Geração sonoquímica de oxidantes em solução aquosa saturada de tetracloreto de carbono

In this work the CCl4 degradation in aqueous solution by sonication with 40 kHz commercial ultrasonic bath was investigated. Sonochemical degradation of CCl4 occur by the cleavage of C-Cl bond into the cavitation bubbles. Oxidation reactions and the pH decreasing in the bulk solution during sonication were attributed to chlorine radicals produced by CCl4 sonolysis, leading to increase the chloride concentration. The formation of oxidizing agents was evaluated employing I- and Fe2+ ion solutions, converted to I2 and HIO, and Fe3+, respectively. The amount of chloride and hydronium ions produced after 3 min of irradiation was 11.52 and 12.19 mmol, respectively, suggesting that the same reaction was involved to produce these ions. Fe2+ oxidation and the pH variation were monitored to estimate chlorine radical formation rate in the presence (0.107 mumol s-1) and absence (0.092 mumol s-1) of metallic ion during the first minute of sonication.

Synthesis and characterization of manganese-glycine and copper-glycine adducts

This work reports the synthesis and characterization of adducts of general formula MCl2.ngly, where M= Mn and Cu; n= 2 and 4, and gly= glycine. The manganese adducts were synthesized by dissolution of both, manganese chloride and glycine in water, whereas the copper adducts were obtained by using an alternative solid state synthesis approach. For all adducts, the obtained infrared data shows that the coordination involves the amine nitrogen atom, as well as an oxygen atom of the COO- group. The TG curves for the synthesized adducts exhibit only one mass loss step associated with the release of glycine molecules.

Oxochloroalkoxide of the Cerium (IV) and Titanium (IV) as oxides precursor

The Cerium (IV) and Titanium (IV) oxides mixture (CeO2-3TiO2) was prepared by thermal treatment of the oxochloroisopropoxide of Cerium (IV) and Titanium (IV). The chemical route utilizing the Cerium (III) chloride alcoholic complex and Titanium (IV) isopropoxide is presented. The compound Ce5Ti15Cl16O30 (iOPr)4(OH-Et)15 was characterized by elemental analysis, FTIR and TG/DTG. The X-ray diffraction patterns of the oxides resulting from the thermal decomposition of the precursor at 1000 °C for 36 h indicated the formation of cubic cerianite (a = 5.417Å) and tetragonal rutile (a = 4.592Å) and (c = 2.962 Å), with apparent crystallite sizes around 38 and 55nm, respectively.

Enantioselective synthesis of aziridines using asymmetric transfer hydrogenation as a precursor for chiral derivatives used as bonding agent for rocket solid propellants

A rapid, expedient and enantioselective method for the synthesis of beta-hydroxy amines and monosubstituted aziridines in up to 99% e.e., via asymmetric transfer hydrogenation of a-amino ketones and cyclisation through treatment with tosyl chloride and base, is described. (1R,2R)-N-(para-toluenesulfonyl)-1,2-ethylenediamine with formic acid has been utilised as a ligand for the Ruthenium (II) catalysed enantioselective transfer hydrogenation of the ketones.The chiral 2-methyl aziridine, which is a potentially more efficient bonding agent for Rocket Solid Propellant has been successfully achieved.

Determinação espectrofotométrica de alumínio em concentrados salinos utilizados em hemodiálise empregando pré-concentração em fluxo

An automatic flow injection procedure for spectrophotometric aluminium determination in purified water and solutions containing high salts concentrations used for hemodyalisis treatment was developed. The method was base on reaction of Al3+ with cianine eriochrome R (ECR) after preconcentration using the AG50W-X8 cationic-exchange resin. Elution was carried out using a 1 % (m/v) calcium chloride solution. The manifold comprised an automatic proporcional injector controlled by a computer equipped with an eletronic interface and software written in QuicBASIC 4.5 with facilities to control the injector and perform data acquisition. Samples with concentration ranging from 4.96 to 19.90 µg L-1 Al were analyzed and recoveries between 88 and 113% were obtained by using the standard addition method. Other profitable analytical characteristics such as a relative standard deviation 1.3 % (n = 10) for a typical sample 14.5 µg L-1 Al, a linear response ranging up to 60.0 µg L-1Al, and a sampling throughput of 10 determinations per hour were achieved. A detection limit of 4.2 µg L-1 Al was estimated as suggested by IUPAC.

