| Summary: | 碩士 === 國立中央大學 === 化學研究所 === 87 === Abstract:
A time and solvent saving method, accelerated solvent extraction (ASE), was developed to extract 4-nonylphenols (4-NP), nonylphenol ethoxy carboxylates (NP1EC) and linear alkylbenzenesulfonates (LAS) in sediment. The effects of various operational parameters (i.e., temperature, pressure, etc.) for the quantitative extraction of 4-NP, NP1EC and LAS by ASE were investigated. The NP1EC and LAS residues were then identified and quantitated by ion-trap GC/MS with ion-pair derivatization in the GC injection-port using a large-volume (10-20 l) direct sample introduction (DSI) device.
The analytes can be completely extracted by methanol at 100C and 100 atm combined with 15 min static and then 20 min dynamic extraction steps with flow-rate 0.5 ml/min. Recovery of 4-NP, NP1EC and LAS in spiked blank kaolin samples were 102%, 96% and 115% with 6%, 3% and 4% RSD, respectively. The degree of recovery of 4-NP in the spiked sediment samples from a reservoir and polluted river were 113% with 3% RSD and 97% with 6% RSD, respectively. For NP1EC, the degree of recovery were 105% with 4% RSD and 96% with 4% RSD, respectively. For LAS, the recovery of was 113% with 3% RSD in reservoir sediment. The ASE method has been tested with spiked and aged samples displaying its perfect applicability for 4-NP, NP1EC and LAS. The extraction efficiency of the ASE was compared with conventional Soxhlet and bath ultrasonication extraction methods using the 4-NP spiked sediment samples.
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