Zimmermann, Thomas ; Ensinger, Wolfgang ; Schmidt, Torsten C. (2004)
In Situ Derivatization/Solid-Phase Microextraction: Determination of Polar Aromatic Amines.
In: Analytical Chemistry, 76 (4)
doi: 10.1021/ac035098p
Artikel, Bibliographie
Kurzbeschreibung (Abstract)
A solid-phase microextraction GC/MS method for the trace determination of a wide variety of polar aromatic amines in aqueous samples was developed. Prior to extraction the analytes were derivatized directly in the aqueous solution by diazotation and subsequent iodination in a one-pot reaction. The derivatives were extracted by direct-SPME using a PDMS/DVB fiber and analyzed by GC/MS in the full-scan mode. By diazotation/iodination, the polarity of the analytes was significantly decreased and as a consequence extraction yields were dramatically improved. The derivatization proved to be suitable for strongly deactivated aromatic amines and even the very polar diamino compounds can efficiently be enriched after derivatization. We investigated 18 anilines comprising a wide range of functional groups, which could be determined simultaneously. The method was thoroughly validated, and the precision at a concentration of 0.5 μg/L was 3.8−11% relative standard deviation for nonnitrated analytes using aniline-d5 as internal standard and 3.7−10% for nitroaromatic amines without internal standard. The in situ derivatization/SPME/GC/MS method was calibrated over the whole analytical procedure and was linear over 2 orders of magnitude. Using 10-mL samples, detection limits of 2−13 ng/L were achieved for 15 of the 18 analytes. For two aminodinitrotoluene isomers and a diaminonitrotoluene, detection limits ranged from 27 to 38 ng/L. By allowing quantification at the 0.1 μg/L level, analysis of all target compounds meets EU drinking water regulations. The method provides high sensitivity, robustness, and high sample throughput by automation. Finally, the method was applied to various real water samples and in wastewater from a former ammunition plant the contents of several aromatic amines were quantified.
| Typ des Eintrags: | Artikel |
|---|---|
| Erschienen: | 2004 |
| Autor(en): | Zimmermann, Thomas ; Ensinger, Wolfgang ; Schmidt, Torsten C. |
| Art des Eintrags: | Bibliographie |
| Titel: | In Situ Derivatization/Solid-Phase Microextraction: Determination of Polar Aromatic Amines |
| Sprache: | Englisch |
| Publikationsjahr: | 15 Februar 2004 |
| Verlag: | ACS |
| Titel der Zeitschrift, Zeitung oder Schriftenreihe: | Analytical Chemistry |
| Jahrgang/Volume einer Zeitschrift: | 76 |
| (Heft-)Nummer: | 4 |
| DOI: | 10.1021/ac035098p |
| Kurzbeschreibung (Abstract): | A solid-phase microextraction GC/MS method for the trace determination of a wide variety of polar aromatic amines in aqueous samples was developed. Prior to extraction the analytes were derivatized directly in the aqueous solution by diazotation and subsequent iodination in a one-pot reaction. The derivatives were extracted by direct-SPME using a PDMS/DVB fiber and analyzed by GC/MS in the full-scan mode. By diazotation/iodination, the polarity of the analytes was significantly decreased and as a consequence extraction yields were dramatically improved. The derivatization proved to be suitable for strongly deactivated aromatic amines and even the very polar diamino compounds can efficiently be enriched after derivatization. We investigated 18 anilines comprising a wide range of functional groups, which could be determined simultaneously. The method was thoroughly validated, and the precision at a concentration of 0.5 μg/L was 3.8−11% relative standard deviation for nonnitrated analytes using aniline-d5 as internal standard and 3.7−10% for nitroaromatic amines without internal standard. The in situ derivatization/SPME/GC/MS method was calibrated over the whole analytical procedure and was linear over 2 orders of magnitude. Using 10-mL samples, detection limits of 2−13 ng/L were achieved for 15 of the 18 analytes. For two aminodinitrotoluene isomers and a diaminonitrotoluene, detection limits ranged from 27 to 38 ng/L. By allowing quantification at the 0.1 μg/L level, analysis of all target compounds meets EU drinking water regulations. The method provides high sensitivity, robustness, and high sample throughput by automation. Finally, the method was applied to various real water samples and in wastewater from a former ammunition plant the contents of several aromatic amines were quantified. |
| Fachbereich(e)/-gebiet(e): | 11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft > Fachgebiet Materialanalytik 11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft 11 Fachbereich Material- und Geowissenschaften |
| Hinterlegungsdatum: | 06 Sep 2012 07:48 |
| Letzte Änderung: | 05 Mär 2013 10:02 |
| PPN: | |
| Sponsoren: | We thank the Restek Corp. for providing the Stx CLPesticides column and Klaus Steinbach for his support. |
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