Navegação por Autores IPEN "GUILHEN, S.N."

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  • IPEN-DOC 25513

    GUILHEN, S.N. ; ORTIZ, N. ; IZIDORO, J.C. ; FUNGARO, D.A. . Activation of biochar obtained from slow pyrolysis of the macauba coconut residue for removing uranium from aqueous solutions. In: BIOCHAR, August 20-23, 2018, Wilmington, Delaware, USA. Abstract... 2018.

    Abstract: Macauba (Acrocomiaaculeata) is a palm tree native to the savannah-like area of Central Brazil. As a result of the oil extraction from its coconuts, a dark stiff residue, the “endocarp”, rich in lignin content, has a potential for being exploited as feedstock for biochar production. This study investigates the activation of biochar obtained from slow pyrolysis of the macauba coconut residue in order to remove uranium from aqueous solutions. The non-activated biochar, referred to as “BC350”, is produced at a pyrolytic temperature of 350°C under Ar atmosphere and a 1- hour residence time. The activated biochar was produced the same way and was further subjected to activation via physical route using CO2 at 850°C for 120 min. The product of this treatment was named “BC350-A”. Both biochars were characterized by specific surface area. The surface area increased from 0.832 (untreated biochar) to 643.12 m2 g-1, confirming the improvement of the porosity. The removal efficiency for uranyl ions (U(VI)) increased from 80.5 (untreated biochar) to 99.2% for 5 mg L-1 initial concentration solution adjusted to pH 3 using a 10 g L-1dosage. Adsorption isotherms were employed to represent the results of the U adsorption onto the BC350-A. An estimation of the best fit was performed by calculating different deviation equations, also called error functions. The Redlich-Peterson isotherm model was the most appropriate for fitting the experimental data. This hybrid model incorporates both Langmuir and Freundlich’s isotherm functionalities. These results demonstrate that a valueadded material can be produced, encouraging the exploration of thermochemical conversion of lignocellulosic biomasses.

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  • IPEN-DOC 25737

    SCAPIN, M.A. ; GUILHEN, S.N. ; AZEVEDO, L.C. ; COTRIN, M.E.B. ; PIRES, M.A.F. . Application of bias correction methods to improve U3Si2 sample preparation for quantitative analysis by WDXRF. Brazilian Journal of Radiation Sciences, v. 7, n. 2A, p. 1-9, 2019. DOI: 10.15392/bjrs.v7i2A.582

    Abstract: The determination of silicon (Si), total uranium (U) and impurities in uranium-silicide (U3Si2) samples by wavelength dispersion X-ray fluorescence technique (WDXRF) has been already validated and is currently implemented at IPEN’s X-Ray Fluorescence Laboratory (IPEN-CNEN/SP) in São Paulo, Brazil. Sample preparation requires the use of approx-imately 3 g of H3BO3 as sample holder and 1.8 g of U3Si2. However, because boron is a neutron absorber, this proce-dure precludes the recovery of U3Si2 from the samples, preventing its use as nuclear fuel. Consequently, a significant amount of uranium is wasted in this process. An estimated average of 15 samples per month is expected to be analyzed by WDXRF, resulting in approx. 320 g of U3Si2 that wouldn’t return to the nuclear fuel cycle. The purpose of this paper is to present a new preparation method, replacing H3BO3 by cellulose acetate {[C6H7O2(OH)3-m(OOCCH3)m], m = 0~3}, thus enabling the recovery of the boron-free U3Si2 from the samples. The results demonstrate that the suggested sample preparation approach is statistically satisfactory, allowing the optimization of the procedure.

    Palavras-Chave: quantitative chemical analysis; sample preparation; uranium silicides; x-ray fluorescence analysis; boron 10; boric acid; acetates; corrections; errors; impurities; mathematical models; optimization

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  • IPEN-DOC 27907

    MACHADO, G.G.; KRUPSKAYA, V.V.; ZAKUSIN, S.V.; HARADA, J.; VICENTE, R. ; SOUZA, R.P.; ARAUJO, L.G. ; MONTALVAN, E.T.; ESPINOSA, D.C.R.; KAHN, H.; GUILHEN, S.N. . Brazilian clays for environmental solutions applied to radioactive waste management. Brazilian Journal of Radiation Sciences, v. 9, n. 1A, p. 1-14, 2021. DOI: 10.15392/bjrs.v9i1A.1539

