Basic Research—Technology
Influence of Calcium Hydroxide Association on the Physical
Properties of AH Plus
Marco Antonio Hungaro Duarte, DDS, MSc, PhD,* Ronald Ordinola-Zapata, DDS,*
Ricardo Affonso Bernardes, DDS, MSc, PhD,† Clovis Monteiro Bramante, DDS, MSc, PhD,*
Norberti Bernardineli, DDS, MSc, PhD,* Roberto Brandão Garcia, DDS, MSc, PhD,*
and Ivaldo Gomes de Moraes, DDS, MSc, PhD*
Abstract
Introduction: This study evaluated in vitro the radio-
pacity, setting time, flow, film thickness, solubility,
and dimensional changes of AH Plus sealer pure (Dents-
ply De Trey Gmbh, Konstanz, Germany) and containing
5% and 10% of calcium hydroxide. Methods: The study
was performed according to the requirements of the ISO
6876:2001 standard and the American National Stan-
dards Institute/American Dental Association (ANSI/
ADA)’s Specification No. 57. The following tests were
performed: setting time, flow, film thickness, dimen-
sional stability, radiopacity, and solubility. Data were
analyzed statistically by analysis of variance and the Tu-
key tests with a significance level of 5%. Results: The
addition of 5% or 10% calcium hydroxide to AH Plus
sealer did not alter significantly the radiopacity or
setting time values (p > 0.05). Adding 10% calcium
hydroxide reduced the flow compared with pure AH
Plus and AH Plus/5% calcium hydroxide. The addition
of 5% and 10% calcium hydroxide increased the solu-
bility and expansion of AH Plus. All materials presented
expansion valued above those recommended by the
ADA. The addition of calcium hydroxide to the sealer re-
sulted in greater film thickness. Conclusions: The addi-
tion of 5% calcium hydroxide did not affect most
physical properties of AH Plus sealer. (J Endod
2010;36:1048–1051)
Key Words
AH Plus, calcium hydroxide, flow, radiopacity, setting
time
From the *Department of Operative Dentistry, Dental Mate-
rials and Endodontics, Dental School of Bauru, University of São
Paulo, Bauru, SP, Brazil; and †Department of Endodontics, Bra-
siliense Dental School, Brası́lia, DF, Brazil.
Address requests for reprints to Dr Marco Antonio Hungaro
Duarte, Rua Anna Pietro Forte, 3-18 (lote A12), Residencial Vil-
lagio 1, CEP: 17018-820 Bauru, SP, Brazil. E-mail address:
mhungaro@travelnet.com.br.
0099-2399/$0 - see front matter
Copyright ª 2010 American Association of Endodontists.
doi:10.1016/j.joen.2010.02.007
1048 Duarte et al.
T here has been an ongoing search for an endodontic sealer that meets the ideal phys-
icochemical properties of sealing, radiopacity, setting time, and flow as well as bio-
logical properties over the last few years. One concern has been to develop materials
that stimulate the repair process (1).
Calcium hydroxide, because of its biological effects, is now accepted along with
endodontic sealers and gutta-percha points. It acts at the tissue level by favoring alkaline
pH and calcium release, producing biochemical effects culminating in speedy repair
process (2–4). Furthermore, the calcium ion exerts essential paper in the
mineralization, stimulating the fibronectin gene expression (4). The high pH values
of calcium hydroxide promote antibacterial activity through an irreversible enzymatic
reaction (3, 5), and calcium release clears up the carbon dioxide that bacteria use
for anaerobic respiration (6). Calcium hydroxide also inhibits irritant lipopolysaccha-
rides present in the external membrane of gram-negative bacteria (7–9).
Sealapex was one of the first commercially available endodontic sealers containing
calcium hydroxide (Sybron Kerr Co, Romulus, MI). Some authors (1, 10) reported
excellent biological results, showing the positive effect of adding calcium hydroxide
to root canal sealers, and this material favors a high pH and calcium release (11).
The epoxy resin-based sealer AH Plus (Dentsply De Trey Gmbh, Konstanz,
Germany) is an improved modification of its precursor AH26 and shows a high flow
(12). An adequate flow ability of the endodontic sealers is a very desirable property
that allows filling irregularities. However, an excessive flow can favor apical extrusion.
The sealer extrusion could injure the periapical tissues because of sealer cytotoxicity
(13) by the low biocompatibility, mainly at the initial stage (14).
