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Journal of Dentistry 66 (2017) 32–36

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Journal of Dentistry
journal homepage: www.elsevier.com/locate/jdent

Effects of smear layer removal agents on the physical properties and MARK
microstructure of mineral trioxide aggregate cement

Nidambur Vasudev Ballala, Mrunali Sonab, Franklin R. Tayc,
a
Department of Conservative Dentistry & Endodontics, Manipal College of Dental Sciences Manipal University, Manipal, Karnataka, India
b
Department of Metallurgical & Materials Engineering, National Institute of Technology, Surathkal, Srinivasnagar, Mangalore, Karnataka, India
c
Department of Endodontics, The Dental College of Georgia, Augusta University, Augusta, GA 30912-1129, USA

A R T I C L E I N F O A B S T R A C T

Keywords: Objective: To compare the effect of QMix (Dentsply Sirona), 7% maleic acid (MA), and 17% ethylenediamine-
Ethylenediaminetetraacetic acid tetraacetic acid (EDTA) on the microhardness, flexural strength and microstructure of mineral trioxide aggregate
Flexural strength (MTA; ProRoot MTA, Dentsply Sirona).
Mineral trioxide aggregate Methods: Forty MTA specimens were divided into four groups: [I] QMix [II] 7% MA [III] 17% EDTA and [IV]
Microhardness
distilled water (control). After treatment with 5 mL of the respective solution for 1 min, the specimens were
Maleic acid
tested for microhardness using a Knoop hardness tester. Forty additional specimens were similarly treated and
QMix
Smear layer evaluated for the flexural strength using a universal testing machine. For microstructure evaluation, MTA spe-
cimens were treated in a similar manner and examined by X-ray diffractometry and scanning electron micro-
scopy (SEM).
Results: For microhardness, there were no differences between distilled water, QMix and EDTA groups.
However, MTA exposed to distilled water had higher microhardness than MA. When compared with QMix and
EDTA, MA had lower microhardness; there was no difference between EDTA and QMix. For flexural strength,
distilled water group had higher flexural strength than the other agents. There were no differences between
EDTA vs MA and EDTA vs QMix. Specimens treated with QMix had higher flexural strength than MA. X-ray
diffraction indicated that EDTA inhibited hydration of MTA. For SEM, all the tested agents altered the micro-
structure of MTA when compared to distilled water.
Conclusion: MA had more detrimental effect on the physical properties of MTA and EDTA was more detrimental
to the hydration of MTA.
Clinical significance: The present study highlights the effect of newer chelating agents on the physical properties
and microstructure of MTA. Preventing the deterioration of MTA is important for its long term success in en-
dodontic procedures.

1. Introduction environmental temperature and presence of air in the mixture may all
affect the physical properties of MTA [4,6]. Torabinejad et al. reported
Mineral trioxide aggregate (MTA) is a biocompatible tricalcium si- that MTA remains soft when it is used in the vicinity of an acidic en-
licate hydraulic cement with numerous applications in endodontics vironment, such as that present in severe inflammation [1]. Nilfor-
[1,2]. Its clinical applications include repair of resorption, pulp cap- oushan et al. reported that the setting behaviour of MTA is adversely
ping, perforation repair, root end filling, apexification, regenerative affected by the presence of alkaline-earth metal chlorides, including
endodontics and as a root canal sealer [1,2].When mixed with an sodium chloride [7]. Lee et al. reported that hydration of MTA is ad-
aqueous solution, ProRoot (white) MTA (Dentsply Sirona, Tulsa Divi- versely affected by an acidic environment, which results in weakening
sion, Tulsa, OK, USA) sets in approximately 3–4 h to form a hard ce- of the material’s microstructure [5].
ment composing mainly of calcium oxide, silicon oxide and bismuth Ideally, MTA should possess adequate strength especially when used
oxide [3]. It has been reported that MTA must be allowed to set in the as a furcation perforation repair material, where it will be subjected to
presence of moisture to optimise the material’s physical and chemical forces by occlusal loading. The strength of a brittle material such as
properties [4,5]. Factors such as particle size, powder-to-liquid ratio, MTA may be evaluated by measuring its compressive or flexural


