RESEARCH AND EDUCATION

An in situ evaluation of the polymerization shrinkage, degree

of conversion, and bond strength of resin cements used for
luting ber posts
Camilo Andrs Pulido, DDS, MS,a Ana Paula Gebert de Oliveira Franco, DDS, MS, PhD,b
Giovana Mongruel Gomes, DDS, MS, PhD,c Bruna Fortes Bittencourt, DDS, MS, PhD,d
Hypolito Jos Kalinowski, BS, MS, PhD,e Joo Carlos Gomes, DDS, MS, PhD,f and
Osnara Maria Mongruel Gomes, DDS, MS, PhDg
Resin cements have been
widely used to lute glass ber
posts in patients with extensive
reconstruction in endodontically treated teeth. Currently,
these posts are an esthetic option that allow retention of the
materials selected for reconstruction. Because their elastic
modulus is more similar to
that of dentin than of metal,1,2
their mechanical properties
may improve the clinical prognosis, as better distribution
of masticatory forces in dental
structures3 reduce the risk of
unrestorable fractures.4,5
Despite their favorable
esthetic and mechanical properties, the adhesion of these
posts in the intraradicular region
presents several challenges for
the clinician, such as heterogeneous dentin characteristics,6,7

ABSTRACT
Statement of problem. The behavior and magnitude of the deformations that occur during
polymerization and the behavior of the luting agents of glass ber posts inside the root canal
require quantication.
Purpose. The purpose of this in vitro study was to investigate the in situ polymerization shrinkage,
degree of conversion, and bond strength inside the root canal of resin cements used to lute ber
posts.
Material and methods. Thirty maxillary canines were prepared to lute ber posts. The teeth were
randomly divided into 2 groups (n=15) according to the cementation system used, which included ARC,
the conventional dual-polymerized resin cement RelyX ARC, and the U200 system, a self-adhesive resin
cement, RelyX U200. Two ber optic sensors with recorded Bragg gratings (FBG) were attached to each
post before inserting the resin cement inside the root canal to measure the polymerization shrinkage
(PS) of the cements in the cervical and apical root regions (m). Specimens were sectioned (into
cervical and apical regions) to evaluate bond strength (BS) with a push-out test and degree of
conversion (DC) with micro-Raman spectroscopy. Data were statistically analyzed with 2-way ANOVA
and the Tukey honestly signicant difference post hoc test (a=.05).
Results. The ARC and U200 system showed similar PS values (-276.4 129.2 m and -252.1 119.2
m, respectively). DC values from ARC were higher (87.5 2.7%) than those of U200 (55.9 9.7%).
The cervical region showed higher DC values (74.8 15.2%) and PS values (-381.6 53.0 m) than
those of the apical region (68.5 20.1% and -146.9 43.5 m, respectively) for both of the resin
cements. BS was only statistically different between the cervical and apical regions for ARC (P<.05).
Conclusions. The ARC system showed the highest PS and DC values compared with U200; and
for both of the resin cements, the PS and DC values were higher at the cervical region than at the
apical region of the canal root. BS was higher in the cervical region only for ARC. (J Prosthet Dent
2016;-:---)

Supported by the Coordenao de Aperfeioamento de Pessoal de Nvel Superior (CAPES), Brazil. Support required to perform the polymerization shrinkage test
provided by the Federal University of Technology, Paran, Brazil.
a
Doctoral student, Department of Restorative Dentistry, School of Dentistry, State University of Ponta Grossa, Ponta Grossa, Brazil.
b
Professor, Department of Electrical Engineering, Federal University of Technology, Paran, Brazil.
c
Professor, Department of Restorative Dentistry, School of Dentistry, State University of Ponta Grossa, Ponta Grossa, Brazil.
d
Professor, Department of Restorative Dentistry, School of Dentistry, State University of Ponta Grossa, Ponta Grossa, Brazil.
e
Professor, Department of Electrical Engineering, Federal University of Technology, Paran, Brazil.
f
Professor, Department of Restorative Dentistry, School of Dentistry, State University of Ponta Grossa, Ponta Grossa, Brazil.
g
Professor, Department of Restorative Dentistry, School of Dentistry, State University of Ponta Grossa, Ponta Grossa, Brazil.

