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© 2016 Indian Journal of Dental Research | Published by Wolters Kluwer - Medknow288
Comparative study of sorption and solubility of heat‑cure
and self‑cure acrylic resins in different solutions
Rajesh Saini, Ravindra Kotian, Prashanthi Madhyastha, Srikant N1
ABSTRACT
Objective: The objective of this study was to compare the sorption and solubility of heat‑cure
and self‑cure acrylic resins in different solutions.
Materials and Methods: One heat‑cure acrylic resin (Trevalon) and one self‑cure acrylic resin
(Rapid Repair) were studied. Five groups of square‑shaped specimens (20 mm × 20 mm ×
2 mm) were prepared for each acrylic resin and then immersed in five solutions: distilled water,
artificial saliva, denture cleansing solution, distilled water, and denture cleaning solution for 12 h
alternatively, artificial saliva and denture cleaning solution for 12 h alternatively at 37 ± 2°C, and
tested sorption and solubility by weight gain/loss method, respectively, after 1, 6, and 11 weeks.
The data were analyzed by one‑way analysis of variance followed by post hoc Tukey’s test.
Results: Water sorption mean values varied from 17.5 ± 0.88 to 27.25 ± 1.04 μg/mm3
for heat
cure and from 12.75 ± 0.55 to 19.75 ± 1.04 μg/mm3
for self‑cure in the different solutions
after different interval periods of 1, 6, and 11 weeks. These values were statistically significant
(P < 0.001). Water solubility mean values varied from 0.25 ± 0.55 to 1.5 ± 0.55 μg/mm3
for
heat cure and from 1.5 ± 0.55 to 6.5 ± 0.55 μg/mm3
for self‑cure in the different solutions after
different interval periods of 1, 6, and 11 weeks. These values were statistically not significant
(P > 0.05). There was no linear correlation between sorption and solubility values. Overall,
analysis of results showed the maximum sorption value in denture cleansing solution followed
by alternative soaking in distilled water and artificial saliva. Least sorption was observed with
artificial saliva followed by distilled water.
Conclusion: Both heat‑cure and self‑cure acrylic resins showed varying water sorption and
solubility. The results of both water sorption and solubility showed compliance with the
International Standards Organization specification. No correlation was found between water
sorption and solubility. Artificial saliva solution is a better storage medium than distilled water
and denture cleansing solution for both heat‑cure and self‑cure acrylic resins.
Key words: Acrylic resin, heat‑cure acrylic, self‑cure acrylic, solubility, water sorption
Address for correspondence:
Dr. Ravindra Kotian
E‑mail: ravindrakotian@yahoo.co.in
sorption and release, which causes dimensional instability,
thereby subjecting the material to internal stresses that
may result in crack formation and eventually fractures of
the denture.[1,2]
Acrylic resins absorb water slowly over a period of time.
This imbibition is due primarily to the polar properties of
the resin molecules.[3,4]
Sorption of material represents the
Acrylic resin is the most utilized material in partial
removable and complete denture bases and facings for fixed
bridges to improve the esthetic value of the restoration.
Prediction of the service life of acrylic resin material
is difficult since many environmental factors affect the
durability. One of the properties of acrylic resins is water
Original Research
Departments of Dental Materials
and 1
Oral Pathology, Manipal
College of Dental Sciences,
Manipal University, Mangalore,
Karnataka, India
Received	 : 10‑06‑14
Review completed	 : 05‑07‑14
Accepted	 : 28-04-16
Access this article online
Quick Response Code: Website:
www.ijdr.in
PMID:
***
DOI:
10.4103/0970-9290.186234
How to cite this article: Saini R, Kotian R, Madhyastha P, Srikant N.
Comparative study of sorption and solubility of heat-cure and self-cure acrylic
resins in different solutions. Indian J Dent Res 2016;27:288-94.
This is an open access article distributed under the terms of the Creative
Commons Attribution‑NonCommercial‑ShareAlike 3.0 License, which allows
others to remix, tweak, and build upon the work non‑commercially, as long as the
author is credited and the new creations are licensed under the identical terms.
For reprints contact: reprints@medknow.com
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Comparison of sorption and solubility of acrylic resins Saini, et al.
289Indian Journal of Dental Research, 27(3), 2016
amounts of water adsorbed on the surface and absorbed
into the body of the material during fabrication or while
the restoration is in service. Since both adsorption and
absorption are involved, the term sorption is generally used
to include the total phenomena. Usually, a serious warpage
and dimensional change in the material are associated with
a high percentage of water sorption.[5]
Dimensional change that occurs on prostheses as a result
of water absorption of acrylic is an alternate event. If the
prosthesis is left in open air and a dry place, it allows water
to leave its structure and undergoes contraction. Therefore,
for patients using removable prostheses, it is recommended
to store the prosthesis in water when they are not in use.
The water absorbed into the material acts as a plasticizer
and decreases the mechanical properties such as hardness,
transverse strength, and fatigue limit.[6,7]
According to the rules of diffusion, water sorption can be
explained in the diffusion forces of the resin molecules to
separate from each other. This, in turn, creates an expansion
in size with water helping to relax the stresses with the
acrylic resin.[8]
Solubility represents the mass of the soluble materials from
polymers. The only soluble materials present in denture
base resins are initiators, plasticizers, and free monomer.
Any observed loss of weight of the resin is the measure of
the specimen’s solubility. Therefore, the water sorption
and solubility are the critical problems that affect the
durability.[9]
Takahashi et al.[10]
found that water molecules spread
between the macromolecules of the material, forcing them
apart. This behavior affects the dimensional behavior and
denture stability; therefore, water sorption and solubility
of these materials should be as low as possible.[11]
Ideally,
polymer networks should be insoluble materials with
relatively high chemical and thermal stability. However,
most of the monomers used in dental resin materials
can absorb water and chemicals from the environment,
and also release components into the surrounding
environment.
Both water sorption and solubility would lead to a variety
of chemical and physical processes that may result in
deleterious effects on the structure and function of dental
polymers.[12]
Denture base acrylic resins have low solubility,
and the little that occurs is a result of the leaching out
of the traces of unreacted monomer and water‑soluble
additives into the oral fluids. However, these monomers
sometimes produce a soft tissue reaction.[13]
It is important
to determine the residual monomer content and solubility of
the tested materials as these properties influence the allergy
susceptibility of these materials.
The water sorption and solubility were determined
according to the International Standards Organization (ISO)
standards 1567:1999.[14]
According to this specification,
water sorption should not exceed 32 μg/mm3
for heat‑cured
or self‑cured materials. The loss in mass per unit volume
(soluble material) should not exceed 1.6 μg/mm3
for
heat‑cured and 8.0 μg/mm3
for self‑cured materials.[14,15]
Because water sorption and solubility play a very important
role in the clinical and mechanical performance of
acrylic materials, it was, therefore, decided to study these
properties of heat‑cure and self‑cure acrylic resins in
different solutions. The aim of this study was to compare the
sorption/solubility of heat‑cure acrylic resin and self‑cure
acrylic resin in the different solutions after 1 week, 6 weeks,
and 11 weeks.
MATERIALS AND METHODS
In this study, one heat‑cure and one self‑cure acrylic denture
base materials were selected for comparative evaluation of
sorption and solubility in different solutions at different
time intervals. The materials and solutions selected are
given in Table 1.
For the study, 25 samples each with dimensions of 20 mm ×
20 mm × 2 mm were prepared using heat‑cure and self‑cure
acrylic resins separately for the different time intervals.
For each solution, five samples were used. Gypsum molds
were used to prepare the samples by using a preformed wax
pattern of standard dimension.
Gypsum mold preparation
Wax patterns measuring 20 mm in length, 20 mm in width,
and 2 mm in thickness were used to prepare a gypsum mold.
