The preparation of an alternative polycarboxylic acid to replace the most promising, but expensive, crosslinking reagent 1,2,3,4-butanetetracarboxylic acid (BTCA) is reported. The reaction of mercaptosuccinic acid with 2,4,6-trichloro-s-triazine (cyanuric chloride) gave a dithiosuccinyl derivative. The preparation reaction was followed using horizontal ATR infrared spectroscopy and capillary electrophoresis. The final product was characterized by FTIR, capillary electrophoresis, and H-1-NMR.