTERNATIONAL ISO
STANDARD 4049
Third edition
2000-07-15
Dentistry — Polymer-based filling,
restorative and luting materials
Art dentaire — Produits d'obturation, de restauration et de scellement à
base de polymères
Reference number
ISO 4049:2000(E)
©
ISO 2000
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
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ii © ISO 2000 – All rights reserved
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
Contents Page
Foreword.iv
Introduction.v
1 Scope .1
2 Normative references .1
3 Terms and definitions .1
4 Classification.2
5 Requirements.2
5.1 Biocompatibility.2
5.2 Physical and chemical properties.2
5.3 Shade, filling and restorative materials.4
5.4 Colour stability after irradiation and water sorption.4
5.5 Radio-opacity .4
6 Sampling.5
7 Test methods.5
7.1 General reagent water .5
7.2 Test conditions .6
7.3 Inspection.6
7.4 Preparation of test specimens .6
7.5 Measurement of film thickness of luting materials.6
7.6 Working time, Class 1 and Class 3 filling and restorative materials.9
7.7 Working time, Class 1 and Class 3 luting materials.11
7.8 Setting time, Class 1 and Class 3 materials.11
7.9 Sensitivity to ambient light, Class 2 materials .13
7.10 Depth of cure, Class 2 materials .14
7.11 Flexural strength.15
7.12 Water sorption and solubility .18
7.13 Shade and colour stability after irradiation and water sorption.21
7.14 Radio-opacity .22
8 Packaging, marking and information to be supplied by the manufacturer .24
8.1 Packaging.24
8.2 Marking .24
8.3 Manufacturer’s instructions and information for the user .25
Bibliography.27
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SIST EN ISO 4049:2000
ISO 4049:2000(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 3.
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 International Standard may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 4049 was prepared by Technical Committee ISO/TC 106, Dentistry, Subcommittee
SC 1, Filling and restorative materials.
This third edition cancels and replaces the second edition (ISO 4049:1988), which has been technically revised to
include those polymer-based restorative materials (inlay/onlay materials) that are processed outside the mouth, in
either the dental operatory or laboratory. These have been added as Class 2, group 2 materials in a redesigned
Classification (see clause 4). Materials that cure by both chemical means and external energy application (dual
cure materials) have also been added to the Classification as Class 3 materials.
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
Introduction
This International Standard now includes requirements for materials intended for the restoration of occlusal
surfaces (type 1 materials). It does not cover materials intended to prevent caries (see ISO 6874) or those used for
veneering metal sub-frames (see ISO 10477). The broad group of polymeric restorative materials that is covered by
this standard is subject to rapid developments and during the drafting of this standard several new types of material
have been marketed. These include “condensable” and “flowable” composites and “ormocers”. The manufacturers
of such materials have the option of claiming compliance with this standard but it should be noted that the materials
were not included in any collaborative testing during the preparation of this standard.
Also, this International Standard now includes requirements for polymer-based luting materials that are intended for
cementing of restorations and appliances such as inlays, onlays, crowns and bridges. This has resulted in new
tests and requirements for the working time and film thickness of luting materials.
In comparison with ISO 4049:1988, alterations have been made to the requirements for flexural properties (see
5.2.9) and water sorption (see 5.2.10). These requirements have been changed following collaborative testing and
review of published data.
Changes have been made to the test methods for water sorption and solubility (see 7.12) and radio-opacity
(see 7.14.) in order to clarify simplify and improve the accuracy of these tests.
Specific qualitative and quantitative requirements for freedom from biological hazard are not included in this
International Standard, but it is recommended that when assessing possible biological or toxicological hazards
reference should be made to ISO 10993-1 and ISO 7405.
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SIST EN ISO 4049:2000
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SIST EN ISO 4049:2000
INTERNATIONAL STANDARD ISO 4049:2000(E)
Dentistry — Polymer-based filling, restorative and luting materials
1 Scope
This International Standard specifies requirements for dental polymer-based filling and restorative materials and
polymer-based luting materials supplied in a form suitable for mechanical mixing, hand-mixing, or intra-oral and
extra-oral external energy activation, and intended for use primarily for the direct or indirect restoration of cavities in
the teeth.
The luting materials covered by this International Standard are intended for use in the cementing or fixation of
restorations and appliances such as inlays, onlays, veneers, crowns and bridges.
This International Standard does not cover requirements for polymeric materials intended for veneering indirectly
restoration metal sub-frames (see ISO 10477) and materials intended to prevent caries (see ISO 6874).