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MATERIAL AND METHODS

Clinical Implications
Polymerization shrinkage of resin cements may
affect the adhesion of glass ber posts to the root
canal. Fiber optic sensors, based on Bragg
gratings, are suitable for studying the resin cement
deformations that occur in the cervical and apical
root regions.

density and orientation of dentinal tubules,8 presence of

endodontic smear layer,9 moisture control in the root canal,10 presence of a ferrule on the tooth,11 high sensitivity of
adhesive techniques,12-14 and polymerization shrinkage of
resin cements.15
One of the biggest difculties with intracanal posts is
gradual loss of retention, which is exacerbated by the
polymerization shrinkage of cementing agents and which
generates gaps at the dentin-resin cement interface.16
Gaps may occur if the polymerization shrinkage forces
exceed the bond strength of the material to dentin,15,16
characterized by unbonded areas that may increase under functional loading, thus resulting in post detachment
and treatment failure.17-21
The bond strength of dentin-resin cement has been
extensively investigated with in vitro microtensile and
push-out tests,10,12,17,22-28 the inuence of the cavity
conguration, the C-factor,15,27 the degree of conversion,29-31 and the kinetics and properties of the resin
cement,30-37 but little is known about the behavior and
magnitude of the deformations that occur during in situ
polymerization. This is explained by the small size of the
root canal, which complicates the placement of
measuring instruments.
Fiber optic sensors based on Bragg gratings are widely
used to monitor material deformations,38 including
dental resins.39,42 Bragg sensors have several advantages
in comparison to conventional sensors, such as their
small size, no susceptibility to electromagnetic interference, and easy placement of the sensor inside the resin
structure.41 These sensors have been used in in vitro
studies that analyzed polymerization shrinkage and
setting expansion during the polymerization process of
dental materials.39,41
However, no studies have been found that evaluated
the behavior and magnitude of the deformations that
occur during the polymerization of resin cements inside
the root canals. Therefore, the purpose of this research
was to study the deformations that occur during polymerization in situ by means of ber optic sensors based
on the Bragg gratings, the degree of conversion of resin
cements in root canals by micro-Raman spectroscopy,
and the bond strength of ber posts to root dentin with a
push-out test.

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Thirty extracted human maxillary canines were stored in

distilled water at 4
C and used within 6 months after
extraction. Teeth that exhibited clinical signs of caries,
root resorption, cracks, or fractures were excluded.
Additionally, all teeth had a root length of 14 1 mm,
measured from the cement-enamel junction (CEJ).
The teeth were transversally sectioned 1 mm above
the CEJ by using a low-speed diamond saw (Isomet 1000;
Buehler) under constant irrigation. Endodontic access
was made using a tapered ssure bur mounted in highspeed. The canal working length was xed to be 1 mm
shorter from the apical foramen. A crown-down technique was used for instrumentation with K les
(Dentsply Maillefer). Apical enlargement was performed
to size 40 and 0.06 taper. Irrigation was performed after
every change of instrument by alternating 1 mL of 1%
NaOCl solution and 17% EDTA (Dentsply Maillefer)
solution. The roots were dried with paper points
(Dentsply Maillefer) and lled with resin-based sealer
(AH Plus; Dentsply Intl) and gutta percha points using
the warm vertical condensation technique. The root access was temporarily lled with interim cement (Coltosol;
Vigodent). The specimens were stored in distilled water
at 37
C for 1 week.
After the storage period, the gutta percha was
removed using numbers 2, 3, and 4 Gates Glidden burs,
leaving 4 mm of the apical seal. The post space was then
prepared with a low-speed bur provided by the post
manufacturer (Whitepost DC number 2; FGM) up to a
xed depth of 10 mm from the CEJ. The diameter of the
post space preparation was constant for all teeth. One
bur was used for 5 preparations.
After preparing the post spaces, the canals were irrigated with 10 mL of distilled water and dried with paper
points. The post space walls were evaluated for the
presence of any residual gutta percha with radiographs
(Dentus E Speed; Agfa). The drill of the number 2 post
(Whitepost DC; FGM) and the cementation of the
smaller diameter number 1 post (Table 1) provided the
space needed for the correct measurement of the optical
bers. Before the cementation procedures, each glass ber post was horizontally sectioned with a water-cooled
diamond rotary cutting instrument so that a total
length of 13 mm remained. The ber posts were cleaned
with 70% alcohol for 5 seconds, and a silane agent was
applied (Ceramic Primer RelyX; 3M ESPE). Ten millimeters of the post length was cemented inside the root
canal, while the remaining cervical 3 mm served as a
guide to standardize the distance of the lightpolymerizing device from the cervical root region.
Specimens (N=30) were randomly divided by drawing
lots in the following 2 groups (n=15 each) according to
the resin cement used for ber post cementation: ARC, a

