Moisture Spectrum of Demineralized

Dentin for Adhesive Systems with

Different Solvent Bases
Alessandra Reisa/Alessandro Dourado Loguercioa/
Caio Lucidius Naberezny Azevedob/Ricardo Marins de Carvalhoc/
Julio da Motta Singerd/Rosa Helena Miranda Grandee

Purpose: To determine the effects of different surface moisture on the bond strength of an ethanol/wa-
ter-based (Single Bond [SB]), an acetone-based (One-Step [OS]), and a water-based (Syntac Single Com-
ponent [SC]) adhesive system to dentin.
Materials and Methods: On 90 human third molars, a flat superficial dentin surface was exposed by
abrasion with 600-grit SiC paper. The adhesives were applied to a delimited area of 52 mm2 according
to the manufacturers’ instructions on either dry (oil-free air/30 s) or rewetted surfaces (1.5, 2.5, 3.5,
4.0 or 4.5 µl of distilled water), and composite crowns were constructed incrementally. After storage in
distilled water at 37°C for 24 h, the teeth were longitudinally sectioned in the “x” and “y” directions to
obtain bonded sticks with a cross-sectional area of 0.8 mm2. The specimens were tested in tension at
0.5 mm/min and the fracture mode analyzed. Resultant bond strength was expressed as an index that
includes bond strength values of the different fracture patterns and the specimens that failed during
preparation for the microtensile testing. The data was analyzed by two-way ANOVA, Tukey’s multiple com-
parison, and regression analysis.
Results: Highly significant main effects and interaction (p < 0.0001) were detected. A quadratic relation-
ship between the bond strength index and the surface moisture was identified (R2 = 0.95, p < 0.001).
SB showed a maximum bond strength (42.2 ± 6.7 MPa) that was statistically similar (p = 0.4996) to the
maximum bond strength of OS (40.1 ± 4.6 MPa), although obtained at a different degree of moisture
(ca 1.5 µl for SB and 3.5 µl for OS). SC showed its maximum bond strength (27.7 ± 3.9 MPa) with 1.5
µl moisture. SB presented its highest bond strength at 1.5 µl of water, which was significantly higher
than the bond strength obtained at any other degree of moisture (p < 0.05). OS achieved its maximum
bond strength at 3.5 µl of water; however, that value was not statistically different (p > 0.05) from the
values obtained with 1.5 µl to 4.0 µl of water. Similarly, highest bond strengths obtained with SC were
not different (p > 0.05) within the range of 0 µl to 3.5 µl of water.
Conclusion: All adhesive systems tested had a different moisture spectrum in which higher bond
strengths were obtained. SB and SC performed better on a drier substrate, while OS showed better per-
formance on wetter substrates. OS and SC had a broader range of moisture within which maximal bond
strength could be achieved.

J Adhes Dent 2003; 5: 183–192. Submitted for publication: 16.09.02; accepted for publication: 10.02.03.

a Assistant Professor, Department of Dental Materials and Operative
Dentistry, University of Oeste de Santa Catarina, SC, Brazil.
b Graduate Student, Department of Statistics, Institute of Mathemat-
ics and Statistics, University of São Paulo, São Paulo, Brazil.
c Associate Professor, Department of Operative Dentistry, Endodon-
tics and Dental Materials, University of São Paulo, Bauru, SP, Brazil.
d Professor, Institute of Mathematics and Statistics, University of São
Paulo, SP, Brazil.
e Associate Professor, Department of Dental Materials, University of
São Paulo, São Paulo, SP, Brazil.
Reprint requests: Dr. Alessandra Reis, Universidade do Oeste de Santa
Catarina, Campus Joaçaba, R. Getúlio Vargas, 2125, Bairro Flor da Ser-
ra, CEP: 89600-000. Joaçaba, SC, Brazil. Tel/Fax: +55-49-551-2000.
e-mail: reis_ale@hotmail.com

