We report the first demonstration of bipolar coding techniques in the optical spectral domain for incoherent optical code division multiple access (CDMA) communication. Based on the modulation and detection principles that we have developed, the power spectrum of an erbium-doped superfluorescent fiber source was encoded using bipolar codes and decoded using an optical bipolar correlator. A CDMA testbed consisting of two encoders and one decoder was implemented with bulk optics and free-space transmission. Our measurements verify the correlations between the bipolar codewords and demonstrate the rejection of multiple access interference.