scholarly journals PENGARUH WAKTU KALSINASI TERHADAP SIFAT FISIKA-KIMIA HIDROKSIAPATIT DARI CANGKANG GELOINA COAXANS

2020 ◽  
Vol 13 (2) ◽  
Author(s):  
Pepi Helza Yanti ◽  
Yendro Gandi

Hidroksiapatit (HAp) merupakan salah satu senyawa biokeramik yang digunakan dalam berbagai aplikasi.  Pada penelitian ini telah dilakukan sintesis hidroksiapatit (HAp) dengan metode pengendapan menggunakan cangkang lokan (Geloina coaxans) dan H3PO4  sebagai prekursor. Analisis menggunakan X-Ray Flourocence (XRF) menunjukkan bahwa komposisi kimia utama pada cangkang lokan (Geloina coaxans) adalah CaO.  Produk terbaik diperoleh melalui waktu kalsinasi pada suhu 900 oC selama 180 menit yang ditunjukkan dengan puncak yang memiliki intensitas tertinggi pada 2θ = 31,7o dan puncak spesifik lainnya untuk hidroksiapatit pada 2θ = 32,89o, 32, 17o, 25,86o dan 49,46o. Difraktogram dibandingkan dengan JCPDS (No 09-0432). Berdasarkan perhitungan menggunakan persamaan Scherrer, didapatkan ukuran kristal dari hidroksiapatit (HAp) adalah 26,62 nm. Analisis menggunakan FTIR juga telah dilakukan untuk mengidentifikasi gugus fungsi pada hidroksiapatit yang diperoleh. Dari spektrum FTIR menunjukkan adanya pita serapan yang khas untuk gugus  OH‒, CO32- dan PO43-pada hidroksiapatit. Morfologi partikel berbentuk granular seperti bola dan gumpalan yang tidak seragam diperoleh melalui analisis menggunakan SEM.. ABSTRACT  Hydroxyapatite (HAp) is a bioceramic compound that is used in various applications. In this research, hydroxyapatite (HAp) synthesis has been carried out by precipitation method using Geloina coaxans shell and H3PO4 as precursors. Analysis using X-Ray Flourocence (XRF) showed that the main chemical composition of Geloina coaxans shell was CaO. The best product was obtained by calcination at 900 oC for 180 minutes indicated by a peak having the highest intensity at 2θ = 31.7o and other specific peaks for hydroxyapatite at 2θ = 32.89o, 32 ,17o, 25.86o and 49.46o. The difractogram was compared to JCPDS (No 09-0432). Based on calculations using the Scherrer equation, the crystallite size of hydroxyapatite was 26.62 nm. Analysis using FTIR has also been carried out to identify the functional groups of the hydroxyapatite obtained. The FTIR spectrum showed that there were unique absorption bands  for OH‒, CO32- and PO43- groups on hydroxyapatite. Analysis using SEM showed that the morphology was granular like balls and non-uniform aggregate

2021 ◽  
pp. 889-896
Author(s):  
Hanan J. Mustafa ◽  
Tagreed M. Al-Saadi

To study the removal of lead (Pb) ions from aqueous solutions, novel magnetite nanoparticles (NPs) of Ni0.31Mg0.15Ag0.04Fe2.5O4 were synthesized by coprecipitation synthesis using metal sulfates, and then coated with Gum Arabic (GA). The prepared NPs were analyzed using various spectroscopic and analytical methods, such as X-Ray diffraction analysis (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Energy Dispersive X-ray spectroscopy (EDX), Fourier Transform Infra-Red spectroscopy (FT-IR), and Atomic Absorption Spectrophotometer (AAS). By using XRD analysis, the cubic inverse spinel structure of the prepared NPs was proven, showing average values of crystallite size, lattice constant, and density of 28.57nm, 8.32582Å, and 5.2890 g/cm3, respectively. FE-SEM analysis revealed the sphere-like shape of the nanoparticles with a measured crystallite size of 25.93nm. The existence of constituent elements was evidenced by EDX. FT-IR test proved the success of the coating process of magnetite NPs by the presence of the main characteristic absorption bands of GA in the FT-IR spectrum of GA-magnetite NPs. The adsorption of Pb ions by GA- magnetite NPs was shown by AAS analysis, where the concentration of Pb ions decreased from 25ppm to 6.6ppm, reaching 1.1ppm at the time of 25min. The porosity of the NPs and the carboxyl groups in GA played an important role in the process.


