Basic Research—Technology

Bonding of Self-adhesive (Self-etching) Root Canal Sealers

to Radicular Dentin
Brian R. Babb, DMD,* Robert J. Loushine, DDS,* Thomas E. Bryan, BS,* Jason M. Ames, DMD,*
Mark S. Causey, BS,* Jongryul Kim, DMD, MS, PhD,† Young Kyung Kim, DDS, PhD,‡
R. Norman Weller, DMD, MS,* David H. Pashley, DMD, PhD,§ and Franklin R. Tay, BDSc (Hons), PhD*,§

Abstract
The latest generation of methacrylate resin–based sealers
has eliminated the use of separate self-etching primers by
incorporating acidic resin monomers in the sealers to
render them self-adhesive to dentin. This study examined
the adhesive strengths, interfacial ultrastructure, and
tracer penetration of a nonetching (EndoREZ; Ultradent,
South Jordan, UT) and two self-adhesive methacrylate
resin–based sealers (MetaSEAL; Parkell, Farmington,
NY, and RealSeal SE; SybronEndo, Orange, CA) when
they were applied to radicular dentin following the manu-
facturers’ recommended use of EDTA as the active final
rinse. A modified push-out testing design was used to
evaluate the dislodgement of core-free sealers. The mixed
sealers were placed in dimensionally identical, artificially
created canal spaces prepared in the coronal, middle,
and apical thirds of radicular dentin. After setting, each
sealer-filled cavity was subjected to compressive loading
until failure. Additional specimens were prepared for
transmission electron microscopy to examine the ultra-
structure and nanoleakage within the sealer-radicular
dentin interface. The two self-adhesive sealers MetaSEAL
and RealSeal SE exhibited higher push-out strengths than
the nonetching sealer EndoREZ when EDTA was used as
the active final rinse. All three sealers showed a 1- to
1.5-mm thick zone of partially demineralized dentin,
with the EDTA dentin demineralization effect masking
the true self-etching potential of MetaSEAL and RealSeal
SE. The true self-etching potential of self-adhesive sealers
is a clinically important attribute that should be further
investigated. Incomplete smear layer removal from the
apical third of instrumented canal walls may jeopardize
the performance of self-adhesive sealers should they fail
to self-etch without the adjunctive use of calcium
chelating irrigants. (J Endod 2009;35:578–582)
I nterests in adhesive endodontics (1) have led to the introduction of three generations of
methacrylate resin–based root canal sealers. EndoREZ (Ultradent, South Jordan, UT),
the first generation (2–4), uses nonacidic, hydrophilic resin monomers to enhance
sealer penetration into dentinal tubules after the removal of canal wall smear layers
(5, 6). The second generation (7–9) (eg, RealSeal; SybronEndo, Orange, CA) is techno-
logically analogous to those resin-based luting cements that use separate self-etching
primers (10, 11) before the application of flowable composites to the primed dentin.
The use of self-etching primers reintroduces the concept of incorporating smear layers
created by hand/rotary instruments in the sealer-dentin interface (12). Provided that they
are aggressive enough to etch through thick smear layers (13), the technique sensitivity of
bonding to root canals may be reduced when smear layers are inadvertently retained in
the apical third of instrumented canal walls.
The third generation of methacrylate resin–based sealers (eg, MetaSEAL; Parkell,
Farmington, NY, and RealSeal SE) (14, 15) is comparable to self-adhesive resin luting
cements (16) in that both were designed with the intention of combining a self-etching
primer and a moderately filled flowable composite into a single product. They represent
a milestone in bonding step reduction, in that acidic resin monomers that are originally
found in dentin adhesive primers are now incorporated into the resin-based sealer/
cement to render them self-adhesive to dentin substrates.
There have been concerns regarding the limited aggressiveness of self-adhesive
resin cements in creating micromechanical retention via dentin hybridization (17).
This probably accounted for their weaker adhesive strengths and poorer marginal
integrity when compared with conventional resin cements that use etch-and-rinse or
self-etch adhesives for bonding (18–20). In theory, the bonding mechanism of self-
adhesive sealers is similar to self-adhesive resin cements. However, the latter are
used on smear layer–covered dentin, whereas the former are presumably applied to
smear layer–depleted dentin after irrigation with EDTA. As EDTA demineralizes radic-
ular dentin apart from removing smear layers (5, 6, 21), the adhesive mechanism of
self-adhesive sealers may be different from the limited dentin hybridization observed
for the self-adhesive resin cements. Thus, the objective of this study was to examine
the adhesive strengths, interfacial ultrastructure, and tracer penetration of two self-
adhesive methacrylate resin–based sealers when they are applied to radicular dentin
following the manufacturers’ recommended use of EDTA as the active final rinse.