Construção e aplicação de eletrodo de aço inoxidável UNS S31254 como eletrodo indicador em titulações condutimétricas

UNS S31254 SS electrodes have been built to substitute platinum in conductimetric titrations. The electrodes were tested in both acid-basic titration (chloridric acid and sodium hydroxide) and precipitation titration (sodium chloride and argentum nitrate as titrant). The practical application was exemplified from conductimetric tritations of HF ¾ HNO3 mixtures used in metalurgical industry to passivate stainless steels. The results were compared with those obtained using commercial platinum electrodes. The equivalent volumes obtained were comparable within 3% experimental error. Its application depends on the nature of electrolyte. These results have shown that stainless steel, less expensive than platinum (about three order of magnitude), can substitute platinum electrodes in routine analyses and didactic laboratories.

Reagenssin pinta-aktiivisuuden hyödyntäminen sinkin uutossa

Työssä tutkittiin sinkin uutossa käytettävän di(2-etyyliheksyyli)fosforihappo (D2EHPA) -uuttoreagenssin faasikäyttäytymistä ja miten laimentimen koostumus, lämpötila ja orgaanisen faasin sinkkipitoisuus vaikuttavat faasitasapainoon. Laimentimen vaikutuksen havaittiin olevan pientä, kun taas lämpötilan nostaminen yli huoneenlämpötilan leventää faasidiagrammin yksifaasialuetta. Pienet orgaanisen faasin sinkkipitoisuudet eivät juuri vaikuta faasitasapainoon. Sinkin ja D2EHPA:n moolisuhteen ollessa välillä 0,1–0,2 kompleksin rakenne ilmeisesti muuttuu. Sinkkipitoisuuden kasvaessa yksifaasialue muodostuu pienemmillä ammoniakkimäärillä. Suurilla orgaanisen faasin sinkkipitoisuuksilla ja ammoniakkimäärillä muodostuu orgaanisen faasin ja vesifaasin välille kolmas nestefaasi. D2EHPA:n (40 p %) vesipitoisuuden ja viskositeetin pH riippuvuutta tutkittiin, kun laimentimena oli alifaattinen hiilivetyliuotin. Nostettaessa pH yli 3,5:n uuttoreagenssi alkoi muodostaa käänteismisellejä, jolloin orgaanisen faasin vesipitoisuus ja viskositeetti kasvoivat eksponentiaalisesti. Sinkin mukana uuttautuu epäpuhtauksia kuten Al3+, Co2+, Cu2+, Na+, Ni2+, Cl- ja F-. Takaisinuuton kautta epäpuhtaudet joutuvat talteenottoelektrolyysiin, jossa ne voivat vaikuttaa tuotteen laatuun ja laskea virtahyötysuhdetta. Tarkoituksena oli tutkia väheneekö epäpuhtauksien myötäuuttautuminen jollakin tietyllä sinkin latausasteella. Fluoridin ja kuparin uuttautumisen havaittiin vähenevän vasta, kun sinkin pitoisuus orgaanisessa faasissa oli yli 20 g/L lämpötilasta riippumatta. Fluoridi uuttautuu mahdollisesti alumiinikompleksina ja/tai fluorihappona. Koboltin ja nikkelin myötäuuttautumisen havaittiin vähenevän, kun sinkin latausaste oli yli 10 g/L. Natrium ja kloridi eivät myötäuuttautuneet.

