TECHNICAL ISO

REPORT TR 11405
First edition
1994-12-15

Dental materials - Guidance on testing of

adhesion to tooth structure

iTeh STANDARD
Produits den taires - PREVIEW
structure de Ia dent
Lignes directrices pour I essai d’adhksion a Ia

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ISO/TR 11405:1994
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0f624eefd762/iso-tr-11405-1994

Reference number
ISO/TR 11405: 1994(E)
ISO/TR 11405:1994(E)

Contents
Page

1 Scope .. .. . .. . .. . .. . .. . .. .. .. .. .. .. . . .. . . ... . .. . .. .. . .. .. .. . ... .. .. .. .. .. .. .. . .. .. . .. . .. . .. .. .. . .. .. 1

2 Normative references ..................................................................... 1

3 Definitions ........................................ ......................................... 1

4 Requirements ............................................................................ 1

5 Sampling .................................................................................... 1

6 Test methods ............................................................................ 1

6.1 Screening tests ....................................................................... 2

6.2 Bond strength measurements ............................................... 3

6.3 Gap measurement test for adhesion to dentin .................... 11

6.4 Microlea kage test ................................................................. 12

6.5 Clinical usage tests ............................................................... 13

iTeh STANDARD PREVIEW
Annex
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14
A Bibliography . . . .. .. .. .. . . .. .. . . .. ... . . .. .. . .. .. .. . .. ... . ... . . .. ... . . .. .. . .. . .. . ... . .. . ..
ISO/TR 11405:1994
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0 ISO 1994
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechanical, including photocopyrng and
microfilm, without Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-l 211 Geneve 20 l Switzerland
Printed in Switzerland

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 0 ISO ISO/TR 11405:1994(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, governmental
and non-governmental, in liaison with ISO, also take patt in the work. ISO
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.

The main task of technical committees is to prepare International Stan-

dards, but in exceptional circumstances a technical committee may pro-
pose the publication of a Technical Report of one of the following types:
iTeh STANDARD PREVIEW
- type1I when the requi red suppo l-t cannot be obtai ned for the
(standards.iteh.ai) publica-
tion of an Inte rnat ional Standard, d espite repeated efforts;

- type 2, when
ISO/TR the subject is still under technical development or where
11405:1994
for any other reason there is the future but not immediate possibility
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of an agreement on an International Standard;
0f624eefd762/iso-tr-11405-1994
- type 3, when a technical committee has collected data of a different
kind from that which is normally published as an International Standard
(“state of the art”, for example).

Technical Reports of types 1 and 2 are subject to review within three years
of publication, to decide whether they tan be transformed into Interna-
tional Standards. Technical Reports of type 3 do not necessarily have to
be reviewed until the data they provide are considered to be no longer
valid or useful.

lSO/TR 11405, which is a Technical Report of type 2, was prepared by

Technical Committee lSO/TC 106, Dentistry, Subcommittee SC 1, Fihg
and res tora tive ma terials.

This document is being issued in the type 2 Technical Report series of

publications (according to subclause G.4.2.2 of part 1 of the ISO/lEC Di-
rectives, 1992) as a “prospective Standard for provisional application” in
the field of adhesion to tooth structure in dentistry because there is an
urgent need for guidance on how Standards in this field should be used
to meet an identified need.

This document is not to be refarded as “International Standard”. lt is pro-

posed for provisional application so that information and experience of its
use in practice may be gathered. Comments on the content of this docu-
ment should be sent to the ISO Central Secretariat.

...
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ISO/TR 11405:1994(E) 0 ISO

A review of this type 2 Technical Report will be carried out not later than
two years after its publication with the Options of: extension for another
two years; conversion into an International Standard; or withdrawal.
Annex A of this Technical Report is for information only.

