Compositions containing biologically active molecules encapsulated in self-assembling, diketopiperazine microspheres (TECHNOSPHEREs) and methods for making and administering such compositions are described herein. The compositions can be used to immunize individuals against agents of biological warfare. The biologically active molecules include atropine, antibodies, antigens, and antibiotics. The compositions can be placed in an inhalation device for self-administration. Pulmonary delivery of TECHNOSPHERE encapsulated atropine, antibodies, vaccines, and antibiotics provides an accelerated onset of immunity to the targeted disease. Furthermore, the TECHNOSPHERE encapsulated atropine, antibodies, vaccines, and antibiotics are stable formulations, suitable for stockpiling, rapid dissemination and mass treatment.