RESEARCH AND EDUCATION

Resin-based luting agents and color stability of bonded

ceramic veneers
Júlia R. Almeida, DDS,a Gabriela U. Schmitt, DDS,b Marina R. Kaizer, DDS, MS,c Noéli Boscato, DDS, MS, PhD,d
and Rafael R. Moraes, DDS, MS, PhDe

Ceramic veneers present high ABSTRACT

clinical success rates, showing Statement of problem. The type of resin-based luting agent might influence the color stability of
up to 93.5% clinical survival ceramic veneers.
over a period of 10 years.1,2
Purpose. The purpose of this study was to investigate the effects of resin-based agents and aging
Feldspathic ceramic is the re-
on the color stability of ceramic veneers bonded to enamel.
storative material that is most
often used for veneers3 because Material and methods. Ceramic disks were cemented to bovine enamel disks with 4 resin-based
of its excellent optical proper- luting agents (n=10): dual-polymerizing cement (RelyX ARC), light-polymerizing cement (RelyX
4 Veneer), flowable composite resin (Filtek Z350 Flow), or composite resin preheated for 30 minutes
ties and its ability to be acid
at 60
C (Filtek Z350 XT). CIE L*, a*, and b* color coordinates were measured 24 hours after
etched,5 thus allowing adhesive cementation (baseline) with a color spectrophotometer and reevaluated after 10 000 and 20 000
cementation to tooth structure.6 thermal cycles. Color variation was calculated by using CIELab (DE*ab) and CIEDE2000 (DE00)
Because they are less expensive methods. Then 95% confidence intervals were calculated for color variation means between
than resin-based cements and baseline and 10 000 thermal cycles and between 10 000 and 20 000 thermal cycles. The 95%
to maximize the range of shades confidence intervals were also calculated for the means of individual color coordinates (L*, a*, and b*).
available, flowable and pre- Results. The dual-polymerizing cement had the highest color variation among all luting agents. No
heated composite resins may be significant differences were found in color variation among the light-polymerizing materials. All
used to cement ceramic veneers, agents showed DE*ab>3.46 and DE00>2.25 after 20 000 thermal cycles. Variations in L*, a*, and b*
provided they achieve proper coordinates were material dependent. The dual-polymerizing agent was yellowish and reddish
after aging.
fluidity and flowability for ce-
mentation. Resin-based luting Conclusions. The dual-polymerizing cement had higher color variation than the light-polymerized
agents possess esthetic char- materials when used for bonding ceramic veneers to enamel. Flowable and preheated composite
acteristics that favor a natural- resins had similar color stability to that of light-polymerizing resin-based cement. (J Prosthet Dent
2015;114:272-277)
looking cemented ceramic
veneer. In addition, adhesive
cementation can strengthen the fragile ceramic veneer.7-9 with extrinsic staining agents. Dual-polymerizing resin-
However, resin-based materials may vary in color based cements usually possess poorer color stability than
during aging,10-13 affecting the esthetic results of ceramic light-polymerizing resin-based cements and therefore
veneers. Polymer discoloration is usually associated with are usually not indicated for the cementation of thin and
the degradation of the polymeric matrix and/or unreacted more translucent ceramic veneers. The poorer color sta-
components from the polymerization system14,15 and bility of dual-polymerizing materials is usually associated

a
Graduate student, Graduate Program in Dentistry, Federal University of Pelotas, Pelotas, Brazil.
b
Private practice, Pelotas, Brazil.
c
Doctoral student, Graduate Program in Dentistry, Federal University of Pelotas, Pelotas, Brazil.
d
Professor, Graduate Program in Dentistry, Federal University of Pelotas, Pelotas, Brazil.
e
Professor, Graduate Program in Dentistry, Federal University of Pelotas, Pelotas, Brazil.

