journal of dentistry 37 (2009) 691–699

available at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/jden

Effects of dentine moisture on the permeability of

total-etch and one-step self-etch adhesives

Geneviève Grégoire *, Philippe Guignes, Karim Nasr

Department of Biomaterials, Faculty of Odontology, University Toulouse III, 3 chemin des maraı̂chers, 31062 Toulouse Cedex 4, France

article info abstract

Article history: Objectives: The aim of this study was to compare the technique sensitivity of a one-bottle
Received 25 March 2009 total-etch adhesive and a self-etch primer adhesive to the moisture condition of the dentine
Received in revised form substrate.
7 May 2009 Methods: The methods used were hydraulic conductance, light microscopy and scanning
Accepted 8 May 2009 electron microscopy.
Results: When the moisture conditions of the dentine surface are modified with respect to
the standard, the bonded interfaces obtained with the one-bottle total-etch Adper Scotch
Keywords: Bond 1 XT (SB) and the all-in-one self-etch Adper Prompt L-Pop (AP) are morphologically
Dentine moisture highly perturbed. But, although this study also showed a significant ( p < 0.01) relationship
Technique sensitivity between increases in permeability of resin-bonded dentine and variations of dentine
Permeability moisture conditions with SB, a significant relationship was found only for the influence
Self-etch adhesive of the over-wet condition with AP.
Conclusion: Within the limitations of this study, the self-etch primer tested gave a greater
reduction in dentine permeability than the one-bottle adhesive, while being more tolerant
to handling. Although excess water should be avoided with both these systems, air-drying
can be an alternative to wet-bonding with the self-etch primers, thus reducing the sensi-
tivity to technique.
# 2009 Elsevier Ltd. All rights reserved.

1. Introduction Some authors have even described up to six different ways of

Obtaining an adherent and impermeable hybrid layer seems to
be a prerequisite for achieving immediate satisfactory
performance and preventing early chemical and mechanical
degradation of bonded interfaces. However, the process of
hybridisation to dentine is still a difficult challenge as it is
dependent on many factors related to the dentine substrate,
the adhesive system and the intervention of the operator.1–4
The moisture of dentine and its management during the
different steps of the bonding procedure is certainly the most
sensitive parameter. Depending on the adhesive system used,
its mode of action and its composition, the degree of moisture
present before the adhesive primer applied is highly variable.
drying the dentine surface.5
Currently, the ‘‘wet-bonding’’ technique6 is the most
popular method for use with total-etch adhesive systems
but also one of the most sensitive technique.7,8 Maintaining a
sufficient degree of humidity is essential after the acid etching
and rinsing steps so as to avoid the collapse of demineralised
collagen fibrils and to provide a porous collagen network for
the infiltration of the adhesive monomers9,10 but an excess of
water leads to dilution of the monomers, which inhibits their
progression and interferes with their polymerisation. To
simplify the bonding procedures and preserve the capabilities
of adhesives to spread through the demineralised dentine
matrix, priming adhesive systems or one-bottle adhesive

* Corresponding author. Tel.: +33 05 62 17 29 40; fax: +33 05 61 25 47 19.

E-mail address: gregoire@cict.fr (G. Grégoire).
0300-5712/$ – see front matter # 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2009.05.010
692 journal of dentistry 37 (2009) 691–699