Wax patterns were invested in the dental stone in the base
of the flask. Two coatings of alginate separating media (cold
mold seal) were then applied onto the set dental stone. The
counterpart of the flask was positioned over the base and
filled with dental stone. The flask was placed on top of the
vibrator, taking care not to cause air entrapment.
The flask was clamped immediately to ensure metal‑to‑metal
contact between the base and the counterpart of the flask.
After setting, the wax was removed by immersing in a hot
water bath without damaging the molds. The molds formed
were then flushed with hot water to remove any traces of
residue followed by the application of separating media. The
mold cavities so obtained were used for the preparation of
acrylic resin specimen.
Preparation of Trevalon ‑ heat‑cure acrylic resin
specimen
The appropriate amount of Trevalon (Dentsply India Pvt.,
Ltd., Bangalore, India) heat‑cure acrylic resin required was
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Comparison of sorption and solubility of acrylic resins Saini, et al.
Indian Journal of Dental Research, 27(3), 2016290
prepared from a mixture of polymer and monomer in the
ratio of 3:1 by volume. The monomer was poured into a
mixing jar and the polymer was slowly added to allow for
wetting of the powder. Excess powder was removed. Then,
it was thoroughly mixed for 1 min. After attaining the
dough forming time, the dough was thoroughly kneaded
between the fingers and the mold cavities were filled. The
flask was closed and trial closure was carried out using
flask clamp. The flask was then clamped, and the pressure
was maintained for 30 min to allow proper penetration of
monomer into polymer.
The flask was immersed in an acrylizer (Confident Dental
Equipment Ltd., Bengaluru, Karnataka, India) at room
temperature. The temperature was raised to 74°C for 1.5 h,
and then the temperature of the water bath was increased
to boiling (100°C) for an additional hour.
After the completion of the curing cycle, the flask was
removed from the water bath, bench‑cooled for 30 min,
and immersed in cold water for 15 min prior to deflasking.
The acrylic specimens were then retrieved, finished, and
polished. The dimensions and quality of the specimens were
verified. Twenty‑five specimens of 20 mm × 20 mm × 2 mm
dimension were obtained by this procedure.
Preparation of Rapid Repair ‑ self‑cure acrylic resin
specimen
The appropriate amount of Rapid Repair (Dentsply India,
Pvt., Ltd.) self‑cure acrylic resin required was prepared
from a mixture of polymer and monomer in the ratio of
3:1 by volume, i.e., three parts of polymer and one part
of monomer. The monomer was poured into a mixing jar
and the polymer was slowly added to allow for wetting
of the powder. Excess powder was removed. Then, it was
thoroughly mixed for 1 min. After attaining the dough
forming time, the dough was thoroughly kneaded between
the fingers and the mold cavities were filled. The flask was
closed and trial closure was carried out using flask‑clamp,
and pressure was maintained for 5 min to allow proper
penetration of monomer into polymer.
After the completion of the self‑curing cycle, the flask was
removed from the trial closure. The acrylic specimen was
then retrieved, finished, and polished. The dimensions
and quality of the specimens were verified. Twenty‑five
specimens of 20 cm × 20 cm × 2 mm dimension were
obtained by this procedure.
Method to obtain sorption and solubility
The specimens were stored in different solutions [Table 1]
at 37 ± 2°C and sorption and solubility were tested by
the weight gain/loss method, respectively, after 1, 6, and
11 weeks.
Sorption and solubility were determined by the method
described in the American Dental Association (ADA)
specification 12 for denture base polymers.[16]
Each sample was dried in desiccators containing anhydrous
calcium chloride until a constant weight was obtained. This
was considered to be the initial weight of the specimen
(W1
).
The samples were then immersed in:
•	 Solution 1: Distilled water
•	 Solution 2: Artificial saliva
•	 Solution 3: Denture cleansing solution
•	 Solution 4: Distilled water and denture cleaning solution
for 12 h alternatively
•	 Solution 5: Artificial saliva and denture cleaning solution
for 12 h alternatively.
Of the processed samples, five each for both heat‑cure and
self‑cure were placed in sealed polyethylene containers
each containing different solutions for 1, 6, and 11 weeks
at 37 ± 2°C.
After each time period, respectively, the samples were
removed from their container, excess water was removed
by blotting with filter paper, and the samples were weighed
by an electronic precision balance (Essae Teraoka Limited,
Gurgoan, India) capable of measuring to 0.001 g. This was
the weight of the specimen after absorption (W2
).
The amount of soluble material lost was measured by placing
the specimens back in the desiccators after each sorption
cycle and then weighing them at regular intervals until a
constant weight after desiccation (W3
).
The water sorption and water solubility per unit volume are
determined according to the ISO standards 1567:1999.[14]
Table 1: List of materials, batch number, and manufacturers
Material type Material brand name Batch number Manufacturer
Heat cure acrylic denture base
resin
Trevalon T121037 Dentsply India Pvt. Ltd.
Self‑cure acrylic denture base resin RR R130102 Dentsply India Pvt. Ltd.
AS Wet mouth C12002 ICPA Health Products Ltd.
Denture cleansing tablets Fitty dent FDT13024 Group Pharmaceuticals Ltd.
DW Demineralized water MD112 Medilise Chemicals
RR=Rapid Repair, DW=Distilled water, AS=Artificial saliva
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Comparison of sorption and solubility of acrylic resins Saini, et al.
291Indian Journal of Dental Research, 27(3), 2016
(μg/mm3
) sorption: W2
− W3
/VSample
(μg/mm3
) solubility: W1
− W3
/VSample
VSample
= 20 mm × 20 mm × 2 mm = 800 mm3
W1
= The initial weight
W2
= The weight after absorption
W3
= The final weight after desiccation.
The above procedure was repeated, and sorption and
solubility data were collected for 1, 6, and 11 weeks. Mean
values and standard deviation of both sorption and solubility
were calculated. Mean values were compared statistically
with one‑way analysis of variance (ANOVA) followed by
post hoc Tukey’s test to determine the significant differences
among the groups at P  0.05 level of significance.
RESULTS
SPSS 20.0 (Version 20, Dentsply India Pvt., Ltd, Bangalore,
India) was used to obtain the statistical results of our study.
One‑way ANOVA test followed by post hoc Tukey’s test
was used to evaluate the sorption and the solubility values
of the heat‑cure and self‑cure resins at a time period of 1,
6, and 11 weeks.
The results of mean and standard deviation are presented
in Tables 2‑4 that show the consolidated results of
ANOVA/post hoc test for sorption of heat‑cured and
self‑cured resins, respectively. Analysis of the results
showed a significant difference in the sorption values
at all time periods as assessed by one‑way ANOVA. No
significant difference was observed in the solubility values
in heat‑cure and self‑cure resins separately. There was no
linear correlation between sorption and solubility values.
According to ANOVA, the type of material, time, and
solution of storage were statistically significant on water
sorption and water solubility (P  0.001).
According to post hoc Tukey’s test, the water solubility
between the time and solution of storage was not statistically
significant (P  0.05).
When the values of water sorption and solubility were
observed according to time, there was a significant
increase in the values of all samples during the 1st
week
of the study.
For heat cure, no linear increase in water sorption was
found during the immersion period of 1 to 11 weeks. Most
of the increase occurred during the first 6 weeks compared
to weeks 6–11 (19.6 ‑ 25.05 ‑ 25.8 ANOVA). Whereas a
linear increase in water sorption was observed in self‑cure
from 1 to 11 weeks (14.3 ‑ 15.75 ‑ 17.85 ANOVA). Water
sorption values for heat cure were significantly higher
than self‑cure in the different interval periods in different
solutions (P  0.001).