Key Words
Adhesion, dislocation resistance, EDTA, hybrid layer,
nanoleakage, push-out test, root canal sealers

From the *Department of Endodontics, School of Dentistry, Medical College of Georgia, Augusta, GA; †Department of Conservative Dentistry, School of Dentistry,
KyungHee University, Seoul, Korea; ‡Department of Conservative Dentistry, School of Dentistry, Kyungpook National University, Daegu, Korea; and §Department of Oral
Biology, School of Dentistry, Medical College of Georgia, Augusta, GA.
Supported by the Dental Research Center, School of Dentistry, Medical College of Georgia, Augusta, GA.
Address requests for reprints to Dr Franklin R. Tay, Department of Endodontics, School of Dentistry, Medical College of Georgia, Augusta, GA 30912-1129. E-mail
address: ftay@mcg.edu.
0099-2399/$0 - see front matter
Copyright ª 2009 American Association of Endodontists.
doi:10.1016/j.joen.2009.01.005

578 Babb et al. JOE — Volume 35, Number 4, April 2009

 Basic Research—Technology
Materials and Methods
Simulated Canal Spaces
Forty-two human canine teeth were used in this study. A 0.90 
0.05-mm thick longitudinal tooth slice was prepared from each tooth
using an Isomet saw (Buehler, Lake Bluff, IL) under water cooling.
Simulated canal spaces were prepared in the coronal, middle, and
apical thirds of the radicular dentin using the protocol introduced by
Huffman et al (22). Briefly, a minidrill press was used to generate verti-
cally oriented truncated cavities (Fig. 1A) that were enlarged with size
40, 0.04 taper ProFile rotary instruments (Dentsply Tulsa, Tulsa, OK)
to their D16 diameter. Each cavity had standardized diameters of 0.94
mm and 1.04 mm along its top and base. The experimental design
also ensured that the artificial canal spaces were devoid of calcospher-
ites (23) that could have augmented a sealer’s retention from the non-
instrumented parts of a true root canal. Tooth slices were randomly
divided into three groups. For each sealer, 20 simulated canal spaces
from 10 slabs were used for evaluating the push-out strengths at three
radicular dentin locations (N = 20).