systems have been developed. These simplified total-etch
systems combine the functions of the dentine primer and
bonding agent in one vial with the incorporation of a
significant amount of hydrophilic monomers such as hydroxyl
ethyl methacrylate (HEMA) combined with various aqueous or
organic solvents. But they still use a phosphoric acid etch
requiring a dentine blot-drying step and remain susceptible to
problems associated with this technique. Self-etching primer
systems also belong to the contemporary generation of
simplified adhesive systems but their strategy of action is
quite different. They incorporate specific monomer molecules
which combine unsaturated polymerisable functions with
carboxylic or phosphoric acid groups.11 Such systems may be
preferred clinically to avoid the rinsing and drying stages and
accelerate the procedure. Moreover, several studies have
claimed that these systems are less sensitive to dentine
moisture with the same performance and better reproduci-
bility on air-dried dentine.12–14 However, the very hydrophilic
monomers in these systems produce polymers that are highly
hydrophilic too, leading to the formation of genuine semi-
permeable membranes before and after polymerisation.15
Several studies have shown that water trees, voids and water
droplets, and phase separation occur in the adhesive interface
of one-bottle and all-in-one adhesives.16–18 Any of these, as
potential sites for hydrolytic degradation, may affect the
longevity of bonded restorations.19 Therefore, it seems that,
whatever the type of simplified adhesive systems used,
obtaining a tight interface appears to be a difficult challenge.
This difficulty is reinforced by clinical conditions under the
rigorous protocols for implementation.
Moreover, although many studies have investigated the
influence of dentine moisture on bond strengths,13,20–22 little
research has attempted to correlate the effects of these
variations on the permeability of the bonding interfaces.
The aim of this study was to compare the technique
sensitivity of two kinds of simplified adhesives, a one-bottle
total-etch and a self-etch primer, under different conditions of
dentine moisture such as blot-drying, air-drying and over-wet,
using staining, light and scanning electron microscopy, and
hydrolytic conductance. The null hypotheses that were tested
were1: that there is no difference in the permeability of resin–
dentine interfaces obtained with total-etch adhesive and self-
etching adhesive systems under normal wet conditions, and2
that self-etching adhesive systems are not sensitive to varia-
tions in the moisture condition of the dentine substrate before
their application.
2. Materials and methods
2.1. Microscopy
60 human molars were used for the study. After extraction, they
were kept in chloramine T at 4 8C until use. The teeth were cut
parallel to the occlusal face using a low-speed saw (Isomet 2000,
Buehler, Evanston Ill.) equipped with a rotating diamond-
impregnated copper disk (11-4244-15 HC, Buehler Ltd.) under
water spray. A fine smear layer was obtained and was
reproducible on all specimens. Deep dentine was chosen for
the tests to favour the diffusion of the dentine bonding system in
demineralised dentine, thus providing the best conditions for
the resin–dentine interaction. The dentine disks were randomly
assigned to two groups: group I received an application of Adper
Prompt L-Pop (3M-ESPE) (AP), a self-etch compound, and group II
received an application of Adper Scotch Bond 1 XT (3M-ESPE) (SB)
preceded by a phosphoric acid etch (Table 1). Each adhesive was
applied to 10 dentine disks according to the manufacturer’s
instructions (N) (Table 2), then to 10 other disks where the
dentine had been made too dry (D) by applying an air jet with an
air-syringe for 5 s to 1 cm from the dentin surface, and to 10
others where the dentin had been made too wet (W) by wiping
the surface with a soaked cotton pellet, as recommended for the

Table 1 – Products, manufacturers, components, batch numbers, chemical compositions of the dentine adhesives tested.
Adhesives tested Manufacturer Classification Batch # Composition

Adper Prompt L-Pop 3M ESPE, St. Paul, One-step self-etch 20021002 Mono- and di- HEMA phosphates, Bis-GMA,
MN, USA adhesive polyalkenoate camphorquinone, substituted
aromatic amine, substituted, aminobenzoate,
phosphine oxide, stabiliser, water

Adper Scotch Bond 1 XT 3M ESPE, St. Paul, One-bottle two-step 158821 Etchant: 35% H3PO4
MN, USA total-etch adhesive 010300167 Adhesive: Bis-GMA, HEMA, dimethacrylates,
polyalchenoic acid, copolymer, ethanol,
water 3–8%, initiators

Table 2 – Manufacturer’s instructions for use of adhesives tested.

