Dealuminated zeolite samples prepared by different methods are characterized by different techniques, and the structural and acidic characteristics are investigated in an effort to identify the parameters that decide their structural and acidic characteristics. The investigation gave evidence that the structure breakdown of the parent type-Y zeolite is mainly dependent on the degree of dealumination, but the nature of extraframework aluminum (EFAl) species formed is dependent on the type of dealumination procedure. Monomeric Al species and oligomeric Si,Al species were formed by steam treatment at relatively low and high temperatures, respectively. Aluminosilicate phases of Si/Al ratios 2.0−4.0 and 8.0 were found in SiCl4-treated and ammonium hexafluorosilicate (AHFS)-treated samples, respectively. EFAl species of octahedral and tetrahedral coordination were observed by NMR spectra in steam and SiCl4-treated samples. High degrees of dealumination within each type of treatment resulted in loss of microporosity of the crystalline material, but the increase of mesoporous and/or macroporous structure was dependent on the type of dealumination. The increase of macroporous structure was the result of crystallite agglomerates formed during the procedure. The number of acid sites determined by the ammonia temperature-programmed desorption method, under appropriate experimental conditions, matched with the FAl content of the dealuminated H−Y samples that do not contain a significant amount of EFAl species. The loss of strong acid sites with the degree of dealumination is evidenced to be dependent on the method of dealumination. Dealumination by AHFS up to ca. 50% does not affect the number of strong acid sites considerably, in contrast to the weak/medium acid sites which decrease almost linearly with a FAl decrease. At higher degrees of dealumination achieved by steaming or SiCl4-treatment, both weak/medium and strong acid sites decrease steeply with FAl decrease. There is evidence that the produced EFAl-species by the different methods have different acidic properties and result in low stoichiometries of adsorbing ammonia probe molecules. The EFAl species produced by the SiCl4 method result in more acidic H−Y zeolite catalysts compared to the high-temperature steamed samples.

The phase separation of lamellar vesicles of anionic surfactants in aqueous solutions and its application as a novel liquid coacervate extraction procedure was examined. Solutions of lauric acid sodium salt separate into two phases in the presence of alkaline earth metals and a water miscible cosurfactant. It is proven that the surfactant phase is built of a perplexed network of multilamellar vesicles consisting of densely packed bilayers. Several factors affecting the formation of this new phase as well as its analytical utility in the preconcentration of metallic ions were assessed on the basis of better exploitation of this new nonspecific extraction technique. In essence, although the procedure to arrive at the optimum conditions seems laborious, the delivered method is straightforward, alleviating the requirement for prereaction with a complexing agent and highly reproducible under the optimum experimental conditions. As an analytical demonstration, the method was successfully applied to the determination of Cd(2+) and Zn(2+) in natural waters. Recoveries were higher than 95%, and detection limits as low as 3 microg L(-)(1) were accomplished by preconcentrating only 10 mL of sample volume in the presence of 0.45% (w/v) anionic surfactant.

A detailed study of the conventional hydrothermal synthesis of zeolites in aqueous sodium alkaline solutions without the use of templates or organic bases is presented. Gel compositions representing most areas of the silica-rich half-triangle of the crystallization field that yield openstructure zeolites were prepared and were crystallized under different conditions in a design of a factorial experiment. The synthesized products were examined for their crystal structure and their Si/Al ratio. The data prove that the gel-alkalinity factor (a) increases the rate of crystallization to a point but further increase reveals a decrease of the phase transformation rate, thus stabilizing metastable structures, and (b) decreases the Si/Al ratio of the zeolitic framework. The increase of the gel-aluminicity (a) generates new crystalline structures that grow simultaneously with those that are formed in low-aluminicity gels and (b) decreases the slope of the framework Si/Al ratio versus alkalinity. An increase of crystallization temperature produces structures that are more dense and stable. Structure stability sequences were established in experiments performed at relatively high gel alkalinity and aluminicity.