Duarte et al (15) incorporated calcium hydroxide to AH Plus and verified an alka-
line pH of the sealer and subsequent release of calcium ions. Any new dental product to
be launched to the market must be previously evaluated for its physical, chemical, bio-
logical, and microbial properties. Regarding the physical properties, the American
National Standards Institute/American Dental Association (ANSI/ADA)’s Specification
No. 57 (16) established guidelines for the evaluation of sealers, such as flow, film thick-
ness, setting time, radiopacity, solubility, and dimensional changes.
Root canal sealers need to have sufficient radiopacity to be distinguished from the
surrounding anatomic structures such as dental tissues and bone. Also, radiopacity is
necessary to verify the correct obturation of the cavity and to facilitate follow-up of the
case (17, 18). Therefore, because radiopacity is an important physical property, the ISO
6876:2001 standard (19) and the ANSI/ADA’s Specification No. 57 (16) have stated 3
mm of aluminum (Al) as the minimum radiopacity value for endodontic material.
The aim of the present study was to determine whether the addition of 5% and 10%
calcium hydroxide to the AH Plus endodontic sealer alters the physical properties of
this material.
Material and Methods
The AH Plus sealer used in the present study has the following composition: epoxy
paste: diepoxy, calcium tungstate, zirconium oxide, aerosol, and dye; amine paste: 1-
adamantane amine, N.N’dibenzyl-5-oxanonandiamine-1,9, TCD-diamine, calcium
tungstate, zirconium oxide, aerosol, and silicon oil. The modified AH Plus sealers
JOE — Volume 36, Number 6, June 2010

were prepared by proportionally adding 5% and 10% (w/w) calcium
hydroxide pa (Merck, Rio de Janeiro, RJ, Brazil) to the sealer. Calcium
hydroxide was incorporated upon mixing on a glass plate. The following
tests were performed.
Setting Time
This test was performed according to the ANSI/ADA’s Specification
No. 57 (16) with modification at the Gilmore needle weight. Six stainless
steel rings were fabricated for the epoxy and modified epoxy calcium
hydroxide-based sealers with an internal diameter of 10 mm and a thick-
ness of 2 mm. They were filled with the original and modified sealers.
The external borders of the molds were fixed with wax on a glass plate
(75  25  1 mm). Three stainless steel rings of each material were
stored in an incubator at 37 C and 95% relative humidity, whereas the
other three rings were stored at room temperature. For the final setting
time determination, a Gilmore needle of 453.6  0.5 g and an active tip
of 1.0  0.1-mm diameter was used. This procedure was repeated at
60-second intervals. The arithmetic mean of three repetitions for
each sealer under dry and moist conditions at 37 C was recorded
and considered as the final setting time.
Flow Test
A total of 0.5 mL of sealer was placed on a glass plate (40  40  5
mm) using a graduated disposable 3-mL syringe. Three minutes after the
start of mixing, another plate with a mass of 20  2 g and a load of 100 g
plus was applied centrally on top of the material. Ten minutes after the
start of mixing, the load was removed, and the average of the major and
minor diameters of the compressed discs was measured using a digital
caliper with a resolution of 0.01 mm (Mitutoyo MTI Corporation, Tokyo,
Japan). If both measurements were consistent to within 1 mm, the results
were recorded. If the major and minor diameter discs were not
uniformly circular or did not match within 1 mm, the test was repeated.
The mean of three measurements for each sealer was taken as the flow of
the material. According to the ANSI/ADA’s Specification No. 57 for the
flow test, a disc of at least a 25-mm diameter must be obtained.
Film Thickness
Two 5-mm-thick flat glass plates (200  25 mm2) were placed
together, and their combined thickness was measured. A volume of
0.5 mL of sealer was placed on the center of one of the plates, and
the second plate was placed centrally on top of the sealer. Three minutes
after the start of mixing, a load of 150 N was applied vertically onto the
top glass plate with a loading device, ensuring that the material filled the
entire space between the top and bottom glass plates. Ten minutes after
the start of mixing, the thickness of the two glass plates and the inter-
posed sealer film was measured with an outside micrometer accurate
to 0.002 mm (Mitutoyo MTI Corporation). The difference in thickness
of the two glass plates, with and without sealer, was taken as the film
thickness of the material. The mean value of three measurements for
each sealer was taken as the film thickness of the material. According
to the ANSI/ADA’s Specification No. 57, only sealers that have values
lower than 50 mm (0.05 mm) pass this test.