Adhesives tested Manufacturer’s instructions

Adper Prompt L-Pop
Adper Scotch Bond 1 XT
Activate blister pack by emptying the liquid out of the red blister into the yellow blister. Brush the adhesive
onto the dentin and enamel surfaces. Massage it in for 15 s, briefly air-dry, apply a second coat for 3 s.
Use a gentle stream of air to thoroughly dry the adhesive to a thin film
Etch enamel for 30 s and dentine for 10 s, rinse with air/water spray for 10 s and blot excess water
using a cotton pellet
Immediately after blotting, apply 2–3 consecutive coats of adhesive to etched enamel and dentine for 15 s
with gentle agitation using a fully saturated applicator. Gently air thin for 5 s to evaporate solvents
 journal of dentistry 37 (2009) 691–699
wet-bonding technique, and thus covering it with 10 ml of water.
The prepared specimens were kept in a humid atmosphere for
48 h.
2.1.1. Specimen preparation for optical microscopy
Five disks of each subgroup were used for optical microscopy.
They were fixed in 10% formaldehyde (Rhone-Poulenc Ltd.,
Manchester, England) for 2 days, demineralised with 5%
trichloroacetic acid (Merck, Darmstadt, Germany) for 5 days,
and then rinsed in water for 2 h. The specimens were
dehydrated in ascending grades of alcohol then cleared in
toluene for h before being impregnated with paraffin (Merck)
for 2 days. They were then embedded in paraffin, and 5 mm
sections were cut with a microtome (Reichert–Jung NuBlock
Germany). The sections were successively stained with
Goldner’s trichrome, a classic bone stain, and with crystal
violet and picric acid. The stained sections were observed and
photographed using an optical microscope (020-507-101 Wild
Leitz GmbH, Heerbrugg, Switzerland).
2.1.2. Specimen preparation for scanning electron microscopy
Five dentine disks from each subgroup were used for scanning
electron microscopy. They were fractured into two parts,
decalcified in phosphoric acid for 20 s and deproteinised for
60 s in 2% sodium hypochlorite. The specimens were fixed in
2.5% glutaraldehyde, then rinsed and dehydrated in alcohol.
They were dried by immersion in pure hexamethyl disilazane
(HMDS) for 20 min. The HMDS was allowed to evaporate for
15 min in air before specimens were sputter-coated in gold
palladium. The specimens were examined and photographed
with an SEM (S450, Hitachi, Tokyo, Japan) using an acceleration
voltage of 15 kV. The structure analysed was the architecture of
the interface.
2.2. Hydraulic conductance
60 extracted non-carious human third molars from patients 18–
25 years old were used for this part of the study. Specimens were
systematically prepared within 1 h of extraction to minimise
the variables of time or mode of storage. Dentine disks were cut
from crown segments parallel to the occlusal surface at the top
of the pulp chamber,23 using a low-speed saw (Isomet 2000;
Buehler, Evanston, Ill.) equipped with a rotating diamond-
impregnated copper disk (11-4244; Buehler). The dentine
specimens were considered to represent deep dentine, an area
where the number and diameter of dentinal tubuli increases.24
Deep dentine was chosen to favour the infiltration of the
dentine bonding systems into the demineralised dentine, thus
providing ideal conditions for the resin–dentine interaction.
Occlusal enamel was removed by means of a second cut parallel
to the section of the dentine, resulting in specimens
1.3  0.1 mm thick. The specimens were reduced to a thickness
of 1 mm by polishing with progressively finer abrasive disks
(Pregrinder; Knuth-Rotor Struers, Copenhegen, Denmark) to
create a smooth, uniform surface on both sides. All polishing
procedures were performed by the same operator, who
measured the thickness with electronic digital callipers
(RS232C; Colombié Cadet, Toulouse, France) with an accuracy
of within 0.03 mm. Any specimens in which presence of the
pulp horn or enamel was detected were eliminated, as were
693
specimens that were found to be less than 1 mm thick after
polishing. The 60 dentine specimens were randomly divided
into 6 groups of 10 by drawing lots. The dentine specimens were
kept in a moist atmosphere (in a flask containing a damp
compress) at laboratory temperature (22  1 8C). For each
specimen, the occlusal and pulpal surfaces were identified by
a mark made with the bur when they were cut. Both sides of the
specimens were etched with 36% phosphoric acid for 15 s to
eliminate the smear layer formed during preparation proce-
dures. The pulpal surface was centred on a polycarbonate disk
made in the authors’ laboratory with a 6-mm diameter circular
perforation in the centre and secured with cyanoacrylate glue
(Araldite; CIBA Sodiema, Coubert, France) that was allowed to
dry for 2 h. The initial fluid flow (200 cm H2O) through a slice of
the dentine was evaluated by measuring the passage of
physiological saline as described below. Any specimens in
which the bubble moved completely through the capillary tube
in less than 15 min (the time allotted for the experiment) were
considered to have a defective cyanoacrylate marginal seal.
These specimens were dismantled and reassembled with a new
layer of cyanoacrylate glue. To compensate for the great
variations in permeability of the various dentine specimens,
all subsequent permeability measurements made on the same
specimen were expressed as a percentage increase or decrease
with respect to the initial hydraulic conductance.25 Thus, each
specimen served as its own control. An experimental, standar-
dised smear layer was produced on the occlusal surface of each
specimen by means of 50 consecutive abrasions executed by
manually moving very fine grained sandpaper (P 4000; Buelher)
horizontally and without vertical force under water irrigation.
Other authors have created a thicker smear layer by using 320
grit sandpaper,26 a dental bur,27 or 60 grit sandpaper but the
present method was chosen to permit comparisons to be made
with the results of our previous study.31 The hydraulic
conductance was measured again after the experimental
abrasion, at time T0. The smear layer was etched for the
control system using separate etching steps and rinsing, and
the hydraulic conductance of these specimens was measured
again, at time T1. The dentine disks were divided into two
groups: 30 to receive AP and 30 SB. Each group was divided into
three subgroups of 10 dentine disks. Each adhesive was applied
to 10 dentine disks according to the manufacturer’s instructions
(Table 2), then to 10 disks where the dentine was too dry and to
10 where it was too wet (Table 3). The hydraulic conductance
was measured for all specimens after application, at time T2.
2.2.1. Measurement of hydraulic permeability
The method employed for measuring hydraulic conductance
was derived from Pashley’s method28 and has been described
in previous works.30,31 Each test specimen was placed
horizontally in the holder so that the pressure was applied
to the pulpal surface of the dentine. Various analyses were
carried out at the following times: at T1, fluid conductance
after creation of a smear layer with respect to the initial acid-
etched conductance value and at T2, fluid conductance after
adhesive application with respect to the initial acid-etched
value. To compensate for the great variation in penetration
capacity among the specimens (due to biological variability),
measurements were expressed as relative rather than
absolute values. Each experimental value was expressed as
694 journal of dentistry 37 (2009) 691–699