272 THE JOURNAL OF PROSTHETIC DENTISTRY

August 2015 273

variation (DE*ab and DE00), while individual color co-

Clinical Implications ordinates were secondary response variables.
Flowable and preheated composite resins had Forty disk-shaped enamel/dentin specimens (diam-
eter 6 mm) were collected from the buccal surfaces of
similar color stability to that of light-polymerizing
bovine incisors by using a water-cooled diamond-coated
resin-based cement when used for bonding ceramic
trephine bur mounted on a bench drill. The top surface of
veneers to enamel.
the disks was all in enamel. The bottom and top surfaces
of the disks were wet-ground to assure they were parallel
to the horizontal plane and the enamel surface was
with the oxidization of the unreacted amine coinitiator
polished with 320-, 600-, and 1200-grit SiC abrasive
from the redox polymerization system. The coinitiators in
papers under running water. Disks with surface defects
light-polymerizing materials are more chemically stable
or discrepancies in color were discarded.
and tend to cause less color variation over time.16 The
Ten cylinders of ceramic (Super Porcelain EX-3, shade
presence of unreacted benzoyl peroxide in dual-
Incisal E1; Kuraray Noritake Dental Inc) with a height of
polymerizing agents may also lead to greater color
13.5 mm and a diameter of 6.3 mm were sintered. To
instability, which will jeopardize the long-term esthetic
obtain each of these cylinders, 1 g of ceramic powder was
appearance of the restoration.
mixed with 0.5 mL of distilled water. The slurry was then
The aging of resin-based materials has been simu-
placed into a metallic mold and uniaxially pressed at
lated in vitro by exposure to radiation and UV/conden-
0.00981 MN for 30 seconds. The ceramic green bodies
sation,17 thermal cycling,18 and static water storage.19 In
were sintered in an electrical furnace (GE-2000; Fortelab)
addition, studies on the color stability of resin-based
according to the manufacturer’s recommendations
luting agents for ceramic veneers usually use methodol-
(Table 2). Forty disk-shaped specimens were obtained by
ogies in which a layer of the luting agent is applied to
cutting the cylinders into 1.1 mm thick slices. The top and
the ceramic,10,13,16,20,21 or monolithic cement specimens
bottom surfaces of the disks were then polished with
are fabricated22-24 with no associated dental structure.
1200-grit SiC abrasive papers under running water. After
In these scenarios, the luting agents are subjected to
polishing, a natural glazing procedure was applied ac-
accelerated aging procedures, and a large surface area of
cording to the manufacturer’s recommendations
specimen agent is exposed to the storage medium.25-31 In
(Table 2). The specimens had a definitive thickness of
the clinical condition, only the margin of the luting agent
1.05 ±0.05 mm as measured with a digital caliper accurate
film of the ceramic veneers that are cemented to tooth
to 0.01 mm (Mitutoyo).
structures is exposed to the oral environment. To the
Two trained (J.R.A. and G.U.S.) investigators pre-
authors’ knowledge, no published study has yet
pared the enamel or ceramic surface for cementation. All
addressed the color stability of ceramic veneers bonded
light-polymerization procedures were carried out by us-
to tooth structures.
ing a light-emitting diode polymerization unit with 800
The purpose of this study was to evaluate in vitro the
mW/cm2 irradiance (FlashLight; Discus Dental). Before
influence of resin-based luting agents (light-polymer-
the cementation procedures, the intaglio surface of the
izing or dual-polymerizing cements and flowable or
ceramic disks was etched with 10% hydrofluoric acid
preheated composite resins) on the color stability of
(Condac Porcelana; FGM) for 1 minute, washed for 30
ceramic veneers bonded to enamel during accelerated
seconds, and air dried until it became white and opaque.
aging by thermal cycling. The study hypothesis was that
A layer of silane (Prosil; FGM) was applied with a
accelerated aging would lead to significant color variation
microbrush, left undisturbed for 1 minute, and air dried
in all the luting agents tested.
for 30 seconds. A layer of a 2-step, etch-and-rinse ad-
hesive (Adper Single Bond 2; 3M ESPE) was applied with
MATERIAL AND METHODS
a microbrush, and excess adhesive was removed with a
This in vitro study investigated the effect of 4 different clean microbrush. The solvent was volatilized by an air
resin-based luting agents on the color stability of bonded stream for 5 seconds at a 10 cm distance from the surface,
ceramic veneers: dual-polymerizing cement, light- followed by light polymerization for 20 seconds. The
polymerizing cement, flowable composite resin, or pre- enamel surface was etched with 37% phosphoric acid
heated composite resin (all shade A1). The 4 resin-based (Condac 37; FGM) for 30 seconds, washed for 30 sec-
luting agents used in this study are described in Table 1. onds, and air dried until it became white and opaque. A
Ten specimens were tested in each group. The color layer of the etch-and-rinse adhesive was applied as
coordinates (L*, a*, and b*) of each ceramic veneer described for the ceramic surface.
bonded to enamel in all groups were measured 3 times: A single trained (M.R.K.) investigator executed the
at baseline, after 10 000 thermal cycles, and after 20 000 cementation procedure by using 7.36 N to standardize
thermal cycles. The primary response variable was color the luting agent layer thickness. The dual-polymerizing