Pulido et al

2016

Table 1. Materials, manufacturers, and composition (according to the manufacturer)

Material

Manufacturer

Phosphoric acid

Dentsply Intl

37% phosphoric acid

Composition

Adper Scotchbond
multipurpose
Plus adhesive

3M ESPE

Activator: ethanol solution of sulnic acid salt and a photoinitiator component.

Primer: HEMA and polialcenoic acid copolymer.
Catalyst: HEMA and Bis-GMA, BPO.

RelyX ARC

3M ESPE

Paste A: Bis-GMA, TEGDMA, zircon and silica inorganic llers (68% wt), photo-initiators, amines and pigments.
Paste B: Bis-GMA, TEGDMA, benzoyl peroxide, zircon and silica inorganic llers (67% wt).

RelyX U200

3M ESPE

Base: berglass, esters, phosphoric acid, methacrylate, triethylene glycol dimethacrylate (TEGDMA), silanated silica
and sodium persulfate, inorganic llers (45% wt).
Catalyst: berglass, substitute dimethacrylate, silanated silica, sodium p-toluenesulfonate and calcium hydroxide.

Number 1 post
Whitepost DC

FGM

80% berglass coronary diameter: 1.6 mm

20% Epoxy resin
Apical diameter: 0.85 mm;
Length: 20 mm

Number 2 drill
Whitepost DC

FGM

Coronary diameter: 1.8 mm

Apical diameter: 1.05 mm
Length: 20 mm

dual polymerizing resin cement (RelyX ARC; 3M ESPE),

and U200, a self-adhesive resin cement (RelyX U200; 3M
ESPE). Ten roots per group were prepared for evaluation
of the polymerization shrinkage of the resin cement, and
the other 5 roots per group were prepared for the degree
of conversion test and the bond strength of the ber
posts to root dentin.
Fiber optic sensors based on the Bragg gratings (FBG)
were used to measure the polymerization shrinkage
(strain values) of the resin cement inside the root canal
(n=10/group). These FBG sensors were recorded in
conventional, nonhydrogenated optical ber (Draktel;
ESMF) using illumination under phase mask at the
wavelength of 193 nm (ArF laser). The peak amplitude of
the ratings was set at 11 dB above the noise oor. A ber
Bragg grating interrogator (SM125; Micron Optics) was
used to measure the spectral shift of the grating reection
spectra from which the strain values were determined.
Before inserting the resin cement inside the canal of
these roots, the demarcation and cut of the post were
carried out to determine the position of 2 optical ber
sensors of approximately 2 mm, which were recorded
with networks of different wavelengths (1537 nm and
1542 nm): one was in the most apical part of the post and
the other at the coronary portion. After the sensors were
positioned, the optical bers were bonded with cyanoacrylate resin (Loctite; Henkel Corp) in the outside part
of the glass ber post (Fig. 1).
For the ARC group, the root canal walls were etched
with 37% phosphoric acid gel (Dental Gel; Dentsply
Intl) for 15 seconds, washed for 30 seconds, and dried
with absorbent paper points, leaving the dentin slightly
moist. The adhesive system (Adper Scotchbond Multipurpose Plus; 3M ESPE) was then applied initially by
carrying the activator inside the root canal, then the
primer, and nally the catalyst with a specic applicator
tip (Points; SDI Ltd). The excess was removed with
absorbent paper points, and the adhesive system was
photopolymerized for 20 seconds. After that, the resin
Pulido et al

Figure 1. Schematic of sensor positioning in root canals.

