Search results for: Palladium

Authors: Shashikant R. Kuchekar, Somnath D. Bhumkar, Haribhau R. Aher, Bhaskar H. Zaware, Ponnadurai Ramasami

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A precise, sensitive, rapid and selective method for the solvent extraction, spectrophotometric determination of palladium(II) using para-methylphenyl thiourea (PMPT) as an extractant is developed. Palladium(II) forms yellow colored complex with PMPT which shows an absorption maximum at 300 nm. The colored complex obeys Beer’s law up to 7.0 µg ml^-1 of palladium. The molar absorptivity and Sandell’s sensitivity were found to be 8.486 x 10³ l mol^-1cm^-1 and 0.0125 μg cm^-2 respectively. The optimum conditions for the extraction and determination of palladium have been established by monitoring the various experimental parameters. The precision of the method has been evaluated and the relative standard deviation has been found to be less than 0.53%. The proposed method is free from interference from large number of foreign ions. The method has been successfully applied for the determination of palladium from alloy, synthetic mixtures corresponding to alloy samples.

Keywords: Para-methylphenyl thiourea, palladium, spectrophotometry.

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Authors: S.Fardindoost, A. Iraji Zad, S.M.Mahdavi

Abstract:

Tungsten trioxide has been prepared by using P-PTA as a precursor on alumina substrates by spin coating method. Palladium introduced on WO3 film via electrolysis deposition by using palladium chloride as catalytic precursor. The catalytic precursor was introduced on the series of films with different morphologies. X-ray diffractometry (XRD), Scanning electron microscopy (SEM) and XPS were applied to analyze structure and morphology of the fabricated thin films. Then we measured variation of samples- electrical conductivity of pure and Pd added films in air and diluted hydrogen. Addition of Pd resulted in a remarkable improvement of the hydrogen sensing properties of WO3 by detection of Hydrogen below 1% at room temperature. Also variation of the electrical conductivity in the presence of diluted hydrogen revealed that response of samples depends rather strongly on the palladium configuration on the surface.

Keywords: Electrolysis, Hydrogen sensing, Palladium, WO3

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Authors: Noor S. Nasri, Eric C. A. Tatt, Usman D. Hamza, Jibril Mohammed, Husna M. Zain

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Catalytic combustion of methane is imperative due to stability of methane at low temperature. Methane (CH4), therefore, remains unconverted in vehicle exhausts thereby causing greenhouse gas GHG emission problem. In this study, heterogeneous catalysts of palladium with bio-char (2 wt% Pd/Bc) and Al2O3 (2wt% Pd/ Al2O3) supports were prepared by incipient wetness impregnation and then subsequently tested for catalytic combustion of CH4. Support-porous heterogeneous catalytic combustion (HCC) material were selected based on factors such as surface area, porosity, thermal stability, thermal conductivity, reactivity with reactants or products, chemical stability, catalytic activity, and catalyst life. Sustainable and renewable support-material of bio-mass char derived from palm shell waste material was compared with those from the conventional support-porous materials. Kinetic rate of reaction was determined for combustion of methane on Palladium (Pd) based catalyst with Al2O3 support and bio-char (Bc). Material characterization was done using TGA, SEM, and BET surface area. The performance test was accomplished using tubular quartz reactor with gas mixture ratio of 3% methane and 97% air. The methane porous-HCC conversion was carried out using online gas analyzer connected to the reactor that performed porous-HCC. BET surface area for prepared 2 wt% Pd/Bc is smaller than prepared 2wt% Pd/ Al2O3 due to its low porosity between particles. The order of catalyst activity based on kinetic rate on reaction of catalysts in low temperature was 2wt% Pd/Bc>calcined 2wt% Pd/ Al2O3> 2wt% Pd/ Al2O3>calcined 2wt% Pd/Bc. Hence agro waste material can successfully be utilized as an inexpensive catalyst support material for enhanced CH4 catalytic combustion.

Keywords: Catalytic-combustion, Environmental, Support-bio-char material, Sustainable, Renewable material.