Specimen Preparation
Two self-etching, dual-curable, methacrylate resin-based sealers
were investigated. MetaSEAL uses 4-methacryloyloxyethyltrimellitate
anhydride, and RealSEAL SE uses a polymerizable methacrylate carbox-
ylic acid/anhydride as the respective acidic resin monomer. EndoREZ,
a dual-curable sealer that contains nonacidic diurethane dimethacrylate
and triethyleneglycol dimethacrylate, was used as the ‘‘nonetch’’ sealer
for comparison.
Tooth slices were ultrasonicated in 6.15% sodium hypochlorite
(NaOCl), 17% EDTA, and sterile distilled water for 2 minutes each to
remove organic debris and smear layers. En masse cleaning ensured
that potential differences in push-out strength at the three dentin loca-
tions were not caused by inadequate cleaning of the apical dentin. The
cavities were bulk filled with sealer without a main thermoplastic core
material, according to the method invented by Jainaen et al (24). The
sealer-filled, glass slide–covered cavities were stored in light-protected
humidors for 3 days until the sealers had completely set in the self-cured
mode, simulating the curing condition encountered in the middle and
apical thirds of true root canals.
Push-out Strength
Bonding of the set sealers to radicular dentin was evaluated with
a thin-slice push-out test design (25, 26) using a custom-built, light-
illuminated, Plexiform push-out device (Fig. 1B). The use of high-inten-
sity fiberoptic illumination greatly enhanced the alignment of a 0.7-mm
diameter plunger with the inverted truncated cavities, with a 0.1-mm
clearance from either side of the dentinal wall (Fig. 1C). The fiberoptic
illumination ensures that the sealer may be dislodged into the under-
lying cylindrical well without the plunger touching the cavity walls.
Each sealer-filled cavity was subjected to compressive loading via a Vi-
trodyne universal testing machine (Liveco Inc, Burlington, VT) at
a cross-head speed of 10 mm/sec until failure.
The circumferences of the coronal (C) and apical aspects (A) of
each cavity were measured using image analysis software (Scion Corp,
Frederick, MA). The sealer-dentin interfacial area was approximated by
0.5(C + A)h, where h represents the tooth slice thickness. Push-out
strength was computed by dividing the maximum load at failure by
the interfacial area. Failure modes were classified as adhesive failure
along the sealer-dentin interface, cohesive failure within the sealer,
or mixed failure.
Figure 1. (A) Preparation of truncated cavities of uniform dimensions in
radicular dentin. As slanted preparations are not amendable to push-out tests,
a minidrill press was used for the preparation of a pilot hole and subsequently
the attachment of rotary nickel titanium instruments to ensure that all cavities
were created perpendicular to the tooth slice. Two tapered cavities each were
prepared in the coronal (C), middle (M), and apical (A) thirds of a root slice.
(B) Fiberoptic light-illuminated push-out testing device. A plunger (P), con-
nected to a 10-kg load cell (L), is set up over the cylindrical well of
a custom-built Plexiglas stage. The stage has a side channel (open arrowhead)
for the insertion of a fiberoptic light guide. (C) Light illumination greatly
simplifies the task of plunger (pointer) alignment with the center of an inverted
truncated cavity in the tooth slice.
Statistical Analysis
Each sealer-filled hole was treated as a statistical unit. Because the
normality and homoscedasticity assumptions of the push-out strength
data appeared to be valid, they were analyzed using two-way analysis
of variance, with sealer type and dentin location as independent vari-
ables. Post hoc comparisons were performed by using a Tukey test.
Statistical significance was set at a = 0.05.
Transmission Electron Microscopy
The remaining four slabs from each sealer group were filled with
sealer as previously described. After setting, excess sealers were polished
off to expose the sealer-dentin interfaces. For each sealer, two slabs were
processed for examination of the ultrastructure of the sealer-dentin
interface. They were fixed in Karnovsky’s fixative and osmium tetroxide,
dehydrated in an ascending ethanol series, transferred to propylene

JOE — Volume 35, Number 4, April 2009 Bonding Self-adhesive Root Canal Sealers to Radicular Dentin 579
Basic Research—Technology
oxide as a transitional fluid, and finally embedded in epoxy resin at
60  C for 48 hours (27). The other two slabs were processed for exam-
ination of nanoleakage within the sealer-dentin interface by first
immersing in 50 wt% ammoniacal silver nitrate tracer solution (28)
for 48 hours. This was followed by conversion of the diamine silver
ion complexes into metallic silver grains within the interface before
the commencement of the epoxy resin–embedding protocol. Unstained,
90- to 120-nm thick nondemineralized sections were prepared and
examined using a JEM-1230 TEM (JEOL, Tokyo, Japan) operated at
110 kV.

