Superabsorbent polymer (SAP) blend has been synthesized from Carboxymethyl Cellulose (CMC) , starch, and aluminum sulfate octadecahydrate cross-linker. Water Absorption Capacity (WAC), FTIR, SEM, DSC, CHO, Flame Photometer and ignition tests are carried out to determine the used CMC formula, investigate the cross-linking process, and suggest a cross-linking model. Flame Photometer results showed there are two sodium acetate groups in the CMC molecule. This result confirmed by theoretical calculations and CHO test . To investigate which of Al 3+ and SO 4 2-ions causes the crosslinking : the extraction of the cross-linked CMC/starch tested with BaCl 2 solution(showed dense white precipitate ; sulfate group not share for blend formation), NaOH solution( showed white precipitate of aluminum hydroxide; Al 3+ ion present (i.e. Al 3+ ion share in the blend structure). These results confirmed by flame test for sodium ion, which showed high Na emission energy (5.75); there is an exchange between Al and Na ions. To check that aluminum is a part of the structure, sample of the cross-linked CMC ignited. A white precipitate appear for aluminum oxide ,which confirms the presence of Al. Based on that there are three CMC molecules connected to each Al atom, theoretical calculations about the amount of Al in the cross-linked CMC molecule showed a good agreement with the CHO results (5.613% Vs. 5.739 % respectively). FTIR spectrum of the cross-linked CMC/starch blend showed that there is a reaction between CMC and starch molecules; i.e. the new repeating unit contains three starch molecules. This conclusion confirmed by theoretical calculations and results of EDX, CHO, and ignition tests. Al% in the new mer appeared a good agreement between theoretical calculations (4.32%) and CHO results (4.512%). Ignition test calculations confirmed that the new mer contains three Al atoms. Evidences of the occurrence of the cross-linking process were obtained from FTIR, morphology, DSC and absorbency results. Absence of the primary hydroxyl alcohol band in the CMC/starch blend spectrum, indicates that this site is active and the reaction between starch and CMC molecules occurs through it. Morphologies studies showed that the sample after crosslinking is more compact than before as well as show one piece for after cross-linking comparing with different pieces before cross-linking.Optimum cross-linking ratio appeared to be 2wt% corresponded to WAC equal to 58 g/g.in distilled water and DSC results indicates that CMC/starch is a miscible blend.