請用此 Handle URI 來引用此文件: http://hdl.handle.net/11455/35088
標題: Application of microwave-assisted desorption/headspace solid-phase microextraction as pretreatment step in the gas chromatographic determination of 1-naphthylamine in silica gel adsorbent
作者: Yan, C.T.
鄭政峰
Jen, J.F.
Shih, T.S.
關鍵字: 1-naphthylamine
microwave-assisted desorption
headspace SPME
silica
gel
workplace monitoring
electron-capture detection
trap mass-spectrometry
aromatic-amines
azo
dyes
gc-ms
extraction
water
derivatization
chlorophenols
aniline
期刊/報告no:: Talanta, Volume 71, Issue 5, Page(s) 1993-1997.
摘要: Pretreatment of silica gel sample containing 1-naphthylamine by microwave-assisted desorption (MAD) coupled to in situ headspace solid phase microextraction (HS-SPME) has been investigated as a possible alternative to conventional methods prior to gas chromatographic (GC) analysis. The 1-naphthylamine desorbs from silica gel to headspace under microwave irradiation, and directly absorbs onto a SPME fiber located in a controlled-temperature headspace area. After being collected on the SPME fiber, and desorbed in the GC injection port, 1-naphthylamine is analyzed by GC-FID. Parameters that influence the extraction efficiency of the MAD/HS-SPME, such as the extraction media and its pH, the microwave irradiation power and irradiation time as well as desorption conditions of the GC injector, have been investigated. Experimental results indicate that the extraction of a 150 mg silica gel sample by using 0.8 ml of 1.0 M NaOH solution and a PDMS/DVB fiber under high-powered irradiation (477 W) for 5 min maximizes the extraction efficiency. Desorption of I-naphthylamine from the SPME fiber in GC injector is optimal at 250 degrees C held for 3 min. The detection limit of method is 8.30 ng. The detected quantity of I-naphthylamine obtained by the proposed method is 33.3 times of that obtained by the conventional solvent extraction method for the silica gel sample containing 100 ng of 1-naphthylamine. It provides a simple, fast, sensitive and organic-solvent-free pretreatment procedure prior to the analysis of 1-naphthylamine collected on a silica gel adsorbent. (c) 2006 Elsevier B.V. All rights reserved.
URI: http://hdl.handle.net/11455/35088
ISSN: 0039-9140
文章連結: http://dx.doi.org/10.1016/j.talanta.2006.09.005
顯示於類別:化學系所

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