Rogério Marcos Dallago

Enzymatic synthesis of fructooligosaccharides by inulinases from Aspergillus niger and Kluyveromyces marxianus NRRL Y-7571 in aqueous–organic medium

This work is focused on the synthesis of the fructooligosaccharides (FOS) from sucrose and inulin, using free, immobilized and pre-treated immobilized inulinase from Kluyveromyces marxianus NRRL Y 7571 and Aspergillus niger in an aqueous-organic system. Initially, the influence of pre-treatment using four different gases, propane, n-butane, CO(2) and liquefied petroleum gas (LPG), was investigated towards FOS production and best results were found when both enzymes were previously treated with LPG. The best reaction yields were obtained when the immobilized enzymes were treated with LPG. Considering FOS synthesis using the enzyme from A. niger, yields of 26.62% of GF2 (kestose), 30.62% of GF3 (nystose) and 8.47% of GF4 (fructosyl nystose) were achieved using sucrose as substrate. Using inulinases from K. marxianus NRRL Y 7571, 11.89% of GF2 and 20.83% of GF3 were obtained, using inulin as substrate. However, promising results were achieved using the free form of inulinase from A. niger (77.19% of GF2; 14.03% of GF3 and 0.07% of GF4) using inulin as substrate.

Qualitative lead extraction from recycled lead-acid batteries slag.

The pyrometallurgic process that the exhausted batteries are submitted for the recovery of metallic lead generates great amount of a by-product called slag. The slag is composed mainly of iron ( approximately 60%) and lead ( approximately 6%), and this residue cannot be disposed in conventional landfill due to the high lead content. This work presents a new methodology for the extraction of lead from slag, based on the complexing effect of EDTA, a chelating ligand that has the ability to solubilize several heavy metals. As the iron (Fe(2+)/Fe(3+)) have a formations constant with EDTA higher than the lead and is present in high concentrations in the samples, the fluoride ion (F(-)) was employed to mask the iron ions. The tests were carried out in a qualitative way, confirming the lead extraction by the formation of a yellow precipitate of lead iodide.

Produção de carvão a partir de resíduo de erva-mate para a remoção de contaminantes orgânicos de meio aquoso

In this work we present a new adsorbent material, obtained by mate waste pyrolisis. The resulting charcoal presented high specific area when compared with other pyrolized materials and also high capacity to remove organic contaminants from aqueous solution. The charcoal showed specific area of 344, 191 and ~0.3 m2 g-1 for sample Mate 1, Mate 2 and Mate 3, respectively. According to the corresponding adsorption isotherm these materials present good adsorption capacity for reactive textile and methylene blue dyes and the herbicide atrazine. Adsorption maxima were respectively 16, 230 and 35 mg g-1 for such substances, when sample Mate 1 was used.In this work we present a new adsorbent material, obtained by mate waste pyrolisis. The resulting charcoal presented high specific area when compared with other pyrolized materials and also high capacity to remove organic contaminants from aqueous solution. The charcoal showed specific area of 344, 191 and ~0.3 m g for sample Mate 1, Mate 2 and Mate 3, respectively. According to the corresponding adsorption isotherm these materials present good adsorption capacity for reactive textile and methylene blue dyes and the herbicide atrazine. Adsorption maxima were respectively 16, 230 and 35 mg g for such substances, when sample Mate 1 was used.

Degradation of dimethyl disulfide using homogeneous Fenton's reaction

In this work the degradation of a model odor compound (dimethyl disulfide, DMDS) using Fentons reaction is reported. Dimethyl disulfide is present in wastewaters generated during production of poultry feather and viscera meal. Oxidation was carried out in batch reactor with temperature control. Experimental design technique was used to investigate the influence of concentration of hydrogen peroxide and Fe(2+), temperature and pH on degradation of DMDS. Control reactions using H(2)O(2) without Fe(2+) were carried out, but DMDS degradation could only reach 60% for a 0.025 mg L(-1) DMDS solution, at pH 3, 60 degrees C using 10,000 mg L(-1) H(2)O(2) in 30 min of reaction. The Fentons reaction could effectively remove DMDS, reaching 95% degradation at pH 3, 60 degrees C, 5 mg L(-1) H(2)O(2) and 1 mg L(-1) Fe(2+) after only 10 min of contact. A kinetic study of the Fentons reaction was carried out, varying the concentration of hydrogen peroxide, Fe(2+) and temperature.

Production and purification of amylolytic enzymes for saccharification of microalgal biomass.

The aim of this study was the production of amylolytic enzymes by solid state or submerged fermentations (SSF or SF, respectively), followed by purification using chemical process or microfiltration and immobilization of purified enzymes in a polyurethane support. The free and immobilized enzymes obtained were used to evaluate enzymatic hydrolysis of the polysaccharides of Spirulina. Microfiltration of the crude extracts resulted in an increase in their specific activity and thermal stability at 40°C and 50°C for 24h, as compared to extracts obtained by SSF and SF. Immobilization of polyurethane purified enzyme produced yields of 332% and 205% for the enzymes obtained by SF and SSF, respectively. Free or immobilized enzymes favor the generation of fermentable sugar, being the application of the purified and immobilized enzymes in the hydrolysis of microalgal polysaccharides considered a promising alternative towards development of the bioethanol production process from microalgal biomass.

