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Synthesis of Hydroxyapatite from egg shell and preparation of bone like Bio-
composites using it
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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
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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
C2 FTIR
Analysis
C3 SEM
Chemical
C4 Silica treatment
C4
Rice Husk
C5
Compressive test
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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
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
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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 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
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
(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
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
(C)
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
Vol.52, No.52, August 2016 DOI:10.15693/ijaist/2016.v52i52.36-47
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
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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
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
46
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
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