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Abstract  

Bayer hydrotalcites prepared using the seawater neutralisation (SWN) process of Bayer liquors are characterised using X-ray diffraction and thermal analysis techniques. The Bayer hydrotalcites are synthesised at four different temperatures (0, 25, 55, and 75 °C) to determine the effect of synthesis temperature on the thermal stability of the Bayer hydrotalcite structures and the mineralogical phases that form. The interlayer distance increased with increasing synthesis temperature, up to 55 °C, and then decreased by 0.14 Å for Bayer hydrotalcites prepared at 75 °C. The three mineralogical phases identified in this investigation are; (1) Bayer hydrotalcite, (2), calcium carbonate species, and (3) hydromagnesite. The DTG curve can be separated into four decomposition steps; (1) the removal of adsorbed water and free interlayer water in hydrotalcite (30–230 °C), (2) the dehydroxylation of hydrotalcite and the decarbonation of hydrotalcite (250–400 °C), (3) the decarbonation of hydromagnesite (400–550 °C), and (4) the decarbonation of aragonite (550–650 °C).

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Abstract  

Insight into the unique structure of layered double hydroxides (LDHs) has been obtained using a combination of X-ray diffraction and thermal analysis. Indium containing hydrotalcites of formula Mg4In2(CO3)(OH)12·4H2O (2:1 In-LDH) through to Mg8In2(CO3)(OH)18·4H2O (4:1 In-LDH) with variation in the Mg:In ratio have been successfully synthesised. The d(003) spacing varied from 7.83 Å for the 2:1 LDH to 8.15 Å for the 3:1 indium containing LDH. Distinct mass loss steps attributed to dehydration, dehydroxylation and decarbonation are observed for the indium containing hydrotalcite. Dehydration occurs over the temperature range ambient to 205 °C. Dehydroxylation takes place in a series of steps over the 238–277 °C temperature range. Decarbonation occurs between 763 and 795 °C. The dehydroxylation and decarbonation steps depend upon the Mg:In ratio. The formation of indium containing hydrotalcites and their thermal activation provides a method for the synthesis of indium oxide-based catalysts.

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Abstract  

The hydrotalcite based upon manganese known as charmarite Mn4Al2(OH)12CO3·3H2O has been synthesised with different Mn/Al ratios from 4:1 to 2:1. Impurities of manganese oxide, rhodochrosite and bayerite at low concentrations were also produced during the synthesis. The thermal stability of charmarite was investigated using thermogravimetry. The manganese hydrotalcite decomposed in stages with mass loss steps at 211, 305 and 793 °C. The product of the thermal decomposition was amorphous material mixed with manganese oxide. A comparison is made with the thermal decomposition of the Mg/Al hydrotalcite. It is concluded that the synthetic charmarite is slightly less stable than hydrotalcite.

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Abstract  

Hydrotalcites based upon gallium as a replacement for aluminium in hydrotalcite over a Mg/Al ratio of 2:1 to 4:1 were synthesised. The d(003) spacing varied from 7.83 Å for the 2:1 hydrotalcite to 8.15 Å for the 3:1 gallium containing hydrotalcite. A comparison is made with the Mg/Al hydrotalcite in which the d(003) spacing for the Mg/Al hydrotalcite varied from 7.62 Å for the 2:1 Mg hydrotalcite to 7.98 Å for the 4:1 hydrotalcite. The thermal stability of the gallium containing hydrotalcite was determined using thermogravimetric analysis. Four mass loss steps at 77, 263–280, 485 and 828 °C with mass losses of 10.23, 21.55, 5.20 and 7.58% are attributed to dehydration, dehydroxylation and decarbonation. The thermal stability of the gallium containing hydrotalcite is slightly less than the aluminium hydrotalcite.

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Thermal stability of stercorite H(NH4)Na(PO4)·4H2O

A cave mineral from Petrogale Cave, Madura, Eucla, Western Australia

Journal of Thermal Analysis and Calorimetry
Authors: Ray L. Frost and Sara J. Palmer

Abstract

Thermogravimetric analysis has been used to determine the thermal stability of the mineral stercorite H(NH4)Na(PO4)·4H2O. The mineral stercorite originated from the Petrogale Cave, Madura, Eucla, Western Australia. This cave is one of many caves in the Nullarbor Plain in the South of Western Australia. The mineral is formed by the reaction of bat guano chemicals on calcite substrates. Upon thermal treatment the mineral shows a strong decomposition at 191 °C with loss of water and ammonia. Other mass loss steps are observed at 158, 317 and 477 °C. Ion current curves indicate a gain of CO2 at higher temperature and are attributed to the thermal decomposition of calcite impurity.

