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Synthesis of Hydroxyapatite from egg shell and preparation of bone like Bio-
composites using it

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DOI: 10.15693/ijaist/2016.v52i52.36-47

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

Synthesis of Hydroxyapatite from egg shell


and preparation of bone like Bio-composites
using it
Prof. S.L.Pandharipande Miss. Smita S. Sondawale
Associate Professor, Department ofChemical M.tech Chemical Engineering student,
Engineering, L.I.T, RTMNU, Nagpur, India L.I.T, RTMNU, Nagpur, India
slpandharipande@gmail.com smitalit2012@gmail.com

Abstract – Hydroxyapatite (HAp) is an inorganic as Chitosan, Gelatin, Carboxymethyl Cellulose


constituent of human bone. Human bone contains (CMC), etc.
67% mineral matter, 22% collagen, 9% water and HAp can be synthesized effectively from egg
remaining proteins, carbohydrates, lipoids, etc. Bio- shell. The idea is to minimize the egg waste
composites that would resemble natural bone
accumulation caused by the day to day increase in
containing HAp as inorganic matter blended with
organic biomaterials are being researched. The consumption of eggs, due to the large demand of
present work is aimed at synthesis of HAp from egg the poultry products such as cakes, fast food, etc.
shell, silica from rice husk and bio-composites C1 to The disposal of egg shell waste in land may cause
C6 using varying compositions of HAp, silica, land degradation that can be minimized by
chitosan, carboxymethyl cellulose (CMC) & gelatin. effective utilization of egg shell in HAp synthesis.
Based on the Fourier Transform Infrared Also silica can be synthesized from rice husk. Rice
Spectroscopy (FTIR) analysis it can be said that HAp husk is a waste product of rice mill and can lead to
and silica are successfully synthesized. The bio- waste accumulation if not disposed of properly. It
composite of HAp with CMC & HAp with CMC,
contains 98% silica. Thus can be utilized in the
chitosan, gelatin & silica are tested for their
mechanical strength such as hardness & compressive synthesis of silica.
strength. The composite of HAp with CMC & The present work aims to synthesize
chitosan are tested for their antimicrobial property. biomaterials; HAp using egg shell, Silica using rice
The test results show that the composites have husk and bio-composites of HAp using different
comparable mechanical properties to that of organic biomaterials mentioned.
cancellous bone of human and also good
antimicrobial property. II. LITERATURE REVIEW
Index terms – Hydroxyapatite, Bone like bio-
i) Synthesis of Hydroxyapatite
composites, Egg shell, Compressive strength, Hardness,
antimicrobial property. Eric M. Rivera et al [3] have worked on
synthesis of hydroxyapatite from eggshell. In this
I. INTRODUCTION paper HAp was synthesized from egg shell by
thermally treating the egg shells The Calcium
Hydroxyapatite (HAp), Ca10(PO4)6(OH)2 is Oxide thus obtained was transformed into HAp in a
an important inorganic biomaterial consisting of phosphate solution. The Ca/P ratio of 1.67 was
calcium and phosphorous which are important used. The final product is characterized by X-ray
minerals found in human bone. Human bone diffraction and scanning electron microscopy SEM.
constitutes 67% mineral matter comprising HAp, Gre´ta Gergely [4] have worked on preparation
22 % organic matter which is mainly collagen, 9% and characterization of hydroxyapatite from
water and remaining is proteins, carbohydrates, eggshell and phosphoric acid as raw materials. The
polysaccharides etc. Thus, natural bone is a present work aimed to synthesize HAp via
composite of inorganic and organic matrix. It mechano chemical activation using ball milling and
consists of calcium and phosphorous in the ratio attrition milling and the phase stability and powder
1.67 which is same as the stoichiometric ratio characteristics were studied. The structures of the
present in the molecular formula of HAp [1],[2]. HAp were characterized by X-ray diffraction,
HAp provides sufficient toughness & hardness scanning electron microscopy and infrared
whereas the organic matrix provides the spectroscopy.
mechanical strength such as compressive & tensile P. Hui [5] have worked on synthesis of
strength to bone. Hence, composites of HAp with hydroxyapatite bio-ceramic powder by
certain organic polymers that resembles collagen hydrothermal method. Egg shells were treated
chemically can be used for bone grafting. The thermally for and the calcium oxide obtained was
organic part may be substituted by polymers such treated with Tricalcium Phosphate solution. The
final product was characterized by X-ray