cement was manipulated according to the manufacturers instructions and inserted into the root canal
space with a syringe (Centrix; DFL) before seating the
ber post. Excess resin cement was removed, and
remaining cement was photopolymerized through the
post for 40 seconds.
For the U200 group, the root canal walls were cleaned
with distilled water and dried with absorbent paper
points. The resin cement was manipulated according to
the manufacturers instructions and inserted into the root
canal space with a syringe (Centrix; DFL) before seating
the ber post. The excess resin cement was removed,
and the remaining cement was photopolymerized
through the post for 40 seconds. All light-polymerizing
procedures were performed with a light-emitting diode
device (Radii Plus; SDI Ltd) with an irradiance of 1200
mW/cm2.
The teeth selected and prepared for polymerization
shrinkage evaluation (n=10/group) were evaluated for 1
hour after ber post cementation. For this purpose, the 2
optical ber sensors, which were coupled to each glass
ber post, were connected to the SM125 interrogator by
means of a coupler with the software, thus enabling the

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wavelengths to be graphed. The range of wavelengths in

time was recorded and converted to a text le for later
tabulation and data collection of the polymerization
shrinkage in microstrain (m).40,41
The same luting procedures were performed in 10
teeth, 5 for each cementation system as described previously, except that the sensors were not coupled to the
ber posts. After cementation, the roots were placed in
separate polyvinyl chloride tubes and embedded in
acrylic resin (Duralay; Reliance Dental Mfg). The portion
of each root containing the bonded ber post was
sectioned perpendicularly to the long axis into six 1-mmthick slices. A diamond saw (Isomet 1000; Buheler) was
used under water cooling to create 2 cervical and 2 apical
slices.
A micro-Raman spectrometer (Senterra; BrukerOptik GmbH) was used to evaluate the degree of conversion. Measurements were made 1 hour after glass
ber post cementation. Raman back-scattered light was
collected through the objective (magnication 100).
Parameters included a slit width of 25 mm; accumulation
time per spectrum of 60 seconds; and 3 spectra
per point. The spectral region analyzed was 1785 to
875 cm1. Raman spectra were obtained as follows:
1637 cm1 peak indicates aliphatic C=C double bonds
of the cement and 1608 cm1 peak represents the aromatic C=C bonds (internal reference). Spectra of the
unpolymerized resin cements were obtained as reference. Postprocessing of the spectra was performed
with software (Opus Spectroscopy v6.5; Bruker Corp).
Peaks were deconvoluted and smoothed to localize their
exact position and intensities. Peaks were integrated,
and the ratio was automatically given by the software.
The DC of the resin cement was calculated using the
equation
!
Rpolymerized
DC%=
100;
RNonpolymerized
where R is the ratio of the aliphatic and aromatic peak
areas at 1637 cm1 and 1608 cm1 in polymerized and
unpolymerized resin cements.7
To evaluate bond strength, the coronal side of each
slice was identied, and its thickness was measured with
digital calipers (Mitutoyo; accuracy of 0.01 mm). Slices
were also photographed on both sides with an optical
microscope at 40 magnication (model BX 51;
Olympus) to measure the coronal and apical diameters of
the posts with the purpose of calculating their individual
bonding areas. This measurement was made with software (ImageTool v3.0; UTHSCSA).
Each specimen (slice) was subjected to a push-out
bond strength test using a universal loading device
(AG-I; Shimadzu Autograph) at a crosshead speed of 0.5
mm/minute. The load was applied in the apical-coronal

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direction until the post was dislodged. Care was taken

