Avaliação da liberação de NH4NO3 ocluido em zeólita 4A a partir de soluções salinas

The zeolite 4A was used to evaluate the thermo kinetics parameters of NH4+ and NO3- ions occluded in its structure. The Osawa method for activation energy calculation was used to evaluate its thermal stability, and the results shown that the ion species interact differently depending on the zeolite pores, which determines the controlled release by its structure.

Purificação e caracterização da quitinase de uva (Vitis vinífera L. cv Red Globe) para a produção de quitosana a partir de quitina de camarão

Chitinase is produced by a wide variety of plants as a defense against peste attacks. In this study, grape chitinases were purified 16 times by fractionation in 80% ammonium sulfate followed by dialysis and filtration. Purified chitinases exhibited enzymatic activity toward chitin azure. The yield of purified chitinase was 229 mg/L with chitinase activity of 563 U/g. Chitinases had molecular masses of 24 and 30 kDa, as evaluated by SDS-PAGE 12.5%. Two pH optima were determined 3.0 and 6.0. The optimal temperature was 42 °C. Pre hydrolysis of crystalline shrimp chitin by chitinases caused in an increase in the deacetylation ratio triggered by chitin deacetylase producing chitooligosaccharides with DA (degree acetylation) of 58.8%.

In situ synthesis of nanoclay filled polyethylene using polymer supported metallocene catalyst system

In situ ethylene polymerizations were performed using bis(cyclopentadiene)titanium dichloride supported on polyethersulfone as catalyst. The bis(cyclopentadiene)titanium dichloride supported on polyethersulfone catalyst activity estimated by ethylene polymerization was 360 kgPE/molTi/h. During polymerization the fillers used were montmorillionite nanoclays having surface modifications with 35-45 wt% dimethyl dialkyl(14-18)amine (FA) and 25-30 wt% trimethyl stearyl ammonium (FB). These fillers were pretreated with methylaluminoxine (MAO; cocatalyst) for better dispersion onto the polymer matrix. The formation of polyethylene within the whole matrix was confirmed by FTIR studies. It was found that the nature of nanofiller did not have any remarkable effect on the melting characteristics of the polymer. TGA study indicates that nanoclay FB filled polyethylene has higher thermal stability than nanoclay FA filled polyethylene. The melting temperature of the obtained polyethylenes was 142 ºC, which corresponds to that synthesized by the polyether sulfone supported catalyst.

Estudo da emissão por fluorescência de ultravioleta na quantificação de um inibidor de corrosão do tipo sal de amônio quaternário em água

Quaternary ammonium salts are the corrosion inhibitors most frequently used by the oil industry. In this study, the ultraviolet fluorescence technique was evaluated for the analysis of a quaternary ammonium salt in water as a corrosion inhibitor. The comparison with standard salt showed that an alkyl aryl quaternary ammonium salt is the main fluorophore, with emission maxima at 306 and 593 nm. The best instrumental parameters were: width of excitation and emission slits of 10 and 15 nm, respectively, and scan rate of 10 nm min-1. The presence of aromatic compounds and biocides affects the analysis of corrosion inhibitors.

Montmorilonita modificada como catalisador heterogêneo em reações de esterificação (m)etílica de ácido láurico

ABSTRACT Montmorillonite was modified with zirconium polyoxycations in the presence of ammonium sulphate. The material was characterized and used as a catalyst in the esterification of lauric acid, the reactions being accompanied by 2³ factorial design. Conversions of up to 95.33 and 83.35% were observed for the methyl and ethyl esterification reactions respectively, proving superior to results obtained by thermal conversion. The material was submitted to three reaction cycles and similar conversions were observed, indicating the catalyst is not significantly deactivated after reuse. The catalyst was also tested under reflux conditions, yielding a maximum conversion of 36.86%.

Isolamento do tungstênio da volframita da mina de Igarapé Manteiga (Rondônia - Brasil) por lixiviação ácida

We report results of the efficiency of tungsten extraction from wolframite concentrate (containing 61.5 wt % WO3) from the Igarapé Manteiga mine (state of Rondônia, Brazil) through acid leaching with strong mineral acids at 100 ºC and 400 rpm for 2-4 h. HCl yielded insoluble matter containing the highest WO3 content (90 wt %). This solid was dissolved in concentrated NH3(aq) at 25 ºC and the insoluble matter filtrated. The filtrate was slowly evaporated. 70 wt % of the tungsten present in the starting concentrate material was recovered as ammonium paratungstate (APT).