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

diffraction, Scanning electron microscopy (SEM), III. PRESENT WORK


Fourier Transform Infrared Spectroscopy (FT-IR),
thermal analysis (TG–DTA). A. Methodology
Ahmed M. Saeed [6] have worked on
synthesis of calcium hydroxyapatite powder from The schematic of the process followed in the
hen’s eggshell and orthophosphoric acid. X-Ray present work [7] is given in figure 1.
diffraction (XRD) and Fourier Transform Infrared
(FT-IR) technique was used to investigate the
B. Materials
formation of HAP powder.
Glassware, egg shell, Diammonium Hydrogen
ii) Synthesis of Sillica Phosphate (DAP), Chitosan, Gelatin,
Carboxymethyl Cellulose CMC, rice husk.
K.V. Selvakumar [8] have worked on
extraction of Silica from burnt paddy husk.
Demineralization of rice husk was done using C. Method
sulphuric acid or nitric acid or hydrochloric acid.
Then the residue was treated with NaOH and the The present work is divided 3 parts:
filtrate so obtained was titrated with acid to obtain  Synthesis of Hydroxyapatite from Egg
the precipitate of silica. The effect of different shell
concentration of ascid and base on the yield of  Synthesis of Silica from Rice husk
silica yield of Silica was examined. The product  Synthesis of bio-composites
was analyzed using SEM.
Majid Monshizadeh [9] carried out the same i) Synthesis of HAp using Egg shell
procedure as above and used magnetic stirrer for The outline of the procedure [3-7] is as given
continuous stirring of the solution. Silica obtained below. The pictorial representation of the process is
was characterized using FTIR, XRD and SEM given in fig 2.
analysis.  Cleaned and boiled egg shells were treated
thermally at 700-8000C for 4 hrs and
iii) Synthesis of Bio-composites crushed to obtain CaO powder.
Subhadra Garai [10] worked on the  Samples of 0.6M DAP solution and 0.3M
synthesis of bio-composite of HAp with CMC. of CaO solution were prepared and mixed
The process consisted of mixing of polymeric in varying proportions thoroughly for 1 hr
solution of CMC with the calcium nitrate tetra under continuous boiling.
hydrate solution and then the solution mixture was  The precipitate of HAp obtained was
treated with di-ammonium hydrogen phosphate filtered using whatmann filter paper and
solution. Varying wt% ratio of CMC and HAp dried in oven at 800C for 4-5 hrs.
were used. The slurry was then dried in Teflon  The final product was sintered in furnace
molds at 500C for 72hrs. The bio-composite was
at 700-8000C for 1 hr.
tested by using FTIR, SEM, XRD and
compressive testing.  Three samples of HAp; P1, P2 &P3 are
Edgar B. Montufar [11] synthesized HAp- synthesized having same as
Gelatin composite scaffolds by mixing α – stoichiometric, half and quarter quantity of
tricalcium phosphate (α- TCP) with HAp and DAP respectively.
the Liquid phase of gelatin was prepared adding
Na2HPO4 as an accelerant. Both the liquid and ii) Synthesis of silica using rice husk
the powder phase were mixed and were molded or The outline of the procedure [8],[9] followed is as
placed into the syringe at room temperature. The given below and the pictorial representation of the
characterization were carried out before and after process is given in fig 2.
immersion of the composites in Ringer’s Solution  Rice husk was demineralized by boiling in
i.e; 0.9 wt% of NaCl solution and 100 % 1N HCl solution followed by heating for
humidity, using FTIR, SEM, XRD and 2hrs .
compressive testing.  Demineralized rice husk was washed till
Mehdi Kazemzadeh Narbat [12] neutral pH of washed water obtained.
synthesized HAp – Gelatin (GEL) composite with  Washed rice husk was then treated with
30, 40 & 50 wt % HAp composition. The 2.5 N NaOH for 2hrs at 80-1000C.
composites were prepared by directly mixing HAp
 The residue obtained was discarded & the
powder and the gelatin solution. The composites
filtrate was titrated with 1N HCl solution
were then molded into Teflon molds and
 The above solution was left to age for
Characterization was done using FTIR, SEM and
24hrs at ambient conditions.
mechanical testing.

