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Effect of storage duration on the

hardness and tensile bond strength of


silicone- and acrylic resin-based resilient
denture liners to a processed denture
base acrylic resin
Ayse Mese, DDS, PhD,a and Kahraman G. Guzel, DDS, PhDb
Dicle University, Dental Faculty, Diyarbakir, Turkey
Statement of problem. Two potential problems commonly identified with a denture base incorporating a resilient
liner are a failure of the bond between the acrylic resin and resilient liner material and a loss of resiliency of the resilient liner material over time.
Purpose. This investigation evaluated the effect of storage duration on the tensile bond strength and hardness of
acrylic resin- and silicone-based resilient liners that were either heat- or autopolymerized onto denture base acrylic
resin.
Material and methods. The denture liners investigated were a definitive acrylic resin-based heat-polymerized (Vertex
Soft), interim acrylic resin-based autopolymerized (Coe-Soft), definitive silicone-based heat-polymerized (MolloplastB), and definitive silicone-based autopolymerized (Mollosil Plus) resilient liner. The resilient liners were processed according to manufacturers instructions. The resilient liner specimens for tensile bond strength testing (n=10) were 10
x 10 x 3 mm and were processed between 2 polymethyl methacrylate (PMMA) (Meliodent) blocks (40 x 10 x 10 mm).
The resilient liner specimens for hardness testing (n=10) were 20 mm in diameter and 12 mm in height. Specimen
shape and liner thickness were standardized. Specimens were stored for 1 day, 1 week, or 1, 3, or 6 months in water
at 37C. Tensile bond strength was measured in a universal testing machine at a crosshead speed of 20 mm/min, and
hardness was measured using a Shore A durometer. Two-way ANOVA and Tukey HSD tests were used to analyze the
data (=.05).
Results. The results indicated that there were significant differences both in the hardness and bond strength values of
resilient liner materials. The definitive silicone-based heat-polymerized (Molloplast-B) resilient liner had significantly
higher bond strength and lower hardness values than the others. Prolonged exposure to water produced significantly
higher hardness values and lower bond strength values.
Conclusions. Within the limitations of this in vitro study, specimens of resilient liners immersed in water demonstrated
significantly (P<.001) lower bond strength values and higher hardness values over time. (J Prosthet Dent 2008;99:153159)

Clinical Implications

The negative effect of the higher hardness values on tensile bond


strength was greatest with the acrylic resin-based, autopolymerized
resilient liner tested, which suggests that the use of this resilient
liner may not provide long-term clinical success.

Resilient denture liner materials


are applied to the intaglio surface of
dentures to achieve more equal force
distribution, reduce localized pressure, and improve denture retention
by engaging undercuts.1,2 Ideal prop-

erties of resilient liners include resiliency, which is desired over a long period of time, and a good bond to the
denture base.3
Resilient denture liners have been
used in dentistry for more than a cen-

Assistant Professor, Department of Prosthodontics.


Professor, Department of Prosthodontics.

Mese and Guzel

tury; the earliest resilient liners were


made from natural rubber.4 One of the
first synthetic resins used as a resilient
liner, a plasticized polyvinyl resin, was
developed in 1945.4 Silicone-based
materials were introduced in 1958.4

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Volume 99 Issue 2
Contemporary resilient liner materials can be divided into 2 groups:
acrylic resin-based and siliconebased.1,4 Both groups are available
in autopolymerized or heat-polymerized forms.1 Autopolymerized resilient
liner materials allow the clinician to
reline a removable denture directly,
intraorally. This method is faster than
using heat-polymerized (laboratoryprocessed) systems, and a patient is
not without the prosthesis during the
time required for laboratory procedures.5 However, it is difficult to produce liner materials of the optimum
thickness with the autopolymerized
technique.6 The optimum thickness
has been reported as approximately
2.5 to 3 mm, which is needed to provide good shock absorption.7,8
Acrylic resin-based resilient liner
materials generally consist of polymers and monomers. The composition of the polymers and monomers is
proprietary, but these materials generally include methacrylate polymers
and copolymers, along with a liquid
containing methacrylate monomer
and plasticizers (ethyl alcohol and/or
phthalate).9 These materials undergo
2 processes when immersed in water:
the leaching of plasticizers and other
soluble materials into the water and
the absorption of water by the polymer.9-11 It has been suggested that
the initial softness of the plasticized
acrylic resins results from the plasticizer, which is also responsible for
maintaining material softness.10,11
The plasticizer lowers the glass transition temperature of the polymer to
a value below mouth temperature so
that the modulus of elasticity of the
resilient material is reduced to a satisfactory level.9 Silicone-based resilient
liner materials are similar in composition to silicone-type impression materials, as they are dimethylsiloxane
polymers.12 Polydimethyl siloxane is a
viscous liquid that can be cross-linked
to form an elastic rubber. No plasticizer is necessary to produce a softening effect with this material.12
Definitive and interim resilient
denture liners have differing uses and

