Dental Materials Journal 2015; 34(1): 1–6

Effect of agitation and storage temperature on water sorption and solubility of

adhesive systems
Saryta ARGOLO1, Paula MATHIAS2, Thaiane AGUIAR3, Adriano LIMA4, Sara SANTOS5, Richard FOXTON6
and Andrea CAVALCANTI7

1
Dentistry Course, Northeast Independent School (FAINOR), Vitoria da Conquista, BA, Brazil
2
School of Dentistry, Federal University of Bahia (FOUFBA), Salvador, BA, Brazil
3
Department of Restorative Dentistry, College of Dentistry, University of Illinois at Chicago, Chicago, IL, USA
4
Department of Restorative Dentistry, State University of Campinas (UNICAMP), Piracicaba, SP, Brazil
5
Private practice, Salvador, BA, Brazil
6
Department of Conservative Dentistry, Kings College London Dental Institute, London, UK
7
Dentistry Course, School of Medicine and Public Health of Bahia (BAHIANA) and School of Dentistry, Federal University of Bahia (FOUFBA),
Salvador, BA, Brazil
Corresponding author, Saryta ARGOLO; E-mail: saryta_argolo@hotmail.com

The purpose of this study was to evaluate the influence of storage temperature and flask agitation on the water sorption (WS) and
solubility (SL) of simplified adhesive systems. Seventy-two disc-shaped specimens were prepared according to the adhesive system
(water/ethanol-based: Adper Single Bond 2; and water-based: One Coat Bond SL) and experimental conditions tested (mechanical
agitation and storage temperature). Statistical analysis (3-way ANOVA, alpha=5%) found significantly greater WS and SL means
for the water/ethanol-based system when compared to the water-based. Irrespective of factors studied, significant differences in WS
and SL were noted between cold and room temperatures, with greater values been obtained at 1°C, and lower ones at 20°C. Agitation
provided increased WS for both materials at all temperatures, but did not affect their SL. The mechanical agitation of the flask may
negatively affect the dynamics of diffusion of simplified adhesive systems, even at extremely cold or warm temperatures.

Keywords: Adhesive systems, Longevity, Sorption, Solubility, Temperature

hydrophilic monomers, and in the displacement of water

INTRODUCTION
Improvements in the performance of polymeric
dental materials has demonstrated important clinical
advancements, enabling more conservative preparations
and better esthetic outcomes1,2). To achieve long-term
success, it is essential to use a safe and durable technique
when bonding to dental tissues. Contemporary adhesive
systems presents different bonding mechanisms to tooth
structure; while the etch and rinse systems act after
etching substrates with phosphoric acid; the self-etching
systems simultaneously etch and diffuse through
enamel or dentin1). Both the etch and rinse and the self-
etching agents have simplified versions, with a lower
number of steps.
Simplifying the adhesive technique may negatively
affect the durability of the adhesive bond due to the
complexity of the adhesive systems3). Simplified etch
and rinse adhesive systems are composed of a mixture
of hydrophilic and hydrophobic monomers, solvents,
stabilizers, initiators and filler particles2). Increasing
the concentration of hydrophilic monomers allows
these systems to infiltrate and diffuse into the collagen
network, forming a hybrid layer3-8). Hydrophilic systems
have an affinity for water, which enables permeation
through dentin but may also promote the formation of a
polymeric structure more susceptible to hydrolysis4,9).
The solvents included in the composition of adhesive
systems act in the dissolution of hydrophobic and
from the acid etched surfaces, ensuring proper monomer
infiltration into the porosities of enamel and dentin8).
The commonly used solvents in dental adhesives are
water, ethanol and acetone, which vary in accordance to
their polarity2). The quality of the hybridization process
is highly dependent on the optimal monomer infiltration
and on the removal of as much water and organic
solvents as possible from the surface prior to curing6).
The higher hydrophilicity and possible presence
of residual solvent in the simplified adhesive agents
means that care is needed to ensure the bonding layer
has optimum mechanical properties8). A frequent
recommendation is to store the adhesives at room
temperature since changes in temperature may
influence bonding10). The storage temperature can
modify the viscosity of the polymeric material,
increasing the penetration capacity, dissolution, time
of solvent evaporation and degree of conversion, which
might impact on the physical and mechanical properties
of the bonding agents11).
A continuous brushing or rubbing, or active
application of the adhesive system, is also an
alternative way of encouraging monomer diffusion and
solvent evaporation12). Active application may increase
agitation of the molecules, thereby allowing greater
evaporation of the solvent and consequently better
dispersion and diffusion of monomers through the
interface13). Nonetheless, the force applied during active

