UWCScholar :: Browsing by Author "Petrik, Leslie F."

Browsing by Author "Petrik, Leslie F."

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Brine treatment using natural adsorbents
(University of the Western Cape, 2011) Mabovu, Bonelwa; Petrik, Leslie F.
Studies involving the use of natural clays such as bentonite, montmorillonite and natural zeolite clinoptilolite in water treatment have been reported. Researchers suggested cost effective processes, such as ion-exchange and adsorption for the removal of heavy metals from waste waters by using naturally occurring and synthetic materials. The current study investigated application of natural adsorbents in brine treatment. Brines are hypersaline waters generated in power stations and mining industries rich in Mg2+, K+, Ca2+,Na+, so,': cr and traces of heavy metals, thus there is a need for these brines to be treated to recover potable water and remove problematic elements. Natural adsorbents have been successfully used in waste water treatment because of their high surface area and high adsorptive properties when they are conditioned with acid or base. The natural adsorbents used in this study were obtained from Ecca Holdings company (Cape bentonite mine) Western Cape in South Africa, comprising bentonite clay and natural zeolite (clinoptilolite) and another clinoptilolite sample was obtained from Turkey. These adsorbents were investigated in their natural and pretreated form for removal of toxic elements in brine water. The pretreatment was aimed at removing Na+, K+, Ca2+, Mg2+ from the clinoptilolite as well as the bentonite and replacing these cations with the H+ cation to activate the materials. The cation exchange capacity (CEC) of natural zeolite from South Africa was found to be 2.14 meq/ g, Turkish Clinoptilolite was 2.98 meq/ g while South African bentonite was 1.73 meq/g. at 25°C using ammonium acetate (pH 8.2) method. Characterization of these natural adsorbents was done prior to pretreatment and after the treatment. ICP-AES analysis was used for determination of toxic elements in brines before and after sorption. The morphology of clays was characterized by X-ray diffraction (XRD), Brunauer Emmett Teller (N2-BET) and Scanning electron microscopy (SEM) for confirmatory purposes and X-ray Fluorescent spectroscopy (XRF) was used for the composition analysis of the natural adsorbent. The results from batch experiments prior to pretreatment of the natural adsorbents showed that these natural adsorbents contained Mg2+, K+, Ca2+, Na+ in their structures as charge balancing cations, thus needed pretreatment to remove the cations. The natural adsorbents were pre-treated with 0.02M HCI. After the pretreatment of natural adsorbents it was possible to enhance the percentage removal of the major cations from brine, and the Na+ and Mg2+ removal achieved (86 % and 85% respectively) from brine was more than C02+ (70% ) the SC was the adsorbent one that gave highest removal of cations in the brines. Trace elements removal was high with Cu2+and Zn2+ being the highest of toxic elements in brine. The optimum contact for the toxic element removal was found to be 30 min for the Turkish clinoptilolite and 1 hr for the South African clinoptilolite and South African bentonite clay. Leaching of Ae+ and Si4+ during adsorption was also investigated and it was found that less than 1 ppm of A13+ and Si4+ were leached into the solution during adsorption experiments indicating that these materials were stable. The investigation of pH showed that natural adsorbents did not perform well at low pH of 4 and 6. The adsorbents were able to work efficiently at the natural pH of 8.52 of the brine solution. These results show that natural adsorbents hold great potential to remove cationic major components and selected heavy metal species from industrial brine wastewater. Heterogeneity of natural adsorbents samples, even when they have the same origin, could be a problem when wastewater treatment systems utilizing natural clinoptilolite and bentonite are planned to be developed. Therefore, it is very important to characterize the reserves fully in order to make them attractive in developing treatment technologies.
Brine treatment using natural adsorbents
(University of the Western Cape, 2011) Mabovu, Bonelwa; Petrik, Leslie F.; Dept. of Chemistry; Faculty of Science
The current study investigated application of natural adsorbents in brine treatment. Brines are hypersaline waters generated in power stations and mining industries rich in Mg2+, K+, Ca2+, Na+, SO4 2- , Cl- and traces of heavy metals, thus there is a need for these brines to be treated to recover potable water and remove problematic elements. Natural adsorbents have been successfully used in waste water treatment because of their high surface area and high adsorptive properties when they are conditioned with acid or base. The investigation of pH showed that natural adsorbents did not perform well at low pH of 4 and 6. The adsorbents were able to work efficiently at the natural pH of 8.52 of the brine solution. These results show that natural adsorbents hold great potential to remove cationic major components and selected heavy metal species from industrial brine waste water. Heterogeneity of natural adsorbents samples, even when they have the same origin, could be a problem when wastewater treatment systems utilizing natural clinoptilolite and bentonite are planned to be developed. Therefore, it is very important to characterize the reserves fully in order to make them attractive in developing treatment technologies.
