Abstract: Fecal sterol has been proposed as a chemical indicator
of human fecal pollution even when fecal coliform populations have
diminished due to water chlorination or toxic effects of industrial
effluents. This paper describes an improved derivatization procedure
for simultaneous determination of four fecal sterols including
coprostanol, epicholestanol, cholesterol and cholestanol using gas
chromatography-mass spectrometry (GC-MS), via optimization study
on silylation procedures using N-O-bis
(trimethylsilyl)-trifluoroacetamide (BSTFA), and
N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide
(MTBSTFA), which lead to the formation of trimethylsilyl (TMS) and
tert-butyldimethylsilyl (TBS) derivatives, respectively. Two
derivatization processes of injection-port derivatization and water bath
derivatization (60 oC, 1h) were inspected and compared. Furthermore,
the methylation procedure at 25 oC for 2h with
trimethylsilydiazomethane (TMSD) for fecal sterols analysis was also
studied. It was found that most of TMS derivatives demonstrated the
highest sensitivities, followed by methylated derivatives. For BSTFA
or MTBSTFA derivatization processes, the simple injection-port
derivatization process could achieve the same efficiency as that in the
tedious water bath derivatization procedure.
Abstract: In this study, the conversion of n-pentane to aromatics is investigated on HZSM-5 zeolites modified by Ga ion-exchange and silylation using tetraethyl orthosilicate (TEOS) via chemical liquid deposition (CLD). The effect of SiO2/Al2O3 ratios of HZSM-5 was also studied. Parameters in preparing catalysts i.e. TEOS loading and cycles of deposition were varied to obtain the optimal condition for enhancing p-xylene selectivity. The highest p-xylene selectivity 99.7% was achieved when the amount of TEOS was 20 vol.%.The catalysts were characterized by TPD, TPO, XRF, and BET. Results show that the conversion of n-pentane was influenced remarkably by the SiO2/Al2O3 ratios of HZSM-5. The highest p-xylene selectivity 99.7% was achieved when the amount of TEOS was 20 vol.%. And cycles of deposition greatly improves HZSM-5 shape-selectivity.
Abstract: Fecal sterol has been proposed as a chemical indicator
of human fecal pollution even when fecal coliform populations have
diminished due to water chlorination or toxic effects of industrial
effluents. This paper describes an improved derivatization procedure
for simultaneous determination of four fecal sterols including
coprostanol, epicholestanol, cholesterol and cholestanol using gas
chromatography-mass spectrometry (GC-MS), via optimization study
on silylation procedures using N-O-bis
(trimethylsilyl)-trifluoroacetamide (BSTFA), and
N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide
(MTBSTFA), which lead to the formation of trimethylsilyl (TMS) and
tert-butyldimethylsilyl (TBS) derivatives, respectively. Two
derivatization processes of injection-port derivatization and water bath
derivatization (60 oC, 1h) were inspected and compared. Furthermore,
the methylation procedure at 25 oC for 2h with
trimethylsilydiazomethane (TMSD) for fecal sterols analysis was also
studied. It was found that most of TMS derivatives demonstrated the
highest sensitivities, followed by methylated derivatives. For BSTFA
or MTBSTFA derivatization processes, the simple injection-port
derivatization process could achieve the same efficiency as that in the
tedious water bath derivatization procedure.