Abstract
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A composite based on three components, including PMMA (Polymethyl Methacrylate), HA (Hydroxyl
Apatite), and LDH (Layered Double Hydroxide), was prepared, characterized, and applied as bone cement.
Bone cement is a biomaterial used for hip and knee joint replacements in clinical applications. Four types
of bone cements are used in dentistry and orthopedics. Including a) acrylic cements based on PMMA and
b) PPF (Polypropyl Fumarate) cements. For decades, polymerized methacrylates have played a pivotal
role in the construction of denture bases, serving as a reliable and widely used material in dentistry.
PMMA polymer is synthesized by free radical polymerization. LDH with the general formula of [M(II)1-
x M(III)x (OH)2 ]x+ .(An- )X/n ·mH2 O has M(II) and M(III) cations and An- inter-layer anion. The importance of LDH is for its planar layered structure. HA is a thermodynamically stable calcium phosphate similar to the
human hard tissues in morphology and composition. [M(II)1-x M(III)x (OH)2 ]x+ .(An- )X/n · mH2 O has M(II) and M(III) cations and an An- inter-layer anion. The importance of LDH is its planar, layered structure. HA is
a thermodynamically stable calcium phosphate similar in morphology and composition to human hard
tissues. In this work, we made a green Zr-Ni LDH and combined it with PMMA and HA in a specific ratio.
The composite is characterized using XRD, FTIR, and SEM analyses.
Keywords: PMMA; HA; LDH; Bone cement; Mechanical properties
Introduction
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Poly Methyl Methacrylate (PMMA) has received significant attention in recent years and
is regarded as one of the most efficient and promising polymers, with applications in diverse
fields [1]. Polymerized methacrylates have been commonly used to make denture bases for
many decades. PMMA polymer is synthesized by free radical polymerization and exhibits low
batch variation compared to other natural or raw polymers. Due to its easy maintenance and
low manufacturing costs, PMMA has been used in numerous applications [1]. Prior to the use
of PMMA as a biomaterial, there was a lot of chemical research done. According to legend, the
discovery of “acide acrylique” occurred in 1843. This is derived from ‘acreolan’, the latin word
for vinegary, acid or acrid and refers to the penetrating smell of the monomer. It was discovered
in 1936 that combining finely ground PMMA powder with a liquid monomer produced a doughy
substance. The PMMA monomer’s partial dissolution is to blame for this. Polymer chains
from the PMMA become available for free radical polymerization, and entanglements of these
chains with newly formed chains lead to an intimate connection between the newly formed
chains [2,3]Jeremy MAhn, Dongchan Eldred, Donald
V Fielitz, Alyssa J Heyl, Tyler R Lee,
Myoungbae Mangold, Shane Pearce, Eric ZReinhardt, Carl W Roggenbuck, Cheryl %J
Macromolecules Photocured
Simultaneous and Sequential PDMS/PMMA Interpenetrating Polymer Networks</
title></titles><pages>5826-5839</pages><volume>55</volume><number>13</
number><dates><year>2022</year></dates><isbn>0024-9297</isbn><urls></urls></
record></Cite></EndNote>.</p>
<p>Layered Double Hydroxides (LDH), which are one type of layered materials and are also
known as anionic clays, are promising layered materials due to some of their interesting
properties, such as ease of synthesis, unique structure, uniform
distribution of different metal cations in the brucite layer, surface
hydroxyl groups, flexible tunability, intercalated anions with
interlayer spaces, swelling properties, oxo-bridged linkage, high
chemical and thermal stability, and ability to intercalate different
types of anions [4,5]. The general formula for these LDHs is (Mg<sub>1–
x</sub>Al<sub>x</sub>(OH)<sub>2</sub>)<sup>x+</sup>(A–)<sup>x-</sup>nH<sub>2</sub>O, where ‘‘A’’ represents the interlamellar
anion that restores the electroneutrality of the compound. We call
these the II-III LDHs. We recently reported that the preparation of
