Estudo dos principais fatores que influenciam na solubilização dos hpas em águas

Polycyclic aromatic hydrocarbons (PAHs) constitute a family of compounds characterized by having two or more condensed aromatic rings and for being a class of substances that are widely distributed in the environment as a complex mixture, being very persistent in the environment due to its low solubility in water. The application of chemometric methods to analytical chemistry has provided excellent results in studying the solubility of PAHs in aqueous media in order to understand the mechanisms involved in environmental contamination. The method consists in analyzing the solubilization of PAHs from diesel oil in water varying parameters such as stirring time, volume of oil added and pH, using a full factorial design of two levels and three factors. PAHs were extracted with n-hexane and analyzed by fluorescence spectroscopy because they have molecular characteristics fluorescent due to the large number of condensed rings and links, and gas chromatography coupled to a mass spectrometer (GC-MS). The results of fluorescence analysis showed that only the stirring time and pH influenced the solubility of PAHs in diesel fuel. How is a non-selective technique for the study of fluorescence was performed on form and semi-quantitative. And for the chromatographic analysis the results showed that the solubility of the different PAHs is influenced differently so that you can classify them into groups by the results of the effects

Estudo da estabilidade térmica de adoçantes naturais e artificiais

Sweeteners provide a pleasant sensation of sweetness that helps the sensory quality of the human diet, can be divided into natural sweeteners such as fructose, galactose, glucose, lactose and sucrose, and articial sweeteners such as aspartame, cyclamate and saccharin. This work aimed to study the thermal stability of natural and artificial sweeteners in atmospheres of nitrogen and syntetic air using thermogravimetry (TG), derivative thermogravimetry (DTG), Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC). Among the natural sweeteners analyzed showed higher thermal stability for the lactose and sucrose, which showed initial decomposition temperatures near 220 ° C, taking advantage of the lactose has a higher melting point (213 ° C) compared to sucrose (191 ° C). The lower thermal stability was observed for fructose, it has the lowest melting point (122 °C) and the lower initial decomposition temperature (170 °C). Of the artificial sweeteners studied showed higher thermal stability for sodium saccharin, which had the highest melting point (364 ° C) as well as the largest initial decomposition temperature (466 ° C under nitrogen and 435 ° C in air). The lower thermal stability was observed for aspartame, which showed lower initial decomposition temperature (158 ° C under nitrogen and 170 ° C under air). For commercial sweeteners showed higher thermal stability for the sweeteners L and C, which showed initial temperature of thermal decomposition near 220 ° C and melting points near 215 ° C. The lower thermal stability was observed for the sweetener P, which showed initial decomposition temperature at 160 ° C and melting point of 130 °C. Sweeteners B, D, E, I, J, N and O had low thermal stability, with the initial temperature of decomposition starts near 160 °C, probably due to the presence of aspartame, even if they have as the main constituent of the lactose, wich is the most stable of natural sweeteners. According to the results we could also realize that all commercial sweeteners are in its composition by at least a natural sweeteners and are always found in large proportions, and lactose is the main constituent of 60% of the total recorded

Craqueamento termocatalítico de óleo de girassol na presença da peneira molecular SAPO-5

The catalytic cracking of triglycerides presents itself as a possible alternative to the production of biofuels with low emission of pollutants. In this work were synthesized the SAPO-5, the catalysts for the cracking reaction of soybean oil is presented. The solids were powder X-ray diffraction (XRD), thermogravimetric analysis (TG/DTG) and infrared spectroscopy (FTIR). The analyses indicated that the synthesis method has employed to obtain materials with high surface area and high acid. The soybean oil thermal and thermal catalytic cracking, realized from the room temperature to 450 ºC in a simple distillation system, has allowed obtaining two liquid fractions, each consisting of two phases, one aqueous and another organic, organic liquid (OL). The OL obtained from first fractions has shown high acid index, even in the thermal catalytic process. The products obtained in the cracking of soybean oil were analyzed by distillation, acid number, infra-red spectroscopy, density, viscosity, carbon residue, cetane number determination and characterization. The analysis of the products obtained in the presence and in the absence of the SAPO-5 permitted to conclude that all the solids tested presented catalytic activity in the deoxygenation of final products only at the second step of the cracking process