should be selected based on the desired service time of the material. Interim resilient liners are acrylic resinbased and may harden at a faster rate
than definitive materials, but they
have other advantages, such as superior elastic quality. Therefore, interim
liners are widely used as tissue conditioners or temporary relines.13
There are several problems associated with the use of resilient denture
liners, including bond failure between
the liner and denture base, colonization by Candida albicans, porosity,
poor tear strength, and loss of softness.2 One of the most serious problems with these materials is bond
failure between the resilient denture
liner and denture base.14 Bond failure
creates a potential surface for bacterial growth, and plaque and calculus
formation.2 Any favorable properties
of a denture liner are useless in the absence of a good bond to the denture
base material. A variety of parameters
affect the bond between the resilient
lining materials and the denture base,
including water absorption, surface
primer use, and denture base composition.15 There are reports on the
bond strength of resilient liners bonded to denture base resin using different methods, such as peel, shear, or
tensile tests.16-27
Long-term softness is another desirable property of resilient liners. Loss
of softness can result in the delivery of
greater occlusal forces to the underlying mucosa and increased clinical
complaints.28 The liner should also
resist the absorption of oral fluids
as well as the release of ethanol and
plasticizer into the saliva. The release
of unpolymerized or soluble products could result in a stiffer, harder
liner material over time. A liner with
a greater degree of conversion, that
is, greater monomer incorporated
into the polymer, would likely demonstrate less absorption and solubility and more stable properties over
time.29-34 This study was performed to
assess the denture base bond strength
and hardness of acrylic resin-based
definitive (Vertex Soft) and interim

The Journal of Prosthetic Dentistry

(Coe-Soft), and silicone-based definitive (Molloplast-B, Mollosil Plus) resilient liners that were either heat- or
autopolymerized. The null hypothesis
was that chemical composition and
immersion time have no effect on
bond strength or hardness of resilient
denture liners.

MATERIAL AND METHODS


Four commonly used commercial
resilient liner materials, including 2
types based on chemical composition
(acrylic resin- and silicone-based),
were selected for investigation. Specimens of all materials were prepared
according to the manufacturers instructions. The resilient liner materials
and denture base resin used are listed
in Table I. Ten rectangular specimens
with a cross-sectional area of 10 x 10
mm2 were prepared for each group
using a heat-polymerized polymethyl
methacrylate (PMMA) denture base
material. Two rectangular PMMA
plates were made by investing brass
dies with a 3-mm-thick spacer in a
conventional denture flask (Teledyne
Hanau, Buffalo, NY). All dies and
spacers were prepared to the same dimensions to standardize the shape of
the denture base blocks and the thickness of the resilient denture liners.
The dies and spacers were invested in hard, but flexible, silicone rubber (Lastic Xtra; Kettenbach, Eschenburg, Germany) to facilitate removal
of the processed specimens from the
flask. Specimens were fabricated by
processing the resilient denture liners
against polymerized PMMA blocks.
The acrylic resin denture base was
prepared by mixing polymer and
monomer for 1 minute, packing it
into the mold with a brass spacer, and
processing in a water bath at 100C
for 30 minutes. After this process, the
2 polymerized PMMA specimens were
removed from the flask and trimmed,
and the surfaces that were to be
bonded were smoothed using 240grit silicone carbide paper (Waterproof Silicone Carbide Paper; A166
Grade P400; English Abrasives and

Mese and Guzel

155

February 2008

Table I. Resilient liner materials and denture base material tested


Type of Polymerization
(Polymer : Monomer Ratio)

Manufacturer

Lot No.

