Imaging tumoral pH may help characterize aggressiveness, metastasis, and therapeutic response. We report the development of hyperpolarized [2–13C,D10]diethylmalonic acid, which exhibits a large pH-dependent 13C chemical shift over the physiologic range. We demonstrate that co-polarization with [1–13C,D9]tert-butanol accurately measures pH via 13C NMR and magnetic resonance spectroscopic imaging in phantoms.