This thesis describes the fabrication of an induction heating apparatus and its use to directly heat small platinum and gold electrodes in electrolyte solution. The heating characteristics of the electrodes were studied via the entropic shift of redox potential with temperature and change in Faradaic current. Temperature pulse voltammetry (TPV) and cyclic voltammetry were used for temperature calibration under various heating conditions. The maximum temperature reached at a 0.25 mm diam platinum electrode surface in solution was 84 degrees C. At heated electrodes an increase in current was found to be due to convection and diffusion. TPV was performed with inductively heated gold (0.5 mm diam) and platinum electrodes, which gave complete current-potential-temperature information. Induction heated Pt electrodes were employed to investigate the kinetics and mass transfer process of oxygen reduction reaction (ORR) in acidic and alkaline media.

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Induktiefgekoppelde-plasmareaktore (IGP’s) het toepassings in verskeie industrieë, insluitend die voorbereiding van metaalpoeiers vir laagvervaardiging. Die skermgas (ook skutgas gnoem) speel ’n belangrike rol in die termiese afskerming van die reaktorwand in ’n IGP. Die energie wat verloor word deur die wand van die reaktor kan verminder word deur die hittesone weg van die wand af te beweeg. Hierdie verplasing van die hittesone word bereik deur ’n skermgas te gebruik wat moeiliker ioniseer as die plasmagas. Die ioniseringsgraad van waterstof is laer as dié van argon weens die hoër elektriese geleidingsvermoë van argon by soortgelyke temperature. Waterstof word dus in klein hoeveelhede in die skutgas gebruik met argon as die hoof bestandeel en hoofplasmagas. Die waterstof voorkom dus plasmavorming naby die wand. Die skutgas het ook ’n heelwat hoër vloeisnelheid en verminder sodoende die beskikbare tyd vir hitte-oordrag na die wand. Die besondere hoë temperature wat in ’n IGP bereik word, belemmer egter die meting van eenvoudige lesings soos vloeisnelheid en temperatuur. Rekenaarmodelle voorsien ons van die geleentheid om die fisiese en chemiese eienskappe van ’n plasma te ondersoek asook die nodige gereedskap om die gedrag van die plasma te analiseer sonder eksperimentele lesings. Daar is verskeie numeriese modelle van IGP-sisteme in die literatuur alhoewel nie een van dié modelle die effek van die skutgassamestelling in ag neem nie. Die hoeveelheid waterstof in die skutgas kan groot newe-effekte hê op die plasmagas a.g.v. die hoër ionisasiepotensiaal van waterstof. ’n Oormaat waterstof in die skutgas is ook ’n verkwisting van voermateriaal. Albei die faktore het ’n invloed op die ekonomiese uitvoerbaarheid van die plasmaproses. Hierdie navorsing het beoog om die optimale skutgassamestelling te vind vir die reaktor wat by Necsa gebruik word vir sferoïedisering. Die werk is uitgevoer met die kommersiële eindige-elementsagtewarepakket COMSOL Multiphysics R. Hierdie rekenaarmodel dui daarop dat die wand beskerm kan word van plasmavorming met ’n waterstof/argon skutgas wat sodoende ook die energieverliese deur die wand verminder. Waterstof verbeter die skutgas se hitte-oordragvermoë, maar verskuif die hittesone weg van die wand af. As gevolg van hierdie twee kompeterende meganismes bestaan daar ’n optimale bedrywingspunt by 3 vol% H2 in die skutgas. Die model is bevestig deur die energiebalans van die model te vergelyk met eksperimentele resultate. / Dissertation (MEng)--University of Pretoria, 2020. / Advanced Metals Initiative Suid Afrikaanse Akademie vir Wetenskap en Kuns / Chemical Engineering / MEng / Unrestricted

