Efficiency of supercritical fluid extraction for determining 4-nonylphenol in municipal sewage sludge

When the sewage sludge containing the persistent, lipophilic, metabolite 4-nonylphenol (4-NP) has been disposed of in the environment it's toxic nature can lead to serious health risks to human beings and can also affect plants and aquatic organisms. Supercritical fluid extraction (SFE) is a new and powerful technique for extracting the organic contaminants from the solid phase. The present study was conducted to investigate optimal conditions for the quantitative extraction of 4-NP by SFE and to determine the concentration of 4-NP in municipal sewage sludge. The effect of several parameters such as temperature, pressure, static extraction time, dynamic extraction time, CO₂ flow-rate, sample mass and modifier on the extraction were investigated. The optimal conditions for the extraction of the spiked sample were fluid pressure 97 bar, temperature 40°C, flow-rate 3.0 ml/min, static extraction time 2 min, dynamic extraction time 5 min and modifier methanol (0.5 ml). Extracts were analyzed by gas chromatography-mass spectrometry. Concentration of 4-NP in the anaerobically degraded sludge of the De-Haw Sewage Treatment Plant in Taiwan was found to be 243.9 mg/kg. The extraction efficiency of the SFE method was compared with the conventional Soxhlet extraction method. The overall recovery of the SFE method was found to be greater and the results indicate that SFE is an efficient method for extracting 4-NP from sewage sludge. Copyright (C) 1999 Elsevier Science B.V.