Optimization of headspace solid-phase microextraction by means of an experimental design for the determination of methyl tert.-butyl ether in water by gas chromatography-flame ionization detection.
A procedure for determination of methyl tert.-butyl ether (MTBE) in water by headspace solid-phase microextraction (HS-SPME) has been developed. The analysis was carried out by gas chromatography with flame ionization detection. The extraction procedure, using a 65-microm poly(dimethylsiloxane)-divinylbenzene SPME fiber, was optimized following experimental design. A fractional factorial design for screening and a central composite design for optimizing the significant variables were applied. Extraction temperature and sodium chloride concentration were significant variables, and 20 degrees C and 300 g/l were, respectively chosen for the best extraction response. With these conditions, an extraction time of 5 min was sufficient to extract MTBE. The calibration linear range for MTBE was 5-500 microg/l and the detection limit 0.45 microg/l. The relative standard deviation, for seven replicates of 250 microg/l MTBE in water, was 6.3%.
Departamento de Química Aplicada, Facultad de Químicas, Universidad del País Vasco, San Sebastián, Spain.
Julien
J
Dron
Rosa
R
Garcia
Esmeralda
E
Millán
D002138:Calibration; D002849:Chromatography, Gas / Q000379:methods*; D008738:Methyl Ethers / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014874:Water Pollutants, Chemical / Q000032:analysis*
D008738:Methyl Ethers; D014874:Water Pollutants, Chemical; C043243:methyl tert-butyl ether