Process control and optimization of bitumen froth treatment during oil sands processing require rapid analysis of asphaltene content in bitumen, solvent-to-bitumen ratio (S/B), and the density of solvent-diluted bitumen. NIR spectroscopy was employed to meet this requirement. The NIR system comprised a spectrometer with no moving parts coupled with a double-pass transflectance probe via a fiber-optic cable. Quantitative calibration models were established using partial least-squares regression in latent variables. The standard errors of calibration were 0.20 wt% for 0 to 20 wt% asphaltenes in bitumen, 1.1 wt% for 20 to 100 wt% asphaltenes in bitumen, 0.1 for S/B of solvent-diluted bitumen, and 0.0017 g/mL for density of solvent-diluted bitumen. It was shown that the process conditions could be monitored through the spectral scores from principal component analysis.