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Magnesium aluminate has high melting point, possesses capability to sustain the strength at extremely high temperatures and is highly resistant against chemical attacks which makes this material suitable as catalysts and catalyst support. It can be useful as thermal as well as electrical insulating materials in fusion reactors, for applications in solid state lasers and as capacitors in electronic devices and electromagnetic absorbers. Spinel magnesium aluminate has a tendency to incorporate a variety of metallic dopants which may alter its structural and electrical properties. The present study focuses on the synthesis of double doped transition metal magnesium aluminate samples. Co doping is carried out to achieve better optimization of electrical resistivity, dielectric constant and dielectric loss values in the samples thus making them suitable as insulators in fusion reactors, dielectric capacitors in electronic devices and for applications in electronic industries as insulators and electromagnetic radiation absorbers. Microwave method is employed for the synthesis and urea is used as a combustion aid.