Hydrocalumite (CaAl-LDH-Cl) was synthesized through a rehydration method involving a freshly prepared tricalcium aluminate (C(3)A) with CaCl2 solution. To understand the intercalation behavior of sodium dodecylsulfate (SDS) with CaAl-LDH-Cl, X-ray diffraction (XRD), Fourier transform infrared (FTIR), scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma-atomic emission spectrometer (ICP), and elemental analysis have been undertaken. The sorption isotherms with SDS reveal that the maximum sorption amount of SDS by CaAl-LDH-CI could reach 3.67 mmol g(-1). The results revealed that CaAl-LDH-CI holds a self-dissolution property, about 20-30% of which is dissolved. And the dissolved Ca2+ and Al3+ ions are combined with SDS to form CaAl-SDS or Ca-SDS precipitation. It has been highlighted that the composition of resulting products is strongly dependent upon the SDS concentration. With increasing SDS concentrations, the main resulting product changes from CaAl-SDS to Ca-SDS, and the value of interlayer spacing increased to 3.27 nm. (C) 2011 Elsevier Inc. All rights reserved.