Determination of N-nitrosodimethylamine levels in some Canadian 2,4-D amine formulations.

Levels of N-nitrosodimethylamine (NDMA) were determined in 112 samples of 2,4-dichlorophenoxyacetic acid, (2,4-D), formulated as the dimethylamine salt, collected over a 2 year period from products on the Canadian market. A sample aliquot is partitioned with dichloromethane, and the co-extracted dimethylamine is removed by cleanup on a silica gel column. The eluates containing NDMA are concentrated, an internal standard of N-nitrosodipropylamine is added, and nitrosamine levels are determined using a gas chromatograph interfaced with a thermal energy analyzer. Recoveries of NDMA and N-nitrosodiethylamine spiked into samples were 103 +/- 16 and 96.3 +/- 9.8%, respectively. Of the 112 samples analyzed, 92 were below 1 part per million (ppm) relative to the amount of 2,4-D in the samples, 16 were between 1 and 5 ppm, and 4 were greater than 5 ppm. The gas chromatographic column used is compared to a conventional packing material for volatile nitrosamine analysis. Formation of NDMA during cleanup and analysis was shown not to occur.