Corresponding author.
E-mail address: ftay@augusta.edu (F.R. Tay).

http://dx.doi.org/10.1016/j.jdent.2017.08.018
Received 7 July 2017; Received in revised form 12 August 2017; Accepted 30 August 2017
0300-5712/ Published by Elsevier Ltd.
N.V. Ballal et al. Journal of Dentistry 66 (2017) 32–36

strength. Flexural strength testing provides a collective measure of both Microhardness was determined using a Knoop hardness tester
compressive stress on the upper surface and tensile stress on the lower (Matsuzawa Seiki Co. Ltd, Tokyo, Japan). Indentations were made with
surface of a specimen. It closely simulates the clinical situation because a Knoop diamond indenter on each specimen using 100 g force and 15 s
fatigue failure via continuous flexion is the principal contributor to the dwell time. The diamond-shaped indentations were examined with an
failure of tooth restorations [8,9]. Microhardness testing of MTA ex- optical microscope equipped with an image analysis software, to enable
posed to various root canal irrigants may be used as an indicator of its accurate measurement of their diagonals. The average length of the two
setting process and its overall strength or resistance to deformation diagonals recorded for each indentation was used to calculate the mi-
under various setting conditions [10]. crohardness value. Three measurements were made on the surface of
The goal of root canal treatment is to completely disinfect the root each specimen, and the mean value was taken as the hardness of that
canal system [11]. This may be achieved by mechanical instrumenta- particular specimen.
tion, irrigation with disinfecting solutions and the use of inter-ap-
pointment intracanal medicaments. Mechanical instrumentation of the 2.2. Flexural strength
root canal produces a smear layer which covers the dentinal tubules in
the canal wall [12]. Removal of the smear layer in bacteria-infected Forty ProRoot MTA beams (25 mm long and 2 mm thick) were
root canals enables more efficient penetration of intracanal medications prepared using a split mould. The MTA was mixed and placed in the
and irrigants into the dentinal tubules [13,14]. Various agents have mould in the manner previously described. The set specimens were
been used for the removal of smear layer. Ethylenediaminetetraacetic randomly divided into four groups(n = 10) and treated with the test
acid (EDTA) is a commonly used chelating agent for removing canal irrigants in the manner described for microhardness testing. All the
wall smear layers [15,16]. When EDTA is used as a final irrigant after specimens were subjected to three-point bending to analyze the flexural
the placement of MTA, the chelating agent may adversely affect the strength. The testing procedure consisted of placing the MTA beams on
physical and chemical properties of the set tricalcium silicate cement. two cylindrical rods mounted parallel to each other at a 20 mm dis-
17% EDTA interferes with the hydration of MTA, resulting in a set tance. The MTA beams were then loaded at the centre with the in-
cement with decreased microhardness, flexural strength and reduced denter. Testing was performed using a universal testing machine
biocompatibility [17,18]. (Model 3366, Instron Corp., Norwood, MA, USA). Flexural strength was
QMix® 2in1 (QMix; Dentsply Sirona, Tulsa Division) is a root canal determined using the equation S = 3PL/2bh2, where P = maximum
irrigant which contains EDTA, chlorhexidine, a detergent and water. It load (N), L = support span (mm), b = width of the specimen (mm),
has been reported that QMix removes canal wall smear layers as ef- and h = height of the specimen (mm). Data was expressed in
fectively as 17% EDTA [19]. Seven percent maleic acid (MA) is a root megaPascals (MPa).
canal irrigant that possesses better smear layer removal capability than
17% EDTA or QMix [20,21]. It is also less cytotoxic compared to17%
2.3. Microstructure
EDTA [22]. To date, no information is available on the effect of QMix or
