Direkt zum Inhalt
Merck
  • Development and validation of a sensitive thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) method for the determination of phosgene in air samples.

Development and validation of a sensitive thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) method for the determination of phosgene in air samples.

Analytical and bioanalytical chemistry (2014-05-13)
Y Juillet, C Dubois, F Bintein, J Dissard, A Bossée
ZUSAMMENFASSUNG

A new rapid, sensitive and reliable method was developed for the determination of phosgene in air samples using thermal desorption (TD) followed by gas chromatography-mass spectrometry (GC-MS). The method is based on a fast (10 min) active sampling of only 1 L of air onto a Tenax® GR tube doped with 0.5 mL of derivatizing mixture containing dimercaptotoluene and triethylamine in hexane solution. Validation of the TD-GC-MS method showed a low limit of detection (40 ppbv), acceptable repeatability, intermediate fidelity (relative standard deviation within 12 %) and excellent accuracy (>95%). Linearity was demonstrated for two concentration ranges (0.04 to 2.5 ppmv and 2.5 to 10 ppmv) owing to variation of derivatization recovery between low and high concentration levels. Due to its simple on-site implementation and its close similarity with recommended operating procedure (ROP) for chemical warfare agents vapour sampling, the method is particularly useful in the process of verification of the Chemical Weapons Convention.

MATERIALIEN
Produktnummer
Marke
Produktbeschreibung

Sigma-Aldrich
Triethylamin, ≥99.5%
Sigma-Aldrich
Triethylamin, ≥99%
Sigma-Aldrich
Triethylamin, puriss. p.a., ≥99.5% (GC)
Sigma-Aldrich
Triethylamin, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Phosgen -Lösung, 15 wt. % in toluene
Sigma-Aldrich
Phosgen -Lösung, ~20% in toluene
Sigma-Aldrich
Triethylamin, for amino acid analysis, ≥99.5% (GC)
Sigma-Aldrich
Triethylamin, ≥99.5%
Sigma-Aldrich
Triethylamin, for protein sequence analysis, ampule, ≥99.5% (GC)
Supelco
Triethylamin, analytical standard
Sigma-Aldrich
Toluol-3,4-dithiol, technical grade, 90%
Supelco
Toluol-3,4-dithiol, for spectrophotometric det. of Mo, Sn, W, and also Ag and Re, ≥97.0%
Sigma-Aldrich
Phosgen-12C -Lösung, ~1 M in benzene, 99.9 atom % 12C