2016 ◽  
Vol 30 (32n33) ◽  
pp. 1650347
Author(s):  
Amarjeet ◽  
Vinod Kumar

[Formula: see text] ([Formula: see text] = 0.1, 0.3 and 0.5) nanoparticles were prepared by chemical co-precipitation method. The developed nanoparticles were characterized for structural properties by powder X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) techniques. Peak position in the X-ray diffraction pattern confirmed the single spinel phase of the developed particles. Infrared (IR) spectroscopy in mid-IR range showed the presence of characteristic absorption bands corresponding to octahedral and tetrahedral bonds in the spinel structure of prepared samples. Thermo-gravimetric analysis (TGA) measurements showed a considerable weight loss in the developed samples above 700[Formula: see text]C. Frequency dependence of the electrical properties of the developed material pellets was studied in the frequency range of 1 kHz–5 MHz. Temperature dependence of the dielectric constant of [Formula: see text] was studied at different temperatures, i.e. at 425, 450 and 475 K, in the frequency range of 1 kHz–5 MHz. It was found that the electrical conductivity decreases with increasing Cu[Formula: see text] ion content while it increases with the increase in temperature.


2014 ◽  
Vol 675-677 ◽  
pp. 728-732 ◽  
Author(s):  
Hu Die Yuan ◽  
Hong Feng Yin ◽  
Yun Tang ◽  
Hang Shuai

Gasification slag is one of the solid wastes forming by water-granulation for molten liquid and residual carbon. In this paper, the basic characteristics of gasification slags from Texaco and Shell gasifier (termed as WH and QP, respectively) were studied. X-ray fluorescence (XRF), X-ray diffraction (XRD), optical microscope (OM), and scanning electron microscopy (SEM) were carried to investigate the chemical composition, phase constituents, petrographical structure and microstructure of the slag, respectively. The results showed that: (1) The main chemical composition of WH and QP is SiO2, Al2O3and CaO. In addition, a large amount of residual carbon is also existed in WH. (2) The main phases of WH and QP are vitreous glass and quartz. In addition, calcite is also detected in WH; (3) The microstructural features of the two slags are nearly the same. Residual carbon in WH is existed with laminar structure.


2021 ◽  
Vol 1160 ◽  
pp. 45-50
Author(s):  
Savitha Kadencheri Unnikrishnan

A facile method was successfully developed to prepare Ternary oxynitride of iron and gallium. Initially mixed oxyhydroxides of Iron and gallium were prepared by co-precipitation method. Then this was nitrided using urea and agar in presence of ammonia at 900°C, which gave mixed cation oxynitride . This mixed oxynitride was characterized using XRD, XPS and SEM. The X-ray diffraction pattern of the Fex’GaxOyNz phase was refined within the cubic spinel structure (space group Fd-3m), using the fullprof program. On assuming 3+ oxidation state for half of iron and whole of gallium, the chemical composition of the oxynitride spinel determined by the X-ray analysis is Fe2GaN2O2. The refinement using these parameters resulted in a good fit to the observed diffraction data, with a crystallographic R factor of 5.92. This ternary oxynitride of iron and gallium is a novel material which can give unique optical and magnetic properties.


2016 ◽  
Vol 3 (02) ◽  
pp. 158
Author(s):  
Iis Nurhasanah ◽  
Nurul Wahyu Puspaningrum ◽  
Ida Nursati

<span>Nanoceria has been proposed as inorganic material for sunscreen product because of its <span>excellent UV absorpsition ability. Fine particle nanoceria and non-aglomeration determines <span>comport and covering capability on human skin. Particle size and aglomeration could be <span>controlled by parameters and medium synthesis. In the present work, nanoceria powders were <span>synthesized using precipitation method in different pH of 7 and 10. Precipitation was caried<br /><span>out in water/isopropanol mixed solvent. Cerium nitrate and amonium hydroxide was used as <span>source of cerium and precipitation agent, respectively. Crystal structure of nanoceria was <span>examined using x-ray diffraction (XRD). Scanning electron microscope (SEM) was used to <span>observe morphology of nanoceria. Diffraction pattern analysis shows that the precipitates <span>were single phase of nanoceria with cubic fluorite structure and lattice contants of 0.5429 nm<br /><span>and 0.5419 nm. Crystallite size and lattice strain were obtained from Williamson-Hall method. <span>Precipitation in pH of 7 resulted in smaller crystallite size which correlated to the larger lattice <span>strain and lattice constant. SEM image shows spherical morphology with less agglomeration <span>occuring for nanoceria precipitated in pH 10.</span></span></span></span></span></span></span></span></span></span></span></span></span><br /></span>


2019 ◽  
Vol 32 (1) ◽  
pp. 49-52
Author(s):  
M. Jaganadha Rao ◽  
K.S.R. Murthy ◽  
Ch. Ravi Shankar Kumar ◽  
Anjali Jha ◽  
G.S.V.R.K. Choudary ◽  
...  

Present day technology requires synthesis of materials with low energy consumption, free mercury pollution and its reliability. A novel material with control of crystallite size, composition and simple for white light relies in synthesis of materials. The present focus of article attributes series of manganese doped Ca1-xMnxWO4 luminescent materials with co-precipitation method. Reported studies attempts with change in structure of calcium tungstate (CaWO4) are observed with dopants like Eu3+, Eu2+, Tb3+, etc. However the effect of Mn2+ on structural properties of CaWO4 are quite interesting. The synthesized samples were characterized with X-ray diffraction for lattice parameters, crystallite size and FTIR studies for bonding mechanism of O-W-O stretching and W-O-W bridge bond. Rietveld profile refinement of XRD patterns using MAUD program Ca1-xMnxWO4 revealed the Scheelite type structure with C4h point group and I41/a space group. Characterization studies reveal that doping of Mn2+ doping upto 0.1 in place of Ca2+ will not change the phase of Scheelite structure.