Table 3 – Results of hydraulic conductance after creation of a smear layer (T1) and after adhesive application (T2), with
respect to the initial acid-etched value.
Bonding agent T1 (smear layer) T2 (post-adhesive) Duncan’s test

Adper Scotch Bond 1 XT (N—normal) 45.435  22.3 54.549  12.6 a

Adper Scotch Bond 1 XT (D—dry) 44.510  12.6 17.535  11.2 b
Adper Scotch Bond 1 XT (W—wet) 38.933  19.6 51.441  19.0 a
Adper Prompt L-Pop (N—normal) 48.126  20.2 62.600  13.8 c
Adper Prompt L-Pop (D—dry) 44.642  14.5 60.660  17.067 c
Adper Prompt L-Pop (W—wet) 43.918  18.5 47.209  16.449 d

a percentage increase or decrease relative to the initial acid-
etched value for the specimen under consideration. Each
specimen thus acted as its own control. The statistical analysis
comprised an analysis of the mean and standard deviation for
each test group, an analysis of variance considering the T1 and
T2 measurements as repeated measurements on a given
specimen, and Duncan’s new multiple range test (a = 0.05).
and the tags are bright pink, and the adhesive is beige. With
the second stain, mineralised dentine is blue and the adhesive
is beige. The hybrid layer and the tags are pink. Both stains
show an irregular hybrid layer and less numerous tags, or even
none at all, when the dentine is too dry or too wet. When the
dentine is over-wet, droplets can be seen in the hybrid layer for
AP (Fig. 6a).