Síntese e caracterização da peneira molecular MCM-41 contendo terras raras na dessulfurização, utilizando tiofeno como molécula sonda

Mesoporous molecular sieves of MCM-41 type are considered as promising support for metal in the refining processes of petroleum-based materials as catalysts and adsorbents for environmental protection. In this work, mesoporous molecular sieves MCM-41 were modified with different rare earth ions (La, Eu e Yb) for the obtaining nanostrutured materials with catalytic properties. The catalysts were synthesized by the hydrothermal method at 100oC for 120 h, presenting, all the samples, in the gel of synthesis molar ratio Si/Ln = 50. The obtained materials after calcination at 500oC for 2 h were characterized by XRD, surface area BET, TG/DTG, FTIR, and hydrothermal stability at 700ºC. The XRD analysis of the catalysts indicated that the materials containing rare earth presented characteristic hexagonal structure of the mesoporous materials of the type MCM-41. The TG curves showed that the decomposition of the structural template occurs in the materials at temperatures lower than 500oC. The samples presented variations as the specific superficial area, average diameter of pores and thickness of the silica wall, as a function of the nature of the rare earth impregnated in the mesoporous material. Hydrotermal stability was evaluated through the exposition of the materials to water vapour at 700°C. The thiophene adsorptions reach a maximum at 80% of conversion and incorporation of the rare earths showed influence in the process. Adsorption capacity followed the sequence: Yb-MCM-41 < La-MCM-41 < Eu-MCM-41 < MCM-41

Tecnologia eletroquímica como tratamento alternativo de efluentes têxteis sintéticos utilizando ânodos de platina e diamante

In this work, the treatment of synthetic wastewaters containing Remazol Red BR (RRB) and Novacron Blue C-D (NB) by anodic oxidation using boron doped diamond anodes (BDD) and Novacron Yellow (YN) using BDD and Platinum (Pt) anodes was investigated. Galvanostatic electrolyses of RRB and NB synthetic wastewaters have led to the complete decolorization removal at different operating conditions (current density, pH and temperature). The influence of these parameters was investigated in order to find the best conditions for dyestuff colour removal. According to the experimental results obtained, the electrochemical oxidation process is suitable for decolorizing wastewaters containing these textile dyes, due to the electrocatalytic properties of BDD and Pt anode. Energy requirements for removing colour during galvanostatic electrolyses of RRB, NB and YN synthetic solutions depends mainly on the operating conditions; for example for RRB, it passes from 3.30 kWh m-3 at 20 mA cm-2 to 4.28 kWh m-3 at 60 mA cm-2 (pH = 1); 15.23 kWh m-3 at 20 mA cm-2 to 24.75 kWh m-3 at 60 mA cm-2 (pH = 4.5); 10.80 kWh m-3 at 20 mA cm-2 to 31.5 kWh m-3 at 60 mA cm-2 (pH = 8) (data estimated per volume of treated effluent). In order to verify the Brazilian law regulations of NB and RRB synthetic solutions after electrochemical decolourisation treatment, Hazen Units values were determined and the total colour removal was achieved; remaining into the regulations. Finally, electrical energy cost for removing colour was estimated

