The major objective in this study was the preparation of polyacrylonitrile (PAN) nanofibers composed of 1,4-bis(o-cyanostyryl)benzene (ER) and 1-(o-cyanostyryl)-4-(p-cyanostyryl)benzene (EB), two kinds of fluorescent whitening agents widely used in the textile industry. The scanning electron microscopy images revealed that the diameters of ER/PAN and EB/PAN fibers ranged from 78 to 154 nm. The IR spectra indicated that the peaks of the -CN group blueshift and the generation of a shoulder peak were obviously due to the interaction between ER or EB and PAN. Furthermore, the UV spectra demonstrated that the distributive status of ER or EB tended toward the molecular state in PAN nanofibers. Finally, the most interesting finding in this study was that the photo luminescence intensity of EB/PAN nanofibers increased magnificently, whereas that of ER/PAN nanofibers decreased remarkably. (c) 2006 Wiley Periodicals, Inc.