A Design of Experiment Approach to the Synthesis of Alendronate-incorporated Hydroxyapatite

2018 ◽  
Vol 69 (8) ◽  
pp. 1944-1948 ◽  
Author(s):  
Adina Turcu Stiolica ◽  
Maria Viorica Bubulica ◽  
Oana Elena Nicolaescu ◽  
Octavian Croitoru ◽  
Mariana Popescu ◽  
...  

A design of experiment (DoE) approach is presented for the optimization of Alendronate-hydroxyapatite nanoparticles� synthesis. The synthesis was performed using the chemical precipitation technique from calcium nitrate, diammonium hydrogen phosphate and alendronate. Synthesis temperature, reactant addition rate and ripening time were chosen as the most relevant experimental factors for our synthesis. Design of Experiments was used in order to measure these conclusive process parameters and their effect on controlling some final nanoparticles parameters, such us: alendronate incorporation efficiency (IncorporationEfficiency, %), hydroxyapatite crystallite size (Size_XRD, nm), hydroxyapatite particle size distribution (Size_DLS, �). Our study found that better HA-AL incorporation efficiency and small nonoparticles can be obtained using the following chemical process parameters: reaction temperature 30oC or smaller, ripening time 108h and addition rate 0.1mol/min. The analysis of more than one nanoparticles characteristics was possible using DoE software, MODDE 9.1. Thus, hydroxyapatite-alendronate incorporation efficiency should be expected to increase with decreasing temperature below 300C, increasing the maturate time at least 108h, at an addition rate of 0.1mol/min, in an N2 atmosphere. The same conditions will ensure nanoparticles small size that would be more desirable for the application of implants.

2012 ◽  
Vol 727-728 ◽  
pp. 1164-1169 ◽  
Author(s):  
Mônica Beatriz Thürmer ◽  
Rafaela Silveira Vieira ◽  
Juliana Machado Fernandes ◽  
Wilbur Trajano Guerin Coelho ◽  
Luis Alberto Santos

Calcium phosphate cements have bioactivity and osteoconductivity and can be molded and replace portions of bone tissue. The aim of this work was to study the obtainment of α-tricalcium phosphate, the main phase of calcium phosphate cement, by wet reaction from calcium nitrate and phosphoric acid. There are no reports about α-tricalcium phosphate obtained by this method. Two routes of chemical precipitation were evaluated and the use of two calcinations temperatures to obtain the phase of cement. The influence of calcination temperature on the mechanical properties of cement was evaluated. Cement samples were characterized by particle size analysis, X-ray diffraction, mechanical strength and scanning electron microscopy. The results demonstrate the strong influence of synthesis route on the crystalline phases of cement and the influence of concentration of reactants on the product of the reaction, as well as, on the mechanical properties of cement.


2019 ◽  
Vol 8 (4) ◽  
pp. 261-276
Author(s):  
Roghayyeh Marefat Seyedlar ◽  
Mohammadbagher Rezvani ◽  
Samira Barari ◽  
Mohammad Imani ◽  
Azizollah Nodehi ◽  
...  

AbstractThe purpose of this study was to synthesize nano-sized β-tricalcium phosphate (nano-TCP) particles and determine its concentration-dependent properties on incipient enamel caries lesions. Nano-TCP was synthesized as a wet chemical through a method using low concentration of precursors and low addition rate of calcium nitrate tetrahydrate as a second phase. Morphology and phase composition of the particles were analyzed by SEM, XRD, and EDXA techniques. Incipient enamel lesions were created in human premolars with an acidic buffer. The teeth were then incubated in aqueous dispersions of nano-TCP as remineralization solutions. Sodium fluoride solution and deionized water were used as positive and negative control groups, respectively. The quality and thickness of the remineralized layer on enamel were investigated using SEM. The data were statistically analyzed by analysis of variance (ANOVA) and post hoc Tukey’s test. The synthesized nano-TCP mostly consisted of porous platelet-like crystals of 50–100 nm thickness and pore diameters of 100–300 nm. SEM observation showed that a homogenous layer was formed on the surface of the enamels remineralized in nano-TCP solutions. The thickness of the mineralized layer was dependent on the incubation time and nano-TCP concentration.


2015 ◽  
Vol 17 (1) ◽  
pp. 123-145 ◽  
Author(s):  
Dana Kralisch ◽  
Denise Ott ◽  
Doerthe Gericke

The implementation of Life Cycle Assessment and related methods in green chemical process and synthesis design strongly supports the development of greener concepts on the basis of deep and profound insights into the dependences between the selection of compounds and process parameters and the resulting environmental impacts.


