In this report, we evaluate the metalorganic framework CuBTC as a real-world adsorbent for protection against three toxic hydride gases: ammonia, arsine, and hydrogen sulfide. We develop a scalable room-temperature synthesis of high-surface-area CuBTC using a benign ethanolwater solvent system. We test the capacity of CuBTC for the hydride gases under microbreakthrough and real-world packed-bed conditions at both low and high humidity conditions. Under microbreakthrough conditions, CuBTC outperforms a broad-spectrum carbon (BSC) adsorbent for uptake of ammonia and arsine, with approximately equivalent uptake of hydrogen sulfide. Under packed-bed conditions, CuBTC outperforms the BSC for ammonia uptake but offers little protection against arsine or hydrogen sulfide. We demonstrate the potential for CuBTC to act not only as an effective adsorbent for ammonia but also for sensing and to indicate saturation on the basis of colorimetric and fluorescence changes. We find that CuBTC is a suitable material for inclusion in respiratory protective devices for protection against ammonia, with potential benefits against other hydride gases.