An attempt has been made to extract the anodic diffusion layer using the Freezing Technique. The method gives a good estimae of concentration profile. The anode material used was copper and a mixture of 10% NaC1+10% v/v HCl was used as electrolyte. Composition of anodic layer was found to contain CuCI, 6H0. The results compare well with the previous results of porous electrode technique, the method no doubt has the advantage giving a good estimate of concentration profile but suffers from poor adhesion frosting and slicing conditions.