Meliodent

Conventional (heat-polymerized)
denture base polymer (23.4 g:10 ml)

Heraeus Kulzer,
Hanau, Germany

012087

Vertex Soft

Heat-polymerized acrylic
resin-based resilient liner (2:1)

Vertex-Dental BV,
Zeist, The Netherlands

100001

Autopolymerized acrylic
resin-based resilient liner (1.5 g:8 ml)

GC America,
Alsip, Ill

0101292

Molloplast-B

Heat-polymerized silicone-based
resilient liner

Detax GmbH & Co KG,


Ettlingen, Germany

010527

Mollosil Plus

Autopolymerized silicone-based
resilient liner

Detax GmbH & Co KG

001003

Product

Coe-Soft

Chemicals Ltd, London, England).


For Molloplast-B, the provided adhesive (Primo) was applied and allowed
to dry for 60 minutes. For Mollosil
Plus, alcohol (Isopropanol 99.7%;
VOCO, Cuxhaven, Germany) was applied to the surfaces, followed by the
adhesive (Primer), which was allowed
to dry for 1 minute. No adhesive was
necessary for the acrylic resin-based
resilient liner materials.
The brass spacers were then removed from the flask. The PMMA
blocks were replaced in the mold
and the resilient denture liner materials were packed into the space left
by the brass spacers, trial packed,
and polymerized. For Vertex Soft, the
polymer-monomer was mixed for 60
seconds and placed in the flasks. The
flasks were placed under pressure in
a standard flask press (No. 01001;
Teledyne Hanau) for 15 minutes, and
immersed in a water bath for 3 hours
at 70C, followed by 30 minutes at
100C. For Coe-Soft, the polymermonomer was mixed, placed in the
flasks, and the flasks were placed under pressure in the flask press for 15
minutes. With Molloplast-B polymerization, the flasks were placed under
pressure in the flask press for 15 minutes, and then immersed in a water
bath for 2 hours at 100C. With Mol-

Mese and Guzel

losil Plus polymerization, the flasks


were placed under pressure in the
flask press for 30 minutes.
After polymerization, the specimens were removed from the flask
and trimmed with a sharp blade
(No:15; Wuxi Xinda Medical Device
Co, Ltd, Jiangsu, China). Each group
(n=10) of specimens was stored in
water at 37C for 1 day, 1 week, or
1, 3, or 6 months. For the tensile test,
specimens were placed under tension
until failure in a universal testing machine (Testometric Micro 500, Type
U4000; Maywood Instruments Ltd,
Basingstoke Hants, England), with a
crosshead speed of 20 mm/min. Bond
strength was calculated as maximum
load (N) divided by the cross-sectional area (mm2) of the specimen and recorded in megapascals (MPa).
For the hardness test, 10 cylindrical wax (National Dental Supplies Ltd,
Southport, UK) specimens (20 mm in
diameter and 12 mm in height) were
prepared for each group by investing brass dies for each group. All wax
specimens were invested in a mold
in the flasks, as previously described.
After elimination of the wax, the resilient liner materials were mixed,
packed into the flasks, trial packed,
and polymerized according to the
manufacturers instructions. After po-

lymerization, each resilient liner specimen was removed from the flask and
trimmed with a sharp blade (No: 15;
Wuxi Xinda Medical Device Co, Ltd).
Each group (n=10) of specimens was
stored in water at 37C for 1 day, 1
week, or 1, 3, or 6 months. Hardness
was determined using a Shore A durometer tester (The Shore Instrument
& Mfg Co Inc, Freeport, NY), which
was calibrated according to ASTM
D2240, and recorded in Shore units.
The differences in the bond strength
and hardness of each resilient liner
material were determined for the 5
test periods and were evaluated statistically using a 2-way ANOVA and the
Tukey HSD post hoc test. All statistical testing was performed at a preset
alpha level of .05.

