Leaves and leaf slices from Aloe arborescens Mill. were used to study the interrelations between Crassulacean acid metabolism, photosynthesis, and respiration. Oxygen exchange of leaf slices was measured polarographically. It was found that the photosynthetic utilization of stored malic acid resulted in a net evolution of oxygen. This oxygen produetion, and the decrease in acid content of the leaf tissue, were completely inhibited by amytal, although the rate of respiratory oxygen uptake was hardly affected by the presence of this inhibitor of mitochondrial electron transport. Other poisons of respiration (cyanide) and of the tricarboxylic acid cycle (trifluoroacetate, 2-diethyl malonate) also were effective in preventing aciddependent oxygen evolution. It is concluded that the mobilization of stored acids during light-dependent deacidification of the leaves depends on the operation of the tricarboxylic acid cycle and of the electron transport of the mitochondria.A mits a closure of the stomata during the hot daytime by making CO, available for photosynthesis from the endogenous acid pools (24).Many striking resemblances exist between the mechanism of CO. assimilation in CAM and that in the C-dicarboxylic acid pathway of CO, fixation which is characterized by the appearance of labeled dicarboxylic acids as first stable products of the photosynthetic assimilation of 'CO2. Many data and concepts have recently been published on the physiological differences which separate C-plants from plants with the "classical" Calvin-Benson pathway of CO2 fixation (C,-plants). Investigations on CAM, however, have been few. This situation is reflected in Hatch and Slack's (13) review on the mechanisms of CO2 assimilation. The photosynthetic use of CO2 from stored malate in chlorophyllous tissue with CAM should be reflected in a light-dependent net evolution of oxygen even in the absence of external CO,. It was the aim of this work to devise a rapid and reproducible method for the measurement of 02 exchange in such tissue under various conditions. This approach was hoped to permit an analysis of the physiological conditions regulating the storage and photosynthetic utilization of CO2 in plants with CAM.The use of intact leaves was not desirable because their gas exchange is influenced by the activity of the stomata and by the diffusion of gases through the bulky tissue. Sectioning of the leaf would lessen, or eliminate, such problems and facilitate the entry of added inhibitors and other substances. Bruinsma (6) had observed, however, that CAM was adversely affected when Bryophyllum leaves were sliced. This appeared to have been due to actions of leached tannins and other phenolic compounds. Therefore, we had to find a plant which was relatively free of such potentially inhibitory compounds. This criterium eliminated nearly all plants which had been used by other investigators in the past, e.g., from the genera Bryophyllum, Sedum, and Kalanchoe. Leaves from Aloe arborescens Mill. (Liliaceae), however, had a very low conten...