Determination of carbofuran in pesticide formulations by flow injection spectrophotometry

A flow injection spectrophotometric method for the determination of carbofuran in commercial pesticide formulations was developed. The determination involves on-line hydrolysis of the extracted carbofuran at room temperature with sodium hydroxide. The resulting carbofuran-phenol is coupled with diazotized 4-aminobenzoic acid in order to achieve an appropriate selectivity and sensitivity for the spectrophotometric measurements. The calibration curve is linear over the range 1–10 mg litre−1 of carbofuran. The proposed method has a detection limit of 0.15 mg litre−1 of carbofuran and a sample frequency of 120 injections per hour. The relative standard deviation of six independent determinations of a sample containing 1 mg litre−1 carbofuran was 0.6%. The suitability of the proposed procedure for the determination of carbofuran in commercial pesticide formulations was studied. The procedure provides results comparable to those obtained by liquid chromatographic analysis. © 2000 Society of Chemical Industry

Variabilidade química de compostos orgânicos voláteis e semivoláteis de populações nativas de Maytenus ilicifolia

This work is focused on the chemical distribution of volatile and semi-volatile compounds of 18 native populations of Maytenus ilicifolia collected all over Brazil. The extracts of bulk samples (30 plants) of each population were obtained by supercritical CO2 extraction technique, and analyzed by GC/MS. The quantification of compounds (phytol, squalene, vitamin E, limonene, stigmasterol, friedelan-3-ol, friedelin, fridelan-3-one, palmitic acid and geranyl acetate) showed significant variations within the different populations, which could be related tom microclimate characteristics.

Optimization of the methodology for lead extraction from waste contaminated with heavy metals

A sequential experimental design strategy is used to optimize the extraction of lead from slag. The slag is composed mainly of iron (≈60%) and lead (≈6%), and cannot be disposed of in conventional landfill due to its high lead content. The extraction of lead is based on the complexing properties of ethylenediaminetetra‐acetic acid (EDTA), the iron being masked with fluoride ions. Atomic absorption spectroscopy (AAS) has been used for monitoring iron and lead concentrations. In a first step, Plackett–Burman PB‐12 experimental design was used for screening the variables and for selecting those to be used. Two central composite designs (CCDs) were then carried out to determine the optimal conditions for lead extraction. The optimized experimental conditions were established to be: contact time with the fluoride solution 30 min; particle size of slag between 150 and 600 µm; molecular concentration of fluoride solution 2.4 × 10−3 mol and of EDTA 5 × 10−4 mol; pH 1.5; 8 h contact time with the EDTA solution; and temperature 60°C. Under these experimental conditions the lead content was reduced by 57% compared with the raw sample.

Study of odor compounds in gaseous effluents generated during production of poultry feather and viscera meal using headspace solid phase microextraction

This work reports the screening and characterization of odor compounds in gaseous effluents generated during the production of poultry feather and viscera meal, the by-products of the poultry meat industry. Chemical analysis was carried out by solid phase microextraction in the headspace (HS-SPME) mode. Exhaust air of thermal processing of poultry feather and viscera were sampled online from a bench-scale digester, condensed, and collected in sampling flasks. Both volatile and semivolatile organic compounds present in the condensed gases were extracted under agitation at constant temperature. The extracts were analyzed with a gas chromatograph coupled to a mass spectrometric detector (GC/MSD). The identification of compounds was carried out by comparing the mass spectra obtained with those from the Wiley library and quantification was accomplished through authentic analytical standards. For the determination of the best extraction conditions and analysis, extraction fibers of different coatings and polarities were tested: divinylbenzene/carboxen/polydimethyilsiloxane (DVB/CAR/PDMS), carbowax/divinylbenzene (CW/DVB), and polydimethylsiloxane (PDMS) and chromatography columns of different polarities: DB-WAX (polar) and DB-5 (nonpolar). The best extraction conditions and analysis of the compounds of interest were obtained by the use of the SPME fiber with DVB/CAR/PDMS coating and analysis by GC/MSD with polar capillary column. Several carboxylic acids were identified, as well as mercaptans, amines, and aldehydes of great environmental importance.

Aspergillus niger inulinase immobilized in polyurethane foam and treated in pressurized LPG: A potential catalyst for enzymatic synthesis of fructooligosaccharides

Abstract Inulinase from Aspergillus niger was immobilized in polyurethane foam (PU). Immobilized catalyst was treated in pressurized liquefied petroleum gas (LPG) system. This biocatalyst was used in the fructooligosaccharide production using sucrose as substrate in aqueous system. The main objective of this study was to evaluate the reaction yield and productivity by using polyurethane foam as a low-cost support for enzyme immobilization in an alternative processes for fructooligosaccharide production in pressurized LPG system with potential for industrial application. The total FOS concentration obtained were 31% as a result of sucrose concentration reduction, and formation of FOS long chain (GF3 and GF4) from kestose (GF2). FOS concentrations of 5%, 22%, and 3% were obtained for GF2, GF3, and GF4, respectively. The methodology suggested in this research work, enzyme immobilization in a low-cost support, and treatment in LPG, showed potential technology for fructooligosaccharide synthesis.