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

 The precipitate of Silica obtained was  The further details of the composite in
filtered, oven dried and sintered in terms of its composition is given in table
furnace. 4.
 Two runs were carried out to prepare 2
The following 6 types of composites are
samples of silica.
prepared:
 Composite 1: C1: CMC + P1
iii) Preparation of Bio-composites  Composite 2: C2: CMC + P2
The outline of the procedure followed is as given  Composite 3: C3: CMC + P3
below:  Composite 4: C4: CMC + HAp + Chitosan
 The preparation of [10-12] bio-composites + Gelatin + Silica
consists of mixing of organic binders;  Composite 5: C5: CMC + HAp
Chitosan, Gelatin, Carboxymethyl  Composite 6: C6: CMC + HAp + Chitosan
Cellulose and inorganic components;
Hydroxyapatite and Silica .
 The Organic binders were prepared in gel
form by adding sufficient amount of
water.
 Hydroxyapatite was added to the gel of
organic binders and stirred till
homogeneous mixture was formed.
 The mixture was poured into cubical
molds and kept in deep freezer followed
by air drying for at least 3 days.

Egg
Shell
Organic Stoichiometric DAP (1)
binders

Hydrothermal Half stoichiometric (2)


DAp
method
Quarter Stoichiometric (3)

(1) (2) (3)


Gelatin Chitosan CMC FTIR
HA p HAp HAp Analysis
(P1) (P2) (P3)
SEM
C1

C2 FTIR

Analysis
C3 SEM
Chemical
C4 Silica treatment

C4
Rice Husk

C5
Compressive test

Mechanical testing Hardness test

Figure 1: Block diagram of the process followed

Egg Shell Boiling Drying in oven Dried egg shell Sintering

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

0.6M DAP solution 0.3 M CaO solution CaO powder

0.6M DAP Heating in oven Precipitate


+ 0.3 M CaO of HAp

Product HAp Sintering Air dried precipitate Filtration

Figure 2: Pictorial representation of HAp synthesis

Rice Husk HCl treatment Filtration NaOH treatment Filtration

Silica gel Filtration Acid treatment

Figure 3 : Pictorial representation of Silica Synthesis

(a) (b) (c) (d) (e) (f)

Figure 4 : Actual photographs of bio-composites synthesized a) C1 b) C2 c) C3 d) C4 e) C5 f) C6

IV. OBSERVATIONS
The details of the process parameters & the yield composites are given in tables 1, 2, 3 & 4
obtained in the synthesis of HAp, silica and bio- respectively

S Samp- Wt of Tempera- Time of CaO Water DAP Wat- Ca/ Wt of


r le egg ture of calcinati- formed added take- er P Pro-
n name shell calcinatio- on (gm) to CaO n adde- rati- duct
o (gm) n (hrs) (ml) (gm) d to o (gm)
(0C) DAP
(ml)
1 H-1 10 800-850 4 5 530 13 163 1.18 5.97

HS-1 The product H-1 was sintered at 800-8500C for 1hr

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

2 H-2 15 800-850 4 8 476 15 189 1.65 4


HS-2 The product H-2 was sintered at 800-8500C for 1hr
3 H-3 15 800-850 4 8 476 15 189 1.65 4
HS-3 The product H-3 was sintered at 800-8500C for 1hr
Table 1: Details of parameters for Synthesis of Hydroxyapatite

Sr no Sample name CaO Water added to CaO DAP Water added to DAP Ca/P ratio
(gm) (ml) (ml)
1 P1 4 238 7.5 94.70 1.65
2 P2 4 238 3.75 47.35 3.29
3 P3 4 238 1.875 23.68 6.59
Table 2: Details of parameters for synthesis of HAp by varying Ca/P ratio

Sr no Samp Wt of Vol & Hrs of Vol & Hrs of Vol of Vol Hrs Wt
-le RH normality HCl molarity NaOH filtrat of of of
name (gm) of HCl treat- of NaOH treatmen -e HCl treat- Sili-
solution ment taken -t (Na2Si solu ment ca
(ml) O3) -tion (gm
(ml) add- )
ed
(ml)
1 S-1 10 150ml 1N 24hrs
160ml 24 275ml 683 24 1.5
2.5M
SS-1 The product S-1formed was sintered at 800-8500C for 1hr
2 S-2 10 450ml 1N Boile- 180ml 2 ---- 130 24 0.7
d for 2.5N
2hrs
SS-2 The product S-2 formed was sintered at 800-8500C for 1hr
Table 3: Details of parameters for Synthesis of Silica

