International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol 3 .
, 2022 .
https://ijeise.
id/ E-ISSN: 2721-8775 Article Synthesis of Hydrosiapatite from Muscle Shell Waste Using The Precipitation Method Ika Nawang Puspitawati1,a*.
Aziz Hafizh Tauhid1.
Abdullah Tsani M.
K1.
Lucky Indrati Utami1,b, and Kindriari Nurma Wahyusi1,c 1 Chemical Engineering Department.
Engineering Faculty.
Universitas Pembangunan Nasional AuVeteranAy.
East Java.
Surabaya, 60294.
Indonesia E-mail: aikanawangpuspita@gmail.
com , bluckyindrati02@gmail.
com, ckindrinurma@gmail.
*Corresponding author: .
kanawangpuspita@gmail.
Received: 30th October 2022.
Revised: 9th November 2022.
Accepted: : 23rd November 2022.
Available online: 23 November 2022.
Published regularly: May and November.
Abstract Hydroxyapatite is a calcium phosphate compound that is the main inorganic component of bones and Hydroxyapatite has a main role in the medical world because of its identical chemical properties and structure to human bone.
Kupang shells have a high CaCO3 content of 95-99% by weight.
So this concurrence, the mussel shells are to be used as good as an ingredient for making Hydroxyapatite.
The variables used in this research are Temperature of the Furnace and Phosphoric Acid Concentration, which were 700AC, 750 AC, 800 AC, 850 AC, 900 AC and Phosphate Acid Concentrations 0.
4M, 0.
8M, 1M, and 1.
The product results were tested with XRD analysis to determine the crystal structure contained in the product and the level of Hydroxyapatite in the product.
The best research results in this study at a temperature of 900AC at a concentration of 1.
2M phosphoric acid with a Hydroxyapatite content of 100% with lattice parameters an (AA)=b (AA) = 9.
422, c (AA)=6.
8835, and gamma = 120A.
Keywords: Hydroxyapatite.
Precipitation.
Temperature.
Concentration Introduction Indonesia is an archipelagic country located between two large oceans, specifically the Pacific Ocean and the Indian Ocean, so it has excellent fishery potential resources .
Kupang is one of the marine biota or shellfish with a small size that lives on the bottom of the waters and is a fishery product that is commonly found in the coastal waters of Sidoarjo.
East Java.
Kupang is processed into a special food, lontong Kupang, favoured by the people of Sidoarjo and Surabaya.
Food production is carried out daily, so the mussel shell waste produced is also abundant .
That is one of the reasons for using research In addition, the main constituent of mussel shells is CaCO3, with 95-99% by weight.
Therefore, mussel shells can be a high source of calcium .
Through the right technology, mussel shell waste can be a product with high economic value, namely hydroxyapatite or .
ydroxyapatite/HA.
Hydroxyapatite (HA.
is a kind of apatite material [M10(XO.
with the chemical formula Ca10(PO.
6OH2.
The composition of the constituent elements .
n ideal weight %) is Ca 9%.
P 18.
H 0.
O 41.
41%, and the ideal calcium-phosphate (Ca-P) ratio is 1.
The type of crystal structure of hydroxyapatite can be monoclinic or hexagonal.
The Monoclinic hydroxyapatite structure was gained only under composition, while the hexagonal hydroxyapatite structure was generally obtained from nonstoichiometric hydroxyapatite synthesis.
The lower the (Ca-P) molar ratio value, the more DOI:10.
4186/ijeise.
id/E-ISSN: 2721-8775 International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol 3 .
, 2022 acidic it is and the more soluble it is .
The monoclinic structure (Fig.
is due to the OHarrangement forming the OH-OH-OH-OHsequence, whereas the hexagonal structure (Fig.
can also be obtained under stoichiometric conditions if the OH- the arrangement is irregular .
The precipitation method is the leading wet chemical widely used to synthesise This technique can synthesise large amounts of HA without using organic solvents and is inexpensive.
This method uses sundry precursors that have contents of calcium and phosphate, such as calcium hydroxide (Ca(OH).
and phosphoric acid (H3PO.
Water is the only by-product, and the reaction does not involve foreign elements .
10 Ca(OH)2 6 H3PO4 E Ca10(PO.
6(OH)2 18 H2O
Fig.
1 Monoclinic Hydroxyapatite (HA.
Structure Fig.
2 Hexagonal Hydroxyapatite (HA.
Structure Hydroxyapatite (HA.
has a density of 3.
g/cm3 and a molecular weight of 502.
31 g/mol.
Hydroxyapatite is a bioceramic compound in solid form.
The components of hydroxyapatite are similar to those of bone.
In the collagen matrix network in bone, hydroxy ions (OH-) can be replaced by F-.
Cl-, and CO32-.