Solubility
A 1.5-mm-thick cylindrical polytetrafluoroethylene mould with in
inner diameter of 20 mm was filled to a slight excess with freshly mixed
sealer. The mold was supported by a larger glass plate and covered with
a cellophane sheet. A nylon thread was placed inside the material, and
another glass plate, also covered with cellophane film, was positioned
on the mold and pressed manually in such a way that the plates touched
the entire mold in a uniform manner. The assembly was placed in an
JOE — Volume 36, Number 6, June 2010
Basic Research—Technology
incubator (37 C, 95% relative humidity) for a period corresponding
to three times the setting time. Immediately after being removed from
the mold, the samples were weighed three times each with an accuracy
of 0.0001 g (Sartorius scale model 1662; Werke AG, Gottingen,
Germany), and the mean reading was recorded. The samples were sus-
pended by nylon thread and placed two by two inside a plastic vessel
with a wide opening containing 50 mL of deionized distilled water,
avoiding contact between them and the inner surface of the container.
The sealed containers were stored for 24 hours in an incubator (37 C,
95% relative humidity). After this period, the samples were removed
from the containers, rinsed with deionized distilled water, blotted dry
with absorbent paper, placed in a desiccator for 24 hours, and then re-
weighed. The experiment was repeated three times for each sealer. The
weight loss of each sample (initial mass minus final mass), expressed as
the percentage of the original mass, was taken as the solubility of the
sealer. According to the ANSI/ADA’s Specification No. 57 a root canal
sealer cannot have solubility greater than 3%.
Dimensional Changes
Three polytetrafluoroethylene molds prepared for the fabrication
of cylindrical specimens (12-mm high  6-mm diameter) were placed
on a glass plate wrapped with a fine cellophane sheet. The molds were
filled with a slight excess of freshly mixed sealers, and a microscope
slide, which was also wrapped in cellophane, was pressed onto the
upper surface of the mold. The assembly was held in a C-shaped clamp,
transferred to an incubator (37 C, 95% relative humidity), and left to
stand for a period corresponding to three times the setting time. After
this period, the flat ends of the molds containing the samples were
ground with 600-grit wet sandpaper. The samples were removed
from the mold, measured with a digital caliper, stored in a vessel con-
taining 50 mL of deionized distilled, and kept in an incubator (37 C,
95% relative humidity) for 30 days. The samples were then blotted
dry on absorbent paper and measured again for length. The percentage
of the dimensional alterations was calculated using the following equa-
tion: L30LL  100; where L30 is the length of the sample after 30 days of
storage under the experimental conditions and L is the initial length of
the sample. The arithmetic mean of three replicates for each sealer was
recorded as the dimensional change of the sealer tested.
The ANSI/ADA’s Specification No. 57 states that the maximum
permitted limit for dimensional changes is 1% contraction or 0.1%
expansion; however, it does not consider the extent to which a sealer
may expand.
Radiopacity
Five cylindrical samples were fabricated from each material by
pouring the manipulated cements into the metallic rings measuring
10 mm in diameter and 1 mm in thickness according to ADA 57 spec-
ifications (16). The filled rings were kept at 37 C until the sealers were
completely set. The specimens were then removed, and the thickness
was checked with a digital caliper (Mitutoyo Corp, Tokyo, Japan).
The dentin cylinders were obtained by sectioning the roots of noncari-
ous freshly extracted human teeth in 1-mm thickness with a water-
cooled Isomet saw (Isomet, Buehler, IL). Disc thickness was checked
with a digital caliper.
The sealers, gutta-percha, and dentin specimens were placed on
five occlusal films (D-speed; Kodak Comp, Rochester, NY) along an
Al step-wedge graduated from 2 to 16 mm of Al (in 2-mm increments).
Radiographs were taken using a radiographic unit (Gnatus XR 6010;
Gnatus, Ribeirão Preto, SP, Brazil) operating at 60 kV and 10 mA
with exposures set at 0.3 seconds and a focus-film distance of 30 cm.
After processing, the radiographs were digitized using a digital scanner
Physical Properties of AH Plus with and without Ca(OH)2. 1049
Basic Research—Technology
TABLE 1. Mean (and Standard Deviation) of the Setting Time (minutes) for the
Tested Materials According to the Environmental Conditions
Environment
Material Dry
AH Plus + 10% Ca(OH)2 810 (10)
AH Plus + 5% Ca(OH)2 810 (12)
AH Plus 815 (15)
and imported into Digora 1.51 for Windows software (Orion Corpora-
tion Soredex, Helsinki, Finland). The radiopacity value was determined
according to the radiographic density and converted into millimeters of
Al following the method as described by Duarte et al (18) using the
following equation:
A2
þ mm Al immediately below RDM
B 5% was added to the sealer and 27.25 mm when 10% was used,
where A = radiographic density of the material (RDM) – radiographic
density of the Al stepwedge increment immediately below RDM and B =
radiographic density of the Al stepwedge increment immediately above
RDM: radiographic density of the Al stepwedge increment immediately
below RDM, and 2 = 2-mm increments of the Al stepwedge.