Water solubility values for both heat‑cure and self‑cure
resins increased significantly from 1 to 11 weeks in different
solutions (HC 0.25 ‑ 0.85 ‑ 1.4 and SC 1.5 ‑ 4.35 ‑ 6.35
ANOVA). Water solubility values for heat‑cure resins
were markedly less when compared to self‑cure resins in
the different interval periods in different solutions and was
statistically significant (P  0.001).
Table 2: Mean and standard deviation of the samples
Brands Groups Mean (SD)
1 week 6 week 11 week
Water sorption
(µg/mm3
)
Heat cure DW 20.5 (0.68)* 26.75 (0.68)* 27.0 (0.68)*
AS 17.5 (0.88)* 21.25 (0.00)* 23.5 (0.55)*
DC 22.5 (0.00)* 27.25 (1.04)* 26.25 (0.88)*
DW+DC 19.0 (0.55)* 26.5 (0.55)* 27.25 (1.04)*
AS+DC 18.5 (1.04)* 23.5 (0.55)* 25.0 (0.88)*
Self‑cure DW 13.75 (0.88)* 16.25 (0.00)* 19.75 (0.55)*
AS 12.75 (0.55)* 14.5 (1.42)* 15.5 (0.68)*
DC 14.75 (1.04)* 16.0 (0.55)* 19.75 (1.04)*
DW+DC 16.25 (0.88)* 17.0 (0.68)* 18.25 (0.68)*
AS+DC 14.0 (1.04)* 15.0 (0.88)* 16.0 (1.04)*
Water solubility
(µg/mm3
)
Heat cure DW 0.25 (0.55)#
0.75 (0.68)#
1.25 (0.00)#
AS 0.25 (0.55)#
0.75 (0.68)#
1.25 (0.00)#
DC 0.25 (0.55)#
0.75 (0.68)#
1.5 (0.55)#
DW+DC 0.25 (0.55)#
1.0 (0.55)#
1.5 (0.55)#
AS+DC 0.25 (0.55)#
1.0 (0.55)#
1.5 (0.55)#
Self‑cure DW 1.25 (0.00)#
4.0 (1.04)#
6.0 (0.55)#
AS 1.5 (0.55)#
4.25 (1.11)#
6.25 (0.00)#
DC 1.5 (0.55)#
4.25 (0.68)#
6.5 (0.55)#
DW+DC 1.5 (0.55)#
4.5 (0.68)#
6.5 (0.55)#
AS+DC 1.75 (0.68)#
4.75 (0.55)#
6.5 (0.55)#
#
Values are not statistically significant (P0.05). Solution 1=DW, Solution 2=AS, Solution 3=DC, Solution 4=DW+DC, Solution 5=AS+DC, SD=Standard deviation,
DW=Distilled water, AS=Artificial saliva, DC=Denture cleanser
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Comparison of sorption and solubility of acrylic resins Saini, et al.
Indian Journal of Dental Research, 27(3), 2016292
For heat‑cure resins, water sorption mean values varied from
17.5 ± 0.88 to 27.25 ± 1.04 μg/mm3
in the different solutions
after different interval periods (1, 6, and 11 weeks). These
values were statistically significant (P  0.001). There was
minimum water sorption in artificial saliva (solution 2) at
week 1, i.e., 17.5 ± 0.88 μg/mm3
while maximum water
sorption was observed in distilled water + denture cleanser
(solution 4) at 11 weeks, i.e., 27.25 ± 1.04 μg/mm3
.
For self‑cure resins, water sorption mean values varied from
12.75 ± 0.55 to 19.75 ± 1.04 μg/mm3
in the different solutions
after different interval periods (1, 6, and 11 weeks). These
values were statistically significant (P  0.001). There was
minimum water sorption in artificial saliva (solution 2) at
week 1, i.e., 12.75 ± 0.55 μg/mm3
. While maximum water
sorption was observed in denture cleanser (solution 3) at
11 weeks, i.e., 19.75 ± 1.04 μg/mm3
.
For heat‑cure resins, water solubility mean values varied
from 0.25 ± 0.55 to 1.5 ± 0.55 μg/mm3
in the different
solutions after 1, 6, and 11 weeks. These values were
statistically not significant (P  0.05). There was minimum
water solubility in distilled water (solution 1) at week 1,
i.e., 0.25 ± 0.55 μg/mm3
, while maximum water solubility
was observed in distilled water + denture cleanser
(solution 4) at 11 weeks, i.e., 1.5 ± 0.55 μg/mm3
.
For self‑cure resins, water solubility mean values varied
from 1.5 ± 0.55 to 6.5 ± 0.55 μg/mm3
in the different
solutions after 1, 6, and 11 weeks. These values were
statistically not significant (P  0.05). There was minimum
water solubility in distilled water (solution 1) at week 1,
i.e., 1.5 ± 0.55 μg/mm3
, while maximum water solubility
was observed in denture cleanser (solution 3) at 11 weeks,
i.e., 6.5 ± 0.55 μg/mm3
.
Overall analysis of results showed the maximum sorption
value in the denture cleansing solution followed by
immersion in distilled water and artificial saliva alternatively.
Least sorption value was seen with artificial saliva followed
by distilled water. Hence, as a clinical point of view, artificial
saliva solution is a better storage medium than distilled water
and denture cleansing solution for both heat‑ and self‑cure
acrylic resins.
DISCUSSION
In the present study, the method recommended by the ISO
for measuring water sorption and solubility was used. The
water sorption was determined according to an increase
in mass per unit volume. In addition, water solubility was
determined according to loss of mass from polymers.[14,15]
The soluble materials present in acrylic resins are initiators,
plasticizers, and free monomer. It has been suggested that
there might be a correlation between residual monomer and
the weight loss determined by the solubility test.[15]
Acrylic resins absorb water slowly over a period of time,
primarily because of the polar properties of the resin
molecules. High equilibrium uptake of water can soften
an acrylic resin because the absorbed water can act as
a plasticizer of acrylate and reduce the strength of the
material.[17]
The extent and rate of water uptake into polymer
Table 3: Consolidated results of analysis of variance/post hoc test for sorption at 1, 6, and 11 weeks for heat‑cure resins
Sorption 1 (%) DW AS DC DW with DC
Sorption at 1 week AS Yes (DW) No
DC Yes (DC) Yes (DC) No
DW with DC Yes (DW) Yes (DW+DC) Yes (DC) No
AS with DC Yes (DW) No Yes (DC) No
Sorption at 6 weeks AS Yes (DW) No
DC No Yes (DC) No
DW with DC No Yes (DW+DC) No No
AS with DC Yes (DW) Yes (AS+DC) Yes (DC) Yes (DW+DC)
Sorption at 11 weeks AS Yes (DW) No
DC No Yes (DC) No
DW with DC No Yes (DW+DC) No No
AS with DC Yes (DW) No No Yes (DW+DC)
DC=Denture cleanser, DW=Distilled water, AS=Artificial saliva
Table 4: Consolidated results of analysis of variance/ post hoc
test for sorption at 1, 6, and 11 weeks for self‑cure resins
Sorption
1 (%)
DW AS DC DW with
DC
Sorption at
1 week
AS No No
DC No Yes (DC) No
DW with DC Yes
(DW+DC)
Yes
(DW+DC)
No No
AS with DC No No No Yes
(DW+DC)
Sorption at
6 weeks
AS Yes (DW) No
DC No No No
DW with DC No Yes
(DW+DC)
NO No
AS with DC No No No Yes
(DW+DC)
Sorption at
11 weeks
AS Yes (DW) No
DC No Yes (DC) No
DW with DC No Yes
(DW+DC)
No No
AS with DC Yes (DW) No Yes (DC) Yes
(DW+DC)
DC=Denture cleanser, DW=Distilled water, AS=Artificial saliva
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Comparison of sorption and solubility of acrylic resins Saini, et al.