One of the applications of hydroxyapatite (HA.
can be used as bioceramics in the medical and dental fields.
Hydroxyapatite has bioactive, osteoconductive properties and low electrical and thermal conductivity.
In addition, hydroxyapatite has excellent biocompatibility properties and a high affinity for biopolymers.
Hydroxyapatite can be synthesised by mixing calcium precursors with phosphate precursors.
Various methods have been developed to make hydroxyapatite by previous researchers, including the hydrothermal method.
the sol-gel method and the precipitation method The precipitation process is an acid-base reaction that produces crystalline solids .
eaction salt.
and water.
The advantages of this method are the process with cheap raw materials, relatively simple chemical reactions, and the size and homogeneity of the particle sizes obtained tend to be good.
A simple process with yields >87% makes it very suitable for large-scale .
production, the absence of foreign contaminants and the only byproduct produced is water, requiring inexpensive reagents.
Also.
Ca/P products with the composition of varying phases can be obtained .
Previous researchers have synthesized hydroxyapatite from cow bone waste Yenti et al.
The materials used for Ca and P precursors are Ca(OH)2 and H3PO4.
Then it was found that hydroxyapatite was more dominant at a (Ca-P) ratio of 1.
As well as variations in the concentration of H3PO4.
HAp was more dominant at concentrations of 0.
8 and 1.
H3PO4 .
This research will use the precipitation method with different raw materials from mussel shell waste.
The resource calcium comes from the shell of mussels and phosphoric acid by controlling the temperature or even the concentration of the solvent.
Material and Method 1 Material The primary material of mussel shells used in this study was mussel shells in Balungdowo Village.
Candi sub-district.
Sidoarjo district.
East Java.
Other ingredients include phosphoric acid and NaOH purchased at the Ngagel Jaya Kimia shop.
Surabaya.
DOI:10.
4186/ijeise.
id/E-ISSN: 2721-8775 International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol 3 .
, 2022 2 Production of Hydroxyapatite Synthesis This research uses a series of calcination tools consisting of a furnace and a furnace pot for synthesising Hydroxyapatite using a magnetic stirrer, glass beaker, and stir bar.
The series of tools for the hydroxyapatite synthesis process below with the following descriptions of numbers 1 to 4 sequentially, namely aluminium cover, glass beaker, stirrer bar, magnetic stirrer at room temperature for 24 hours.
After that, the precipitate formed was filtered using Whatman 42 filter paper.
Then the precipitate was dried using an oven at 100oC for 5 hours.
The dry precipitate obtained was then heated at a temperature corresponding to the changing variables .
oC, 750oC, 800oC, 850oC, 900oC) for 3 hours to increase the degree of crystallinity.
10Ca(OH)2 6H3PO4 -E Ca10(PO.
6(OH)2 18H2O 6 Hydroxyapatite Analysis with XRD Fig.
3 The Set Up of Hydroxyapatite Synthesis The variable used is the stirring speed of 300 rpm, and the pH is set to 10.
The variable changes in this study are the furnace temperature of 700AC, 750AC, 800AC, 850AC, and 900AC and the concentration of phosphoric acid is 0.
1M and 1.
3 Preparation of Primary Material Preparing primary materials begins with cleaning the mussel shell with a brush and running water.
Then it is dried in the open air and under the sun.
Then it was pulverized with a wooden pulverizer to a powder size of about 100 4 Calcination Process After the mashed mussel shells, it calcined in a furnace at 900 AC for 5 hours.
After it was calcined, the mussel's shell was then sieved with a mesh sieve according to the provisions of 100 Mesh.
5 Hydroxyapatite Synthesis Process The calcium hydroxide suspension was stirred at 300 rpm for 1 hour while the temperature was maintained at 90AC, and the pH was adjusted to 10.
Then the mixture was aged The characterization of the synthesized hydroxyapatite was carried out using X-ray Diffraction (XRD).
Before being used, the tool is calibrated first and the control XG .
n the form of curren.
, water flow, shutter and door open are set.
While waiting for the calibration of the instrument, as much as 2 mg of the sample was placed in the holder of the diffractometer.
The voltage used is 40 Kv and the generator current is 30 mA with a wavelength source of 1.
The results obtained in the form of a diffractogram identified based on the intensity and angle of 2.
Determination of the emerging phase refers to the Joint Committee on Powder Diffraction Standard (JCPDS).
Results and Discussion Kupang Shell Calcination The calcination process in mussel shell waste aims to eliminate organic components and convert the initial compound calcium carbonate (CaCO.
into Calcium Oxide (CaO) compounds which will later be used as Calcium (C.
The calcination proces at a temperature of 250AC.
The water will evaporate then all organic components will be oxidized below a temperature of 450AC.