Results
Push-out strengths of EndoREZ (in MPa) at the coronal, middle,
and apical locations were 8.7  4.3, 9.1  2.9, and 7.6  2.1, respec-
tively. Push-out strengths of MetaSEAL at the coronal, middle, and apical
locations were 18.6  4.8, 18.2  4.8, and 16.1  4.6, respectively.
Push-out strengths of RealSeal SE at the coronal, middle, and apical
locations were 12.6  4.3, 14.9  5.5, and 14.4  8.1, respectively.
The push-out strength results (Fig. 2A) were significantly influ-
enced by sealer type (p < 0.001) but not by dentin location (p =
0.297). There was no significant interaction between these two factors
(p = 0.364). MetaSEAL has a higher overall push-out strength than
RealSeal SE (p < 0.05), which, in turn, has a higher overall push-out
strength than EndoFREZ (p < 0.05). MetaSEAL failed predominantly
in the mixed failure mode (76.6%), whereas RealSEAL SE and EndoREZ
failed predominantly by adhesive failure (55% and 75%, respectively)
(Fig. 2B).
Interfacial ultrastructure and nanoleakage results are shown in
Figure 3. Irrespective of whether the sealer is nonetching or self-
etching, the use of EDTA as the final rinse resulted in a 1- to 1.5-mm
thick zone of partially demineralized dentin (ie, hybrid layer) along
the dentin surface (Fig. 3B, D, and F). The occurrence of gaps along
the sealer-dentin interface and the extent of resin infiltration (ie, nano-
leakage) within the hybrid layers could be readily discerned after silver
impregnation. EndoREZ exhibited extensive silver deposits in the gaps
between the sealer and dentin (Fig. 3A). Extensive nanoleakage was
seen throughout the hybrid layer and peritubular cuff in RealSeal SE
(Fig. 3C). Large interfacial gaps were less readily apparent in MetaSEAL;
potential gaps and incomplete sealer infiltration within the hybrid layer
could be identified as a discontinuous line of silver deposits along the
hybrid layer surface and as a fine reticular pattern of silver deposits
within the hybrid layer (Fig. 3B).
Discussion
The goal for obturation of a tooth is to obtain an adequate seal
between the root canal and the periradicular tissues. Thus, there
appears to be no direct clinical correlation between sealer bond
strengths and apical leakage. However, with continued efforts to develop
sealers that bond to radicular dentin, examination of the dentin-sealer
interface has become more relevant. Disruption of the established seal
is a primary concern. This disruption may occur because of mechanical
stresses caused by tooth flexure or post space preparation. In this sense,
the mechanical properties of the interface between dentin and sealer are
important factors to consider.
The analysis of failure modes correlates well with the results of the
push-out tests. As the resistance to dislocation increases, disruption of
the sealer-dentin interface becomes less likely and failure is more likely
to occur within the sealer itself. Thus, MetaSEAL, with its higher push-
out strength, had a higher component of cohesive failure than did the
other two sealers. Based on the results of this study, MetaSEAL provided
increased resistance to dislocation and may provide a more imperme-
Figure 2. (A) A bar chart showing the effects of sealer type and radicular
dentin location on push-out strength. For each methacrylate resin–based
sealer, dentin location subgroups that are connected by the same line above
the colored bars are not significantly different in their push-out strengths
(p > 0.05). Sealers labeled with different letters (A, B, and C) are significantly
different in their overall push-out strengths (p < 0.05). (B) Failure mode
distributions (adhesive, cohesive, or mixed failure) in cavities filled with the
two self-etching, self-adhesive sealers (MetaSEAL and RealSeal SE) and the
nonetching sealer (EndoREZ).
able seal to coronal leakage. This has to be confirmed in future clinical
trials.
Although testing designs that use natural canal spaces have prag-
matic appeals to clinicians, they have severe limitations from a materials
science perspective (22). The application of a compressive load over
a thermoplastic material, which has the tendency to deform during
testing (29), generates erroneous results that could have been respon-
sible, in part, for the report that sealers tested in thin films were consid-
erably weaker than when they were tested in bulk by eliminating the
compliant core material from the canal space (24). To minimize this
shortcoming, the largest plunger that corresponds to the size of the
core material is usually selected (30). Although this is a legitimate
compromise, the procedure requires the use of different diameter
plungers for the different root sections created from a tapered canal.
Because the contact surface areas of the plungers are different, nonstan-
dardized data generated from different parts of the canal walls render
statistical comparisons difficult. The presence of calcospherites-con-
taining noninstrumented regions in instrumented oval-shaped canals
(31) would also have increased undercut retention and contact surface
areas. These regions may unpredictably alter the sealer rankings unless
they are meticulously quantified for adjustments in the push-out
strength results using more robust statistical methods that incorporate
the contribution of covariates in accessing treatment outcomes.