Vol 5, No 3, 2003 183

Reis et al
t is known that resin infiltration to form the hybrid
I layer depends on intra- and intertubular dentin per-
meability.22 Demineralization of intertubular dentin
and maintenance of interfibrillary porosity is re-
quired for monomer penetration into the dentin.
When demineralized dentin is air dried, collagen
fibrils are brought closer together, resulting in the
collapse of the matrix, which reduces the permeabil-
ity of the demineralized zone.21 This has been shown
to cause marked reduction of the bond strengths to
dentin.11,19
Conversely, when dentin is kept moist, fibrils are
observed to be upright and separated by wide inter-
fibrillary spaces, resulting in a better opportunity
for resin infiltration.36,39 Higher bond strengths
have been consistently reported when adhesives
are applied on wet substrate than when applied to
previously air-dried dentin surfaces.10,19
Although wet bonding has been considered the
ideal technique for current adhesives, an examina-
tion of several in vitro and in vivo studies indicates
that there is no consensus regarding the proper de-
gree of moisture to be used with such adhesives.
Laboratory investigators usually report that adhe-
sives were applied according to manufacturers’ di-
rections; however, the moisture concept varies
widely among the instructions for different adhe-
sive systems as well as among investigators.
Kanca17 has shown a great variability of bond
strength values by varying the drying time and the
tooth/air-syringe distance.
Tay et al36 attempted to characterize an optimal
moisture zone between the two extremes of over-
drying and overwetting, in which optimal hybridiza-
tion and tubular seal is obtained, and reported it as
the “window of opportunity”. According to these au-
thors, the extent of such an optimal moisture zone
is governed by material factors, such as the pre-
sence of water in the respective adhesive system,
and environmental factors, including the intrinsic
surface wetness of the acid-conditioned dentin.
As a consequence, some authors have suggest-
ed that the ideal moisture spectrum may differ de-
pending on the composition of the adhesive, partic-
ularly the type of solvent included.7,36 Thus, the
adoption of standard surface moisture may lead to
less than optimal quality of bonding depending on
the type of adhesive used. Although it is practically
impossible to precisely determine the ideal surface
moisture in a clinical situation, in vitro studies are
useful to properly establish the ratio of water vol-
ume per surface area of dentin, thereby permitting
184
the control of the surface moisture. To our knowl-
edge, no study has attempted to investigate the re-
lationship between controlled surface moisture and
the bond strengths obtained with adhesive sys-
tems containing different solvents.
The objective of this study was to determine the
effects of different degrees of surface moisture on
the bond strength to dentin of three adhesive sys-
tems with different solvents. The null hypothesis
was that there is no influence of the surface mois-
ture on the bond strength of the adhesives, regard-
less of the type of solvent in their composition.
MATERIALS AND METHODS
Three systems with different solvent bases were
tested: Single Bond (SB, 3M ESPE, St Paul, MN,
USA), an ethanol/water-based system; One-Step
(OS, Bisco, Schaumburg, IL, USA), an ace-
tone-based system; and Syntac Single Component
(SC, Vivadent, Schaan, Liechtenstein), a wa-
ter-based system. Their composition, application
mode, and batch number are described in Table 1.
For this experiment, 90 extracted human third
molars were used. The teeth were collected after
obtaining the patient’s informed consent under a
protocol approved by the University of São Paulo In-
stitutional Review Board. The teeth were disinfect-
ed in 0.5% chloramine9 and used within six months
after extraction. The samples were divided into
eighteen experimental groups of 5 teeth for each
tested condition, as shown in Fig 1.
A flat dentin surface was exposed after wet grind-
ing the occlusal enamel on 180-grit SiC paper. The
enamel-free, exposed dentin surfaces were further
polished on wet 600-grit SiC paper for 60 s to cre-
ate a standardized smear layer. The bonding area
was demarcated by placing a piece of masking tape
with a punched hole of 8.45 mm diameter on the
center of the surface. This yielded a standard area
for bonding of approximately 52 mm2.
After acid etching with the respective etchants
(Table 1), the surfaces were rinsed with distilled wa-
ter for 20 s and severely air dried for 30 s with
oil-free compressed air. The adhesives were applied
on a surface that was either kept dried (0 µl of wa-
ter) or rewetted (Fig 1) with different amounts of dis-
tilled water (1.5, 2.5, 3.5, 4.0 or 4.5 µl) by means
of a micropipette (Pipetman, Gilson, NY, USA). The
adhesives were applied after rewetting the surface,
and light activated for the time recommended by the
The Journal of Adhesive Dentistry
 Reis et al

Table 1 Adhesive systems and application sequence

Adhesive systems Composition Application mode Batch number

Single Bond 1. Scotchbond: 37% phosphoric acid a, b, c, d*, e1, f1, g1 9CX
(3M ESPE) 2. Adhesive: bis-GMA, HEMA, dimethacrylates, polyalquenoic
acid copolymer, initiators, water and ethanol

