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Determination of isocyanic acid in air
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
Work Environment Chemistry, Lund University.
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2004 (English)In: Journal of Environmental Monitoring, ISSN 1464-0325, Vol. 3, no 4, 432-436 p.Article in journal (Refereed) Published
Abstract [en]

A method is presented for the determination of isocyanic acid (ICA), HNCO, in air samples as a di-n-butylamine (DBA) derivative. The method is based on sampling in midget impinger flasks containing 10 ml of 0.01 mol l–1 DBA in toluene. Quantification was made using liquid chromatography (LC) and electrospray mass spectrometry (MS) monitoring positive ions. The instrumental detection limit for the LC-MS was 10 fmol of ICA-DBA. ICA was generated by thermal decomposition of urea. A standard solution containing the DBA derivatives of ICA was prepared by collecting the emitted ICA in an impinger flask containing DBA. ICA in the reference solution was characterised by LC and time-of-flight (TOF) MS and quantified by LC chemiluminescent nitrogen detection (LC-CLND). The instrumental detection limit for the LC-CLND was 1 ng of nitrogen. ICA was emitted during thermal degradation of PFU resins and polyurethane (PUR) lacquers, from car metal sheets. ICA was the most dominant isocyanate and in PUR coating up to 8% of the total weight was emitted as ICA and for PFU resins up to 14% was emitted as ICA. When air samples were collected in an iron foundry during casting in sand moulds with furan resins, concentrations of ICA in the range 50–700 µg m–3 were found in the working atmosphere

Place, publisher, year, edition, pages
Royal Society of Chemistry , 2004. Vol. 3, no 4, 432-436 p.
Keyword [en]
AIRBORNE ISOCYANATES; THERMAL-DEGRADATION; COMPLEX-MIXTURES; CHEMILUMINESCENT NITROGEN; LIQUID-CHROMATOGRAPHY; POLYURETHANE; AMINES; SURVEILLANCE; DIISOCYANATE; DETECTOR
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:su:diva-23246DOI: 10.1039/b103476fOAI: oai:DiVA.org:su-23246DiVA: diva2:190903
Note
Part of urn:nbn:se:su:diva-204Available from: 2004-08-20 Created: 2004-08-20 Last updated: 2010-01-05Bibliographically approved
In thesis
1. Isocyanates and Amines – Sampling and Analytical Procedures
Open this publication in new window or tab >>Isocyanates and Amines – Sampling and Analytical Procedures
2004 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis covers sampling and analytical procedures for isocyanates (R-NCO) and amines (R-NH2), two kinds of chemicals frequently used in association with the polymeric material polyurethane (PUR). Exposure to isocyanates may result in respiratory disorders and dermal sensitisation, and they are one of the main causes of occupational asthma. Several of the aromatic diamines associated with PUR production are classified as suspected carcinogens. Hence, the presence of these chemicals in different exposure situations must be monitored.

In the context of determining isocyanates in air, the methodologies included derivatisation with the reagent di-n-butylamine (DBA) upon collection and subsequent determination using liquid chromatography (LC) and mass spectrometric detection (MS). A user-friendly solvent-free sampler for collection of airborne isocyanates was developed as an alternative to a more cumbersome impinger-filter sampling technique. The combination of the DBA reagent together with MS detection techniques revealed several new exposure situations for isocyanates, such as isocyanic acid during thermal degradation of PUR and urea-based resins. Further, a method for characterising isocyanates in technical products used in the production of PUR was developed. This enabled determination of isocyanates in air for which pure analytical standards are missing. Tandem MS (MS/MS) determination of isocyanates in air below 10-6 of the threshold limit values was achieved.

As for the determination of amines, the analytical methods included derivatisation into pentafluoropropionic amide or ethyl carbamate ester derivatives and subsequent MS analysis. Several amines in biological fluids, as markers of exposure for either the amines themselves or the corresponding isocyanates, were determined by LC-MS/MS at amol level. In aqueous extraction solutions of flexible PUR foam products, toluene diamine and related compounds were found.

In conclusion, this thesis demonstrates the usefulness of well characterised analytical procedures and techniques for determination of hazardous compounds. Without reliable and robust methodologies there is a risk that exposure levels will be underestimated or, even worse, that relevant compounds will be completely missed.

Place, publisher, year, edition, pages
Stockholm: Institutionen för analytisk kemi, 2004. 65 p.
Keyword
Isocyanates, Amines, Polyurethane, Air sampling, Industrial hygiene, Mass spectrometry, Liquid chromatography, Chemiluminescence
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:su:diva-204 (URN)91-7265-917-3 (ISBN)
Public defence
2004-09-10, Vita salongen, Hässleholms kulturhus, Järnvägsgatan 23, Hässleholm, 10:00
Opponent
Supervisors
Available from: 2004-08-20 Created: 2004-08-20Bibliographically approved

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