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  • 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
ABSTRACT

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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Triethylamine, SAJ first grade, ≥98.0%
Sigma-Aldrich
Phosgene solution, 15 wt. % in toluene
Sigma-Aldrich
Triethylamine, for protein sequence analysis, ampule, ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, for amino acid analysis, ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Triethylamine, puriss. p.a., ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, ≥99%
Supelco
Triethylamine, analytical standard
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Toluene-3,4-dithiol, technical grade, 90%
Sigma-Aldrich
Phosgene-12C solution, ~1 M in benzene, 99.9 atom % 12C
Supelco
Toluene-3,4-dithiol, for spectrophotometric det. of Mo, Sn, W, and also Ag and Re, ≥97.0%