Cover: The MAK Collection for Occupational Health and Safety

The MAK Collection for Occupational Health and Safety

Deutsche Forschungsgemeinschaft – Ständige Senatskommission zur Prüfung gesundheitsschädlicher Arbeitsstoffe (MAK-Kommission)

ISSN 2509-2383



Diacetyl (butanedione) – Method for the determination of diacetyl in workplace air using liquid chromatography (HPLC‐UV or HPLC‐MS)

Air Monitoring Method – Translation of the German version from 2016

Claudia Schuh1 (Method development)
Michael Kirchner2 (External verification)
  Ralph Hebisch3 (Head of the working group “Air Analyses” of the Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area, Deutsche Forschungsgemeinschaft)
  Thomas Helmut Brock4 (Head of the working group "Analytics")
  Andrea Hartwig5 (Chair of the Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area, Deutsche Forschungsgemeinschaft)
  MAK Commission6

1 German Social Accident Insurance Institution for the foodstuffs industry and the catering trade (BGN), Dynamostraße 7–11, 68165 Mannheim, Germany
2 Institute for the Research on Hazardous Substances of the Insurance Institution for the raw materials and chemical industry (IGF), Institute at the Ruhr‐University Bochum, Waldring 97, 44789 Bochum, Germany
3 Federal Institute for Occupational Safety and Health (BAuA), Friedrich-Henkel-Weg 1–25, 44149 Dortmund, Germany
4 German Social Accident Insurance, Institution for the raw materials and chemical industry, Prevention - Department of Hazardous Substances, Biological Agents and Analytical Chemistry, Kurfürsten-Anlage 62, 69115 Heidelberg, Germany
5 Institute of Applied Biosciences, Department of Food Chemistry and Toxicology, Karlsruhe Institute of Technology (KIT), Adenauerring 20a, Building 50.41, 76131 Karlsruhe, Germany
6 Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area, Deutsche Forschungsgemeinschaft, Kennedyallee 40, 53175 Bonn, Germany

This analytical method is a validated measurement procedure for the determination of 2,3‐butanedione (diacetyl) in workplace air in a concentration range of a tenth up to twice the currently valid Occupational Exposure Limit (OEL) or MAK value. Sampling is performed by drawing a defined volume of air through a cartridge filled with silica gel impregnated with 2,4‐dinitrophenylhydrazine (DNPH) using a suitable flow‐regulated pump with a volumetric flow rate of 1 mL/min. For sampling 1 hour or 15 min (checking the short‐term value) can be used. The formed diacetyl‐2,4‐DNPH derivatives are desorbed with acetonitrile containing a defined amount of DNPH and analysed by means of liquid chromatography (HPLC‐UV or HPLC‐MS). Quantitative evaluation is based on a 10‐point calibration using methacrolein‐2,4‐DNPH as internal standard. The limit of quantification for diacetyl is 0.002 mg/m3 based on an air sample volume of approx. 60 L or 0.006 mg/m3 based on an air sample volume of approx. 15 L (for short‐term value).

Joint Publication of the Analytical Subcommittee of the Chemistry Board of Experts of the Expert Committee Raw Materials and Chemical Industry of the German Social Accident Insurance and the Working Group “Air Monitoring Methods” of the Permanent Senate Commission of the DFG for the Investigation of Health Hazards of Chemical Compounds in the Work Area.


Keywords

Diacetyl, Luftanalysen, Analysenmethode, Arbeitsplatzmessung, Gefahrstoff, Hochleistungsflüssigkeitschromatographie, UV-Detektion oder Massenspektrometrie, HPLC-UV oder HPLC-MS, Silicagel, imprägniert mit 2,4-DNPH, Flüssigdesorption