Neutron diffraction and isotopic labeling have been used to determine the distribution of toluene sorbed into the interlamellar space of complexes of vermiculite with alkyl trimethylammonium bromide complex of alkyl chain lengths C-12, C-14, and C-16 and in a mixed C-12/C-16 complex. The toluene remains in a liquid-like form and fills and swells the interlamellar space space up to a point where there remains a small amount of overlap of the alkyl chains of the surfactant. If the complex is between vermiculite and one surfactant only this results in the toluene concentration being reduced in the center of the interlamellar space, with maxima on either side. On the other hand, in a complex of mixed-length surfactants, the toluene distribution reaches its maximum at the center of the interlamellar space. (C) 2003 Elsevier Inc. All rights reserved.