Determination of N-nitrosodipropylamine in trifluralin emulsifiable concentrates using minicolumn cleanup and gas chromatography with thermal energy analyzer.

D Wotherspoon, R Hindle

Index: J. Assoc. Off. Anal. Chem. 71(2) , 333-6, (1988)

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Abstract

A quick method for determining N-nitrosodipropylamine (NDPA) levels in trifluralin emulsifiable concentrate formulations is described. At least 18 samples can be analyzed at one time in a minimum of fumehood space, with up to 90% savings on solvents and materials. A sample aliquot is mixed with a solution containing nitrosamine recovery standards, and nitrosamines are separated by minicolumn cleanup. Internal standard is added directly to the eluate containing the nitrosamines, and levels are determined by gas chromatography with thermal energy analyzer. Recoveries of spiked nitrosamines ranged from 98 to 102%. Coefficients of variation for samples containing less than 0.5 ppm NDPA are less than 13%. Minimum detectable limit, calculated as 3 times the noise, is 0.06 ppm. Comparison with the method formerly used by this laboratory shows no significant difference in the analytical results at 95% confidence limits, and control experiments were performed to ensure that there was no artifact formation of NDPA.