Received Mar 11, 2014: Accepted May 29, 2014

doi:10.4012/dmj.2014-033 JOI JST.JSTAGE/dmj/2014-033
2 Dent Mater J 2015; 34(1): 1–6

application may be relatively difficult to control and
standardize. Thus, operator variability is expected when
active rubbing of the adhesive system is being conducted.
Mechanically agitating the adhesive system bottle can
standardize any influence on the wetting ability of the
adhesive system, is free of operator variability and
regional characteristics of the cavities. However at
present, there is still no scientific evidence with respect
to the effectiveness of this method.
Because the durability of simplified systems is
directly related to their permeability, it is important to
investigate whether variations in storage temperature
and the mode of application may interfere with the
gain or loss of the material mass after water exposure.
Thus, the aim of this study was to investigate the
effect of agitation before application, and of the storage
temperature of the flask, on the water sorption and
solubility of simplified conventional adhesive systems.
The null hypotheses tested were that simplified
adhesive systems with different solvents can present
similar water sorption and solubility; agitation before
application of the adhesive system, and the temperature
of the flasks would interfere with the loss or gain of
mass.
MATERIALS AND METHODS
Specimen preparation and experimental groups
Two commercial etch and rinse adhesive systems with
distinct chemical compositions were used in this study
(Table 1). Both adhesives were categorized as simplified/
etch and rinse, but different types of solvents were
present in their composition: ethanol/water-based—
Adper Single Bond 2 (3M ESPE); water-based— One
Coat Bond SL (Coltène, Vigodent). Both adhesive
systems were evaluated in two different conditions: (1)
mechanical agitation or not and (2) storage temperature
(1°C, 20°C and 40°C) as illustrated in Fig. 1
Storage temperature of the adhesive system flask
The flasks containing the adhesives were stored
at experimental temperatures of 1°C (refrigerator
temperature), 20°C (room temperature) and 40°C
(oven temperature) for 1 h before their application14).
These temperatures were verified using a digital
thermometer (Omron CO. Inc., Dalian, China). To
avoid changes in the temperature of the flask during
specimen preparation, the bonding agent was stored in
the experimental temperature condition for 1 h and
then used again.
Mechanical agitation of the flask before application
In the case of the groups undergoing mechanical
agitation, before each adhesive system application, each
respective flask was agitated in a plaster vibrator (VH
Equipment Medicos Odontologicos Ltda, Araraquara,
SP, Brazil) at a constant speed of 60 Hz/40 W for 20 s.
Assessment of loss/gain of mass: Water sorption and
solubility
The water sorption and solubility test was based on the
International Organization for Standardization (ISO)
specifications n. 4049:2000 Dentistry –Polymer-based
filing, restorative and luting materials15). Seventy-two
disc-shaped specimens (6 per group) were prepared (8.0
mm diameter × 1.0 mm thick) using a silicone matrix
(Elite HD+, Zhermack, Badia Polesine, Italy) according
to the groups to which they belonged.
In order to prepare the specimen, three drops of
each adhesive were dispensed directly into the matrix

Table 1 Manufacturer, composition and lot number of adhesive systems used in this investigation

Adhesive system
Composition Lot number
(Manufacturer)

Ethanol; water; Bis-GMA; UDMA; silanized silica particles;

Adper Single Bond 2
HEMA; 1-glycerol; 3-dimethacrylate; copolymer of acrylic #1119200635
(3M ESPE; St Paul, MN, USA)
acid and itaconic acid.

