The present paper describes an interaction study of phenol, o-cresol, and p-cresol with a rich-clay soil sample (clay content of 62.3%). Experiments performed using long contact times, in concentrations of 50.0 mg L(-1) showed practically no signal of phenol, o-cresol, and p-cresol after 48, 72, and 120 h, respectively, suggesting a sorption process. Sorption experiments in the period of 24 h were carried out with the phenolic compounds in concentrations between 5.00 and 500.0 mg L(-1), and negligible interaction between the phenolic species and the soil was observed. Additional experiments were carried out using HgCl(2) or NaN(3) solution as biodegradation inhibitors. After 10 days of contact time in the presence of inhibitors, no alterations in the concentrations of the three compounds studied were observed, and the results suggest no sorption process, with the compounds being almost entirely biodegraded by the soil sample, or possibly the formation of nonextractable residues could occur.
This work proposes a liquid-phase microextraction (LPME) method to extract the highly polar compounds phenol (Ph), o-cresol (o-Cr), m-cresol (m-Cr), p-cresol (p-Cr), and 2,4-dimethylphenol (2,4-DMP) from aqueous matrices. The first extraction step of the LPME method employed a common volumetric flask and n-octanol, and the second extraction step used NaOH as the acceptor phase. The optimized extraction conditions were 900 μL of n-octanol as the extraction solvent, NaOH at 0.60 mol L(-1) as the acceptor phase, an extraction time of 5.0 min, HCl at 0.01 mol L(-1) and NaCl at 20.0% as the donor phase, and an extraction temperature of 20.0°C. The analysis of 50.0 mL of aqueous sample, pretreated under the optimized LPME conditions, afforded a limit of detection (LOD) between 0.3 and 3.5 μg L(-1), a limit of quantification (LOQ) between 1.2 and 11.6 μg L(-1), and a linear range from 2.50 to 50.0 μg L(-1) for Ph, o-Cr, m-Cr and p-Cr and from 12.5 to 250 μg L(-1) for 2,4-DMP. The proposed LPME method was a successful sample preparation strategy, and allowed for precise and accurate quantification of polar phenolic compounds in aqueous matrices such as tap water, river water, groundwater, and seawater, and also in a soil extract. The recovery values ranged from 72.5% to 126.0%, and the relative standard deviation was between 0.3 and 11.5%.
Neste trabalho, propõe-se a determinação de fenol e o-cresol por análise por injeção em fluxo (FIA) com detecção espectrofotométrica, utilizando a reação com 4-aminoantipirina, a fim de quantificar essas espécies em extratos de solo. Após otimização das condições por planejamento fatorial, constatou-se uma maior frequência de amostragem em comparação com o método convencional, bem como valores de recuperação, limites de detecção e de quantificação comparáveis para ambos os métodos. Tais aspectos sugerem que esse método pode ser uma alternativa viável para a determinação de compostos fenólicos em extratos de solos. Phenol and o-cresol determination by flow injection analysis (FIA) with spectrophotometric detection, employing the 4-aminoantipyrine reaction, is proposed in this work in order to quantify these species in soil extracts. The method was improved by a factorial planning, being verified a higher sampling rate in comparison with the conventional method, and recovery values, limits of detection and quantification similar for both methods. These aspects suggest this method as a feasible alternative for phenolic compound determinations in soil extracts.
O objetivo deste estudo foi o de monitorar o nível de poluição de sedimentos subaquáticos de florestas de mangue utilizando espectroscopias de ressonância paramagnética eletrônica (EPR) e de infravermelho próximo (NIR) e análises químicas. A espectroscopia de EPR foi útil para determinar a presença de radicais livres orgânicos de semiquinonas, bem como, fornecer informações sobre a presença de ferro trivalente em domínios diluídos e concentrados nos espectros das amostras. Concluiu-se que, o uso de EPR e NIR, no intervalo espectral adequado, tornou possível avaliar, de forma não destrutiva, o nível de poluição ambiental em sedimentos subaquáticos costeiros de florestas de mangue. Assim, em um período relativamente curto e imprescindível, as autoridades podem tomar as decisões necessárias a fim de evitar danos ambientais.The objective of this study was the monitoring of the pollution level of underwater mangrove sediments using electron paramagnetic resonance (EPR), near-infrared (NIR) spectroscopy and chemical analyses. EPR spectroscopy was useful to determine the presence of organic free radical semiquinone, as well as, to provide information about the presence of trivalent iron in diluted and concentrated or clustered dominion in the sediment samples spectra. It was concluded that by using EPR and NIR spectroscopy measurement, in the appropriate spectral range, it was possible to nondestructively assess the environmental pollution level of coastline underwater mangrove sediments. Though, in a relatively small period of time, the authorities can take the necessary decisions to avoid environmental damages.
Análises por espectroscopias de ressonância paramagnética eletrônica (EPR) e de ultravioleta-visível por refletância difusa (DRUV-VIS) de solos intensamente intemperizados contendo altos níveis de óxidos-hidróxidos de ferro, a partir de um projeto-piloto de agricultura de precisão, incluindo 13 fazendas no sudoeste do estado do Paraná, Brasil, foram realizadas, visando definir parâmetros de fertilidade dos solos. Os resultados dos estudos espectroscópicos no laboratório foram comparados com aqueles obtidos através da utilização de um espectrorradiômetro portátil, em condições de campo. Os solos estudados apresentaram como constituintes inorgânicos, principalmente minerais de argila 1:1, óxidos e hidróxidos de ferro (principalmente goetita e hematita) e de alumínio (principalmente gibbsita), características de solos altamente intemperizados, como por exemplo, Latossolos. Os espectros de EPR, típicos de agregados de íons Fe 3+ com interação magnética, apresentaram aumento na largura da linha do sinal em g ca. 2 quando obtidos em temperatura de nitrogênio líquido, em comparação com os obtidos a temperatura ambiente. Este fenômeno pode ter sido causado por mudanças no ambiente do campo cristalino dos íons Fe 3+ ou pelo mecanismo de relaxação spin-spin, o que provoca aumento da largura de linha quando a temperatura diminui. As curvas espectrais eletrônicas obtidas com o espectrorradiômetro portátil apresentaram-se menos detalhadas, porém mais específicas de cada amostra de solo analisada. Os resultados indicam que o uso do espectrorradiômetro portátil juntamente com ferramentas matemáticas, como a segunda derivada da função Kubelka-Munk, é uma boa alternativa para analisar solos argilosos ricos em óxidos-hidróxidos metálicos. Foram feitas atribuições das absorções espectrais, principalmente para as transições eletrônicas d-d entre níveis de energia de pares de íons Fe Electron paramagnetic resonance (EPR) spectroscopy and optical analyses of intensively weathered soils containing high levels of oxide-hydroxide of iron from a pilot project on precision agriculture, including 13 farms in the southwest of Paraná state, Brazil, were carried out, aiming at defining parameters of soil fertility. The results of the optical studies in the laboratory were compared with those obtained by the use of a portable spectroradiometer in field conditions. The studied soils were mainly composed of 1:1 clay minerals, oxides and oxide hydroxides of iron (mainly goethite and hematite) and aluminum (mainly gibbsite), characteristics of highly weathered soils, as for example Ferralsols. The EPR spectra, typical of mutual magnetic interaction of aggregated Fe 3+ ions, showed a signal linewidth increase at g ca. 2 upon cooling. This phenomenon can be caused by changing the crystal field environment of Fe 3+ ions or by the spin-spin relaxation mechanism, which causes an increase of linewith when the temperature decreases. The optical spectral curves obtained from the portable spectroradiometer presented less detailed but more specific features...
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