293Indian Journal of Dental Research, 27(3), 2016
networks are predominantly controlled by resin polarity,
dictated by the concentration of polar sites available to form
hydrogen bonds with water and network topology.[12]
Arima et al.[18]
suggested that the chemical nature of
the polymer versus that of the water molecule directly
affected the water sorption of resin. Water is absorbed into
polymers by the polarity of the molecules in the polymers
by unsaturated bonds of the molecules or unbalanced
intermolecular forces in the polymers. The present study
showed the least sorption value (12.75 μg/mm3
) for
self‑cure resin in artificial saliva and highest sorption value
(27.25 μg/mm3
) for heat‑cure resin in distilled water +
denture cleanser.
The solubility value of the heat‑cure resin showed the
highest value (1.5 μg/mm3
) in distilled water + denture
cleanser and for self‑cure resin, the highest solubility value
(6.5 μg/mm3
) was seen in denture cleanser. The principal
difference between self‑cure and heat‑cure resins is that
more residual monomer is present in the self‑cure resins.
In addition, with a high monomer to polymer ratio, residual
monomer content in the polymerized acrylic resin would
be large.[13]
Fletcher et al.[19]
found that self‑cure resins exhibited higher
residual monomer levels than did heat‑cure resins. These
higher residual monomer contents could be related to the
higher solubility levels of self‑cure resins reported. It is
obvious that the greater amount of residual monomer in
self‑cure polymethyl methacrylate (PMMA) also affects the
solubility values more than heat‑cure PMMA does, of which
the residual monomer content is considerably lower.[15]
In the present study, heat‑cure acrylic resin had lower
solubility values than the self‑cure acrylic resin. The results
of the water sorption and solubility either self‑cure or
cold‑cure acrylic resins were in accordance with the ISO
specification.[16]
According to earlier studies,[15,17,18]
the water sorption of
different types of acrylates is 10–25 μg/mm3
. In the present
study, the water sorption values were in accordance with
these studies.
The rate at which the materials absorbed water or lost
soluble components varied considerably with the type of
material, the amount of plasticizer or filler content, and the
solution in which they were immersed.[20]
This study has demonstrated that the solubility of heat‑cure
and self‑cure resins in artificial saliva with denture cleanser
was significantly higher than that in distilled water.
The observed weight loss probably occurred because the
plasticizers are more soluble in ionic solutions than in water.
Conversely, the percentage sorption of artificial saliva by
heat‑cure and self‑cure resins was significantly lower than
that of distilled water (P  0.001).
The lower uptake in artificial saliva is explicable in terms of
the ionic impurities in the polymer. This leads to an enhanced
uptake in distilled water since water droplets will form at
the impurity sites until elastic and osmotic forces balance.
The osmotic pressure will be proportional to the difference
in ionic concentrations between the polymer and external
liquid, this difference being greater for water than for
artificial saliva.[20]
Acrylic resins undergo two processes
when immersed in water. Plasticizers and other soluble
materials have leached into the water, and water is absorbed
by the polymer. The balance between these two processes
affects both the compliance and dimensional stability of
the materials.
The absorption of water by the material results in a weight
and volume increase. The compliance of the materials tested
is dependent either on the presence of a plasticizer as in
the case of the acrylic materials. An ideal material should,
therefore, have no component which is soluble in saliva or
water and should have a low level of absorption.[20]
The water sorption and water solubility were determined
according to the ISO standards 1567:1999.[16]
According
to this specification, water sorption should not exceed
32 μg/mm3
for heat‑cured or self‑cured materials. The loss
in mass per unit volume (soluble material) should not exceed
1.6 μg/mm3
for heat‑cured and 8.0 μg/mm3
for self‑cured
materials.[14,15]
The values of water sorption that were obtained as a result of
our study are consistent with ADA standards and the values
of water sorption that were mentioned by researchers above.
In general, acrylic resins with incomplete polymerization
cannot interact with the media during polymerization
because of using all reactive substances. Furthermore,
polymer molecules have very little capability of passing
through the layers of epidermal tissue and being diffused
because of their sizes.
The reaction products and residual monomers that are
present in the polymer structure move toward the surface
and interact with the soft tissues. Thus, only the substances
being on the surface are biologically important.[21]
To reduce the amount of these substances in acrylic resin,
this material needs to be kept in water for a long time. In
this way, the substances with low molecular weight, in
other words, more reactive substances pass into the water.[22]
Consequently, these substances cannot solute into a patient’s
mouth and, in this way, the amount of potential allergen
[Downloaded free from http://www.ijdr.in on Thursday, April 23, 2020, IP: 106.207.172.140]
Comparison of sorption and solubility of acrylic resins Saini, et al.
Indian Journal of Dental Research, 27(3), 2016294
is reduced. The concentration of residual monomer can be
reduced following an appropriate method of polymerization
and for that reason, sufficient temperature and time are
required.[21,23]
In our study, highly polymerized resin samples absorb
more water than other samples. To reduce the amount of
residual monomer in acrylic resins and pass it into water,
prolonged boiling during processing and keeping in water
for long period is essential. The water molecules fill the
space created in the structure of acrylic resin by diffusion.
Therefore, more water sorption in heat‑cured acrylic resins
was observed compared to self‑cured resins in different time
intervals and solutions.
CONCLUSION
Following conclusions can be drawn from the present
investigation:
1.	 Both heat‑cure and self‑cure acrylic resins showed
varying water sorption and solubility
2.	 The results of both the water sorption and solubility
showed compliance with the ISO specification
3.	 No correlation was found between water sorption and
solubility
4.	 The highest sorption value was in denture cleansing
solution followed by alternate immersion in distilled
water and artificial saliva
5.	 The least sorption value was seen with artificial saliva
followed by distilled water
6.	 Both heat‑cure and self‑cure acrylic resins showed
higher solubility in artificial saliva + denture cleaner
than in distilled water alone; the value was not
statistically significant.
Financial support and sponsorship
Nil.
Conflicts of interest
There are no conflicts of interest.
REFERENCES
1.	 Hiromori K, Fujii K, Inoue K. Viscoelastic properties of denture base
resins obtained by underwater test. J Oral Rehabil 2000;27:522‑31.
2.	 Wong DM, Cheng LY, Chow TW, Clark RK. Effect of processing method
on the dimensional accuracy and water sorption of acrylic resin
dentures. J Prosthet Dent 1999;81:300‑4.
3.	 Varpu M, Vallittu PK. Water sorption and solubility of glass
fiber‑reinforced denture polymethyl methacrylate resin. J Prosthet
Dent 1996;76:531‑4.
4.	 Lai CP, Tsai MH, Chen M, Chang HS, Tay HH. Morphology and properties
of denture acrylic resins cured by microwave energy and conventional
water bath. Dent Mater 2004;20:133‑41.
5.	 Craig RG. Restorative Dental Materials. 12th
ed. Missouri, USA: Mosby
Co.; 2002. p. 656.
6.	 Woelfel JB, Paffenbarger GC, Sweeney WT. Some physical properties
of organic denture base materials. J Am Dent Assoc 1963;67:499‑504.
7.	 Dixon DL, Ekstrand KG, Breeding LC. The transverse strengths of three
denture base resins. J Prosthet Dent 1991;66:510‑3.
8.	 Fujii K. Fatigue properties of acrylic denture base resins. Dent Mater
J 1989;8:243‑59.
9.	 Phillips RW. Skinner’s Science of Dental Materials. 9th
ed. Philadelphia:
WB. Saunders Comp.; 1991. p. 177‑213.