Statistical Analysis
Statistically significant differences among the sealers regarding ra-
diopacity, setting time, flow, film thickness, solubility, and dimensional
changes were analyzed statistically by analysis of variance and the Tukey
tests with a significance level of 5%.
Results
The means (and standard deviations) for the setting time values
(minutes) in the presence or absence of moisture are shown in
Table 1. There was no statistically significant differences ( p > 0.05)
between AH Plus and AH Plus modified with 5% or 10% calcium
hydroxide in both environments.
Table 2 shows the means (and standard deviations) of the flow
(mm), film thickness (mm), solubility (%), and dimensional changes
(%). There was no statistically significant differences ( p > 0.05) in the
flow of AH Plus and AH Plus modified with 5% calcium hydroxide. AH
Plus modified with 10% calcium hydroxide showed the lowest flow
values and differed significantly from the other materials ( p < 0.05).
Table 3 lists the radiopacity results in mm of Al. All sealers showed
significantly ( p < 0.05) higher radiopacity values than dentin and gutta-
percha ( p < 0.05). There was no statistically significant difference
between AH Plus and the modified AH Plus sealers (with 5% and
10% calcium hydroxide).
Discussion
The addition of calcium hydroxide to endodontic sealers has been
proposed to improve the biological and antimicrobial activity (11, 15).
A previous study of calcium ion release and pH determination showed
TABLE 2. Mean (and Standard Deviation) of the Flow (mm), Film Thickness (mm), Solubility (%), and Dimensional Changes (%)
Material Mean (flow)
b a
AH Plus + 10% Ca(OH)2 27.25 (0.65)
AH Plus + 5% Ca(OH)2 37.00 (0.83)a
AH Plus 40.25 (0.65)a
a,b
Different letters indicate statistically significant difference among the properties.
*Positive values indicate expansion of the material.
1050 Duarte et al.
that the addition of 5% and 10% calcium hydroxide favored a higher
alkaline pH and a greater calcium ion release compared with pure
AH Plus sealer (15). The high pH of calcium hydroxide normally
promotes antibacterial activity and inhibits the effect of lipopolysaccha-
Humid rides present in gram-negative bacteria (3, 7–9).
845 (15) The flow test results revealed that the values found in this study
870 (13) (40.25 mm) were higher than the minimum required by the ANSI/
955 (11) ADA (20 mm) (16). The reported values were also higher than the
values reported by Versani et al (20) and lower than the values reported
by Almeida et al (12). During the root canal–filling procedures per-
formed with this sealer, sealer extrusion has been clinically evident
(21); however, the addition of 5% and 10% of calcium hydroxide to
the material composition has been proposed to decrease the AH Plus
flow.
Sealer extrusion could injure the periapical tissues because of
sealer cytotoxicity (13) and low biocompatibility, mainly at the initial
stage (14). The flow values in the present study were 37 mm when
revealing the possibility of verifying a decrease in the flow ability
when using 10% calcium hydroxide ( p < 0.05). However, these values
are still above the minimum value recommended by the ISO (18) and
the ANSI/ADA (16). It is evident that in large root canals with wider
foramen adding a proportion of 10% could help prevent extrusion.
Another test was performed to evaluate the setting time. The value
obtained for AH Plus was 14 hours in a dry environment and 15 hours in
a wet environment. The manufacturer reported a setting time value of 8
hours at 37 C. The setting time found in this study was higher than the
manufacturer’s reported setting time and higher than the setting time
observed by other authors, which was 8 hours (22). This could be
caused by the differences in the weight of the needles used in the tests
in the studies, which varied from 100 g to 453.6 g. Moisture did not
seem to significantly alter AH Plus setting time, perhaps because of
the presence of silicon oil in the AH Plus composition. Increasing the
calcium hydroxide showed no significant interferences in the setting
time according to Table 1.