Sr no Composite name HAp Chitosan CMC Gelatin Silica


(gm) (gm) (gm) (gm) (gm)

1 C1 2.37 - 0.26 - -
2 C2 2.37 - 0.26 - -
3 C3 2.37 - 0.26 -
4 C4 4 0.25 0.6 0.25 1
5 C5 4 - 1 - -
6 C6 4 0.3 0.7
Table 4: Details of the composition of bio-composites (weight basis)

V. CHARACTERIZATION
i) FTIR analysis
The characterization is divided into two parts:
The FTIR analysis of the samples was done for
 Characterization of biomaterials determination of the various functional groups
 Characterization of bio-composites present that include OH-, PO43- in case of HAp and
Silinol OH group in case of silica. The fig no 5a,
A. Characterization of Biomaterials 5b, 5c, 5d, 5e, 5f, 5g & 5h show the graphs of FTIR
analysis of HS-1, H-2, HS-2, P-1, P-2, P-3, S-1 &
The biomaterials synthesized i.e; HS-1, H-2,
SS-1 samples respectively.
HS-2, P-1, P-2, P-3, S-1 & SS-2 were characterized
using FTIR and SEM techniques.
.

40
International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

(a) (b)

(c ) (d)

(e) (f)

(g) (h)

Figure 5: FTIR analysis of biomaterials synthesized a) HS-1 b) H-2 c) HS-2 d) P1 e) P2 f) P3 g) S-1 h) SS-1

ii) SEM analysis texture. The fig nos 6a, 6b, 6c & 6d shows the
The SEM analysis of HAp as well as silica SEM micrographs of HS-1, H-2, HS-2 & SS-1
samples was carried out to determine the surface respectively
morphology, approximate particle size and surface

41
International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

(a) (b)

( c) (d)

Figure 6: SEM micrograph of the biomaterials synthesized a) HS-1 b) H-2 c) HS-2 d) SS-1

B. Characterization of Bio-composites crosshead speed of 1mm/min. Fig 7a & 7b show


The bio-composites were tested for the load vs displacement characteristics of sample
compressive strength, hardness and anti-microbial C4 & C5 respectively. The details of dimensions
properties. of the cubical slabs along with the details of
mechanical compressive strength is given in table
i) Compressive strength testing 5.
The specimen was compressed between two
square plates of 5cm x 5cm dimension with a

(a) (b)
Figure 7: Load vs Displacement characteristics of bio-composites a) C4 b) C5

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

Sample Bio-composite Cross Sectional Maximum load Strain Compressive


no Name area (mm2) (KN) (%) strengths (MPa)
Initial Final
1 C4 86.47 - 0.142 41.39 1.642
2 C5 85.42 57.86 2.435 38.55 28.503
Table 5 Compressive strength of composites

ii) Hardness or Fracturability test a distance of about 4 mm. Fig no 8a, 8b & 8c show
The samples C1, C2, C3 are tested for hardness the force vs time characteristic of bio-composites
or fracturability using cylindrical flat probe of 2 C1, C2 & C3 respectively. The table 3.6 shows the
mm diameter. The penetration speed of the probe hardness of the samples.
during testing was 1mm/sec and was penetrated to

Fo rce (g ) F Fo rce (g ) F
D1 D1

Time (sec)
Time (sec)

(a) (b)

Fo rce (g ) F
D1

Sample Bio- Cross Maximum Hardness


no composite sectional load (GPa)
Name area of (KN)
probe
(m2)
1 C1 3.14 x 62.24 19.8
10-6
2 C2 3.14 x 55.53 17.7
10-6
3 C3 3.14 x 55.01 17.5
10-6
Time (sec)
Table 6: Hardness of bio-composites

(C)

Figure 8: Force vs time characteristic of bio-composite


a) C1 b) C2 c) C3

iii) Anti microbial property testing agar media for its anti microbial property over
HAp is an inorganic biomaterial having 48hrs.
strong resistance to microbial growth. The
incorporation of organic binders into the inorganic VI. RESULTS & DISCUSSION
HAp must not alter its antimicrobial properties.
The bio-composite should exhibit similar The following sections give the detailed
antimicrobial property. Hence, bio-composite C6 discussion on various observations related to
having HAp + Chitosan + CMC, is tested in Blood synthesis & analysis of bio-composite materials as