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 0 ISO lSO/TR 11405:1994(E)

Introduction
The increasing importante of adhesion in restorative dentistry has made
it evident that information is needed on the relative Performance of ma-
terials which are claimed to bond to tooth structure. In the absence of
comparative clinical trials, much emphasis has been placed on laboratory
assessment of bond strength. While bond strengths cannot predict clinical
behaviour, they are valuable for screening.
Adhesive materials are used in many types of restorative and prophylactic
work. Even if the stress on the bond in most circumstances tan be de-
fined as either tensile, shear or a combination of these, there are no spe-
cific laboratory or clinical tests which tan be valid for all the various clinical
applications of adhesive materials.

iTeh STANDARD PREVIEW

lt is, therefore, the intention of this Technical Report to standardize as far
as possible different procedures whereby the effect or quality of a bond
(standards.iteh.ai)
between a dental material and the tooth structure may be substantiated.
By gaining experience with a specific testing System, a correlation be-
tween laboratory and clinical Performance of the materials should be
sought.ISO/TR
Data 11405:1994
from such correlations may then form the basis for revision
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of the document and simplification of appropriate testing.
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TECHNICAL REPORT Q ISO ISO/TR 11405:1994(E)

Dental materials - Guidance on testing of adhesion

to tooth structure

1 Scope 3.2 adherence: State in which two surfaces are held

together by interfacial forces.
This Technical Report specifies test methods for
evaluation of the adhesive bond between dental ma- 3.3 adherend: Body that is held, or is intended to
terials and tooth structure, i.e. enamel and dentine. lt be held, to another body by an adhesive.
describes two bond strength measurement tests,
tensile and shear, a test for measurement of marginal 3.4 adhesion: State in which two surface are held
gaps around fillings, a microleakage test, and gives together by Chemical or physical forces or both with
the aid of an adhesive.
iTeh STANDARD PREVIEW
guidance on clinical usage tests for such materials.

(standards.iteh.ai)
3.5 adhesive: Substance capable
terials together by adhesion.
of holding ma-

2 Normative references
ISO/TR 11405:1994 3.6 bond strength: Forte per unit area required to
The following Standardshttps://standards.iteh.ai/catalog/standards/sist/330ebb7a-6e09-4b98-aa68-
contain provisions which, break a bonded assembly with failure occurring in or
through reference in this text, constitute0f624eefd762/iso-tr-11405-1994
provisions near the adhesiveladherend interface.
of this Technical Report. At the time of publication,
the editions indicated were valid. All Standards are 3.7 Substrate: Material upon the surface of which
subject to revision, and Parties to agreements based an adhesive-containing substance is spread for any
on this Technical Report are encouraged to investi- purpose, such as bonding or coating.
gate the possibility of applying the most recent edi-
tions of the Standards indicated below. Members of
IEC and ISO maintain registers of currently valid 4 Requirements
International Standards.
This Technical Report contains no requirements for
ISO 3696: 1987, Water for analytical laboratory use - dental materials.
Specification and test methods.
5 Sampling
ISO 3823-1:1986, Dental rotary instruments -
Part 7: Steel and carbide burs. The amount of test material shall be sufficient for all
planned tests and have the Same lot or batch number.
DIN 69176: 1985, Körnungen aus Elektrokorund und
Siiiciumkarbid für Schleifmittel auf lJn terlagen -
Teil 1: Bezeichnung und Korngrössenverteilung.
6 Test methods
This Technical Report describes various types of
tests:
3 Definitions
a) screening tests;
For the purposes of this Technical Report, the follow-
ing definitions apply. UL 121 b) bond strength measurements;

3.1 adhere: Be in a state of adherence. c) gap measurement test for adhesion to dentine;

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ISO/TR 11405:1994(E 0 ISO

d) microlea kage test; ment on human teeth (6.2.2 and 6.2.3) should be
used.
e) clinical usage tests.
All forces exerted on a bond tan be resolved into
For some types, specific tests are described in detail. shear and tensile components and, since there is no
For other types, guidelines are given. lt is not the in- direct relation between the results obtained from the
tention to recommend testing each material by two measurements, it is preferable to measure both.
every test; some tests will not be appropriate. How-
ever, the quality and sophistication of a laboratory test 6.1.3.2 Condition of adhesive
cannot compensate for the fact that the final evidente
of adhesive properties has to be a clinical usage test. Bonding materials may be used in a thin film or in
bulk.
6.1 Screening tests As far as possi ble , materials should be applied in a
manner w hich dup licates thei clinical use.
6.1.1 Introduction
6.1.3.3 Storage of test specimens
Many screening tests may be necessary in the de-
velopment of new adhesive materials or for pro- Test specimens shall be prepared at (23 &- 2) “C and
duction control. Such tests may be performed on stored in water at (37 + 2) “C Prior to testing at
bovine teeth. (23 + 2) “C. Storage in water for 24 h is normally
sufficient to discriminate between those materials
However, the chemistry and especially the structure
which cannot and those which tan withstand a wet
of bovine teeth are not identical to those of human
environment. Thermal cycling between 5 “C and
teeth, and results from bovine teeth cannot replace
iTeh STANDARD PREVIEW
those from human teeth. The results of such tests
55 “C may be used as an accelerated ageing test.
Longer periods of water storage may be necessary to
should not be used for advertising or Promotion of the
material. (standards.iteh.ai)
show durability of bond.