Zn-Ti LDH and Co-Ti LDH consisting of di- and tetra-valent cations
is possible [6,7]. The present work examines the possibility of
preparing another example consisting of bi- and tetra-valent
cations, LDH, by a mechanochemical route that has been known as
a green method.</p>
<a id="Experimental Methods" class="pm">
<h4>Experimental Methods</h4></a>
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<p><b>Synthesis of Ni-Zr LDH in a mortar</b></p>
<p>Ni-Zr LDH were prepared by a mechanochemical route with a
simple and green mechanical grinding method [8]. NaOH pellets
(4.5g, 112.5mmol) were added to a powder mixture of nickel (II)
nitrate hexahydrate (9.16g, 31.5mmol) and zirconium nitrate
(5.79g, 13.5mmol) and manually ground to a paste. The paste
was washed four times with deionized water (20mL), dried under
vacuum at 40 °C, powdered, and analyzed [9].</p>
<p><b>Synthesis of three-component composite</b></p>
<p>In this case samples were prepared with 3%(w/w) of
hydroxyapatite and 0,1,3,5,7,10%(w/w) LDH. In the first step
hydroxyapatite, PMMA and LDH powder were thoroughly combined
at the designated weight percentage. The MMA liquid was then
added to the mixture. The mixture was kept in a vacuum state for
30 seconds to let gases escape. To prepare composie tablets, the
mixture was added to the cast and waited for it to become hard.</p>
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<p><b>Ni/Zr LDH characterization</b></p>
<p>Figure 1 shows XRD pattern which indicates that the Ni-Zr LDH
was directly synthesized. Two sharp peaks in different 2θ 10.31,
20.33, 34.02, 38.08, 44.80, 60.49 and 61.50 were referred to (003),
(006), (012), (015), (018), (110) and (113) plates, respectively
[10]. The FTIR spectrum of Ni-Zr LDH was shown in Figure 2.
The widespread and intense band in the 3446cm-1 area is due to
the stretch vibrations of O-H groups present in the interlayer and
water molecules, which are in layers. 1625cm-1 is related to water
bending vibrations. The sharp bands in 1379cm−1 and 827cm−1
are related to stretch and bending vibrations of interlayer nitrate
anion, respectively. However, the band seen in 1357cm−1 is related
to CO3
2- which is caused by existing CO2 in deionized water [6,8].
Figure 3 shows the infrared spectrum of the virgin sample; the C=O
stretching vibration of the ester group appears around 1725cm−1,
the two doublet bands at (1140, 1190cm-1) and (1240, 1265cm-1)
correspond to the C-O stretching vibrations of ester groups. The
absorptions around 1440 and 1480cm-1 characterize, respectively,
the asymmetric bending vibrations of the (C-CH3) and (C−CH2)
bonds [11].</p>
<p><strong>Figure 1:</strong>The XRD pattern of Ni-Zr LDH.</p>
<center><a href="../images/NPMS.000511.G001.png"target="_blank"><img src="../images/NPMS.000511.G001.png" title="Click here to view Large image 1" width="60%"></a></center>
<br>
<p><strong>Figure 2:</strong>FTIR spectrum of Ni-Zr LDH.</p>
<center><a href="../images/NPMS.000511.G002.png"target="_blank"><img src="../images/NPMS.000511.G002.png" title="Click here to view Large image 2" width="60%"></a></center>
<br>
<p><strong>Figure 3:</strong>FTIR spectrum of PMMA.</p>
<center><a href="../images/NPMS.000511.G003.png"target="_blank"><img src="../images/NPMS.000511.G003.png" title="Click here to view Large image 3" width="60%"></a></center>
<br>
<P><B>Scanning electron microscopy</B></P>
<P>The method was selected to investigate the morphology and
particle size of Ni-Zr LDH. Figure 4 shows FE-SEM images, which
indicate that the Ni-Zr LDH plates were directly synthesized.</P>
<p><strong>Figure 4:</strong>The LDH FE-SEM images.</p>
<center><a href="../images/NPMS.000511.G004.png"target="_blank"><img src="../images/NPMS.000511.G004.png" title="Click here to view Large image 4" width="60%"></a></center>
<br>
<p><b>Three component composite images</b></p>
<p>Figure 5 shows images of three component composite with 0,
1,3,5,7 and 10%(w/w) LDH, respectively. Pores were not observed
for 1 and 3% (w/w) of LDH. Figure 6 shows an image of a threecomponent
composite with 5, 7, and 10% (w/w) LDH, respectively.
