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



4-Methyl-3-penten-2-one – Determination of 4-methyl-3-penten-2-one (mesityl oxide) in the workplace air using high-performance liquid chromatography (HPLC-DAD)

Air Monitoring Method – Translation of the German version from 2025

Lutz Nitschke1 (Method development)
Adela Frenzen1 (Method development)
Dietmar Breuer2 (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)
  Uta Lewin-Kretzschmar4 (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 Bavarian State Office for Health and Food Safety (LGL), Pfarrstraße 3, 80538 München, Germany
2 Hochschule Bonn-Rhein-Sieg, Department of Natural Sciences, Grantham-Allee 20, 53757 Sankt Augustin, Germany
3 Federal Institute for Occupational Safety and Health (BAuA), Friedrich-Henkel-Weg 1–25, 44139 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

Abstract

The working group “Air Analyses” of the German Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area (MAK Commission) developed and verified the presented analytical method. It is used to determine the levels of 4-methyl-3-penten-2-one [141-79-7] that occur in the workplace air. The method covers concentrations in the range from one tenth up to twice the current occupational exposure limit value (OELV) of 8.1 mg/m3. The method is also suitable for verifying the short-term exposure limit (STEL; excursion factor 2). Samples are collected by drawing a defined volume of air through a sampling tube filled with silica gel using a flow regulated pump at a volumetric flow rate of 0.5 l/min. Exposure during the shift is measured with a sampling period of 2 hours and the short-term exposure with a period of 15 minutes. The 4-methyl-3-penten-2-one adsorbed to the silica gel is extracted by liquid extraction with methanol and analysed by high-performance liquid chromatography using diode array detection. The quantitative determination is based on multiple-point calibrations with external standards. A relative limit of quantification (LOQ) of 0.06 mg/m3 is obtained for an air sample volume of 60 litres. As the LOQ for a sample volume of 30 litres is 0.03 mg/m3, the STEL can also be measured. The recovery is approx. 100% and the expanded uncertainty is 14% for a sampling period of 2 hours and below 16% for a period of 15 minutes.


Keywords

4-Methyl-3-penten-2-on, Luftanalysen, Analysenmethode, Arbeitsplatzmessung, Gefahrstoff, Hochleistungsflüssigkeitschromatographie, Diodenarray-Detektion, HPLC-DAD, Silicagel, Flüssigdesorption