scholarly journals Determination of the Ca/P ratio in calcium phosphates during the precipitation of hydroxyapatite using X-ray diffractometry

2013 ◽  
Vol 7 (2) ◽  
pp. 93-95 ◽  
Author(s):  
Zoltan Zyman ◽  
Dmytro Rokhmistrov ◽  
Kateryna Loza
Keyword(s):  
Phase Composition ◽  
Calcium Phosphate ◽  
Initial Data ◽  
Calcium Phosphates ◽  
Diffraction Method ◽  
Synthesis Time ◽  
X Ray ◽  
Simple Processing ◽  
Wet Synthesis

The applicability of the X-ray powder diffraction method to the determination of phase composition and Ca/P ratio in precipitates during the nitrous wet synthesis of hydroxyapatite (HA) has been shown. The plotted dependences of the phase composition and the Ca/P ratio on the synthesis time can be used as initial data for the development of new and simple processing routes of calcium phosphate ceramics based on HA of any desired composition.

Control of the phase composition of advanced calcium phosphates using an x-ray diffractometer with a curved position-sensitive detector

2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov
Keyword(s):  
Phase Composition ◽  
Calcium Phosphates ◽  
Position Sensitive Detector ◽  
Sensitive Detector ◽  
X Ray Diffraction ◽  
X Ray ◽  
Impurity Phases ◽  
Position Sensitive ◽  
Diffraction Peaks ◽  
Diffraction Patterns

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.

Study on Synthesis of Calcium Phosphate Biomaterials Containing SMB

2007 ◽  
Vol 330-332 ◽  
pp. 1033-1036 ◽  
Author(s):  
M.H. Li ◽  
Shu Xin Qu ◽  
R. Shen ◽  
N. Yao ◽  
P.D. Ren ◽  
...  
Keyword(s):  
Calcium Phosphate ◽  
Salvia Miltiorrhiza ◽  
Reaction System ◽  
Absorption Peak ◽  
X Ray Diffraction ◽  
Wet Chemical Method ◽  
Obvious Effect ◽  
X Ray ◽  
Wet Chemical ◽  
Wet Synthesis

Calcium phosphate (CaP) biomaterials containing Chinese medicine, Danshen (Salvia Miltiorrhiza Bunge, SMB), have been synthesized in our previous study via the wet chemical method. However, CaP biomaterials were generally synthesized in the alkaline solution. The purpose of the present study was to investigate the effect of pH on SMB and the influence of SMB on the synthesis of CaP biomaterials. The SMB solutions of different pH from 5.0 to 10.0, were scanned with the UV-VIS spectrophotometer (UV-VIS) in the wavelength ranged from 200.00 to 400.00 nm. CaP biomaterials containing SMB were synthesized from (NH4)2HPO4, Ca(NO3)2, NH4OH and SMB. The filtrates of the wet synthesis of CaP biomaterials containing SMB were measured by UV-VIS. The synthesized CaP biomaterials containing SMB were characterized by the X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). The results showed that the maximum absorption peak appeared at 281.00 nm for solutions of pH 5.0, 6.0 and 7.0. Although there were a new absorption peaks as the pH were 8.0 and 9.0, the absorption curves of SMB became similar to that of SMB as pH at 7.0 after the pH were readjusted to 7.0. The absorption peak appeared an Einstein shift to 347.00 nm at pH 10.0, which did not return to 281.00 nm when the pH of SMB solution was readjusted to 7.0. The absorption peak of filtrates containing SMB of CaP biomaterials reaction system was still at 281.00 nm when their pH was 7.0 and 8.0. Moreover, SMB had no obvious effect on the phase component and functional groups of products. Hence, it could be predicted that calcium phosphate biomaterials containing SMB, such as DCPD and TCP containing SMB, which could be prepared at the pH ranged from 5.0 to 9.0.

scholarly journals Magnetically Oriented Powder Crystal to Indexing and Structure Determination

2014 ◽  
Vol 70 (a1) ◽  
pp. C1560-C1560
Author(s):  
Fumiko Kimura ◽  
Wataru Oshima ◽  
Hiroko Matsumoto ◽  
Hidehiro Uekusa ◽  
Kazuaki Aburaya ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Powder Diffraction ◽  
Diffraction Method ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Lattice Parameters

