期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1010, 期 2, 页码 243-253出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/S0021-9673(03)01123-3
关键词
water analysis; environmental analysis; pyrolysis; derivatization; GC; amines; aromatic; N-allyl-N '-arylthioureas; aryl isothiocyanates
Derivatization of aromatic primary amines to N-allyl-N'-arylthioureas by reaction with allyl isothiocyanate and GC-MS of the derivatives, when pyrolysis to aryl isothiocyanates occurs in the heated injector, has been used to determine aromatic amines in the range 0.5-50 mug l(-1) with a correlation coefficient, r, in the range 0.9902-0.9992. The limit of detection ranged 8 to 30 ng l(-1) when 60 ml of sample were preconcentrated, after derivatization, on a styrene-divinylbenzene copolymer sorbent. The pyrolytic cleavage of sym- and unsym-diaryl or alkyl-/arylthioureas has been rationalized. The chromatography of isothiocyanates is much superior to that of aryl amines and the specific mass fragmentation pen-nits positive identification of amines. The method has been applied to spiked drinking water, groundwater and river water samples, when the recovery ranged from 84 to 109% with RSD of 5-9%, and to detect aromatic amines formed by reductive cleavage of azo dyes in effluents when the recovery of amine was in the range 81-95% with RSD 8-15%. The method is not applicable to nitroanilines. (C) 2003 Elsevier B.V. All rights reserved.
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