    Abstract: Clayey materials have been adopted in most nuclear waste producing countries as a key constituent in engineered barrier systems for final disposal facilities at all levels of radioactive wastes (LILW-SL, LILW-LL, and HLW). The following study presents a thorough characterization upon five Brazilian clay-rich deposits, mostly smectite bearing clays, aiming to evaluate their expected performance as barrier under the conditions associated to a Low and Intermediate Level Waste Repository; being the former a matter of national strategic interest. Samples coming from the Brazilian states of Paraná, Bahia, Paraíba, and Maranhão were treated and analyzed by means of X-Ray diffraction as main technique. Other techniques such as FTIR, LALLS, XRF, and SEM-EDS, were performed in order to establish the mineralogical composition, particle size distribution, and chemical composition. Moreover, several standard clay treatments over the <1 μm size fraction were carried out to reveal information regarding layer charge, major interlayer cations, unit formula and other crystal features of smectite species present in a mineralogical assembly, aiming to provide information for the construction of a molecular model over which would be realistic to simulate the diffusion of radionuclides. Results obtained on 133Cs adsorption experiments indicate that mineralogical composition would probably be the single most influential factor controlling transport capacity of positively charged radionuclides in the current setup. The composition is especially expressed in terms of smectite contents, favoring montmorillonite rich materials containing majorly Na+ as compensating cation in interlayer position. All tested samples can be considered as suitable candidates to be used in the design of final destination storage for nuclear waste. Thus, efficiency on 133Cs adsorption trials also indicate that these materials could have potential uses as sorptive matrices (Sorbents) for water treatment of radionuclide polluted waters such as TENORM waste waters. However, these trends are yet to be contrasted against hydraulic conductivity measurements and swelling pressure in order to have a more comprehensive perspective of this clayey prospects as barrier enhanced layer; aligned to the multilayer barrier system approach for nuclear waste management.

    Palavras-Chave: radioactive waste storage; fourier transformation; infrared spectra; cesium 133; clays

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  • IPEN-DOC 27851

    GUILHEN, S.N. ; SOUZA, A.L.; COTRIM, M.E.B. ; PIRES, M.A.F. . Direct determination of aluminum in low-enriched UAlx targets (UAlx-Al) by ICP OES. Brazilian Journal of Radiation Sciences, v. 9, n. 1A, p. 1-18, 2021. DOI: 10.15392/bjrs.v9i1A.1247

    Abstract: The production of molybdenum-99 (99Mo) using low-enriched uranium targets (< 20% 235U) dispersed in aluminum (UAlx) is a very promising strategy towards the independence in 99Mo local production. A thorough control must be performed to ensure that these targets meet the regulatory requirements to achieve the expected efficiency in the reactor. The determination of the targets’ composition is of high interest, because the distribution of Al in different phases may have an impact on the U concentration. Among the techniques used for this purpose, inductively coupled plasma optical emission spectrometry (ICP OES) stands out because of its high sensitivity and precision, allowing for simultaneous determination of several elements in a variety of samples and matrices. However, because U exhibits a complex emission spectrum, spectral interferences are prone to affect the analysis of Al, calling for time consuming preparation steps to remove the U from the matrix. This study proposes a method of direct determination of Al in UAlx targets through the selection of specific emission lines enabled by the evaluation of the associated interferences on the recovery values.

    Palavras-Chave: aluminium; chemical analysis; emission spectroscopy; molybdenum 99; plasma; technetium 99; uranium 235 target

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  • IPEN-DOC 29694

    SILVESTRIN, G.A. ; GONCALVES, M.H. ; GODOI, C.M. ; MAIA, V.A. ; FERREIRA, J.C. ; GUILHEN, S.N. ; NETO, A.O. ; SOUZA, R.F.B. de . Effective phosphate removal from water by electrochemically mediated precipitation with coffee grounds biocarbon obtained by non-thermal plasma method. The Academic Society Journal, v. 7, n. 1, p. 3-12, 2023. DOI: 10.32640/tasj.2023.1.3