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Abstract  

Thermal analysis complimented with evolved gas mass spectrometry has been applied to hydrotalcites containing carbonate prepared by coprecipitation and with varying divalent/trivalent cation ratios. The resulting materials were characterised by XRD, and TG/DTG to determine the stability of the hydrotalcites synthesised. Hydrotalcites of formula Mg4(Fe,Al)2(OH)12(CO3)·4H2O, Mg6(Fe,Al)2(OH)16(CO3)·5H2O, and Mg8(Fe,Al)2(OH)20(CO3)·8H2O were formed by intercalation with the carbonate anion as a function of the divalent/trivalent cationic ratio. XRD showed slight variations in the d-spacing between the hydrotalcites. The thermal decomposition of carbonate hydrotalcites consists of two decomposition steps between 300 and 400°C, attributed to the simultaneous dehydroxylation and decarbonation of the hydrotalcite lattice. Water loss ascribed to dehydroxylation occurs in two decomposition steps, where the first step is due to the partial dehydroxylation of the lattice, while the second step is due to the loss of water interacting with the interlayer anions. Dehydroxylation results in the collapse of the hydrotalcite structure to that of its corresponding metal oxides and spinels, including MgO, MgAl2O4, and MgFeAlO4.

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Abstract  

Hydrotalcites containing carbonate, vanadate and molybdate were prepared by coprecipitation. The resulting materials were characterized by XRD, and TG/DTA to determine the stability of the hydrotalcites synthesized. The thermal decomposition of carbonate hydrotalcites consist of two decomposition steps between 300 and 400°C, attributed to the simultaneous dehydroxylation and decarbonation of the hydrotalcite lattice. Water loss ascribed to dehydroxylation occurs in two decomposition steps, where the first step is due to the partial dehydroxylation of the lattice, while the second step is due to the loss of water interacting with the interlayer anions. Dehydroxylation results in the collapse of the hydrotalcite structure to that of its corresponding metal oxides, including MgO, Al2O3, MgAl2O4, NaMg4(VO4)3 and Na2Mg4(MoO4)5. The presence of oxy-anions proved to be beneficial in the stability of the hydrotalcite structure, shown by the delay in dehydroxylation of oxy-anion containing hydrotalcites compared to the carbonate hydrotalcite. This is due to the substantial amount of hydroxyl groups involved in a network of hydrogen bonds involving the intercalated anions. Therefore, the stability of the hydrotalcite structure appears to be dependent on the type of anion present in the interlayer. The order of thermal stability for the synthesized hydrotalcites in this study is Syn-HT-V>Syn-HT-Mo> Syn-HT-CO3-V>Syn-HT-CO3-Mo>Syn-HT-CO3. Carbonate containing hydrotalcites prove to be less stable than oxy-anion only hydrotalcites.

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Abstract  

The mineral reevesite and the cobalt substituted reevesite have been synthesised and studied by thermal analysis and X-ray diffraction. The d(003) spacings of the minerals ranged from 7.54 to 7.95 Å. The maximum d(003) value occurred at around Ni:Co 0.4:0.6. This maximum in interlayer distance is proposed to be due to a greater number of carbonate anions and water molecules intercalated into the structure. This increase in carbonate anion content is attributed to an increase in surface charge on the brucite like layers. The maximum temperature of the reevesite decomposition occurs for the unsubstituted reevesite at around 220 °C. The effect of cobalt substitution results in a decrease in thermal stability of the reevesites. Four thermal decomposition steps are observed and are attributed to dehydration, dehydroxylation and decarbonation, decomposition of the formed carbonate and oxygen loss at ~807 °C. A mechanism for the thermal decomposition of the reevesite and the cobalt substituted reevesite is proposed.

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Abstract  

Dynamic and controlled rate thermal analysis has been used to characterise synthesised jarosites of formula [M(Fe)3(SO4)2(OH)6] where M is Pb, Ag or Pb–Ag mixtures. Thermal decomposition occurs in a series of steps. (a) dehydration, (b) well defined dehydroxylation and (c) desulphation. CRTA offers a better resolution and a more detailed interpretation of water formation processes via approaching equilibrium conditions of decomposition through the elimination of the slow transfer of heat to the sample as a controlling parameter on the process of decomposition. Constant-rate decomposition processes of water formation reveal the subtle nature of dehydration and dehydroxylation. CRTA offers a better resolution and a more detailed interpretation of the decomposition processes via approaching equilibrium conditions of decomposition through the elimination of the slow transfer of heat to the sample as a controlling parameter on the process of decomposition. Constant-rate decomposition processes of non-isothermal nature reveal separation of the dehydroxylation steps, since in these cases a higher energy (higher temperature) is needed to drive out gaseous decomposition products through a decreasing space at a constant, pre-set rate.

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Abstract  

Dynamic and controlled rate thermal analysis (CRTA) has been used to characterise alunites of formula [M(Al)3(SO4)2(OH)6] where M+ is the cations K+, Na+ or NH4 +. Thermal decomposition occurs in a series of steps: (a) dehydration, (b) well-defined dehydroxylation and (c) desulphation. CRTA offers a better resolution and a more detailed interpretation of water formation processes via approaching equilibrium conditions of decomposition through the elimination of the slow transfer of heat to the sample as a controlling parameter on the process of decomposition. Constant-rate decomposition processes of water formation reveal the subtle nature of dehydration and dehydroxylation.

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