The recommended procedure is as follows:

6.1.2 Tooth Substrate, and preparation ISO/TR 11405:1994
storage
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Test type 1: Short term test after 24 h in water at
The condition, storage and preparation of teeth,0f624eefd762/iso-tr-11405-1994
either 37 “C.
human or bovine, should be as described in 6.2 to
64. . Test type 2: Thermocycling test comprising 500
cycles in water between 5 “C and 55 “C, starting
6.1.3 Test methods after 20 h to 24 h storage in water at 37 “C. The
exposure to each bath should be at least 20 s, and
the transfer time between baths 5 s to IO s.
6.1.3.1 Type of test
Test type 3: Long term test after six-month
Many types of screening tests are available, for
storage in water at 37 “C.
example bond strength measurements, microleakage
tests, marginal gap measurements. If bond strength
measurements are used, the method adopted should 6.1.3.4 Strain rate for bond breakage
be either
The Standard rate of loading a bonded specimen is
a) tensile (bond broken by a forte perpendicular to recommended to be (0,75 + 0,30) mm/min cross-
head Speed, or more accurately (50 -+ 2) N/min. (The
the tooth surface); or
stiffness in the various testing machines and bond
b) shear (bond broken by a forte parallel to the tooth assemblies varies widely and hence 50 N/min is more
surface). meaningful than 0,75 mm/min.)

Methods which introduce “peel” Stresses are not ac- 6.1.3.5 Treatment of results
ceptable. Many current test methods fail to exert
purely tensile or shear forces on the bond. A special The bond strength values obtained by tensile or shear
Problem is the alignment in the tensile test and the testing show large coefficients of Variation, i.e. 20 %
correct and reproducible loading in the shear test- lt to 50 %. If the Variation is above 50 %, a thorough
is recommended that similar tests for screening pur- inspection of the Overall procedure is recommended.
poses to those described for bond strength measure- For screening purposes, six to ten specimens are re-

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0 ISO ISO/TR 11405:1994(E)

quired to give a meaningful average. Of greater im- appears that most changes occur in the initial days or
portance at this Stage may be inspection of fracture weeks after extraction, and therefore teeth one
surfaces visually at x 10 magnification and to deter- month, but not more than six months, after extraction
mine whether the fracture Pattern is of an adhesive, should be used. DO not use root-filled teeth. Teeth
cohesive or mixed nature. which have been extracted for longer than six months
may undergo degenerative changes in dentinal pro-
6.2 Bond strength measurements tein.

6.2.1 Introduction 6.2.2.3 Condition of teeth

The measurement of bond strength may be important The teeth used for bond strength measurement
when evaluating an adhesive material. However, the should be caries-free and preferably unrestored.
technique-sensitivity of such tests and the scatter of However, small and superficial restorations not in the
results due to variations in the Substrate, adhesive adhesion test area may be present. There is some
and handling limit the importante and use of the re- evidente to suggest that different areas of the
sults. dentition may give different results with bonding to
dentine and enamel. Bearing in mind the number of
Adhesive materials are used for many different pur- measurements required, it is not possible to control
poses in the mouth. The choice of test shall be con- variables such as age of the donating Patient, cultural
sidered according to the intended use of the material. and dietary history, state of health, or to standardize
the composition and structure of the teeth.
This Technical Report describes two types of tests,
tensile and shear. In addition, several variations such
6.2.2.4 Storage of teeth
as application in thin film and bulk, and short or long
exposure time to a wet environment are described.
iTeh STANDARD washedPREVIEW
Prior
A set of tests may be necessary properly to evaluate
to storage, the teeth should be thoroughly
in running water and all blood and adherent
the bond strength of a material.
(standards.iteh.ai)
tissue removed, preferably by the clinician. Teeth
should be placed immediately after extraction in dis-
When bond strength is to be measured, the raw data
are in units of forte (newtons). lt is desirable ISO/TR to con-11405:1994 tilled water (grade 3, ISO 3696) or in a 0,5 %
vert this into stress units, i.e., forte per unit area Chloramine bacteriostatic/bactericidal
https://standards.iteh.ai/catalog/standards/sist/330ebb7a-6e09-4b98-aa68- Solution for a
(megapascals). Hence, control of the surface for ap- maximum of 1 week and thereafter stored in distilled
0f624eefd762/iso-tr-11405-1994
plication of the adhesive material is paramount. water in a refrigerator at a nominal 4 “C. To minimize
deterioration, the storage medium should be replaced
6.2.2 Tooth Substrate and storage periodically. lt is essential that no other Chemical
agents be used. Such agents may be absorbed by,
6.2.2.1 Substrate and alter, tooth substance.

