This paper describes the development and operation of an autonomous robotic system designed for pyroprocess automation. The unique challenges of pyroprocess automation, such as the need for a highly dry atmosphere to handle materials like chloride, are addressed through this system. For the experiments, a specialized dehumidifier and dry mock-up facility were designed to produce dry air condition. Performances of dry air conditioning for the various simulated situations were evaluated, including assessing worker access within a mock-up to determine the system’s feasibility. To enable automation, containers used for processing materials were modified to fit the gripper system of the gantry robot. The loading and unloading of materials in each equipment were automated to connect them with the robotic system. This gantry robot primarily utilized macro motions to approach waypoints containing process materials, reducing the need for precise approach motions. Its tapered jaw design allowed it to grip target objects even with imperfect positioning. The robot’s motions were programmed initially using a robot simulator for positioning and motion planning, and real-world accuracy was tested in a dry mock-up facility using the OPC platform. Finally, the paper discusses the potential application of XR (eXtended Reality) technology in this context, which could enhance the robot’s operation and provide valuable insights into the automation process. Further analysis of XR technology’s feasibility and benefits for this specific pyroprocess automation system are presented.