Synthesis, characterization and thermal behaviour of solid state compounds of 2-chlorobenzylidenepyruvate with trivalent aluminium, gallium, indium and scandium metals

Solid state compounds M-2-Cl-BP, where 2-Cl-BP is 2-chlorobenzylidenepyruvate and M represents Al, Ga, In, and Sc were prepared. X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA), have been used to characterize and to study the thermal behavior of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition of the compounds.

Synthesis and thermal studies of solid state 2-chloro-benzylidenepyruvic acid and its compounds with sodium, aluminium (III), gallium (III) and indium (III) cations

The synthesis of sodium 2-chlorobenzylidenepyruvate and its corresponding acid as well as binary, binary together with it's acid or hydroxo-2-chorobenzylidenepyruvate of aluminium (III), gallium (III) and indium (III), were isolated. Chemical analysis, thermogravimetry, derivative thermogravimetry (TG/DTG), simultaneous thermogravimetry-differential thermal analysis (TG-DTA) and X-ray powder diffractometry have been employed to characterize and to study the thermal behaviour of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition.

Synthesis, characterization and thermal behaviour of solid state compounds of 4-methoxybenzoate with Manganese, Nickel and Copper

Solid state M-L compounds, where M stands for bivalent Mn, Ni, Cu and L is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry - differential thermal analysis (TG-DTA), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

Synthesis, characterization and thermal studies of solid state 4-methylbenzylidenepyruvate of some trivalent metal ions

Solid state compounds of 4-methylbenzylidenepyruvate with Al(III), Ga(III), In(III) and Sc(III) have been synthesized. Complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA) have been used to characterize and to study the thermal behavior of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition of these compounds.

Synthesis, characterization and thermal behaviour of solid-state compounds of 2-methoxybenzoate with some bivalent transition metal ions

Solid-state M-2-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 2-MeO-Bz is 2-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), thermogravimetry, derivative thermogravimetry (TG/DTG), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to have information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

Synthesis, characterization and thermal behaviour of solid-state compounds of 4-methoxybenzoate with lanthanum (III) and trivalent lighter lanthanides

Solid-state M-4-MeO-Bz compounds, where M stands for trivalent La, Ce, Pr, Nd and Sm and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, polymorphic transformation, ligand's denticity, thermal behaviour and thermal decomposition of the isolated compounds.

Synthesis, characterization and thermal studies on solid state 3-methoxybenzoate of lighter trivalent lanthanides

Solid-state Ln -3-MeO-Bz compounds, where Ln stands for lighter trivalent lanthanides (La Sm) and 3-methoxybenzoate, have been synthesized. Thermogravimetry (TG), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information concerning the composition, dehydration, polymorphic transformation, thermal behaviour and thermal decomposition of the synthesized compounds.

Thermal decomposition of solid state compounds of lanthanide and yttrium benzoates in CO2 atmosphere

Solid-state Ln-Bz compounds, where Ln stands for trivalent lanthanides and Bz is benzoate have been synthesized. Simultaneous thermogravimetric and differential thermal analysis in a CO2 atmosphere were used to study the thermal decomposition of these compounds.

Comparison of the dehydration kinetics of solid state compounds of 2-methoxybenzylidenepyruvate with some divalent metal ions

Divalent metal complexes of ligand 2-methoxybenzylidenepyruvate with Fe, Co, Ni, Cu and Zn as well as sodium salt were synthesized and investigated in the solid state. TG curves of these compounds were obtained with masses sample of 1 and 5mg under nitrogen atmosphere. Different heating rates were used to characterize and study these compounds from the kinetic point of view. The activation energy and pre-exponential factor were obtained applying the Wall-Flynn-Ozawa method to the TG curves. The obtained data were evaluated and the values of activation energy (Ea / kJ mol-1) was plotted in function of the conversion degree (α). The results show that due to mass sample, different activation energies were obtained. The results are discussed mainly taking into account the linear dependence between the activation energy and the pre exponential factor, where was verified the effect of kinetic compensation (KCE) and possible linear relations between the dehydrations steps of these compounds.

Investigation of Oxygen Cutting Process in Solid-State Welding

The oxygen cutting is a thermal cutting process, in which metal is heated locally up to its ignition temperature and burnt off by oxygen blast. Oxygen cutting can be used to remove upset metal of a hollow bar occurred due to solid-state welding process. The main goal of this research was to establish a connection between oxygen blasts and mass of metal removed and relate findings to production to suggest improvements to the current process. This master´s thesis describes the designing and building of a test rig for oxygen blowing measurements. It also contains all executed tests and test results, which were carried out. There are different cutting parameters which were studied as well as their effect on cutting process. The oxygen cutting process, used in solid-state welding process, can be improved by the test results.

