scholarly journals Heterogeneous Distribution of Interlayer Cations and Iron as a Plausible Explanation of the Non-Exfoliation of Commercial Vermiculites Post Alcohol Treatment and Microwave Irradiation

Minerals ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 835
Author(s):  
Celia Marcos ◽  
Zulema del Río ◽  
Alaa Adawy

Two commercial vermiculites from China and Libby were treated with different alcohols (methanol, ethanol, propanol and butanol) at room temperature for up to one month and afterwards irradiated with microwaves. The exfoliated and non-exfoliated particles were characterized by X-ray diffraction, high-resolution transmission microscopy, thermal gravimetric analyses and infrared spectroscopy to explain the inconsistencies in relation to potassium distribution and the exfoliation observed in previous investigations. The percentages of the exfoliated and non-exfoliated particles of the investigated vermiculites greatly varied, with no indication of a relationship between the resultant exfoliation and alcohol treatment. The crystallinity and structural order of the phases composing the particles are independent of the success of their exfoliation. The existence of a mosaic structure, the intra-particle mosaic-like intergrowth of the different mineral phases, in the treated and pristine commercial vermiculites could be attributed to the heterogeneous distribution on the nanoscale of interlayer cations as potassium and iron.

Author(s):  
Alexander M. Antipin ◽  
Olga A. Alekseeva ◽  
Natalia I. Sorokina ◽  
Alexandra N. Kuskova ◽  
Michail Yu. Presniakov ◽  
...  

The La2Mo2O9(LM) and Pr2Mo2O9(PM) single crystals are studied using precision X-ray diffraction and high-resolution transmission microscopy at room temperature. The crystal structures are determined in the space groupP213. La and Pr atoms, as well as Mo1 and O1 atoms, are located in the vicinity of the threefold axes rather than on the axes as in the high-temperature cubic phase. In both structures studied, the O2 and O3 positions are partially occupied. The coexistence of different configurations of the Mo coordination environment facilitates the oxygen-ion migration in the structure. Based on the X-ray data, the activation energies of O atoms are calculated and the migration paths of oxygen ions in the structures are analysed. The conductivity of PM crystals is close to that of LM crystals. The O2 and O3 atoms are the main contributors to the ion conductivity of LM and PM.


1978 ◽  
Vol 33 (1-2) ◽  
pp. 39-49 ◽  
Author(s):  
Douglas L. Dorset ◽  
Walter A. Pangborn ◽  
Anthony J. Hancock ◽  
Iris S. Lee

Abstract Diffraction studies on natural 1,2-dipalmitin and on analogs, including those based on the configurational isomers of cyclopentane-1,2,3-triol reveal that the 1,2-diglycerides crystallize from solvent with chain methylene packing identical to the monoclinic form of even-chain alkanes. The chains probably are folded back in “hairpin” fashion as found in phospholipid crystal structures. Acyl shifts are observed to occur in the crystalline solid state at room temperature to give the 1,3-diglyceride. Analogs based on the above-mentioned cyclitols show that isomers with adjacent chains trans to the ring (possibly extended chain packing) or with chains cis to the ring (“hair­ pin”) crystallize readily. Both possibly extended chain configurational isomers have the α-form as well as β′-forms and a β-polymorph. The hairpin isomers each give a β′-polymorph but only the all-cts isomer gives an α-form.


2012 ◽  
Vol 548 ◽  
pp. 77-81
Author(s):  
Jia Hua Ma ◽  
Cheng Jia Tan ◽  
Xia Deng ◽  
Chao Xin

Preparation techniques of chitosan from Catharsius molossus L. processing discards were studied by orthogonal design. Preparation techniques were as follows:demineralizing: soaked for 30 min at 80 °C with 1.3 mol•L-1 HCl, then kept for 12 h under room temperature. Deproteinization and delipidation: treated for 6 h at 90 °C with 4 mol•L-1 NaOH. Decolorizing: soaked at room temperature with 3% KMnO4, then treated with 2% oxalic acid at 70 °C. Deacetylation: treated for 6 h at 110 °Cwith 14 mol•L-1 NaOH. Properties of chitosan were characterized by Fourier transform infrared spectroscopy(FTIR), X-ray diffraction (XRD), etc. It proved the technique was stable and feasible. The result also preliminarily showed that chitosan from Catharsius molossus L. was better than shrimp’s. It will be widely applicated in biomedical and other industrial areas with such exiciting properties.


Molbank ◽  
10.3390/m1287 ◽  
2021 ◽  
Vol 2021 (4) ◽  
pp. M1287
Author(s):  
Alise Kirilova ◽  
Aleksandrs Pučkins ◽  
Sergey Belyakov ◽  
Elena Kirilova

Herein, we describe the synthesis of 3-[N-(4-methoxybenzyl)amino]benzo[de]anthracen-7-one via a two-step procedure including 3-aminobenzanthrone condensation with anisaldehyde and following reduction of obtained imine to appropriate amine by sodium borohydride. The structure of the synthesized compounds was established by elemental analysis, nuclear magnetic resonance spectroscopy, mass spectrometry (EI-MS), and infrared spectroscopy (FT-IR) and confirmed by single-crystal X-ray diffraction. The title compound was analyzed by thermal gravimetric analysis, UV/vis, and fluorescence spectroscopy.


