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Abstract  

The thermal decomposition of natural iowaite of formula Mg6Fe2(Cl,(CO3)0.5)(OH)16·4H2O was studied by using a combination of thermogravimetry and evolved gas mass spectrometry. Thermal decomposition occurs over a number of mass loss steps at 60°C attributed to dehydration, 266 and 308°C assigned to dehydroxylation of ferric ions, at 551°C attributed to decarbonation and dehydroxylation, and 644, 703 and 761°C attributed to further dehydroxylation. The mass spectrum of carbon dioxide exhibits a maximum at 523°C. The use of TG coupled to MS shows the complexity of the thermal decomposition of iowaite.

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Abstract  

Thermogravimetric and differential thermogravimetric analysis has been used to characterize alunite of formula [K2(Al3+)6(SO4)4(OH)12]. Thermal decomposition occurs in a series of steps (a) dehydration up to 225°C, (b) well defined dehydroxylation at 520°C and desulphation which takes place as a series of steps at 649, 685 and 744°C. The alunite minerals were further characterized by infrared emission spectroscopy (IES). Well defined hydroxyl stretching bands at around 3463 and 3449 cm−1 are observed. At 550°C all intensity in these bands is lost in harmony with the thermal analysis results. OH stretching bands give calculated hydrogen bond distances of 2.90 and 2.84–7 Å. These hydrogen bond distances increase with increasing temperature. Characteristic (SO4)2− stretching modes are observed at 1029.5, 1086 and 1170 cm−1. These bands shift to lower wavenumbers on thermal treatment. The intensity in these bands is lost by 550°C.

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Thermogravimetric analysis of synthetic smithsonite and hydrozincite, two secondary minerals of zinc, was used to determine their relative thermal stability. Thermal decomposition of smithsonite occurs at 293°C and hydrozincite at 220°C showing that the carbonate mineral is more stable than the hydroxy-carbonate mineral hydrozincite. Hot stage Raman spectroscopy confirms the decomposition of smithsonite and hydrozincite by 300 and 250°C, respectively. Thermogravimetry shows that a small amount of hydrozincite is formed during the synthesis of smithsonite. No evidence is found for the separate loss of the carbonate and hydroxyl units from hydrozincite.

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Abstract  

Synthetic Fe—Mn alkoxide of glycerol samples are submitted to controlled heating conditions and examined by IR absorption spectroscopy. On the other hand, the same sample is studied by infrared emission spectroscopy (IRES), upon heating in situ from 100 to 600°C. The spectral techniques employed in this contribution, especially IRES, show that as a result of the thermal treatments ferromagnetic oxides (manganese ferrite) are formed between 350 and 400°C. Some further spectral changes are seen at higher temperatures.

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Abstract  

Evidence for the existence of primitive life forms such as lichens and fungi can be based upon the formation of oxalates. These oxalates form as a film like deposit on rocks and other host matrices. Humboldtine as the natural iron(II) oxalate mineral is a classic example. Thermogravimetry coupled to evolved gas mass spectrometry shows dehydration takes place in two steps at 130 and 141°C. Loss of the oxalate as carbon dioxide occurs at 312 and 332°C. Dehydration is readily followed by Raman microscopy in combination with a thermal stage and is observed by the loss of intensity of the OH stretching vibration at 3318 cm-1. The application of infrared emission spectroscopy supports the results of the TG-MS. Three Raman bands are observed at 1470, 1465 and 1432 cm-1 attributed the CO symmetric stretching mode. The observation of the three bands supports the concept of multiple iron(II) oxalate phases. The significance of this work rests with the ability of Raman spectroscopy to identify iron(II) oxalate which often occurs as a film on a host rock.

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Abstract  

A combination of high resolution thermogravimetric analysis coupled to a gas evolution mass spectrometer has been used to study the thermal decomposition of synthetic hydrotalcites reevesite (Ni6Fe2(CO3)(OH)164H2O) and pyroaurite (Mg6Fe2(SO4,CO3)(OH)164H2O) and the cationic mixtures of the two minerals. XRD patterns show the hydrotalcites are layered structures with interspacing distances of around 8.0. . A linear relationship is observed for the d(001) spacing as Ni is replaced by Mg in the progression from reevesite to pyroaurite. The significance of this result means the interlayer spacing in these hydrotalcites is cation dependent. High resolution thermal analysis shows the decomposition takes place in 3 steps. A mechanism for the thermal decomposition is proposed based upon the loss of water, hydroxyl units, oxygen and carbon dioxide.

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Abstract  

The concentration of As, Ba, Ca, Co, Cr, Cs, Dy, Eu, Fe, Ga, Hf, K, La, Lu, Mn, Mo, Na, Ni, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, U, Yb, and Zn were determined by instrumental neutron activation analysis in block shale samples of the New Albany Group (Devonian-Mississippian) in the in the Illinois Basin. Uranium content of the samples was as high as 75 ppm and interfered in the determination of samarium, molybdenum, barium and cerium. In the determination of selenium a correction was made for interference from tantalum. U, As, Co, Mo, Ni and Sb as well as Cu, V and pyritic sulphur which were determined by other methods, were found to correlate positively with the organic carbon content of the samples.

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Abstract  

The precursors of carbonate minerals have the potential to react with greenhouse gases to form many common carbonate minerals. The carbonate bearing minerals, magnesite, calcite, strontianite and witherite, were synthesised and analysed using a combination of thermogravimetry and evolved gas mass spectrometry. The DTG curves show that as both the mass and the size of the metal cationic radii increase, the inherent thermal stability of the carbonate also increases dramatically. It is proposed that this inherent effect is a size stabilisation relationship between that of the carbonate and the metal cation. As the cationic radius increases in size, the radius approaches and in the case of Sr2+ and Ba2+ exceeds that of the overall size of the carbonate anion. The thermal stability of these minerals has implications for the geosequestration of greenhouse gases. The carbonates with the larger cations show significantly greater stability.

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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  

Evidence for the existence of primitive life forms such as lichens and fungi can be based upon the formation of oxalates. These oxalates form as a film like deposit on rocks and other host matrices. The anhydrous oxalate mineral moolooite CuC2O4 as the natural copper(II) oxalate mineral is a classic example. Another example of a natural oxalate is the mineral wheatleyite Na2Cu2+(C2O4)2·2H2O. High resolution thermogravimetry coupled to evolved gas mass spectrometry shows decomposition of wheatleyite at 255°C. Two higher temperature mass losses are observed at 324 and 349°C. Higher temperature mass losses are observed at 819, 833 and 857°C. These mass losses as confirmed by mass spectrometry are attributed to the decomposition of tennerite CuO. In comparison the thermal decomposition of moolooite takes place at 260°C. Evolved gas mass spectrometry for moolooite shows the gas lost at this temperature is carbon dioxide. No water evolution was observed, thus indicating the moolooite is the anhydrous copper(II) oxalate as compared to the synthetic compound which is the dihydrate.

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