Estudo termoanalítico da perlita hidrofobizada com óleo de linhaça

In this work, expanded perlite, a mineral clay, consisting of SiO2 and Al2O3 in the proportions of 72.1 and 18.5%, respectively, was used as an adsorbent for oil in its pure expanded form as well as hydrofobized with linseed oil. Thermogravimetry (TG), Derivative Thermogravimetry (DTG) and Differential Thermal Analysis (DTA) were used to study the thermal behavior and quantify the percent adsorption of perlite in differents processes comparing the results with the ones obtained using Gravimetric Analysis. In the process of hydrophobization with linseed oil granulometric fractions > 20, 20-32 and 32-60 mesh were used and adsorption tests with crude oil were performed in triplicate at room temperature. The results obtained by TG/DTG in dynamic atmosphere of air showed mass losses in a single step for the expanded perlite with pure adsorbed oil, indicating that the adsorption of oil was limited and that the particle size did not in this process. Linseed oil has performed well as an agent of hydrophobized perlite (32 to 60 mesh) indicating a maximum percentage of 59.9% and 68.6% the linseed with a fraction range from considering the data obtained by thermogravimetry and Gravimetry, respectively. The adsorption of oil in the expanded perlite and hydrofobized pure perlite with linseed oil did not produce good results, characterizing an increase of 0.5 to 4.6% in pure perlite and 3.3% in hydrofobized perlite with granulometric 32 to 60 mesh

Avaliação da síntese e caracterização de zeólita ZSM-5 ausente de direcionador orgânico estrutural

The catalytic processes play a vital role in the worldwide economy, a business that handles about US$ 13 billion per year because the value of products depends on the catalytic processes, including petroleum products, chemicals, pharmaceuticals, synthetic rubbers and plastics, among others. The zeolite ZSM-5 is used as catalyst for various reactions in the area petrochemical, petroleum refining and fine chemicals, especially the reactions of cracking, isomerization, alkylation, aromatization of olefins, among others. Many researchers have studied the hydrothermal synthesis of zeolite ZSM-5 free template and they obtained satisfactory results, so this study aims to evaluate the hydrothermal synthesis and the physicochemical properties of ZSM-5 with the presence and absence of template compared with commercial ZSM-5. The methods for hydrothermal synthesis of zeolite ZSM-5 are of scientific knowledge, providing the chemical composition required for the formation of zeolitic structure in the presence and absence of template. Samples of both zeolites ZSM-5 in protonic form were obtained by heat treatment and ion exchange, according to procedures reported in the literature. The sample of commercial ZSM-5 was acquired by the company Sentex Industrial Ltda. All samples were characterized by XRD, SEM, FTIR, TG / DTG / DSC, N2 adsorption and desorption and study of acidity by thermo-desorption of probe molecule (n-butylamine), in order to understand their physicochemical properties. The efficiency of the methods applied in this work and reported in the literature has been proved by well-defined structure of ZSM-5. According as the evaluation of physicochemical properties, zeolite ZSM-5 free template becomes promising for application in the refining processes or use as catalytic support, since its synthesis reduces environmental impacts and production costs

Obtenção de biodiesel através da transesterificação do óleo de farelo de arroz utilizando KI/Al2O3

This study proposes to find a biodiesel through transesterification of rice bran oil with KI/Al2O3 checking the influence of two types of alumina (Amorphous and Crystalline) for conversion into methyl esters. The catalyst was synthesized by the wet impregnation method. Adding 30 mL of 35% KI(aq.) in 10 g of alumina, under stirring at 80 °C for 3 hours. The reaction conditions used in this study were optimized, with a molar ratio methanol:oil of 15:1, 8 h of reaction time and reflux temperature. The catalyst amount was varied in the range of 1 to 5 % wt. The solid catalysts materials were analyzed by: x-ray diffraction (XRD), thermogravimetry (TG), N2 adsorption/desorption, scanning electron microscopy (SEM) and basicity, for the identification of its structure and composition, verifying the presence of basic sites. The results showed that Al2O3(A) presents an amorphous structure, high surface area and a better catalytic activity, in relation to the catalyst synthesized with Al2O3(C) support that proved to have a more crystalline structure, having as well, a lesser surface area, enabling difficulties for the incorporation of active sites. The obtained biodiesel with 5% wt. KI/Al2O3(A) presented physicochemical properties within the standards specified by the Resolution No 7/2008 ANP and obtained the best reaction yield with 95.2%, according to quantitative measurement from the TG, which showed 96.2% conversion into methyl esters. It was furthermore found that with the increasing amount of the quantity of the catalyst in the reaction, there was also an increase in the ester content obtained. The specific mass and the kinematic viscosity were reduced with the increase of the amount of quantity of the catalyst, indicating an increase in the conversion of triglycerides

