scholarly journals β-Tricalcium Phosphate Interferes with the Assessment of Crystallinity in Burned Skeletal Remains

2018 ◽  
Vol 2018 ◽  
pp. 1-10 ◽  
Author(s):  
Giampaolo Piga ◽  
Ana Amarante ◽  
Calil Makhoul ◽  
Eugénia Cunha ◽  
Assumpció Malgosa ◽  
...  
Keyword(s):  
Tricalcium Phosphate ◽  
Crystallinity Index ◽  
Attenuated Total Reflectance ◽  
X Ray Diffraction ◽  
Human Bones ◽  
Advanced Technologies ◽  
Complex Process ◽  
Induced Changes ◽  
Ci Calculation ◽  
Mineralogical Phases

The analysis of burned remains is a highly complex process, and a better insight can be gained with advanced technologies. The main goal of this paper is to apply X-ray diffraction, partially supported by infrared attenuated total reflectance spectroscopy to determine changes in burned human bones and teeth in terms of mineral phase transformations. Samples of 36 bones and 12 teeth were heated at 1050°C and afterwards subjected to XRD and ATR-IR. The crystallinity index was calculated for every sample. A quantitative evaluation of phases was documented by using the Rietveld approach. In addition to bioapatite, the following mineralogical phases were found in the bone: β-tricalcium phosphate (β-TCP) (Ca3(PO4)2), lime (CaO), portlandite (Ca(OH)2), calcite (CaCO3), and buchwaldite (NaCaPO4). In the case of bone, besides bioapatite, only the first two mineralogical phases and magnesium oxide were present. We also observed that the formation of β-TCP affects the phosphate peaks used for CI calculation. Therefore, caution is needed when its occurrence and evaluation are carried out. This is an important warning for tracking heat-induced changes in human bone, in terms of physicochemical properties related to structure, which is expected to impact in forensic, bioanthropological, and archaeological contexts.

scholarly journals Understanding the Crystallinity Indices Behavior of Burned Bones and Teeth by ATR-IR and XRD in the Presence of Bioapatite Mixed with Other Phosphate and Carbonate Phases

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Giampaolo Piga ◽  
David Gonçalves ◽  
T. J. U. Thompson ◽  
Antonio Brunetti ◽  
Assumpció Malgosa ◽  
...  
Keyword(s):  
Crystallinity Index ◽  
Mechanical Processing ◽  
Spectroscopy Data ◽  
X Ray Diffraction ◽  
Human Teeth ◽  
X Ray ◽  
Human Bones ◽  
Burned Bones ◽  
Tcp Phase ◽  
Xrd Patterns

We have critically investigated the ATR-IR spectroscopy data behavior of burned human teeth as opposed to the generally observed behavior in human bones that were subjected to heat treatment, whether deliberate or accidental. It is shown that the deterioration of the crystallinity index (CI) behavior sometimes observed in bones subjected to high temperature appears to be of higher frequency in the case of bioapatite from teeth. This occurs because the formation of the β-tricalcium phosphate (β-TCP) phase, otherwise known as whitlockite, clearly ascertained by the X-ray diffraction (XRD) patterns collected on the same powdered specimens investigated by ATR-IR. These results point to the need of combining more than one physicochemical technique even if apparently well suitable, in order to verify whether the assumed conditions assessed by spectroscopy are fully maintained in the specimens after temperature and/or mechanical processing.

scholarly journals Electrospun Membranes Based on Polycaprolactone, Nano-Hydroxyapatite and Metronidazole

Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 931
Author(s):  
Ioana-Codruţa Mirică ◽  
Gabriel Furtos ◽  
Ondine Lucaciu ◽  
Petru Pascuta ◽  
Mihaela Vlassa ◽  
...  
Keyword(s):  
Fiber Diameter ◽  
Maximum Load ◽  
Guided Bone Regeneration ◽  
Attenuated Total Reflectance ◽  
X Ray Diffraction ◽  
Sem Images ◽  
Total Reflectance ◽  
X Ray ◽  
Electrospun Membranes