to center the push-out pin on the center of the post
surface without stressing the surrounding post space
walls. With regard to the tapered design of the post,
different sizes of punch pins matching the diameter of
the post at the different root thirds being tested were
used.
The maximum failure load (N) was recorded and
converted to millipascals by dividing the applied load by
the bonded area (SL); the latter, being the lateral surface
of a truncated cone, was calculated by using the formula
h
i0:5
SL =pR+r h2 +Rr2
;
where p=3.14, R=coronal post radius, r=apical post
radius, and h=root slice thickness.26
Data obtained from polymerization shrinkage, degree
of conversion, and push-out bond strength were
analyzed by 2-way ANOVA (factors: resin cement
and radicular region) and the Tukey HSD post hoc test
(a=.05).
RESULTS
Mean standard deviation (SD) polymerization shrinkage values (m) for each experimental group are presented in Table 2. Two-way ANOVA showed that the
interactions between the resin cement and root region
factors were not statistically signicant (P=.889). The
main factors, resin cement types, were not statistically
different (P=.119), but the main factor root region was
(P<.001). The cervical region showed higher polymerization shrinkage values than the apical region for both
resin cements.
For degree of conversion, mean SD values (%) for
each experimental group are presented in Table 3. Twoway ANOVA also showed no signicant differences between interactions of the resin cement and root region
(P=.096). The main factors, resin cement (P<.001) and
root region (P=.035), were statistically different, with the
DC values at the cervical third higher than DC values at
the apical third for both resin cements. Also, RelyX ARC
showed statistical higher values than RelyX U200
(P<.001).
The mean SD bond strength values (MPa) for
each experimental group are shown in Table 4. Twoway ANOVA showed that the interaction between the
factors resin cement and root region was statistically
signicant (P=.03). The highest values were found for
the cervical third of RelyX ARC, which was higher
than the apical third from the same resin cement.
For U200, no differences were found between the
cervical and apical thirds. Both of the resin cements
showed statistically similar results at the apical third
(P>.05).
Pulido et al

2016

Table 2. Mean SD polymerization shrinkage values (m) for each

experimental group (n=10)
Root Region
Resin Cement
RelyX ARC

Table 3. Mean SD degree of conversion values (%) for each experimental group (n=5)

Apical

Main Factor
Resin Cement

Resin Cement

Cervical

Apical

Main Factor
Resin Cement

-392.7 50.6

-160.1 51.2

-276.4 129.2a

RelyX ARC

88.2 3.4

86.7 1.8

87.5 2.7A

61.5 7.6

50.3 8.8

55.9 9.7B

74.8 15.2A

68.5 20.1B

RelyX U200

-370.5 55.7

-133.6 31.5

Main factor root region

-381.6 53.0A

-146.9 43.5B

-252.1 119.2

Different superscript uppercase letters indicate statistical signicance (P<.05) in columns;

Difference superscript lowercase letters indicate statistical signicance (P<.05) in rows.

DISCUSSION
The polymerization reaction is based on monomer conversion into a polymeric chain, an inherent feature of
which is polymerization shrinkage. Resin cements used
in this study exhibited dual polymerization: chemical
(when the base and catalyst are mixed) and physical
(when the light interacts with the photoinitiator), which
is directly proportional to the light source intensity; if the
light intensity decreases, polymerization will be
compromised. Even with the use of translucent glass ber posts, light transmission through the root canal
signicantly decreased in the apical region and that
chemical reaction did not reach suitable properties, which
in turn, promoted low polymerization. This may explain
the lowest polymerization shrinkage values obtained
in the apical region: the highest distance from the light
unit, the lowest polymerization. As a consequence, the
lowest polymerization shrinkage also occurred.31
Discrepancies in the degree of conversion values between the root regions, regardless of the resin cement,
were signicant, with the highest values found in the
cervical region. This conrmed the previous hypothesis
that in the apical region, because of the deciency in the
physical activation, the lower monomer conversion
would decrease the polymerization shrinkage.32
Moreover, the inclusion of multiple steps increases
technique sensitivity,13 difculty in removing adhesive
excess, and solvent evaporation into the apical region. All
these negative effects decreased bond strength values to
radicular dentin,44 which may explain the lower bond
strength values found in the apical region for RelyX ARC
cement compared with the cervical region, even with a
high conversion values.
The ARC group showed the highest conversion values
in both of the analyzed regions compared with the U200
group. Despite the fact that the degree of conversion is
composition-dependent and a careful comparison between materials is important, differences between the
resin cements (conventional and self-adhesive) were
observed. A plausible explanation may be the triethylene
glycol dimethacrylate (TEGDMA) content in each resin
cement. Probably, ARC has a higher content of the
diluent monomer compared with the more viscous U200.
This increased viscosity of self-adhesive cements may
affect the ability of radicals to migrate and continue the
Pulido et al

Root Region

Cervical

RelyX U200
Main factor Root region

Different superscript letters show statistically signicant differences (P<.05).