Cation-exchanged zeolites-A prepared from South African fly ash feedstock for CO2 adsorption
(University of the Western Cape, 2015) Muvumbu, Jean-Luc Mukaba; Petrik, Leslie F.; Musyoka, Nicholas
In South Africa coal combustion constitutes up to 90 % of the country’s energy need. This coal combustion activity is known to contribute to the amount of about 40 % of the total CO2 atmospheric emissions worldwide that are responsible for global warming effects. In addition burning of coal generates a large quantity of fly ash which creates environmental pollution since only a small portion of it is currently used in some applications. In order, on one hand to mitigate and sequester CO2 and on the other hand to reprocess fly ash and reuse it, this study focuses on developing new technologies with cost-effective and less energy consumption in the domain of CO2 capture and sequestration. CO2 has priority attention for being the largest contributor to global warming. Various techniques have been used for CO2 capture and sequestration, such as aqueous alkylamine absorption or adsorption onto a solid adsorbent such as zeolites. In this study NaA zeolite adsorbent was hydrothermally synthesised from South African fly ash. This fly ash based NaA zeolite was then used as starting material to prepare LiA, CaA, and MgA zeolite catalysts via ion-exchange for comparative CO2 adsorption capacity. A systematic design of the ion-exchange procedure was undertaken at either 30 °C or 60 °C for a contact time of 1 hr, 4 hrs, and 8 hrs with 1, 2 and 3 consecutive exchanges in each case in order to determine the optimum conditions for loading each cation exchanged. The adsorption of CO2 on the ion- exchanged fly ash based zeolite-A catalysts was carried out at 40 °C similar to the temperature of flue gas since the catalysts obtained in this study were also prepared with a view to their applications in flue gas system. The CO2 desorption temperature ranged between 40-700 °C. All materials used in this study, starting from fly ash feedstock, werecharacterized using various techniques to monitor the mineral and structural composition, the morphology, surface area and elemental composition and the adsorption capacity. The techniques included mainly Fourier transform infra-red, X-ray diffraction, Scanning electron microscopy, Transmission electron microscopy, Energy dispersive spectroscopy, X-ray fluorescence, Temperature programmed desorption.The results obtained from both Fourier transform infra-red and the X-raydiffraction spectroscopy for samples exchanged at either 30° C or 60 °C showedlower crystallinity in CaA and MgA zeolite samples. This decrease in crystallinitymainly affected the D4R (0-20° 2) and was demonstrated in the study to beinversely proportional to the increase of the atomic radius of cations (Li+ > Mg2+ >Ca2+). In the Fourier transform infra-red, the vibration band at 677 cm-1 attributedto the extra-framework cation, also proportionally increased with the decrease ofthe atomic radius or size of the cations, and was intense in LiA zeolite samples.
Characterization and chemical speciation modelling of saline effluents at Sasol Synthetic Fuels Complex-Secunda and Tukuta power station
(University of the Western Cape, 2009) Nyamhingura, Amon; Petrik, Leslie F.; Dept. of Chemistry; Faculty of Science
The study shows conclusively that brine composition and concentration is highly variable at these South African power utilities and processes such as RO, contact with ash and CO2 ingress can have an impact upon the overall brine quality. Aq.QA was found to be a more accurate tool for classifying waters according to dominant ions than Stiff diagrams but Stiff diagrams still have the superior advantage of being a mapping tool to easily identify samples of similar composition as well as quickly identify what has been added or what has been removed from a water stream. Chemical speciation could identify effluent streams where CO2 dissolution had taken place.
Chemical, physical and morphological changes in weathered brine slurried coal fly ash
(University of the Western Cape, 2011) Nyale, Sammy Mwasaha; Petrik, Leslie F.; Akinyeye, Richard Odunayo; Gitari, Wilson M.
Energy production from coal comes with an environmental cost because of the toxic waste produced during coal combustion such as coal ash and brine which are potential water and soil pollutants. Coal ash and brine contain toxic elements which can leach and contaminate soils and ground water if not properly disposed. This study investigated the mobility of species in coal fly ash co-disposed with brine at Sasol Secunda power station in order to establish if the ash dam could act as a salt sink. The ash was dumped as a slurry with 5:1 brine/ash ratio and the dam was in operation for 20 years. It was hypothesized that the disposed Secunda fly ash was capable of leaching toxic metal elements into the surrounding soils and ground water and therefore could not be used as a long term sustainable salt sink. Weathered fly ash samples were collected along a 51 m depth core at the Secunda ash dam by drilling and sampling the ash at 1.5 m depth intervals. A fresh fly ash sample was collected from the hoppers in the ash collection system at the power station. Characterization of both Secunda fresh ash and Secunda weathered ash core samples was done using X-ray diffraction (XRD) for mineralogy, X-ray fluorescence (XRF) for chemical composition and scanning electron microscopy (SEM) for morphology. Analysis of extracted pore water and moisture content determination of Secunda fresh ash and Secunda weathered ash core samples was done in order to evaluate the physico-chemical properties of the fly ash. The chemical partitioning and mobility of metal species in the ash dam was evaluated using the sequential extraction procedure. The XRD spectra revealed quartz, mullite and calcite as the dominant mineral phases in the weathered Secunda ash core samples while Secunda fresh ash contained quartz, mullite and lime. The major oxides identified by XRF analysis for both Secunda fresh ash and Secunda weathered ash include: SiO₂, Al₂O₃, CaO, Fe₂O₃, MgO, Na₂O, TiO₂ and K₂O. The minor oxides identified for both Secunda fresh