Um experimento-charada usando data-show e resinas de troca iônica

A demonstractive experiment was proposed in order to verify students' habilities in recognizing the presence and nature of ions in solutions, before and after their passage through ion-exchange columns. The students have no previous contact with ion-exchange resins, so they must deduce how they work and explain the experimental facts. The performance of classes, at different stages of learning, is compared and discussed.

Uso da tecnologia de troca iônica no tratamento de águas contaminadas com Nitrato do Aqüífero Dunas-Barreiras, Natal/RN-Brasil

The city of Natal comprises an area of about 170 km² (65,63 squares miles). The Dunas-Barreiras Aquifer is the most important reservoir of the coastal basin of RN. It is being responsible for the water supplying of about 70% of the population, however, due to the sewage disposal system by cesspools and drains, it is presently affected in a great extent by nitrates contamination. Thus, the present work proposes to research the utilization of contaminated water by nitrates of this fountainhead and find cost of the potable water through the ionic exchange technology. This technology consists in the removal of mineral salts by the exchange of cations for one ion of hydrogen (H+), through the passage of water by cationic resin bed and, secondly, by the exchange of the anions for hydroxyl ions (OH-) through a anionic resin bed. The obtained results have showed the waters derived from fountains, big water holes and shallow wells were microbiologically contaminated, while the waters derived from deep wells (above 70 m 76,58 yards) were free of contamination. Thus, only these ones are suitable to the use of ionic technology. The experiments were conducted with the resin IMAC-HP-555 such as kinetic, thermodynamic, and adsorption by fixed bed studies, being obtained several project variables for the experimental column, as follow: work temperature of 25oC; resin maximum capacity maximum e mean of adsorption ==0,01692 g NO3-1/g R e 0,0110 g NO3-1/g R, respectively. On the experimental column were performed breakthrough tests which pointed for an average ideal average speed of work of 13.2 m / h, with an average efficiency of 45% of adsorption, an optimal concentration of NaCl desorption of 8%, and an ideal desorption time of 80 minutes for the equilibrium conditions of water from the Dunas-Barreiras aquifer. Scale projection for ion-exchange column for denitrification, for these variables, using a computer modeling programme, to project the column of ion exchange ROREX-420/2000, obtained a cost for the drinking water denitrified by this system of R$ 0,16 / m3

Emprego de carvão ativado e resinas de troca ionica na remoção de substâncias orgânicas contaminantes do alcool etílico

This work had with objective to characterize and evaluate the performance of the combined system, involving activated charcoal and ionic exchange resins in the removal of substances organic contaminating of the ethyl alcohol from the fermentation of the cassava starch. To testing was used ethyl alcohol PA 96 oGL, conductivity of 0.90 μS/cm at 25 oC, acidity of 60 mg/L and Barbet test of 43 minutes at 15 oC. The contaminated alcohol was composed of ethyl alcohol additive of higher alcohols, organic acids, ester, diol, aldehydes, ketone and ether. Contaminated alcohol was added 2% activated charcoal and after the adsorption isotherm in ionic exchange resins was tested. The adsorption with activated charcoal was performed in a Water Bath at 30 oC for one hour and a half and shaking. Already adsorption ionic exchange columns occurred at room temperature on columns of 93,4 cm in filling height and diameter of 2.29 cm, for flows of 180 mL/min and 90 mL/min. Samples were collected in the tests with charcoal and with each one of the resins and the following analyses were performed: conductivity, acidity and Barbet test. The medium values for conductivity, acidity and Barbet test after the adsorption in charcoal and cation and anion resins were respectively: conductivity was 240; 354 and 465 μS/cm to 25 oC; acidity of 1.081; 1.103 and 1.062 mg/L and the Barbet test was 21; 20 and 9 minutes to 15 oC. It was observed that the addition of 2% of activated charcoal and the permanence in the columns of adsorption was not sufficient to remove the organic substances contaminating of the ethyl alcohol.

Recuperação e purificação de proteínas do soro de queijo tipo coalho usando cromatografia de troca iônica e interação hidrofóbica em leito na forma expandida