    Abstract: This study investigates the use of biocarbon electrodes, produced from coffee grounds through plasma pyrolysis, in the electrochemically mediated precipitation process for phosphorus removal in a flow reactor. The structural and electrochemical properties of biocarbon were analyzed using X-ray powder diffraction (XRD), Raman spectroscopy, and cyclic voltammetry. The results show that biocarbon consists of both graphene oxide and lignocellulose with surface OH groups that facilitate the breakdown of water, a key step in the electrochemically mediated precipitation process for phosphorus removal. The addition of graphite to the biocarbon paste was found to be necessary to obtain a response from the biocarbon in cyclic voltammetry. The Gr75BC25 electrode achieved higher phosphorus removal rates than other tested electrodes, particularly at low flows, due to the functional groups present in biocarbon enhancing the breakdown of water. However, electrodes with a greater amount of biocarbon exhibit lower rates of phosphorus removal and higher consumption of electrical power, which can be attributed to their higher electrical resistivity. Thus, to optimize its use, it is important to balance the benefits of increased phosphorus removal rates with the trade-off of increased energy consumption and decreased phosphorus removal at higher levels of biocarbon. The results suggest that biocarbon produced from coffee grounds by plasma pyrolysis has the potential to be used as an effective electrode material for electrochemically mediated precipitation processes.

    Palavras-Chave: electrochemistry; synthesis; phosphates; removal; carbon; water treatment

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  • IPEN-DOC 25784

    GUILHEN, S.N. ; COLETI, J.; TENORIO, J.A.S.; FUNGARO, D.A. . Influence of adsorption parameters on uranium adsorption capability by biochar derived from macauba coconut residue. Brazilian Journal of Radiation Sciences, v. 7, n. 2A, p. 1-14, 2019. DOI: 10.15392/bjrs.v7i2A.590

    Abstract: Biochar (BC) is a carbon-rich product obtained when biomass is thermally decomposed at relatively low temperatures (under 700ºC) and limited supply of oxygen in a process called pyrolysis. Because of its porous structure, charged sur-face and surface functional groups, BC exhibits a great potential as an adsorbent. Its characteristics strongly depend on the feedstock and the pyrolysis conditions. The aim of this study was to evaluate the adsorption potential for the remov-al of uranium, U(VI) from aqueous solutions using BC obtained through slow pyrolysis of the macauba coconut endo-carp. The influence of parameters such as pH, sorbent dose and initial concentration on the adsorption of U(VI) was investigated. The BC obtained at 350 °C (BC350) presented a removal percentage of approx. 80 %, demonstrating its applicability for the treatment of uranium contaminated aqueous solutions.

    Palavras-Chave: adsorption; uranium; chars; biological materials; concentration ratio; coconut palms; temperature dependence; waste water; pyrolysis; ph value

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  • IPEN-DOC 24621

    GUILHEN, S.N. ; COLETI, J.; TENARIO, J.A.S.; FUNGARO, D.A. . Influence of pyrolytic temperature on uranium adsorption capability by biochar derived from macauba coconut residue. In: 60 YEARS OF IEA-R1: INTERNATIONAL WORKSHOP ON UTILIZATION OF RESEARCH REACTORS, November 28 - December 01, 2017, São Paulo, SP. Abstract... São Paulo, SP: Instituto de Pesquisas Energéticas e Nucleares, 2017. p. 97-98.

    Abstract: Biochar (BC) is a carbon-rich product obtained when biomass is thermally decomposed at relatively low temperatures (under 700 C) and limited supply of oxygen in a process called pyrolysis. The conversion of biomass into BC can not only result in renewable energy source of synthetic gas and bio-oil, but also decrease the content of CO2 in the atmosphere, as well as improving soil fertility. Because of its porous structure, charged surface and surface functional groups, BC exhibits a great potential as an adsorbent. Brazilian agro energy chain involves tons of biomass waste, providing a wide range of biomasses with different chemical and physical properties. BC characteristics strongly depend on the feedstock and the pyrolysis conditions, in which the temperature is the key parameter. The aim of this study was to evaluate the adsorption potential for the removal of uranium, U(VI), from aqueous solutions using BC obtained through the pyrolysis of the macauba (Acrocomia aculeata) coconut endocarp as a function of the final pyrolytic temperature. BCs produced at higher temperatures are likely to present lower H/C and O/C ratios, indicating the loss of easily degradable carbon compounds such as volatile matter. In contrast, low-temperature pyrolysis produces not only a higher BC yield, but also richer in surface functional groups which will likely enable interactions with the U(VI) ions. The endocarp was subjected to six different pyrolytic temperatures, ranging from 250 C to 750 C. The influence of parameters such as pH, sorbent dose and initial concentration on the adsorption of U(VI) was investigated. The maximum adsorption capacity (q) was achieved for the BC obtained at 250 C (BC250), which presented a removal percentage of approx. 86%, demonstrating the potential of the BC from macauba endocarp for treatment of wastewaters. Thus, submitting the endocarp to temperatures higher than 250 C becomes unnecessary, saving time and reducing operating costs.