10.	 Takahashi Y, Chai J, Kawaguchi M. Effect of water sorption on the
resistance to plastic deformation of a denture base material relined
with four different denture reline materials. Int J Prosthodont
1998;11:49‑54.
11.	 Cucci AL, Vergani CE, Giampaolo ET, Afonso MC. Water sorption,
solubility, and bond strength of two autopolymerizing acrylic resins
and one heat‑polymerizing acrylic resin. J Prosthet Dent 1998;80:434‑8.
12.	 Malacarne J, Carvalho RM, de Goes MF, Svizero N, Pashley DH, Tay FR,
et al. Water sorption/solubility of dental adhesive resins. Dent Mater
2006;22:973‑80.
13.	 Craig RG, O’Brien WJ, Powers JM. Dental materials – Properties and
manipulation. Plastics in Prosthetics. 5th
ed. St. Louis: CV Mosby; 1992.
14.	 Geukens S, Goossens A. Occupational contact allergy to (meth)
acrylates. Contact Dermatitis 2001;44:153‑9.
15.	 Miettinen VM, Vallittu PK, Docent DT. Water sorption and solubility of
glass fiber‑reinforced denture polymethyl methacrylate resin. J Prosthet
Dent 1997;77:531‑4.
16.	 Council of Dental Materials and Devices. Revised American Dental
Association specification no. 12 for denture base polymers. JADA
1975;90:451‑8.
17.	 Barsby MJ. A denture base resin with low water absorption. J Dent
1992;20:240‑4.
18.	 Arima T, Murata H, Hamada T. The effects of cross‑linking agents on
the water sorption and solubility characteristics of denture base resin.
J Oral Rehabil 1996;23:476‑80.
19.	 Fletcher AM, Purnaveja S, Amin WM, Ritchie GM, Moradians S,
Dodd AW. The level of residual monomer in self‑curing denture‑base
materials. J Dent Res 1983;62:118‑20.
20.	 Kazanji MN, Watkinson AC. Soft lining materials: Their absorption of,
and solubility in, artificial saliva. Br Dent J 1988;165:91‑4.
21.	 Henriks‑Eckerman ML, Suuronen K, Jolanki R, Alanko K. Methacrylates
in dental restorative materials. Contact Dermatitis 2004;50:233‑7.
22.	 Boeckler AF, Morton D, Poser S, Dette KE. Release of dibenzoyl
peroxide from polymethyl methacrylate denture base resins: An in vitro
evaluation. Dent Mater 2008;24:1602‑7.
23.	 Wiltshire WA, Ferreira MR, Ligthelm AJ. Allergies to dental materials.
Quintessence Int 1996;27:513‑20.
[Downloaded free from http://www.ijdr.in on Thursday, April 23, 2020, IP: 106.207.172.140]

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Comparison of Sorption Rates Between Acrylic Resins

  • 1. © 2016 Indian Journal of Dental Research | Published by Wolters Kluwer - Medknow288 Comparative study of sorption and solubility of heat‑cure and self‑cure acrylic resins in different solutions Rajesh Saini, Ravindra Kotian, Prashanthi Madhyastha, Srikant N1 ABSTRACT Objective: The objective of this study was to compare the sorption and solubility of heat‑cure and self‑cure acrylic resins in different solutions. Materials and Methods: One heat‑cure acrylic resin (Trevalon) and one self‑cure acrylic resin (Rapid Repair) were studied. Five groups of square‑shaped specimens (20 mm × 20 mm × 2 mm) were prepared for each acrylic resin and then immersed in five solutions: distilled water, artificial saliva, denture cleansing solution, distilled water, and denture cleaning solution for 12 h alternatively, artificial saliva and denture cleaning solution for 12 h alternatively at 37 ± 2°C, and tested sorption and solubility by weight gain/loss method, respectively, after 1, 6, and 11 weeks. The data were analyzed by one‑way analysis of variance followed by post hoc Tukey’s test. Results: Water sorption mean values varied from 17.5 ± 0.88 to 27.25 ± 1.04 μg/mm3 for heat cure and from 12.75 ± 0.55 to 19.75 ± 1.04 μg/mm3 for self‑cure in the different solutions after different interval periods of 1, 6, and 11 weeks. These values were statistically significant (P < 0.001). Water solubility mean values varied from 0.25 ± 0.55 to 1.5 ± 0.55 μg/mm3 for heat cure and from 1.5 ± 0.55 to 6.5 ± 0.55 μg/mm3 for self‑cure in the different solutions after different interval periods of 1, 6, and 11 weeks. These values were statistically not significant (P > 0.05). There was no linear correlation between sorption and solubility values. Overall, analysis of results showed the maximum sorption value in denture cleansing solution followed by alternative soaking in distilled water and artificial saliva. Least sorption was observed with artificial saliva followed by distilled water. Conclusion: Both heat‑cure and self‑cure acrylic resins showed varying water sorption and solubility. The results of both water sorption and solubility showed compliance with the International Standards Organization specification. No correlation was found between water sorption and solubility. Artificial saliva solution is a better storage medium than distilled water and denture cleansing solution for both heat‑cure and self‑cure acrylic resins. Key words: Acrylic resin, heat‑cure acrylic, self‑cure acrylic, solubility, water sorption Address for correspondence: Dr. Ravindra Kotian E‑mail: ravindrakotian@yahoo.co.in sorption and release, which causes dimensional instability, thereby subjecting the material to internal stresses that may result in crack formation and eventually fractures of the denture.[1,2] Acrylic resins absorb water slowly over a period of time. This imbibition is due primarily to the polar properties of the resin molecules.[3,4] Sorption of material represents the Acrylic resin is the most utilized material in partial removable and complete denture bases and facings for fixed bridges to improve the esthetic value of the restoration. Prediction of the service life of acrylic resin material is difficult since many environmental factors affect the durability. One of the properties of acrylic resins is water Original Research Departments of Dental Materials and 1 Oral Pathology, Manipal College of Dental Sciences, Manipal University, Mangalore, Karnataka, India Received : 10‑06‑14 Review completed : 05‑07‑14 Accepted : 28-04-16 Access this article online Quick Response Code: Website: www.ijdr.in PMID: *** DOI: 10.4103/0970-9290.186234 How to cite this article: Saini R, Kotian R, Madhyastha P, Srikant N. Comparative study of sorption and solubility of heat-cure and self-cure acrylic resins in different solutions. Indian J Dent Res 2016;27:288-94. This is an open access article distributed under the terms of the Creative Commons Attribution‑NonCommercial‑ShareAlike 3.0 License, which allows others to remix, tweak, and build upon the work non‑commercially, as long as the author is credited and the new creations are licensed under the identical terms. For reprints contact: reprints@medknow.com [Downloaded free from http://www.ijdr.in on Thursday, April 23, 2020, IP: 106.207.172.140]
  • 2. Comparison of sorption and solubility of acrylic resins Saini, et al. 289Indian Journal of Dental Research, 27(3), 2016 amounts of water adsorbed on the surface and absorbed into the body of the material during fabrication or while the restoration is in service. Since both adsorption and absorption are involved, the term sorption is generally used to include the total phenomena. Usually, a serious warpage and dimensional change in the material are associated with a high percentage of water sorption.[5] Dimensional change that occurs on prostheses as a result of water absorption of acrylic is an alternate event. If the prosthesis is left in open air and a dry place, it allows water to leave its structure and undergoes contraction. Therefore, for patients using removable prostheses, it is recommended to store the prosthesis in water when they are not in use. The water absorbed into the material acts as a plasticizer and decreases the mechanical properties such as hardness, transverse strength, and fatigue limit.[6,7] According to the rules of diffusion, water sorption can be explained in the diffusion forces of the resin molecules to separate from each other. This, in turn, creates an expansion in size with water helping to relax the stresses with the acrylic resin.