The Indian Environmental Protection Act (EPA) came into force in 1986 after Bhopal Gas Tragedy. It stipulates that no person or industry or processor shall discharge or emit environmental pollutants in excess of prescribed standards. Dihydroxyl ammonium 5,5-bistetrazole-1,1-diolate, abbreviated as TKX-50, was synthesized in this laboratory. During synthesis of TKX-50 a large volume of effluent was generated, which was acidic and hazardous in nature and therefore can damage the environment if discharged without proper treatment. Literature survey reveals that TKX-50 effluent analysis and its treatment have not been reported so far. In order to meet EPA norms and protect the environment TKX effluent samples of different steps of synthesis were collected and analyzed for environmental parameters such as pH, chemical oxygen demand (COD), bio-chemical oxygen demand (BOD), total dissolved solids (TDS) and bioassay test (toxicity to zebra fish survival) followed by the treatment of composite effluent. This paper presents analysis results of TKX-50 effluent samples before and after treatment. The results of finally treated TKX-50 effluent indicate that the same can be safely discharged on land for irrigation without adverse effect on environment. This study may be suitable for environmentalists and community of high energy materials.