Avaliação da influência da matéria orgânica, na determinação quantitativa de metais em amostras de sedimento, por espectrometria de absorção atômica e análise de metais traços por fluorescência de raios-X

The proposal of this work is to evaluate the influence of the organic matter on the results of the analyses of the metals (Zn, Pb, Al, Cu, Cr, Fe, Cd e Ni) for Atomic Absorption Spectrometry (AAS), so much in the extraction stage as in the reading using for that the chemometrics. They were used for this study sample of bottom sediment collected in river Jundiaí in the vicinity of the city of Macaíba-RN, commercial humus and water of the station of treatment of sewer of UFRN. Through the analyses accomplished by EAA it was verified that the interference of the organic matter happens in the extraction stage and not in the reading. With relationship to the technique of X Ray Fluorescence Spectrometry (XRFS), the present work has as intended to evaluate the viability of this technique for quantitative analysis of trace metals (Cr, Ni, Cu, Zn, Rb, Sr and Pb) in having leached obtained starting from the extraction with acqua regia for an aqueous solution. The used samples constitute the fine fraction (<0.063 mm) of sediments of swamp of the river Jundiaí. The preparation of tablets pressed starting from the dry residue of those leached it allowed your analysis in the solid form. This preliminary study shows that, in the case of the digestion chemistry partially of the fine fractions of bottom sediments used for environmental studies, the technique of applied EFRX to the analysis of dry residues starting from having leached with acqua regia, compared her it analyzes of the leached with ICP-OES, it presents relative mistakes for Cu, Pb, Sr and Zn below 10%

Estudo termoanalítico de medicamentos de referência, genérico e similar

This study aimed to apply, thermogravimetriy /derivative Thermogravimetriy (TG/DTG), differential scanning calorimetry (DSC), Differential Thermal Analysis (DTA), to conduct a comparative study on drug reference, generic and whose active principles are similar captopril hydrochlorothiazide, ampicillin, paracetamol, aspirin and mebendazole sold in local pharmacies. Samples of the active ingredients and dosage forms were also characterized by absorption infrared spectroscopy (IR), X-ray diffraction (XRD) and microscopy scanning electron (SEM). The TG / DTG curves showed a general similarity in the thermal behavior of the samples, but also showed the influence of excipients on the thermal stability. The DSC curve of the generic base hydrochlorothiazide showed no peak on the fusion of the drug due to interference of lactose as a diluent, which causes interaction with the active principle causing their degradation before the merger. The DSC curves of the drugs consisting of paracetamol showed reproducibility at the melting point of the active and the other thermal events. The DSC result of binary mixtures involving captopril / magnesium stearate and mebendazole/magnesium stearate showed possible interactions or incompatibilities evidenced by the displacement of the melting point of both drugs. The other mixtures showed no change. The infrared spectra presented were very similar, indicating the presence of functional groups characteristic of the constituents of the samples. The X-ray diffraction showed peaks indicative of crystalline structure of the active ingredients as well as some of the ingredients in the formulation of the drug and the micrographs indicate a general heterogeneity in the size distribution of particles in the samples

Adsorção de Mn (II) e Zn (II) em soluções aquosas usando perlita expandida revestida com quitosana

