RESUMEN
An existing laboratory procedure for selenium analysis using open-vessel wet digestion and liquid chromatographic fluorescence determination was modified for use with microwave digestion. The proposed microwave digestion method eliminated the hazards associated with the use of HClO4 while maintaining excellent recoveries of selenium. A 2-step HNO3/H2O2 digestion procedure was developed. Digested samples were derivatized with 2,3-diaminonaphthalene, and the resultant piazselenol complex was measured fluorometrically using a liquid chromatograph. Measured values were in agreement with 9 different certified reference materials. The detection limit for this method was 0.54 ng Se/g tissue (3 sigma), and the calibration curve remained linear (r2 = 0.9968) up to 2 microg Se/g.
Asunto(s)
Química Orgánica/métodos , Cromatografía Liquida/métodos , Microondas , Selenio/análisis , 2-Naftilamina/análogos & derivados , 2-Naftilamina/análisis , Azoles/análisis , Azoles/química , Calibración , Productos Pesqueros/análisis , Análisis de los Alimentos/métodos , Concentración de Iones de Hidrógeno , Compuestos de Organoselenio/análisis , Compuestos de Organoselenio/química , Reproducibilidad de los Resultados , Sensibilidad y EspecificidadRESUMEN
Some of the most fertile agricultural land in Atlantic Canada includes dykelands, which were developed from rich salt marshes along the Bay of Fundy through the construction of dykes. A 2-yr field experiment was conducted on dykeland soil to evaluate the effect of fertility treatments: source-separated municipal solid waste (SS-MSW) compost, solid manure, commercial fertilizer, and gypsum on (1) timothy/red clover forage productivity, (2) N, S, and other nutrients uptake, and (3) residual NO(3)-N and NH(4)-N in the soil profile. All fertility treatments increased dry matter yields from the two cuts each year relative to the control. Residual soil NO(3)-N and NH(4)-N concentrations in the fall of the second year decreased with depth, and beyond 20-cm depth were lower than 1 mg kg(-1). Gypsum application equivalent to 40 kg S ha(-1) increased dry matter yields and N uptake by forage, and increased soil Mehlich 3-extractable S, tissue S, and uptake of S, Ca, P, Cu, Fe, and Mn relative to the control. High rates of compost can provide sufficient N, S, and perhaps other nutrients to a perennial forage system under the cool wet climate of Atlantic Canada with no heavy metal enrichment of forage. However, the chemical N provided greater total N uptake than organic sources, except the high rate of compost, suggesting that the N availability from organic sources was not well synchronized with forage N demand. Municipal solid waste compost may also increase soil and forage tissue Na, which might be of concern.