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Purpose. The purpose of this study was to examine the effects of denture base resin surface pretreatments with
different chemical etchants preceding the silicone-based resilient liner application on microleakage and bond
strength. The initial effects of chemical etchants on the denture base resin in terms of microstructural changes
and flexural strength were also examined.
Material and methods. Forty-two polymethyl methacrylate (PMMA) denture base resin (Meliodent) specimens consisting of 2 plates measuring 30 3 30 3 2 mm were prepared and divided into 7 groups (n=6).
Specimen groups were treated by immersion in acetone for 30 (A30) or 45 (A45) seconds, methyl methacrylate
monomer for 180 (M180) seconds, and methylene chloride for 5 (MC5), 15 (MC15) or 30 (MC30) seconds.
Group C had no surface treatment and served as the control. Subsequently, an adhesive (Mollosil) and a silicone-based resilient denture liner (Mollosil) were applied to the treated surfaces, and all specimens were immersed in the radiotracer solution (thalium-201 chloride) for 24 hours. Tracer activity (x-ray counts), as a
parameter of microleakage, was measured using a gamma camera. For bond-strength measurement, 84 rectangular PMMA specimens (10 3 10 3 40 mm) were surface-smoothed for bonding and treated with the different
chemical etchants using the same previously described group configurations. The adhesive and the siliconebased denture liner were applied to the treated surfaces. Tensile bond-strength (MPa) was measured in a universal testing machine. Flexural strength measurement was performed with 49 PMMA specimens (65 3 10 3
3.3 mm according to ISO standard 1567) in 7 groups (n=7), with 1 flat surface of each treated with 1 of the
chemical etchants preceding adhesive application. The flexural strength (MPa) was measured using a 3-point
bending test in a universal testing machine. The data were analyzed by 1-way analysis of variance and the Tukey
HSD test (a=.05).
Results. Significant differences were found between the groups in terms of microleakage (P,.0001). The lowest microleakage was observed in group M180 (30,000 x-ray counts) and the highest in the control group
(44,000 x-ray counts). The mean bond strength to PMMA resin ranged from 1.44 to 2.22 MPa. All treated
specimens showed significantly higher bond strength than controls (P,.01). The flexural strength values all
significantly differed (P,.05). All experimental specimens that had chemical surface treatments showed
lower flexural strength than controls (P,.05).
Conclusion. Treating the denture base resin surface with chemical etchants increased the bond strength of
silicone-based resilient denture liner to denture base and decreased the microleakage between the 2 materials.
Considering the results of both tests together, the use of methyl methacrylate monomer for 180 seconds was
found to be the most effective chemical treatment. (J Prosthet Dent 2006;95:143-51.)
CLINICAL IMPLICATIONS
Results from this study showed that treating a denture base acrylic resin surface with chemical
etchants prior to adhesive application reduced the microleakage and increased the bond strength
when using silicone-based resilient liners. However, these chemical treatments decreased the
flexural strength of the acrylic resin when compared to the untreated group.
FEBRUARY 2006
their chemical structures as plasticized acrylic resins, using either chemical or heat polymerization, vinyl resins,
polyurethane and polyphosphazine rubbers, and silicone rubbers.4 Silicone rubbers are not dependent on
leachable plasticizers and, therefore, retain their elastic
properties for prolonged periods. Silicone rubber materials may be chemically or heat polymerized. Placement
of chemically polymerized resilient liners is relatively
straightforward when compared to heat polymerized
liners.4
There are disadvantages to the use of resilient liners,
including various degrees of softness or poor tear
strength. One problem with silicone-resilient liners is
the failure of adhesion between a resilient liner and a
denture base.2,5,6 Mechanical roughening of denture
base resin by airborne particle abrasion was reported to
have a weakening effect on the bond strength of silicone-based resilient liners.7,8
Bond failure between the liner and denture base also
creates a potential interface for microleakage. Therefore,
effective bonding is important for longevity, and longterm bonding cannot be accomplished without also preventing leakage of fluids between the liner and denture
base.7,9 Many techniques have been used to determine
microleakage between dental materials: use of bacteria,
compressed air, chemical tracers, electrochemical changes,
autoradiographic studies, scanning electron microscopy
(SEM), and die penetration.10 Use of radioisotopes can
provide finer detail in leakage patterns, as well as serve as
a method to quantify and compare leakage values.11
Radionuclide imaging is accepted as a gold standard in
physiologic visualization of the human body and is a
part of routine diagnostic imaging procedures.12
High-performance gamma cameras and positron
emission topography are powerful tools used in nuclear
medicine.13 With the development of various radionuclides, nuclear medicine applications in dental research
have gained popularity. Thallium is a metallic element
of Group IIIA in the periodic table. Thallium-201 chloride is a cyclotron-generated radionuclide. This tracer is
produced by the 203Tl (p,3n) 201Pb 201 / Tl reaction. It decays (physical half life=73 hours) by electron
capture to mercury-201, emitting mercury x-rays of 69
to 83 keV (94.4% abundant; used for imaging) and thallium gamma rays of minimal abundance.13 The hydrated
thallium ion is similar in size and biological behavior to
the hydrated potassium ion and can easily follow water
molecules in any medium.14 One of the advantages of
gamma camera imaging versus autoradiography is the
possibility of digital processing of acquired images
with the possibility of quantification. Thus, tracing thallium-201 ions is feasible with its sufficiently long half
life, and it can also be imaged in high resolution due
to its low energy level.15 The possibility of reliable imaging and counting thallium-201 ion quantity in a bonding zone provides investigators an opportunity to
144
SARAC ET AL
SARAC ET AL
Product
Batch No.