In this work, chitosan was used as a coating of pure perlite in order to increase the accessibility of the groups OH- e NH2+the adsorptionof ions Mn2+ e Zn2+.The characterization results of the expanded perlite classified as microporous and whose surface area 3,176 m2 g-1after the change resulted in 4,664 m2g-1.From the thermogravimetry(TG) it was found that the percentage of coating was34,3%.The infrared analysis can prove the presence of groups Si-OH, Si-O e Al-O-Siresulting from the perlite and C=O, NH2and OH characterization of chitosan. The experiments on experiments on the adsorption of Mn and Zn were performed in the concentration range of10 a 50 mgL-1and the adsorption capacity inpH 5,8 e 5,2 was 19,49 and 23,09 mgg-1to 25 oC,respectively.The adsorption data were best fitted to Langmuir adsorption model to Langmuir adsorption model for both metalionsisindicative of monolayer adsorption. The kinetics of adsorption were calculated from the equation of Lagergren fitting the model pseudo-second-order for all initial concentrations, suggesting that adsorption of ions Mn2+ and Zn2+ follows the kinetics of pseudo-second-order and whose constant Speedk2(g/mg.min) are 0,105 e 3,98 and capacity and maximum removal qe 4,326 e 3,348,respectively.In this study we used a square wave voltammetry cathodic stripping voltammetry to quantify the adsorbed ions, and the working electrode glassy carbon, reference electrode silver / silver chloride and a platinum auxiliary electrode. The attainment of the peaks corresponding to ions Mn2+ and Zn2+ was evaluated in and electrochemical cell with a capacity of 30 mL using a buffer system (Na2HPO4/NaH2PO4)at pH 4 and was adjusted with solutionsH3PO4 0,1molL-1and NaOH 0,1 molL-1and addition of the analyte has been a cathodic peak in- 0,873 Vand detection limit of2,55x10-6molL-1para Zn.The dough used for obtaining the adsorption isotherm was 150 mg and reached in 120 min time of equilibrium for both metal ions.The maximum adsorption for 120 min with Mn concentration 20 mgL-1 and Zn 10 mgL-1,was91, 09 e 94, 34%, respectively

Aplicação da tecnologia eletroquímica como alternativa para a remoção de corante têxteis em efluentes sintéticos e reais utilizando anodos de platina e diamante

In this work, electrochemical technology was used to treat synthetic wastewater containing Methyl Red (MR) and Blue Novacron (BN) by anodic oxidation using anodes platinum (Pt) and real samples of textile effluents using DDB anodes and platinum (Pt). The removal of color from the galvanostatic electrolysis of synthetic wastewater MR and BN, and the actual sample has been observed under different conditions (different current densities and temperature variation). The investigation of these parameters was performed in order to establish the best conditions for removal of color and chemical oxygen demand (BOD). According to the results obtained in this study, the electrochemical oxidation processes suitable for the degradation process of color and COD in wastewater containing such textile dyes, because the electrocatalytic properties of Pt and BDD anodes consumption energy during the electrochemical oxidation of synthetic solutions AN and MR and real sample, mainly depend on the operating parameters of operation, for example, the synthetic sample of MR, energy consumption rose from 42,00kWhm-3 in 40 mAcm-2 and 25 C to 17,50 kWhm-3 in 40mAcm-2 and 40 C, from the BN went 17,83 kWhm-3 in 40mAcm and 40°C to 14,04 kWhm- 3 in 40mAcm-2 and 40 C (data estimated by the volume of treated effluent). These results clearly indicate the applicability of electrochemical treatment for removing dyes from synthetic solutions and real industrial effluents

Determinação do teor de cálcio através da termogravimetria, em medicamentos utilizados no tratamento da osteoporose: um estudo comparativo

