1978 Volume 27 Issue 10 Pages 616-621
A method for simultaneous determination of ethanolamines and N-nitrosodiethanolamine in commercial cutting fluids was developed. The procedure is as follows. A sample (about 10 mg) is taken into a test tube with a cap and then ethanol(1 ml), urea (2%, 0.5 ml) and acetic acid (0.1 ml) are added to it for destroying nitrite which is generally present in a sample. After being shaken slowly, the mixture is dried up by heating under the stream of nitrogen gas. Ethanol (about 1 ml) is added to the residue and dried up again. The residue is dried till it does not smell of acetic acid, and is silylated with dimethylformamide (200μl) and N, O-bis (trimethylsilyl)-trifluoroacetamide (200μl) at 60°C in an oil bath for 10 min. The silylated solution is diluted with dimethylchloride and an aliquot is injected into the GC-FID or GC-MS-MID. Selected mass numbers(m/e) of ethanolamines (mono, di and tri) and N-nitrosodiethanolamine are 102, 130, 262 and 130, respectively. Through the analytical process, artifact formation of N-nitrosodiethanolamine was notobserved. The detection limit for ethanolamines (mono, di and tri) and N-nitrosodiethanolamine by mass fragmentography were 1, 1, 1 and 5 ng and by gas chromatography were 4, 2, 2 and 4μg, respectively.
