Determination of nitrite by GC and GC/MS

We devised a sensitive and simple method to determine nitrite, using an extractive alkylation technique and gas chromatography. Nitrite was alkylated with pentafluorobenzylbromide, with tetradecyldimethylbenzyl-ammonium chloride as the counter-ion in an alkaline solution. The alkylated nitrite, α -nitro-2, 3, 4, 5, 6-pentafluorotoluene, was analyzed qualitatively by gas chromatography/mass spectrometry and quantitatively by gas chromatography with an electron capture detection. The lower limit of detection was 0.01 μmol/ml. The calibration curve was liner in the concentration range from 0.02 to 1.00 μmol/ml.