One Step 1. Uni-Etch: 32% phosphoric acid a, b, c, d*, e1, f1, g1 CE0459
(Bisco) 2. Adhesive: bis-GMA, BPDM, HEMA, initiator, and acetone

Syntac Single Com- 1. Total Etch: 37% phosphoric acid a, b, c, d*, e2, f2, g2, D56201
ponent (Vivadent) 2. Maleic acid, HEMA, polyacrylic acid modified by methacry- e2, f2, g2
lates, initiators, and water

a – acid etch (15 s); b – rinse (15 s); c – air-dry (30 s); d* – dentin kept dry or rewetted with different amounts of water; e1 – two coats of adhesive systems,
brushed for 10 s each; e2 – one adhesive coat kept for 20 s, brushed for 10 s; f1 – air dry for 10 s at 20 cm; f2 – air dry for 20 s at 5 cm; g1 – light cure
(10 s, 600 mW/cm2); g2- light cure (20 s, 600 mW/cm2)

Fig 1 Experimental design.

manufacturers using a VIP light unit with a light in-
tensity of 600 mW/cm2 (Bisco, Schaumburg, IL,
USA). The time elapsed between rewetting and ad-
hesive application was approximately 10 s, which
was the time required to open the bottles, pour the
adhesive on the microbrush, and take it to the tooth
surface. Resin composite build-up “crowns” (Z 250,
3M ESPE) were constructed on the bonded surfaces
in increments of 1 mm that were each light activat-
ed for 30 s using the same light unit and light inten-
sity. All the bonding procedures were carried out by
a single operator at room temperature (24°C) and
50% relative humidity.2
After storage in distilled water at 37ºC for 24 h,
the specimens were longitudinally sectioned in
both “x” and “y” directions across the bonded inter-
face with a diamond saw in a Labcut 1010 machine
(Extec, Enfield, CT, USA), to obtain a total of 30
bonded sticks per tooth, each with a cross-section-
al area of approximately 0.8 mm2.
The number of prematurely debonded sticks (D)
per tooth during specimen preparation was record-

Vol 5, No 3, 2003 185

Reis et al
ed. Specimens originated from the areas immedi-
ately above the pulp chamber, and their remaining
dentin thickness (RDT) was measured with digital
calipers and recorded (Absolute Digimatic, Mitu-
toyo, Tokyo, Japan). The cross-sectional area of
each stick was measured with the digital calipers to
the nearest 0.01 mm and recorded for the calcula-
tion of the bond strength.
The sticks were individually attached to a modi-
fied caliper for microtensile testing4 with cyanoacry-
late resin (Zapit, Dental Ventures of North America,
Corona, CA, USA) and subjected to a tensile force
in a universal testing machine (Kratos Dina-
mometros, São Paulo, SP, Brazil) at a crosshead
speed of 0.5 mm/min.
The bond failure modes were evaluated at 400X
under a light microscope (HMV-2, Shimadzu, Tokyo,
Japan) and classified as cohesive (failure exclu-
sively within dentin or resin composite, C) and ad-
hesive or mixed (failure at resin/dentin interface or
mixed with cohesive failure of the neighboring sub-
strates, A/M).
Data Treatment
For each tooth, a bond strength index was calculat-
ed assuming the relative contribution of the possi-
ble mode of failures, according to the following for-
mula (values in MPa):
Bond strength index:
I t = ( BA/M × % A/M ) + ( C D × % D ) + ( C R × % R ) + ( B D × % D )
Where:
BA/M is the average bond strength of sticks with
adhesive/mixed fracture pattern;
%A/M is the percentage of sticks with adhe-
sive/mixed fracture pattern;
CD is the cohesive strength of dentin;
%D is the percentage of sticks that failed cohe-
sively in dentin;
CR is the cohesive strength of resin;
%R is the percentage of sticks that failed cohe-
sively in resin;
BD is the bond strength attributed to sticks that
spontaneously debonded during preparation
(4 MPa);
%D is the percentage of sticks debonded during
preparation.
186
The formula assumes the cohesive strength of
the resin composite (CR) as the average value of all
specimens (from a single tooth) that failed in that
manner. The cohesive strength of dentin (CD) was
calculated similarly. In this particular study, no co-
hesive failures were observed in the resin compos-
ite; therefore, this value was zero in the formula.
The value attributed to specimens that failed pre-
maturely during preparation and could not be test-
ed was 4 MPa. This value is arbitrary and corre-
sponds to approximately half of the minimum bond
strength value that could be measured in this study
(ca 7.5 MPa).23 A bond strength index was calculat-
ed for each of the five teeth used per group. These
were averaged to express the mean bond strength
index for every material at each degree of moisture.
A two-way ANOVA (material vs moisture degree)
and Tukey’s multiple test were used to compare the
microtensile bond strength indexes.20 Regression
analysis was applied to identify the best moisture
range for each material. The level of confidence
was established at α = 5%.
RESULTS
The remaining dentin thickness (RDT) for all speci-
mens ranged from 2.3 to 2.7 mm, indicating that
the interfaces were located in medium dentin.40 A
regression analysis demonstrated that there was
no influence of RDT on the bond strength (p > 0.05,
not shown). The mean cross-sectional area ranged
from 0.78 to 0.82 mm2 and no difference among
the treatment groups was detected (p > 0.05).
The average strength of all specimens that failed
cohesively in dentin was 68.1 MPa (68.1 ± 13.1, n
= 26). The percentage of sticks that failed prema-
turely during specimen preparation and the fre-
quency of each fracture pattern in each group are
shown in Table 2.
The means and standard deviations of the bond
strength indices are shown in Table 3. Highly signif-
icant main effects and interaction (p < 0.0001)
were detected. Regression analysis revealed a qua-
dratic significant relationship between the mean
bond strength index and the amount of water on
dentin surface (R2 = 0.95, p < 0.001). The estimat-
ed curves are shown in Fig 2.
The moisture degree range in which the maxi-
mum bond strength index was observed was differ-
ent among the materials. Table 4 shows the esti-
mated maximum bond strength indices and the es-
The Journal of Adhesive Dentistry
 Reis et al