Solid-state reference and ion-selective electrodes : towards portable potentiometric sensing

Potentiometric sensors are very attractive tools for chemical analysis because of their simplicity, low power consumption and low cost. They are extensively used in clinical diagnostics and in environmental monitoring. Modern applications of both fields require improvements in the conventional construction and in the performance of the potentiometric sensors, as the trends are towards portable, on-site diagnostics and autonomous sensing in remote locations. The aim of this PhD work was to improve some of the sensor properties that currently hamper the implementation of the potentiometric sensors in modern applications. The first part of the work was concentrated on the development of a solid-state reference electrode (RE) compatible with already existing solid-contact ion-selective electrodes (ISE), both of which are needed for all-solid-state potentiometric sensing systems. A poly(vinyl chloride) membrane doped with a moderately lipophilic salt, tetrabutylammonium-tetrabutylborate (TBA-TBB), was found to show a satisfactory stability of potential in sample solutions with different concentrations. Its response time was nevertheless slow, as it required several minutes to reach the equilibrium. The TBA-TBB membrane RE worked well together with solid-state ISEs in several different situations and on different substrates enabling a miniature design. Solid contacts (SC) that mediate the ion-to-electron transduction are crucial components of well-functioning potentiometric sensors. This transduction process converting the ionic conduction of an ion-selective membrane to the electronic conduction in the circuit was studied with the help of electrochemical impedance spectroscopy (EIS). The solid contacts studied were (i) the conducting polymer (CP) poly(3,4-ethylienedioxythiophene) (PEDOT) and (ii) a carbon cloth having a high surface area. The PEDOT films were doped with a large immobile anion poly(styrene sulfonate) (PSS-) or with a small mobile anion Cl-. As could be expected, the studied PEDOT solid-contact mediated the ion-toelectron transduction more efficiently than the bare glassy carbon substrate, onto which they were electropolymerized, while the impedance of the PEDOT films depended on the mobility of the doping ion and on the ions in the electrolyte. The carbon cloth was found to be an even more effective ion-to-electron transducer than the PEDOT films and it also proved to work as a combined electrical conductor and solid contact when covered with an ion-selective membrane or with a TBA-TBB-based reference membrane. The last part of the work was focused on improving the reproducibility and the potential stability of the SC-ISEs, a problem that culminates to the stability of the standard potential E°. It was proven that the E° of a SC-ISE with a conducting polymer as a solid contact could be adjusted by reducing or oxidizing the CP solid contact by applying current pulses or a potential to it, as the redox state of the CP solid-contact influences the overall potential of the ISE. The slope and thus the analytical performance of the SC-ISEs were retained despite the adjustment of the E°. The shortcircuiting of the SC-ISE with a conventional large-capacitance RE was found to be a feasible instrument-free method to control the E°. With this method, the driving force for the oxidation/reduction of the CP was the potential difference between the RE and the SC-ISE, and the position of the adjusted potential could be controlled by choosing a suitable concentration for the short-circuiting electrolyte. The piece-to-piece reproducibility of the adjusted potential was promising, and the day-today reproducibility for a specific sensor was excellent. The instrumentfree approach to control the E° is very attractive considering practical applications.

Downstream processing of pectinase produced by Aspergillus niger in solid state cultivation and its application to fruit juices clarification

In this work, a protocol for the formulation of an enzyme concentrated product to be applied in fruit juice treatment is described. Downstream processing conditions for the recovery and concentration of pectinases produced by the new strain Aspergillus niger LB-02-SF in solid state cultivation were assessed. The solid-liquid ratio in the extraction step of pectinases recovery from the cultivated media was evaluated and the highest activity was obtained with a solid-liquid ratio of 1:10. The crude extract was concentrated by ultrafiltration and the total pectinase (TP) activity was 73.6-fold concentrated in relation to the crude extract, and a final TP titer of 663 U mL–1 was obtained with 73.7% of recovery yield. KCl and different glycerol concentrations were added to the concentrated extract and the stability of pectinases during the storage at 5°C for 59 weeks was tested. The formulation with 50% w/w glycerol was applied to the treatment of apple and grape juices and the results of these tests were statistically comparable to those obtained with two high-quality commercial preparations.

Enhanced extraction of phenolic compounds from coffee industry’s residues through solid state fermentation by Penicillium purpurogenum

Abstract The use of agroindustrial residues is an economical solution to industrial biotechnology. Coffee husk and pulp are abounding residues from coffee industry which can be used as substrates in solid state fermentation process, thus allowing a liberation and increase in the phenolic compound content with high added value. By employing statistical design, initial moisture content, pH value in the medium, and the incubation temperature were evaluated, in order to increase the polyphenol content in a process of solid state fermentation by Penicillium purpurogenum. The main phenolic compounds identified through HPLC in fermented coffee residue were chlorogenic acid, caffeic acid, and rutin. Data obtained through HPLC with the radical absorbance capacity assay suggest the fermented coffee husk and pulp extracts potential as a source of phenolic acids and flavonoids. Results showed good perspectives when using P. purpurogenum strain to enhance the liberation of phenolic compounds in coffee residues.

Raman spectra of polymethyl methacrylate optical fibres excited by a 532 nm diode pumped solid state laser

Polymethyl methacrylate (PMMA) optical fibres are fabricated by a preform drawing process. The Raman spectra of PMMA fibres are recorded using a diode pumped solid state laser emitting at 532 nm and a CCD-spectrograph in the 400–3800 cm−1 range. The variation of the Raman intensity with the length of the optical fibre is studied. Investigations are carried out on the variation of FWHM of the Raman peak at 2957 cm−1 with the length of the optical fibre and pump power. The differential scattering cross section and gain coefficient of the Raman peak at 2957 cm−1 in PMMA are calculated in relation to that of toluene.