Table 4. Mean SD bond strength (MPa) for each experimental group

(n=5)
Root Region
Resin Cement

Cervical

RelyX ARC

16.6 4.5A

11.8 1.5B

Apical

RelyX U200

8.7 1.6C

9.5 1.5BC

Different superscript letters show statistically signicant differences (P<.05).

setting reaction, lowering the degree of conversion

values.45
Another possible explanation for the higher conversion values from the ARC group is the use of alternative
co-initiators in the Adper Scotchbond Multi-Purpose
Plus adhesive system. Arrais et al43 evaluated the inclusion of aromatic sodium sulfonate salts in adhesives. This
addition allowed components to start self-polymerization
even when light was not available. The increase in conversion values induced by this adhesive system with coinitiators, specically in the apical region, did not increase
polymerization shrinkage. If polymerization shrinkage
and shrinkage stress decreased, then, as a consequence,
better mechanical properties and higher bond strength
values43 would be achieved.
Furthermore, composition variations may affect the
mechanical properties of dental resin cements. The ller
weight content of RelyX ARC (approximately 67% [wt%])
is higher than that of RelyX U200 (approximately 45%
[wt%]). In addition, RelyX ARC contains particles with a
higher average ller size than those of RelyX U200.
Although self-etch and conventional resin cements have
similar clinical indications, differences in chemical
composition and ller type or size may directly affect the
exural properties and shrinkage behavior. During the
polymerization process, monomers react to form a covalent bond, and the distance between the molecules is
reduced, leading to free volume reduction, which, in turn,
results in volumetric shrinkage in the nal polymeric
network. The mobility of the monomer-chain can be
restricted by the amount of the llers, leading to
decreased monomers and radical mobility thus resulting
in lower shrinkage.45
RelyX ARC has a higher ller content (which may
increase the elastic modulus) and probably a higher
TEGDMA content (which may decrease the elastic
modulus). However, U200 has a lower ller content and
possibly a higher Bis-GMA percentage, increasing the

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elastic modulus. These factors (ller content versus BisGMA/TEGDMA content) may have balanced each
other.46 Also, the polymerization kinetics of both materials may be similar. This may explain the similar
behavior of the polymerization shrinkage of the resin
cements, regardless the differences in degree of conversion. However, these statements are only speculations, as
the monomer content in the resin cements is not
described in the composition given by the manufacturer.
RelyX U200 is a recently introduced cement which
will replace RelyX U100 with a similar composition. Our
results were similar to those presented in other studies,
with similar bond strength values in the apical and cervical regions.28,47 The manufacturer claims that these
self-adhesive resin cements show a chemical interaction
between the acidic monomers and hydroxyapatite from
dentin.29 A higher degree of conversion values was found
in the cervical region; however, bond strength values in
the apical region did not decrease. This may be attributed
to the number of dentinal tubules in the apical region,
which is considerably lower compared with the cervical
third, and the fact that more hydroxyapatite-enriched
intertubular space was available to react chemically
with the resin cement.
The present study evaluated only 1 of each type of
resin cement (dual conventional and dual self-adhesive),
which does not necessarily reect the general behavior of
these groups. Thus, future studies should investigate
more resin cements in order to investigate the differences
between the classications.
CONCLUSIONS
Within the limitations of this in vitro study, the following
conclusions were drawn:
1. The optic ber sensor based on Bragg gratings
proved to be an efcient device for measuring
deformation of resin cements.
2. The conventional resin cement showed the highest
polymerization shrinkage and degree of conversion
values compared with the self-adhesive resin
cement.
3. For both resin cements, the polymerization
shrinkage and degree of conversion values were
higher at the cervical region than at the apical region
of the canal root.
4. The highest bond strength values were found in the
cervical region when the conventional resin cement
was used.
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Corresponding author:
Dr Camilo A. Pulido
Rua Vicente Spsito 188
Bloco 10 ap 04
Ponta Grossa, Paran 84031900
BRAZIL
Email: capulidomora@hotmail.com
Copyright 2016 by the Editorial Council for The Journal of Prosthetic Dentistry.

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