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  • IPEN-DOC 24945

    GUILHEN, S.N. ; PITOL-FILHO, L.; FUNGARO, D.A. . Kinetic study of uranium removal from aqueous solutions by macauba biochar. In: ENCONTRO BRASILEIRO SOBRE ADSORCAO, 12., 23-25 de abril, 2018, Gramado, RS. Anais... 2018.

    Abstract: Macauba (Acronomia aculeata) is a palm tree native of the Brazilian “cerrado” and a valuable renewable source of vegetable oil for human consumption and biodiesel production. Residue from the extraction of the coconut oil, the shell, or endocarp, can be used as a raw material for the production of biochar (BC) aiming the removal of uranium from aqueous solutions. Biochars are obtained by thermal decomposition of the biomass under inert atmosphere (pyrolysis) and, because of their surface properties and porous structure, they exhibit great potential as adsorbents. Adsorption of U(VI) was studied by a batch technique using a biochar produced through slow pyrolysis at 350°C of the macauba endocarp. The effect of contact time was investigated and a kinetic study was conducted to determine the mathematical model that best describes the adsorption process. The adsorption capacity (qmax) obtained for BC350 was 405 mg g-1.

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  • IPEN-DOC 24803

    ULRICH, J.C. ; GUILHEN, S.N. ; COTRIM, M.E.B. ; PIRES, M.A.F. . Method development and validation for simultaneous determination of IEA-R1 reactor’s pool water uranium and silicon content by ICP OES. Journal of Physics: Conference Series, v. 975, n. 012012, p. 1-5, 2018. DOI: 10.1088/1742-6596/975/1/012012

    Abstract: IPEN’s research reactor, IEA-R1, an open pool type research reactor moderated and cooled by light water. High quality water is a key factor in preventing the corrosion of the spent fuel stored in the pool. Leaching of radionuclides from the corroded fuel cladding may be prevented by an efficient water treatment and purification system. However, as a safety management policy, IPEN has adopted a water chemistry control which periodically monitors the levels of uranium (U) and silicon (Si) in the pool’s reactor, since IEA-R1 employs U3Si2-Al dispersion fuel. An analytical method was developed and validated for the determination of uranium and silicon by ICP OES. This work describes the validation process, in a context of quality assurance, including the parameters selectivity, linearity, quantification limit, precision and recovery.

    Palavras-Chave: validation; pool type reactors; uranium; silicon; emission spectroscopy; optical systems; plasma

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  • IPEN-DOC 25816

    GUILHEN, S.N. ; MASEK, O.; ORTIZ, N. ; IZIDORO, J.C. ; FUNGARO, D.A. . Pyrolytic temperature evaluation of macauba biochar for uranium adsorption from aqueous solutions. Biomass and Bioenergy, v. 122, p. 381-390, 2019. DOI: 10.1016/j.biombioe.2019.01.008

    Abstract: This study aims to evaluate the effect of the pyrolytic temperature on the biochar derived from the macauba endocarp for the removal of uranium (VI) from aqueous solutions. The endocarp was subjected to six different pyrolytic temperatures, ranging from 250 °C to 750 °C. The biochars obtained at each temperature were evaluated for their adsorption capacities (“q”). The highest adsorption capacities were obtained for the biochar produced at 250 °C (BC250), followed by the one obtained at 350 °C (BC350), with removal efficiencies of 86% and 80%, respectively. The best condition was achieved when the endocarp was subjected to temperatures between 300 and 350 °C, at which it was possible to obtain a satisfactory balance among adsorption capacity, gravimetric yield and fixed carbon content. This characteristic, combined with the high removal efficiency, points to an ideal working temperature of 350 °C. Elemental analysis showed a decrease of the H/C and O/C ratios when higher pyrolytic temperatures were applied, indicating an inverse relationship between the carbonization and the surface polar functional groups, which were likely responsible for an increased adsorptive capacity in biochars produced at lower temperatures. Both FTIR and XPS analysis indicated that oxygen-containing groups such as hydroxyls and carboxylic acids were involved with the binding of uranyl ions.

