Using various methods different tin phosphate samples were prepared. One of them was amorphous, while the others were crystalline with monoclinic structure, having unit cell parameters as follows: a=4.586Å, b=13.618Å, c=5.818Å, β=99.61° [Sn (H2PO4)2] and a=8.612Å, b=4.964Å, c=15.860Å, β=98.87° [Sn(HPO4)2], respectively. The crystal water content and the method of thermal decomposition of the samples were determined. The chemical composition of the end products of preparations was determined by promt-gamma activation analysis and was found to be Sn:P=1:2 for all samples independent of their preparation method. The oxidation state of tin atoms in samples as determined by Mossbauer spectroscopy was mainly +2 in sample no. 2, while in some other samples it was +4.