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 Stud
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- 作者：Yiannis C. Fiamegos ; Constantina N. Konidari ; and Constantine D. Stalikas
- 刊名：Analytical Chemistry
- 出版年：2003
- 出版时间：August 15, 2003
- 年：2003
- 卷：75
- 期：16
- 页码：4034 - 4042
- 全文大小：102K
- 年卷期：v.75,no.16(August 15, 2003)
- ISSN：1520-6882
文摘
A GC method using phase-transfer catalysis for thesimultaneous derivatization, extraction, and preconcentration of the highly polar cyanuric acid (CYA) wasdeveloped. The method was based on the extractiveN-methylation of the analyte of concern in two- and three-phase systems, whereby the 1,3,5-trimethyl-1,3,5-triazine-2,4,6-(1H,3H,5H)trione was formed. Subsequentdetection was performed using flame thermoionic specificdetection (FTD) and mass spectrometry (MS) selective-ion monitoring (SIM) using electron impact. The optimalexperimental conditions related to pH, kind of catalyst andsolvents, methyl iodide concentration, phase volumes,reaction time, temperature, and agitation were suitablyestablished. Inter alia, the resulting method is highlysensitive, almost free from interferences, and was easilyapplied to the determination of cyanuric acid in swimmingpool water, surface water, human urine, and simulatedair filter samples. The minimal quantitable concentrationwas found to be less than 1 and 90 
g L-1 using GC-MS(SIM) and GC-FTD, respectively. The overall precisionfor the workup procedure did not exceed 3.6% (n = 6)for 5.0 g L-1 CYA-spiked urine and river water while therespective value for the same matrixes spiked at aconcentration of 200 g L-1 was calculated to be in therange 1.9-4.0% (n = 6). The overall recovery from spikedsamples was 98 ± 5% for microgram per liter levels ofCYA. A kinetic study conducted was helpful to get a betterinsight into the N-methylation reaction mechanism.
g L-1 using GC-MS(SIM) and GC-FTD, respectively. The overall precisionfor the workup procedure did not exceed 3.6% (n = 6)for 5.0 g L-1 CYA-spiked urine and river water while therespective value for the same matrixes spiked at aconcentration of 200 g L-1 was calculated to be in therange 1.9-4.0% (n = 6). The overall recovery from spikedsamples was 98 ± 5% for microgram per liter levels ofCYA. A kinetic study conducted was helpful to get a betterinsight into the N-methylation reaction mechanism.