RESUMEN
Microwave-enhance catalytic degradation (MECD) of 4-chlorophenol (4-CP) using nickel oxide was studied. A mix-valenced nickel oxide was obtained from nickel nitrate aqueous solution through a precipitation with sodium hydroxide and an oxidation by sodium hypochlorite (assigned as PO). Then, the as-prepared PO was irradiated under microwave irradiation to fabricate a high active mix-valenced nickel oxide (assigned as POM). Further, pure nanosized nickel oxide was obtained from the POM by calcination at 300, 400 and 500 degrees C (labeled as C300, C400 and C500, respectively). They were characterized by X-ray (XRD), infrared spectroscopy (IR) and temperature-programmed reduction (TPR). Their catalytic activities towards the degradation of 4-CP on the efficiency of the degradation were further investigated under continuous bubbling of air through the liquid-phase and quantitative evaluation by high pressure liquid chromatography (HPLC). Also, the effects of temperature, pH and kinds of catalysts on the efficiency of the degradation have been investigated. The results showed that the 4-CP was degraded completely by MECD method within 20 min under pH 7, T=40 degrees C and C=200 g dm(-3) over POM catalyst. The relative activity was affected significantly with the oxidation state of nickel.
Asunto(s)
Clorofenoles/química , Microondas , Níquel/química , Contaminantes Químicos del Agua/química , Catálisis , Concentración de Iones de Hidrógeno , Tamaño de la Partícula , Temperatura , Purificación del Agua/métodosRESUMEN
As part of an evaluation of focused microwave-assisted extraction (FMAE) using an open-vessel system, the effects of matrix, moisture content, ageing, and solvent have been studied on the extraction efficiency of polycyclic aromatic hydrocarbons (PAHs) from spiked soils. PAHs were spiked onto three different uncontaminated air dried and originally wet soil matrices with 1- and 20-day ageing periods. Solvents used were hexane-acetone (1:1), cyclohexane-acetone (1:1) and dichloromethane. FMAE only required a small amount of solvent (20 ml) and short extraction time (10 min) in the open cell under 90 W of microwave power. The results revealed that the extraction efficiency strongly depends on the nature of soil matrix; moisture content may enhance the recoveries of PAHs for many cases; and, the influence of the type of solvent is not significant. A comparison between microwave extraction and 16-h Soxhlet extraction has been made on spiked soils. It evidenced that the microwave method under ambient pressure is a suitable alternative to Soxhlet method for the analysis of PAHs in soils. For the evaluation of the developed FMAE method, three reference materials were used. The PAHs recovered from three reference materials were in a good agreement with reference values.
Asunto(s)
Técnicas de Química Analítica/métodos , Hidrocarburos Policíclicos Aromáticos/aislamiento & purificación , Técnicas de Química Analítica/instrumentación , Microondas , Estándares de Referencia , Reproducibilidad de los Resultados , Suelo/análisis , Contaminantes del Suelo/aislamiento & purificación , Solventes/química , Factores de TiempoRESUMEN
Application of the microwave-enhanced catalytic degradation (MECD) method on the abatement of 4-nitrophenol (4-NP) using nickel oxide was studied. A mix-valenced nickel oxide was prepared from nickel nitrate aqueous solution through a precipitation with sodium hydroxide and an oxidation by sodium hypochlorite with/without microwave-assisted heating. They were characterized by X-ray (XRD), infrared spectroscopy (IR), temperature programmed reduction (TPR), and transmission electron micrographs (TEM). Their catalytic activities towards the degradation of 4-NP were investigated through continuous bubbling of air during the liquid phase and evaluated quantitatively with high pressure liquid chromatography (HPLC). Also, the effect of the kinds of catalyst, temperature, pH, initial concentration, and dosage of catalyst on the efficiency of 4-NP degradation was investigated. The results showed that the 4-NP was completely degraded using the high efficiency MECD method within 15 min under [H(+)] = 1.0M, T = 40 °C, and C = 200 ppm over nickel oxide.