Almeida et al THE JOURNAL OF PROSTHETIC DENTISTRY

274 Volume 114 Issue 2

Table 1. Composition of resin-based luting agents tested (shade A1)

Luting Agent Organic Phasea Inorganic Phasea
Dual-polymerizing TEGDMA, Bis-GMA, dimethacrylate functionalized polymer, triphenyl antimony Silanized ceramic and silica particles
(RelyX ARC)
Light-polymerizing dimethacrylate functionalized polymer, triphenyl antimony Silanized ceramic and silica particles
(RelyX Veneer)
Flowable composite Bis-GMA, TEGDMA, Bis-EMA6, dimethacrylate functionalized polymer Silanized ceramic, silica/zirconia particles
(Filtek Z350 Flow)
Preheated composite Diurethane dimethacrylate, Bis-EMA6, Bis-GMA, polyethylene glycol Silanized ceramic, silica/zirconia particles
(Filtek Z350 XT) dimethacrylate, TEGDMA, hydroxybutyl toluene

TEGDMA, triethyleneglycol dimethacrylate; Bis-GMA, bisphenol-A glycydil dimethacrylate; Bis-EMA6, ethoxylated bisphenol-A dimethacrylate.
a
All materials are products of 3M ESPE. Information presented herein was obtained from manufacturer technical or informative publication.

cement, light-polymerizing cement, and flowable
composite resin agents were mixed (when needed) and
applied to the treated ceramic surface. The veneer was
then positioned on top of the enamel disk, and a con-
stant cementation load was applied for 2 minutes. The
excess luting agent was removed with a clean micro-
brush, and the specimen was light polymerized for 1
minute through the ceramic. For the preheated com-
posite resin group, the material was placed in a glass
container and heated at 60
C for 30 minutes in an
incubator. Immediately after removing the increment
from incubation, it was applied on the ceramic surface,
and the cementation procedure was carried out as for the
other groups.
Color coordinates L*, a*, and b*, based on the
Commission Internationale de l’Éclairage (CIE) system,
were measured with a spectrophotometer (Easyshade;
Vita Zahnfabrik). The device has repeatability varying
from 0.815 to 0.928 according to the color parameter
under evaluation.32 A baseline color reading was per-
formed 24 hours after cementation. Meanwhile, the
specimens were immersed in distilled water at 37
C.
After baseline readings, all specimens were thermal
cycled by using 20 000 cycles. Each thermal cycle con-
sisted of alternated immersion in distilled water at 5 ±5
C
and 55 ±5
C for 30 seconds for each dwell time.
Color coordinates were measured after 10 000 and 20 000
thermal cycles. CIELab color variation between 2
different color readings was determined by using the
following equation33:

1 2
=
DEab = ðDLÞ2 +ðDaÞ2 +ðDbÞ2 : groups after either 10 000 or 20 000 thermal cycles.
CIELab values were also converted into CIEDE2000 color
notation formula,33,34 which was additionally used to
calculate color difference by using the equation:
h i1 2
= While coordinate L* had decreased values with time for
DE00 = ðDL0 =kL SL Þ2 +ðDC0 =kC SC Þ2 +ðDH0 =kH SH Þ2 +RT ðDC0 =kC SC ÞðDH0 =kH SH Þ
where DL0 , DC0 , and DH0 are differences in lightness,
chroma, and hue between 2 color readings and RT is the
rotation function that accounts for the interaction be-
tween chroma and hue differences in the blue region. SL,
Table 2. Porcelain sintering and glazing conditions
Initial Drying Heating Sintering Holding
Procedure Temperature Time Rate Temperature Time
Sinteringa 600
C 10 min 45
C/min 945
C -



