In order to decompose and transform the toxic refractory typical pollutants from Acrylonitrile-Butadiene-Styrene (ABS) resin wastewater and improve the biodegradability of the wastewater, the wastewater was pretreated by the ferric-carbon micro-electrolysis. The decomposition and transformation of the aromatic pollutants from ABS wastewater was detected rapidly by three-dimensional fluorescence spectra technology. The results showed that under the condition of influent pH 4.0, the removal efficiency of COD
Cr and total fluorescence intensity was 53.27% and 73.45%, respectively, after 30 days of continuous and stable run of mico-electrolysis. The removal efficiency of COD
Cr was affected directly by the influent pH. The COD
Cr removal efficiency of three micro-electrolysis reactors with different influent pH in sequence was as follows: pH=4.0>pH=6.0>pH=8.0. However, the removal efficiency of total fluorescence intensity did not comply with this law. The removal efficiency of total fluorescence intensity was all between 73.45% and 74.88% with different influent pH. In other words, the effect of influent pH on the degradation or transformation of aromatics by the ferric-carbon micro-electrolysis reactors was small.