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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  

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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Abstract  

The thermal stability and thermal decomposition pathways for synthesized composite iowaite/woodallite have been determined using thermogravimetry analysis in conjunction with evolved gas mass spectrometry. Dehydration of the hydrotalcites occurred over a range of 56–70�C. The first dehydroxylation step occurred at around 255�C and, with the substitution of more iron(III) for chromium(III) this temperature increased to an upper limit of 312�C. This trend was observed throughout all decomposition steps. The release of carbonate ions as carbon dioxide gas initialised at just above 300�C and was always accompanied by loss of hydroxyl units as water molecules. The initial loss of the anion in this case the chloride ion was consistently observed to occur at about 450�C with final traces evolved at 535 to 780�C depending of the Fe:Cr ratio and was detected as HCl (m/z=36). Thus for this to occur, hydroxyl units must have been retained in the structure at temperatures upwards of 750�C. Experimentally it was found difficult to keep CO2 from reacting with the compounds and in this way the synthesized iowaite-woodallite series somewhat resembled the natural minerals.

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Abstract  

The thermal decomposition of beaverite and plumbojarosite was studied using a combination of thermogravimetric analysis coupled to a mass spectrometer. The mineral beaverite Pb(Fe,Cu)3(SO4)2(OH)6 decomposes in three stages attributed to dehydroxylation, loss of sulphate and loss of oxygen, which take place at 376 and 420, 539 and 844°C. In comparison three thermal decomposition steps are observed for plumbojarosite PbFe6(SO4)4(OH)12 at 376, 420 and 502°C attributed to dehydroxylation; loss of sulphate occurs at 599°C; and loss of oxygen and formation of lead occurs at 844 and 953°C. The temperatures of the thermal decomposition of the natural plumbojarosite were found to be less than that for the synthetic jarosite. A comparison of the thermal decomposition of plumbojarosite with argentojarosite is made. The understanding of the chemistry of the thermal decomposition of minerals such as beaverite, argentojarosite and plumbojarosite and related minerals is of vital importance in the study known as ‘archeochemistry’.

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Abstract  

TG combined with MS has been used to study the thermal decomposition of a synthetic aurichalcite with varying copper-zinc ratios from 0.1:0.9 to 0.5:0.5. In general, five decomposition steps are observed at 235, 280, 394, 428 and 805°C. The principal mass loss step increases in temperature from 255°C (0.1/0.9) to 300°C (0.5/0.5). MS using ion current curves show that the OH units and carbonate units decompose simultaneously and the two decomposition steps after the main decomposition are attributed to the decomposition of ZnCO3 and CuCO3. A higher temperature decomposition at around 805°C, based upon the ion current curves is assigned to the decomposition of CuO to Cu. The thermal decomposition of aurichalcite offers a method of preparing metal oxides mixed at the molecular level making the thermally activated aurichalcites as suitable for use as catalysts.

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Abstract  

Iron doped boehmite nanofibres with varying iron content have been prepared at low temperatures using a hydrothermal treatment in the presence of poly(ethylene oxide) surfactant. The resultant nanofibres were characterized by X-ray diffraction (XRD), and transmission electron microscopy (TEM). TEM images showed the resulting nanostructures are predominantly nanofibres when Fe doping is no more than 5%; in contrast nanosheets were formed if Fe doping was above 5%. For the 10% Fe doped boehmite, a mixed morphology of nanofibres and nanosheets were obtained. Nanotubes instead of nanofibres were observed in samples with 20% added iron. The Fe doped boehmite and the subsequent nanofibres/nanotubes were analysed by thermogravimetric and differential thermogravimetric methods. Boehmite nanofibres decompose at higher temperatures than non-hydrothermally treated boehmite and nano-sheets decompose at lower temperatures than the nanofibres.

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Abstract  

Hydrotalcites of formula Mg6A12(OH)16(PO4)�4H2O formed by intercalation with the phosphate anion as a function of pH show variation in the d-spacing attributed to the size of the hydrated anion in the interlayer. The value changes from 11.91 � for pH 9.3, to 7.88 � at pH 12.5. No crystalline hydrotalcites with phosphate in the interlayer were formed at pH 9.3. Thermal decomposition identifies three steps namely dehydration, dehydroxylation and some loss of carbonate during the thermal treatment. The addition of a thermally activated ZnAl-HT to a phosphate solution resulted in the uptake of the phosphate and the reformation of the hydrotalcite. The technology has the potential for water purification through anion removal.

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Abstract  

Thermogravimetry combined with mass spectrometry has been used to study the thermal decomposition of a synthetic hydronium jarosite. Five mass loss steps are observed at 262, 294, 385, 557 and 619C. The mass loss step at 557C is sharp and marks a sharp loss of sulphate as SO3 from the hydronium jarosite. Mass spectrometry through evolved gases confirms the first three mass loss steps to dehydroxylation, the fourth to a mass loss of the hydrated proton and a sulphate and the final step to the loss of the remaining sulphate. Changes in the molecular structure of the hydronium jarosite were followed by infrared emission spectroscopy. This technique allows the infrared spectrum at the elevated temperatures to be obtained. Infrared emission spectroscopy confirms the dehydroxylation has taken place by 400 and the sulphate loss by 650C. Jarosites are a group of minerals formed in evaporite deposits and form a component of the efflorescence. The minerals can function as cation and heavy metal collectors. Hydronium jarosite has the potential to act as a cation collector by the replacement of the proton with a heavy metal cation.

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Abstract  

A combination of DSC and high resolution DTG coupled to a gas evolution mass spectrometer has been used to study the thermal properties of a series of Mg/Zn hydrotalcites of formulae MgxZn6-xAl2(OH)16(CO3) 4H2O where x varied from 6 to 0. The effect of increased Zn composition results in the decrease of the endotherms and mass loss steps to lower temperatures. Evolved gas mass spectrometry shows that water is lost in a number of steps. The interlayer carbonate anion is lost simultaneously with hydroxyl units.

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Abstract  

A method for the preparation of a radioactive tracer for sand,56Mn-labelled sand, using NH4MnF3 as the label carrier was developed. The labelling process is based on the adsorption of the label carrier onto the sand particles.

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