Determination of N-nitrosodimethylamine in dimethylamine by gas chromatography with nitrogen selective detection and nitrosamine selective detection

Abstract

The separation of N-nltrosodimethylamine from dimethylamine using a silica gel column chromatography procedure which permits trace analysis of the nitrosamine In the amine matrix using a gas chromatographic nitrogen selective detector (NPD) procedure Is described. Recovery percentages are over 90% for nitrosamine levels as low as 4 ppm and 60-80 % for levels around 0,1-0.2 ppm. Precision at the lowest level was ±15%.Confirmation of the nitrosamine identity was provided by examination on gas chromatographic columns of different characteristics, gas chromatography/mass spectometry, Thermal Energy Analysis (TEA) and photodecomposition studies. Confirmation of the quantitative GC/NPD work was provided by GC/TEA. The presence of dimethylnitramine, and its detection using GC/TEA, are also discussed.

Functional group analysis

“…JV-Nitrosodimethylamine in dimethylamine can be analyzed below a level of 0.2 ppm with good recoveries, selectivity, and precision, using a prior isolation of the nitrosamine on a silica gel column, followed by gas chromatographic analysis with a nitrogen selective detector (63).…”