Abstract. A method is presented in which gas chromatography coupled with mass spectrometry (GC-MS) allows quantitative simultaneous detection of mixtures of phenol (Ph), 2-chlorophenol (2-CPh), 3-cholorphenol (3-CPh), and 4-cholorophenol (4-CPh) in aqueous mixtures after being adsorbed on silicalita-1, utilizing selected-ion monitoring (SIM) and full-scan modes mass selective detection. GC-MS with SIM at m/z = 64 and m/z = 128 showed good detection selectivity for mixtures of Ph, 2-CPh and 3-CPh (M 1), and 2-CPh and 4-CPh (M 2). Silicalita-1 was obtained from an amorphous organo-alumino-silicic gel from rice husk, an abundant and low cost agricultural waste residue that is readily available in large quantities. This product was used as a sorbent for solid phase extraction of organic analytes from aqueous solutions. The adsorption of the three chlorophenol isomers, ortho-, meta-, and para-, by silicalite-1 has been studied independently, showing that meta- and para-chlorophenol isomer
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