7% MA on the microstructure and physical properties of MTA. Ac-
2.3.1. X-ray diffraction
cordingly, the objectives of the present in-vitro study were to compare
The crystalline phases of MTA after treatment with the test irrigants
the effect of QMix, 7% MA and 17% EDTA on the microhardness,
was determined by X-ray diffraction (XRD). Twelve rectangular-shaped
flexural strength and microcrystalline structure of MTA cement. The
ProRoot MTA specimens (5 mm long, 3 mm wide, 2 mm thick) were
null hypotheses tested were: (1) there are no differences in the potential
prepared and randomly divided into four groups (n = 3). The speci-
of QMix, 7% MA and 17% EDTA in reducing the microhardness and
mens were prepared and treated with the test solutions in the same
flexural strength of set MTA cement; and (2) there is no difference in
manner described for microhardness testing. After treatment with the
the microstructure of set MTA cement after it is treated with QMix, 7%
respective solution, the specimens were examined with an X-ray dif-
MA or 17% EDTA.
fractometer (JDX-8P-XRD, JEOL, Tokyo, Japan) using Ni filter and Cu
Kα radiation; the latter was generated at 30 kV and 20 mA. The spe-
2. Materials and methods
cimens were scanned from 10° to 60° 2θ and the data was collected in a
continuous scan mode at a scanning rate of 4°/min. Crystalline changes
2.1. Microhardness
was identified by a computer-automated system and compared with
Joint Committee on Powder Diffraction Standards (JCPDS) files.
Forty ProRoot MTA cylindrical shaped specimens (6 mm high, 4 mm
diameter) were prepared using a split mould. The MTA cement was
mixed according to the manufacturer’s instructions and packed into the 2.3.2. Scanning electron microscopy
mould using MTA carrier (Dentsply Sirona, Tulsa Division). The spe- Twelve cylindrical-shaped ProRoot MTA specimens (6 mm high,
cimens were stored in a 100% relative humidity chamber at room 4 mm diameter) were prepared using a split mould. The specimens were
temperature for 24 h. After the specimens were completely set, they randomly divided into four groups (n = 3) and treated with the test
were separated from the mould and were grounded flat using a pol- irrigants in the same manner described for microhardness testing. The
ishing machine with a series of ascending grades of silicon carbide specimens were rinsed and dehydrated subsequently using ascending
abrasive papers (500, 800, 1000, 1200 grit) under distilled water. Final grades of ethanol (25%, 50%, 75% and 100%) for 15 min each,
polishing was achieved with 0.1 μm alumina suspension (Ultra-Sol R, mounted on metal stubs, coated with gold using an ion-sputtering
Eminess Technologies. Scottsdale, Arizona, USA) on a rotary felt disk. machine and examined with a scanning electron microscope (SEM;
The polished specimens were randomly divided into four groups JSM-6010, JEOL). Images were taken to identify the surface char-
(n = 10) based on the irrigant used: [I] QMix:5 mL of QMix (pH 8.0) acteristics of the MTA specimens at 3500× magnification and 10 kV.
for 1 min; [II] MA: 5 mL of 7% MA solution (pH 1.3; MilliporeSigma, St.
Louis, MO, USA) for 1 min; [III] EDTA: 5 mL of 17% EDTA solution (pH 2.4. Statistical analysis
8.5; Vista Dental Products, Racine, WI, USA) for 1 min; and [IV] con-
trol: 5 mL of distilled water for 1 min. For all groups, the specimens Because the microhardness and flexural strength data appeared to
were immersed in a beaker containing the respective irrigant. A mag- have violated the normality and equal variance assumptions, the data
netic stirrer was placed inside the beaker to ensure complete wetting of were analyzed separately using Kruskal-Wallis analysis of variance and
the specimens with the irrigating solutions. After 1 min of treatment, all Dunn’s multiple comparison procedures. For all analyses, the sig-
the specimens were rinsed with distilled water and air-dried. nificance level was pre-set at α = 0.05.

