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This paper focuses on the implementation of various diagnostics for optimizing chemical oxygen iodine laser. This paper also dwells on the measurement methodologies and instrumentation employed in these diagnostic systems. The prime diagnostics are for the measurement of vital species in form of iodine, singlet oxygen, and chlorine. Iodine concentration measurement (absorption at λ = 499 nm ), chlorine utilization (absorption at λ = 330 nm), and singlet oxygen yield (emission at λ = 1.27 μm) have been implemented based on optical absorption/emission principle. Furthermore, online Mach number determination, which is critical for supersonic gas flows, laser pulse detection (at λ = 1315 nm ), and flow rate measurement and control over wide range, have been carried out. A dedicated diagnostics and data acquisition system (DDAS) customized for parameter monitoring have been developed. The developed DDAS also serves the purpose of precise operation sequencing and parameter control. It is a 168-channel personal-computer-based system with customized interface electronics employing Visual C++ programming language with user-friendly graphical user interfaces. A detailed uncertainty analysis of various critical parameters has been also presented.