ash and Secunda weathered ash were P₂O₅, SO₃ and MnO. The trace elements identified for both Secunda fresh ash and Secunda weathered ash were As, Ba, Ce, Co, Nb, Ni, Pb, Rb, Sr, V, Y, Zr and Th. However, U was detected in some of the Secunda weathered ash samples but not in Secunda fresh ash. Both Secunda fresh ash and Secunda weathered ash was classified as class F based on the sum of the oxides of silicon, aluminium and iron by mass and the CaO content as reported by XRF analysis, and further classified as sialic and ferrocalsialic type highlighting the significant levels of Si, Al, Ca and Fe in the fly ash based on XRF analysis. The XRF analysis further showed that brine codisposal on the ash may have been responsible for the slight enrichment of some species such as Na, SO₄²⁻, Mg, K and V in the disposed Secunda weathered fly ash. However, there was no significant accumulation of these species in the disposed fly ash despite continuous addition of an estimated 117.65 billion litres of brine over the 20 year period that the dam existed. Furthermore, Secunda ash dam showed an overall total salt capture capacity of only -0.01 weight %, a strong indication that the ash dam was incapable of holding salts and would release elements to the environment over time. The scanning electron microscopy (SEM) analysis revealed spherical particles with smooth outer surfaces for Secunda fresh ash while Secunda ash core samples consisted of agglomerated, irregular particles appearing to be encrusted, etched and corroded showing that weathering and leaching had occurred in the ash dam. A decrease in pH, electrical conductivity (EC) and total dissolved solids (TDS) was observed in Secunda ash core samples compared to Secunda fresh ash. While Secunda fresh ash (n = 3) had a pH of 12.38 ± 0.15, EC value of 4.98 ± 0.03 mS/cm and TDS value of 2.68 ± 0.03 g/L, the pH of Secunda ash core (n = 35) was 10.04 ± 0.50, the EC value was 1.08 ± 0.14 mS/cm and the TDS value was 0.64 ± 0.08 g/L. The lower pH in the ash dam created an environment conducive to the release of species through leaching, while the lower EC and TDS in the ash dam implied the loss of ionic species from the ash which resulted from leaching. The moisture content (MC) analysis indicated that Secunda ash dam was very damp with an average MC of 54.2 ± 12.66 % for Secunda ash core creating favourable conditions for leaching of species in the ash dam while Secunda fresh ash had MC of 1.8 ± 0.11 %. The bottom of Secunda ash dam appeared water logged which could cause slumping of the dam. The sequential extraction procedure revealed that the major and trace elements contained in both Secunda fresh fly ash and Secunda weathered fly ash could leach upon exposure to different environmental conditions. The elements showed partitioning between five geochemical phases i.e. water soluble fraction, exchangeable fraction, carbonate fraction, Fe & Mn fraction and residual fraction. The labile phases consisted of the water soluble fraction, exchangeable fraction and carbonate fraction. The % leached out in the labile phases was expressed as a fraction of each element‟s total content e.g. Si (6.15 %) meant that 6.15 % of the total amount of Si in the ash was released in the labile phases. Na was the most labile among the major elements in the ash dam while Si and Al which form the major aluminosilicate ash matrix also showed significant lability. The % leached out in the labile phases for these major elements was as follows: for Secunda fresh ash: Si (6.15 %), Al (7.84 %), Na (11.31 %); for weathered Secunda ash core samples (n = 35): Si (7.53 %), Al (8.12 %), Na (11.63 %). This study showed that the fly ash generated at Sasol Secunda power station could not be used as a long term sustainable salt sink. The wet disposal method used at Sasol Secunda power station poses a high risk of groundwater contamination due to the high liquid to solid ratio used to transport the ash for disposal, which may lead to rapid dissolution of all the soluble components in the fly ash. The large volumes of brine that pass through Secunda ash dam in the wet ash handling system present a greater environmental concern than the dry ash handling system which involves small amounts of brine entering the ash dump.
CO2 sequestration using brine impacted fly fish
(University of the Western Cape, 2009) Muriithi, Grace Nyambura; Petrik, Leslie F.; Dept. of Chemistry; Faculty of Science
It was hypothesized that South African FA and brine could sequester CO2 through mineral carbonation. A statistical approach was undertaken to optimize the % CaCO3 formed from FA/brine/CO2 interaction with input parameters of temperature, pressure, particle size and solid/liquid ratio (S/L) being varied. The ranges adopted for the input parameters were: temperature of 30 ºC or 90 ºC; pressure of 1 Mpa or 4 Mpa; four particle sizes namely bulk ash, > 150 μm, < 20 μm and 20 μm- 150 μm particle size range; S/L ratios of 0.1, 0.5 or 1. The FA/ brine dispersions were carbonated in a high pressure reactor varying the above mentioned input parameters. The fresh Secunda FA of various size fractions was characterized morphologically using scanning electron microscopy, chemically using X-ray fluorescence and mineralogically using qualitative X-ray diffraction. The carbonated solid residues on the other hand were characterized using quantitative X-ray diffraction, scanning electron microscopy, thermal gravimetic analysis and Chittick tests. The raw brine from Tutuka together with the carbonation leachates were characterized using inductively coupled mass spectrometry and ion chromatography. Total acid digestion was carried out to evaluate the differences in the total elemental content in both the fresh ash and the carbonated solid residues. The results suggested that South African FA from Secunda belongs to class F based on the CaO content as well as the total alumina, silica and ferric oxide content, while the RO brine from Tutuka were classified as NaSO4 waters.
Degradation of bisphenol-a and 2-Nitrophenol by combined advanced oxidation technologies
(University of the Western Cape, 2015) Tijani, Jimoh Oladejo; Petrik, Leslie F.; Perold, Willem J.; Fatoba, Ojo.O.