2017 ◽  
Vol 36 (1-2) ◽  
pp. 429-440 ◽  
Author(s):  
Pinki Chakraborty ◽  
Aman Kothari ◽  
Rajamani Nagarajan

Polyaniline was synthesized by the chemical oxidative polymerization procedure at room temperature employing hydrogen peroxide (H2O2) as oxidant and ferrous chloride (FeCl2·2H2O) and vanadyl sulphate (VOSO4·H2O) as co-catalysts, respectively. The obtained polymers were characterized by high resolution powder X-ray diffraction, Fourier transform infrared spectroscopy, Raman, UV–Visible, photoluminescence spectroscopy, thermogravimetric Field Emission Scanning Electron Microscopy (FESEM) and Transmission Electron Microscopy (TEM) techniques. Ordered arrangement indicative of semi-crystalline nature of polyaniline was evidenced from the presence of intense reflection at d = 13.72 Å in the powder X-ray diffraction pattern followed by two lesser intense peaks at 4.61 and 3.47 Å. Fourier transform infrared spectroscopy and Raman spectroscopic results indicated the polyaniline to be emeraldine salt form. Fibrous morphology was observed in scanning electron microscope images. Nearly 93% of Methyl Orange dye was adsorbed in 30 min by the ordered polyaniline at room temperature. No significant difference in the crystallinity and/or ordering was noticed in the powder X-ray diffraction pattern after dye adsorption. The correlation between the ordered structure of polyaniline and its higher adsorption property derived in the current study has the potential to fabricate devices consisting polyaniline to detect dye molecules.


2017 ◽  
Vol 49 (3) ◽  
pp. 277-284 ◽  
Author(s):  
Zorica Lazarevic ◽  
Cedomir Jovalekic ◽  
Martina Gilic ◽  
Valentin Ivanovski ◽  
Ana Umicevic ◽  
...  

Yttrium orthoferrite (YFeO3) powder was prepared by a mechanochemical synthesis from a mixture of Y2O3 and ?-Fe2O3 powders in a planetary ball mill for 2.5 h. The obtained YFeO3 powder sample was characterized by X-ray diffraction (XRD), Raman and infrared spectroscopy. The average crystallite size calculated by the Scherrer equation was 12 nm. The M?ssbauer spectroscopy at room temperature confirms the superparamagnetic character of YFeO3 orthoferrite sample.


2006 ◽  
Vol 928 ◽  
Author(s):  
Zhiwei Zhao ◽  
Beng Kang Tay

ABSTRACTTitanium oxide thin films were prepared by filtered cathodic vacuum arc (FCVA) at low temperatures ranged from room temperature to 330°C. Spectroscopic study of the deposited films were carried out by X-ray diffraction, Raman Scattering, Fourier transform infrared spectroscopy (FTIR) and photoluminescence (PL), respectively. The films remained amorphous up to the substrate temperature of 230°C. Nanocrystalline titanium oxide thin films occurred at 330°C with the strongest peak intensity from anatase (101) plane. The average grain size was around 20 nm and no rutile phase could be found. Various allowed vibrational frequencies (e.g. 152, 199, 399, 640 cm−1) in Raman spectra and Ti-O-Ti transverse mode at 436 cm−1 in the FTIR spectrum evidently verified the presence of anatase phase in the films at 330°C. Moreover, at room temperature only crystalline film exhibited a PL peak with the center at 379 nm in PL spectrum and the origin was discussed.


2014 ◽  
Vol 631 ◽  
pp. 36-42 ◽  
Author(s):  
Celso A. Bertran ◽  
Otto V.M. Bueno

In this work, attention was paid to the understanding of the chemical modifications occurring in xerogeis of 58S bioglass (60% mol SiO2; 36%mol CaO; 4%mol P2O5), during the 58S bioglass synthesis, prepared by the sol-gel (SG) and sol-gel self-propagating combustion (SGSPC) methods using citric acid as reductant/fuel. The chemical modifications of the xerogels were evaluated in the temperature range 70-920°C. Characteristic functional groups were evidenced by Fourier transform infrared spectroscopy (FTIR), and the thermal behaviour was evidenced by thermal gravimetric (TG) and differential thermal (DSC) analysis, the transition from glass to glass ceramic was also followed by X-ray diffraction.


2007 ◽  
Vol 330-332 ◽  
pp. 511-514 ◽  
Author(s):  
Z. Yang ◽  
E.S. Thian ◽  
Serena Best ◽  
Ruth Cameron

α-tricalcium phosphate (α-TCP) was prepared by a wet precipitation reaction between calcium hydroxide and orthophosphoric acid solutions. The as-synthesised powder was then characterised using a Scanning Electron Microscope (SEM) equipped with Energy Dispersive Spectroscope (EDS), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscope (FTIR). Analyses revealed that a phase-pure powder with a Ca/P ratio of 1.5 was produced. In addition, nanosized α-TCP particles of diameter ~ 70 nm were agglomerated to form larger particles of 10μm in diameter. It was found that by the combination of attritor milling and solution evaporation, the agglomerates of α-TCP nanoparticles could be broken down, and distributed evenly within the poly(D,L-lactic-co-glycolic acid) (PLGA) matrix. Thus, a α-TCP/PLGA nanocomposite was successfully produced by a modified solution evaporation method at room temperature followed by hot pressing at 150 °C. The achievable ceramic loading was approximately 38 wt.%, which was confirmed by thermal gravimetric analysis (TGA).


Author(s):  
C. Wolpers ◽  
R. Blaschke

Scanning microscopy was used to study the surface of human gallstones and the surface of fractures. The specimens were obtained by operation, washed with water, dried at room temperature and shadowcasted with carbon and aluminum. Most of the specimens belong to patients from a series of X-ray follow-up study, examined during the last twenty years. So it was possible to evaluate approximately the age of these gallstones and to get information on the intensity of growing and solving.Cholesterol, a group of bile pigment substances and different salts of calcium, are the main components of human gallstones. By X-ray diffraction technique, infra-red spectroscopy and by chemical analysis it was demonstrated that all three components can be found in any gallstone. In the presence of water cholesterol crystallizes in pane-like plates of the triclinic crystal system.


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