X-ray Diffraction (XRD) spectra and thermogravimetric instruments can be used to analyze the changes in a copper phosphate compound before and after heating. The product synthesized in optimum condition has been subjected first to thermogravimetric analysis and the residue left over was used for X-ray diffraction confirms the presence of copper pyrophosphate in Argon and air as the two different environments at 600°C. The sample prepared from copper dihydrogen phosphate was studied through thermogravimetric analysis and the phases in which the compound existed were confirmed through X-ray diffraction. The copper phosphate compounds were studied by thermal analysis in two different environments, argon and air and on two different surfaces crucible and tungsten disc. Here the copper phosphate compounds decomposition behavior of the mixture and the resulting products were studied through pyrolysis when heated to high temperatures. X-ray diffraction was used to identify the phases formed during decomposition and to study any changes in the crystal structure. By observing the positions and intensities of the diffraction peaks in the spectrum, the crystal structure of the compound was determined along with the phases present. The diffraction pattern is novel to the crystal lattice arrangement, helping us in the identification of different crystalline phases around 100°C-150°C to be orthophosphate and at second transition temperature 200°C-600°C there is the formation of copper pyrophosphate. The diffraction pattern is unique to the crystal lattice arrangement, in this journal I have accurately determined the crystal structure at 600°C for different concentration of copper phosphate compounds to be reported to be copper pyrophosphate at 600°C on different substrate of Tungsten and crucible however the sample prepared of copper phosphate compound before heating was quite ambiguous.