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Authors: Tossaporn Jindarat, Siriporn Jongpatiwut, Somchai Osuwan, Suchada Butnark

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Deoxygenation of beef fat for the production of hydrogenated biodiesel is investigated in a high pressure continuous flow fixed bed reactor over palladium-supported mesoporous titania catalyst synthesized via a combined single-step sol-gel process with surfactant-assisted templating method (SATM). The catalyst possessed a mesoporous charactheristic with high surface area and narrow pore size distribution. The main products of all Pd/TiO2 catalysts are n-heptadecane (n-C17) and n-pentadecane (n-C15) resulting from decarbonylation reaction. Pd/TiO2 catalyst synthesized via a combined single-step sol-gel process with SATM (SSSG) gave higher activity and selectivity to the desired products when compared to IWI/SG-TiO2 and IWI/P25-TiO2, respectively. SSSG catalyst gave the average conversion up to 80-90 % and 80 % for the selectivity in diesel range hydrocarbons. This result may cause by the higher surface area and the ability in dispersion of palladium ion in mesoporous of TiO2 during sol-gel process.

Keywords: Beef fat, Deoxygenation, Hydrogenated biodiesel, Pd/TiO2

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Authors: Dalia Angeles-Wedler, Katrin Mackenzie, Frank-Dieter Kopinke

Abstract:

Palladium-catalyzed hydrodechlorination is a promising alternative for the treatment of environmentally relevant water bodies, such as groundwater, contaminated with chlorinated organic compounds (COCs). In the aqueous phase hydrodechlorination of COCs, Pd-based catalysts were found to have a very high catalytic activity. However, the full utilization of the catalyst-s potential is impeded by the sensitivity of the catalyst to poisoning and deactivation induced by reduced sulfur compounds (e.g. sulfides). Several regenerants have been tested before to recover the performance of sulfide-fouled Pd catalyst. But these only delivered partial success with respect to re-establishment of the catalyst activity. In this study, the deactivation behaviour of Pd/Al2O3 in the presence of sulfide was investigated. Subsequent to total deactivation the catalyst was regenerated in the aqueous phase using potassium permanganate. Under neutral pH condition, oxidative regeneration with permanganate delivered a slow recovery of catalyst activity. However, changing the pH of the bulk solution to acidic resulted in the complete recovery of catalyst activity within a regeneration time of about half an hour. These findings suggest the superiority of permanganate as regenerant in re-activating Pd/Al2O3 by oxidizing Pd-bound sulfide.

Keywords: Deactivation, hydrodechlorination, Pd catalyst, regeneration.

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Authors: Alexey P. Antropov, Alexander V. Ragutkin, Nicolay A. Yashtulov

Abstract:

The original controlled technology for power active nanocomposite membrane-electrode assembly engineering on the basis of porous silicon is presented. The functional nanocomposites were studied by electron microscopy and cyclic voltammetry methods. The application possibility of the obtained nanocomposites as high performance renewable energy sources for micro-power electronic devices is demonstrated.

Keywords: Cyclic voltammetry, electron microscopy, nanotechnology, platinum-palladium nanocomposites, porous silicon, power activity, renewable energy sources.

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Authors: K. Ahmad, M. Suhaimi, Mohamad N. Azmi, K. Awang, Mohd A. Nafiah

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The conceptually construction of axially chiral indolostilbenesi.eN-(2-{(E)-2-[2'-(1-Acetyl-1H-indol-2-yl)-3'chloro-4,4',6,6'-tetramethoxy[1,1'-biphenyl]-2yl]ethenyl}phenyl)acetamide and N-(2-{(E)-2-[2'-(1-Acetyl-1H-indol-2-yl)-3'-chloro-2,4',6,6'-tetramethoxy[1,1'-biphenyl]-4-yl]ethenyl}phenyl) acetamide are described in this paper. These structure, were obtained by the tactical combination of palladium-catalyzed coupling which produced 10-acetamido-3,5-dimethoxystilbene, follow by FeCl₃-induced oxidative cyclization/dimerisation. All structures were unambiguously confirmed by 1D (¹H, ¹³C) and 2D NMR experiment, (COSY, HMQC, HMBC) and mass spectrometry.