RESULTS
There were significant interactions
between materials and time periods
with respect to both bond strength
and hardness, as shown by the 2-way
ANOVA (Tables II and III). Mean and
standard deviation values of bond
strength and hardness of resilient
liner materials for the 5 time intervals
are given in Table IV. There were significant differences in bond strength
between the materials at each time

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Volume 99 Issue 2

Table II. Two-way ANOVA results for comparison of bond strength values
SS

df

MS

Group

134.92

44.97

376.29

<.001

Time

19.51

4.88

40.80

<.001

Group x time

1.13

12

.84

7.06

<.001

Error

21.39

179

.12

Total

492.77

199

Source

Table III. Two-way ANOVA results for comparison of hardness values


SS

df

MS

Group

31248.98

10416.33

2763.61

<.001

Time

1890.30

472.58

125.38

<.001

Group x time

935.76

12

77.98

20.69

<.001

Error

678.44

180

3.77

Total

307777.03

200

Source

Table IV. Mean (SD) values of tensile bond strength (MPa) and hardness (Shore units) of resilient liner materials for
5 time intervals (n=10)

Bond Strength

Hardness

Vertex
Soft

CoeSoft

MolloplastB

Mollosil
Plus

Vertex
Soft

CoeSoft

MolloplastB

Mollosil
Plus

1 day

3.50Ca(0.44)

0.45Cb(0.18)

1.58Cc(0.19)

1.20Bd(0.41)

49.08Aa(1.34)

12.37Ab(0.81)

42.28Ac(0.89)

29.33Ad(1.43)

1 week

3.07Ca(0.46)

0.39Cb(0.04)

1.42BCc(0.31)

1.12Bd(0.19)

49.38Aa(1.15)

17.82Bb(1.45)

42.42Ac(1.46)

29.60ABd(2.46)

1 month

2.57Ba(0.29)

0.23Bb(0.05)

1.16ABc(0.12)

1.07Bd(0.58)

51.22Aa(2.98)

20.88Cb(1.31)

43.02Ac(1.44)

31.06Bd(0.87)

3 months

1.91Aa(0.71)

0.22Bb(0.04)

1.10ABc(0.53)

0.77Ad(0.15)

50.88Aa(4.48) 23.01Db(1.43)

43.78Ac(1.84)

33.94Cd(1.26)

6 months

1.70Aa(0.46)

0.11Ab(0.01)

1.03Ac(0.44)

0.50Ad(0.22)

64.08Ba(2.83) 24.02Db(1.28)

46.16Bc(2.15)

34.64Cd(2.06)

Different superscripted uppercase letters indicate statistically different means within each column (P<.001).
Different superscripted lowercase letters indicate statistically different means within each row (P<.001).

period (Table IV). The results of the


bond strength test demonstrated
that the mean bond strength values
(SD) of the heat-polymerized resilient
liners after 1 day (3.50 (0.44) MPa;
1.58 (0.19) MPa) were significantly
(P<.001) greater than those of autopolymerized liners (0.45 (0.18) MPa;
1.20 (0.14) MPa) in both the acrylic

resin- and silicone-based groups, respectively. Considering each material separately, the differences in bond
strength with respect to time are also
shown in Table IV. For Vertex Soft,
there were significant differences in
bond strength values between 1 week
and 1 month and also between 1
month and 3 months. For Coe-Soft,

The Journal of Prosthetic Dentistry

there were significant differences between 1 week and 1 month and also
between 3 months and 6 months. For
Molloplast-B, significant differences
were observed between 1 day and 1
month, and also between 1 day and
6 months. For Mollosil Plus, there
was a significant difference between 1
month and 3 months.