[8] Solubility represents the mass of the soluble materials from polymers. The only soluble materials present in denture base resins are initiators, plasticizers, and free monomer. Any observed loss of weight of the resin is the measure of the specimen’s solubility. Therefore, the water sorption and solubility are the critical problems that affect the durability.[9] Takahashi et al.[10] found that water molecules spread between the macromolecules of the material, forcing them apart. This behavior affects the dimensional behavior and denture stability; therefore, water sorption and solubility of these materials should be as low as possible.[11] Ideally, polymer networks should be insoluble materials with relatively high chemical and thermal stability. However, most of the monomers used in dental resin materials can absorb water and chemicals from the environment, and also release components into the surrounding environment. Both water sorption and solubility would lead to a variety of chemical and physical processes that may result in deleterious effects on the structure and function of dental polymers.[12] Denture base acrylic resins have low solubility, and the little that occurs is a result of the leaching out of the traces of unreacted monomer and water‑soluble additives into the oral fluids. However, these monomers sometimes produce a soft tissue reaction.[13] It is important to determine the residual monomer content and solubility of the tested materials as these properties influence the allergy susceptibility of these materials. The water sorption and solubility were determined according to the International Standards Organization (ISO) standards 1567:1999.[14] According to this specification, water sorption should not exceed 32 μg/mm3 for heat‑cured or self‑cured materials. The loss in mass per unit volume (soluble material) should not exceed 1.6 μg/mm3 for heat‑cured and 8.0 μg/mm3 for self‑cured materials.[14,15] Because water sorption and solubility play a very important role in the clinical and mechanical performance of acrylic materials, it was, therefore, decided to study these properties of heat‑cure and self‑cure acrylic resins in different solutions. The aim of this study was to compare the sorption/solubility of heat‑cure acrylic resin and self‑cure acrylic resin in the different solutions after 1 week, 6 weeks, and 11 weeks. MATERIALS AND METHODS In this study, one heat‑cure and one self‑cure acrylic denture base materials were selected for comparative evaluation of sorption and solubility in different solutions at different time intervals. The materials and solutions selected are given in Table 1. For the study, 25 samples each with dimensions of 20 mm × 20 mm × 2 mm were prepared using heat‑cure and self‑cure acrylic resins separately for the different time intervals. For each solution, five samples were used. Gypsum molds were used to prepare the samples by using a preformed wax pattern of standard dimension. Gypsum mold preparation Wax patterns measuring 20 mm in length, 20 mm in width, and 2 mm in thickness were used to prepare a gypsum mold. Wax patterns were invested in the dental stone in the base of the flask. Two coatings of alginate separating media (cold mold seal) were then applied onto the set dental stone. The counterpart of the flask was positioned over the base and filled with dental stone. The flask was placed on top of the vibrator, taking care not to cause air entrapment. The flask was clamped immediately to ensure metal‑to‑metal contact between the base and the counterpart of the flask. After setting, the wax was removed by immersing in a hot water bath without damaging the molds. The molds formed were then flushed with hot water to remove any traces of residue followed by the application of separating media. The mold cavities so obtained were used for the preparation of acrylic resin specimen. Preparation of Trevalon ‑ heat‑cure acrylic resin specimen The appropriate amount of Trevalon (Dentsply India Pvt., Ltd., Bangalore, India) heat‑cure acrylic resin required was [Downloaded free from http://www.ijdr.in on Thursday, April 23, 2020, IP: 106.207.172.140]
  • 3. Comparison of sorption and solubility of acrylic resins Saini, et al. Indian Journal of Dental Research, 27(3), 2016290 prepared from a mixture of polymer and monomer in the ratio of 3:1 by volume. The monomer was poured into a mixing jar and the polymer was slowly added to allow for wetting of the powder. Excess powder was removed. Then, it was thoroughly mixed for 1 min. After attaining the dough forming time, the dough was thoroughly kneaded between the fingers and the mold cavities were filled. The flask was closed and trial closure was carried out using flask clamp. The flask was then clamped, and the pressure was maintained for 30 min to allow proper penetration of monomer into polymer. The flask was immersed in an acrylizer (Confident Dental Equipment Ltd., Bengaluru, Karnataka, India) at room temperature. The temperature was raised to 74°C for 1.5 h, and then the temperature of the water bath was increased to boiling (100°C) for an additional hour. After the completion of the curing cycle, the flask was removed from the water bath, bench‑cooled for 30 min, and immersed in cold water for 15 min prior to deflasking. The acrylic specimens were then retrieved, finished, and polished. The dimensions and quality of the specimens were verified. Twenty‑five specimens of 20 mm × 20 mm × 2 mm dimension were obtained by this procedure. Preparation of Rapid Repair ‑ self‑cure acrylic resin specimen The appropriate amount of Rapid Repair (Dentsply India, Pvt., Ltd.) self‑cure acrylic resin required was prepared from a mixture of polymer and monomer in the ratio of 3:1 by volume, i.e., three parts of polymer and one part of monomer. The monomer was poured into a mixing jar and the polymer was slowly added to allow for wetting of the powder. Excess powder was removed. Then, it was thoroughly mixed for 1 min. After attaining the dough forming time, the dough was thoroughly kneaded between the fingers and the mold cavities were filled. The flask was closed and trial closure was carried out using flask‑clamp, and pressure was maintained for 5 min to allow proper penetration of monomer into polymer. After the completion of the self‑curing cycle, the flask was removed from the trial closure. The acrylic specimen was then retrieved, finished, and polished. The dimensions and quality of the specimens were verified. Twenty‑five specimens of 20 cm × 20 cm × 2 mm dimension were obtained by this procedure. Method to obtain sorption and solubility The specimens were stored in different solutions [Table 1] at 37 ± 2°C and sorption and solubility were tested by the weight gain/loss method, respectively, after 1, 6, and 11 weeks. Sorption and solubility were determined by the method described in the American Dental Association (ADA) specification 12 for denture base polymers.[16] Each sample was dried in desiccators containing anhydrous calcium chloride until a constant weight was obtained. This was considered to be the initial weight of the specimen (W1 ). The samples were then immersed in: • Solution 1: Distilled water • Solution 2: Artificial saliva • Solution 3: Denture cleansing solution • Solution 4: Distilled water and denture cleaning solution for 12 h alternatively • Solution 5: Artificial saliva and denture cleaning solution for 12 h alternatively. Of the processed samples, five each for both heat‑cure and self‑cure were placed in sealed polyethylene containers each containing different solutions for 1, 6, and 11 weeks at 37 ± 2°C. After each time period, respectively, the samples were removed from their container, excess water was removed by blotting with filter paper, and the samples were weighed by an electronic precision balance (Essae Teraoka Limited, Gurgoan, India) capable of measuring to 0.001 g. This was the weight of the specimen after absorption (W2 ). The amount of soluble material lost was measured by placing the specimens back in the desiccators after each sorption cycle and then weighing them at regular intervals until a constant weight after desiccation (W3 ). The water sorption and water solubility per unit volume are determined according to the ISO standards 1567:1999.[14] Table 1: List of materials, batch number, and manufacturers Material type Material brand name Batch number Manufacturer Heat cure acrylic denture base resin Trevalon T121037 Dentsply India Pvt. Ltd. Self‑cure acrylic denture base resin RR R130102 Dentsply India Pvt. Ltd. AS Wet mouth C12002 ICPA Health Products Ltd. Denture cleansing tablets Fitty dent FDT13024 Group Pharmaceuticals Ltd. DW Demineralized water MD112 Medilise Chemicals RR=Rapid Repair, DW=Distilled water, AS=Artificial saliva [Downloaded free from http://www.ijdr.in on Thursday, April 23, 2020, IP: 106.207.172.140]