The aim of this research was to develop new electrospun membranes (EMs) based on polycaprolactone (PCL) with or without metronidazole (MET)/nano-hydroxyapatite (nHAP) content. New nHAP with a mean diameter of 34 nm in length was synthesized. X-ray diffraction (XRD) and attenuated total reflectance Fourier transform infrared spectroscopy (FTIR-ATR) were used for structural characterization of precursors and EMs. The highest mechanical properties (the force at maximum load, Young’s modulus and tensile strength) were found for the PCL membranes, and these properties decreased for the other samples in the following order: 95% PCL + 5% nHAP > 80% PCL + 20% MET > 75% PCL + 5% nHAP + 20% MET. The stiffness increased with the addition of 5 wt.% nHAP. The SEM images of EMs showed randomly oriented bead-free fibers that generated a porous structure with interconnected macropores. The fiber diameter showed values between 2 and 16 µm. The fiber diameter increased with the addition of nHAP filler and decreased when MET was added. New EMs with nHAP and MET could be promising materials for guided bone regeneration or tissue engineering.

scholarly journals Chemical and Structural Characterization of Maize Stover Fractions in Aspect of Its Possible Applications

Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1527
Author(s):  
Magdalena Woźniak ◽  
Izabela Ratajczak ◽  
Dawid Wojcieszak ◽  
Agnieszka Waśkiewicz ◽  
Kinga Szentner ◽  
...  
Keyword(s):  
Structural Characterization ◽  
Biogas Production ◽  
Structural Parameters ◽  
C:N Ratio ◽  
Crystallinity Index ◽  
Degree Of Crystallinity ◽  
Cellulose Content ◽  
X Ray Diffraction ◽  
Maize Stover

In the last decade, an increasingly common method of maize stover management is to use it for energy generation, including anaerobic digestion for biogas production. Therefore, the aim of this study was to provide a chemical and structural characterization of maize stover fractions and, based on these parameters, to evaluate the potential application of these fractions, including forbiogas production. In the study, maize stover fractions, including cobs, husks, leaves and stalks, were used. The biomass samples were characterized by infrared spectroscopy (FTIR), X-ray diffraction and analysis of elemental composition. Among all maize stover fractions, stalks showed the highest C:N ratio, degree of crystallinity and cellulose and lignin contents. The high crystallinity index of stalks (38%) is associated with their high cellulose content (44.87%). FTIR analysis showed that the spectrum of maize stalks is characterized by the highest intensity of bands at 1512 cm−1 and 1384 cm−1, which are the characteristic bands of lignin and cellulose. Obtained results indicate that the maize stover fraction has an influence on the chemical and structural parameters. Moreover, presented results indicate that stalks are characterized by the most favorable chemical parameters for biogas production.

scholarly journals Valorization of Byproducts of Hemp Multipurpose Crop: Short Non-Aligned Bast Fibers as a Source of Nanocellulose

Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4723
Author(s):  
Sara Dalle Vacche ◽  
Vijayaletchumy Karunakaran ◽  
Alessia Patrucco ◽  
Marina Zoccola ◽  
Loreleï Douard ◽  
...  
Keyword(s):  
Infrared Spectroscopy ◽  
Thermogravimetric Analysis ◽  
Cannabis Sativa ◽  
Crystallinity Index ◽  
Residual Lignin ◽  
Chemical Pretreatment ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bast Fibers ◽  
Seed Maturity

Nanocellulose was extracted from short bast fibers, from hemp (Cannabis sativa L.) plants harvested at seed maturity, non-retted, and mechanically decorticated in a defibering apparatus, giving non-aligned fibers. A chemical pretreatment with NaOH and HCl allowed the removal of most of the non-cellulosic components of the fibers. No bleaching was performed. The chemically pretreated fibers were then refined in a beater and treated with a cellulase enzyme, followed by mechanical defibrillation in an ultrafine friction grinder. The fibers were characterized by microscopy, infrared spectroscopy, thermogravimetric analysis and X-ray diffraction after each step of the process to understand the evolution of their morphology and composition. The obtained nanocellulose suspension was composed of short nanofibrils with widths of 5–12 nm, stacks of nanofibrils with widths of 20–200 nm, and some larger fibers. The crystallinity index was found to increase from 74% for the raw fibers to 80% for the nanocellulose. The nanocellulose retained a yellowish color, indicating the presence of some residual lignin. The properties of the nanopaper prepared with the hemp nanocellulose were similar to those of nanopapers prepared with wood pulp-derived rod-like nanofibrils.

