Details

Autor(en) / Beteiligte

• Fiamegos, Yiannis C
• Konidari, Constantina N
• Stalikas, Constantine D

Titel

Cyanuric acid trace analysis by extractive methylation via phase-transfer catalysis and capillary gas chromatography coupled with flame thermoionic and mass-selective detection

Ist Teil von

• Analytical chemistry (Washington), 2003-08, Vol.75 (16), p.4034

Ort / Verlag

Washington: American Chemical Society

Erscheinungsjahr

2003

Quelle

Alma/SFX Local Collection

Beschreibungen/Notizen

• A GC method using phase-transfer catalysis for the simultaneous derivatization, extraction, and preconcentration of the highly polar cyanuric acid (CYA) was developed. The method was based on the extractive N-methylation of the analyte of concern in two- and threephase systems, whereby the 1,3,5-trimethyl-1,3,5-triazine-2,4,6-(1H,3H,5H)trione was formed. Subsequent detection was performed using flame thermoionic specific detection (FID) and mass spectrometry (MS) selectiveion monitoring (SIM) using electron impact The optimal experimental conditions related to pH, kind of catalyst and solvents, methyl iodide concentration, phase volumes, reaction time, temperature, and agitation were suitably established. Inter alia, the resulting method is highly sensitive, almost free from interferences, and was easily applied to the determination of cyanuric acid in swimming pool water, surface water, human urine, and simulated air filter !samples. The minimal quantitable concentration was found to be less than 1 and 90 jig L- I using GC-MS(SIM) and GC-FID, respectively. The overall precision for the workup procedure did not exceed 3.6% (n = 6) for 5.0 microng L- I CYA-spiked urine and river water while the respective value for the same matrixes spiked at a concentration of 200 microng L-1 was calculated to be in the range 1.9-4.0% (n = 6). The overall recovery from spiked samples was 98 plus or minus 5% for microgram per liter levels of CYA. A kinetic study conducted was helpful to get a better insight into the N-methylation reaction mechanism. [PUBLICATION ABSTRACT]