Water; HEMA;hydroxypropyl methacrylate; glycerol

One Coat Bond SL
dimethacrylate; UDMA; polyalkenoate methacrylate; #0175579
(VIGODENT; Rio de Janeiro, Brazil)
photoinitiator and inhibitor.

Bis-GMA: bisphenol A glycidyl methacrylate; UDMA: di-urethane dimethacrylate; HEMA: 2-hydroxyethyl methacrylate

Fig. 1 Schematic presentation of experimental conditions (n = 6)

 Dent Mater J 2015; 34(1): 1–6 3

so that it was completely filled. All visible air bubbles
were carefully removed with the aid of a dental explorer
probe before light activation. Compressed air from a
3-in-1 syringe spray was used for 10 s at a distance of
20 cm to evaporate the solvent (40-psi air-pressure). A
polyester strip and a glass coverslip were placed on the
matrix and the surface was then light-activated for 60
s (Radii-Plus, SDI Limited, Australia), taking care that
the tip of the light curing unit covered the entire surface
of the specimen. The light output of the light curing unit
was 1,500 mW/cm2. Afterwards, the specimens were
carefully removed from the matrix and the opposing
surface was light-activated for additional 60 s16).
Immediately after polymerization, the specimens
were measured with a digital caliper with an accuracy
of 0.01 mm (Mitutoyo Sul Americana Ltda, Suzano,
SP, Brazil) in order to calculate the volume (V) of
each specimen (mm3). The specimens were stored
in a desiccator containing silica gel at 37°C for pre-
conditioning and repeatedly weighed at intervals of 24
h until a constant mass (M1) was obtained (variation of
less than 0.2 mg over a period of 24 h). The weighing
procedures were performed on an analytical balance
(Model AUW-220D, Shimadzu, Kyoto, Japan) with a
precision of one hundred-thousandth of a gram.
After mass stabilization, the specimens were
individually stored in 10 mL of distilled water for 7
days at 37ºC, in accordance to ISO specification. The
specimens were kept immersed in a vertical position
and water was not changed daily. Afterwards, the
specimens were washed under running water and
excess water was removed with absorbent paper (Celupa
Guaíba Industrial Pulp and Paper Ltd., Guaiba, RS,
Brazil). The specimens were weighed and the mass
was recorded (M2). After, specimens were dried as
previously described and weighed until a constant mass
was obtained (M3). The values of water sorption (WS)
and solubility (SL) were calculated in µg/mm3 using the
following formulas:
M2−M3 M1−M3
WS= SL=
V V
Where: M1 is the mass of the sample in μg before
immersion in distilled water, M2 is the mass of the
sample in μg after immersion in distilled water for 7
days, M3 is the mass of the sample in μg after being
reconditioned in a desiccator and V is the volume of the
sample (mm3)16).
Statistical analysis
Initially, an exploratory analysis was carried out to
verify the Analysis of Variance parameters (ANOVA).
Water sorption and solubility data were statistically
analyzed by three-way ANOVA, with main factors
adhesive system, agitation and temperature. All
possible statistical interactions were included in the
model; when interactions were considered as non-
significant, main factors were analyzed separately.
Multiple pairwise comparisons were done with the
Tukey post-hoc test (SAS program, version 9.1, at a level
of significance of 5%). Tables 2 and 3, show the means
and standard deviations for the water sorption and
solubility data, respectively.
RESULTS
In accordance with the statistical analysis, none
interaction between the main factors was considered as
significant, neither for water sorption nor for solubility
data (p>0.05). For this reason, each main factor (adhesive
system, agitation and temperature) was analyzed
separately.
The analysis of water sorption data indicated that
irrespective of the type of adhesive system and flask
agitation, significant differences existed between the
cold and room temperatures, with greater values
obtained at 1oC, and lower ones at 20oC (p=0.04). At
40°C, the results showed intermediate values,