Expanded Bed Adsorption plays an important role in the downstream processing mainly for reducing costs as well as steps besides could handling cells homogenates or fermentation broth. In this work Expanded Bed Adsorption was used to recover and purify whey proteins from coalho cheese manufacture using Streamline DEAE and Streamline SP both ionic resins as well as a hydrophobic resin Streamline Phenyl. A column of 2.6 cm inner diameter with 30 cm in height was coupled to a peristaltic pump. Hydrodynamics study was carried out with the three resins using Tris-HCl buffer in concentration of 30, 50 and 70 mM, with pH ranging from 7.0 to 8.0. In this case, assays of the expansion degree as well as Residence Time Distribution (RTD) were carried out. For the recovery and purification steps, a whey sample of 200 mL, was submitted to a column with 25mL of resin previously equilibrated with Tris/HCl (50 mM, pH 7.0) using a expanded bed. After washing, elution was carried out according the technique used. For ionic adsorption elution was carried out using 100 mL of Tris/HCl (50 mM, pH 7.0 in 1M NaCl). For Hydrophobyc interaction elution was carried out using Tris/HCl (50 mM, pH 7.0). Adsorption runs were carried out using the three resins as well as theirs combination. Results showed that for hydrodynamics studies a linear fit was observed for the three resins with a correlation coefficient (R2) about 0.9. In this case, Streamline Phenyl showed highest expansion degree reaching an expansion degree (H0/H) of 2.2. Bed porosity was of 0.7 when both resins Streamline DEAE and Streamline SP were used with StremLine Phenyl showing the highest bed porosity about 0.75. The number of theorical plates were 109, 41.5 and 17.8 and the axial dipersion coefficient (Daxial) were 0.5, 1.4 and 3.7 x 10-6 m2/s, for Streamline DEAE, Streamline SP and Streamline Phenyl, respectively. Whey proteins were adsorved fastly for the three resins with equilibrium reached in 10 minutes. Breakthrough curves showed that most of proteins stays in flowthrough as well as washing steps with 84, 77 and 96%, for Streamline DEAE, Streamline SP and Streamline Phenyl, respectively. It was observed protein peaks during elution for the three resins used. According to these peaks were identified 6 protein bands that could probably be albumin (69 KDa), lactoferrin (76 KDa), lactoperoxidase (89 KDa), β-lactoglobulin (18,3 KDa) e α-lactoalbumin (14 KDa), as well as the dimer of beta-lactoglobulin. The combined system compound for the elution of Streamline DEAE applied to the Streamline SP showed the best purification of whey proteins, mainly of the α-lactoalbumina

Purificação, modelagem e simulação da adsorção de bioprodutos por troca iônica em coluna de leito expandido

A produção de proteínas através de microrganismos tornou-se uma técnica muito importante na obtenção de compostos de interesse da indústria farmacêutica e alimentícia. Extratos brutos nos quais as proteínas são obtidas são geralmente complexos, contendo sólidos e células em suspensão. Usualmente, para uso industrial destes compostos, é necessário obtê-los puros, para garantir a sua atuação sem interferência. Um método que vem recebendo destaque especialmente nos últimos 10 anos é o uso da cromatografia de troca iônica em leito expandido, que combina em uma única etapa os passos de clarificação, concentração e purificação da molécula alvo, reduzindo assim o tempo de operação e também os custos com equipamentos para realização de cada etapa em separado. Combinado a este fato, a última década também é marcada por trabalhos que tratam da modelagem matemática do processo de adsorção de proteínas em resinas. Está técnica, além de fornecer informações importantes sobre o processo de adsorção, também é de grande valia na otimização da etapa de adsorção, uma vez que permite que simulações sejam feitas, sem a necessidade de gasto de tempo e material com experimentos em bancada, especialmente se é desejado uma ampliação de escala. Dessa forma, o objetivo desta tese foi realizar a modelagem e simulação do processo de adsorção de bioprodutos em um caldo bruto na presença de células, usando inulinase e C-ficocianina como objeto de estudo e purificar C-ficocianina utilizando resina de troca iônica em leito expandido. A presente tese foi então dividida em quatro artigos. O primeiro artigo teve como objeto de estudo a enzima inulinase, e a otimização da etapa de adsorção desta enzima em resina de troca iônica Streamline SP, em leito expandido, foi feita através da modelagem matemática e simulação das curvas de ruptura em três diferentes graus de expansão (GE). As máximas eficiências foram observadas quando utilizadas maiores concentrações de inulinase (120 a 170 U/mL), e altura de leito entre 20 e 30 cm. O grau de expansão de 3,0 vezes foi considerado o melhor, uma vez que a produtividade foi consideravelmente superior. O segundo artigo apresenta o estudo das condições de adsorção de C-ficocianina em resina de troca iônica, onde foi verificado o efeito do pH e temperatura na adsorção e após construída a isoterma de adsorção. A isoterma de adsorção da C-ficocianina em resina Streamline Q XL feita em pH 7,5 e a 25°C (ambiente), apresentou um bom ajuste ao modelo de Langmuir (R=0,98) e os valores qm (capacidade máxima de adsorção) e Kd (constante de equilíbrio) estimados pela equação linearizada da isoterma, foram de 26,7 mg/mL e 0,067mg/mL. O terceiro artigo aborda a modelagem do processo de adsorção de extrato não clarificado de C-ficocianina em resina de troca iônica Streamline Q XL em coluna de leito expandido. Três curvas de ruptura foram feitas em diferentes graus de expansão (2,0, 2,5 e 3,0). A condição de adsorção de extrato bruto não clarificado de C-ficocianina que se mostrou mais vantajosa, por apresentar maior capacidade de adsorção, é quando se alimenta o extrato até atingir 10% de saturação da resina, em grau de expansão 2,0, com uma altura inicial de leito de 30 cm. O último artigo originado nesta tese foi sobre a purificação de C-ficocianina através da cromatografia de troca iônica em leito expandido. Uma vez que a adsorção já havia sido estudada no artigo 2, o artigo 4 enfoca na otimização das condições de eluição, visando obter um produto com máxima pureza e recuperação. A pureza é dada pela razão entre a absorbância a 620 nm pela absorbância a 280 nm, e dizse que quando C-ficocianina apresenta pureza superior a 0,7 ela pode ser usada em como corante em alimentos. A avaliação das curvas de contorno indicou que a faixa de trabalho deve ser em pH ao redor de 6,5 e volumes de eluição próximos a 150 mL. Tais condições combinadas a uma etapa de pré-eluição com 0,1M de NaCl, permitiu obter C-ficocianina com pureza de 2,9, concentração 3 mg/mL, e recuperação ao redor de 70%.