    Palavras-Chave: biomass; carbon; pyrolysis; pyrolytic carbon; temperature dependence; radioactive wastes; uranium; adsorption; coconut palms

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  • IPEN-DOC 24998

    SILVA, K.C. ; GUILHEN, S.N. ; IZIDORO, J.C. ; FUNGARO, D.A. . Removal of cadmium and zinc from aqueous solutions using zeolite synthesized from coal fly ash and industrial aluminium waste. In: ENCONTRO BRASILEIRO SOBRE ADSORCAO, 12., 23-25 de abril, 2018, Gramado, RS. Anais... 2018.

    Abstract: Coal fly ash can be used as a source of Silicon and Aluminum for 4A zeolite synthesis. It is necessary to consider the adequate proportion of Si / Al for the synthesis, so the aluminum waste from tertiary industry was used as an alternative and sustainable aluminum source. The synthesis was carried out by alkaline fusion followed by the hydrothermal treatment obtaining sodium aluminosilicate, which was then crystallized in NaOH solution. The samples were characterized by XRF, XRD and cation exchange capacity. The zeolite produced has the capacity to adsorb the Cd (II) and Zn (II) ions from aqueous solutions. The maximum adsorption capacity was 78.0 and 35.8 mg.g-1 for the Cd and Zn, respectively. The results showed that the aluminum waste and the fly ash together can be transformed into zeolite A, considered as value-added material and with promising adsorption properties.

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  • IPEN-DOC 23916

    REIS, A.S. ; GUILHEN, S.N. ; ORTIZ, N. . Water treatment adsorption and UV photodecomposition processes for antibiotics: Cephalexin and Amoxicillin. In: IWA LEADING EDGE CONFERENCE ON WATER AND WASTEWATER TECHNOLOGIES, 13th, June 13-16, 2016, Jerez de la Frontera, Spain. Resumo expandido... 2016.

    Abstract: The developed of water treatment process to adsorb and decompose the pharmaceutical antibiotic amoxicillin and cephalexin using iron oxide –hematite, quitosan and UV radiation. The equilibrium time te= 180 min and the removal percentage for amoxicillin was 90% similar with those found in literature. In same experimental parameters the Cephalexin removal percentage was 25% some parameter have been alter to promote the photodecomposition such antibiotic mixture. The results confirm an indicate the possible use of UV photodecomposition reaction as a promising water treatment to treat, adsorb and decompose antibiotic residues in the environment.

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A elaboração do projeto do RI do IPEN foi iniciado em novembro de 2013, colocado em operação interna em julho de 2014 e disponibilizado na Internet em junho de 2015. Utiliza o software livre Dspace, desenvolvido pelo Massachusetts Institute of Technology (MIT). Para descrição dos metadados adota o padrão Dublin Core. É compatível com o Protocolo de Arquivos Abertos (OAI) permitindo interoperabilidade com repositórios de âmbito nacional e internacional.

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A elaboração do projeto do RI do IPEN foi iniciado em novembro de 2013, colocado em operação interna em julho de 2014 e disponibilizado na Internet em junho de 2015. Utiliza o software livre Dspace, desenvolvido pelo Massachusetts Institute of Technology (MIT). Para descrição dos metadados adota o padrão Dublin Core. É compatível com o Protocolo de Arquivos Abertos (OAI) permitindo interoperabilidade com repositórios de âmbito nacional e internacional.

O gerenciamento do Repositório está a cargo da Biblioteca do IPEN. Constam neste RI, até o presente momento 20.950 itens que tanto podem ser artigos de periódicos ou de eventos nacionais e internacionais, dissertações e teses, livros, capítulo de livros e relatórios técnicos. Para participar do RI-IPEN é necessário que pelo menos um dos autores tenha vínculo acadêmico ou funcional com o Instituto. Nesta primeira etapa de funcionamento do RI, a coleta das publicações é realizada periodicamente pela equipe da Biblioteca do IPEN, extraindo os dados das bases internacionais tais como a Web of Science, Scopus, INIS, SciElo além de verificar o Currículo Lattes. O RI-IPEN apresenta também um aspecto inovador no seu funcionamento. Por meio de metadados específicos ele está vinculado ao sistema de gerenciamento das atividades do Plano Diretor anual do IPEN (SIGEPI). Com o objetivo de fornecer dados numéricos para a elaboração dos indicadores da Produção Cientifica Institucional, disponibiliza uma tabela estatística registrando em tempo real a inserção de novos itens. Foi criado um metadado que contém um número único para cada integrante da comunidade científica do IPEN. Esse metadado se transformou em um filtro que ao ser acionado apresenta todos os trabalhos de um determinado autor independente das variáveis na forma de citação do seu nome.