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent editions of the normative documents indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 3665:1996, Photography — Intra-oral dental radiographic film — Specification.
ISO 3696:1987, Water for analytical use — Specification and test methods.
ISO 7491:1999, Dental materials — Determination of colour stability of dental materials.
ISO 8601:1988, Data elements and interchange formats — Information interchange — Representation of dates and
times.
3 Terms and definitions
For the purposes of this International Standard, the following terms and definitions apply.
3.1
opaquer luting material
intensely pigmented polymer-based luting material intended to mask underlying tooth structure
3.2
opaque
shade of a polymer-based restorative material intended to be less translucent than a non-opaque shade
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
4 Classification
For the purposes of this International Standard, dental polymer-based restorative materials are categorized as one
of the following types.
a) Type 1: polymer-based filling and restorative materials claimed by the manufacturer as suitable for
restorations involving occlusal surfaces;
b) Type 2: all other polymer-based filling and restorative materials.
NOTE 1 It is not necessary to classify polymer-based luting materials into types.
The three classes of dental polymer-based filling, restorative and luting materials are as follows.
� Class 1: materials whose setting is effected by mixing an initiator and activator (“self-curing” materials).
� Class 2: materials whose setting is effected by the application of energy from an external source, such as blue
light or heat (“external-energy-activated” materials). They are subdivided as follows:
1) Group 1: materials whose use requires the energy to be applied intra-orally;
2) Group 2: materials whose use requires the energy to be applied extra-orally. When fabricated, these
materials will be luted into place.
Certain materials may be claimed by manufacturers to be both Group 1 and Group 2. In this event the material
should fulfil the requirements for both groups.
NOTE 2 Class 2 luting materials will fall into Group 1 only.
� Class 3: materials that are cured by the application of external energy and also have a self-curing mechanism
present [“dual cure” materials; see 8.3 e)].
5 Requirements
5.1 Biocompatibility
See the Introduction for guidance on biocompatibility. See ISO 7405 and ISO 10993-1 for further information.
5.2 Physical and chemical properties
5.2.1 General
If a filling and restorative material is supplied by the manufacturer in various shades, each shade, including opaque
shades, shall be capable of satisfying all the requirements for sensitivity to ambient light (5.2.7), depth of cure
(5.2.8), shade (5.3) and colour stability (5.4) appropriate to the material type and class. If the material is supplied
such that it can be “tinted” or “blended” to the user’s specification, the material shall comply with the requirements
both when used alone and when used with the maximum recommended proportion of tint or blender [see 8.3 d)].
Similarly, if the manufacturer supplies a luting material in various shades, each shade, including opaquer luting
materials, shall be capable of satisfying all the requirements for depth of cure (5.2.8). Colour stability (5.4) of luting
materials shall not be tested unless the manufacturer claims such a property.
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
In respect of the other requirements of 5.2 and those of 5.5, only one representative shade of luting, filling and
restorative materials shall be tested. This representative shade shall be either that classified by the manufacturer
�
1)
as “universal” or, in the event that no shade is so classified, that shade corresponding to “A3” in the Vita
classification of shade.
5.2.2 Film thickness of luting materials
The film thickness of luting materials when determined in accordance with 7.5 shall be no more than 10�m above
any value claimed by the manufacturer and in any event shall be no greater than 50�m.
5.2.3 Working time, Class 1 and Class 3 filling and restorative materials
The working time for Class 1 and Class 3 filling and restorative materials, determined in accordance with 7.6, shall
be not less than 90 s.
5.2.4 Working time, Class 1 and Class 3 luting materials
When tested in accordance with 7.7, the material shall be capable of forming a thin layer; during its formation there
shall be no detectable change in its homogeneity.
5.2.5 Setting time, Class 1 materials
The setting time for Class 1 filling and restorative materials, determined in accordance with 7.8, shall be not more
than 5 min. The setting time for Class 1 luting materials, determined in accordance with 7.8, shall be not more than
10 min.
5.2.6 Setting time, Class 3 materials
The setting time for Class 3 materials, determined in accordance with 7.8, shall be not more than 10 min.
5.2.7 Sensitivity to ambient light, Class 2 materials
When tested in accordance with 7.9, the material shall remain physically homogeneous.
5.2.8 Depth of cure, Class 2 materials
When determined in accordance with 7.10, the depth of cure of Class 2 filling and restorative materials shall be not
less than 1 mm if they are labelled by the manufacturer as opaque, or not less than 1,5 mm for other filling and
restorative materials.