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N.V. Ballal et al. Journal of Dentistry 66 (2017) 32–36

Table 1
Microhardness of the MTA specimens after treatment with different smear layer
removing agents.

Groups (n = 10) Microhardness*

Distilled water (control) 147.90 ± 19.84a


Ethylenediaminetetraacetic acid 144.40 ± 26.11a
QMix 142.60 ± 12.42a
Maleic acid 67.10 ± 15.36b

* Values are means ± standard deviations. Groups labelled with the same letter
superscripts are not significantly different (p > 0.05).

3. Results

3.1. Microhardness

Microhardness of the four groups are summarised in Table 1. There


was a significance difference in microhardness among the 4 groups
(p < 0.05). The MA group had significantly lower microhardness than Fig. 1. X-ray diffraction spectra of hydrated, set mineral trioxide aggregate specimens
the distilled water (control) group (p < 0.001), the QMix group after treatment with distilled water (control), ethylenediaminetetraacetic acid (EDTA),
QMix and maleic acid (MA). A: peaks corresponding to tricalcium silicate; B: dicalcium
(p < 0.001) and the EDTA group (p < 0.001). There was no sig-
silicate; C: tricalcium aluminate; P: portlandite; E: ettringite.
nificance difference between the microhardness of the control and
QMix, the control and EDTA, and between EDTA and QMix (p > 0.05
for all pairwise comparisons). experimental solutions are shown in Fig. 2. The microstructure of MTA
treated with distilled water (control) had needle-shaped crystals
3.2. Flexural strength (Fig. 2A). In the EDTA-treated (Fig. 2B) and the MA-treated MTA spe-
cimens (Fig. 2C), there were more amorphous materials among the
Flexural strength of the four groups are summarised in Table 2. exposed crystals. In the QMix treated group, the MTA surface had more
There was a significant difference in flexural strength among the 4 cuboidal-shaped crystals (Fig. 2D).
groups (p < 0.05). The flexural strength in the distilled water control
group was significantly higher than the other 3 experimental groups 4. Discussion
(p < 0.001). Flexural strengths of the three experimental groups were
in the order: QMix = EDTA > EDTA = MA (p < 0.05). The present study evaluated the effect of various smear layer re-
moval root canal irrigants on the microhardness, flexural strength and
3.3. X-ray diffraction microstructure of white MTA cement. Because treatment with7% MA
resulted in significantly lower microhardness and flexural strength of
Representative XRD patterns of MTA specimens treated with dif- the set MTA cement specimens, the first null hypothesis that “there are
ferent irrigants are shown in Fig. 1. The four groups all demonstrated no differences in the potential of QMix, 7% MA and 17% EDTA in re-
distinct peaks of tricalcium silicate [20]. The intensities of the tri- ducing the microhardness and flexural strength of set MTA cement” has
calcium silicate peaks were similar for the QMix, MA and distilled water to be rejected.
groups, which were considerably lower than the tricalcium silicate The adverse effect of 7% MA on the physical and quasistatic me-
peaks obtained for the EDTA group. Additional peaks of dicalcium si- chanical properties of set MTA may be attributed to acidity of this ir-
licate and tricalcium aluminate were also detected. These peaks cor- rigant (pH = 1.3). This finding is similar to the results achieved with
responded to similar unreacted mineral phases in the XRD spectrum of exposure of set MTA to other types of acidic solutions [5,24–27], in that
non-hydrated MTA powder (not shown). Additional peaks corre- an acidic environment is detrimental to the physical properties and
sponding to portlandite (crystalline calcium hydroxide) and small et- hydration behaviour of MTA. Deterioration of the mechanical proper-
tringite (hydrated calcium sulphoaluminate) peaks were seen in the set ties (compressive strength) of different tricalcium silicate cements in
hydrated specimens that were exposed to distilled water (control). The the presence of an acidic environment has also been reported [28]. As a
portlandite and ettringite peaks were not apparent in the MTA speci- hydraulic cement, MTA solidifies into a hard structure upon hydration
mens after exposure to EDTA, MA or QMix. of the dry cement powder [6]; dissolution of the non-hydrated mineral
phases is followed by crystallisation of the hydrates into an interlocking
3.4. Scanning electron microscopy mass [29]. When an acidic root canal irrigant comes in contact with the
set MTA, it causes dissolution of the poorly-crystallised calcium silicate
Representative SEM images of MTA treated with different hydrate (C-S-H) binding phase and reduces the cohesiveness of the
crystalline structure of the set cement [30]. This probably accounts for
Table 2 the reduction in microhardness and flexural strength. Acid-induced
Flexural strength of the MTA beams after treatment with different smear layer re- dissolution of the CSH phase in set tricalcium silicate cements has po-
moving agents. tential undesirable consequences when these cements are used in en-
dodontics as a sealer for filling material. These undesirable con-
Groups (n = 10) Flexural strength*
sequences may include reduction in margin sealing quality [31,32] as
Distilled water (control) 15.74 ± 0.60a well as reduction in dislocation resistance [33,34]. In contrast, reduc-
Ethylenediaminetetraacetic acid 5.13 ± 0.78b,c tions of the microhardness and flexural strength of MTA after treatment
QMix 5.72 ± 0.42b
with EDTA or QMix were minimal. This may be attributed to the neutral
Maleic acid 4.52 ± 0.38c
or alkaline pH of these two irrigants, which is less corrosive on the C-S-
* Values are means ± standard deviations. Groups labelled with the same letter H binding phase in the irrigant-treated cement [35]. Similar to the re-
superscripts are not significantly different (p > 0.05). sults of the present study, the solubility of different tricalcium silicate-

