In-line flocculation of oil sands tailings is a technique widely used in the oil sands industry to dewater fluid fine tailings. In this method, flocculants are added to the tailings to aggregate the fine particles and increase the settling rate and dewatering performance. Among the factors controlling the flocculation performance, the flocculant dose, rate and time of mixing play a crucial role. Consequently, the development of techniques that can monitor flocculation and provide feedback information to adjust flocculant dose and mixing conditions is of significant interest to the oil sands industry. This paper examines how hyperspectral imagery can be used to monitor tailings flocculation through post-depositional spectral measurements and image analysis. The results show that hyperspectral imagery can detect under-dosed and over-sheared samples, but experiments over a wider range of flocculation conditions are required to validate the results and calibrate the method. This study represents the initial step in the development of a spectral method for monitoring and assessment of the flocculation process.