Quantitative NMR (qNMR) is a valuable analytical technique that is widely applied to simultaneously evaluate chemical identity and content in pharmaceutical research and development. Despite continuous advances in external calibration over the last two decades, adoption of these approaches has been slow. In fact, numerous qNMR procedures still rely on the use of internal reference materials. This presentation will summarize our efforts to design, develop, validate, and implement a robust methodology to perform volume-corrected, externally calibrated qNMR analysis. Applications of this methodology to support small-molecule drug discovery and development organizations at Genentech will be discussed.