Processing of spent NiW/Al2O3 catalysts

Spent oxidized (500 ºC, 5 h) commercial NiW/Al2O3 catalysts were processed using two different routes: a) fusion with NaOH (650 ºC, 1 h), the roasted mass was leached in water; b) leaching with HCl or H2SO4 (70 ºC, 1-3 h). HCl was the best leachant. In both routes, soluble tungsten was extracted at pH 1 with Alamine 336 (10 vol.% in kerosene) and stripped with 2 mol L-1 NH4OH (25 ºC, one stage, aqueous/organic ratio = 1 v/v). Tungsten was isolated as ammonium paratungstate at very high yield (> 97.5%). The elements were better separated using the acidic route.

Desenvolvimento de um método analítico baseado em microextração líquido-líquido para a determinação de cromo (VI) em amostras aquosas com detecção por espectrometria de absorção atômica em chama

In this study, a method for determination of hexavalent chromium in aqueous samples using liquid-liquid microextraction (LLME) and detection by Flame Atomic Absorption Spectrometry (F AAS) was developed. The LLME procedure was based on the extraction of Cr (VI) by acetone at a sample pH of 1.2. The use of saturated ammonium sulphate solution allowed effective separation of the aqueous and organic phases and acetone extracted chromium. The sample pH, acetone volume and stirring time were optimized by a full factorial design.

Produção de biossurfactantes por microrganismos isolados de solo contaminado com óleo diesel

The aim of this work was to produce biosurfactants through submerged fermentation using microorganisms isolated from soil contaminated with diesel. Microorganisms were isolated, characterized by the production of biosurfactants, and used to study the influence of type, induction and concentration of ammonium sulfate as a nitrogen source in the culture medium. The microorganisms that showed best results, in terms of production of biosurfactants, were identified as being of the genus Pseudomonas and Bacillus. The biosurfactants produced proved capable of reducing the surface tension of the media to 39 mN/m and 34 mN/m, respectively. Higher biosurfactant production was obtained in the medium containing 1% soybean oil without ammonium sulfate.

Emissões de óxido nitroso do tanque de aeração de uma estação de tratamento de esgotos com sistema de lodos ativados convencional

Nitrous oxide (N2O) emissions were measured monthly from January to June 2010 in the aeration tank of a wastewater treatment plant (WWTP) in Southeast Brazil. Emissions were lower in summer than winter and were positively related with influent ammonium (NH4+) concentration. The average N2O emission was 1.11 kg N day-1 corresponding to 0.02% of the influent total nitrogen load. The average emission factor calculated for the population served was 2.5 lower than that proposed by the Intergovernmental Panel on Climate Change (IPCC) for inventories of N2O emissions from WWTPs with controlled nitrification and denitrification processes.

Acúmulo de cargas elétricas em propelente sólido compósito com matriz de polibutadieno líquido hidroxilado

Composite solid propellants prepared with HTPB prepolymer - Hydroxyl Terminated Polybutadiene, AP - Ammonium Perchlorate as oxidizer and aluminum particles as an additive metal, have characteristics of high electrical resistivity. The loading process of the polymer matrix did not obtain homogeneity, resulting in clusters, mainly of metal particles. The effect of clustering in the composite was studied and observed experimentally, and this effect was one of the factors explaining the phenomenon of electrical charging of the composite. This electrical potential, when discharged abruptly, can generate an electric spark with sufficient energy for sustained ignition of a solid rocket motor.

Desenvolvimento de um método para a determinação de tioconazol associado a nanocápsulas poliméricas por cromatografia líquida

The aim of this work was to develop and validate an analytical method for the quantification of tioconazole in polymeric nanocapsule suspensions by high performance liquid chromatography with UV detection. The analysis was performed with a mobile phase composed of methanol:water (80:20) and 0.18% ammonium hydroxide; RP-18 column and UV detection at 219 nm. The method proved to be linear in the concentration range of 5-50 µg mL-1 (r = 0.9999), specific, precise (repeatability RSD = 1.42%, intermediate precision RSD = 1.17%), accurate (98 - 102%) and robust (RSD < 2.0%). In conclusion, a simple and rapid method was validated proving suitable for quantification of tioconazole in polymeric nanocapsules.

