Herbicide wastewater is one of tne industrial wastewater, it has high salt content, poor biodegradability, biodegradable characteristics. Nitrogen-containing organic compounds are dominated in dissolved organic matter and dissolved organic matter of wastewater, BOD : COD= 0. 045, C : N : P= 692 : 426 : 1. Applying static headspace, purg and trap, solid-phase extraction, solid-phase microextraction and liquid-liquid extraction as pretreatment methods combined with gas chromatography/mass spectrometry (GC/MS), which qualitatively analyzed the organic components of the Atrazine, acetochlor herbicide production wastewater and researched the UV spectrum, three-dimensional fluorescence spectroscopy of the wastewater and its major pollutants. The study of GC/MS indicated that Wastewater contained chlorinated hydrocarbons, BTEX and triazines, amides herbicides etc. 38 kinds of volatile and semi-volatile organic compounds, atrazine and acetochlor herbicides accounted for 87. 99%. Affected monocyclic or heterocyclic substances, the ultraviolet absorption spectrum of the wastewater in 210 similar to 230 and 250 similar to 270 nm in that the amino group lead to the UV absorption red shift 20 nm. Wastewater generated 5 fluorescence peak in lambda(ex)/lambda(em) =200 similar to 280/300 similar to 400 nm, such as a(225/305 nm), b(265/365 nm), c(275/305 nm), d(285/390 nm) e(320/375 nm). Based on three-dimensional fluorescence results of the different functional groups of the characteristics organic, fluorescent area of unsaturated bond is in lambda(ex)/lambda(em) =215 similar to 230/290 similar to 340 nm, the main contribution of the fluorescent substance in the region were olefins, benzene, heterocyclic in the wastewater; fluorescent area of Phenolic hydroxyl and carbonyl is in lambda(ex)/lambda(em) =270/300 nm, the main contribution of the fluorescent substance in the region were phenols, ketones.
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