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
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presented in the previous section. The discussion is of HS-1, H-2 & HS-2, and S-1 & SS-2 is given in
presented in 5 parts: Synthesis, FTIR, SEM, table 7 and 8 respectively.
compressive, hardness and antimicrobial property As seen from the table 7, the FTIR analysis of
test. three HAp samples are confirmatory of presence of
all the functional groups. The peak for CO32- is
A. Synthesis results of HAp and Silica seen additionally due to the substitution of either
The present work has successfully synthesized OH- or PO43- by the CO32- group during the
HAp and Silica. The process parameters were atmospheric contact of the product. The FTIR
chosen at optimal condition based on literature graphs of the samples P1, P2, P3 show the peaks
review. The yield of CaO from egg shell is around for all the functional groups. The difference in the
50%. In Run-1 the Ca/P ratio was less as compared depth of the CO32- peak. The depth is seen
to Run-2 and 3. In Run-2 and 3 the Ca/P ratio is increasing with increase in the Ca/P ratio i.e;
according to stoichiometry and any undissolved decrease in the phosphate content. The reason may
Ca(OH)2 is discarded. The physical observations of be due to increase in the possibility of substitution
HAp synthesized is indicative of its formation of CO32- group in place of OH- or PO43- [1].
based on color, size and texture. The FTIR analysis of silica samples i.e; S-1
Similarly the yield of silica synthesized varies and SS-1 show that the non sintered silica (S-1)
from 7-15% and its formation is visually supported shows the peak for silinol OH present. This may be
by its white color, crystalline fine powder structure due to the presence of absorbed H2O molecules
and texture. which disappears in the sintered silica sample (SS-
1). The peaks for the Si-O-Si bond and vibration of
the gel network are seen in both the samples which
B. Interpretation of FTIR graphs
constitutes the structural formula of silica [8], [9].
The interpretation of FTIR graphs is necessary
to confirm the presence of various functional
groups. This is usually done by mapping the graphs
of FTIR of samples with those of standard
functional group as reported in literature. The
detailed interpretation of FTIR graphs of 4 samples

Sr Sample Vibrational frequencies (cm-1)


no name
PO43- OH- CO32-
Stretching Bending
Symmetric Asymmetric
1 HS-1 963.04 1019.57 675.73, 3398.41, 2358.82,
600.40 1632.44 1414.32
2 H-2 962.33, 1022.80 600.49, 3638.4, 1418.10,
450.97 559.62 1652.06 873.52,
3242.02 2881.81,
2161.61

3 HS-2 961.79, 1087.00, 562.94, 3640.54, 1418.28


469.19 1022.24 599.21, 3571.55,
629.39 1652.90
4 P-1 962.18, 1022.32 601.38, 3214.96, 2882.90,
462.25 559.90, 1641.54 2159.87,
500.50 1422.64
5 P-2 962.51, 1022.53 600.22, 3208.46 2883.44,
454.56 559.84 2517.08,
2159.91,
1413.32
6 P-3 962.51, 1025.75 600.79, 3696.32, 2881.27,
469.79 561.98 3638.08, 2506.01,
3225.52 2159.81,
1410.22
Table 7: FTIR interpretation of HAp samples

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

Sr Sample Vibrational frequencies (cm-1)


no name
Silinol OH group Siloxane bonds (Si-O-Si) Vibration mode of gel
network

1 S-1 3750.35, 3744.24, 1052.24, 1497.05, 1489.30, 1473.07, 795.51, 668.24


3734.78, 3710.84, 1450.92, 1436.32, 1418.72
3689.01, 3675.12,
3628.58, 3618.71,
3587.29, 3566.68
2 SS-1 NA 1063.52, 1448.40 787.19
Table 8: FTIR interpretation of Silica samples