Table 2 Percentage of specimens (%) according to the fracture pat-

tern* or premature debonding (D) for each experimental condition

Adhesive systems
Moisture SB OS SC
(µl) A/M C D A/M C D A/M C D

0 92 0 8 74.6 0 25.4 84 0 16
1.5 90 4.6 5.4 66.6 5.4 28 88 0 12
2.5 82 0 18 74.6 1.4 24 93.4 0.6 6
3.5 69.4 0 30.6 83.4 4.6 12 68.7 0.6 30.7
4.0 79.4 0 20.6 76.6 0 23.4 58 0 42
4.5 44 0 56 0 0 100 55.4 0 44.6

* A/M = adhesive or mixed failure; C = cohesive failure in dentin (no resin cohesive fracture pattern
was observed).

Table 3 Mean, standard deviation (MPa) and statistical significance

of bond strength indexes at each moisture degree (*)

Adhesive systems
Moisture (µl) SB OS SC

0 26.1 ± 1.1 b, c 18.0 ± 1.9 c 24.0 ± 3.6 b, c

1.5 42.2 ± 6.7 a 33.8 ± 6.1 b 27.7 ± 3.9 b
2.5 32.6 ± 1.5 b 31.9 ± 2.2 b 25.9 ± 3.4 b, c
3.5 19.8 ± 1.6 b, c 40.1 ± 4.6 a, b 21.4 ± 1.9 b, c
4.0 21.3 ± 1.2 b, c 31.4 ± 6.1 b 12.5 ± 2.6 c
4.5 10.6 ± 3.7 c, d 4.0 ± 0.0 c, d 10.4 ± 2.5 c, d

(*) Same superscript letters indicate no statistically significant difference (p > 0.05).

Fig 2 Estimated curves of bond strength

indices versus water volume for each adhe-
sive system.

