Isocyanates, Amines and Alkanolamines : Sampling, Chromatography and Detection

• Main Author: Riddar, Jakob B.
• Format: Doctoral Thesis
• Language: English
• Published: Stockholms universitet, Institutionen för analytisk kemi 2013
• Subjects: Air-sampling; Isocyanates; Aromatic amines; Aliphatic amines; Alkanolamines; Hydrophilic Interaction Liquid Chromatography; Dry Denuder-Filter sampler; Liquid Chromatography–tandem Mass Spectrometry; Polyurethane Foam Extraction
• Online Access: http://urn.kb.se/resolve?urn=urn:nbn:se:su:diva-94067; http://nbn-resolving.de/urn:isbn:978-91-7447-747-4

Isocyanates, aromatic-, aliphatic- and alkanolamines are commonly used in the industry today. Millions of workers in Europe are exposed. The most frequent health symptoms are respiratory and dermal disorder. Due to the health risk most of the compounds in this thesis are regulated by authorities and have occupational exposure limits (OELs). Consequently, reliable and robust air sampling methods are urgently needed. In this thesis dry samplers for isocyanates, aliphatic- and alkanolamines have been developed and evaluated. The isocyanate sampler is now a commercial product (ASSET EZ4-NCP Dry Sampler, Supelco). The samplers were based on a denuder with a filter in series. The denuder and filter were impregnated with di-n-butylamine for the isocyanate sampler and with sulphuric acid for the aliphatic- and alkanolamine sampler. The robustness of the dry samplers was extensively evaluated. This was performed in a climate chamber containing a controlled atmosphere of the studied compounds. New methods based on hydrophilic interaction liquid chromatography (HILIC) coupled with tandem mass spectrometry (MSMS) were developed for determination of aromatic-, aliphatic- and alkanolamines in aqueous solutions. Isocyanates were determined by reversed-phase liquid chromatography MSMS. HILIC in combination with MS is a most powerful system, and highly sensitive determinations, several orders of magnitude below the OELs, of polar compounds present in the work environment can be accomplished. The selected samplers enable sampling during short sampling times and for whole work shifts. The samplers can be stored for months before and after sampling. The performance of the samplers was unaffected by variation in temperature, humidity, flow-rate and pre- and post-sampling of ambient air. Sampling for the compounds studied is now greatly simplified, and assessment of the work environment is facilitated. === <p>At the time of the doctoral defence the following papers were unpublished and had a status as follows: Paper 1: Epub ahead of print; Papers 3-5: Manuscripts</p>