C. SEM analysis matter. Also they act as binders. The


The interpretation based on SEM micrographs can combination of these have given the best
be summarized as follows: composites in the form of C5.
 Sample HS-1 show agglomerate formation
E. Hardness and Fracturability test
with pores not necessarily interconnected.
There is indication of inhomogeneity in The hardness of the samples C1, C2 & C3
the surface morphology of the sample. composed of HAp and CMC in the ratio 90:10 are
 Non-sintered sample H-2 as well as in the range of 17-19 GPa The hardness is more
sintered sample HS-2 show a micro sized than that of the hardness of cancellous bone ; 0.345
grain agglomerates with interconnected GPa and that of cortical bone; 0.396 GPa [13].
structures. The size may be ranging from
2-5 micro meter or even less than that. F. Microbial testing
 HS-2 sample is observed to be more The application of composites synthesized in
uniform in size and structured particles are present work are in biomedical field and
formed. Whereas non sintered sample has particularly in bone grafting. The anti microbial
varied nature of size and shape of properties of these bio-composites is thus
particles. important. Based on the test report of sample C5
 The sintered silica sample i.e; SS-1 has comprised of HAp, Chitosan & CMC, it can be said
needle shaped crystalline particles having that it posess anti microbial properties and no
size of 10 micro meter in length and upto growth of micro organisms was observed for 48 hrs
1 micrometer in diameter. [14].
VII. CONCLUSION
D. Compressive strength testing
The interpretation of compressive strength of The present work addresses to synthesis of
composites as mentioned in table 3 is given below: bio-composites of HAp, CMC, gelatin, silica &
 The thickness reduction of various chitosan. The main aim of the present work is to
samples that can be expressed as % strain synthesize bio-composites that resemble natural
ranged between 38-40 % and. The % bone. Natural bone constitutes inorganic to organic
strain is defined as (original thickness- matter in the ratio of 70 : 30. In the present work
Final thickness)/Original thickness x 100. HAp is used as an inorganic biomaterial source
 The composite formed by addition of whereas CMC, gelatin & chitosan are tried as
silica to HAp, CMC, Chitosan and Gelatin organic biomaterial source. The methodology of
showed compressive strength of 1.642 the present work includes synthesis of HAp and
MPa. This is least amongst the two and silica and their bio-composites using mentioned
may be due to non homogeneity of biomaterials.
composite due to the addition of silica. Based on the FTIR analysis of HAp and silica
 The compressive strength of sample C5 samples, it can be said that these biomaterials are
comprising of HAp and CMC is 28.503 successfully been synthesized. Three sample of
MPa. bio-composites C1, C2 & C3 having 90:10
 The purpose of addition of CMC, composition (wt%) of HAp and CMC are
Chitosan and gelatin to HAp is to make it synthesized. Similarly C5 is synthesized using
more like a natural bone containing 67% same biomaterials with 80:20 composition (wt%).
inorganic matter and remaining organic C6 contains HAp, CMC & chitosan .having

45
International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

inorganic to organic ratio of 80:20. C4 contains 5 and Nanotechnology, ISBN: 978-953-307-235-