2018 ◽  
Vol 34 ◽  
pp. 02042 ◽  
Author(s):  
Rajeb Salem Hwidi ◽  
Tengku Nuraiti Tengku Izhar ◽  
Farah Naemah Mohd Saad

In Malaysia, limestone is essentially important for the economic growth as raw materials in the industry sector. Nevertheless, a little attention was paid to the physical, chemical, mineralogical, and morphological properties of the limestone using X-ray fluorescence (X-RF), X-ray diffraction (X-RD), Fourier transform infrared spectroscopy (FTIR), and Scanning electron microscopy / energy dispersive x-ray spectroscopy (SEM-EDS) respectively. Raw materials (limestone rocks) were collected from Bukit Keteri area, Chuping, Kangar, Perlis, Malaysia. Lab crusher and lab sieved were utilized to prepare five different size of ground limestone at (75 µm, 150 µm, 225 µm, 300, and 425 µm) respectively. It is found that the main chemical composition of bulk limestone was Calcium oxide (CaO) at 97.58 wt.% and trace amount of MnO, Al2O3, and Fe2O3 at 0.02%, 0.35%, and 0.396% respectively. XRD diffractograms showed characteristic peaks of calcite and quartz. Furthermore, main FTIR absorption bands at 1,419, 874.08 and 712.20 cm-1 indicated the presence of calcite. The micrographs showed clearly the difference of samples particle size. Furthermore, EDS peaks of Ca, O, and C elements confirmed the presence of CaCO3 in the samples.


2006 ◽  
Vol 309-311 ◽  
pp. 7-10
Author(s):  
S. Bertazzo ◽  
Celso A. Bertran

In this work, some modifications that occur in crystallites that compose the mineral phase of bone throughout the lives of animals were studied by X-ray diffractometry. The Debye-Scherrer equation was applied to the diffractograms, allowing the determination of the mean crystallite size and the changes in the mean crystallite size with relation to the diffraction planes 002 and 310. Likewise, the intensity of peaks in the diffractograms corresponding to the same diffraction planes was correlated with the number of crystallographic planes or of unit cells present in the crystallites.


2016 ◽  
Vol 72 (3) ◽  
pp. 385-390 ◽  
Author(s):  
Francisco Tiago Leitão Muniz ◽  
Marcus Aurélio Ribeiro Miranda ◽  
Cássio Morilla dos Santos ◽  
José Marcos Sasaki

The Scherrer equation is a widely used tool to determine the crystallite size of polycrystalline samples. However, it is not clear if one can apply it to large crystallite sizes because its derivation is based on the kinematical theory of X-ray diffraction. For large and perfect crystals, it is more appropriate to use the dynamical theory of X-ray diffraction. Because of the appearance of polycrystalline materials with a high degree of crystalline perfection and large sizes, it is the authors' belief that it is important to establish the crystallite size limit for which the Scherrer equation can be applied. In this work, the diffraction peak profiles are calculated using the dynamical theory of X-ray diffraction for several Bragg reflections and crystallite sizes for Si, LaB6and CeO2. The full width at half-maximum is then extracted and the crystallite size is computed using the Scherrer equation. It is shown that for crystals with linear absorption coefficients below 2117.3 cm−1the Scherrer equation is valid for crystallites with sizes up to 600 nm. It is also shown that as the size increases only the peaks at higher 2θ angles give good results, and if one uses peaks with 2θ > 60° the limit for use of the Scherrer equation would go up to 1 µm.


2011 ◽  
Vol 194-196 ◽  
pp. 730-733 ◽  
Author(s):  
Wen Qiang Zhang ◽  
De Yuan Zhang ◽  
Jun Cai

In order to fabricate flake-shaped core-shell micro particles (FCMP) with light weight efficiently, deposition on diatomite was carried out by thermal decomposition. The deposition of Fe on diatomite was accomplished by thermal decomposition of pentacarbonyl iron (Fe(CO)5). The scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), and X-ray diffraction (XRD) are used to make clear their morphology microstructure, chemical composition, and crystal structure. The average diameter of FCMP is around 40μm, and the average aspect ratio is over 15. The main chemical composition of the FCMP is Fe, Si, Oand C. The XRD result revealed that crystal structures of the FCMP is close to α-Fe. The vibrant sample magnetometer (VSM) result revealed that the FCMP belong to soft magnetic material. The density test results show that the density of FCMP is close to the 2.6, which is lower than the density of pure carbonyl iron powder.


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