Dtermination of Aromatic Sufactant Residues in Sediments using Accelerated Solvent Extraction and On-line Derivatization GC/MS

• Main Authors: John, Chih-Hau Fan, 范志豪
• Other Authors: Wang-Hsien Ding
• Format: Others
• Language: zh-TW
• Published: 1999
• Online Access: http://ndltd.ncl.edu.tw/handle/22908658934746495344

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 100C 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.