In pharmaceutical sciences, the crystal structure is of primary importance because it influences drug efficacy. Due to difficulties of growing a large single crystal suitable for the single crystal X-ray diffraction analysis, powder diffraction method is widely used. In powder method, two-dimensional diffraction information is projected onto one dimension, which impairs the accuracy of the resulting crystal structure. To overcome this problem, we recently proposed a novel method of fabricating a magnetically oriented microcrystal array (MOMA), a composite in which microcrystals are aligned three-dimensionally in a polymer matrix. The X-ray diffraction of the MOMA is equivalent to that of the corresponding large single crystal, enabling the determination of the crystal lattice parameters and crystal structure of the embedded microcrytals.[1-3] Because we make use of the diamagnetic anisotropy of crystal, those crystals that exhibit small magnetic anisotropy do not take sufficient three-dimensional alignment. However, even for these crystals that only align uniaxially, the determination of the crystal lattice parameters can be easily made compared with the determination by powder diffraction pattern. Once these parameters are determined, crystal structure can be determined by X-ray powder diffraction method. In this paper, we demonstrate possibility of the MOMA method to assist the structure analysis through X-ray powder and single crystal diffraction methods. We applied the MOMA method to various microcrystalline powders including L-alanine, 1,3,5-triphenyl benzene, and cellobiose. The obtained MOMAs exhibited well-resolved diffraction spots, and we succeeded in determination of the crystal lattice parameters and crystal structure analysis.

scholarly journals Determination of Chromite Sands Suitability for Use in Moulding Sands

2017 ◽  
Vol 17 (2) ◽  
pp. 107-110
Author(s):  
K. Stec ◽  
J. Podwórny ◽  
B. Psiuk ◽  
Ł. Kozakiewicz
Keyword(s):  
Phase Composition ◽  
High Temperature ◽  
Chemical Composition ◽  
Chemical Properties ◽  
Grinding Process ◽  
X Ray Diffraction ◽  
Scanning Microscope ◽  
Spectroscopy Technique ◽  
X Ray

Abstract Using the available analytical methods, including the determination of chemical composition using wavelength-dispersive X-ray fluorescent spectroscopy technique and phase composition determined using X-ray diffraction, microstructural observations in a highresolution scanning microscope equipped with an X-ray microanalysis system as well as determination of characteristic softening and sintering temperatures using high-temperature microscope, the properties of particular chromite sands were defined. For the study has been typed reference sand with chemical properties, physical and thermal, treated as standard, and the sands of the regeneration process and the grinding process. Using these kinds of sand in foundries resulted in the occurrence of the phenomenon of the molding mass sintering. Impurities were identified and causes of sintering of a moulding sand based on chromite sand were characterized. Next, research methods enabling a quick evaluation of chromite sand suitability for use in the preparation of moulding sands were selected.

An X-ray Diffraction Method for the Determination of Temperatures in Coke Reactions

1984 ◽  
Vol 28 ◽  
pp. 383-388 ◽  
Author(s):  
Jack L. Johnson ◽  
Seymour Katz
Keyword(s):  
Diffraction Method ◽  
Temperature History ◽  
Maximum Temperature ◽  
Slag Formation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Potential Source ◽  
History Of ◽  
Extract Information

Information about the conditions and reactions in a foundry cupola is essential to understand the thermochemistry of a cupola and thus improve its efficiency. A potential source of such information is coke taken from inside an operating cupola. In the region of the cupola that extends from the melt zone to the taphole, coke is directly involved in important chemical processes such as combustion, gasification, slag formation, iron sulfurization, carbon pickup, and oxide reduction. Coke is also suspected of being involved in the transport of silicon to the liquid iron. Each of these processes produces characteristic physical and/or chemical changes in the coke, making it possible to extract information about the processes from an examination of coke pieces taken from within an operating cupola. A program to study such coke samples is in progress. To effectively interpret these data it is necessary to know the temperature history of the coke being examined, especially the maximum temperature attained by the coke piece in the cupola.

scholarly journals Thickness Determination of Surface Film for Textured Specimens by X-ray Diffraction

1997 ◽  
Vol 30 (1-2) ◽  
pp. 71-79 ◽  
Author(s):  
Liu Yu-Shu ◽  
Zhao Yu
Keyword(s):  
Surface Film ◽  
Diffraction Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thickness Determination

A simple and convenient X-ray diffraction method is proposed to determine the thickness of surface film for textured specimens. The analysis result for a synthetic specimen with surface film has proved that the method is applicable and reliable.

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