Impact of sample preparation on mineralogical analysis of iron reactive barrier materials

Permeable reactive barriers (PRBs) of zero-valent iron (Fe0) are increasingly being used to remediate contaminated ground water. Corrosion of Fe0 filings and the formation of precipitates can occur when the PRB material comes in contact with ground water and may reduce the lifespan and effectiveness of the barrier. At present, there are no routine procedures for preparing and analyzing the mineral precipitates from Fe0 PRB material. These procedures are needed because mineralogical composition of corrosion products used to interpret the barrier processes can change with iron oxidation and sample preparation. The objectives of this study were (i) to investigate a method of preparing Fe0 reactive barrier material for mineralogical analysis by X-ray diffraction (XRD), and (ii) to identify Fe mineral phases and rates of transformations induced by different mineralogical preparation techniques. Materials from an in situ Fe0 PRB were collected by undisturbed coring and processed for XRD analysis after different times since sampling for three size fractions and by various drying treatments. We found that whole-sample preparation for analysis was necessary because mineral precipitates occurred within the PRB material in different size fractions of the samples. Green rusts quickly disappeared from acetone-dried samples and were not present in air-dried and oven-dried samples. Maghemite/magnetite content increased over time and in oven-dried samples, especially after heating to 105°C. We conclude that care must be taken during sample preparation of Fe0 PRB material, especially for detection of green rusts, to ensure accurate identification of minerals present within the barrier system.

Impact of sample preparation on mineralogical analysis of zero-valent iron reactive barrier materials

Permeable reactive barriers (PRBs) of zero-valent iron (Fe⁰) are increasingly being used to remediate contaminated ground water. Corrosion of Fe⁰ filings and tbe formation of precipitates can occur when the PRB material comes in contact with ground water and may reduce the lifespan and effectiveness of the barrier. At present, there are no routine procedures for preparing and analyzing the mineral precipitates from Fe⁰ PRB material. These procedures are needed because mineralogical composition of corrosion products used to interpret the barrier processes can change with iron oxidation and sample preparation. The objectives of this study were (i) to investigate a method of preparing Fe⁰ reactive barrier material for mineralogical analysis by X-ray diffraction (XRD), and (ii) to identify Fe mineral phases and rates of transformations induced by different mineralogical preparation techniques. Materials from an in situ Fe⁰ PRB were collected by undisturbed coring and processed for XRD analysis after different times since sampling for three size fractions and by various drying treatments. We found that whole-sample preparation for analysis was necessary because mineral precipitates occurred within the PRB material in different size fractions of the samples. Green rusts quickly disappeared from acetone-dried samples and were not present in air-dried and oven-dried samples Maghemite/magnetite content increased over time and in oven-dried samples, especially after heating to 105°C. We conclude that care must be taken during sample preparation of Fe⁰ PRB material, especially for detection of green rusts, to ensure accurate identification of minerals present within the barrier system.

Forensic analysis of wooden safety matches - A case study

In this case, an individual was suspected of attempting to burn materials potentially relating to a murder case. A number of spent and unspent matches were seized at the scene by police for forensic examination. Coincidentally, a police raid at the suspect's house revealed a number of matchboxes, all of the same brand, containing matches that had a visual similarity to those recovered at the scene. Stable Isotope Profiling (SIP) was used to assess whether matches could either be distinguished or shown to be indistinguishable by 13C and 2H isotopic composition. These results were then compared to those from the X-ray diffraction (XRD) analysis of match heads and microscopy of the wood. SIP showed the scene matches and seized matches to be different, which was confirmed by XRD and microscopy analyses.

Development of composite tissue scaffolds containing naturally sourced mircoporous hydroxyapatite