Vol 5, No 3, 2003 187

Reis et al
Table 4 Estimated maximum bond strength and respective moisture
content [confidence interval] for each adhesive system
Parameter SB
Maximum bond
37.3 [33.9; 40.7]
strength (MPa)
Moisture content (µl) 1.7 [1.4; 1.9]
timated respective moisture degree as well as the
confidence intervals for all the adhesives.
Table 3 shows that SB had a maximum bond
strength of 42.2 ± 6.7 MPa that was statistically
similar (p = 0.4996) to the maximum bond strength
of OS (40.1 ± 4.6 MPa), although the degrees of
moisture differed (ca 1.5 µl for SB and 3.5 µl for
OS). SC showed its maximum bond strength index
(27.7 ± 4.0 MPa) at the same moisture degree as
SB (ca 1.5 µl); however, it was significantly lower
(p < 0.0001) than the maximum bond strength in-
dices obtained by the other systems at that mois-
ture degree.
SB presented its highest bond strength index at
1.5 µl of moisture, and that was significantly higher
than the bond strength index obtained at any other
degree of moisture (p < 0.05), indicating that max-
imum bond strength with this material could only be
obtained in this limited range of moisture. Con-
versely, OS achieved its maximum bond strength in-
dex at 3.5 µl of moisture, but this value was not
statistically different (p > 0.05) from the values ob-
tained in the range of 1.5 µl to 4.0 µl of moisture.
Similarly, the highest bond strength indices ob-
tained with SC were not different (p > 0.05) within
the range of 0 µl to 3.5 µl. This indicates that OS
and SC have a broader range of moisture within
which maximum bond strengths can be achieved.
DISCUSSION
Conventional shear or tensile bond strength test
studies usually report sample sizes of 8 to 12
teeth for each experimental condition, while most
microtensile studies use 2 to 4 teeth in each
group.12,19,27,32,40 Although this may be consid-
ered an advantage of the microtensile over conven-
188
Adhesive systems
OS SC
39.1 [35.6; 42.6] 28.1 [24.7; 31.4]
2.2 [2.1; 2.3] 1.4 [0.9; 2.0]
tional tests, care must be taken when interpreting
each “stick” as an experimental unit. According to
Neter et al,20 an experimental unit is the smallest
subunit of the experiment in which two different
treatments can be applied. When microtensile is
the test of choice, the several bonded sticks origi-
nating from one single tooth usually received the
same treatment; therefore, they cannot be consid-
ered separate experimental units. It is therefore ad-
visable to use a minimum of four teeth per experi-
mental group to satisfy statistical requirements.25
In a preliminary phase of this study, the average
bond strengths were calculated based on the spec-
imens that failed exclusively in an adhesive or
mixed mode. Specimens that failed prematurely
during preparation were disregarded in the analy-
sis, as is usually done in most of the microtensile
studies. However, such an approach was unable to
distinguish differences in the performance of SB
and OS under drier conditions, since it did not take
into account the frequency of prematurely debond-
ed specimens and the frequency of cohesive frac-
tures within the substrates (Table 2), which were
different for SB and OS.30 Undoubtedly, a high inci-
dence of debonded specimens during preparation
suggests a greater fragility of the bonding. Howev-
er, if debonded specimens are ignored in the calcu-
lation and the average bond strength is calculated
solely based on the specimens that survived the
preparation, the performance of that system may
be misleading. Conversely, a high incidence of co-
hesive failures within the substrates may indicate
that the adhesive interface was stronger than the
calculated average bond strength, although it does
not mean that the resin-dentin bonds are uniformly
higher than the intrinsic strength of the substrates.
To overcome such interpretation drawbacks of
the method, this study recommends the use of a
The Journal of Adhesive Dentistry

