Zusammenfassung
Das beschriebene Verfahren dient zur Bestimmung von chlorierten Verbindungen (chlorierte Benzole, Hexachlorcyclohexane, polychlorierte Biphenyle, DDT-Gruppe) in niedrigen Konzentrationen (pg/m3) in Luft. Da die meisten dieser Verbindungen gasförmig vorkommen, wurde eine Probenahmemethode für große Volumina unter Verwendung von sorgfältig vorgereinigtem Polyurethanschaum als Adsorptionsmedium entwickelt. Proben von 2000–4000 m3 wurden an verschiedenen Stellen der Arktis genommen. Die Vorbehandlung des Schaums und der Probe wird ausführlich beschrieben. Bei ng-Mengen lag die Wiederfindung bei 80–115%. Die Leistungsfähigkeit der ersten Schaumschicht lag bei 80–100%. Durch Temperatur, Luftfeuchtigkeit und Probenahmevolumen wird die Leistungsfähigkeit beeinflußt. Zur Identifizierung und quantitativen Bestimmung wurde die Negativionen-Massenspektrometrie mit chemischer Ionisation und die EC-Detektion mit der Hochleistungs-Gas-Chromatographie kombiniert. Die Nachweisgrenze lag für die meisten Verbindungen bei weniger als einigen pg/m3. Einige Daten der arktischen Messungen werden vorgestellt und kurz diskutiert.
Summary
A method has been developed for the determination of very low concentrations (pg/m3) of organic chlorinated compounds in air. Chlorinated benzenes, hexachlorocyclohexanes, polychlorinated biphenyls and the DDT group. Since most of the atmospheric burden of such compounds occurs in the gas phase, a high volume sampling method has been developed using carefully precleaned polyurethane foam as collection medium. Samples of 2000–4000 m3 were taken at different sites in the Arctic. The foam quality as well as the precleaning procedure of the foam and the clean-up of the sample are described in detail. The recovery of both the extraction and sample pretreatment was in the range of 80–115% for nanogram amounts. Sampling efficiency for the first foam plug was 80–100%.
The sampling efficiency is influenced by different factors (temperature, air humidity, sampling volume). For quantification and identification, the highly selective methods of negative ion chemical ionization mass spectrometry and electron capture detection were combined with high resolution gas chromatography. The detection limit of the method was for most compounds less than a few pg/m3. Some preliminary data from the Arctic measurements are presented and are briefly discussed.
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Oehme, M., Stray, H. Quantitative determination of ultra-traces of chlorinated compounds in high-volume air samples from the Arctic using polyurethane foam as collection medium. Z. Anal. Chem. 311, 665–673 (1982). https://doi.org/10.1007/BF00488942
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DOI: https://doi.org/10.1007/BF00488942