Improving detection limits for organotin compounds in several matrix water samples by derivatization-headspace-solid-phase microextraction and GC-MS |
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Authors: | L. Segovia-Martí nez,A. Seco-Torrecillas |
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Affiliation: | a Dpto. Ingeniería Química, Universidad de Valencia, Doctor Moliner 50, 46100 Burjassot, Valencia, Spain b Dpto. Química Analítica, Universidad de Valencia, Doctor Moliner 50, 46100 Burjassot, Valencia, Spain |
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Abstract: | Triethyltin, tributyltin, diphenyltin and triphenyltin were selected as model compounds. The method is based on in situ ethylation and simultaneous headspace-solid-phase microextraction (HS-SPME) and gas chromatographic-mass spectrometry analysis (GC-MS). The extraction procedure was optimized studying some variables such as reaction time, salinity, sample volume and headspace volume. SPME-GC-MS and SPME-GC-FID techniques were compared; quality assurance parameters such as sensitivity, selectivity and precision were established. The proposed procedure showed limits of detection between 0.025 and 1 ng/L. The linearity was in the 0.025-5000 ng/L range. The precision expressed as relative standard deviations (RSD), were below 20%. Real wastewaters and seawaters were analyzed. The method permits controlling legislated annual average values. |
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Keywords: | Gas chromatography Mass detection Headspace solid-phase-microextraction Ethylation Organotin compounds |
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