bond strength index formula that considers the rel-
ative contribution of all types of bond failures to
create a bond strength index for each individual
tooth employed in microtensile studies. The final
bond strength index for each experimental variable
is then calculated as an average of all the teeth
used in that particular experimental group. In every
study, the cohesive strength of the substrates ob-
tained in each tooth is used in the formula. This
permits such constants to be adjusted to any spe-
cific experiment, depending on the type of resin
composite used and the respective cross-sectional
area of the specimens, since the apparent
“strength” of the specimens will vary according to
the cross-sectional area.31
The constant value assigned for the prematurely
debonded specimens is somewhat arbitrary. Bouil-
laguet et al5 showed that most specimens that
debonded during preparation could have had bond
strengths as high as 13 MPa. Pashley et al23 re-
ported that values as low as 4 MPa could not be
measured using microtensile tests. Theoretically,
specimens that debonded before being actually
tested could present an estimated “bond strength”
value that would be somewhere in the range be-
tween zero and the minimum bond strength value
that was measured in that specific study. In the
present study, no values lower than 7.5 MPa were
obtained, so we arbitrarily assigned a value of
4 MPa for all specimens that failed during prepara-
tion (approximately half of the minimum tested val-
ue).
Another approach is to include prematurely de-
bonded specimens in the calculation of the average
bond strength by assigning them an MPa value of 0
(zero).38 Although this increases the standard devi-
ation of the group, it also reflects the sensitivity of
that specific group to the experimental design. Re-
gardless of the approach used in the data treat-
ment, researchers should always report that infor-
mation to avoid misinterpretation of their data.
Our data suggest that when demineralized den-
tin is dehydrated by air, a certain amount of water,
albeit different for each adhesive, is required to re-
wet the surface in order to optimize bond strengths.
Several studies have already reported that a moist
dentin surface is essential to allow resin infiltration
with current adhesives.11,16,19,28 When water is
present within the collagen interfibrillary and in-
trafibrillary spaces, it maximizes the expansion of
the demineralized matrix.21 If demineralized dentin
is severely air dried, most of the water is removed
Vol 5, No 3, 2003
Reis et al
and causes shrinkage of the matrix,8 thus reducing
its permeability for resins22 and ultimately compro-
mising the bond.
Full expansion of a thick layer (ca 200 µm) of
demineralized dentin matrix does require some
time to occur.24 However, a very thin layer (ca 3 to
5 µm) re-expands quite rapidly and an extra water
rewetting time is not required, apart from the time
necessary for pouring the adhesive on the micro-
brush.
The three adhesive systems used in this study
were chosen based on their different solvent con-
stituent. Single Bond contains ethanol and water,
Syntac Single Component contains only water, and
One-Step is an acetone (water-free) based system.
It has been previously demonstrated that bond
strengths of adhesives to dentin are related to their
solvent type15 and, more specifically, to the ability
of the solvent to re-expand and maintain the inter-
fibrillary spaces within the demineralized dentin
matrix.6,21,24 When dentin was air dried for 30 s, it
is likely that water filling the interfibrillary spaces
had been removed, allowing the fibrils to touch one
another and causing the collapse of the matrix.21
In this situation, both water-based adhesives pro-
vided significantly higher bond strengths than the
water-free adhesive. Additionally, the number of
specimens lost during preparation was relatively
higher for the acetone-based system.
When dentin is air dried and collapsed, collagen
fibrils touch and form hydrogen bonds (H-bonds) to
one another. This results in a shrunken and stiff-
ened matrix18 with very little permeability to adhe-
sive resins,22 and also increases the hydrophobic
features of demineralized dentin; this phenomenon
is highly dependent upon the drying time.13 To re-
create the interfibrillary spaces for resin infiltration,
the monomer/solvent combination of the adhesive
must be able to break such interpeptide H-bonds
and permit the matrix to re-expand.24 Several sol-
vents and monomers have been ranked according
to their ability to re-expand dried, shrunken, de-
mineralized dentin. According to Pashley et al,24
only solvents with a solubility parameter for hydro-
gen bonding (δh) higher than 19.0 [(J/cm3)1/2] are
capable of breaking the interpeptide H-bonds and
re-expanding the matrix. Water has a δh of 37.3
(Hansen’s solubility parameter3), while acetone has
a δh of only 7.0.3 The presence of water in the SB
and SC adhesives probably resulted in a mixture
with a δh higher than 19.0 that allowed partial ex-
pansion of the collapsed matrix, thus resulting in
189
Reis et al
better resin infiltration and improved bond strength.
The same phenomenon did not occur with OS be-
cause of its much lower δh due to the presence of
acetone and absence of water. This self-expanding
ability has been demonstrated to occur only with wa-
ter-based systems.39
Within the limits of the over-dry and over-wet
range of this study, it is clear that all three adhe-
sives presented much lower bond strengths at the
