scholarly journals Synthesis, Crystal Structures, and Spectroscopic Characterization of Bis-aldehyde Monomers and Their Electrically Conductive Pristine Polyazomethines

Polymers ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 1498 ◽  
Author(s):  
Abdul Hafeez ◽  
Zareen Akhter ◽  
John F. Gallagher ◽  
Nawazish Ali Khan ◽  
Asghari Gul ◽  
...  

Bis-aldehyde monomers 4-(4′-formyl-phenoxy)benzaldehyde (3a), 3-methoxy-4-(4′-formyl-phenoxy)benzaldehyde (3b), and 3-ethoxy-4-(4′-formyl-phenoxy)benzaldehyde (3c) were synthesized by etherification of 4-fluorobenzaldehyde (1) with 4-hydroxybenzaldehyde (2a), 3-methoxy-4-hydroxybenzaldehyde (2b), and 3-ethoxy-4-hydroxybenzaldehyde (2c), respectively. Each monomer was polymerized with p-phenylenediamine and 4,4′-diaminodiphenyl ether to yield six poly(azomethine)s. Single crystal X-ray diffraction structures of 3b and 3c were determined. The structural characterization of the monomers and poly(azomethine)s was performed by FT-IR and NMR spectroscopic techniques and elemental analysis. Physicochemical properties of polymers were investigated by powder X-ray diffraction, thermogravimetric analysis (TGA), viscometry, UV–vis, spectroscopy and photoluminescence. These polymers were subjected to electrical conductivity measurements by the four-probe method, and their conductivities were found to be in the range 4.0 × 10−5 to 6.4 × 10−5 Scm−1, which was significantly higher than the values reported so far.

2019 ◽  
Vol 37 (3) ◽  
pp. 304-309
Author(s):  
Azeezaa Varsha Mohammed ◽  
Suresh Sagadevan

AbstractL-cysteine hydrogen fluoride (LCHF) single crystals were grown from aqueous solution. Single crystal X-ray diffraction, FT-IR, UV-Vis-NIR, and TG-DTA were used to test the grown crystals. The specimen dielectric and mechanical behaviors were also studied. Powder X-ray diffraction of the grown crystal was recorded and indexed. The optical properties of the LCHF crystal were determined using UV-Vis spectroscopy. It was found that the optical band gap of LCHF was 4.8 eV. The crystal functional groups were identified using FT-IR. Second harmonic generation (SHG) efficiency of the LCHF was three times higher than that of KDP. The dielectric constant, dielectric loss and AC conductivity were measured at different frequencies and temperatures.


2014 ◽  
Vol 5 ◽  
pp. 1760-1766 ◽  
Author(s):  
Wojciech Kempiński ◽  
Szymon Łoś ◽  
Mateusz Kempiński ◽  
Damian Markowski

The review of four experimental methods: X-ray diffraction, Raman spectroscopy, electron paramagnetic resonance and four-point electrical conductivity measurements is presented to characterize carbon nanoparticles. Two types of carbon nanoparticle systems are discussed: one comprising the powder of individual carbon nanoparticles and the second as a structurally interconnected nanoparticle matrix in the form of a fiber. X-ray diffraction and Raman spectroscopy reveal the atomic structure of the carbon nanoparticles and allow for observation of the changes in the quasi-graphitic ordering induced by ultrasonic irradiation and with the so-called quasi-high pressure effect under adsorption conditions. Structural changes have strong influence on the electronic properties, especially the localization of charge carriers within the nanoparticles, which can be observed with the EPR technique. This in turn can be well-correlated with the four-point electrical conductivity measurements which directly show the character of the charge carrier transport within the examined structures.


2019 ◽  
Vol 73 (9) ◽  
pp. 1074-1086
Author(s):  
Valentina Aguilar-Melo ◽  
Alejandro Mitrani ◽  
Edgar Casanova-Gonzalez ◽  
Mayra D. Manrique-Ortega ◽  
Griselda Pérez-Ireta ◽  
...  

