This study was a small part of the EURARE project concerned with the processing of eudialyte concentrates from Greenland and Norra Kärr, Sweden. Eudialyte is a potential rare earth elements (REE) primary resource due to its good solubility in acid, low radioactivity and relatively high REE content. The main challenge is avoiding the formation of silica gel, which is non-filterable when using acid to extract REE. Some methods have been studied to address this issue and, based on previous research, this paper examined a complete hydrometallurgical treatment of eudialyte concentrate to the production of REE carbonate as a preliminary product. Dry digestion with concentrated hydrochloric acid (10 M) and subsequent water leaching of the treated eudialyte concentrate resulted in high REE extraction while avoiding gel formation. Experiments were performed at a small scale to obtain the optimal parameters. After the first two stages, 88.8% REE was leached under the optimal conditions (HCl:concentrate ratio 1.25:1, digestion time 40 min, water:concentrate ratio 2:1, leaching temperature 20–25°C and leaching time 30 min). After obtaining the pregnant leach solution, preliminary removal of impurities by a precipitation method was examined as well. When adjusting the pH to ~4.0 using calcium carbonate, zirconium, aluminium and iron were removed at 99.1%, 90.0% and 53.1%, respectively, with a REE loss of 2.1%. Finally, a pilot plant test was performed to demonstrate the feasibility and recovery performance under optimal parameters. The material balance in the upscaling test was also calculated to offer some references for future industrial application. A REE carbonate containing 30.0% total REE was finally produced, with an overall REE recovery yield of 85.5%.
The adsorption and diffusion of species in activated carbons is fundamental to many processes in catalysis and energy storage. Nuclear magnetic resonance (NMR) gives an insight into the molecular-level mechanisms of these phenomena thanks to the unique magnetic shielding properties of the porous carbon structure, which allows adsorbed (in-pore) species to be distinguished from those in the bulk (ex-pore). In this work we investigate exchange dynamics between ex-pore and in-pore solvent species in microporous carbons using a combination of one-dimensional (1D) and two-dimensional (2D) NMR experiments. We systematically compare the effects of four variables: particle size, porosity, solvent polarity and solvent viscosity to build up a picture of how these factors influence the exchange kinetics. We show that exchange rates are greater in smaller and more highly activated carbon particles, which is expected due to the shorter in-pore–ex-pore path length and faster diffusion in large pores. Our results also show that in-pore–ex-pore exchange of apolar solvents is slower than water, suggesting that the hydrophobic chemistry of the carbon surface plays a role in the diffusion kinetics, and that increased viscosity also reduces the exchange kinetics. Our results also suggest the importance of other parameters, such as molecular diameter and solvent packing in micropores.
Introduction “Solid-State NMR in Zeolite Catalysis” was written by four professors from the Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, who have tremendous expertise in the fields of solid-state nuclear magnetic resonance (solid-state NMR) and heterogeneous catalysis. This book is Volume 103 in the series ‘Lecture Notes in Chemistry’ published by Springer. It...
We review developments in the study of the stability of platinum-iridium standard weights, in particular the kilogram prototypes manufactured from alloy supplied by Johnson Matthey in the 1880s that still stand at the heart of the International System of Units (abbreviated SI from the French: Système international d’unités). The SI has long since moved on from length standards based on physical artefacts fabricated from this alloy, but the SI unit of mass is still defined in this way, as the mass of a real physical object. The stability of these reference masses has been a concern since the 1930s, with mass loss or gain at the surface being the principal concern. In recent years X-ray photoelectron spectroscopy (XPS) has been particularly valuable in elucidating the types of contamination present and the mechanism by which contamination takes place. While direct studies on the International Prototype Kilogram are understandably difficult, at Newcastle University we have examined the surfaces of six Pt mass standards also manufactured in the mid-19th century, using XPS to identify contamination chemically. XPS shows a significant quantity of mercury on the surfaces of all six. The most likely source of Hg vapour is the accidental breakage of thermometers and barometers, and the mechanism of contamination may be similar to the poisoning of platinum group metal (pgm) catalysts by Hg, an effect known for almost a century.