  • 4. Comparison of sorption and solubility of acrylic resins Saini, et al. 291Indian Journal of Dental Research, 27(3), 2016 (μg/mm3 ) sorption: W2 − W3 /VSample (μg/mm3 ) solubility: W1 − W3 /VSample VSample = 20 mm × 20 mm × 2 mm = 800 mm3 W1 = The initial weight W2 = The weight after absorption W3 = The final weight after desiccation. The above procedure was repeated, and sorption and solubility data were collected for 1, 6, and 11 weeks. Mean values and standard deviation of both sorption and solubility were calculated. Mean values were compared statistically with one‑way analysis of variance (ANOVA) followed by post hoc Tukey’s test to determine the significant differences among the groups at P 0.05 level of significance. RESULTS SPSS 20.0 (Version 20, Dentsply India Pvt., Ltd, Bangalore, India) was used to obtain the statistical results of our study. One‑way ANOVA test followed by post hoc Tukey’s test was used to evaluate the sorption and the solubility values of the heat‑cure and self‑cure resins at a time period of 1, 6, and 11 weeks. The results of mean and standard deviation are presented in Tables 2‑4 that show the consolidated results of ANOVA/post hoc test for sorption of heat‑cured and self‑cured resins, respectively. Analysis of the results showed a significant difference in the sorption values at all time periods as assessed by one‑way ANOVA. No significant difference was observed in the solubility values in heat‑cure and self‑cure resins separately. There was no linear correlation between sorption and solubility values. According to ANOVA, the type of material, time, and solution of storage were statistically significant on water sorption and water solubility (P 0.001). According to post hoc Tukey’s test, the water solubility between the time and solution of storage was not statistically significant (P 0.05). When the values of water sorption and solubility were observed according to time, there was a significant increase in the values of all samples during the 1st week of the study. For heat cure, no linear increase in water sorption was found during the immersion period of 1 to 11 weeks. Most of the increase occurred during the first 6 weeks compared to weeks 6–11 (19.6 ‑ 25.05 ‑ 25.8 ANOVA). Whereas a linear increase in water sorption was observed in self‑cure from 1 to 11 weeks (14.3 ‑ 15.75 ‑ 17.85 ANOVA). Water sorption values for heat cure were significantly higher than self‑cure in the different interval periods in different solutions (P 0.001). Water solubility values for both heat‑cure and self‑cure resins increased significantly from 1 to 11 weeks in different solutions (HC 0.25 ‑ 0.85 ‑ 1.4 and SC 1.5 ‑ 4.35 ‑ 6.35 ANOVA). Water solubility values for heat‑cure resins were markedly less when compared to self‑cure resins in the different interval periods in different solutions and was statistically significant (P 0.001). Table 2: Mean and standard deviation of the samples Brands Groups Mean (SD) 1 week 6 week 11 week Water sorption (µg/mm3 ) Heat cure DW 20.5 (0.68)* 26.75 (0.68)* 27.0 (0.68)* AS 17.5 (0.88)* 21.25 (0.00)* 23.5 (0.55)* DC 22.5 (0.00)* 27.25 (1.04)* 26.25 (0.88)* DW+DC 19.0 (0.55)* 26.5 (0.55)* 27.25 (1.04)* AS+DC 18.5 (1.04)* 23.5 (0.55)* 25.0 (0.88)* Self‑cure DW 13.75 (0.88)* 16.25 (0.00)* 19.75 (0.55)* AS 12.75 (0.55)* 14.5 (1.42)* 15.5 (0.68)* DC 14.75 (1.04)* 16.0 (0.55)* 19.75 (1.04)* DW+DC 16.25 (0.88)* 17.0 (0.68)* 18.25 (0.68)* AS+DC 14.0 (1.04)* 15.0 (0.88)* 16.0 (1.04)* Water solubility (µg/mm3 ) Heat cure DW 0.25 (0.55)# 0.75 (0.68)# 1.25 (0.00)# AS 0.25 (0.55)# 0.75 (0.68)# 1.25 (0.00)# DC 0.25 (0.55)# 0.75 (0.68)# 1.5 (0.55)# DW+DC 0.25 (0.55)# 1.0 (0.55)# 1.5 (0.55)# AS+DC 0.25 (0.55)# 1.0 (0.55)# 1.5 (0.55)# Self‑cure DW 1.25 (0.00)# 4.0 (1.04)# 6.0 (0.55)# AS 1.5 (0.55)# 4.25 (1.11)# 6.25 (0.00)# DC 1.5 (0.55)# 4.25 (0.68)# 6.5 (0.55)# DW+DC 1.5 (0.55)# 4.5 (0.68)# 6.5 (0.55)# AS+DC 1.75 (0.68)# 4.75 (0.55)# 6.5 (0.55)# # Values are not statistically significant (P0.05). Solution 1=DW, Solution 2=AS, Solution 3=DC, Solution 4=DW+DC, Solution 5=AS+DC, SD=Standard deviation, DW=Distilled water, AS=Artificial saliva, DC=Denture cleanser [Downloaded free from http://www.ijdr.in on Thursday, April 23, 2020, IP: 106.207.172.140]
  • 5. Comparison of sorption and solubility of acrylic resins Saini, et al. Indian Journal of Dental Research, 27(3), 2016292 For heat‑cure resins, water sorption mean values varied from 17.5 ± 0.88 to 27.25 ± 1.04 μg/mm3 in the different solutions after different interval periods (1, 6, and 11 weeks). These values were statistically significant (P 0.001). There was minimum water sorption in artificial saliva (solution 2) at week 1, i.e., 17.5 ± 0.88 μg/mm3 while maximum water sorption was observed in distilled water + denture cleanser (solution 4) at 11 weeks, i.e., 27.25 ± 1.04 μg/mm3 . For self‑cure resins, water sorption mean values varied from 12.75 ± 0.55 to 19.75 ± 1.04 μg/mm3 in the different solutions after different interval periods (1, 6, and 11 weeks). These values were statistically significant (P 0.001). There was minimum water sorption in artificial saliva (solution 2) at week 1, i.e., 12.75 ± 0.55 μg/mm3 . While maximum water sorption was observed in denture cleanser (solution 3) at 11 weeks, i.e., 19.75 ± 1.04 μg/mm3 . For heat‑cure resins, water solubility mean values varied from 0.25 ± 0.55 to 1.5 ± 0.55 μg/mm3 in the different solutions after 1, 6, and 11 weeks. These values were statistically not significant (P 0.05). There was minimum water solubility in distilled water (solution 1) at week 1, i.e., 0.25 ± 0.55 μg/mm3 , while maximum water solubility was observed in distilled water + denture cleanser (solution 4) at 11 weeks, i.e., 1.5 ± 0.55 μg/mm3 . For self‑cure resins, water solubility mean values varied from 1.5 ± 0.55 to 6.5 ± 0.55 μg/mm3 in the different solutions after 1, 6, and 11 weeks. These values were statistically not significant (P 0.05). There was minimum water solubility in distilled water (solution 1) at week 1, i.e., 1.5 ± 0.55 μg/mm3 , while maximum water solubility was observed in denture cleanser (solution 3) at 11 weeks, i.e., 6.5 ± 0.55 μg/mm3 . Overall analysis of results showed the maximum sorption value in the denture cleansing solution followed by immersion in distilled water and artificial saliva alternatively. Least sorption value was seen with artificial saliva followed by distilled water. Hence, as a clinical point of view, artificial saliva solution is a better storage medium than distilled water and denture cleansing solution for both heat‑ and self‑cure acrylic resins. DISCUSSION In the present study, the method recommended by the ISO for measuring water sorption and solubility was used. The water sorption was determined according to an increase in mass per unit volume. In addition, water solubility was determined according to loss of mass from polymers.[14,15] The soluble materials present in acrylic resins are initiators, plasticizers, and free monomer. It has been suggested that there might be a correlation between residual monomer and the weight loss determined by the solubility test.