The depth of cure of luting materials when determined in accordance with 7.10 shall not be less than 0,5 mm if they
are labelled by the manufacturer as opaquer materials, or not less than 1,5 mm for other materials.
In any event, the values for all materials, with the exception of opaquer luting materials, shall be no more than
0,5 mm below the value stated by the manufacturer.
5.2.9 Flexural strength, type 1 and type 2 materials
The flexural strength of type 1 and type 2 materials, determined in accordance with 7.11, shall be equal to or
greater than the limits specified in Table 1.
�
1) Vita is the trade name of a product supplied by Vita Zahnfabrik, H. Rauter GmbH & Co. KG, Postfach 1338, D-79704 Bad
Säckingen, Germany. This information is given for the convenience of the users of this International Standard and does not
constitute an endorsement of this product by ISO.
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
Table 1 — Minimum flexural strength
Type 1 Class 1 80 MPa
Class 2, group 1 80 MPa
Class 2, group 2 100 MPa
Class 3 80 MPa
Type 2 Class 1 50 MPa
Class 2, group 1 50 MPa
Class 3 50 MPa
5.2.10 Water sorption and solubility
When determined in accordance with 7.12:
3
a) the water sorption of all materials shall be less than or equal to 40µg/mm .
3
b) the solubility of all materials shall be less than or equal to 7,5µg/mm .
5.3 Shade, filling and restorative materials
When the material is assessed in accordance with 7.13 and ISO 7491, the shade of the set material shall match
closely that of the manufacturer’s shade guide. If a shade guide is not supplied by the manufacturer, then the
manufacturer shall nominate a commercially available shade guide that shall be used in assessing compliance with
this requirement [see 8.3 l)]. In addition, the set material shall be evenly pigmented when viewed without
magnification.
5.4 Colour stability after irradiation and water sorption
When the material is tested in accordance with 7.13 and ISO 7491, no more than a slight change in colour shall be
observed for filling and restorative materials. In respect of luting materials, colour stability shall be tested only in the
event of a manufacturer’s claim for colour stability. In the event of such a claim, no more than a slight change in
colour shall be observed after the material has been tested in accordance with 7.13 and ISO 7491.
5.5 Radio-opacity
If the manufacturer claims that the material is radio-opaque [see 8.2.3 h)], the radio-opacity, determined in
accordance with 7.14, shall be equal to or greater than that of the same thickness of aluminium and no less than
0,5 mm of any value claimed by the manufacturer. In the event of a dispute regarding the compliance of a material
with this requirement, Method A (7.14.2, 7.14.3, 7.14.4) shall be used.
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
Table 2 — Physical and chemical property requirements 5.2.3, 5.2.5, 5.2.6, 5.2.8, 5.2.10
for filling and restorative materials (see Table 1 for minimum flexural strength)
Requirement (subclause)
a
Working time Setting time Depth of cure Water sorption Solubility
Material (5.2.3) (5.2.5, 5.2.6) (5.2.8) (5.2.10) (5.2.10)
Class
3 3
s min mm µg/mm µg/mm
min. max. min. max. max.
5
Class 1 90 — 40 7,5
(5.2.5)
1 (opaque shade)
Class 2 —— 40 7,5
1,5 (others)
10
Class 3 90 — 40 7,5
(5.2.6)
a
The values for all materials shall be no more than 0,5 mm below the value stated by the manufacturer.
Table 3 — Physical and chemical property requirements 5.2.2, 5.2.4, 5.2.5, 5.2.6, 5.2.8 5.2.10
for luting materials
Requirement (subclause)
Film Working Setting Depth Water Solubility
a b
Material
thickness time time of cure sorption (5.2.10)
Class (5.2.2) (5.2.4) (5.2.5, 5.2.6) (5.2.8) (5.2.10)
3 3
µm s min mm µg/mm µg/mm
max. min. max. min. max. max.
10 40
Class 1 50 60 — 7,5
(5.2.5)
0,5 (opaquer)
Class 2 50 —— 40 7,5
1,5 (others)
10
Class 3 50 60 — 40 7,5
(5.2.6)
a
The determined value shall be no more than 10 µm above any value claimed by the manufacturer.
b
The values for all materials, with exception of opaquer luting materials, shall be no more than 0,5 mm below the value
stated by the manufacturer.
6 Sampling
The test sample shall consist of packages prepared for retail sale from the same batch and containing enough
material to carry out the specified tests, plus an allowance for repeat tests, if necessary.
NOTE 50 g should be sufficient.