Mese and Guzel

157

February 2008
The highest bond strength was observed for specimens stored in water
for 24 hours, followed by specimens
stored for 1 week. The bond strength
values of the specimens became lower
as the storage time increased. The
lowest bond strength values for all
resilient liner materials were observed
after 6 months of storage. With respect to the different types of material, the reduction was greater in the
autopolymerized versus heat-polymerized resilient liner materials (1.59
MPa). The mean bond strength (SD)
of acrylic resin-based resilient liners
(3.50 (0.44) MPa) was significantly
greater than that of silicone-based
liners (1.58 (0.19) MPa) in the heatpolymerized category after 1 day. The
change in bond strength over time for
the acrylic resin-based resilient liner
materials was greater than that of the
silicone-based liners materials (1.59
MPa) within both the heat- and autopolymerized groups.
There were significant differences
in hardness between the materials at
each time period, as shown in Table
IV. The results of the hardness test
demonstrated that the mean hardness
(SD) of the heat-polymerized resilient
liners after 1 day (49.08 (1.34) Shore;
42.28 (0.89) Shore) was significantly
(P<.001) greater than that of autopolymerized liners (12.37 (0.81) Shore;
29.33 (1.43) Shore) in the acrylic
resin- and silicone-based groups, respectively. Differences in hardness
for each material over time are also
shown in Table IV. For Vertex Soft and
Molloplast-B, there was a significant
difference between 3 months and
6 months. For Coe-Soft, there were
significant differences between 1 day
and 1 week, 1 week and 1 month, and
also between 1 month and 3 months.
For Mollosil Plus, there were significant differences between 1 day and
1 month, 1 month and 3 months,
and also between 3 months and 6
months.
The lowest hardness values were
seen in the specimens stored in the
water for 24 hours, followed by the
specimens stored for 1 week. Hard-

Mese and Guzel

ness values of the specimens were


higher as the storage time increased.
The highest hardness values for all resilient liner materials were observed
after 6 months of storage. Considering the different types of material, the
change was greater in the autopolymerized versus the heat-polymerized
resilient liner materials (40.06 Shore).
The mean hardness (SD) of acrylic resin-based resilient liners (49.08 (1.34)
Shore) was significantly greater than
that of silicone-based liners (42.28
(0.89) Shore) within the heat-polymerized group at day 1. The change in
hardness over time for the acrylic resin-based resilient liner materials was
greater than for the silicone-based
liner materials (17.92 Shore) within
both the heat- and autopolymerized
groups.

DISCUSSION
The results of the study support rejection of the null hypothesis because
chemical composition and immersion
time affected both the bond strength
and hardness of the resilient denture
liners examined. Adequate softness of
resilient liner materials and sufficient
bond strength between the resilient
denture liners and denture base material are required for long-term clinical
use.2,15,28 As reported in other studies,
bond strength and softness values of
resilient denture liners were found to
vary according to chemical composition.1,19,26,28
In the current study, the bond
strength of 4 resilient denture liners was determined by a tensile test,
and softness of the resilient denture
liners was measured as resistance to
indentation in a material for the 5
test periods. These tests apply different forces than those to which the
resilient denture lining materials are
subjected clinically; however, this in
vitro study could provide preliminary
information regarding the materials,
based on bond strength and hardness
test results.
The definitive heat-polymerized
acrylic resin-based Vertex Soft liner

had the greatest bond strength compared with the other materials at 24
hours, because the chemical composition of Vertex Soft is similar to
that of the PMMA denture base polymer.26 This result is in agreement with
those of others,3,13,15-17 who reported
that heat-polymerized acrylic resinbased resilient liner materials have
the greatest bond strengths to acrylic
resin-based dentures. Related to similar chemical compositions, a chemical bond forms between the acrylic
resin-based liners and the PMMA
denture base polymer.3 Since silicone
liners have little or no chemical bond
to PMMA, an adhesive is needed to
bond the liner to the polymerized
denture base. Consequently, the bond
strength of silicone denture base liners depends on the tensile strength of
the liner materials, as well as the adhesive used.19
The interim autopolymerized
acrylic resin-based Coe-Soft liner has
a similar chemical composition to
PMMA, but it demonstrated the lowest bond strength at day 1, which was
in agreement with the findings of Sertgoz and Aydin.19,20 This result indicated that heat-polymerized liners have a
greater bond strength than autopolymerized products. This may have been
due to the mode of polymerization of
this resilient liner material.
The bond strength values of all
the resilient liner materials were lower
with increasing duration of immersion. These results agree with those
of other investigators,14,21,22 who suggested that water storage reduced resilient liner bond strength. The lower
bond strength may result from the
swelling and stress formation at the
bond interface, or from a change in
the viscoelastic properties of the liner,
rendering the material stiffer and better able to transmit external loads to
the bond site.
The acrylic resin-based liners
demonstrated a greater reduction in
bonding strength values compared
to the silicone products during the 6month immersion test. These findings
support those of Jepson25 and Mese,26