At a temperature of 540AC, calcium carbonate (CaCO.
decomposition into CaO at a temperature of 750AC .
CaCO3 E CaO CO2 HAp was synthesized using the precipitation method with variable furnace temperatures of 700AC, 750AC, 800AC, 850AC, and 900AC.
The hydroxyapatite was tested using XRD analysis, and the results were compared to standard DOI:10.
4186/ijeise.
id/E-ISSN: 2721-8775 International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol 3 .
, 2022
Effect of Temperature Concentration HAp Temperatu 900AC 850AC 800AC 750AC 700AC I) 9,41 9,413 9,41 9,38 9,35 c .
I) 6,879 6,876 6,87 6,87 6,88 Gamma
(A)
Fig.
The Graph of Concentration HAp versus Temperature (AC) Table 1 shows that at a temperature of 900AC the best value got 100% hydroxylapatite acid, lattice parameters an (AA) = b (AA) = 9.
41, c (AA) = 6.
879, and gamma = 120A.
That shows that the crystal structure of the product is close to the literature, which shows the lattice parameters a = b = 9.
432 AA, c = 6.
881 AA, and gamma = 120A.
Based on Figure 4.
shows that the higher the temperature equivalent with the yield of hydroxyapatite obtained, and at a concentration 4 M phosphoric acid with the lowest value at a temperature of 700AC and the good results at a temperature of 900AC, the following graphs of XRD analysis results at a concentration of phosphoric acid at 900AC.
Fig 6.
The Graph of result Analysa XRD with Posphate Acid Concentration 0.
8M and Temperature 900 AC The graph above shows the position of the angle 2: 34.
0467 also obtained a hydroxyapatite intensity of 100% with a height of 606.
71 cts.
Fig.
5 The Graph of result Analysa XRD with Posphate Acid Concentration 0.
4M and Temperature 900 AC In the graph, a temperature of 900AC and concentration of 0.
4 M peaks the highest intensity at an angle of 2: 34.
hydroxyapatite 100% obtained with 455.
Table 1.
Hydroxyapatite kisi parameter value Table 2.
Hydroxyapatite kisi parameter value Tempera 900AC 850AC 800AC 750AC 700AC I) 9,418 c .
I) 6,8835 6,884 6,885 6,883 6,881 Gamma
(A)
9,412 9,424 9,423 9,421
Table 2.
it can be seen that the excellent value was had at a temperature of 900AC, which is 100% hydroxylapatite acid, with lattice DOI:10.
4186/ijeise.
id/E-ISSN: 2721-8775 International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol 3 .
, 2022 parameters an (AA) = b (AA) = 9.
418, c (AA) = 8355, and gamma = 120A.
of the hydroxyapatite intensity is 100% at the peak altitude of 784 cts.
Concentration 0,4 M Concentration 0,6 M Figure 7.
Graph of XRD analysis results at a concentration of 1.
2M phosphoric acid at a temperature of 900 AC Concentration 0,8 M The perfect result where the concentration 2M with a temperature of 900AC shows an angle position of 2: 31.
7092 with a 100% Hydroxyapatite presentation with a height of 784 Concentration 1 M Table 3.
Hydroxyapatite kisi parameter value Tempera 900AC 850AC 800AC 750AC 700AC I) 9,422 c .
I) 6,8835 6,886 6,89 6,869 6,84 Gamma
(A)
9,42
Concentration 1,2 M
9,418 9,414 9,41
Based on table 3.
it showed that at a temperature of 900AC the finest value was obtained, which is hydroxyapatite acid of 100%, with lattice parameters an (AA) = b (AA) = 9.
c (AA) = 6.
8835, and gamma = 120A.
The product's crystal structure is close to the literature, which shows a = b = 9.
432 AA, c = 881 AA, and gamma = 120A of the lattice According to the picture below, the hydroxyapatite of the diffractogram shows a similar characterisation result pattern from the XRD analysis of hydroxyapatite from the JCPDS Committee on Powder Diffraction Standards Data.
According to de Wolf (JCPDS 09- 0.
, the three significant peaks of hydroxyapatite are at 2.
77A, 32.
90A and 32.
19A respectively.
The concentration of 1.
2M is close to the current value at 2.
The value Fig 8.
Graph of the comparison of all concentrations at a temperature of 900AC Conclusions The shell waste of mussel shells can be used as the primary material for the manufacture of Increasing temperature would make the intensity of hydroxyapatite that would be produced more The concentration of phosphoric acid does not affect the product's concentration but affects the product's lattice parameters.
The best results were at a temperature of 900AC and at a concentration of 1.
2 M phosphoric acid, which obtained 100% hydroxyapatite acid, with lattice parameters an (AA) = b (AA) = 9.
422, c (AA) = 8835, and gamma = 120A.
References