Synthetic, relatively well-crystallized aluminum-substituted maghemite samples, γ-(Aly·Fe1−y)2O3, with y = 0, 0.032, 0.058, 0.084, 0.106 and 0.151 have been studied by X-ray diffraction and zero-field Mössbauer spectroscopy in the range 8 K to 475 K, and also with an external field of 60 kOe at 4.2 K and 275 K. It was found that there are two different converging models for fitting the zero-field spectra of the maghemites with a superposition of two Lorentzian-shaped sextets, both resulting in inconsistent values for the hyperfine fields (Hhf) and/or the center shifts (δ) of the tetrahedral (A) and octahedral (B) ferric ions. From the applied-field measurements it is concluded that there is a constant difference of 0.12 ± 0.01 mm/s between δB and δA, regardless of the Al content. For the Al-free sample the center shifts are found as: δA = 0.370 mm/s and δB = 0.491 mm/s at 4.2 K and δA = 0.233 mm/s and δB = 0.357 mm/s at 275 K (relative to metallic iron), with an estimated error of 0.005 mm/s. Both δA and δB are observed to decrease with increasing Al concentration. The effective hyperfine fields for the non-substituted maghemite sample are: Heff,A = 575 kOe and Heff,B = 471 kOe at 4.2 K and Heff,A = 562 kOe and Heff,B = 449 kOe at 275 K, with an error of 1 kOe. The B-site hyperfine field remains approximately constant with Al substitution, while for the A site a slight decrease with increasing Al content was observed.

A series of organo-montmorillonites and organo-hectorites was prepared by complete ion-exchange from the pure sodium form of the parent smectites. The organic cations were tetramethylammonium, trimethylated quaternary ammonium derivatives of the lysine and of the ornithine methyl esters, quaternarized polyammonium cations, or tetraphenylphosphonium (TPP). These organo-smectites were used as packing material for gas chromatography columns. Mixtures of light hydrocarbons (methane to n-butane; “C1” to “C4”) could be separated. The degree of separation depends on the presence of micropores or of organophilic mesopores. The BET surface area, the micropore and mesopore volumes, as well as the size distribution of micropores and mesopores were measured for several systems. As a general trend, the retention times of the light hydrocarbons decrease with an increase of the micropore volume. In the case of TPP-montmorillonite, characterized by a large mesopore volume but for which no microporosity could be detected, separation of longer linear hydrocarbons (n-pentane to n-octane) could also be achieved.

Ba-bearing clinoptilolite (with >2 wt. % BaO) occurs in Neogene marine siliceous sediments from ODP Leg 127 Site 795 in the Japan Sea. Ba-bearing clinoptilolite is formed by reaction of volcanic glass and Ba-rich pore water during burial diagenesis.

Pillared structures with an interlayer opening of ∼0.3 nm were obtained after successive heat treatments of the PILC precursor in reducing and oxidizing conditions. This precursor was prepared by reacting a Na+-montmorillonite with an intercalant containing Al and Fe oxo-hydroxides (Al/Fe = 1). Powder X-ray diffraction, elemental analysis, 57Fe Mössbauer spectroscopy, catalytic activity measurements and surface area data were used to characterize the samples. On the basis of Mössbauer spectra taken at temperatures between 4.2 and 300 K, it is deduced that oxidizing steps produce Al substituted maghemite which converts into Al substituted magnetite upon reducing heat treatment. Firing the precursor in oxidizing atmosphere forms pillars of few nm in diameter. However, heating under reducing conditions yields pillars of smaller diameter. This later behaviour is maintained even after reheating the material in oxidizing atmosphere. From the temperature dependence of Mössbauer spectra it is deduced that the diameter of the Fe oxide particles in the pillars is smaller than 10 nm.

A number of smectitic samples from Almeria (SE Spain) were studied by chemical analysis, DTA, TG, XRD (oriented aggregates with ethylene glycol treatment and Greene-Kelly test), FTIR and MAS NMR. Chemically they resembled a beidellite-montmorillonite series, displaying DTA/TG characteristics already quoted in the literature in beidellite descriptions. They did not swell after the Greene-Kelly test, as it has also been reported for some beidellites. Nevertheless XRD of the oriented, glycolated samples, FTIR, MAS NMR and revision of the chemical analysis demonstrated that they were mixed-layered kaolinite/montmorillonite. It is possible that some of the reported beidellites in the literature are kaolinite/montmorillonite. Beidellite characterization must be supported by several different techniques.