3.1.2. Interface structure observed by scanning electron

3. Results microscopy
Representative SEM micrographs of the dentine interfaces
3.1. Microscopy obtained with the two adhesives following the technique
recommended by the manufacturer on normally humid
3.1.1. Interface structure observed by optical microscopy dentine, and with over-dry or over-wet dentine are shown
Representative optical micrographs using Goldner’s trichrome in Figs. 7–13. The interface obtained with SB in normal
and crystal violet and picric acid are shown in Figs. 1a–6b. With conditions has a thick hybrid layer (2–10 mm thick), and tags up
the first stain, mineralised dentine is yellow, the hybrid layer to 100 mm long with a conical swelling at the base and side

Fig. 1 – Distribution of specimens depending on the humidity of the dentin (N: normal, D: air-dried for 10 s with a spray of
air, W: wet with 10 ml of water), and analytical techniques (light microscopy (LM), scanning electron microscopy (SEM) or
hydraulic conductance).
 journal of dentistry 37 (2009) 691–699 695

Figs. 2–4 – Fig. 2(a) and (b): Representative light micrographs of the dentin with Adper Scotch Bond 1 XT. The hybridized
complex is thick with numerous tags. V-shaped plugs are visible at the tubuli mouths. Fig. 3(a) and (b): Representative light
micrographs of the dentin with Adper Scotch Bond 1 XT when the dentin is too dry. Irregular tags are visible. Most are not
homogeneous. Fig. 4 (a) and (b): Representative light micrographs of wet dentin with Adper Scotch Bond 1 XT. The
hybridized complex is generally thick but is sometimes not continuous. In particular many gaps are visible with the stain
used in (b). The tags lack density and voids are often visible with the stain used in (a).

branches (Fig. 7). The specimens of SB on over-dry dentine
show an interface with a thin and irregular hybrid layer
varying in thickness between 1 and 3 mm (Fig. 8). With over-
wet dentine, frequent voids and porosity are clearly visible in
the adhesive layer. The hybrid layer itself does not appear to be
particularly perturbed, nor do the tags (Figs. 9 and 13). AP used
in normal conditions shows a regular hybrid layer. The layer
becomes irregular when the dentine is over-dry, with the
hybrid layer becoming detached from the adhesive in places
(Fig. 11). When the dentine is over-wet, numerous droplets can
be seen in the hybrid layer (Fig. 12).
3.2. Hydraulic conductance
The results at T1 and T2 are presented in Table 3. The creation
of a smear layer entailed a mean decrease of permeability of
between 40 and 50% with relatively high standard deviations
with respect to the mean value, indicating differences among
the dentine specimens used. The variability in dentine
specimens justified the use of each specimen as its own
control. Analysing the ‘‘adhesive’’ factor by comparing the
mean and standard deviation revealed that, when the normal
protocol was used, the self-etch adhesive led to a greater
reduction in permeability (62.6%) than the adhesive with a
separate etch (54.5% reduction). This difference is significant.
For AP, the values for over-dry and normal dentine were fairly
similar, whereas over-wet dentine led to a permeability
variation (47.2% reduction). For SB the values for over-wet
and normal dentine were fairly close (51.4 and 54.5%
reductions) while the over-dry dentine gave a permeability
reduction of only 17.5%. The factor ‘‘normal’’, ‘‘over-wet’’,
‘‘over-dry’’ was analysed for each type of adhesive separately.
Within the SB group, an ANOVA showed that the NWD factor
was a significant one. The value of F was 19.430. Analysis by
Duncan’s new multiple range tests showed that over-dry was
different from over-wet and normal. For AP: analysing the
696 journal of dentistry 37 (2009) 691–699

Figs. 5–7 – Fig. 5(a) and (b): Representative light micrographs of the dentin with Adper Prompt L-Pop. The hybrid layer is thick
and continuous. Tags are numerous and thick, and V-shaped at their junction with the hybridized complex (original
magnification 320T). Fig. 6(a) and (b): Representative light micrographs of the dentin with Adper Prompt L-Pop when the
dentin is too dry. Tag formation is less marked. Fig. 7(a) and (b): Representative light micrographs of the dentin with Adper
Prompt L-Pop when the dentin is too wet. Numerous droplets can be observed in the hybrid layer.