That indicates pores will increase with an increasing percentage
of LDH. This phenomenon causes an increase in the concentration
of tension and a decrease in the strength of the composite. Due to
the increase in LDH percentage and hydroxyl groups, the active
sites of polymer will be occupied, and the porosity will increase.
Figure 7 shows the relationship between the force applied to the
composite and its displacement, which is the method to calculate
the composite modulus. This figure Shows good repeatability of
the nanoindentation test of the sample with 3% (w/w) LDH, which
indicates the test is reliable. Table 1 explains that three-component
composites have the best elastic modulus with 5% of LDH. With
3% hydroxyapatite and 5% LDH, PMMA’s elastic modulus rises to
15.3%, approaching the mudolus of human bone.</p>
<p><strong>Figure 5:</strong>Images of three component composite with 0, 1,3,5,7 and 10% (w/w) LDH.</p>
<center><a href="../images/NPMS.000511.G005.png"target="_blank"><img src="../images/NPMS.000511.G005.png" title="Click here to view Large image 5" width="60%"></a></center>
<br>
<p><strong>Figure 6:</strong>Images of a three-component composite with 5, 7, and 10% (w/w) LDH.</p>
<center><a href="../images/NPMS.000511.G006.png"target="_blank"><img src="../images/NPMS.000511.G006.png" title="Click here to view Large image 6" width="60%"></a></center>
<br>
<p><strong>Figure 7:</strong>Force-displacement diagram of 5 sample with 3% LDH.</p>
<center><a href="../images/NPMS.000511.G007.png"target="_blank"><img src="../images/NPMS.000511.G007.png" title="Click here to view Large image 7" width="60%"></a></center>
<br>
<p><strong>Table 1:</strong>Comparison of 0%, 1%, 3%, 5%, 7% and 10%(
w/w) LDH elastic modulus.</p>
<center><a href="../table/NPMS.000511.T001.png"target="_blank"><img src="../table/NPMS.000511.T001.png" title="Click here to view Large table 1" width="70%"></a></center>
<br>
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<li><a href="#Conclusion">Conclusion</a></li>
<li><a href="#References">References</a></li>
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<p>Ni-Zr LDH were proposed to compose with cement bone
because of micro sized particle of LDH and Zr mechanical properties.
Micro size of LDH will prevent from concentration of tension and
decreasing strength of composite. But pores will increase in macro
size by increasing of percentage of LDH. This phenomena cause
increasing of concentration of tension and decrease of strength of
composite. In addition 5% of LDH will increase the elastic modulus
15%, which approaches human bone elasticity modulus.</p>
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<ol>
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<li><a href="https://pubmed.ncbi.nlm.nih.gov/14585704/">Hendriks J, Horn JRV, Mei HCVD, Busscher HJ (2004) Backgrounds of antibiotic-loaded bone cement and prosthesis-related infection. Biomaterials 25(3): 545-556.</a></li>
<li><a href="https://pubs.acs.org/doi/epdf/10.1021/acs.macromol.2c00425">Beebe JM, Ahn D, Eldred DV, Fielitz AJ, Heyl TR, et al. (2022) Photocured simultaneous and sequential PDMS/PMMA interpenetrating polymer networks. Macromolecules 55(13): 5826-5839.</a></li>
<li><a href="https://www.sciencedirect.com/science/article/abs/pii/S0169131717305707">Mishra G, Dash B, Pandey S (2018) Layered double hydroxides: A brief review from fundamentals to application as evolving biomaterials. Applied Clay Science 153: 172-186.</a></li>
<li><a href="https://pubmed.ncbi.nlm.nih.gov/34216900/">Mittal J (2021) Recent progress in the synthesis of layered double hydroxides and their application for the adsorptive removal of dyes: A review. J Environ Manage 295: 113017.</a></li>
<li><a href="https://link.springer.com/article/10.1007/s10853-007-2097-5">Saber O (2007) Preparation and characterization of a new nano layered material, Co-Zr LDH. Journal of Materials Science 42(23): 9905-9912.</a></li>
<li><a href="https://pubs.rsc.org/en/content/articlehtml/2021/nj/d0nj04890a">Toole ON, Lecourt C, Suffren Y, Toche F, Chiriac R, et al. (2021) Intercalation of a manganese (II)-thiacalixarene luminescent complex in layered double hydroxides: Synthesis and photophysical characterization. New J Chem 45(1): 343-350.</a></li>
<li><a href="https://www.sciencedirect.com/science/article/abs/pii/S0926337321003441">He F, Zhuang J, Lu B, Liu X, Zhang J, et al. (2021) Ni-based catalysts derived from Ni-Zr-Al ternary hydrotalcites show outstanding catalytic properties for low-temperature CO<sub>2</sub> Applied Catalysis B: Environmental 293: 120218.</a></li>
