Synthesis and Physicochemical Analysis of Polystyrene-Anchored Pd(II) Metal Complex

2014 ◽  
Vol 11 (2) ◽  
pp. 45
Author(s):  
Siti Kamilah Che Soh ◽  
Siti Aminah Jusoh ◽  
Mustaffa Shamsuddin

A polystyrene (PS)-anchored Pd(II) metal complex was synthesized on cross-linked polymer by heating a mixture of chlorometylated polystyrene with phenyldithiocarbazate and carbon disulfide in the presence of potassium hydroxide (KOH) in dimethylformamide (DMF). The reaction mixture was heated at 80 °C to form the corresponding phenyldithiocarbazate-functionalized polymer. Then, it was treated with bis(benzonitrile)palladium(II) chloride. The properties of dark colored polymer, impregnated with the metal complex was then characterized by various spectroscopic technique such as Fourier Transform Infrared (FTIR), Scanning Electron Microscopy/Energy Dispersive X-ray (SEM/EDX), CHNS elemental analysis, BET surface area, X-ray Diffraction (XRD), Thermogravimetric (TGA) and Inductively Coupled Plasma-Optical Emission (ICP-OES) spectroscopy.

2018 ◽  
Vol 7 (1) ◽  
pp. 38-44 ◽  
Author(s):  
А. Рашковский ◽  
A. Rashkovskiy ◽  
Е. Политова ◽  
E. Politova ◽  
А. Меркушкин ◽  
...  

In this investigation the structure of «green» silica maid with rice husk has been studied by methods of physicochemical analysis. By method of X-ray diffraction it has been found that the samples of «green» silica powders are completely amorphous, and the observed amorphous halo consists of two components. By method of scanning electron microscopy it has been revealed that nano-particles of «green» SiO2 can form agglomerates and microstructures with dimensions from 0,1 to 500 microns, containing numerous pores, which presence has been confirmed by sorption measurements. By method of mass spectrometry with inductively coupled plasma has been found the presence of aluminum, titanium and nickel mechanical impurities in the «green» SiO2 powders. By method of X-ray photoelectron spectroscopy significant amount of fluorine atoms in «green» silica (up to 5% (at.)) has been revealed, which could be introduced in SiO2 in the process of its preparation. In such a case, it was found that fluorine interacts with «green» silica by means of two mechanisms, leading to appearance of two phases within fluorinated powders of «green» SiO2.


2020 ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno ◽  
Alessandro Del Vecchio

Abstract This work focuses on the hydrothermal synthesis of Na-P1 zeolite by using a kaolinite rock coming from Romana (Sassari, Italy). The kaolin is calcined at a temperature of 650 °C and then mixed with calculated quantities of NaOH. The synthesis runs are carried out at ambient pressure and at variable temperatures of 65 ° and 100 °C. For the first time compared to the past, the Na-P1 zeolite is synthesized without the use of additives and through a protocol that reduces both temperatures and synthesis times. The synthesis products are analysed by X-ray diffraction, high temperature X-ray diffraction, infrared spectroscopy, scanning electron microscopy and inductively coupled plasma optical emission spectrometry. The cell parameters are calculated using the Rietveld method. Density and specific surface area are also calculated. The absence of amorphous phases and impurities in synthetic powders is verified through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods.The results make the experimental protocol very promising for an industrial transfer.


Coatings ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 553
Author(s):  
Dominik Höhlich ◽  
Thomas Mehner ◽  
Ingolf Scharf ◽  
Thomas Lampke

Ag–W two-phase system was prepared by electrodeposition using anhydrous 1-ethyl-3-methylimidazolium chloride [EMIm]Cl ionic-liquid (IL) solution with AlCl3 in different ratios. The deposition took place outside the glove box with a continuous Ar stream over the electrolyte at 120 °C and a pulsed-like current regime. Resultant layers show areas of Ag and W with an overall W content with a mass fraction of w W   = 50% (mole fraction x W   = 36.9%). The phase composition of Ag–W layers was observed by X-ray diffraction, and the chemical composition was characterized by scanning electron microscopy and inductively coupled plasma optical emission spectroscopy.


Author(s):  
Ilhem Rekkab-Hammoumraoui ◽  
Abderrahim Choukchou-Braham

A series of metal-loaded (Ru, Pt, Co) alumina catalysts were evaluated for the catalytic oxidation of cyclohexane using tertbutylhydroperoxide (TBHP) as oxidant and acetonitrile or acetic acid as solvent. These materials were prepared by the impregnation method and then characterized by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES), H2 chemisorption, Fourier Transformed Infrared Spectroscopy (FTIR), High-Resolution Transmission Electron Microscopy (HRTEM), and X-ray Diffraction (XRD). All the prepared materials acted as efficient catalysts. Among them, Ru/Al2O3 was found to have the best catalytic activity with enhanced cyclohexane conversion of 36 %, selectivity to cyclohexanol and cyclohexanone of 96 % (57.6 mmol), and cyclohexane turnover frequency (TOF) of 288 h-1. Copyright © 2018 BCREC Group. All rights reservedReceived: 26th May 2017; Revised: 17th July 2017; Accepted: 18th July 2017; Available online: 22nd January 2018; Published regularly: 2nd April 2018How to Cite: Rekkab-Hammoumraoui, I., Choukchou-Braham, A. (2018). Catalytic Properties of Alumina-Supported Ruthenium, Platinum, and Cobalt Nanoparticles towards the Oxidation of Cyclohexane to Cyclohexanol and Cyclohexanone. Bulletin of Chemical Reaction Engineering & Catalysis, 13(1): 24-36 (doi:10.9767/bcrec.13.1.1226.24-35) 