Keywords: Indolostilbene, FeCl3-oxidative cyclization, Oligostilbenooids, Oxidative cyclization/dimerization.

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Authors: Asım Egitmen, Aysen Demir, Burcu Darendeli, Fatma Ulusal, Bilgehan Güzel

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Synthesizing supercritical carbon dioxide (scCO₂) soluble precursors would be helpful for many processes of material syntheses based on scCO₂. Ligand (amphi-(1Z, 2Z)-N-(2-fluoro-3-(trifluoromethyl) phenyl)-N'-hydroxy-2-(hydroxyimino) were synthesized from chloro glyoxime and flourus aniline and Pd(II) complex (precursor) prepared. For scCO₂ deposition method, organometallic precursor was dissolved in scCO₂ and impregnated onto the SBA-15 at 90 °C and 3000 psi. Then the organometallic precursor was reduced with H₂ in the CO₂ mixture (150 psi H₂ + 2850 psi CO₂). Pd deposited support material was characterized by ICP-OES, XRD, FE-SEM, TEM and EDX analyses. The Pd loading of the prepared catalyst, measured by ICP-OES showed a value of about 1.64% mol/g Pd of catalyst. Average particle size was found 5.3 nm. The catalytic activity of prepared catalyst was investigated over Suzuki-Miyaura C-C coupling reaction in different solvent with K₂CO₃ at 50 ^oC. The conversion ratio was determined by gas chromatography.

Keywords: Nanoparticle, nanotube, oximes, precursor, supercritical CO2.

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Authors: M. G. Rostedt, M. J. Hall, L. Shi, R. D. Matthews

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Silicon substrates coated with multiwalled carbon nanotubes (MWCNTs) were experimentally investigated to determine spark breakdown voltages relative to uncoated surfaces, the degree of surface degradation associated with the spark discharge, and techniques to minimize the surface degradation. The results may be applicable to instruments or processes that use MWCNT as a means of increasing local electric field strength and where spark breakdown is a possibility that might affect the devices’ performance or longevity. MWCNTs were shown to reduce the breakdown voltage of a 1mm gap in air by 30-50%. The relative decrease in breakdown voltage was maintained over gap distances of 0.5 to 2mm and gauge pressures of 0 to 4 bar. Degradation of the MWCNT coated surfaces was observed. Several techniques to improve durability were investigated. These included: chromium and gold-palladium coatings, tube annealing, and embedding clusters of MWCNT in a ceramic matrix.

Keywords: Ionization sensor, spark, nanotubes, electrode, breakdown.

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Authors: Tebogo Phetla, Edison Muzenda, M Belaid

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This study investigated possible ways to improve the efficiency of the platinum precipitation process using ammonium chloride by reducing the platinum content reporting to the effluent. The ore treated consist of five platinum group metals namely, ruthenium, rhodium, iridium, platinum, palladium and a precious metal gold. Gold, ruthenium, rhodium and iridium were extracted prior the platinum precipitation process. Temperature, reducing agent, flow rate and potential difference were the variables controlled to determine the operation conditions for optimum platinum precipitation efficiency. Hydrogen peroxide was added as the oxidizing agent at the temperature of 85-90oC and potential difference of 700-850mV was the variable used to check the oxidizing state of platinum. The platinum was further purified at temperature between 60-65oC, potential difference above 700 mV, ammonium chloride of 200 l, and at these conditions the platinum content reporting to the effluent was reduced to less than 300ppm, resulting in optimum platinum precipitation efficiency and purity of 99.9%.

Keywords: Platinum Group Metals (PGM), Potential difference, Precipitation, Redox reactions.