CROMATOGRAFIA DE AFINIDADE COM CORANTE RED A versus TROCA IÔNICA-PERMEABILIDADE EM GEL: COMPARAÇÃO DA PRATICIDADE NA PURIFICAÇÃO DE ENTEROTOXINA ESTAFILOCÓCICA A

Culture supernatant of Staphylococcus aureus 722 in 3% triptone plus 1% yeast extract was used for EEA purification, proceeding comparison between dye ligand Red A affinity chromatography and classic chromatography. The capture of SEA with Amberlite CG-50 allowed rapid enterotoxin concentration from the culture supernatant. However, the ratio of 15 mg of the resin to a total of 150 mg of the toxin satured the resin, giving only 10 to 30% of SEA recuperation from the supernatant. The elution of concentrated material throught the Red A column resulted in a recovery of 60,87% of the toxin, and required 76 hours, indicating advantage on classic chromatography. Ion exchange column plus gel filtration recovered only 6,5 % of the SEA, and required 114 hours to conclude the procedure. The eletrophoresis of purified SEA indicated high grade of toxin obtained from Red A column, with 90 % of purity, compared to 60 % of classic column.

Avaliação da disponibilidade de manganês e ferro em solos pelo uso do método modificado da resina de troca iônica

A avaliação do método modificado da resina de troca de íons para extração de Mn e Fe dos solos foi o objetivo desta pesquisa. Foram utilizadas 44 amostras de solo, cujos teores de Mn variaram de baixos a altos e de Fe de médios a altos. Como plantas-teste, utilizaram-se o milho e a soja, cultivadas em casa de vegetação. O Fe e o Mn do solo foram determinados, usando o método modificado da resina de troca de íons, DTPA, AB-DTPA, Mehlich-1 e Mehlich-3. Os coeficientes de correlação entre Mn no solo e Mn acumulado na parte aérea da soja foram: resina (0,62*), DTPA (0,58*), Mehlich-3 (0,54*), Mehlich-1 (0,51*) e AB-DTPA (0,26NS). Para o milho, houve correlação entre Mn-solo e Mn-planta somente nas amostras de solo com baixos teores desse elemento, para todos os extratores, exceto para AB-DTPA. Concluiu-se que a resina foi tão eficiente quanto os extratores DTPA, M-1 e M-3 em avaliar a disponibilidade de Mn para a soja, e que nenhum extrator foi eficiente em avaliar a disponibilidade de Fe para as plantas de milho e soja, com 53 dias de idade, cultivadas em casa de vegetação.

Troca iônica no estado sólido de európio3+ em zeólita Y: influência do tempo de reação

Rare earth elements supported in zeolites are the most important catalysts in the fluid cracking of petroleum. The solid state ion exchange of Eu3+ in Y zeolite was investigated. First of all, the hydrated EuCl3 was well mixed in a ball mill and was then heated at 300ºC for different times. The quantitative determination of Eu3+ showed that the degree of ion exchange depends on the reaction time at constant temperature, being ~95% in 4 h. The X-ray study showed that the crystallinity of the zeolite is little affected by the exchange procedure. The study of spectroscopic properties of Eu3+, emission spectra and lifetime, give information about the migration and position of the ion in the zeolite cages.

Determinação de potássio em méis após precipitação com tetrafenilborato de sódio e separação em coluna de troca-iônica

A new method for determination of potassium in honey samples of different colors was developed as an alternative method for determination of this metal. Analysis of genuine honeys attested by the qualities and quantities tests officially adopted in Brazil, showed that the concentration of potassium ranged from 181 to 315 mg/kg for light honeys, from 393 to 570 mg/kg for medium honeys and from 791 to 915 mg/kg for dark honeys. Recoveries making use of spikes of potassium added to the honey samples and to the deionized distilled water showed results close by hundred percent at pH <= 2,0 under temperature bellow 20°C.