158

Volume 99 Issue 2
who reported that water storage reduced the liner strength of acrylic
resin-based products more than that
of silicone-based products. Moreover,
the bond strength values of autopolymerized products showed greater
reduction than those of heat-polymerized materials over the course of the
current study. These findings agree
with those of Mese26 and Waters,27
who reported that water storage reduces the bond strength of autopolymerized liners more than that of heatpolymerized materials.
The definitive heat-polymerized
acrylic resin-based Vertex Soft liner
had the greatest hardness compared
with the other materials at 24 hours
after immersion. These results concur
with those of Dootz,17,24 who suggested that heat-polymerized acrylic resin-based resilient liner materials have
the greatest hardness. Vertex Soft liner
and heat-polymerized silicone-based
Molloplast-B liner were harder than
the interim autopolymerized acrylic
resin-based Coe-Soft liner and definitive autopolymerized silicone-based
Mollosil Plus liner. The results confirm
those of Polyzois1 and Gregory,34 who
reported that heat-polymerized liners are harder than autopolymerized
products.
The hardness values of all the resilient liner materials evaluated were
higher with increased duration of
immersion. The hardness values of
the acrylic resin-based Vertex Soft
and Coe-Soft liners showed greater
change than those of the silicone
products. The results of the current
study are in agreement with those of
other researchers,30-32 who reported
that water storage increased resilient
liner hardness in acrylic resin-based
products more than in silicone-based
products. The initial softness was due
to the quantity of plasticizer in the liquid, since plasticizers are responsible
for maintaining the softness of the
acrylic resin-based resilient liner materials. Leaching of plasticizers causes
hardening of the acrylic resin-based
resilient liners as the duration of immersion increases.7,10 Silicone-based

resilient liners have superior elastic recovery, and their softness is controlled
by the amount of cross-linking in the
rubber; thus, no plasticizer is necessary to produce a softening effect.1 In
addition, the hardness values of the
Coe-Soft and Mollosil Plus liners demonstrated greater change than those
of the Vertex Soft and Molloplast-B
liners over the duration of the current
study. These findings agree with those
of Qudah12 and Hekimoglu,33 who
reported that the mechanical properties of autopolymerized resilient liners
are affected more by immersion compared with heat-polymerized resilient
liner materials.
According to the results of the present study, hardness values of resilient
liner materials were higher in conjunction with increased duration of water
storage, but bond strength values
were lower. Factors such as processing methods, water absorption, and
bonding agents require further investigation to predict which materials will
provide the best clinical service. Hardness, weight change, tensile strength,
tear strength, and color stability are
additional properties of resilient denture liners that warrant investigation.
Selection of a particular liner cannot
be based on any single property. Material selection is influenced not only
by the properties offered but also by
the particular treatment situation.
The results of the present investigation support a common trend
reported in previous studies14,16,18,25;
namely, heat-polymerized siliconebased resilient liners have more optimal properties. Heat-polymerized
acrylic resin-based resilient liners
have good properties initially, but deteriorate with long-term use, and autopolymerized resilient liners have a
useful, but limited, role. However, further investigation is needed for longer
periods, along with clinical studies
to assess whether other physical or
chemical properties are influenced by
the processing procedure or time involved.

The Journal of Prosthetic Dentistry

CONCLUSIONS
Within the limitations of this
study, the 4 resilient liners tested demonstrated significantly higher hardness values, to varying degrees, after
water immersion, according to their
chemical compositions and increased
immersion time. Furthermore, bond
strength values of the resilient liner
materials were significantly lower over
time.

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Corresponding author:
Dr Ayse Mese
Dicle niversitesi
Dishekimligi Fakltesi Protez Blm
Diyarbakr
TURKEY
Fax: 0090412-2488100
E-mail: amese@dicle.edu.tr
Acknowledgements
The authors thank Professor Ensar Baspinar,
Yuzuncu Yil University, Biostatistic Department, Van, Turkey, for providing statistical
consultation.
Copyright 2008 by the Editorial Council for
The Journal of Prosthetic Dentistry.