<li><a href="https://onlinelibrary.wiley.com/doi/abs/10.1002/zaac.200801287">Ay NA, Karan BZ, Mafra L (2009) A simple mechanochemical route to layered double hydroxides: Synthesis of hydrotalcite‐like Mg‐Al‐NO<sub>3</sub>‐LDH by manual grinding in a mortar. Journal of inorganic and general chemistry 635(9‐10): 1470-1475.</a></li>
<li><a href="https://aiche.onlinelibrary.wiley.com/doi/abs/10.1002/ep.13744">Motandi MK, Zhang Z, Inkoua S, Yan L (2022) Application of zirconium modified layered double hydroxide and calcination product for adsorptive removal of phosphate from aqueous solution. Environmental Progress & Sustainable Energy 41(2): e13744.</a></li>
<li><a href="https://link.springer.com/article/10.1007/s10854-023-10549-w">El Morsy MA, Awwad NS, Ibrahium HA, Bajaber MA, Farea MO, et al. (2023) Optical and electrical conductivity improvement of polystyrene/polymethyl methacrylate blend embedded by silver nanoparticles for electrical devices. Journal of Materials Science: Materials in Electronics 34(14): 1162.</a></li>
</ol>
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<p>© 2022. Faranak Manteghi. This is an open access article distributed under the terms of the <a href="https://licensebuttons.net/l/by/4.0/80x15.png">Creative Commons Attribution License </a>, which permits unrestricted use, distribution, and build upon your work non-commercially.</p>
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<script type="text/javascript">
function checkspecial_menuscript(evt){
//alert();
var charCode;
if (window.event)
{
charCode = window.event.keyCode;
//alert(charCode);
}
else
charCode = evt.which; //for firefox
if (charCode == 39) //for <space> symbol
return false;
if (charCode == 34) //for <space> symbol
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if (charCode == 62) //for <space> symbol
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if (charCode == 35) //for <space> symbol
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if (charCode == 43) //for <space> symbol
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if (charCode == 126) //for <space> symbol
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if (charCode == 96) //for <space> symbol
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return true;
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function checkspecial(evt)
{
//alert();
var charCode;
if (window.event)
{
charCode = window.event.keyCode;
// alert(charCode);
}
else
charCode = evt.which; //for firefox
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{
return false;
}
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return false;
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return false;
if (charCode == 60) //for <space> symbol
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if (charCode == 33) //for <space> symbol
return false;
if (charCode == 64) //for <space> symbol
return false;
if (charCode == 35) //for <space> symbol
return false;
if (charCode == 36) //for <space> symbol
return false;
if (charCode == 37) //for <space> symbol
return false;
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return false;
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return false;
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return false;
if (charCode == 126) //for <space> symbol
return false;
if (charCode == 96) //for <space> symbol
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if (charCode == 47) //for <space> symbol
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if (charCode == 58) //for <space> symbol
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if (charCode == 59) //for <space> symbol
return false;
// cust code
var notin = [44, 91, 93, 123, 125, 92, 124, 50, 45];
// var tt = notin.indexOf(charCode);
if(notin.indexOf(charCode) > -1)
return false;
// if (charCode == 32) //for space symbol
// return false;
// if (charCode == 44) //for , symbol
// return false;
// if (charCode == 46) //for . symbol
// return false;
// if (charCode == 91) //for [ symbol
// return false;
// if (charCode == 93) //for ] symbol
// return false;
// end cust code
return true;
}
function checkspecialname(evt)
{
//alert('hi');
var charCode;
if (window.event)
{
charCode = window.event.keyCode;
}
else
charCode = evt.which; //for firefox
//alert(charCode);
if (charCode == 39) //for <space> symbol
return false;
if (charCode == 44) //for <space> symbol
return false;
if (charCode == 35) //for <space> symbol
return false;
if (charCode == 33) //for <space> symbol
return false;
if (charCode == 123) //for <space> symbol
return false;
if (charCode == 125) //for <space> symbol
return false;
if (charCode == 91) //for <space> symbol
return false;
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return false;
if (charCode == 34) //for <space> symbol
return false;
if (charCode == 61) //for <space> symbol
return false;