A burial and a rich offering were found under Room 2 in the Murals Building, Bonampak, a Mayan archaeological site situated in Chiapas, Mexico. This burial may be related with the creation of the famous mural paintings. A rich set of jewelry made of green stones was among the different objects found. Green stones have great importance in Mesoamerican cultures, those composed of jadeite being the most appreciated. To characterize the green stones, different spectroscopic techniques were used in a complementary way: Raman and infrared spectroscopies (FT-IR) were used for global mineralogical analysis, while X-ray diffraction (XRD) and X-ray fluorescence (XRF) were applied simultaneously in situ on the artifacts that were not successfully identified by these molecular techniques. In addition, XRF was used to contrasts the elemental information from pieces composed of pyroxenes that may be related to the raw sources of jade in Guatemala. The main minerals identified within the beads and earrings were jadeite with omphacite and jadeite with albite; to a minor extent, quartz, and serpentine. In this paper, the main features of the molecular and X-ray techniques are compared in order to determine the advantages and limitations of these spectroscopies for mineral identification. With this combination of techniques, it was possible to undertake a suitable characterization of the analyzed objects. This paper focuses on the XRD–XRF combined analysis for in situ noninvasive characterization.


2021 ◽  
Author(s):  
Faiza Lughmani ◽  
Farzana Nazir ◽  
Shahid Ali Khan ◽  
Mudassir Iqbal

Abstract In this study, microcrystalline cellulose (MCC) was modified to oxidized cellulose (OC), 6-deoxycellulose hydrazide and 6-deoxycellulose(N,N-diethyl)amine (MCC-Hyd and MCC-DEM) derivatives and employed as supporting material for the synthesis of copper nanoparticles (NPs). Copper ions from aqueous solution were adsorbed and then reduced to zero valent copper (ZVC) NPs using sodium borohydride on films of prepared derivatives. The characterization of prepared derivatives and Cu NPs embedded films was performed using Fourier Transform Infrared Spectroscopy (FT-IR), Elemental analysis, X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Nuclear Magnetic Resonance (NMR) spectroscopy. Ultraviolet/Visible (UV-VIS) spectroscopy was performed for the degradation studies of 4-nitrophenol (4-NP) and various azo dyes viz. Congo Red (CR), Methylene Blue (MB), and Methyl orange (MO). Results revealed that all the films showed degradation only in the presence of ZVC NPs. Oxidized cellulose, MCC-Hyd and MCC-DEM showed excellent degradation efficiencies (> 85%) in all the cases. Our findings revealed that MCC derivatives could be efficient and renewable candidates for removal of water pollutants in future.


2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
P. V. Oliveira ◽  
M. S. S. Viana ◽  
O. A. Barros ◽  
P. T. C. Freire ◽  
F. I. Bezerra ◽  
...  

The preservation of fossils depends on several interactions of organic and inorganic chemical processes. The hard parts, which are more suitable for fossilization, might record valuable information of biogenic processes, while the taphonomic characteristics supply information on postmortem chemical transformation. Here, X-ray fluorescence, X-ray diffraction, and infrared spectroscopy analyses were carried out in Early Eoholocene fragments of bones collected from the subsurface at Gruta do Urso Fóssil, Ubajara National Park, northeast of Ceará State in Brazil. It is suggested a lower degree of decomposition, a preservation of the original mineral composition, along with some incidence of encrustation, and the occurrence of different animal species are analyzed. These preliminary data serve as a basis for future studies involving fossil biota from the deposits of Gruta do Urso Fóssil using spectroscopic techniques.


2018 ◽  
Vol 73 (11) ◽  
pp. 753-758
Author(s):  
Enrique J. Baran ◽  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Beatriz S. Parajón-Costa

AbstractThe crystal structure of pyridinium 6-methyl-1,2,3,-oxathiazine-4(3H)-one-2,2-dioxide [(C5NH6)(C4H4NO4S)], for short, pyH(ace), was determined by X-ray diffraction methods. It crystallizes as a twin in the monoclinic space group P21/c with a=6.9878(9), b=7.2211(7), c=21.740(2) Å, β=91.67(1)° and Z=4 molecules per unit cell. The structure was determined employing 1599 reflections with I>2σ(I) from one of the twin domains and refined employing 2092 reflections from both crystal domains to an agreement R1 factor of 0.0466. Besides electrostatic attractions, intermolecular pyH···O=C(ace) hydrogen bonds stabilize the acesulfamate anion and the pyridinium cation into planar discrete units parallel to the (100) crystal plane. The units form stacks of alternating ace− and pyH+ ions along the a axis that favors inter-ring π–π interactions. The Fourier transform-infrared (FT-IR) spectrum of the compound was recorded and is briefly discussed. Some comparisons with related pyridinium saccharinate salts are also made.