The inductively coupled plasma mass spectrometer (ICP-MS) is the instrument of choice for trace and ultra-trace elemental analysis. However, the ICP-MS suffers from matrix effects. Matrix effects occur when instrument response varies as the composition of the sample matrix is changed. Matrix effects, or non-spectroscopic interferences, limit the accuracy of routine analysis. Identification of the sources of matrix effects provide a basis for reducing or eliminating them. As inaccuracies in the ICP-MS are more severe than those in the ICP atomic emission spectrometer, the problem may be due, at least in part, to the vacuum interface used to couple the plasma source and mass spectrometer. The research herein is a study of matrix effect sources in the first stage of the vacuum interface. This study utilized laser-induced fluorescence of atomic species to identify factors affecting analyte transport through the sampling orifice of the vacuum interface. Several non-idealities in the performance of the interface were found. (1) Operating conditions and sample compositions can negatively affect the efficiency with which ions are extracted through the vacuum interface coupling the plasma source to the mass spectrometer. (2) The sampling cone itself was found to suppress and narrow ion distributions in the plasma. (3) Changes in the degree of ionization were identified in the first vacuum stage. The evidence of recombination and state-changing collisions was observed in the first vacuum stage at lower power settings. Matrix effects occur in the first vacuum stage, the first step of the ion extraction process. This work shows that changes in ion transport through the first vacuum stage of the vacuum interface of an ICP-MS affect the overall performance of the instrument.

The Direct Simulation Monte Carlo algorithm as coded in FENIX is used to model the transport of trace ions in the first vacuum stage of the inductively coupled plasma mass spectrometer. Haibin Ma of the Farnsworth group at Brigham Young University measured two radial trace density profiles: one 0.7 mm upstream of the sampling cone and the other 10 mm downstream. We compare simulation results from FENIX with the experimental results. We find that gas dynamic convection and diffusion are unable to account for the experimentally-measured profile changes from upstream to downstream. Including discharge quenching and ambipolar electric fields, however, makes it possible to account for the way the profiles change.

Tooth enamel is among the most durable substances in the human body and as such has high recoverability in forensic anthropology cases. Its crystalline hydroxyapatite matrix has a slightly variable chemical composition which incorporates biologically available trace elements. The trace elements are derived from an individual's diet and the water he or she consumes during the period of enamel formation. As a result, trace element profiles of enamel can reflect the geology, pollution, and certain cultural dietary factors of the area in which the individual resided during this period. This research examines a sample of teeth with known demographic information from the Antioquia Modern Skeletal Reference Collection in Medellin, Colombia. A sample set of 75 teeth from 61 individuals born in areas throughout northwestern Colombia were analyzed using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), a minimally destructive, semi-quantitative technique. Analysis was performed at the Center for Archaeology, Materials, and Applied Spectroscopy (CAMAS) at Idaho State University. 33 elements were analyzed in the sample. Nonparametric methods were used to assess the relationship between elemental profiles and region of origin. Sr, Mo, Ag, Ba, Eu, and Tm concentration profiles were found to vary among regional groups. Al, Ni, Cr, Mn, Co, Sr, Cd, Sb, Sm, Eu, and U were found to predict region of origin. Differences in municipality were classified with 72% accuracy, variation across the department of Antioquia was classified with 67% accuracy, and the age of the geologic substrate was classified with 67% accuracy. The results suggest that trace element analysis of permanent tooth enamel may be of some use in estimating an individual's region of origin in forensic anthropological contexts. Further research with both larger sample sizes and more geographic variation is necessary.

The Neolithic and late Iron Age pottery from the settlement site of Pool, Sanday, Orkney, was studied on two levels. Firstly, a morphological and technological study was carried out to establish a sequence for the site. Secondly an assessment was made of the usefulness of X-ray Fluorescence Analysis, Inductively Coupled Plasma Spectrometry and Petrological analysis to coarse ware studies, using the Pool assemblage as a case study. Recording of technological and typological attributes allowed three phases of Neolithic pottery to be identified. The earliest phase included sherds of Unstan Ware. This phase was followed by an assemblage characterised by pottery with incised decoration, which was stratified below a traditional Grooved Ware assemblage. The change in pottery styles and manufacturing methods with the Grooved Ware indicated that it evolved elsewhere. Grass tempered and burnished pottery characterised the Iron Age assemblage. Pottery samples from all phases of the site were analysed by XRF and ICPS. In addition, pottery from late Iron Age sites in the area was analysed for comparison with the Pool Iron Age pottery. XRF and ICPS analyses did not distinguish between either different phases at Pool or different Orcadian sites. This was attributed to the similarities in geological deposits over much of Orkney and the variations which can occur within a clay source. A clay survey was carried out in the vicinity of the site, and samples taken for comparison with the Pool pottery. Identification of rocks and minerals in thin section, and grain-size analysis, indicated that the Pool pottery was made locally to the site, and that both primary and secondary clays were used. It was concluded that petrological analysis is more suitable than elemental analysis in the study of coarse wares. / Science-based Archaeology'Committee of the Science and Engineering Research Council.

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No description available.