A method for the determination of nickel in industrial wastewater by atomic absorption spectrometry with carboxy lated carbon nanotubes as solid phase dispersion adsorption material was established.Based on the rapid adsorption of Ni ions in neutral environment and the rapid desorption of Ni ions under acidic conditions，the pretreatment method of sample enrich ment and purification based on carboxylated carbon nanotubes was established by optimizing the parameters.The samples after enrichment and purification were determined by atomic absorption spectrometry.Results showed that the linearity of the method was good in the range of 0.36~2.50 mg/L（R2=0.999 1）.The limit of detection was 0.11 mg/L and the limit of quantity was 0.36 mg/L.The recoveries were 97.4%~99.3% and the relative standard deviation（RSD） was 1.48%~1.97% at the concentrations of 0.5，1.5，2.5 mg/L.