Synthesis of Alpha-Tricalcium Phosphate by Wet Reaction and Evaluation of Mechanical Properties

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
Keyword(s):  
Mechanical Properties ◽  
Calcium Phosphate ◽  
Tricalcium Phosphate ◽  
Calcium Nitrate ◽  
Chemical Precipitation ◽  
Particle Size Analysis ◽  
Size Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Calcium Phosphate Cements

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.

scholarly journals Synthesis, Characterization and Biological Properties of Intercalated Kaolinite Nanoclays: Intercalation and Biocompatibility

2019 ◽  
Vol 19 (1) ◽  
pp. 83-99 ◽  
Author(s):  
B. Yilmaz ◽  
E. T. Irmak ◽  
Y. Turhan ◽  
S. Doğan ◽  
M. Doğan ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Human Lymphocytes ◽  
Biological Properties ◽  
Attenuated Total Reflectance ◽  
X Ray Diffraction ◽  
Cytotoxic Effects ◽  
X Ray ◽  
Human Risk ◽  
Transmission Electron ◽  
Reflectance Ftir

AbstractThe aims of the present study were to synthesize the intercalated kaolinite samples with dimethylsulfoxide (DMSO), glutamic acid (GA), succinimide (SIM), cetylpyridiniumchloride (CPC), and hexadecyltrimethylammoniumchloride (HDTMA+); to characterize by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR), and to determine the hemocompatibility and the cytotoxic effects of the intercalated kaolinite nanoclays on human lymphocytes. It was found that the intercalation with DMSO did not cause any decrease in cell viability until its maximum concentration (500 µg/mL), however, the intercalation with SIM, CPC, and (HDTMA+) causd important decreases in lymphocyte viabilities. It was determined that no significant decrease was observed in protein content of the lymphocyte cells exposed to the kaolinite nanoclays except the ones intercalated with SIM. Furthermore, the pristine kaolinite nanoclays which were intercalated with DMSO, GA, and SIM exhibited high hemocompatibility and the nanoclays intercalated with CPC and (HDTMA+) were highly hemocompatibile for the amounts below 125 and 500 µg/mL, respectively. All the results of this work can serve for the human risk assesment of intercalated nanoclays.

scholarly journals Effect of Tetramethylammonium Hydroxide on Nucleation, Surface Modification and Growth of Magnetic Nanoparticles

2012 ◽  
Vol 2012 ◽  
pp. 1-10 ◽  
Author(s):  
Ângela L. Andrade ◽  
José D. Fabris ◽  
José D. Ardisson ◽  
Manuel A. Valente ◽  
José M. F. Ferreira
Keyword(s):  
Zeta Potential ◽  
Magnetite Nanoparticles ◽  
Heat Dissipation ◽  
Tetramethylammonium Hydroxide ◽  
Precipitation Method ◽  
Attenuated Total Reflectance ◽  
X Ray Diffraction ◽  
Experimental Conditions ◽  
Transmission Electron ◽  
Magnetite Particles

Nanoparticles of magnetite (Fe3O4) were obtained by reacting ferric chloride with sodium sulphite, through the reduction-precipitation method. The effects of adding tetramethylammonium hydroxide (TMAOH) during or after the precipitation of the iron oxide were studied in an attempt to obtain well-dispersed magnetite nanoparticles. Accordingly, the following experimental conditions were tested: (i) precipitation in absence of TMAOH (sample Mt), (ii) the same as (i) after peptizing with TMAOH (Mt1), (iii) TMAOH added to the reaction mixture during the precipitation of magnetite (Mt2). Analyses with transmission electron microscopy (TEM), X-ray diffraction, Mössbauer spectroscopy, attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), zeta potential, and magnetization measurements up to 2.5 T revealed that magnetite was normally formed also in the medium containing TMAOH. The degree of particles agglomeration was monitored with laser diffraction and technique and inspection of TEM images. The relative contributions of Néel and Brownian relaxations on the magnetic heat dissipation were studied by investigating the ability of suspensions of these magnetite nanoparticles to release heat in aqueous and in hydrogel media. Based on ATR-FTIR and zeta potential data, it is suggested that the surfaces of the synthesized magnetite particles treated with TMAOH become coated with (CH3)4N+cations.