Author(s):  
C. A. Griffiths ◽  
S. S. Dimov ◽  
S. G. Scholz ◽  
G. Tosello ◽  
A. Rees

The paper reports an experimental study that investigates part demoulding behavior in micro-injection moulding with a focus on the effects of pressure and temperature on the demoulding forces. In particular, the demoulding performance of a representative microfluidics part was studied as a function of four process parameters, melt temperature, mould temperature, holding pressure, and injection speed, employing the design of experiment approach. In addition, the results obtained using different combinations of process parameters were analyzed to identify the best processing conditions in regards to demoulding behavior of microparts when utilizing a COC polymer to mould them.


2014 ◽  
Vol 46 (2) ◽  
pp. 185-193 ◽  
Author(s):  
B. Mirhadi

A nano sized beta tricalcium phosphate (?-TCP) powder was conventional sintered (CS) and microwave sintered (MW), in order to obtain dense ?-TCP ceramics. In this work the effect of microwave sintering conditions on the microstructure, phase composition and mechanical properties of materials based on tricalcium phosphate (TCP) was investigated by SEM (scanning electron microscopy)and XRD(X-ray diffraction) and then compared with conventional sintered samples. Nano-size ?-TCP powders with average grain size of 80 nm were prepared by the wet chemical precipitation method with calcium nitrate and diammonium hydrogen phosphate as calcium and phosphorus precursors, respectively. The precipitation process employed was also found to be suitable for the production of submicrometre ?-TCP powder in situ. The ?-TCP samples microwave (MW) sintered for 15 min at 1100?C, with average grain size of 3?m, showed better densification, higher density and certainly higher hardness than samples conventionally sintered for 2 h at the same temperature. By comparing sintered and MW sintered ?-TCP samples, it was concluded that MW sintered ?-TCP samples have superior mechanical properties.


2019 ◽  
Vol 809 ◽  
pp. 527-532
Author(s):  
Michael Petrich ◽  
Christoph Hoffmeister ◽  
Axel Herrmann

Carbon fibre reinforced plastics (CRFP) are high performance materials with an outstanding lightweight potential. Recycling applications for production waste though, are still scarce and not fully established. In the CaroLIn (carbon fibre nonwovens optimised for aircraft interior components) research project a novel aerodynamic textile process is developed, in order to produce highly orientated non-wovens form recycled carbon fibres. In the first stage of the project a laboratory plant for the orientation of fibres has been constructed and implemented. Afterwards a process window has been defined and a number of process parameters identified. The influence of those parameters was then investigated, using the statistical design of experiment (DOE) method.


2019 ◽  
Vol 825 ◽  
pp. 56-61
Author(s):  
Hagino Masahiro ◽  
Ikeuchi Kouji ◽  
Usuki Hiroshi ◽  
Inoue Takashi

In this study, machining was performed on stainless steel (AISI304) by face-milling. Design of experiment was implemented to develop the experimental layout. The aim of this work was to relate the response to the process parameters. An optimization routine was applied to determine the optimal conditions that would enhance the minimization of the deformation. As a result, mathematical models were developed to determine the relationship between the process parameters and the deformation after machining. The effects of process parameters on the deformation amount were defined.


2018 ◽  
Vol 69 (4) ◽  
pp. 759-766
Author(s):  
Rodica Elena Patescu ◽  
Claudia Maria Simonescu ◽  
Gheorghe Nechifor ◽  
Christu Tardei ◽  
Ionela Camelia Ionascu

Two types of nanohydroxyapatite samples have been obtained by wet chemical precipitation synthesis, involving calcium nitrate tetrahydrate and diammonium hydrogen phosphate as precursors in different conditions. Powders obtained were characterized by X-ray diffraction (XRD) and FTIR spectroscopy. The equilibrium isotherm models related with lead and zinc ions removal from synthetic aqueous solutions have been also investigated. According to this research study, it has been found that the nanohydroxyapatite samples show good heavy metals adsorption capacity, and selectivity for lead ions. It was also observed a slow decreasing of sorption capacity of heavy metal ions from binary solutions compared to that registered from single heavy metal ion solutions.


2007 ◽  
Vol 27 (4) ◽  
pp. 725-728 ◽  
Author(s):  
S.K. Roy ◽  
R. Dey ◽  
A. Mitra ◽  
S. Mukherjee ◽  
M.K. Mitra ◽  
...  

1999 ◽  
Vol 599 ◽  
Author(s):  
D Bayraktar ◽  
A C. Tas

AbstractAn important inorganic phase of synthetic bone applications, calcium hydroxyapatite (HA, Ca10(PO4)6(OH)2), was prepared as a single-phase and sub-micron bioceramic powder. Carbonated HA precursors were synthesized from calcium nitrate tetrahydrate and diammonium hydrogen phosphate salts dissolved in “synthetic body fluid” (SBF) solutions, containing urea (H2NCONH2) and enzyme urease, under the biomimetic conditions of 37°C and pH 7.4, by using a novel chemical precipitation technique.


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