NWD factor gave a value of 2.793 for F with p = 0.0790. The only
noteworthy feature was that there was higher standard
deviation with respect to the mean for over-wet dentine than
for over-dry or normal. No statistically significant difference
was found among over-dry, over-wet and normal but there
was a statistically significant difference between over-wet and
over-dry. Analysis using a t-test and least squares showed that
the value of t between over-wet and over-dry was 2.170
( p = 0.039 (significant)), between over-dry and normal was
0.273 ( p = 0.786 (not significant)) and between over-wet and
normal was 1.896 ( p = 0.687 (significant)).
4. Discussion
Hydraulic conductance is a non-destructive method that does
not require dehydration of the samples and allows tests to be
performed in close-to-physiological conditions with the
implicit role of pulpal pressure. This methodology has already
been used successfully in studies of water fluid flow within
resin–dentine bonds during and after bonding procedures
with total-etch and self-etch adhesives.29–31 But this study is
the first to apply it to compare the influence of moisture
conditions on dentine permeability of the bonded interfaces.
Both adhesive systems used, Adper Prompt L-Pop (AP) and
Adper Scotch Bond 1 XT (SB), are contemporary, water-based,
hydrophilic, simplified adhesive systems incorporating water
or water/ethanol solvents respectively. The manufacturers
recommend that the wet dentine surface should be blot-dried
before application of the adhesive system, so as to obtain an
optimal amount of water in the dentine substrates, experi-
mentally determined as 1.5 ml.32 Thus, our air-dried (5 s) and
over-wet conditions (10 ml of water) could appear to be
extreme. Actually, these conditions are frequently encoun-
tered in the clinical environment, where use of the air-syringe
is a common gesture and where the contamination of
dentinal surfaces with blood, saliva and gingival fluid can
exist.
 journal of dentistry 37 (2009) 691–699 697

Figs. 8–14 – Fig. 8: Representative SEM micrographs showing the adhesive–dentin interface with Adper Scotch Bond 1 XT. A
conical swelling can be observed. Note the thick, uniform hybridized complex and the numerous tags with conical swellings at
their junction with the hybrid layer (original magnification 2500T). Fig. 9: Representative SEM micrographs showing the
adhesive–dentin interface with Adper Scotch Bond 1 XT when the dentin is too dry. A thin, discontinuous hybrid layer can be
seen (original magnification 1500T). Figs. 10 and 14: Representative SEM micrographs showing the adhesive–dentin interface
with Adper Scotch Bond 1 XT when the dentin is too wet. Note the presence of numerous porosities (original magnification
1000–2500T). Fig. 11: Representative SEM micrographs showing the adhesive–dentin interface with Adper Prompt L-Pop. A
thick hybridized complex can be seen, with numerous tags. Tags systematically show marked conical swellings at their
bases, which is the sign of a good seal (original magnification 2500T). Fig. 12: Representative SEM micrographs of the dentin
with Adper Prompt L-Pop when the dentin is too dry. Particularly noteworthy is the small number of tags. The hybrid layer is
detached from the dentin in places. Fig. 13: Representative SEM micrographs of the dentin with Adper Prompt L-Pop when the
dentin is too wet. Numerous droplets are observed in the hybrid layer.