Emerging micropollutants such as bisphenol-A and 2-nitrophenol present a great threat in drinking water due to their adverse effects. Most conventional technologies in water and wastewater treatment are not designed to eliminate these xenobiotics; instead pollutants are merely transferred from one phase to another. Advanced oxidation technologies (AOTs) however, have been identified as suitable routes for the degradation of these potential damaging substances based on free radical mechanisms and use of less expensive chemicals. Moreover, due to the structural complexity of wastewater and the existence of pollutants as mixtures, no single advanced oxidation technology can convincingly remove all forms of contaminants and then most often than not, a combination of treatment processes is required for an effective purification process. Besides, the problem of adequate degradation of emerging contaminants in the environment, when AOT(s) are used individually, they present inherent problems. For instance, powder TiO₂ photocatalysts obstruct light penetration, thus prevent effective interaction of UV light with the target pollutants, and particulates present problems of post-filtration and recovery of catalyst particles after treatment. Additionally, TiO₂ has a high band gap energy, high electron-hole recombination rate, and is prone to aggregation of the suspended particles. Similarly, the dielectric barrier discharge (DBD) system produces ultra violet light and hydrogen peroxide within the plasma zone which is not fully maximised for the mineralization of persistent organic pollutants. Rapid oxidation and aggregation of nano zero valent iron particles in photo-Fentons process reduce the particles mobility and affect its performance. In the same vein, the jet loop reactor (JLR) system is characterised by low impingement yield, which is responsible for low mineralization rate. In light of this background, this research investigated the degradation of bisphenol-A and 2- nitrophenol in aqueous solution using the following combined advanced oxidation methods: DBD/supported TiO₂ or Ag doped TiO₂ photocatalysts, DBD/photo-Fenton induced process and JLR/UV/H₂O₂. The target was to assess the performance of each single system and then identify the best combined AOTs capable of significantly mineralizing the target compounds. Firstly, two materials were developed namely supported TiO₂ and stabilized nano zero valent Fe. The TiO₂ photocatalyst supported on a stainless steel mesh was synthesised using sol-gel solution of 8 % PAN/DMF/TiCl₄. The influence of calcination temperature and holding time on the formation of nanocrystals was investigated. Afterwards, various amounts of metallic silver were deposited on the (optimum) supported TiO₂ photocatalyst using thermal evaporation. The catalysts were characterized by several analytical methods; HRSEM, HRTEM, EDS, SAED, FTIR, TGA-DSC, UV-vis/diffuse reflectance spectroscopy, XRD, BET, and XPS. The photocatalytic activity of the prepared catalysts was determined using methylene blue as a model pollutant under ultra-violet light irradiation. Secondly, the TiO2 photocatalyst and 2.4 % Ag doped TiO₂ nanocomposites obtained as optimums (in section 1) were combined with the DBD to decompose BPA or 2-NP in aqueous solution. Moreover, the photo-Fenton process was applied for degradation of the model pollutants, and different dosages of stabilized nZVI (in the range of 0.02 -1.00 g) were added to the DBD system to induce the photo-Fenton process and improve BPA or 2-NP degradation efficiency. Finally, a jet loop reactor (JLR) presenting advanced mixing by the “impinging effect” was explored to decompose BPA or 2-NP in aqueous solution as a function of inlet applied pressure, solution pH, and initial concentration of BPA or 2-NP. Subsequently, different concentrations of hydrogen peroxide (H₂O₂) were added to the JLR to enhance the mineralization process. Furthermore, a combination of JLR with in-line UV light and H₂O₂ were further utilised to decompose BPA or 2-NP in aqueous solution. The residual concentration of the model compounds and intermediates were analysed using high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LCMS). The concentration of the ozone, hydrogen peroxide and hydroxyl radicals generated by the DBD in the presence or absence of a catalyst was monitored using Ultraviolet-visible spectroscopy and Photoluminescence spectroscopy. The results revealed that the optimal thermal conditions to obtain well supported uniformly grown, highly active crystalline TiO₂ catalysts with high specific surface area was 350 ºC at a 3 h holding time in N2 atmosphere with a flow rate of 20 mL/min. Pyrolysis temperature and holding time played an important role on the crystalline nature and photocatalytic activity of the catalyst. Moreover, 2.4 % Ag doped TiO₂ nanocomposites exhibited higher photocatalytic activity for methylene blue degradation than the undoped supported TiO₂ nanocrystals. The results indicated that combining DBD with 2.4 % Ag doped TiO₂ nanocomposites achieved 89 % and 81 % removal efficiency for BPA or 2-NP compared to 67.22 % or 56.8 % obtain when using the DBD system alone. The 2.4 % Ag doped TiO₂ nanocomposites demonstrated excellent activity and offered photochemical stability after four repeated applications.In the case of the photo-Fenton induced process, nano zero valent iron particles (nZVI) stabilized with polyethylene glycol were synthesised using a modified borohydride reduction method. The HRSEM, BET, XRD, and XPS analysis confirmed the formation of filamentous, high surface area iron nanoparticles in the zero valent state. Unlike combined DBD/Ag doped TiO2 nanocomposites, 100 % or complete removal of BPA or 2-NP in aqueous solution was achieved with DBD/nZVI system within 30 minutes compared to 67.9 % (BPA) or 56.8 % (2-NP) with DBD alone after 80 minutes. The removal efficiency was attributable to the production of an increased concentration of OH radicals as well as existence of a synergetic effect in the combined DBD/nZVI system. Five new transformation products namely: 4-nitrophenol (C₆H₅NO₃), 4-nitrosophenolate (C₆H₄NO₂), 4-(prop-1-en-2-yl) cyclohexa-3,5-diene-1,2-dione, (C₉H₈O₂), 4-(2- hydroxylpropan-2-yl)cyclohexane-3,5-diene-1,2-dione (C₉H₁₀O₃), and 