Glaze 600 C 5 min 55 C/min 925
C -
a
Sintering process carried out under vacuum.
SC, and SH are weighting functions used to adjust the
total color difference for variation in perceived magnitude
with variation in the location of the color coordinate
difference between 2 color readings. kL, kC, and kH are
correction terms for the experimental conditions.
Confidence intervals (95% CI) were calculated for
color variation means (DE*ab and DE00) between baseline
and 10 000 thermal cycles and between 10 000 and 20 000
thermal cycles. The 95% CIs were also calculated for the
means individual color coordinates (L*, a*, and b*).
Groups were considered significantly different when the
95% CI bounds did not overlap.
RESULTS
The results for color variation are presented in Figure 1.
After 10 000 thermal cycles, the DE*ab for the dual-
polymerizing agent was higher than for the preheated
composite, whereas the light-polymerizing agent and
flowable composite had intermediate results. After 20 000
thermal cycles, the dual-polymerizing agent had higher
CIELab color variation than all the other groups. As
regards the DE00, the results were slightly different but
showed similar trends; the dual-polymerizing agent had
higher CIEDE2000 color variation than all the other
Variations in individual color coordinates from the
baseline reading to after 20 000 thermal cycles are shown
in Table 3. Significant variations with time were observed
for the 3 coordinates depending on the material tested.
; the preheated composite, coordinate a* presented sig-
nificant increased values with time for all groups except
the light-polymerizing agent. For coordinate b*, the
flowable composite resin showed lower values after
thermal cycling, while the dual-polymerizing agent
showed higher b* values after aging.

THE JOURNAL OF PROSTHETIC DENTISTRY Almeida et al

August 2015 275

10 Table 3. Results for individual color coordinates for all groups (n=10)
a Color Coordinates (mean ±95% CI)
Resin-Based
8 Luting Agent Color Reading L* a* b*
A b b DP Baseline 90.5 ±1.2a -0.5 ±0.3b 7.7 ±0.4b
6 AB b AB
ΔE*ab

After 20K cycles 87.7 ±2.1a 0.1 ±0.2a 8.5 ±0.3a

B
4 LP Baseline 91.7 ±1.4 a
-0.5 ±0.3 a
7.6 ±0.4a
ΔE*ab=3.46
After 20K cycles 89.8 ±1.1a 0.1 ±0.3a 7.5 ±0.5a
2
FC Baseline 90.4 ±0.7a -0.5 ±0.1b 7.6 ±0.4a
0 After 20K cycles 89.4 ±1.1 a
0.2 ±0.1 a
6.7 ±0.3b
DP LP FC HC HC Baseline 91.8 ±1.2 a
-0.3 ±0.2 b
6.5 ±0.4a
After 10K cycles After 20K cycles After 20K cycles 89.3 ±0.7 b
0.6 ±0.2 a
6.7 ±0.4a

6 DP, dual-polymerizing cement; LP, light-polymerizing cement; FC, flowable composite resin;
a HC, preheated composite resin.
5 For each material, different letters indicate significant differences between baseline and 20K
A b b cycles for each color coordinate.
4 b B
B
ΔE00