Magnesium-Silicon Substituted Carbonate Hydroxyapatite (Mg-Si CHA): Factors Affecting Sintering

2016 ◽  
Vol 694 ◽  
pp. 88-93
Author(s):  
Ahmad Fauzi Mohd Noor ◽  
Harmiza Zainudin
Keyword(s):  
Mechanical Properties ◽  
Single Phase ◽  
Physical And Mechanical Properties ◽  
Major Effect ◽  
Carbonate Content ◽  
X Ray Diffraction ◽  
Factors Affecting ◽  
Complex Process ◽  
Powder Properties ◽  
Properties Of Materials

Sintering has major effect on the final properties of materials such as density, porosity and microstructure. Sintering of Mg-Si CHA in particular is a complex process since changes could occur during sintering, which include phase formation, grain size, pore size and carbonate content, and this in turn affects the mechanical properties. Improved mechanical properties of Mg-Si CHA is critical in load bearing implant applications. Poor control of thermal treatment of Mg-Si CHA during sintering would cause carbonate loss, leading to partial or total decomposition of Mg-Si CHA, subsequently would affect the physical and mechanical properties. The influence of powder properties (particle size, porosity, morphology) and sintering parameters (heating rate, firing atmosphere) on the sintered Mg-Si CHA microstructure was studied using scanning electron microscopy (SEM) characterization technique. The SEM results showed that we are able to produce sintered Mg-Si CHA without cracking of the compacted pellets, while keeping the carbonate level in the amount required (2 – 8%). X-Ray diffraction (XRD) was also performed on the sintered samples and the results indicated that a single phase Mg-Si-CHA was obtained, while Fourier transform infra-red (FTIR) spectroscopy result confirmed that as-synthesized Mg-Si CHA powder was a B-type.

High pressure studies on the packing forces and intermolecular interaction in polyphenyls

2003 ◽  
Vol 771 ◽  
Author(s):  
G. Heimel ◽  
P. Puschnig ◽  
M. Oehzelt ◽  
K. Hummer ◽  
B. Koppelhuber-Bitschnau ◽  
...  
Keyword(s):  
Bulk Modulus ◽  
Structural Changes ◽  
Equations Of State ◽  
Ambient Conditions ◽  
X Ray Diffraction ◽  
Pressure Derivative ◽  
Molecular Arrangement ◽  
High Pressure Studies ◽  
Phenyl Rings ◽  
Induced Changes

AbstractIn this work, we report on pressure induced structural changes in crystalline oligo(paraphenylenes) containing two to six phenyl rings. Revisiting the crystal structures at ambient conditions reveals details in the packing principle. A linear relationship between the density at ambient conditions and the number of phenyl rings is found. Energy dispersive X-ray diffraction has been performed in a systematic study on polycrystalline powders of biphenyl, paraterphenyl, p-quaterphenyl, p-quinquephenyl and p-sexiphenyl under hydrostatic pressure up to 60 kbar. Our investigations not only yield pressure dependent lattice parameters and hints towards pressure induced changes in the molecular arrangement, but also allow for an analysis of the equations of state of these substances as a function of oligomer length. We report the previously unknown bulk modulus of p-quaterphenyl, p-quinquephenyl, and p-sexiphenyl (B0 = 83 kbar, 93 kbar, and 100 kbar respectively) and its pressure derivative (B0' = 6.4, 7.5, and 5.6). A linear dependence of the bulk modulus on the inverse number of phenyl rings in the molecules is found.

scholarly journals Fabrication of Silk Resin with High Bending Properties by Hot-Pressing and Subsequent Hot-Rolling

Materials ◽  
2020 ◽  
Vol 13 (12) ◽  
pp. 2716
Author(s):  
Hoang Anh Tuan ◽  
Shinji Hirai ◽  
Shota Inoue ◽  
Alharbi A. H. Mohammed ◽  
Shota Akioka ◽  
...  
Keyword(s):  
Hot Rolling ◽  
Hot Pressing ◽  
Bending Strength ◽  
Decomposition Temperature ◽  
Attenuated Total Reflectance ◽  
X Ray Diffraction ◽  
Bending Properties ◽  
X Ray ◽  
Bombyx Mori Silk ◽  
Increased Strength

This research reports the processability and mechanical properties of silk resins prepared by hot-pressing followed by hot-rolling and then analyzes their thermal and structural properties. The results show that regenerated silk (RS) resins are better suited for hot-rolling than Eri and Bombyx mori silk resins (untreated silk). When hot-rolling at 160 °C with a 50% of reduction ratio, maximum bending strength and Young’s modulus of RS resin reaches 192 MPa and 10.2 GPa, respectively, after pretreatment by immersion in 40 vol% ethanol, and 229 MPa and 12.5 GPa, respectively, after pretreatment by immersion in boiling water. Increased strength of the material is attributed to the increased content of aggregated strands and intramolecular linking of β sheets (attenuated total reflectance Fourier-transform infrared spectroscopy) and higher crystallinity (X-ray diffraction analysis). After hot-pressing and hot-rolling, RS resins have a stable decomposition temperature (297 °C).

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