A headspace SPME-GC-ECD method suitable for determination of chlorophenols in water samples

• Tipo: Artigo em Revista Científica Internacional
• Data: 2011

Autores

Paulo de Morais (Autor) Outra; Teodor Stoichev (Autor) Outra; Clara C P Basto (Autor) FCUP; Pedro N Carvalho (Autor) Outra; Teresa T S D Vasconcelos (Autor) Outra

Revista

Título: Analytical and Bioanalytical Chemistry

Vol. 399 Nº 7

Páginas: 2531-2538

ISSN: 1618-2642

Editora: Springer Nature

Indexação

ISI Web of Knowledge - 17 Citações

Scopus - 16 Citações

Classificação Científica

FOS: Ciências exactas e naturais > Química

Outras Informações

ID Authenticus: P-002-TR3

DOI: 10.1007/s00216-010-4610-y

Abstract (EN): A headspace solid phase microextraction coupled to gas chromatography with electron capture detector (HS-SPME-GC-ECD) method was optimized for the determination of seven chlorophenols (CPs) with different levels of chlorination. This is the first time that HS-SPME-GC-ECD with acetylation of the analytes is used for the simultaneous determination of CPs in water samples. The influence of fibre type, derivatization conditions, salt addition, temperature and time of extraction and temperature of desorption was checked. Possible sources of contamination and analyte losses were considered. The best results were obtained with the polydimethylsiloxane/divinylbenzene fibre, derivatization by acetylation using 100 mu L of acetic anhydride and 0.1 g of anhydrous sodium carbonate per 10 mL of sample, salt addition of 100 g L(-1) sodium chloride, extraction at 70 A degrees C for 60 min and desorption in the GC injector at 260 A degrees C for 6 min. The limits of detection (LOD) for monochlorophenols were 12 and 122 ng L(-1) for 2-chlorophenol and 4-chlorophenol, respectively. For polychlorinated CPs, the LODs were lower than 6 ng L(-1), values similar to the existing methods that use SPME with derivatization for CPs determination in water samples. The method is suitable for the determination of CPs in most environmental aqueous samples. Repeatability and reproducibility were less than 16.8% and 11.7%, respectively. The optimized method was successfully applied for the analysis of waters with complex matrices such as river and estuarine water samples.

Idioma: Inglês

Tipo (Avaliação Docente): Científica

Nº de páginas: 8