Table 2 Mean values (standard deviation) of water sorption (μg/mm3) of the adhesive systems according to the agitation
mode and temperature

Agitation
Temperature Adhesive System
Absent Present

Adper Single Bond 2 247.29 (18.10) a 263.06 (25.75) a

Room (20°C) B
One Coat Bond SL 141.05 (11.95) b 155.51 (14.23) b

Adper Single Bond 2 263.80 (10.83) a 269.86 (13.41) a

Cold (1°C) A
One Coat Bond SL 158.41 (15.07) b 164.78 (6.26) b

Adper Single Bond 2 259.34 (18.84) a 262.10 (6.53) a

Warm (40°C) AB
One Coat Bond SL 154.33 (12.77) b 156.85 (14.00) b

* #

Different letters and symbols represent the means with statistical significance (3-way ANOVA, alpha=5%). Different symbols
compare the levels of agitation within adhesive system/temperature; capital letters compare the levels of temperature within
agitation/adhesive system. Lower case letters compare adhesive systems, irrespective of the temperature or agitation.
4 Dent Mater J 2015; 34(1): 1–6
Table 3 Mean values (standard deviation) of solubility (μg/mm3) of the adhesive systems according to the agitation mode
and temperature
Temperature Adhesive System
Adper Single Bond 2
Room (20°C)
One Coat Bond SL
Adper Single Bond 2
Cold (1°C)
One Coat Bond SL
Adper Single Bond 2
Warm (40°C)
One Coat Bond SL
Different letters represent the means with statistical significance (3-way ANOVA, alpha=5%). Capital letters compare the
levels of temperature within agitation/adhesive system. Lower case letters compare adhesive systems, irrespective of the
temperature or agitation. No significant difference between the levels of agitation was noted.
statistically similar to those at the other temperatures.
In addition, agitation resulted in increased water
sorption for both adhesive systems at all temperatures
tested (p=0.04). Finally, the water-based adhesive
system resulted in statistically lower water sorption
when compared to the water/ethanol-based agent, at all
conditions tested (p<0.001) (Table 2).
Solubility data analysis showed similar statistical
significance among temperatures, with greater means
found at 1oC and lower at 20oC (p=0.04). Between
adhesive systems, higher solubility was exhibited by
the water/ethanol-based agent (p<0.001). Nevertheless,
mechanical agitation did not provide any statistically
significant differences among the solubility data of the
groups (p=0.08) (Table 3).
DISCUSSION
The advent of adhesive systems has promoted
meaningful changes in restorative procedures,
since current bonding agents exhibit better clinical
performance10). However, regarding the simplified
bonding systems, long-term adhesive stability is still a
major challenge. One of the reasons for early adhesive
degradation might be the increased presence of
hydrophilic monomers. Their low molecular weight in
the adhesive makes their matrices highly permeable17,18).
This greater hydrophilicity may allow external water
sorption from the oral environment when exposed to both
salivary fluids and internal sorption from the subjacent
hydrated dentin5,18).
Water sorption and solubility have a significant
impact on the clinical behavior of polymeric materials4),
since exposure to water can result in irreversible
changes such as cracks, fissures and hydrolytic
degradation of the chemical components of the resin
matrix5). As a result, the early and long-term bond
strengths of the adhesive systems to the dentin
substrate may be affected18,19).
Resin-based materials may absorb water to varying
degrees and this mechanism may be related to the
Agitation
Absent Present
80.99 (6.39) a 78.62 (7.41) a
B
11.68 (0.89) b 12.49 (1.90) b
79.13 (6.24) a 85.98 (3.13) a
A
11.16 (2.02) b 13.20 (2.08) b
77.92 (6.66) a 82.63 (6.48) a
AB
11.16 (1.15) b 11.25 (1.5) b
molecular and microstructure aspect of the polymer19).
Among the molecular characteristics, the pendant
hydroxyl groups are capable of forming hydrogen bonds
with water. In addition, the ionic and hydrophilic
resin monomers facilitate ionic movement within the
polymerized resin matrix in the presence of residual
water, which approaches the molecules to the structure
by a process of attraction19). Porosity and density of
polymer bonds are among the microstructural aspects5).
Therefore, the quality of the polymer network formed