3 B
ΔE00=2.25
2
1
0
DP LP FC HC
Figure 1. Means ±95% confidence intervals of CIELab color variation
(DE*ab) and CIEDE2000 color variation (DE00) for different resin luting
agents tested. DP, dual-polymerizing cement; LP, light-polymerizing
cement; FC, flowable composite resin; HC, preheated composite resin.
DE values were calculated based on color differences between baseline
and 10 000 thermal cycles, and between 10 000 and 20 000 thermal cy-
cles. Uppercase letters indicate significant differences among materials
after 10 000 thermal cycles. Lowercase letters indicate significant differ-
ences among materials after 20 000 thermal cycles.
DISCUSSION
The thermal cycling procedure determined significant
color variation for all the luting agents tested, confirming
the study hypothesis. In addition, at the end of the 20 000
thermal cycles, all groups presented DE*ab>3.46 or
DE00>2.25, which are considered 50% acceptability
threshold values for the color alteration of dental mate-
rials.19 Previous studies have reported color variation of
resin-based luting agents after different methods of
artificial aging.11,13,22 However, those studies used either
thick, monolithic specimens of the luting agents or a thin
layer of the agents bonded to ceramic disks with no
dental structure involved. For both configurations, a large
surface area of a luting agent is homogeneously exposed
to the aging medium. However, this condition does not
relate well to the clinical situation, in which only a thin
line of the luting agent is exposed to the oral environ-
ment. The aforementioned aging approaches may lead
to inconclusive results, as they establish overexposure
conditions to external agents or overestimate the hy-
drolytic degradation of the luting agents.
The dual-polymerizing cement presented higher
CIELab and CIEDE2000 color variation after 20 000 ther-
mal cycles than all the light-polymerizing luting agents
tested, which showed similar results. The cemented
ceramic veneers tested in this study were aged by thermal
cycling and were exposed to constant variations in tem-
perature and to water baths. Different aging methods may
lead to color variation in resin-based materials.10,18,19
Discoloration induced by accelerated artificial aging
methods has been associated with the hydrolytic degra-
dation of organic components in resin-based materials,
mostly with a chemical degradation of the polymerization
promoters.15,25 Oxidation of the amine coinitiator23 is the
main cause of color variation in dual-polymerizing mate-
rials. Dual-polymerizing resin-based materials usually
contain a combination of distinct amines, one to react with
benzoyl peroxide (redox polymerization system) and
another to react with camphorquinone (light-polymeri-
zation system). The amine in the redox system is usually
aromatic and more prone to degradation, whereas the
coinitiator in the light polymerization system is usually
aliphatic and more chemically stable, tending to cause less
color variation.
The presence of unreacted benzoyl peroxide can also
cause color instability in dual-polymerizing resin-based
materials. The reaction between benzoyl peroxide and
amine is not very efficient, as it depends on the physical
encounter of these 2 molecules for chemical interaction
during polymerization. The mobility of the initiators
becomes restricted as the luting agent polymerizes and
the system viscosity is increased, leaving unreacted
species in the polymer network. Corroborating the
results of the present study, Archegas et al10 and Turgut
et al21 observed higher color variation for dual-
polymerizing luting agents, with the exception of Vari-
olink II (Ivoclar Vivadent AG), which presented results
similar to light-polymerizing materials. The authors
hypothesized that this finding could be associated with
the proportion between photosensitizers and chemical
initiators in the polymerization system of Variolink II.
Therefore, if a dual-polymerizing luting agent is chosen
for the placement of an indirect restoration, better
color stability can be anticipated for materials with
high concentrations of photosensitive components.