Human permanent teeth are required for the 6.2.2.5 Tooth surface preparation
measurement of clinically relevant bond strength.
When measuring bond strength to dentine, this A Standard, reproducible, flat surface is required.
Technical Report recommends that the superficial Tooth surfaces shall be kept wet at all times. Expo-
dentine, i.e. as close to enamel as possible, at the Sure of a tooth surface to the air for more than 15
buccal aspect of the third permanent molar from pa- minutes may Cause irreversible changes in bonding
tients in the age group 18 to 25 years be used to re- Character. Dentine is especially sensitive to dehy-
duce variations. However, if this restriction is difficult dration. The use of high-speed handpieces to prepare
to fulfil, the other molars or premolars may be used, tooth surfaces for bonding studies is to be avoided.
provided the teeth used are listed in the report of the A Standard surface is recommended such as that
investigation. produced against a Silicon carbide abrasive Paper with
a mean grit size of approximately 18 Pm (Grade 1000,
6.2.2.2 Time after extraction DIN 69176) under running water. To control the plan-
ing and the angle of the surface during surface prep-
There is increasing evidente that changes in dentine aration, the tooth should be mounted in a holder by
occur after extraction which may influence bond means of a dental die stone or a cold-curing resin. The
strength measurements. The effect may vary with absorption of resin and the heat of polymerization may
different types of bonding materials. ldeally, bond adversely affect the tooth. Avoid smearing of embed-
strengths should be measured immediately post- ding material on the tooth surface during final prepa-
extraction, but clearly this is not generally feasible. lt ration against the 1000 grade Silicon carbide, e.g. by

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ISO/TR 11405:1994(E) 0 ISO

mounting the tooth above the surface of the embed- (tooth CUP); b) is the counterpart either as a holder for
ding material. the adhesive materials applied in bulk, i.e. the material
cup or as the second Substrate, i.e. a small rod, when
6.2.2.6 Re-use of teeth applying the adhesive in thin film. For Iight-curing
Systems, the material cup may be made totally of a
Fresh teeth should preferably be used. If it is not transparent material, or alternatively it may be Split
possible to use a fresh tooth for every measurement, into two Parts with a smaller cup in a transparent resin
it is essential that “control” measurements using a and the connection to c) in metal, where c) is the
Standard material be undertaken frequently to check coupling to the alignment rod.
for irreversible changes caused by previous treat-
ments. Figure2 Shows the bonding alignment apparatus with
alignment rods, a), and the bonding alignment block,
6.2.3 Tensile bond strength b) .

6.2.3.1 Apparatus Figure3 Shows the measurement alignment block, b),

and the necessary alignment rods, a).
The various Parts of the tensile test specimen are
shown in figure 1: a) is a holder for mounting of teeth Figure4 Shows the polishing block.

Dimensions in millimetres

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a) Tooth cup

Hole

b) Material cuo/rod

Figure 1 - Tensile specimen

 ISO/TR 11405: 1994(E)

Dimensions in millimetres

t
6 63
m
a) ALiqnment rod for bondinq block (2 needed)

4 screws M 5 x 12
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0f624eefd762/iso-tr-11405-1994

b) Bondinq alignment block

Figure 2 - Bonding alignment apparatus