In this study a series of thermosetting acrylic polymer light conduits (PLCs) with the composition of A(x)B(y)C(z) were synthesized to investigate the structure-property relationships. The A and B components were selected from methyl methacrylate (MMA), butyl acrylate (BA), or 2,2,3,3-tetrafluoropropyl methacrylate (TFPMA). Various bifunctional acrylics were used for the C component. High numerical aperture values were found in the prepared large-diameter PLCs. The peak maxima of the optical loss spectra vary from 735 nm to 145 nmr which satisfactorily agree with the theoretical calculation from the FTIR spectra. They are due to the fifth harmonic of the C-H stretching vibration band. The peak maximum and intensity can be adjusted by varying molecular composition. The peak intensity of the optical loss spectrum is proportional to the C-H bond density of the polymer core. The replacement of the MMA moiety by the TFPMA. moiety in the three-component thermosetting PLCs reduces the peak intensity.