Hidrogenofosfato de titânio lamelar: síntese, troca iônica e intercalação

The development associated with the research field involving crystalline inorganic lamellar titanium hydrogenphosphate, Ti(HPO4).H2O, synthesized as alpha or gamma forms, is directly linked to the huge number of reactions, that occur inside the free interlamellar space. Two distinguishable well-characterized features such as ion-exchange and intercalation reactions are explored here. From the interactive point of view, the acidic OH centres distributed on the lamella can interact with cations or with basic polar molecules to exchange or to intercalate them. These chemical reactions are normally followed by an expansion of the interlamellar space, proportional to the amount intercalated, reflecting in ion radii or organic molecule size lengths used in ion-exchange or insertion processes, respectively. The effectiveness of the exchange increased when the original matrix has the proton of OH group previously ion-exchanged by an alkaline or an alkylammonium cations. Monoalkyl-, dialkyl- and heterocyclic amines are focused in this revision as clear and elucidative examples of acid-base interactive processes, that come out inside of the well-formed infinite sequence of inorganic lamellar structure.

Determinação de bromato em melhoradores de farinha por cromatografia de troca iônica com detecção espectrofotométrica

KBrO3 is registered by the FAO/OMS as a genotoxic and carcinogenic compound. In spite of this, KBrO3 is still employed by Brazilian bakeries. Nowadays ion exchange chromatography (IEC) is the most rapid and trustful method for BrO3- analysis. When at high concentrations, chloride ions can interfere in the BrO3- analysis, if the detection is performed by electrical conductivity. On the other hand, spectrophotometric detection, presented here is based on the absorption of BrO3- in the ultraviolet region (210 - 230 nm) where the absortion of chloride ions is very low, thus making possible the qualitative and quantitative analysis of BrO3- in flour improver samples.

Cromatografia de troca-iônica aplicada ao isolamento da fração ácida do óleo de copaíba (Copaifera multijuga) e da sacaca (Croton cajucara)

Plant extracts are usually complex mixtures which contain several molecules of different sizes with varied functional groups. Such extracts are a challenge to the chemist of natural products. Ion exchange chromatography in non-aqueous medium, used for separation of basic or acidic fractions from plant extracts, is an important unit operation in preparative scale separations. Anionic macroporous resin in non-aqueous medium was used with success in this study for separation of the acid fraction of Copaifera multijuga (Copaiba oil), rich in labdanic diterpenes and for the methanolic extract of Croton cajucara (acetyl aleuritoric acid).

Aspectos estruturais relacionados ao processo de troca iônica no niobato lamelar K4Nb6O17

The niobate with formula K4Nb6O17 has a layered structure formed by stacked negative sheets and exchangeable cations in the interlayer region. In this study we discuss some structural aspects related to the ion exchange in layered hexaniobate based on X-ray diffractometry and vibrational Raman spectroscopy data. Hexaniobate has two distinct interlayer regions and the potassium ions of one interlayer in particular are preferably exchanged by other cations, leading to an interstratified material.

Sinterabilidade de pós de precursor vitrocerâmico do sistema LZSA tratados por troca iônica

Ion exchange method was employed by means of surface modification of the glass powders of LZSA (Li2O-ZrO2-SiO2-Al2O3) system submitted to a 70wt% NaNO3/30wt% NaSO4 bath salt followed by a heat treatment. Chemical analysis by X-ray fluorescence was used to evaluate the efficiency of ion exchange, while optical dilatometry was employed to evaluate sintering of compacts. Evaluation of the structure of sintered bodies was made by scanning electron microscopy. Substitution of Li+ ions by Na+ ions on the surface of powders during heat treatments of 450 and 600 ºC for 2-10 h promoted an increase in densification of the sintered bodies.

Remoção de íons metálicos de soluções aquosas, por apatitas sintéticas, usando o método de troca iônica em coluna

Foi investigada a remoção dos íons Al3+, Mn2+, Cu2+, Zn2+, Cd2+ and Pb2 +, em solução aquosa, por apatitas sintéticas usando o método de coluna. Sob as mesmas condições, hidroxiapatitas foram mais seletivas para a remoção de cátions que carboapatitas. Usando hidroxiapatita, a capacidades de troca aumentaram na seguinte ordem: Mn2+ < Zn2+ < Cu2+ < Cd2+ < Al3+ < Pb2+. A seqüência acima é similar a obtida em trabalhos prévios, usando o método de batelada. Análises de DRX e IV indicaram a formação de uma fase única atribuída a uma Pb-apatita.