The detection and quantification of alternate polymorphs of active pharmaceutical ingredients (APIs), particularly at low concentrations is a key issue for the manufacture and analysis of solid-state formulations. Each polymorph can possess unique physical and chemical properties which in turn can directly affect factors such as solubility and bioavailability. Near infra-red (NIR) and Raman spectroscopies can be used for the rapid characterisation and quantification of polymorphs in solid samples. In this study we have generated a model tablet system with two excipients and a 10% API concentration, where the API is a mixture of the FII and FII polymorphs of piracetam. Using transmission Raman spectroscopy (TRS) and NIR spectroscopy it was possible to detect FII polymorph contamination in these model tablets with limits of detection (LODs) of 0.6 and 0.7%, respectively, with respect to the total tablet weight (or similar to 6-7% of the API content). The IRS method is the superior method because of the speed of analysis (similar to 6s per sample), better sampling statistics, and because the sharper, more resolved bands in the Raman spectra allowed for easier interpretation of the spectral data. In addition the IRS used here provides facile access to the low frequency wavenumber region for analysis of solid-state lattice modes. (C) 2012 Elsevier B.V. All rights reserved.