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The use of thermo-XRD-analysis in the study of organo-smectite complexes
Robert Mackenzie memorial lecture
Summary Thermo-XRD-analysis is applied to identify whether or not the adsorbed organic species penetrates into the interlayer space of the smectites mineral. In this technique an oriented smectite sample is gradually heated to temperatures above the irreversible dehydration of the clay, and after each thermal treatment is diffracted by X-ray at ambient conditions. In the thermal treatment of organo-clays, under air atmosphere at temperatures above 250°C, the organic matter is in part oxidized and charcoal is formed from the organic carbon. In inert atmosphere e.g. under vacuum above 250°C the organic matter is pyrolyzed and besides small molecules, charcoal is formed. If the adsorbed organic compound is located in the interlayer space, the charcoal is formed in that space, preventing the collapse of the clay. A basal spacing of above 1.12 nm suggests that during the adsorption the organic compound penetrated into the interlayer space. Thermo-XRD-analyses of montmorillonite complexes with anilines, fatty acids, alizarinate, protonated Congo red and of complexes of other smectites with acridine orange are described. To obtain information about spacings of the different tactoids that comprise the clay mixture, curve-fitting calculations on the X-ray diffractograms were adapted.
Abstract
The mechanochemical solid-state adsorption of the cationic dye crystal violet (CV) by montmorillonite was investigated by XRD and simultaneous DTA-TG. Solid CV was ground with the clay for 5 min and four different varieties of CV mechanochemically treated clay were investigated. X-ray and DTA data were compared with those of CV-montmorillonite obtained from an aqueous suspension. X-ray and DTA studies of a ground mixture and a ground mixture heated at 110°C suggest that the mechanochemical adsorption of organic cations takes place on the external surfaces of the clay. The study of a ground mixture washed with water, and washed with water and acetone reveal that water is essential for the penetration of CV into the interlayer space.
Abstract
The mechanochemical solid-state adsorption of the cationic dye rhodamine-6G (R6G) by montmorillonite was investigated by XRD and simultaneous DTA-TG. Five different mixtures of R6G and montmorillonite were investigated. They contained 10, 20, 35, 50 and 100 mmol R6G per 100 g clay. The solid R6G was ground with the clay for five minutes. Mixtures were ground both in the absence of water (dry grinding) and with the adding of drops of water periodically, (wet grinding). There were no differences between samples obtained by wet or dry grinding. X-ray and DTA data were compared with those of R6G-montmorillonite obtained from aqueous suspensions. The mechanochemical products were different from those obtained from aqueous suspensions. The X-ray and DTA studies suggest that the mechanochemical adsorption of organic cations takes place on the external surfaces of the clay whereas in suspensions the adsorption takes place into the interlayer space. In the latter case the final stages of oxidation occur in temperatures higher than those of the neat dye whereas in the former they occur at lower temperatures.
Abstract
Montmorillonite and Laponite loaded with different amounts of tributylammonium cations (TBAH+), up to 40 and 30 mmol, respectively, per 100 g clay, were studied by thermo-XRD-analysis. TBAH-smectites heated at 300 and 420°C exhibited basal spacings of 1.30 and 1.24 nm, attributed to smectite tactoids with low- and high-temperature-stable monolayer charcoals, respectively in the interlayers. DTA-EGA and TG of the TBAH-smectites showed four stages of mass loss labeled A, B, C and D. Stage A below 250°C, accompanied by an endothermic DTA peak, resulted from the dehydration of the clay. Mass loss stages B, C and D, at 250–380, 380–605°C and above 605°C, respectively, accompanied by exothermic DTA peaks, were due to three oxidation steps of the organic matter. In mass loss stage B (first oxidation step) mainly organic hydrogen was oxidized to H2O whereas carbon and nitrogen formed low- and high-temperature-stable charcoals. In stages C and D (second and third oxidation steps) low- and high-temperature- stable charcoals were oxidized, respectively. Dehydroxylation of the smectites occurred together with the second and third oxidation steps. Thermal mass loss at each step was calculated from the TG curves showing that in montmorillonite the percentage of high-temperature-stable charcoal from total charcoal decreased with higher TBAH+ loadings of the clay whereas in Laponite this percentage increased with higher loadings of the clay.
Partially exchanged organophilic bentonites
Part I. characterization by thermal analysis on calcined mass basis
-009-0427-3 . 19. Yariv , S , Lapides , I 2005 The use of thermo-XRD-analysis in the study of organo-smectite complexes . J Therm Anal Calorim 80 : 11 – 26 10.1007/s10973-005-0608-7 . 20
– 128 . 24. Yariv , S , Lapides , I 2005 The use of thermo-XRD-analysis in the study of organo-smectite complexes . J Therm Anal Calorim 80 : 11 – 26 10.1007/s10973
Marcel Dekker New York 345 – 462 . 28. Yariv , S , Lapides , I 2005 The use of thermo-XRD-analysis in the study of organo-smectite complexes . J Therm Anal Calorim. 80 : 11 – 26 10
Thermal analysis of hexadecyltrimethylammonium-montmorillonites
Part 2. Thermo-XRD-spectroscopy-analysis
. Yariv , S , Lapides , I . The use of thermo-XRD-analysis in the study of organo-smectite complexes . J Therm Anal Calorim . 2005 ; 80 : 11 – 26 . 10.1007/s10973-005-0608-7 . 20