[15] Acrylic resins absorb water slowly over a period of time, primarily because of the polar properties of the resin molecules. High equilibrium uptake of water can soften an acrylic resin because the absorbed water can act as a plasticizer of acrylate and reduce the strength of the material.[17] The extent and rate of water uptake into polymer Table 3: Consolidated results of analysis of variance/post hoc test for sorption at 1, 6, and 11 weeks for heat‑cure resins Sorption 1 (%) DW AS DC DW with DC Sorption at 1 week AS Yes (DW) No DC Yes (DC) Yes (DC) No DW with DC Yes (DW) Yes (DW+DC) Yes (DC) No AS with DC Yes (DW) No Yes (DC) No Sorption at 6 weeks AS Yes (DW) No DC No Yes (DC) No DW with DC No Yes (DW+DC) No No AS with DC Yes (DW) Yes (AS+DC) Yes (DC) Yes (DW+DC) Sorption at 11 weeks AS Yes (DW) No DC No Yes (DC) No DW with DC No Yes (DW+DC) No No AS with DC Yes (DW) No No Yes (DW+DC) DC=Denture cleanser, DW=Distilled water, AS=Artificial saliva Table 4: Consolidated results of analysis of variance/ post hoc test for sorption at 1, 6, and 11 weeks for self‑cure resins Sorption 1 (%) DW AS DC DW with DC Sorption at 1 week AS No No DC No Yes (DC) No DW with DC Yes (DW+DC) Yes (DW+DC) No No AS with DC No No No Yes (DW+DC) Sorption at 6 weeks AS Yes (DW) No DC No No No DW with DC No Yes (DW+DC) NO No AS with DC No No No Yes (DW+DC) Sorption at 11 weeks AS Yes (DW) No DC No Yes (DC) No DW with DC No Yes (DW+DC) No No AS with DC Yes (DW) No Yes (DC) Yes (DW+DC) DC=Denture cleanser, DW=Distilled water, AS=Artificial saliva [Downloaded free from http://www.ijdr.in on Thursday, April 23, 2020, IP: 106.207.172.140]
  • 6. Comparison of sorption and solubility of acrylic resins Saini, et al. 293Indian Journal of Dental Research, 27(3), 2016 networks are predominantly controlled by resin polarity, dictated by the concentration of polar sites available to form hydrogen bonds with water and network topology.[12] Arima et al.[18] suggested that the chemical nature of the polymer versus that of the water molecule directly affected the water sorption of resin. Water is absorbed into polymers by the polarity of the molecules in the polymers by unsaturated bonds of the molecules or unbalanced intermolecular forces in the polymers. The present study showed the least sorption value (12.75 μg/mm3 ) for self‑cure resin in artificial saliva and highest sorption value (27.25 μg/mm3 ) for heat‑cure resin in distilled water + denture cleanser. The solubility value of the heat‑cure resin showed the highest value (1.5 μg/mm3 ) in distilled water + denture cleanser and for self‑cure resin, the highest solubility value (6.5 μg/mm3 ) was seen in denture cleanser. The principal difference between self‑cure and heat‑cure resins is that more residual monomer is present in the self‑cure resins. In addition, with a high monomer to polymer ratio, residual monomer content in the polymerized acrylic resin would be large.[13] Fletcher et al.[19] found that self‑cure resins exhibited higher residual monomer levels than did heat‑cure resins. These higher residual monomer contents could be related to the higher solubility levels of self‑cure resins reported. It is obvious that the greater amount of residual monomer in self‑cure polymethyl methacrylate (PMMA) also affects the solubility values more than heat‑cure PMMA does, of which the residual monomer content is considerably lower.[15] In the present study, heat‑cure acrylic resin had lower solubility values than the self‑cure acrylic resin. The results of the water sorption and solubility either self‑cure or cold‑cure acrylic resins were in accordance with the ISO specification.[16] According to earlier studies,[15,17,18] the water sorption of different types of acrylates is 10–25 μg/mm3 . In the present study, the water sorption values were in accordance with these studies. The rate at which the materials absorbed water or lost soluble components varied considerably with the type of material, the amount of plasticizer or filler content, and the solution in which they were immersed.[20] This study has demonstrated that the solubility of heat‑cure and self‑cure resins in artificial saliva with denture cleanser was significantly higher than that in distilled water. The observed weight loss probably occurred because the plasticizers are more soluble in ionic solutions than in water. Conversely, the percentage sorption of artificial saliva by heat‑cure and self‑cure resins was significantly lower than that of distilled water (P 0.001). The lower uptake in artificial saliva is explicable in terms of the ionic impurities in the polymer. This leads to an enhanced uptake in distilled water since water droplets will form at the impurity sites until elastic and osmotic forces balance. The osmotic pressure will be proportional to the difference in ionic concentrations between the polymer and external liquid, this difference being greater for water than for artificial saliva.[20] Acrylic resins undergo two processes when immersed in water. Plasticizers and other soluble materials have leached into the water, and water is absorbed by the polymer. The balance between these two processes affects both the compliance and dimensional stability of the materials. The absorption of water by the material results in a weight and volume increase. The compliance of the materials tested is dependent either on the presence of a plasticizer as in the case of the acrylic materials. An ideal material should, therefore, have no component which is soluble in saliva or water and should have a low level of absorption.[20] The water sorption and water solubility were determined according to the ISO standards 1567:1999.[16] According to this specification, water sorption should not exceed 32 μg/mm3 for heat‑cured or self‑cured materials. The loss in mass per unit volume (soluble material) should not exceed 1.6 μg/mm3 for heat‑cured and 8.0 μg/mm3 for self‑cured materials.[14,15] The values of water sorption that were obtained as a result of our study are consistent with ADA standards and the values of water sorption that were mentioned by researchers above. In general, acrylic resins with incomplete polymerization cannot interact with the media during polymerization because of using all reactive substances. Furthermore, polymer molecules have very little capability of passing through the layers of epidermal tissue and being diffused because of their sizes. The reaction products and residual monomers that are present in the polymer structure move toward the surface and interact with the soft tissues. Thus, only the substances being on the surface are biologically important.[21] To reduce the amount of these substances in acrylic resin, this material needs to be kept in water for a long time. In this way, the substances with low molecular weight, in other words, more reactive substances pass into the water.[22] Consequently, these substances cannot solute into a patient’s mouth and, in this way, the amount of potential allergen [Downloaded free from http://www.ijdr.in on Thursday, April 23, 2020, IP: 106.207.172.140]
  • 7. Comparison of sorption and solubility of acrylic resins Saini, et al. Indian Journal of Dental Research, 27(3), 2016294 is reduced. The concentration of residual monomer can be reduced following an appropriate method of polymerization and for that reason, sufficient temperature and time are required.[21,23] In our study, highly polymerized resin samples absorb more water than other samples. To reduce the amount of residual monomer in acrylic resins and pass it into water, prolonged boiling during processing and keeping in water for long period is essential. The water molecules fill the space created in the structure of acrylic resin by diffusion. Therefore, more water sorption in heat‑cured acrylic resins was observed compared to self‑cured resins in different time intervals and solutions. CONCLUSION Following conclusions can be drawn from the present investigation: 1. Both heat‑cure and self‑cure acrylic resins showed varying water sorption and solubility 2. 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