Manufacturer
Meliodent
Mollosil
Meliodent
01266
040902
K26610813-924
K23408449-644
012101
chemical etchants preceding placement of a siliconebased resilient liner application on microleakage and
bond strength was evaluated. Secondly, the initial effects
of chemical etchants on a denture base resin in terms
of microstructural changes and flexural strength was
examined. The research hypothesis was that the duration
of application or the type of chemical etchants would
have different effects on the bond strength of the silicone-based resilient liner to denture base resin and on
the amount of microleakage between the 2 materials.
Group
Group
Group
Group
Group
Group
Group
Surface pretreatment
C
A30
A45
M 180
MC5
MC15
MC30
Untreated (control)
30-s acetone
45-s acetone
180-s methyl methacrylate
5-s methylene chloride
15-s methylene chloride
30-s methylene chloride
SARAC ET AL
Fig. 2. Testing apparatus for (A) tensile bond strength test and (B) flexural strength test.
Background correction was performed for each specimen unit. To accomplish this, the mean OSC value of
the 6 size-matched PMMA blocks was accepted as a normal contamination value and was subtracted from the
total count value of each microleakage specimen unit to
detect radiation attributable only to microleakage. The
amount of OSC-subtracted total specimen counts was
assumed to be directly proportional to the quantity of
the inward diffusing tracer. OSC-subtracted counts
were used in the statistical analysis of the groups and
were compared with each other using 1-way analysis of
variance (ANOVA) (SPSS 12.0; SPSS Inc, Chicago,
Ill) and Tukey HSD tests (a=.05).
Eighty-four rectangular PMMA blocks with a 10 3
10-mm2 cross-sectional area and 40-mm length were
prepared for tensile bond strength test. For the preparation of the PMMA blocks, 2 brass dies with 10 3 10mm2 cross-sectional area and 40-mm length were
used. These dies were invested in silicone rubber
(Zetaplus; Zhermack Spa). The obtained mold was
used for the preparation of the wax blocks, which were
used for the production of the PMMA blocks. Acrylic
resins were processed in a water bath 75C for 9 hours.
After polymerization, PMMA blocks were ground with
320-grit silicone carbide paper (Carbimet; Buehler,
Lake Bluff, Ill) to remove surface irregularities and
excess material. Two PMMA blocks with a 3-mm-thick
brass spacer between them were invested in a denture
flask (Atlas flask; Handler Mfg, Westfield, NJ) using
silicone rubber (Zetaplus; Zhermack Spa) to allow for
easy removal of the specimens from the flask. The
PMMA blocks were then removed from the flask, and
the surfaces to be bonded were smoothed and pretreated with different chemical treatments as described
in the microleakage test. The adhesive (Mollosil-specific; DETAX) was applied to the treated surfaces with
a brush and left to dry for 1 minute. Next, the PMMA
blocks were placed back into the molds, and the silicone-based resilient liner was then packed into the space
VOLUME 95 NUMBER 2
SARAC ET AL
Mean
SD
Group
Group
Group
Group
Group
Group
Group
C
A30
A45
M180
MC5
MC15
MC30
A30
A45
M180
MC5
MC15
MC30
44,000
5,000
32,000
3,000
X
43,000
7,000
30,000
6,000
X
42,000
5,000
33,000
6,000
X
39,000
7,000
X
X
X
X
Between groups
Within groups
Total
Sum of squares
df
Mean square
Sig.
