Determination of trace amounts of primary and secondary amines (methylamine, ethylamine, propylamine, isopropylamine, butylamine, isobutylamine,
s-butylamine, dimethylamine, diethylamine, dipropylamine, dibutylamine, and diisobutylamine) in water has been developed by gas chromatography mass spectrometry. The principle of this method is to determine the reaction products of amines with 1-fluoro-2, 4-dinitrobenzene (FDNB) water. To 200 ml of sample alkalized with 20 ml of 2.5 % sodium tetraborate (Na
2B
4O
7·10H
2O), 15 ml of FDNB solution (20 ml of FDNB in 250 ml of 1, 4-dioxane) was added, and the mixture was heated in a boiling water bath for 15 min. After cooling, the solution was transferred to a 300-ml separatory funnel. The solution was shaken for 15 min to hydrolyze the excess FDNB by adding 20 ml of 2 N NaOH. 2, 4-Dinitrophenylamine derivatives (2, 4-DNPA) were extracted with benzene (40 ml, 30 ml). The benzene extract was washed with 20 ml of 0.1 N NaOH, dehydrated with an anhydrous Na
2SO
4 column, and passed through an activated (5 g, Woelm Pharma, Basic aluminium oxide, Activity grade I) column(1.5 cm i. d.). Most of 2, 4-DNPA were eluted with 20 ml of ethyl acetate from the alumina column. The benzene and ethyl acetate eluted were combined and concentrated to 1 ml with a Kuderna-Danish evaporator under reduced pressure. Each 2, 4-DNPA was determined by a gas chromatograph-mass spectrometer with a multiple ion detector, which enable to detect less than nanogram amounts. As an internal standard, [
2H
3]methylamine was used. FDNB reacted quantitatively with aliphatic amines except
t-butylamine and diisopropylamine. Residual FDNB, 2, 4-dinitroaniline produced by FDNB and ammonia, and bis(2, 4-dinitrophenyl) ether produced by hydrolysis of FDNB could be removed from the benzene extract by alumina-column chromatography. By this method, aliphatic amines (methylamine, ethylamine, dimethylamine, and diethylamine) in sewage can be determined in the range of (13) ppb.
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