biomaterials; HAp, silica, chitosan, CMC & 7.
gelatin. 3. Eric M. Rivera, Miguel Araiza , Witold
The composites C1, C2 & C3 are tested for Brostow, Victor M. Castan, J.R. D´ıaz-Estrada,
R. Herna´ndez, J. Rogelio Rodr´ıguez
hardness test and its value is in the range of 19-17 ,Synthesis of hydroxyapatite from eggshells;
GPa, greater than the hardness of cancellous and Materials Letters 41 (1999). 128–134.
cortical bone of human. The sample C4 & C5 are 4. Gre´ta Gergely, Ferenc We´ber , Istva´n
tested for compressive strength. The compressive Luka´cs , Attila L. To´th , Zsolt E. Horva´th,
strength of sample C4 is 1.642 MPa and that of C5 Judit Miha´ly, Csaba Bala´zsi, Preparation and
is 28.503 MPa. The strength of C4 is less as characterization of hydroxyapatite from
compared to cancellous bone which is in the range eggshell; Ceramics International 36 (2010)
of 2-20MPa. The reason may be due to insufficient 803–806.
amount of organic matter to bind the inorganic 5. P. Hui, S.L. Meena, Gurbhinder Singh, R.D.
Agarawal, Satya Prakash, Synthesis of
components i.e; HAp & silica. The strength of Hydroxyapatite Bio-Ceramic Powder by
composite C5 is greater than that of cancellous Hydrothermal Method, Journal of Minerals &
bone. Composite C6 is tested for its antimicrobial Materials Characterization & Engineering, Vol.
property and it was found that there was no 9, No.8, pp.683-692 (2010).
microbial growth within 48 hrs. 6. Ahmed M. Saeed, Raaed A. Hassan ,Khalid M.
Thus, it can be concluded that the present work Thajeel, Synthesis of calcium hydroxyapatite
has successfully synthesized bone like bio- powder from hen’s eggshell; Iraqi Journal of
composites using HAp, CMC, gelatin, silica & Physics, (2011) Vol. 9, No.16, PP. 24-28.
chitosan which has comparable mechanical as well 7. Smita S. Sondawale, August 2016, Synthesis
of Hydroxyapatite from egg shell and
as antimicrobial properties to that of human bone. preparation of bone like bio-composites from
it, Major project report submitted to RTMNU,
Nagpur.
8. K.V. Selvakumar, A. Umesh, P. Ezhilkumar, S.
VIII. ACKNOWLEDGEMENT Gayatri, P. Vinith, V. Vignesh, Extraction of
Silica from Burnt Paddy Husk, International
 The authors are thankful to Director L.I.T, Journal of ChemTech Research, Vol.6, No.9,
RTMNU, Nagpur, for the facilities and pp 4455-4459 (2014).
encouragement provided. 9. Manee Sumran, Paisan Kongkachuichay,
 The authors are thankful to H.O.D, Food Synthesis of Silica from Rice Husk by One
Step Combustion, Fluidized Bed Combustion
technology department, L.I.T, RTMNU,
and Alkaline Extraction, KKU Engineering
Nagpur, for hardness test. Journal Vol.30 No.2 (165-172), 2003.
 The authors are thankful to H.O.D, 10. Subhadra Garai, Arvind Sinha, Biomimetic
Physics department, University campus, nanocomposites of carboxymethyl cellulose–
Nagpur, for SEM analysis hydroxyapatite: Novel three dimensional load
 The authors are thankful to H.O.D, bearingbone grafts, Colloids and Surfaces B:
Chemical and Metallurgical department, Biointerfaces 115 (2014) 182–190.
V.N.I.T, Nagpur, for FTIR analysis and 11. Edgar B. Montufar, Tania Traykova, Etienne
Schacht, Luigi Ambrosio, Matteo Santin, Josep
compressive test. A. Planell, Maria-Pau Ginebra, Self-hardening
 The authors are thankful to Parate calcium deficient hydroxyapatite/gelatine
Pathology laboratory for Antimicrobial foams for bone regeneration, J Mater Sci:
test. Mater Med (2009).
 The authors are thankful to India mart for 12. Mehdi Kazemzadeh Narbat, Fariba Orung,
providing DAP samples. Mehran Solati Hashtjin, Azadeh Goudarzi,
Fabrication of Porous Hydroxyapatite-Gelatin
Composite Scaffolds for Bone Tissue
IX. REFERENCES
Engineering, Iranian Biomedical Journal 10
(4): 215-223 (2006).
1. Shekhar L. Pandharipande, Smita S. 13. Sumit Pramanik, Avinash Kumar Agarwal, and
Sondawale, Review on the characterization K. N. Rai, Development of High Strength
methods of Hydroxyapatite and its Bio- Hydroxyapatite for Hard Tissue Replacement,
composites, International Journal of Science, Trends Biomater. Artif. Organs, Vol 19 (1), pp
Engineering and Technology Research 46-51 (2005).
(IJSETR) Volume 5, Issue 7 (2016). 14. H. S. Ragab et al, Synthesis and In Vitro
2. Anton Ficai, Ecaterina Andronescu, Georgeta Antibacterial Properties of Hydroxyapatite
Voicu and Denisa Ficai (2011). Advances in Nanoparticles, IOSR Journal of Pharmacy and
Collagen/Hydroxyapatite Composite Materials, Biological Sciences (IOSR-JPBS) e-ISSN:
Advances in Composite Materials for Medicine 2278-3008, p-ISSN:2319-7676. Volume 9,
Issue 1 Ver. VI (Feb. 2014), PP 77-85.

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International Journal of Advanced Information Science and Technology (IJAIST) ISSN: 2319:2682
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47

Author’s Profile credit as coworker and has more than 60 papers


published in journals of repute.
Shekhar Pandharipande is an
Associate Professor in Chemical
Engineering Department of
Laxminarayan Institute of Smita Sondawale is a M.tech (Chemical
Technology, Rashtrasant Tukadoji Maharaj Engineering) student from Laxminarayan Institute
University, Nagpur. He did his masters in 1985 & of Technology, Nagpur.
joined LIT as a Lecturer. He has coauthored three
books titled ‘Process Calculations’, ‘Pririnciples of
Distillation’ & ‘Artificial Neural Network’. He has
two copyrights ‘elite-ANN’ & ‘elite-GA’ to his

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