1234492735
1138056501
2372549236
6
35
41
205748789
32515900
6.328
.0001
previously described in the microleakage test. All specimens were allowed to air dry for 2 minutes after pretreatment, and the adhesive was applied to the treated
surfaces of the plates with a brush and dried for 1 minute.
The flexural strength of the specimens was measured using a 3-point bending test in a universal testing machine
(Lloyd LRX; Lloyd Instruments) with a 1000-N load
cell and a crosshead speed of 5 mm/min (Fig. 2 B).
The flexural strength of each specimen unit was determined using the formula:
S
3WL
2bd2
RESULTS
The mean amount of radiotracer adhesion to the
outer surface of the PMMA blocks used to determine
the OSC value was 7400 6 100 x-ray counts. The
mean microleakage values of the groups from which
the OSC value was subtracted are given in Table III.
The 1-way ANOVA (Table IV) indicated significant differences between the groups (P,.001). The lowest microleakage occurred for the group M180 specimens
(30,000 x-ray counts) and the highest, for the control
147
SARAC ET AL
Group
Group
Group
Group
Group
Group
Group
Mean
C
A 30
A 45
M 180
MC 5
MC 15
MC 30
1.44
2.10
1.57
2.22
1.59
2.05
1.74
SD
0.07
0.03
0.05
0.04
0.45
0.06
0.06
b
a
a
b
Same lower case letter indicates mean values of groups were not statistically
different (P..05).
Group
Group
Group
Group
Group
Group
Group
C
A30
A45
M180
MC5
MC15
MC30
Adhesive
Cohesive
Mixed
2
4
3
2
3
5
5
Between groups
Within groups
Total
Sum of squares
df
Mean square
Sig.
3.336
.095
3.431
6
35
41
.556
.003
205
.001
Group
Group
Group
Group
Group
Group
Group
Mean
C
A 30
A 45
M 180
MC 5
MC 15
MC 30
75.7
71.5
65.0
70.6
73.1
72.5
68.5
SD
0.9
1.4
1.2
1.1
0.8
0.5
0.7
a,b
a
b
b
Same lower case letter indicates mean values of groups were not statistically
different (P..05).
Between groups
Within groups
Total
Sum of squares
df
Mean square
Sig.
501
40
541
6
42
48
83
.96
87
.001
SARAC ET AL
Fig. 3. SEM micrographs of acrylic denture base resin surfaces after treatment. A, Untreated (control). B, Treated with acetone for
30 seconds. C, Treated with acetone for 45 seconds. D, Treated with MMA for 180 seconds. E, Treated with methylene chloride
for 5 seconds. F, Treated with methylene chloride for 15 seconds. G, Treated with methylene chloride for 30 seconds. Original
magnification 32000; bar, 10 mm.
DISCUSSION
The results of this study support the hypothesis that
the duration of the application or the type of chemical etchants would have different effects on the bond
strength of the silicone-based resilient liner to denture
base resin and on the amount of microleakage between
the 2 materials. The control groups for the microleakage
and tensile strength tests showed significantly higher
microleakage and lower bond strength values than the
experimental groups (P,.001).
Several factors may affect the bond between the resilient lining materials and the denture bases, such as aging
in water, use of adhesive, and the nature of the denture
base material.2 When the resilient lining material absorbs water, stress occurs between the bonding surfaces
and the viscoelastic properties of the resilient liners
change.21 The material becomes brittle and transfers
the external loads to the bond area.2 To simulate these
natural conditions in the present study, the specimens
of the microleakage and tensile bond strength test
were thermal cycled.