1,2-dimethyl-4-(2- nitropropan-2-yl)benzene (C₉H₁₀NO₄) were identified during the degradation of BPA. While, three aromatic intermediate compounds such as 2-nitro-1,3,5-benzenetriolate (C₆H₂NO₅), 2- nitro-1,4-benzoquinone (C₆H₃NO₄), and 2,5-dihydroxyl-1,4-benzoquinone (C₆H₄O₄) respectively were identified during the degradation of 2-NP for the first time in the DBD with JT14 or JT17 using LC-MS. These intermediate compounds have never been reported in the literature, thereby expanding the number of BPA or 2-NP intermediates in the data base in the DBD/JT14 or DBD/nZVI system. BPA degradation proceeded via ozonation, hydroxylation, dimerization, and decarboxylation and nitration step, while 2-NP proceeded via hydroxylation, nitration and denitration respectively. Furthermore, maximum removal efficiency of BPA or 2-NP in aqueous solution using JLR alone under the optimum solution pH (3), inlet pressure (4 bar), flow rate (0.0007 m3/s) was 14.0 % and 13.2 % respectively after 80 minutes. A removal efficiency of 34.9 % was recorded for BPA while 33.2 % was achieved for 2-NP using combined JLR/UV under the same conditions as JLR alone. For the combined JLR/H₂O₂ under optimum conditions of inlet pressure (4 bar), solution pH (3) and peroxide dosage (0.34 g/L), a 51.3 % and 50.1 % removal efficiency was achieved for BPA and 2-NP respectively under same conditions relative to JLR alone. Combination of JLR/UV/H₂O₂ achieved 77.7 % (BPA) or 76.6 % (2- NP) removal efficiency under the same conditions. The combined JLR/UV/H₂O₂ process was found to be most effective combination under the optimized operating parameters due to existence of a synergetic index value of 6.42 or 6.84. This implies that JLR should be coupled with UV and H₂O₂ to achieve greater mineralization efficiency instead of using the system individually. The obtained experimental data of these combined treatment processes fitted the pseudo-first order kinetic models. The combination of the JLR/UV/H₂O₂ was found to be energy efficient and could effectively degrade BPA or 2-NP in aqueous solution to a greater extent than the JLR, JLR/UV or JLR/H₂O₂ system. However, the total organic carbon (TOC) reduction value by all combined DBD and JLR system recorded was not completely achieved due to the formation of recalcitrant intermediate compounds under the applied conditions. In conclusion, this study is reporting for the first time a combination of supported 2.4 % Ag doped TiO₂ nanocomposites with dielectric barrier discharge system for BPA/2-NP degradation in aqueous solution; a combination jet loop reactor based on impingement with in-line UV lamp and H2O2 for successfully decomposing BPA or 2-NP in aqueous solution; as well as a combination of dielectric barrier discharge system and stabilised nano zero valent iron particles, which induced a photo-Fenton process for highly effective removal of BPA or 2-NP in aqueous solution. This study conclusively supports the hypothesis that combined advanced oxidation technologies offer a sustainable and highly efficient means of achieving partial or complete removal of BPA or 2-NP in aqueous solutions. Considering all the combinations of AOTs investigated in this study, the novel DBD/photo-Fenton-induced process under optimised operating parameters was found to be the most efficient in the elimination of BPA or 2-NP in aqueous solutions. The combination of DBD with photo- Fenton like process offers a promising advanced waste water purification technology in the immediate future. Based on these findings, it is recommended that DBD should be redesigned to prevent loss of ozone and JLR system reconfigured to increase impingement and cavitational yield in order to have an effective combination treatment strategy for waste water purification especially in large scale waste water management.
Extraction, fractionation, nanoparticles formulation, and antimicrobial activity of lipids from black soldier fly larvae
(University of Western Cape, 2021) Omores, Raissa Andong; Petrik, Leslie F.
Hermetia illucens (Diptera: Stratiomyidae) known as the black soldier fly (BSF) is an efficient ecological organic waste decomposer. Its larvae grow through six larval instars on a variety of decomposing organic substrates inhabited by a variety of microorganisms, including pathogenic ones. Survival in these environments requires a good functioning immune system to protect them from pathogen invasion, hence it can be expected that the BSF larvae possess antimicrobial substances. BSF larvae farming has recently gained popularity as a new source of protein and lipid. The lipid is highly sourced due to its applications in a variety of areas which span across food and pharmaceutical industries. Different extraction methods have been used to extract lipid from different sources.
Factors influencing pigment production by halophilic bacteria and its effect on brine evaporation rates
(Wiley, 2018) Silva-Castro, Gloria Andrea; Moyo, Anesu Conrad; Khumalo, Londiwe; van Zyl, Leonardo Joaquim; Petrik, Leslie F.; Trindade, Marla
The disposal of reject brine, a highly concentrated waste by-product generated by various industrial processes, represents a major economic and environmental challenge. The common practice in dealing with the large amounts of brine generated is to dispose of it in a pond and allow it to evaporate. The rate of evaporation is therefore a key factor in the effectiveness of the management of these ponds. The addition of various dyes has previously been used as a method to increase the evaporation rate. In this study, a biological approach, using pigmented halophilic bacteria (as opposed to chemical dyes), was assessed. Two bacteria, an Arthrobacter sp. and a Planococcus sp. were selected due to their ability to increase the evaporation of synthetic brine. When using industrial brine, supplementation of the brine with an iron source was required to maintain the pigment production. Under these conditions, the Planococcus sp. CP5-4 produced a carotenoid-like pigment, which resulted in a 20% increase in the evaporation rate of the brine. Thus, the pigment production capability of halophilic bacteria could potentially be exploited as an effective step in the management of industrial reject brines, analogous to the crystallizer ponds used to mine salt from sea water.