580 Babb et al. JOE — Volume 35, Number 4, April 2009

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Figure 3. Transmission electron microscopy of sealer-dentin interfaces created by the three sealers. Specimens that had been immersed in ammoniacal silver
nitrate are shown at low magnifications to illustrate the extent of silver nanoleakage in the sealer-dentin interfaces (A, C, and E). To avoid redundancy, specimens
that had not been immersed in silver nitrate are shown only at high magnifications (B, D, and F) to demonstrate the 1- to 1.5-mm thick partially demineralized
hybrid layers (between open arrows). S, sealer; M, mineralized radicular dentin; T, resin tag. (A) Nanoleakage in EndoREZ appeared as heavy silver deposits (open
arrowheads) on top of the partially demineralized hybrid layer, creating gaps between the sealer and the top of the hybrid layer. (B) High magnification of the
EndoREZ interface showing apatite crystallite remnants (open arrowhead) within the partially demineralized hybrid layer. As EndoREZ is nonetching in nature,
this partially demineralized zone is created by the use of 17% EDTA as the final rinse. F, electron-dense fillers. (C) Nanoleakage in MetaSEAL occurred as
fine, reticular silver deposits in the hybrid layer (open arrowheads). (D) High magnification of the MetaSEAL interface showing a partially demineralized hybrid
layer containing apatite crystallite remnants (open arrowhead). Asterisk: spherical zirconium oxide fillers; arrow: silica fillers. (E) Nanoleakage in RealSeal SE was
found throughout the entire hybrid layer (asterisk) and the subsurface peritubular cuff of partially demineralized dentin (pointer). Although no gap was apparent
between the sealer and the hybrid layer, there was poor infiltration of the sealer into the partially demineralized zone created by EDTA. (F) High magnification of the
RealSEal SE interface showing apatite crystallite remnants (open arrowhead) within the partially demineralized hybrid layer. F, electron-dense fillers.

JOE — Volume 35, Number 4, April 2009 Bonding Self-adhesive Root Canal Sealers to Radicular Dentin 581
Basic Research—Technology
Under identical cleaning and shaping conditions, the push-out
strengths of all three sealers are independent of the location of the
radicular dentin. These results suggest that variations in tubular density
or sclerotic dentin along the canal walls are unlikely to alter their
mechanical retention. The use of EDTA for smear layer removal resulted
in the consistent appearance of a 1- to 1.5-mm thick zone of partially
demineralized root dentin in the resin-dentin interfaces of all three
sealers, including the nonetching EndoREZ sealer (6, 32). The
universal use of EDTA instead of NaOCl as the active final rinse further
ensured that differences in the overall push-out strengths of the three
sealers to radicular dentin were not influenced by the adverse oxidizing
effect of NaOCl on methacrylate resin polymerization (33).
Under identical cleaning and shaping conditions, push-out
strengths of the two self-adhesive sealers are significantly higher than
the nonetch sealer. Although a variable extent of sealer resin monomer
infiltration for MetaSEAL (Fig. 3C) and RealSeal SE (Fig. 3E) could have
contributed to the difference in their push-out strengths, the true self-
etching potential (17) of these two self-adhering resin-based sealers
could not be assessed with the present study design in which the manu-
facturers’ recommended use of EDTA as the final rinse was strictly fol-
lowed. The ability of these self-adhering sealers to etch through thick
canal wall smear layers to create micromechanical retention and
achieve gap-free sealing of the canal walls has important clinical impli-
cations because debris and smear layer removal may be incomplete in
the apical thirds of the canal walls with many of the contemporary irri-
gation protocols (34, 35). Thus, it is worthwhile to examine in future
studies the self-etching potential of these self-adhesive sealers to ensure
that they are aggressive enough to etch through smear layers and demin-
eralize the intact radicular dentin without the adjunctive use of EDTA.
This may be tested by bonding the self-adhesive sealers to dentin with
thick smear layers and dentin with minimal smear layers. The latter
may be created by polishing dentin with diamond pastes of successively
finer particle sizes. This will provide important information, both to
clinicians as well as manufacturers, on whether these self-adhesive
resin-based sealers are capable of bonding to the most inaccessible
and challenging sites within the instrumented root canal spaces, thereby
achieving strong dislocation resistance as well as a fluid-tight seal.
Acknowledgments
The EndoREZ and MetaSEAL kits used in this study were
generous gifts from Ultradent Products Inc. and Parkell Inc., respec-
tively. The authors are grateful to Mrs Michelle Barnes for her secre-
tarial support.
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