Bonding between the denture base resin and siliconebased lining material relies completely on the adhesive, a
solvent that dissolves the denture base resin surface,
such as acrylic resin monomer.4 The results of the present study showed that the application of different
chemical etchants increased the bond strength of silicone-based resilient denture lining material to denture
base resin, compared to the control group. Among the
experimental groups, the highest bond strength was
FEBRUARY 2006
treatments reduced the microleakage between the denture base resin and silicone-based denture lining material compared to untreated control specimens. The
swelling of the outer denture base by chemical etchants
and the penetration of the adhesive that resulted in a reduction of the leakage of fluids within this interface was
shown to be an effective procedure compared to the untreated specimens. Sarac et al15 used APA and MMA as a
denture base surface treatment and reported that wetting the denture base surface with MMA and a subsequent reduction of fluid leakage within the interface
was more effective than either an airborne-particleabraded surface or the use of only an adhesive application. Using MMA and adhesive together may effectively
increase the dissolution of the denture base resin surface
prior to resilient liner application.15 This study showed
that the lowest microleakage value was also obtained
with the 180 second MMA treatment (30,000 x-ray
counts).
The chemical etchants make the denture base resin
surfaces porous by dissolving the latter and create a
type of mechanical interlocking structure between the
2 materials.16,19 The type of chemical etchants and the
duration of application are important parameters for
a more effective bond between the 2 materials.
Methylene chloride application for 15 seconds was a
nearly equally effective chemical etchant, increasing
the bond strength and reducing the microleakage in
an almost comparable fashion to that of the 180-second
MMA treatment.
The comparison of the bond strength values obtained
by 3 different methylene chloride application times has
shown that the 15-second application significantly increased the bond strength compared to the 5- and 30second applications. However, no significant difference
between the microleakage results of the 3 groups was
observed. This can be explained, in part, with SEM
photomicrographs. A 15-second methylene chloride
application created the most suitable surface structure
smoother than the 30-second application and more
irregular than the 5-second application.
Resilient liners exert significant influence on the associated denture bases. As the thickness of a resilient liner
is increased, the thickness of the accompanying denture
base must be decreased, which results in decreased denture base strength.4 Furthermore, materials used in conjunction with resilient liners, such as adhesives and
monomers, may cause partial dissolution of the accompanying denture base. The resultant decrease in base
strength may cause fracture during clinical service. In
the present study, flexural strength testing was used to
investigate the effect of chemical surface treatments on
the strength of the denture base. The outcome demonstrated that chemical treatments significantly decreased
the strength of the denture base, compared to the control. The highest flexural strength was obtained with the
150
SARAC ET AL
CONCLUSION
Within the limitations of this in vitro study, the following conclusions were drawn:
1. Treating a denture base resin surface with chemical
etchants significantly increased the bond strength of
a silicone-based resilient denture liner to a denture
base (P,.001) and decreased the microleakage between
the 2 materials (P,.0001). Considering the results of
both tests together, the use of methyl methacrylate for
180 seconds was found to be the most effective chemical
treatment overall (P,.001).
2. The results for methylene chloride and acetone application were also found to be similar to methyl methacrylate (P..05). The 15- and 30-second applications,
respectively, were the most effective.
3. All chemical treatments performed in this study
significantly decreased the flexural strength of acrylic
resin compared to the untreated group (P,.001).
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3. Garcia RM, Leon BT, Oliveira VB, Del Bel Cury AA. Effect of a denture
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11th ed. St. Louis: Elsevier; 2003. p. 751-3.
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bond strength of six silicone-based, resilient liners. J Prosthet Dent
2003;89:303-10.
VOLUME 95 NUMBER 2
SARAC ET AL
FEBRUARY 2006
22. Arena CA, Evans DB, Hilton TJ. A comparison of bond strengths among
chairside hard reline materials. J Prosthet Dent 1993;70:126-31.
23. Rached RN, Del-Bel Cury AA. Heat-cured acrylic resin repaired with
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J Prosthet Dent 2004;92:79-82.
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woven metal and glass fiber: effect of methylene chloride pretreatment.
J Prosthet Dent 2001;85:496-500.
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27. International Organization for Standardization. ISO 1567: 1999. Dentistrydenture base polymers. Available at: http://www.iso.ch/iso/en/
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Reprint requests to:
DR DUYGU SARAC
ONDOKUZ MAYIS UNIVERSITESI
DIS HEKIMLIGI FAKULTESI
PROTETIK DIS TEDAVISI A.D.
55139 KURUPELIT
SAMSUN
TURKEY
FAX: 190 362 457 60 32
E-MAIL: dsarac@omu.edu.tr
0022-3913/$32.00
Copyright 2006 by The Editorial Council of The Journal of Prosthetic
Dentistry.
doi:10.1016/j.prosdent.2005.11.012
151