Geochemical and mineralogical evaluation of toxic contaminants mobility in weathered coal fly ash: as a case study, Tutuka dump site, South Africa
(University of the Western Cape, 2011) Akinyemi, Segun Ajayi; Petrik, Leslie F.; Akinlua, Akin; Gitari, Wilson M.; NULL; Faculty of Arts
The management and disposal of huge volumes of coal combustion by products such as fly ash has constituted a major challenge to the environment. In most cases due to the inadequate alternative use of coal fly ash, the discarded waste is stored in holding ponds, slag heaps, or stock piled in ash dumps. This practice has raised concerns on the prospect of inorganic metals release to the surface and groundwater in the vicinity of the ash dump. Acceptable scientific studies are lacking to determine the best ash disposal practices. Moreover, knowledge about the mobility patterns of inorganic species as a function of mineralogical association or pH susceptibility of the dry disposed ash dump under natural weathering conditions are scarce in the literature. Fundamental understanding of chemical interactions of dry disposed ash with ingressed CO2 from atmosphere, percolating rain water and brine irrigation within ash disposal sites were seen as key areas requiring investigation. The mineralogical association of inorganic species in the dry disposed ash cores can be identified and quantified. This would provide a basis for understanding of chemical weathering, mineralogical transformations or mobility patterns of these inorganic species in the dry ash disposal scenario. The current study therefore aims to provide a comprehensive characterisation of weathered dry disposed ash cores, to reveal mobility patterns of chemical species as a function of depth and age of ash, with a view to assessing the potential environmental impacts. Fifty-nine samples were taken from 3 drilled cores obtained respectively from the 1 year, 8 year and 20-year-old sections of sequentially dumped, weathered, dry disposed ash in an ash dump site at Tutuka - a South African coal burning power station. The core samples were characterized using standard analytical procedures viz: X-ray fluorescence (XRF), X-ray diffraction (XRD), Fourier transforms infrared (FTIR) techniques, Scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS) and Acid neutralisation capacity (ANC) test. A modified sequential extraction (SE) method was used in this study. The chemical partitioning, mobility and weathering patterns in 1 year, 8 year and 20-year-old sections of the ash dump were respectively investigated using this modified sequential extraction scheme. The sequence of the extractions was as follows: (1) water soluble, (2) exchangeable, (3) carbonate, (4) iron and manganese and (5) residual. The results obtained from the 5 steps sequential extraction scheme were validated with the total metal content of the original sample using mass balance method. The distribution of major and trace elements in the different liquid fractions obtained after each step of sequential extraction of the 59 drilled core samples was determined by inductively coupled plasma mass spectrometry (ICPMS). The data generated for various ash core samples were explored for the systematic analysis of mineralogical transformation and change in ash chemistry with ageing of the ash. Furthermore, the data was analyzed to reveal the impact of ingressed CO2 from atmosphere, infiltrating rain water and brine irrigation on the chemistry of ash core samples. Major mineral phases in original ash core samples prior to extraction are quartz (SiO2) and mullite (Al2O3·2SiO2). Other minor mineral phases identified were hematite (Fe2O3), calcite (CaCO3), lime (CaO), anorthite (CaAl2Si2O8), mica (Ca (Mg, Al)3 (Al3Si) O10 (OH)2), and enstatite (Mg2Si2O6). X-ray diffraction results show significant loss of crystallinity in the older ash cores. The presence of minor phases of calcite and mica in dry disposed ash cores are attributed to reduction in the pore water pH due to hydration, carbonation and pozzolanic reactions. The X-ray diffraction technique was unable to detect Fe-oxyhydroxide phase and morealuminosilicate phases in ash core samples due to their low abundance and amorphous character. X-ray fluorescence results of the original ash core samples showed the presence of major oxides, such as SiO2, Al2O3, Fe2O3, while CaO, K2O, TiO2, Na2O, MnO, MgO, P2O5, and SO3 occur in minor concentrations. The ratio of SiO2/Al2O3 classified the original core samples prior to extraction as a silico-aluminate class F fly ash. The ternary plot of major elements in 1-year-old ash core samples was both sialic and ferrocalsialic but 8 year and 20-year-old ash core samples were sialic in chemical composition. It is noteworthy that the mass % of SiO2 varies through the depth of the core with an increase of nearly 3 %, to 58 mass % of SiO2 at a depth of 6 m in the 1-year-old core whereas in the case of the 8-year-old core a 2 % increase of SiO2 to a level of 57.5 mass % can be observed at levels between 4-8 m, showing dissolution of major components in the matrix of older ash cores.. The Na2O content of the Tutuka ash cores was low and varied between 0.6-1.1 mass % for 1-year-old ash cores to around 0.6-0.8 mass % for 8-year-old ash cores. Sodium levels were higher in 1-year-old ash cores compared to 8 year and 20-year-old ashcores. Observed trends indicate that quick weathering of the ash (within a