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While wandering in the jungle at Nagandi in Africa, Jungle Jim bravely but unsuccessfully tries to rescue a native from an attacking leopard. From the clutched hand of the dead man, Jim retrieves a small golden vial, which he takes to Godfrey Marsden, the district commissioner. Marsden sends the vial to the Archaeology Department and discovers that it came from the temple at Zimbalu, the lost burial place of the ancient kings. Soon after, government scientist Hilary Parker arrives to head an expedition to search for the lost temple, and hires Jim as their guide. Intrigued by promises of hidden treasure, photographer Bruce Edwards decides to follow them. Impatient to get underway, Hilary identifies the gummy substance found in the vial as a poison that can cure polio. Jim then informs Hilary that the poison is used by witch doctors known as "devil doctors" to paralyze their foes, and warns her that the devil doctors may have usurped the temple. As they begin their trek through the jungle, retracing the steps of the dead native, Hilary and Jim are joined by Kolu, Jim's faithful native friend and his seductive sister Zia. When the expedition is dogged by a series of uncanny accidents, Jim becomes suspicious and decides to set booby traps to awaken the camp in case of an intruder. That night, Edwards falls into one of the traps and claims that he is lost in the jungle. Against Jim's better judgment, Hilary agrees to let Edwards accompany them as the expedition's photographer. As they round a treacherous mountain trail, Edwards pretends to faint, falling into Jim and pushing him over the edge of a cliff. Acting swiftly, Kolu lowers himself over the cliff and pulls Jim to safety. Upon nearing the temple, the expedition is attacked by the devil doctors of Zimbalu. While running to escape their pursuers, Kolu stumbles into a pit containing a ferocious lion. Jim climbs into the pit to rescue his friend, while Hilary, Zia and the others are taken captive by the devil doctors. After killing the lion, Jim sneaks into the temple and finds the devil doctors preparing to kill their prisoners. Edwards, who has ingratiated himself with the devil doctors by taking their photographs, stuffs his pack with golden treasure. When he is deprived of his "magic powers" after Jim's pet hawk plucks the lens out of his camera, Edwards becomes the object of the devil doctors' fury. In the chaos, Jim liberates his friends and together, they overpower the devil doctors. While greedily trying to seize the treasure, Edwards plunges to his death into a pit of fire. His mission completed, Jim invites Hilary to join him for further adventures.