determines the extension of degradation that the aqueous
environment can cause the resin matrix to undergo4).
Solvent retention within adhesive layers may also
be a reason for adhesive degradation. In previous
studies, authors have agreed that water sorption may
vary among adhesive systems and is highly dependent
on the composition of each material20,21). Interestingly,
Nihi et al.22) assessed the spontaneously evaporation
of different commercial adhesive systems and found
lower solvent evaporation capacity of ethanol-, water-
and ethanol/water-based adhesives when compared to
acetone-based agents. In addition, Yiu et al.23) evaluated
the water retention in comonomer blends after
evaporation, and demonstrated that the addition of
water to comonomer-ethanol mixture led to increased
retention since both water and ethanol solvents can form
hydrogen bond to the monomers. In this investigation,
the ethanol/water-based adhesive system (Adper Single
Bond 2) showed higher water sorption and solubility
values when compared to the water-based agent (One
Coat Bond SL) regardless of the temperature and
agitation mode. Despite differences in their monomer
content, it seems that the solvent mixture may affect the
solvent evaporation, which may impair the mass loss22)
and accelerate the hydrolytic degradation23). Therefore,
it was denied the hypothesis that simplified systems
with different solvents could behave similarly.
It is known that the rate of evaporation of any
substance is determined by its vapor pressure2),
but also, the extent of solvent retention in polymer
networks depends on resin polarity24). In view of the
 Dent Mater J 2015; 34(1): 1–6
results of this study, it is possible to suggest that in
the presence of a thick layer of adhesive system, as the
one necessary for a specimen tested in water sorption
and solubility, 10 s of air drying to evaporate the solvent
was not sufficient to remove it completely. Thus, the
presence of residual water may have impaired polymer
cross-linking by the plasticizing process, creating
spaces for greater water penetration through the
structures19,25). However, it must be considered that
one of the experimental hypotheses of this work was to
verify if temperature and agitation could induce greater
or less solvent retention in adhesive films. Thus, the
total absence of solvents would not allow such
assumptions.
The monomer composition of the adhesive systems
is also a determining factor in bond strength durability.
In this investigation, both materials tested belong
to the group of urethane dimethacrylate materials.
According to Dhanpal et al.5), under normal conditions
of polymerization, urethane is known to form weaker
hydrogen bonds with water molecules than the hydroxyl
group in Bis-GMA, which is reflected by the lower
cohesive energy density of the urethane group (1,425
J/cm3) in comparison with the hydroxyl group (2,980
J/cm3) in Bis-GMA. Due to the lower energy needed in
the urethane group, the links of hydrogen bridges are
established more easily, which favors a greater gain of
water, and in turn, the loss of these water molecules also
occurs in a simpler way. Although this is uncertain, since
each respective manufacturer does not reveal the exact
chemical composition of each material, the presence of a
higher amount of UDMA in the composition of the water/
ethanol-based adhesive system could possibly justify a
higher gain and loss of mass when compared with the
other adhesive system.
Phase separation between the hydrophobic and
hydrophilic parts of the resin matrix might lead to
greater porosity within the adhesive layer and also
contribute to an increase in water sorption26,27). Using
a ternary phase diagram, Ye et al.28) observed that the
monomer content (BisGMA and HEMA) in the aqueous
phase decreased with the increase of water in the
mixture and, the resin phase became more hydrophobic
with increasing the water amount. Thus, the presence
of water as observed in both Adper Single Bond 2 and
One Coat Bond SL adhesive systems may lead to resin
phase separation. In addition, some studies indicated
that the hydrophilic portion of most simplified adhesive
systems (i.e. 2-hydroxyethyl methacrylate, HEMA) could