The results of this study indicated that, when moisture morphologically highly perturbed. However, although the study
conditions at the dentine surface were modified with regard to also showed a significant ( p < 0.01) relationship between
the standard, the bonded interfaces obtained with the one- increases in the permeability of resin-bonded dentine and
bottle total-etch SB and the all-in-one self-etch AP were the variations of dentine moisture conditions with SB, a
698 journal of dentistry 37 (2009) 691–699
significant relationship was found concerning only the influ-
ence of the over-wet condition with AP. These results could be
explained, on the one hand, by differences in the modes of
action and the compositions of the adhesives tested and, on
the other, by the hydrodynamic properties of the hydraulic
conductance.
When the wet-blotting technique is used, according to
previous studies, SB and AP form quite similar bonded
interfaces with a continuous and uniform hybrid layer and
a forest of laterally branched cylindrical-conical resin tags.33,34
However, in spite of a thinner hybrid layer, AP provided a
better reduction in permeability in the present investigation.
This similarity of action can be explained by the low
concentration and pH of AP acidic monomers, which allow
it to completely dissolve the smear layer and smear plugs.35
Because self-etching systems such as AP do not require a
rinsing step, the smear layer is impregnated but not
eliminated and the interfibrillar spaces in the walls of etched
tubules are not filled with water. Previous studies have shown
that, with water-based solvent total-etch systems, such as SB,
water remaining after the rinsing step could be responsible for
elution and incomplete polymerisation of the adhesive
monomers, resulting in a lack of contact between the resin
tags and the tubule walls33 and a discrepancy between the
depth of acid etching and resin infiltration into exposed
collagen matrices. This incomplete hybridisation of resin tags
to tubule walls could permit fluid movement from dentinal
tubules to adhesive interfaces in total-etch adhesives.
When demineralised dentine is air-dried, water contained
in the interfibrillar spaces is removed and the collagen fibril
network collapses, creating a veritable shrink grate reinforced
by interpeptide hydrogen bonds, which is practically
impermeable to adhesive resins. Moreover, the desiccation
decreases the wettability of the dentine surface. SB is an
ethanol/water-based solvent adhesive, containing 32.5 wt%
(45 vol.%) of ethanol, the optimal concentration of solvent for
this adhesive formulation to allow a decrease of the viscosity
that facilitates the wetting of the surface and the penetration
of the adhesive into the wet demineralised dentine matrices.36
Water/ethanol solvents with a solubility parameter for
hydrogen bonding (dh) higher than 19.0 (J/cm3)1/2 are supposed
to be able to break these interpeptide bonds, re-expanding the
matrix and facilitating the wetting of the adhesive.37 Our
results tend to show that their action is insufficient, with a
hybrid layer that is thinner than that obtained under wet-
blotting conditions and often intermittent, and correlated
with a dramatic increase of the dentine permeability.
Similarly, the active rubbing of the surface, recommended
for the resulting increase of entropy, does not appear to
improve the performance of SB on air-dried demineralised
dentine substrate in this case.38
Without an etching step, the risk of collapse is inexistent
for self-etching adhesives. But water is essential to maintain
the ionisation state of these functional monomers and to
allow them to express their acidic potential. SEM micrographs
of air-dried specimens treated with AP showed a hybrid layer
that was still uniform and compact but accompanied by
smoother and less numerous tags of resin. We speculate that
the deficit in water of the dentine substrate associated with its
very hydrophilic character entail an absorption of the water of
the adhesive solution by the underlying dentine, decreasing
the action of the acid and thus the depth of demineralisation.
However, our results showed that the decrease in the
permeability of air-dried dentine after AP application was
not significantly different from that obtained on wet-blotted
dentine, confirming the importance of a good-quality hybrid
layer independently of the number and length of resin tags.
Under conditions of excessive moisture, the semi-perme-
able membrane properties, already highlighted by several
studies, are exacerbated, with the formation of droplets and
water blisters.15,39 The origin of these droplets of water is
mainly attributed to the presence of HEMA in the formulation
of these simplified adhesives.40 Depending on the adhesive
used, these droplets have different localisations with refer-
ence to the adhesive layer, different sizes and different
behaviours. SB showed droplets located throughout the
adhesive layer, which gave it a very porous aspect. The
origin of these inclusions of water is attributed to a phase-
separation reaction. SB contains 60–70 wt% of Bis-GMA and
30–40 wt% of HEMA. 30–40% seems to be the optimal
concentration of HEMA to prevent phase separation under
normal conditions of moisture.41 Beyond a ratio of 25% of
water, HEMA and Bis-GMA separate into two distinct
phases.42 Hydrophobic particles rich in Bis-GMA would be
isolated and included in a matrix rich in hydrophilic HEMA.
Devoid of purely hydrophobic monomers, the droplets
formed at the bonding interfaces of AP with over-wet dentine
do not come from a phenomenon of phase separation. These
droplets result from water attraction, diffusion of water and
osmosis through the cured adhesive layer as previously
suggested. These droplets are situated only at the resin-
composite boundary, a zone which corresponds to the
oxygen-inhibition layer, a hypertonic area. Whatever their
origin, these droplets reduce the thickness of the layer of resin
and provide real spaces for the passage of water between the
underlying dentine and the adhesive/composite interface.
Our measurements of the water conductivity confirm that
this phenomenon is accentuated by the pulpal pressure as
already noted in a previous study.43
It has been shown that, even in the conditions of moisture
recommended by the manufacturer, when the pulpal pres-
sure is applied to a bonded interface devoid of droplets, some
can eventually appear at the adhesive/composite interface.
Moreover, their formation and movement across the hybrid
layer thickness could explain the imperfect sealing of these
adhesive resins to dentine under normal dentine moisture.
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