7 Test methods
7.1 General reagent — Water
For the tests use water prepared in accordance with ISO 3696 Grade 2.
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
7.2 Test conditions
Unless specified otherwise by the manufacturer, prepare and test all specimens at (23� 1) °C. Control the relative
humidity to ensure that it remains greater than 30 % at all times. If the material was refrigerated for storage, allow it
to attain (23� 1) °C.
For Class 3 materials, the tests for working time (see 7.6) and setting time (see 7.8) shall be performed in the
absence of activating radiation. Ambient light, both natural and artificial, is capable of activating these materials.
2)
For good control the test should be performed in a dark room with any artificial light filtered by a yellow filter .
7.3 Inspection
Inspect visually to check that requirements specified in clause 8 have been met.
7.4 Preparation of test specimens
For the preparation of Class 2 and Class 3 materials, reference should be made to the manufacturer’s instructions
[see 8.3 e)] that state the external energy source or sources recommended for the materials to be tested. Care
shall be taken to ensure that the source is in a satisfactory operating condition.
Mix or otherwise prepare the material in accordance with the manufacturer’s instructions and the test conditions
specified in 7.2.
Where fully cured specimens are required for testing (7.11 to 7.14), it is important to ensure that the specimens are
homogeneous after removal from the mould. There should be no voids, clefts or air-blows present when viewed
without magnification.
Some polymer-based materials, particularly certain luting materials, have a chemical affinity for base metals. This
property creates difficulty when removing specimens from metal moulds. Reference shall be made to the
information supplied by the manufacturer (see 8.3) regarding this property and, if it is claimed, moulds for the
preparation of specimens of such materials may be made from non-metallic material such as high density
polyethylene.
7.5 Measurement of film thickness of luting materials
7.5.1 Apparatus
7.5.1.1 Two glass plates, optically flat, square or circular, each having a contact surface area of
2
(200� 25) mm . Each plate shall be of a uniform thickness of not less than 5 mm.
NOTE If it is desired to re-use the plates after testing, the glass surface may be coated with a release agent that has no
effect on the film thickness of the material under test.
7.5.1.2 Loading device of the type illustrated in Figure 1, or an equivalent means, whereby a force of
(150� 2) N may 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 shall be horizontal and parallel to the base. The load shall be applied smoothly
and in such a manner that no rotation occurs.
NOTE A holder may be used to assist in the positioning of the plates. Such a device consists of a baseplate with three
vertical pins to align circular plates or four pins to align square plates (see Figure 2).
2) Polyester filter 101, Lee Filters, Andover, Hants, UK, is an example of a suitable product available commercially. This
information is given for the convenience of the users of this International Standard and does not constitute an endorsement of
this product by ISO.
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
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 or equivalent measuring instrument, accurate to 1µm.
Key
1 Specimen
2 Glass plates
Figure 1 — Loading device for use in measurement of film thickness (7.5)
7.5.2 Test procedure
7.5.2.1 Preliminary steps
Measure, to an accuracy of 1µm, the combined thicknesses of the two optically flat glass plates stacked in contact
with the micrometer (reading A). Remove the upper plate and place between 0,02 ml and 0,1 ml of the test material
treated in accordance with the manufacturer’s instructions in the centre of the lower plate and place this centrally
below the loading device on its lower platen. Replace the second glass plate centrally on the test specimen in the
same orientation as in the original measurement. The holder (Figure 2) is helpful.
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SIST EN ISO 4049:2000
ISO 4049:2000(E)
7.5.2.2 Class 1 materials
At (60� 2) s after mixing Class 1 materials, carefully apply a force of (150� 2) N vertically and centrally to the
specimen via the top plate for (180� 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 thicknesses of the two glass plates and the specimen film (reading B).
Record the difference between reading A and reading B, to the nearest micrometre, as the film thickness of the
luting agent.
Carry out five determinations.
The diameter d slightly exceeds the diameter of the glass plates.
The height h of the pins is 1,5 times the height of one of the glass plates.
Figure 2 — Holder to assist stabilization of the glass plates (7.5.1.2)
7.5.2.3 Class 2 and Class 3 materials
Immediately after dispensing Class 2 materials or after mixing Class 3 materials, carefully apply a force of
(150� 2) N vertically and centrally to the specimen via the top plate for (180� 10) s. Ensure that the cement has
completely filled the space between the glass plates. After (180� 10) s, release the loading system and irradiate
the specimen through the centre of the upper glass plate for twice the recommended exposure time.
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 thicknesses of the two glass plates and the specimen film (reading B).
Record the difference between reading A and
...
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