2020 ◽  
Vol 11 (1) ◽  
pp. 8034-8042

The incorporation of magnesium (Mg) in tricalcium phosphate (TCP) was prepared through a precipitation method followed by calcination at 850 °C in air. Calcium hydroxide, (Ca(OH)2), phosphoric acid, (H3PO4), and magnesium chloride (MgCl2.6H2O) with a Ca/P ratio of 1.5, were mixed as the precursor materials. The concentration of added Mg was varied with respect to calcium (Ca) precursor molarity as such Mg/(Ca +Mg) molar ratio was 0.05, 0.10, and 0.15, while the (Ca+Mg)/P ratio was maintained at 1.50 throughout the experiment. The influence of Mg-doped TCP on phase composition, chemical structure, and a functional group at different weight percentages were accomplished through X-ray diffraction (XRD), inductively coupled plasma optical emission spectroscopy (ICP-OES) and Fourier Transform Infrared Spectroscopy (FTIR) analyses. Based in the results of this research, the presence of magnesium led to the formation of Mg-doped calcium-deficient apatite (MgCDA) at 80°C and Mg-doped β-TCP at 850°C; the incorporation of Mg into the TCP phase causing an expansion of the lattice and increase in the lattice parameter. This result could be considered rather unusual.


2003 ◽  
Vol 763 ◽  
Author(s):  
S. Kosaraju ◽  
I. Repins ◽  
C. A. Wolden

AbstractIn the synthesis of copper chalcopyrite solar absorbers the chalcogen source is always supplied in excess due to its low reactivity. This paper describes preliminary work aimed at addressing this issue through plasma processing. An inductively coupled plasma (ICP) was use to activate both sulfur and selenium vapors. First, the thermodynamic arguments for using activated chalcogens are presented. Next, this paper describes the experimental ICP setup and its characterization using optical emission spectroscopy (OES). Stable discharges have been achieved with both sulfur and selenium vapors using argon as a carrier gas. The potential of this approach was demonstrated by converting indium films into In2Se3 and InSx. The indium samples were inserted into chalcogen-containing ICP plasmas. Through X-ray diffraction it was observed that chalcogen conversion was achieved in a matter of minutes at room temperature by plasma processing.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Daniela Novembre ◽  
Domingo Gimeno ◽  
Alessandro Del Vecchio

AbstractThis work focuses on the hydrothermal synthesis of Na-P1 zeolite by using a kaolinite rock coming from Romana (Sassari, Italy). The kaolin is calcined at a temperature of 650 °C and then mixed with calculated quantities of NaOH. The synthesis runs are carried out at ambient pressure and at variable temperatures of 65 and 100 °C. For the first time compared to the past, the Na-P1 zeolite is synthesized without the use of additives and through a protocol that reduces both temperatures and synthesis times. The synthesis products are analysed by X-ray diffraction, high temperature X-ray diffraction, infrared spectroscopy, scanning electron microscopy and inductively coupled plasma optical emission spectrometry. The cell parameters are calculated using the Rietveld method. Density and specific surface area are also calculated. The absence of amorphous phases and impurities in synthetic powders is verified through quantitative phase analysis using the combined Rietveld and reference intensity ratio methods. The results make the experimental protocol very promising for an industrial transfer.


2014 ◽  
Vol 976 ◽  
pp. 119-123
Author(s):  
Jaime Guerrero-Paz

The effect of the powder quantity on the effectiveness of the mechanical alloying process using different ductile powder systems was studied. X-ray diffraction, inductively coupled plasma-optical emission spectroscopy and energy dispersive x-ray spectrometry-scanning electron microscopy were the techniques employed to characterize the mechanically alloyed powders. Results showed that a same volume of powders, which represented different powder mass quantities for each system and composition, was used to mechanically alloy in an effective way in horizontal ball mills.


Author(s):  
Yangyang Zhang ◽  
Chuan Shao ◽  
Dongling Qin ◽  
Gang Yang

Solid acid-catalyzed dehydration of fructose to produce 5-hydroxymethylfurfural (5-HMF) has been a hotspot in biomass conversion research in recent years. In this study, a novel SAPO‑34‑based catalyst was prepared by consecutive steps of titanium doping, sulfuric acid impregnation, and sulfonic acid functionalization. Characterization of the catalyst with X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett-Teller (BET), inductively coupled plasma optical emission spectrometer (ICP-OES), and acid-base titration revealed different pore structures and more acid content compared to SAPO‑34. The catalyst was applied to the preparation of 5-HMF by dehydration of fructose, and the maximum yield (74.0%) of 5-HMF was obtained by reacting in dimethyl sulfoxide (DMSO) at 170 °C for 50 min. In addition, the applicability of the catalytic system to other substrates and the stability of the catalyst after five cycles were investigated, which are valuable for further probing on the concerned aspects.


2002 ◽  
Vol 16 (06n07) ◽  
pp. 1132-1137 ◽  
Author(s):  
N. JIANG ◽  
S. XU ◽  
K. N. OSTRIKOV ◽  
E. L. TSAKADZE ◽  
J. D. LONG ◽  
...  

An attempt for modification of carbon nitride material by introduction of Al to form a ternary Al-C-N compound in a thin film deposited using inductively coupled plasma (ICP) assisted DC magnetron sputtering is reported. Optical emission spectroscopy (OES) is used for in-situ observation and identification of reactive species. The films were characterized using x-ray photoelectron spectroscopy (XPS) and x-ray diffraction spectroscopy (XRD). The results indicate that C-N bond is formed in the plasma. The XPS narrow scam spectra confirm the existence of C-Al, sp2C-N and sp3C-N bonds. Elemental proportion of carbon increases with the CH4/N2 flow rate ratio, and has a tendency to saturate. The film is dominated by c-AlN (111), mixed with Al4C3 and AlCN ternary compound.


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