The aims of this work were to investigate the conversion of a marine alga into hydroxyapatite (HA), and furthermore to design a composite bone tissue engineering scaffold comprising the synthesised HA within a porous bioresorbable polymer. The marine alga Phymatolithon calcareum, which exhibits a calcium carbonate honeycomb structure, with a natural architecture of interconnecting permeable pores (microporosity 4-11 mu m), provided the initial raw material for this study. The objective was to convert the alga into hydroxyapatite while maintaining its porous morphology using a sequential pyrolysis and chemical synthesis processes. Semi-quantitative XRD analysis of the post-hydrothermal material (pyrolised at 700-750 degrees C), indicated that the calcium phosphate (CaP) ceramic most likely consisted of a calcium carbonate macroporous lattice, with hydroxyapatite crystals on the surface of the macropores. Cell visibility (cytotoxicity) investigations of osteogenic cells were conducted on the CaP ceramic (i.e., the material post-hydrothermal analysis) which was found to be non-cytotoxic and displayed good biocompatibility when seeded with MG63 cells. Furthermore, a hot press scaffold fabrication technique was developed to produce a composite scaffold of CaP (derived from the marine alga) in a polycaprolactone (PCL) matrix. A salt leaching technique was further explored to introduce macroporosity to the structure (50-200 mu m). Analysis indicated that the scaffold contained both micro/macroporosity and mechanical strength, considered necessary for bone tissue engineering applications. (C) 2008 Published by Elsevier B.V.

Haematite in Lateritic Soils Aids Groundwater Disinfection

Microbiologically contaminated water severely impacts public health in low-income countries, where treated water supplies are often inaccessible to much of the population. Groundwater represents a water source that commonly has better microbiological quality than surface water. A 2-month intensive flow and quality monitoring programme of a spring in a densely settled, unsewered parish of Kampala, Uganda, revealed the persistent presence of high chloride and nitrate concentrations that reflect intense loading of sewage in the spring’s catchment. Conversely, thermotolerant coliform bacteria counts in spring water samples remained very low outside of periods of intense rainfall. Laboratory investigations of mechanisms responsible for this behavior, achieved by injecting a pulse of H40/1 bacteriophage tracer into a column packed with locally derived granular laterite, resulted in near-total tracer adsorption. X-ray diffraction (XRD) analysis showed the laterite to consist predominantly of quartz and kaolinite, with minor amounts (<5%) of haematite. Batch studies comparing laterite adsorption capacity with a soil having comparable mineralogy, but with amorphous iron oxide rather than haematite, showed the laterite to have a significantly greater capacity to adsorb bacteriophage. Batch study results using pure haematite confirmed that its occurrence in laterite contributes substantially to micro-organism attenuation observed and serves to protect underlying groundwater.

Microstructure and mechanical properties of low nickel maraging steel

Austenitization with lower temperature and intercritical annealing were introduced in the treatment of a maraging steel with a composition of Fe–12.94Ni–1.61Al–1.01Mo–0.23Nb (wt.%). Scanning electron microscopy was employed to study the microstructure after austenitization at 950 °C and intercritical annealing, followed by aging at 485 and 600 °C. X-ray diffraction (XRD) analysis was applied to evaluate the formation of retained or reverted austenite. Thermodynamic calculation was employed to calculate equilibrium phase mole fractions. Hardness and Charpy impact toughness of the steel were measured. Intercritical annealing treatments did not result in significant increase of hardness either before or after aging. The Charpy impact toughness of the alloy in aged condition was enhanced after austenitization at 950 °C. No austenite was observed in XRD. However, suspected reverted austenite was found after austenitization at 950 °C followed by aging at 600 °C for 4 h. Relationships among heat treatment, microstructure and mechanical properties are discussed.

Solution-based synthesis of cobalt-doped ZnO thin films

Undoped and cobalt-doped (1-4 wt.%) ZnO polycrystalline, thin films have been fabricated on quartz substrates using sequential spin-casting and annealing of simple salt solutions. X-ray diffraction (XRD) reveals a wurzite ZnO crystalline structure with high-resolution transmission electron microscopy showing lattice planes of separation 0.26 nm, characteristic of (002) planes. The Co appears to be tetrahedrally co-ordinated in the lattice on the Zn sites (XRD) and has a charge of + 2 in a high-spin electronic state (X-ray photoelectron spectroscopy). Co-doping does not alter the wurzite structure and there is no evidence of the precipitation of cobalt oxide phases within the limits of detection of Raman and XRD analysis. Lattice defects and chemisorbed oxygen are probed using photoluminescence and Raman spectroscopy - crucially, however, this transparent semiconductor material retains a bandgap in the ultraviolet (3.30-3.48 eV) and high transparency (throughout the visible spectral regime) across the doping range. © 2012 Elsevier B.V.