Determinação da atividade antitríptica em proteínas de produtos do amendoim isoladas por cromatografia de afinidade

The peanut is an oleaginous plant of high nutritional value, a source of protein and a trypsin inhibitor. Trypsin inhibitors are proteins present in the vegetable kingdom, considered anti-nutritional factors for animals. However, there have been several recent reports about their heterologous and beneficial effects on human health. These important effects have been the focus of studies investigating these inhibitors in foods. The aim of the present study was to isolate and determine the estimated molecular mass and specific inhibitory activity, for trypsin in the Japanese peanut, peanut butter, and peanut nougat using the techniques of precipitation with ammonium sulfate and affinity chromatography on trypsin - Sepharose CNBr 4B. The techniques used in this study were efficient for isolating the protein inhibitors with antitryptic specific activity of 694 UI mg-1, 823 UI mg-1 and 108 UI mg-1 for the Japanese peanut, peanut nougat, and peanut butter, respectively. The techniques featured high selectivity of the adsorbent, with consequent efficiency in isolation, given the low amount of dosed proteins and specific antitryptic activity presented by the products studied. The various health-related benefits show the importance of detecting and isolating efficient trypsin inhibitors in foods, taking into account the health claims attributed to the vegetable and its high consumption by humans.

RAPID AND SENSITIVE DETERMINATION OF PALLADIUM USING HOMOGENEOUS LIQUID-LIQUID MICROEXTRACTION VIA FLOTATION ASSISTANCE FOLLOWED BY GRAPHITE FURNACE ATOMIC ABSORPTION SPECTROMETRY

A method for the determination of trace amounts of palladium was developed using homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA) followed by graphite furnace atomic absorption spectrometry (GFAAS). Ammonium pyrrolidine dithiocarbamate (APDC) was used as a complexing agent. This was applied to determine palladium in three types of water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added to the extraction cell which contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Parameters affecting extraction efficiency were investigated and optimized. Under the optimum conditions, the calibration graph was linear in the range of 1.0-200 µg L-1 with a limit of detection of 0.3 µg L-1. The performance of the method was evaluated for the extraction and determination of palladium in water samples and satisfactory results were obtained. In order to verify the accuracy of the approach, the standard addition method was applied for the determination of palladium in spiked synthetic samples and satisfactory results were obtained.

NANOPARTICLES OF TUNGSTEN AS LOW-COST MONOMETALLIC CATALYST FOR SELECTIVE HYDROGENATION OF 3-HEXYNE

Low-cost tungsten monometallic catalysts containing variable amounts of metal (4.5, 7.1 and 8.5%W) were prepared by impregnating alumina with ammonium metatungstate as an inexpensive precursor. The catalysts were characterized using ICP, XPS, XRD, TPR and hydrogen chemisorption. These techniques revealed mainly WO3-Al2O3 (W6+) species on the surface. The effects of the content of W nanoparticles and reaction temperature on activity and selectivity for the partial hydrogenation of 3-hexyne, a non-terminal alkyne, were assessed under moderate conditions of temperature and pressure. The monometallic catalysts prepared were found to be active and stereoselective for the production of (Z )-3-hexene, had the following order: 7.1WN/A > 8.5 WN/A ≥ 4.5 WN/A. Additionally, the performance of the synthesized xWN/A catalysts exhibited high sensitivity to temperature variation. In all cases, the maximum 3-hexyne total conversion and selectivity was achieved at 323 K. The performance of the catalysts was considered to be a consequence of two phenomena: a) the electronic effects, related to the high charge of W (+6), causing an intensive dipole moment in the hydrogen molecule (van der Waals forces) and leading to heterolytic bond rupture; the H+ and H- species generated approach a 3-hexyne adsorbate molecule and cause heterolytic rupture of the C≡C bond into C- = C+; and b) steric effects related to the high concentration of WO3 on 8.5WN/A that block the Al2O3 support. Catalyst deactivation was detected, starting at about 50 min of reaction time. Electrodeficient W6+ species are responsible for the formation of green oil at the surface level, blocking pores and active sites of the catalyst, particularly at low reaction temperatures (293 and 303 K). The resulting best catalyst, 7.1WN/A, has low fabrication cost and high selectivity for (Z )-3-hexene (94%) at 323 K. This selectivity is comparable to that of the classical and more expensive industrial Lindlar catalyst (5 wt% Pd). The alumina supported tungsten catalysts are low-cost potential replacements for the Lindlar industrial catalyst. These catalysts could also be used for preparing bimetallic W-Pd catalysts for selective hydrogenation of terminal and non-terminal alkynes.