AH Plus showed a high radiopacity value equivalent to 6.94 mm of
Al. This value is higher than the gutta-percha value, which is in accor-
dance with the findings of Resende et al (22). However, the results in
this study were lower than the values presented by other authors
(23–25). The AH Plus radiopacity values vary in different published
works, probably because of the variations of the methodology
applied or the manipulation of the sealer during the mixing process.
Because AH Plus is a paste-catalytic sealer, its components can get
deposited at the lower end of the tube, whereas the upper portions
can present lower quantity of the radiopacifying agent.
AH Plus and AH26 have different radiopacifying agents. AH Plus
presents zirconium oxide and calcium tungstate, which are both white
in color. Zirconium oxide occurs naturally in the mineral baddeleyite
and finds wide application in dermatology (26). AH26 has bismuth
oxide, which is yellow in color, occurs naturally within the bismite
mineral, and is mainly used as an astringent (26). The addition of
5% or 10% calcium hydroxide does not significantly influence the ra-
diopacity according to the data in Table 3. Pure AH Plus, AH Plus +
Film thickness Solubility Dimensional changes*
b
76.60 (5.70) 0.70 (0.18) +1.14 (0.26)a
70.00 (10.00)a 0.60 (0.22)ab +0.93 (0.14)a
43.30 (11.54)b 0.30 (0.03)a +0.57 (0.10)a
JOE — Volume 36, Number 6, June 2010

TABLE 3. Mean (and Standard Deviation) of the Radiopacity in Millimeters
of Al
Material Radiopacity (mm of Al)
AH Plus 10% Ca(OH)2 6.94 (2.32)
AH Plus 5% Ca(OH)2 6.95 (2.33)
AH Plus 6.99 (2.34)
Gutta-percha 6.79 (2.27)
Dentin 1.92 (0.64)
5% calcium hydroxide, and AH Plus + 10% calcium hydroxide radio-
pacity values were significantly higher than the values for gutta-
percha. However, all the endodontic materials tested in this study
presented higher radiopacity values than 3 mm of Al, respectively, which
is the minimum value recommended by the ISO (19) and the ANSI/ADA
(16), and values higher than the radiopacity of dentin.
The use of digitized images and computer-aided radiographic
image analysis with softwares especially designed for this purpose
has allowed the development of radiopacity studies with more simpli-
fied and reproducible methodologies that can provide reliable results
(17, 18, 23, 27, 28). In a recent study comparing the radiopacity
measured with a digital system (radiographic density) and with
a photodensitometer (optical density), Baksi et al (28) concluded
that the use of a digital system for the measurement of radiographic
density is a viable option for the analysis of the radiopacity of
endodontic sealers and showed that the ISO standard for the radiopac-
ity of dental root canal sealing materials needs modifications for digital
systems. The methodology used in the present study is simple and
accessible, whereas the use of a photodensitometer for the analysis
of radiopacity of the materials in relation to the optical density requires
the use of more expensive equipment.
The addition of calcium hydroxide increased the film thickness of
AH Plus, being that the higher calcium hydroxide concentration
produced a thicker film probably because of the greater density and
lower flow of the sealer. The result obtained for pure AH Plus in the
present study was similar to those of a previous study (29) and better
than those of other investigations (20, 30).
The original AH Plus formulation presented lower solubility and
had similar results to those of other studies (29, 30). The addition of
calcium hydroxide increased the solubility, which favors the
occurrence of an alkaline pH and the release of calcium ions, as
reported elsewhere (11). Regarding the dimensional changes, all mate-
rials presented expansion above the limit recommended by the ANSI/
ADA’s specification no. 57, which is in accordance with the findings
of previous studies (20, 22, 29, 30) for the original AH Plus
formulation. It was also observed that the incorporation of calcium
hydroxide increased the sealer expansion although without
a statistically significant difference. The higher expansion values were
found when the 10% concentration used and could be attributed to
the hygroscopic action of calcium hydroxide, which might have
favored a higher water sorption and led to expansion of the material.
AH Plus sealer modified by the addition of 5% calcium hydroxide
showed similar physicochemical characteristics to AH Plus in radiopac-
ity, flow, setting time, solubility, and dimensional changes. AH Plus
sealer modified by the addition of 10% calcium hydroxide showed
similar radiopacity and setting time but lower flow than AH Plus. To
verify whether incorporating calcium hydroxide to the epoxy sealer
improves the biocompatibility certainly warrants further research in
the future.
JOE — Volume 36, Number 6, June 2010
Basic Research—Technology
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Physical Properties of AH Plus with and without Ca(OH)2. 1051