Determinação potenciométrica em fluxo de cloreto de cetilpiridinio em desinfectantes bucais

The work describes a new procedure for cetylpyridinium chloride determination in oral disinfectants, based on a flow-injection system with potentiometric detection. The determination was based on the measurement of picrate concentration decrease as result of ion-pair reaction with the analyte present in the injected sample. In the optimised set-up the sample injection volume was kept at 400 µL and merged downstream with the reagent solution containing 1,0 x10-5 mol/L of picrate adjusted to pH 5.0 with citrate/citric acid buffer. The flow rate was fixed at 8 mL/min and the reactor length at 40 cm. The proposed procedure enables the determination of cetylpyridinium in the analytical range of 5,0x10-6 - 7,5x10-5 mol/L at a sampling rate of 60/h. The results for real samples had a precision better than 3% and were comparable to the labelled values.

Aplicações eletroanalíticas com eletrodos de prata confeccionados a partir de CDs graváveis

This paper presents a new way for the construction of silver electrodes utilizing recordable CDs. The new electrodes were explored for the quantification of chloride (by potentiometry/FIA), cyanide (by amperometry/FIA) and for lead analysis (by square wave voltammetry). For the flowing measurements, a digital multimeter, connected to a microcomputer (via RS 232 interface) was used to collect directly the potential signal (for Cl- measurements) or to take the output signal from a potentiostat (for CN- measurements). The square wave voltammetry analysis was performed in a commercial instrument. The results shown good performance of the new electrodes and the detection limit (s/n = 3) attained for these three analytes were: 0.2, 50, and 200 µg L-1 for Pb2+, Cl-, and CN- respectively.

Emprego de óxidos tipo perovskita nas oxidações do propano e CO

Simultaneous oxidation/co-precipitation of an equimolar mixture of La(III) and Co(II) nitrates and La(III) nitrate and Mn(II) chloride afforded a hydroxide gel, which was converted to LaCoO3 and LaMnO3 on calcination at 600 °C. After calcination, the obtained perovskites have been characterised by X-ray diffraction (XRD), X- ray photoelectron spectroscopy (XPS), thermogravimetric analysis (DTA - TGA) and BET specific surface determination. Specific surface areas of perovskites were 12 - 60 m²/g. XRD analysis showed that LaCoO3 and LaMnO3 are simple phase perovskite - type oxides. Traces of LaOCl, in addition to the perovskite were detected in the LaMnO3. The catalytic behavior was examined in the propane and CO oxidation. The LaCoO3 catalyst was more active to CO2 than the LaMnO3 catalyst.

Fouling management and retention in nanofiltration of integrated paper mill effluents

Nanofiltration performance was studied with effluents from the pulp and paper industry and with model substances. The effect of filtration conditions and membrane properties on nanofiltration flux, retention, and fouling was investigated. Generally, the aim was to determine the parameters that influence nanofiltration efficiency and study how to carry out nanofiltration without fouling by controlling these parameters. The retentions of the nanofiltration membranes studied were considerably higher than those of tight ultrafiltration membranes, and the permeate fluxes obtained were approximately the same as those of tight ultrafiltration membranes. Generally, about 80% retentions of total carbon and conductivity were obtained during the nanofiltration experiments. Depending on the membrane and the filtration conditions, the retentions of monovalent ions (chloride) were between 80 and 95% in the nanofiltrations. An increase in pH improved retentions considerably and also the flux to some degree. An increase in pressure improved retention, whereas an increase in temperature decreased retention if the membrane retained the solute by the solution diffusion mechanism. In this study, more open membranes fouled more than tighter membranes due to higher concentration polarization and plugging of the membrane material. More irreversible fouling was measured for hydrophobic membranes. Electrostatic repulsion between the membrane and the components in the solution reduced fouling but did not completely prevent it with the hydrophobic membranes. Nanofiltration could be carried out without fouling, at least with the laboratory scale apparatus used here when the flux was below the critical flux. Model substances had a strong form of the critical flux, but the effluents had only a weak form of the critical flux. With the effluents, some fouling always occurred immediately when the filtration was started. However, if the flux was below the critical flux, further fouling was not observed. The flow velocity and pH were probably the most important parameters, along with the membrane properties, that influenced the critical flux. Precleaning of the membranes had only a small effect on the critical flux and retentions, but it improved the permeability of the membranes significantly.