Cover: The MAK Collection for Occupational Health and Safety

The MAK Collection for Occupational Health and Safety

German Research Foundation – Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area
(MAK Commission)

ISSN 2509-2383



Method for the determination of hydrazine in workplace air using gas chromatography‐mass spectrometry (GC‐MS)

Air Monitoring Method

Wilhelm Krämer1 (Method development)
  Thomas Helmut Brock2 (Head of the working group "Analytics")
  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)
  Andrea Hartwig4 (Chair of the Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area, Deutsche Forschungsgemeinschaft)
  MAK Commission5

1 BASF SE, ESE/MA ‐ Z 570, Carl-Bosch-Straße 38, 67056 Ludwigshafen, Germany
2 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
3 Federal Institute for Occupational Safety and Health (BAuA), Friedrich-Henkel-Weg 1–25, 44149 Dortmund, Germany
4 Institute of Applied Biosciences, Department of Food Chemistry and Toxicology, Karlsruhe Institute of Technology (KIT), Adenauerring 20a, Geb. 50.41, 76131 Karlsruhe, Germany
5 Permanent Senate Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area, Deutsche Forschungsgemeinschaft, Kennedyallee 40, 53175 Bonn, Germany

Abstract

This analytical method is a validated measurement procedure for the determination of hydrazine in workplace air for risk assessment at work. Sampling is performed by drawing a defined volume of air through an adsorption tube filled with XAD‐2 impregnated with 2,4‐pentanedione using a flow‐regulated pump. The flow rate is set to 200 mL/min with a recommended air sample volume of approx. 48 litres at a sampling period of 4 hours. After sampling the formed 3,5‐dimethylpyrazole is extracted with methanol and analysed by means of gas chromatography‐mass spectrometry (GC‐MS). The absolute limit of quantification (LOQ) is 0.05 ng and the relative LOQ is 0.002 mg/m3 based on an air sample volume of approx. 48 litres. The mean recovery was 82% and the expanded uncertainty for the overall measurement method 18%.

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 Analyses” of the Permanent Senate Commission of the DFG for the Investigation of Health Hazards of Chemical Compounds in the Work Area.


Keywords

hydrazine, air analyses, analytical method, workplace measurement, hazardous substance, gas chromatography, mass spectrometry, GC-MS, XAD-2, impregnated with 2,4-pentanedione, liquid desorption