Before joining Johnson Matthey, Tuğçe Eralp Erden was a Marie Curie PhD student at the University of Reading, UK, studying model chiral adsorption systems using synchrotron-based structural and spectroscopic techniques (1–5). After completing her PhD, she joined the advanced characterisation department at Johnson Matthey, Sonning Common, UK, where she is currently leading the surface...
The accurate and precise characterisation of disordered, mesoporous solids continues to be an ongoing challenge due to the high level of complexity of such materials. Common, indirect methods, such as gas sorption and mercury porosimetry, still offer relatively cheap, and, most importantly, statistically representative characterisations of macroscopic samples. This work reviews and expands upon recent developments aimed at increasing, and cross-validating, the information obtained from such methods. This involves developing a better understanding of the pore-pore co-operative effects that emerge only in extensive, disordered pore networks to better interpret raw characterisation data, and to use these effects to deliver more information on the void space. This work also describes novel hybrid methods that also greatly increase the information that indirect methods can deliver on complex mesoporous solids.
It is known that platinum-rhodium thermocouples exhibit mass loss when in the presence of oxygen at high temperatures due to the formation of volatile oxides of platinum and rhodium. The mass losses of platinum, Pt-6%Rh and Pt-30%Rh wires, commonly used for thermocouples, were considered in this paper to characterise the mass loss of wires of the three compositions due to formation and evaporation of the oxides PtO2 and RhO2 under the conditions that would be seen by thermocouples used at high temperature. For the tests, the wires were placed in thin alumina tubes to emulate the thermocouple format, and the measurements were performed in air at a temperature of 1324°C, i.e. with oxygen partial pressure of 21.3 kPa. It was found that the mass loss of the three wires increases linearly with elapsed time, consistent with other investigations, up to an elapsed time of about 150 h, but after that, a marked acceleration of the mass loss is observed. Remarkably, previous high precision studies have shown that a crossover after about 150 h at 1324°C is also observed in the thermoelectric drift of a wide range of platinum-rhodium thermocouples, and the current results are compared with those studies. The mass loss was greatest for Pt-30%Rh, followed by Pt6%Rh, then platinum.
Sensors are vital to process and product control across a large number of industries. A network of sensors is used for monitoring and controlling machinery, systems and processes in chemicals, pharmaceuticals, biotechnology, energy, water, wastewater, oil, gas, plastic, paper, food and beverages among others. Technologies for Sensing The technologies are as varied as the applications....
1. Introduction There are few mathematical breakthroughs that have had as dramatic impact on the scientific process as the Fourier transform. Defined in 1807 in a paper by Jean Baptiste Joseph Fourier (1) to solve a problem in heat conduction, the integral transform, Equation (i): (i) and its inverse, Equation (ii): (ii) provide the framework to determine the spectral make up of a time...
In Part I (1), the failure response of a 1 Ah layered pouch cell with a commercially available nickel manganese cobalt (NMC) cathode and graphite anode at 100% state of charge (SOC) (4.2 V) was investigated for two failure mechanisms: thermal and mechanical. The architectural changes to the whole-cell and deformations of the electrode layers are analysed after failure for both mechanisms. A methodology for post-mortem cell disassembly and sample preparation is proposed and demonstrated to effectively analyse the changes to the electrode surfaces, bulk microstructures and particle morphologies. Furthermore, insights into critical architectural weak points in LIB pouch cells, electrode behaviours and particle cracking are provided using invasive and non-invasive X-ray computed tomography techniques. The findings in this work demonstrate methods by which LIB failure can be investigated and assessed.
The assessment of lithium-ion battery (LIB) safety is a multiscale challenge: from the whole-cell architecture to its composite internal three-dimensional (3D) microstructures. Substantial research is required to standardise failure assessments and optimise cell designs to reduce the risks of LIB failure. In this two-part work, the failure response of a 1 Ah layered pouch cell with a commercially available nickel manganese cobalt (NMC) cathode and graphite anode at 100% state of charge (SOC) (4.2 V) is investigated. The mechanisms of two abuse methods: mechanical (by nail penetration) and thermal (by accelerating rate calorimetry) are compared by using a suite of post-mortem analysis methods.