The present study utilized the thermogravimetry (TG) and optical emission spectroscopy with inductively coupled plasma - ICP / OES to determine the calcium content in tablets of carbonate, citrate and calcium lactate used in the treatment of osteoporosis. The samples were characterized by IR, SEM, TG / DTG, DTA, DSC and XRD. The thermal analysis evaluated the thermal stability and physical-chemical events and showed that the excipients influence the decomposition of active ingredients. The results of thermogravimetry indicated that the decomposition temperature of the active CaCO3 (T = 630.2 °C) is lower compared to that obtained in samples of the tablets (633.4 to 655.2 °C) except for sample AM 2 (Ti = 613.8 oC). In 500.0 °C in the samples of citrate and calcium lactate, as well as their respective active principles had already been formed calcium carbonate. The use of N2 atmosphere resulted in shifting the initial and final temperature related to the decomposition of CaCO3. In the DTA and DSC curves were observed endo and exothermic events for the samples of tablets and active ingredients studied. The infrared spectra identified the main functional groups in all samples of active ingredients, excipients and tablets studied, such as symmetric and asymmetric stretches of the groups OH, CH, C = O. Analysis by X-ray diffraction showed that all samples are crystalline and that the final residue showed peaks indicative of the presence of calcium hydroxide by the reaction of calcium oxide with moisture of the air. Although the samples AM 1, AM 2, AM 3 and AM 6 in their formulations have TiO2 and SiO2 peaks were not observed in X-ray diffractograms of these compounds. The results obtained by TGA to determine the calcium content of the drugs studied were satisfactory when compared with those obtained by ICP-OES. In the AM 1 tablet was obtained the content of 35.37% and 32.62% for TG by ICP-OES, at 6 AM a percentage of 17.77% and 16.82% and for AM 7 results obtained were 8.93% for both techniques, showing that the thermogravimetry can be used to determine the percentage of calcium in tablets. The technique offers speed, economy in the use of samples and procedures eliminating the use of acid reagents in the process of the sample and efficiency results.

Uso da palha de carnaúba em revestimento de dutos

In this work, the plant species Copernicia prunifera (Miller) H. E. Moore (carnauba), naturally occurring which prevails in the northeast region of Brazil was the subject of studies aiming its use as external coating of pipelines used in petroleum industry. The part of the plant worked were the leaves, also called straw, which were coated with resinous material. For this purpose, it was necessary to evaluate the effectiveness of the use of acrylic resins in the straw carnauba coating. The properties of the untreated carnauba straw and chemically treated with sodium hydroxide, hexane and carbon tetrachloride were investigated by ATRFTIR, SEM and thermal analysis. The first two techniques showed that treatment with solvents has caused major changes in the straw surface, while the thermal analysis indicated that the sodium hydroxide caused variations in thermal stability of straw constituents. Water absorption measurements showed that treatments have accelerated the absorption process and the reduction of contact angle values for treated samples with solvents indicated higher hidrophilicity of straw. The tensile tests showed lower values of elastic modulus and tensile strength for treated samples. Furthermore, coatings using pure commercial resins A and B as well as the formulations with clay were applied in straw and they were examined once again through thermal analysis, water absorption measurements, contact angle and mechanical tests. To analyze the effect of heat ageing, samples were subjected to tensile tests again in order to assess its resistance. The results showed that the resins/clay formulations increased thermal stability of straw, they promoted a good impermeabilization and caused significant decrease in the values of elastic modulus and tensile strength. Evaluating the ageing effect on the mechanical properties, it has been showed good recovery to the coated straw with the formulations A 60 and A 80% in modulus and tensile strength values and elongation at break values have remained very close. It is thus concluded that the carnauba straw can be used as a coating of pipelines with significant cost savings, since there is no need for pretreatment for its use and shows itself as a viable biotechnology alternative, contributing to the quality of coatings material and environment preservation.

Caracterização do processo de gelificação de soluções quitosana utilizando reometria e espalhamento dinâmico da luz

Gels consist of soft materials with vast use in several activities, such as in pharmaceutical industry, food science, and coatings/textile applications. In order to obtain these materials, the process of gelification, that can be physical (based on physical interactions) and/or chemical (based on covalent crosslinking), has to be carried out. In this work we used dynamic light scattering (DLS) and rheometry to monitor the covalent gelification of chitosan solutions by glutaraldehyde. Intensity correlation function (ICF) data was obtained from DLS and the exponential stretched Kohrausch-William-Watts function (KWW) was fitted to them. The parameters of the KWW equation, β, Γ and C were evaluated. These methods were effective in clarifying the process of sol-gel transition, with the emergence of non-ergodicity, and determining the range of gelation observed in about 10-20 minutes. The dependence between apparent viscosity on reaction time was used to support the discussion proposed.