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Authors: Lalita Saeaeh, Sirirat Jitkarnka

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Pyrolysis of waste tire is one of alternative technique to produce petrochemicals, such as light olefins, mixed C4, and monoaromatics. Noble metals supported on acid zeolite catalysts were reported as potential catalysts to produce the high valuable products from waste tire pyrolysis. Especially, Pd supported on HBeta gave a high yield of olefins, mixed C4, and mono-aromatics. Due to the high prices of noble metals, the objective of this work was to investigate whether or not a non-noble Ni metal can be used as a substitute of a noble metal, Pd, supported on HBeta as a catalyst for waste tire pyrolysis. Ni metal was selected in this work because Ni has high activity in cracking, isomerization, hydrogenation and the ring opening of hydrocarbons Moreover, Ni is an element in the same group as Pd noble metal, which is VIIIB group, aiming to produce high valuable products similarly obtained from Pd. The amount of Ni was varied as 5, 10, and 20% by weight, for comparison with a fixed 1 wt% Pd, using incipient wetness impregnation. The results showed that as a petrochemical-producing catalyst, 10%Ni/HBeta performed better than 1%Pd/HBeta because it did not only produce the highest yield of olefins and cooking gases, but the yields were also higher than 1%Pd/HBeta. 5%Ni/HBeta can be used as a substitute of 1%Pd/HBeta for similar crude production because its crude contains the similar amounts of naphtha and saturated HCs, although it gave no concentration of light mono-aromatics (C6-C11) in the oil. Additionally, 10%Ni/HBeta that gave high olefins and cooking gases was found to give a fairly high concentration of the light mono-aromatics in the oil.

Keywords: Catalytic pyrolysis; Waste tire; Pd; Ni; HBeta

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Authors: M. Areekijseree, M. Pumipaiboon, S. Nuamsukon, K. Kittiwattanawong, C. Thongchai, S. Sikiwat, T. Chuen-Im

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There are few studies on eggshell of leatherback turtle which is endangered species in Thailand. This study was focusing on the ultrastructure and elemental composition of leatherback turtle eggshells collected from Andaman Sea Shore, Thailand during the nesting season using scanning electron microscope (SEM). Three eggshell layers of leatherback turtle; the outer cuticle layer or calcareous layer, the middle layer or middle multistrata layer and the inner fibrous layer were recognized. The outer calcareous layer was thick and porosity which consisted of loose nodular units of various crystal shapes and sizes. The loose attachment between these units resulted in numerous spaces and openings. The middle layer was compact thick with several multistrata and contained numerous openings connecting to both outer cuticle layer and inner fibrous layer. The inner fibrous layer was compact and thin, and composed of numerous reticular fibers. Energy dispersive X-ray microanalysis detector revealed energy spectrum of X-rays character emitted from all elements on each layer. The percentages of all elements were found in the following order: carbon (C) > oxygen (O) > calcium (Ca) > sulfur (S) > potassium (K) > aluminum (Al) > iodine (I) > silicon (Si) > chlorine (Cl) > sodium (Na) > fluorine (F) > phosphorus (P) > magnesium (Mg). Each layer consisted of high percentage of CaCO3 (approximately 98%) implying that it was essential for turtle embryonic development. A significant difference was found in the percentages of Ca and Mo in the 3layers. Moreover, transition metal, metal and toxic non-metal contaminations were found in leatherback turtle eggshell samples. These were palladium (Pd), molybdenum (Mo), copper (Cu), aluminum (Al), lead (Pb), and bromine (Br). The contamination elements were seen in the outer layers except for Mo. All elements were readily observed and mapped using Smiling program. X-ray images which mapped the location of all elements were showed. Calcium containing in the eggshell appeared in high contents and was widely distributing in clusters of the outer cuticle layer to form CaCO3 structure. Moreover, the accumulation of Na and Cl was observed to form NaCl which was widely distributing in 3 eggshell layers. The results from this study would be valuable on assessing the emergent success in this endangered species.

Keywords: Leatherback turtle (Dermochelys coriacea), SEM (SEI/EDX), turtle eggshell.

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