PCB 47, 51, 68 – Bestimmung von PCB 47, 51, 68 in der Luft am Arbeitsplatz mittels Gaschromatographie (GC-ECD)

Luftanalysen-Methode

Silke Werner¹ (Methodenentwicklung)
  Ralph Hebisch² (Leitung der Arbeitsgruppe „Luftanalysen“ der Ständigen Senatskommission zur Prüfung gesundheitsschädlicher Arbeitsstoffe, Deutsche Forschungsgemeinschaft)
Michael Tschickardt³ (Methodenprüfung)
  Andrea Hartwig⁴ (Vorsitz der Ständigen Senatskommission zur Prüfung gesundheitsschädlicher Arbeitsstoffe, Deutsche Forschungsgemeinschaft)
  MAK Commission<sup>5

1</sup> Institut für Arbeitsschutz der Deutschen Gesetzlichen Unfallversicherung (IFA), Alte Heerstraße 111, 53757 Sankt Augustin, Deutschland
² Bundesanstalt für Arbeitsschutz und Arbeitsmedizin (BAuA), Friedrich-Henkel-Weg 1–25, 44149 Dortmund, Deutschland
³ Wissenschaftliche Beratung für Umwelt- und Arbeitsschutz (WBUA), Westring 24, 55120 Mainz, Deutschland
⁴ Institut für Angewandte Biowissenschaften, Abteilung Lebensmittelchemie und Toxikologie, Karlsruher Institut für Technologie (KIT), Adenauerring 20a, Gebäude 50.41, 76131 Karlsruhe, Deutschland
⁵ Ständige Senatskommission zur Prüfung gesundheitsschädlicher Arbeitsstoffe, Deutsche Forschungsgemeinschaft, Kennedyallee 40, 53175 Bonn, Deutschland

Abstract

This analytical method is a validated measurement procedure for the determination of the three tetrachlorinated biphenyls PCB 47 [2437-79-8], PCB 51 [68194-04-7] and PCB 68 [73575-52-7] in workplace air in a concentration range of 0.16 to 0.62 µg/m³. It was developed to detect PCB that only may be generated during the manufacture of silicone products with peroxidic crosslinking with bis(2,4-dichlorobenzoyl) peroxide. By measurement in manufacturing plants it could be proven that the PCB to be investigated are present exclusively in vapour form. For this reason, the method was only validated for vaporous samples. There are currently no valid evaluation criteria for these PCB. Therefore, the German Occupational Exposure Limit Value for the sum of all PCB (5 × sum of the 6 indicator PCB [28, 52, 101, 138, 152, 180]) of 3 µg/m³ was used as the assessment standard for each congener. For sampling, a defined volume of air is drawn through a sorbent tube filled with Florisil. The flow rate is set to 1 l/min and sampling duration is 4 hours (which correspond to a sampling volume of 240 l). The PCB are extracted with n‑hexane at 40 °C in an ultrasonic bath and subsequently analysed using gas chromatography with electron capture detection. The quantitative determination is based on a calibration function. The limit of quantification is 0.11 µg/m³ based on an air sample volume of 240 l. The mean recovery is 96% and the expanded uncertainty for the validation range of 0.16 to 0.62 µg/m³ is 22 to 24%.

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