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Determination of polar organic pollutants in aqueous samples of former ammunition sites in lower saxony by means of HPLC/photodiode array detection (HPLC/PDA) and proton nuclear magnetic resonance spectroscopy (H-NMR)



Acta Hydrochimica et Hydrobiologica 26 (1998), Nr.6, S.330-337
ISSN: 0323-4320
ISSN: 1863-0669
ISSN: 1521-401X
Fraunhofer ITA ( ITEM) ()
water; explosive; ammunition; high performance liquid chromatography; nuclear magnetic resonance spectroscopy

Leachate, ground-, and surface water from former ammunition sites and areas which are known to be contaminated by nitroaromatic compounds in Lower Saxony (Germany) were investigated in order to identify and quantify acidic nitroaromatic compounds (e.g., nitrobenzoic acids, aminonitrobenzoic acids, nitrophenols, and nitrocresols). Acidic and neutral nitroaromatic compounds were enriched by solid-phase extraction (SPE) on a polystyrenedivinylbenzene copolymer and routinely screened for acidic compounds by means of HPLC/photodiode array detection (HPLC/PDA). Qualitative and quantitative results obtained in this way were corroborated by proton nuclear magnetic resonance spectroscopy (1H-NMR). Validation data for the quantification procedure using this technique are given. The results show that all samples contaminated with 2,4,6-trinitrotoluene (TNT) and related compounds are also contaminated by acidic nitroaromatic compounds (e.g., 2,4-dinitrobenzoic acid, 3,5-dinitrophenol, and especially with 2-amino-4,6-dinitrobenzoic acid) in the g/L range. This current work shows that 1 H-NMR allows the quantitative determination of protoncarrying analytes in mixtures after solid-phase extraction down to the upper ng/L range after addition of an internal standard to the SPE extract. This is even possible when reference compounds are not commercially available.