34
N.V. Ballal et al. Journal of Dentistry 66 (2017) 32–36

Fig. 2. Scanning electron microscopy images of hy-


drated, set mineral trioxide aggregate specimens
after exposure to [A] distilled water (control), [B]
17% EDTA, [C] 7% maleic acid and [D] QMix for
1 min.

based cements has been reported to be in the order: pH 4.4 > pH group, the intensity of the tricalcium silicate peaks were considerably
7.4 > pH 10.4 [36]. stronger than similar peaks present in the spectra derived from the
Changes in the physical and mechanical properties of MTA in the other groups. The tricalcium silicate peaks in the hydrated MTA spe-
presence of different root canal irrigants are reflected by alterations in cimens represent unreacted cement particles that are surrounded by the
the microstructure of the specimen surfaces. Hence, the second null reaction phases after the hydration reaction. The presence of much
hypothesis that “there is no difference in the microstructure of set MTA stronger tricalcium silicate peaks in the EDTA group suggests disruption
cement after it is treated with QMix, 7% MA or 17% EDTA” has to be of continuing hydration of MTA by EDTA. When compared to MA and
rejected. The presence of needle-like crystals on the set MTA cement QMix, EDTA may have chelated more Ca2+ ions from the MTA to form
surface of the control specimens (i.e. after treatment with distilled Ca-EDTA complexes. This probably leads to the reduction of reaction
water) is similar to the observation reported by Lee et al. [17]. These phases such as amorphous C-S-H and crystalline calcium hydroxide
needle-shaped crystals probably represent ettringite, the hydration re- (portlandite) due to lack of free calcium ions. It has also been reported
action product of calcium aluminate with water, in the presence of that EDTA decreased the apical sealing ability of MTA when used as a
gypsum (CaSO4). Nevertheless, hydration of tricalcium silicate cements root end filling material [41,42]. This may be attributed to the removal
produces predominantly C-S-H and portlandite [23,37,38]. The process of inorganic content of the smear layer by EDTA [43] and also its effect
proceeds in two stages: dissolution of the tricalcium complex in water, on MTA hydration.
and precipitation and crystallisation of the hydrated compounds
[39,40]. In contrast with MTA specimens that had been exposed to 5. Conclusion
distilled water, surfaces of MTA specimens treated with EDTA and MA
appeared less crystalline and more porous, probably due to the dis- The present study demonstrated that exposing a set mineral trioxide
solution of the ettringite and portlandite interlocking crystalline com- aggregate cement to maleic acid is more detrimental on its physical
ponents. These crystalline phases are important in interlocking the properties, when compared to exposing similar specimens to EDTA or
entire mass of the set, hydrated material [27]. Their disappearance may QMix. In addition, EDTA is more detrimental to the hydration of mi-
cause the material hardness to decrease as seen in the present study. neral trioxide aggregate cement than the other tested agents.
Cuboidal crystals were observed on the surface of MTA specimens
treated with QMix; these crystals were not identified from the other Acknowledgement
three groups. They probably represent crystallisation of a component
(EDTA, chlorhexidine or detergent) derived from the QMix irrigant that The authors thank Mrs. Marie Churchville for administrative sup-
leached out from the internal porosities of the set MTA cement. Al- port.
though the specimens were rinsed prior to ethanol dehydration, liquids
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