if (charCode == 60) //for <space> symbol
return false;
if (charCode == 62) //for <space> symbol
return false;
//if (charCode == 33) //for <space> symbol
// return false;
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return false;
if (charCode == 37) //for <space> symbol
return false;
if (charCode == 94) //for <space> symbol
return false;
if (charCode == 38) //for <space> symbol
return false;
if (charCode == 42) //for <space> symbol
return false;
if (charCode == 40) //for <space> symbol
return false;
if (charCode == 41) //for <space> symbol
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if (charCode == 43) //for <space> symbol
return false;
if (charCode == 126) //for <space> symbol
return false;
if (charCode == 96) //for <space> symbol
return false;
if (charCode == 63) //for <space> symbol
return false;
if (charCode == 47) //for <space> symbol
return false;
if (charCode == 58) //for <space> symbol
return false;
if (charCode == 59) //for <space> symbol
return false;
return true;
}
function onlyNumericMobile(evt,id=null)
{
var charCode;
if (window.event)
{
charCode = window.event.keyCode;
// alert(charCode);
}
else
charCode = evt.which; //for firefox
if(charCode>=48 && charCode <=57)
{
return true;
}else{
return false;
}
// if((charCode>=97 && charCode <=122)||(charCode>=65 && charCode <=90))
// {
// return false;
// }
// alert(charCode)
// if (charCode == 39) //for <space> symbol
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// if (charCode == 34) //for <space> symbol
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// if (charCode == 60) //for <space> symbol
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// if (charCode == 62) //for <space> symbol
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// if (charCode == 33) //for <space> symbol
// return false;
// if (charCode == 64) //for <space> symbol
// return false;
// if (charCode == 35) //for <space> symbol
// return false;
// if (charCode == 36) //for <space> symbol
// return false;
// if (charCode == 37) //for <space> symbol
// return false;
// if (charCode == 94) //for <space> symbol
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// if (charCode == 38) //for <space> symbol
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// if (charCode == 42) //for <space> symbol
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// if (charCode == 41) //for <space> symbol
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// if (charCode == 95) //for <space> symbol
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// if (charCode == 43) //for <space> symbol
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// if (charCode == 126) //for <space> symbol
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// if (charCode == 96) //for <space> symbol
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// if (charCode == 63) //for <space> symbol
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// if (charCode == 47) //for <space> symbol
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// if (charCode == 58) //for <space> symbol
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// if (charCode == 59) //for <space> symbol
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// if (charCode == 45) //for <space> symbol
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// return true;
// return true;
}
function urlSpecial(evt)
{
var charCode;
if (window.event)
{
charCode = window.event.keyCode; //for IE
//alert(charCode);
}
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charCode = evt.which; //for firefox
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return false;
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return false;
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return false;
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return false;
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return false;
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return false;
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return false;
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return false;
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return false;
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return false;
if (charCode == 63) //for <space> symbol
return false;
if (charCode == 94) //for <space> symbol
return false;
if (charCode == 123) //for <space> symbol
return false;
if (charCode == 124) //for <space> symbol
return false;
if (charCode == 125) //for <space> symbol
return false;
if (charCode == 126) //for <space> symbol
return false;
if (charCode == 91) //for <space> symbol
return false;
if (charCode == 93) //for <space> symbol
return false;
return true;
}
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