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

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