excess water condition (> 4.0 µl of water, Fig 2).
Under over-wet conditions, acetone-based systems
undergo phase separation of the hydrophobic and
hydrophilic moieties, resulting in blister and globule
formation on the dentin surface that ultimately
compromises resin infiltration.36,37 Apparently,
such blisters do not form when water-based adhe-
sives are used under over-wet conditions; however,
there is evidence that excess water dilutes the res-
in monomers and compromises the hybrid layer for-
mation.35
The degree of re-expansion of demineralized, dry
dentin is proportional to the water content of the ad-
hesive/primer.21 Although SB contains water, its
highest bond strength was obtained when dentin
was previously rewetted with 1.5 µl of water
(Table 3). Perhaps the 3% to 8% water content of this
material28 is not enough to permit optimal re-expan-
sion when directly applied to a dry dentin surface,
thus requiring previous moisture on the surface for
improved bond strength. Additional amounts of wa-
ter, however, resulted in a gradual, significant de-
crease in bond strength of SB. It is probable that the
slight addition of surface water (from 1.5 to 2.5 µl)
was sufficient to cause monomer dilution and com-
promise the bonding. Moreover, residual water after
solvent evaporation may have also compromised
the polymerization of the resin. It has been demon-
strated that an addition of approximately 20 µl of
water reduces the conversion degree of a water-free
bonding resin from 53.5% to about 25%.15
As water evaporates from the surface, monomer
concentration rises rapidly within the demineralized
collagen network. This decreases the ability of wa-
ter to evaporate and results in residual water en-
trapped in the matrix. The presence of solvents
with higher vapor pressure in the adhesives facili-
tates the evaporation of this residual water. This
probably explains why SB resulted in higher bond
strengths than SC under the same surface water
content (Table 3).
SB contains ethanol while SC uses only water as
a solvent. Presumably, the same phenomenon oc-
190
curred when OS was applied to a previously rewet-
ted surface. However, OS contains acetone and be-
cause of its much higher vapor pressure relative to
water (ca 200 mmHg and 47.1 mmHg, respective-
ly), it may have allowed less water to remain.26 Only
when dentin was rewetted with amounts higher
than 4.0 µl of water did the bond strengths of OS
decrease significantly. Abate et al1 have shown that
water-based systems present a much lower evapo-
ration rate than acetone-based systems. Kanca16
demonstrated that primers based on a HEMA/ace-
tone mixture resulted in the highest bond strength,
followed by HEMA/ethanol and HEMA/water mix-
tures when applied to moist dentin.
It is generally accepted that water-based sys-
tems are less sensitive to surface moisture than
acetone-based systems.14,29 However, considering
the moisture range in which the highest bond
strength was obtained by each adhesive system
tested here, we cannot confirm this. OS presented
statistically similar highest bond strengths from 1.5
to 4.0 µl of water. Although lower than the other two
adhesives, SC presented highest bond strengths
between 0 and 3.5 µl. The significantly highest
bond strength of SB was obtained at only 1.5 µl of
water. This indicates that SB was the most sensitive
material to surface moisture in this study. Swift and
Bayne33 concluded that the degree of moisture had
little influence on the bond strength of SB. Contrary
to this study, most of the reports on the influence
of surface moisture on bond strength have relied on
the subjective assessment of moisture degree on
dentin surface. The lack of controlled measurement
of the amount of water used to rewet the surface
may lead researchers to interpret their findings
based on a moisture spectrum in which no differ-
ences in bond strength can be realized. For in-
stance, if we compare the bond strengths of SB at
0, 2.5, 3.5, and 4.0 µl of water, no statistical differ-
ences are noted. We trust that our method may offer
a better opportunity to properly assess the amount
of water relative to the available surface area for ad-
hesion.
The results of this study are applicable to the
particular adhesive systems used here, and may
not be directly extrapolated to other water-based or
water-free systems. Differences such as monomer
composition, solvent or water content, initiators,
etc, may implicate different sensitivity to surface
moisture. It is interesting to note that the bond
strengths of the three adhesives to air-dried dentin
were not negligible, even for the water-free system
The Journal of Adhesive Dentistry

(OS). This indicates that the critical amount of wa-
ter necessary to provide spaces for resin infiltration
may be much less than previously thought. Addi-
tionally, solvents other than water, eg, ethanol and
methanol, are capable of re-expanding demineral-
ized shrunken dentin.21,24 Perhaps future adhe-
sives may consider the use of such solvents in-
stead of water in order to re-expand air-dried den-
tin. This would allow the use of more hydrophobic
adhesive agents, thereby rendering them less sus-
ceptible to water degradation over time.34
ACKNOWLEDGMENTS
This study was supported, in part, by CAPES; CNPq 300086/
01-6, 300481/95-0; FAPESP 99/05124-0, 99/10611-8. We
would like to thank Prof. Rafael Yagüe Ballester for his expert
advice regarding the bond strength index and also Marcela
Rocha de Oliveira Carrilho for the help provided.
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