year) leached out Na+ from the ash dump. No evidence of Na+ encapsulation even though the ash dump was brine irrigated. Thus the dry disposal ash placement method does not result in a sustainable salt sink for Na-containing species over time. The total content of each of the elements in 1 year and 20-year-old ash cores was normalised with their total content in fresh ash from same power station to show enrichment and depletion factor. Major elements such as K+, Mn showed enrichment in 1-year-old ash cores whereas Al, Si, Na+, Ti, Ca, Mg, S and Fe showed depletion due to over time erosion. Trace elements such as Cr, Sr, P, Ba, Pb, V and Zn showed enrichment but Ni, Y, Zr showed depletion attributed to over time erosion. In 20-year-old ash cores, major elements such as Al, Na+ and Mn showed enrichment while Si, K+, Fe, Mg and Ca showed depletion highlighting their mobility. Trends indicated intensive flushing of major soluble components such as buffering constituents (CaO) by percolating rain water. The 1-year-old and 20-year-old coal ash cores showed a lower pH and greater loss/depletion of the soluble buffering constituents than the 2-week-old placed ash, indicating significant chemical weathering within a year. Based on ANC results the leaching behaviours of Ca, Mg, Na+, K+, Se, Cr, and Sr were found to be controlled by the pH of the leachant indicating high mobility of major soluble species in the ash cores when in contact with slightly acid rain water. Other investigated toxic metals such as As, Mo and Pb showed amphoteric behaviour with respect to the pH of the leachant. Chemical alterations and formation of transient minor secondary mineral phases was found to have a significant effect on the acid susceptibility and depletion pattern of chemical species in the core ash samples when compared to fresh ash. These ANC results correlated well with the data generated from the sequential extraction scheme. Based on sequential extraction results elements, showed noticeable mobility in the water soluble, exchangeable and carbonate fractions due to adsorption and desorption caused by variations in the pore water pH. In contrast, slight mobility of elements in the Fe and Mn, and residual fractions of dry disposed fly ashes are attributed to the co-precipitation and dissolution of minor amount of less soluble secondary phase overtime. The 1-year-old dry disposed ash cores were the least weathered among the 3 drilled ash cores. Therefore low concentration of toxic metals in older ash cores were ascribed to extensive weathering with slower release from residual mineral phases over time. Elements were found to associate with different mineral phases depending on the age or depth of the core samples showing greater heterogeneity in dispersion. For instance the average amount of total calcium in different mineral associations of 1-year-old ash cores is as follows; water soluble (10.2 %), exchangeable (37.04 %), carbonate (37.9 %), Fe and Mn (7.1 %) and residual (2.97 %). The amount of total Na+ in different mineral phases of 1-year-old ash cores followed this trend: water soluble (21 %), exchangeable (11.26 %), carbonate (2.6 %), Fe and Mn (4.7 %) and residual (53.9 %). The non-leachable portion of the total Na+ content (namely that contained in the residual fraction) in the 1-year-old ash core samples under conditions found in nature ranged between 5-91 %. This non-leachable portion of the Na+ showed the metastability of the mineral phases with which residual Na+ associates. Results showed older ash cores are enriched in toxic elements. Toxic elements such as As, B, Cr, Mo and Pb are enriched in the residual fraction of older ash cores. For instance As concentration in the residual fraction varied between 0.0003- 0.00043 mg kg-1 for 1-year-old ash cores to around 0.0003-0.0015 mg kg-1 for 20-year-old ash cores. This suggests that the older ash is enriched in toxic elements hence dust from the ash dump would be toxic to human health. The knowledge of mobility and ecotoxicological significance of coal fly ash is needed when considering its disposal or reuse in the environment. The mobility and ecotoxicology of inorganic metals in coal fly ash are determined by (i) mineralogical associations of inorganic species (ii) in-homogeneity in the ash dumps (iii) long and short term exposure to ingress CO2 and percolating rain water. Management issues such as inconsistent placement of ash in the dumps, poor choice of ash dump site, in-homogeneity in brine irrigation, no record of salt load put on the ash dumps and lack of proper monitoring requires improvement. The thesis provides justification for the use of the modified sequential extraction scheme as a predictive tool and could be employed in a similar research work. This thesis also proved that the dry ash disposal method was not environmental friendly in terms of overall leaching potential after significant chemical weathering. Moreover the study proved that the practice of brine co-disposal or irrigation on ash dumps is not sustainable as the ash dump did not act as a salt sink.
Homogeneity of nanophase electrocatalysts supported on mesoporous materials
(University of the Western Cape, 2006) Godongwana, Ziboneni Governor; Linkov, Vladimir M.; Petrik, Leslie F.; Dept. of Chemistry; Faculty of Science
Hydrothermal synthesis and optimisation of zeolite Na-P1 from South African coal fly ash
(2009) Musyoka, Nicholas Mulei; Petrik, Leslie F.
