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Diplomska naloga obsega razvoj metode priprave vzorcev za določevanje spojin obstojnih organskih onesnaževal z metodo plinske kromatografije povezane z masno spektrometrijo (GC/MS). Vsebnosti polikloriranih alkanov (PCA) v ekstraktih vodnih vzorcev smo določevali z analitsko tehniko kemične ionizacije in zaznavo negativnih ionov (ECNI). Primerjali smo dve analitski tehniki priprave vodnih vzorcev, ekstrakcijo tekoče-tekoče in ekstrakcijo na trdni fazi. Prednostno smo obravnavali razvoj metode določevanja polikloriranih alkanov in način odstranjevanja pri analizi motečih vplivov polikloriranih bifenilov (PCB). Za čiščenje ekstraktov smo uporabili antropogeno in Florisilno kolono. Določili smo optimalne pogoje ločitve motečih spojin polikloriranih bifenilov od polikloriranih alkanov na Florisilni koloni. Za kvantitativno določitev smo uporabili standardne raztopine analitov PCA (C10-C13, SCCP) in PCB 209 ter γ-heksaklorocikloheksan kot spojini internih standardov. PCA v površinskih vodah smo določali v koncentracijskem območju od 0,05 μg/L do 0,15 μg/L. The diploma thesis includes the development of the method for sample preparation for the determination of persistent organic pollutants by gas chromatography and mass spectrometry (GC/MS). Levels of polychlorinated alkanes (PCAs) in extracts of water samples were determined using an analytical technique of chemical ionization and negative ion detection (ECNI). We compared two analytical techniques, liquid-liquid extraction and solid phase extraction. We addressed the development of the method for determination of polychlorinated alkanes and the method for disposal of polychlorinated biphenyls (PCBs), which cause problems in the analysis. The anthropogenic and the Florisil column were used for cleaning extracts. Optimal conditions for the separation of interfering compounds PCBs from polychlorinated alkanes in the Florisil column were determined. For the quantitative determination standard solutions of analytes PCA (C10-C13, SCCP), PCB 209 and γ-hexachlorocyclohexane as internal standards were used. PCA in surface waters were determined in the concentration range from 0,05 μg/L to 0,15 μg/L. |