2014 ◽  
Vol 69 (11-12) ◽  
pp. 1119-1123 ◽  
Author(s):  
Christian B. Benda ◽  
Thomas F. Fässler

Abstract From an anhydrous pyridine extract of the binary Zintl phase K12Si17 in the presence of the cation sequestering agent [2.2.2]crypt (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) crystals of the compound [K([2.2.2]crypt)][C10H8N2] have been isolated which contains the 4,4′- bipyridine radical monoanion. This compound was fully characterized by X-ray diffraction, 1H, 13C NMR, EPR, IR and UV=Vis spectroscopy


Catalysts ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 1041
Author(s):  
Jesús Isaías De León Ramírez ◽  
Víctor Alfredo Reyes Villegas ◽  
Sergio Pérez Sicairos ◽  
Esteban Hernández Guevara ◽  
Mirna Del Carmen Brito Perea ◽  
...  

The contamination of both soil and water by nitrobenzene (NB) is a problem that has been studied, where several reactive agents have been developed for the degradation of this compound as well as different methods. Nanoparticles with semiconductive properties have been studied for organic compounds photodegradation due to their assistance in optimizing the degradation processes. Two of the most promising photocatalysts are ZnO and TiO2 because of their optimal results. In the present work the performance of the zinc peroxide (ZnO2) nanoparticles was evaluated. ZnO2 nanoparticles were synthesized from zinc acetate and hydrogen peroxide using the Sol-Gel method under ultrasound assistance. The characterization was carried out by UV–Vis spectroscopy, infrared Fourier transform total reflectance (ATR-FT-IR) spectroscopy, Raman spectroscopy, X-ray diffraction (XRD), Zeta potential, dynamic light scattering (DLS), field emission scanning electron microscopy (FE-SEM), and Energy Dispersive X-ray spectroscopy (EDX). The experiments for the degradation of NB were carried out in a photoreactor with UV lamps of 254 nm at 25 °C, using a solution of nitrobenzene with the nanoparticles. The best conditions for NB photodegradation were 30 ppm (ZnO2) and 15 ppm (NB) at pH 2, reaching up to 90% degradation in 2 h. The intermediates formed during the photodegradation of NB were identified by gas chromatography mass spectrometry.


2021 ◽  
Vol 26 (2) ◽  
Author(s):  
Dorian Polo-Cerón ◽  
María Mercedes Hincapié-Otero ◽  
Andrey Joaqui-Joaqui

N-acylhydrazones 2-(4-chlorophenyl)-N0 -(2-hydroxybenzylidene)acetohydrazide, N0 -(2-hydroxybenzylidene)-2-(4-methoxyphenyl)acetohydrazide, 2-(4-chlorophenyl)-N0 -(2,4-dihydroxybenzylidene)-acetohydrazide, and N0 -(2,4-dihydroxybenzylidene)-2-(4-methoxyphenyl)acetohydrazide were successfully synthesized by a multistep procedure. The obtained organic molecules were characterized by spectroscopic techniques (FT-IR, 1D and 2D NMR, UV-Vis) and mass spectrometry. The structure of 2-(4-chlorophenyl)-N0 -(2-hydroxybenzylidene)acetohydrazide was also confirmed by X-ray diffraction. Ab initio computational simulations of the ligand spectra were in good agreement with experimental data and validated the hypothesis about the existence of a conformational mixture of each ligand in solution. Finally, the complexation potential of the synthesized ligands to Cu2+ was assessed by continuous variation experiments and FT-IR spectroscopy.


Sign in / Sign up

Export Citation Format

Share Document