Almeida et al THE JOURNAL OF PROSTHETIC DENTISTRY

276
However, manufacturers do not always make this in-
formation clear. Thus, light-polymerizing luting agents
are still the first choice for luting procedures that involve
highly esthetic areas.
The amine in light-polymerizing resin-based mate-
rials is used as a coinitiator for camphorquinone, which
presents a yellowish pigmentation. Camphorquinone
undergoes photobleaching during polymerization, and
this reaction leads to slight color changes during poly-
merization. The effectiveness of light-polymerization
depends on the number of amine molecules available
to pair up with camphorquinone and is directly related to
the mechanical and optical properties of the polymerized
material.26,27 Light-polymerization polymers present
increased yellowish appearance during the first 24 hours
after polymerization15 because unreacted molecules of
camphorquinone return to their initial state/color: yellow.
The presence of unreacted or oxidized molecules from
the polymerization system should also be taken into
account because the optical properties of resin-based
materials can be influenced by the elution of unreacted
components.
The literature shows that resin-based luting agents
that are polymerized under ceramic structures present
lower discoloration compared with scenarios in which
monolithic cement specimens are tested.10,13,22-24 This
finding can be associated with a possible masking effect
of the ceramic over the luting agent layer.28 It should also
be considered that a thin layer of a luting agent that is
adhered to the ceramic surface has low volume of poly-
meric material and extended surface area exposed to the
storage medium; this is a condition that is highly favor-
able for the elution of components. Therefore, if oxidized
and unreacted components of the polymerization system
were eluted, less intense color variation could be ex-
pected. In monolithic cement specimens, the intrinsic
components that work as pigments during aging are
present in higher amounts. Thus, longer aging times
would be necessary to elute the discolored components
from the bulk of the specimen.
Another point that should be addressed is that the
polymerization reaction tends to be less effective in thick
cement specimens because of the reduced penetration of
the polymerization light, impairing the excitation and
reaction of the polymerization promoters.29 In the present
study, to better reproduce the clinical scenario, a thin
luting agent film was used, and the agent was confined
between ceramic and enamel disks. This condition led to
values of color variation after 20 000 thermal cycles that
were generally higher than those previously described in
the literature for resin-based luting agents.10,11,13,24 Fac-
tors such as the composition of the luting agents and the
aging method chosen may also explain the differences in
color variation. To the authors’ knowledge, the present
study is the only study in which the luting agent was aged
THE JOURNAL OF PROSTHETIC DENTISTRY
Volume 114 Issue 2
with only the cementation line exposed to the storage
medium; therefore, much less surface area was available
for the elution of the components.
The results for the color coordinates showed a
material-dependent effect of aging over the individual
coordinates, which is in line with previous studies.10,22 The
darkening effect (reduction in L* values) can be associated
with increased pigment content in the bulk of the mate-
rial. The fact that the specimens were not exposed to
external staining agents suggests that the darkening effect
was caused by the presence of oxidized or unreacted
components from the polymerization system and that the
components may act as intrinsic pigments. Similar to the
results of Albuquerque et al,15 variations from negative a*
values (green) to positive a* values (red) during storage
indicates a tendency toward a reddish discoloration. With
regard to coordinate b*, the dual-polymerizing cement
was the only agent that presented a yellowing effect
during aging. The aged dual-polymerizing cement was
yellowish and reddish; this was most likely due to the
presence of unreacted camphorquinone and oxidized
amine molecules that were not eluted because the cement
was almost fully isolated from the storage medium. All the
luting agents tested in this study contain TEGDMA and
Bis-GMA, which are monomers that have chemical
structure groups that are prone to hydrolysis and/or
hydrogen bridging with water: ether in TEGDMA, hy-
droxyl in Bis-GMA, and ester in both. Hydrolytic degra-
dation and hygroscopic effects are determinant factors for
color variation in resin-based materials.30
The increased demand for esthetic treatments requires
clinicians to choose their restorative materials carefully.
Ceramic veneers are frequently used in esthetic restora-
tions, and the luting agent influences their esthetics. Thus,
the selection of the luting agent is key to the long-lasting
success of the treatment, although no clinical studies are
available that evaluate the discoloration of veneer luting
agents. Despite the limitations of this in vitro study, the
present results corroborate the general belief that light-
polymerizing luting agents show better color stability
than dual-polymerizing materials. In addition, flowable
and preheated composite resins may be used as luting
agents for ceramic veneers, as both materials showed
similar results in color stability with the light-polymerizing
cement tested. Clinicians should consider physical prop-
erties, shade range, accessibility, and cost benefits when
choosing a luting agent for ceramic veneers.
CONCLUSIONS
The results of the present study showed that aging
by thermal cycling and types of resin luting agents are
factors that may influence the color stability of ceramic
veneers bonded to enamel. The dual-polymerizing
resin-based cement had higher color variation than the
Almeida et al
August 2015
light-polymerizing cement, flowable composite resin,
and preheated composite resin.
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Corresponding author:
Dr Rafael R. Moraes
School of Dentistry, Federal University of Pelotas
Rua Gonçalves Chaves 457, Rm 505
96015-560, Pelotas-RS
BRAZIL
Email: moraesrr@gmail.com
Copyright © 2015 by the Editorial Council for The Journal of Prosthetic Dentistry.
THE JOURNAL OF PROSTHETIC DENTISTRY