dramatically reduce the evaporation of residual water5,6).
Nonetheless, again, both systems tested in the present
investigation use an unknown proportion of HEMA on
their composition.
There are reports with respect to the effect
changing the fluidity of the bonding agent, since the
lower the viscosity of the polymeric material, the
greater the evaporation of the solvent and consequently,
improvement in mechanical properties13,29). In this
investigation, mechanical agitation of the adhesive
flask using a plaster vibrator was used to provide a
5
standardized molecular change on the adhesive layer,
in an attempt to facilitate solvent evaporation. It was
hypothesized that this method would allow an increase
in the molecule agitation by changing the fluidity of the
bonding agent.
In this study, agitation revealed a significant
increase in water sorption for both adhesive systems.
These findings suggest that shaking the flask of the
adhesive system probably enabled the incorporation of
air into the adhesive mixture, which resulted in the
inclusion of non-visible air bubbles in the specimen,
allowing higher uptake when stored in water. Another
possibility for this greater gain of mass after agitation
could be due to the increase in molecular kinetics
caused by shaking the flask, resulting in larger links of
hydrogen bridges with water, thus attracting molecules
to the adhesive matrix13). However, considering that
agitation has not influenced the solubility of both
adhesive systems, one can speculate that such air
incorporation does not have a significant effect on the
formation of the resin matrix, thus it cannot directly
influence the loss of mass.
With regard to temperature, an increase in the
storage temperature of the adhesive bottles resulted
in intermediate values, statistically similar to those
observed at room and cold temperatures. Conversely,
Loguercio et al. 30) assessed the effect of temperature on
the adhesive and concluded that using ethanol/water-
based adhesive systems at 37°C or 50°C and an acetone-
based at 37°C could improve the performance of the
bonding agent. Moreover, the temperature has practical
relevance in the kinetics of the light polymerization
reaction since, with an increase in temperature,
there is greater molecular mobility due to the lower
viscosity19,25,31).
Irrespective of the type of the adhesive system and
previous agitation, lower water sorption and solubility
values were found at room temperature, compared to
those observed at a cold temperature. It is possible that
a reduction in temperature made the adhesive systems
more viscous and hence may have hindered evaporation
of the solvent. As a consequence, the residual solvent may
facilitate the higher gain and loss of mass when stored
in water. Similarly, Alexandre et al.10) tested the effects
of adhesive systems applied at different temperatures
on bond strength to enamel and, concluded that their
use at room temperature (20°C) promoted stronger
links in the bond formed. Although storing adhesive
systems in the refrigerator seems to provide benefits
with respect to material conservation10), at the time of
applying the bonding agent to the substrate, it must be
at the room temperature, since in this storage condition
adhesive systems underwent less loss and gain of mass.
Nevertheless, further studies are needed since there
is still insufficient information about the behavior of
adhesive materials with different fluidity. In addition,
this characteristic may determine the molecular kinetics
of the adhesive layer and therefore lead to a different
clinical performance over the course of time.
6 Dent Mater J 2015; 34(1): 1–6
CONCLUSIONS
Within the limitations of the present study, it was
possible to conclude that:
• Changes in the water sorption and solubility
between the adhesive systems seems to be directly
related to the composition of each material;
• Mechanical agitation of the flask had a negative
effect on the water sorption of the simplified
water/ethanol-based and water-based adhesives
systems evaluated;
• The use of bonding agents at room temperature
resulted in lower loss and gain of mass and this
clinical approach should be widely disseminated.
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