Millions of tonnes of fly ash are generated worldwide every year to satisfy the large demand for energy. Management of this fly ash has been a concern and various approaches for its beneficial use have been investigated. Over the last two decades, there has been intensive research internationally that has focused on the use of different sources of fly ash for zeolite synthesis.However, most of the studies have concentrated on class C fly ash and very few have reported the use of South African class F fly ash as feedstock for zeolite synthesis.Class F fly ash from South Africa has been confirmed to be a good substrate for zeolite synthesis due to its compositional dominance of aluminosilicate and silicate phases. However, because differences in quartz-mullite/glass proportions of fly ash from different sources produces impure phases or different zeolite mineral phases under the same activation conditions, the present study focused on optimization of synthesis conditions to obtain pure phase zeolite Na-P1 from class F South African coal fly ash. Synthesis variables evaluated in this study were; hydrothermal treatment time (12 - 48 hours), temperature (100 – 160 oC) and addition of varying molar quantities of water during the hydrothermal treatment step (H2O:SiO2 molar ratio ranged between 0 - 0.49).Once the most suitable conditions for the synthesis of pure phase zeolite Na-P1 from fly ash were identified, a statistical approach was adopted to refine the experiments, that was designed to evaluate the interactive effects of some of the most important synthesis variables. In this case, the four synthesis variables; NaOH concentration (NaOH: SiO2 molar ratio ranged between 0.35– 0.71), ageing temperature (35 oC – 55 oC), hydrothermal treatment time (36 - 60 hours) and temperature (130 oC – 150 oC) were studied. The response was determined by evaluating the improvement in the cation exchange capacity of the product zeolite.The starting materials (fly ashes from Arnot, Hendrina and Duvha power stations) and the synthesized zeolite product were characterized chemically, mineralogically and morphologically by X-Ray fluorescence spectrometry, X-ray powder diffraction, scanning electron microscopy, and transmission electron microscopy. Other characterization technique used in the study were Fourier transform infrared spectroscopy to provide structural information and also monitor evolution of crystallinity during synthesis, as well as cation exchange capacity to determine the amount of exchangeable positively charged ions. Nitrogen adsorption was used to determine the surface area and porosity, and inductively coupled mass spectrometry for multi-elemental analysis of the post-synthesis supernatants.The results from the X-ray diffraction spectroscopy showed that the most pure zeolite Na-P1 phase was achieved when the molar regime was 1 SiO2 : 0.36 Al2O3 : 0.59 NaOH : 0.49 H2O and at synthesis conditions such that ageing was done at 47 oC for 48 hours while the hydrothermal treatment time and temperature was held at 48 hours and 140 oC, respectively. Results from statistically designed experiments show that there was a distinct variation of phase purity with synthesis conditions. From the analysis of linear and non linear interactions, it was found that the main effects were ageing temperature and hydrothermal treatment time and temperature, which also showed some interactions. This experimental approach enabled a clearer understanding of the relationship between the synthesis conditions and the purity of the zeolite Na-P1 obtained.The quality of zeolites is a major determinant in the efficiency of toxic element removal from waste water. Preliminary experiments conducted using optimised zeolite Na-P1 obtained in this study with a cation exchange capacity of 4.11 meq/g showed a high percentage removal of Pb,Cd, Ni, Mn, V, As, B, Fe, Se, Mo Sr, Ba and Zn from process brine obtained from Emalahleni water reclamation plant.In summary, a pure phase of zeolite Na-P1 was obtained from South African class F fly ash feedstock at relatively mild temperature. The systematic approach, incorporating statistical design of experiments, developed in this study resulted in a better understanding regarding the relationships of synthesis parameters in the formation of zeolites from fly ash. The zeolite Na-P1 synthesized with a high cation exchange capacity was effective for removal of toxic elements from brine.
Identification and quantification of chemicals of emerging concern (persistence organic and inorganic pollutants) in some selected marine environments of Cape Town, South Africa
(University of Western Cape, 2020) Ojemaye, Cecilia Yejide; Petrik, Leslie F.
The increasing evidence of chemicals of emerging concern (CECs) in water bodies is causing major concern around the world because of their toxicological effects upon humans and aquatic organisms. The release of wastewater to the aquatic environment is most likely to introduce some trace levels of organic contaminants, some of which may be toxic, carcinogenic, or endocrine disruptors, as well as, persistent in the environment. These compounds are often persistent but not regularly monitored because they are mostly still excluded from environmental legislation. Their fate and persistence in the environment are not well understood
Identification and quantification of chemicals of emerging concern (persistent organic and inorganic pollutants) in some selected marine environments of cape town, South Africa
(University of the Western Cape, 2020) Ojemaye, Cecilia Yejide; Petrik, Leslie F.
The increasing evidence of chemicals of emerging concern (CECs) in water bodies is causing major concern around the world because of their toxicological effects upon humans and aquatic organisms. The release of wastewater to the aquatic environment is most likely to introduce some trace levels of organic contaminants, some of which may be toxic, carcinogenic, or endocrine disruptors, as well as, persistent in the environment. These compounds are often persistent but not regularly monitored because they are mostly still excluded from environmental legislation. Their fate and persistence in the environment are not well understood.
Identification, separation and quantification of persistent organic pollutants using capillary electrophoresis
(University of the Western Cape, 2022) Omoniyi, Emmanuel Oluseyi; Petrik, Leslie F.
Water quality deterioration and scarcity can be attributed to natural causes and anthropogenic activities which include climate change and an incessant industrialisation, yet with lack of functional and reliable wastewater treatment facilities. As a consequence of these activities, many chemicals have found their way into water bodies and subsequently compromise the quality of water systems. Among these chemicals are persistent organic pollutants (POPs), including pharmaceuticals, endocrine disrupting compounds (EDCs), etc. In order to separate, identify and quantify persistent and emerging contaminants in the water samples, this study considered the pre-concentration and separation steps followed by quantification using capillary electrophoresis.
Multi-component Platinum Group Metals for the methanol electro-oxidation process
(University of the Western Cape, 2018) Javu, Bulelwa Patricia; Petrik, Leslie F.
The purpose of this study was to develop a high performance-lower cost catalyst to be applied in Direct Methanol Fuel Cells (DMFC). The study also aimed to prepare plurimetallic supported platinum (Pt), platinum-ruthenium (PtRu), platinum-ruthenium-vanadium (PtRuV) and platinum ruthenium-vanadium-iron (PtRuVFe) upon multi-walled carbon nanotube (MWCNT) as well as upon multiwalled carbon nanotube-titanium oxide (MWCNT/TiO2) supports. Platinum is very active but prone to poisoning by carbon monoxide (CO), which may be present in the fuel used in fuel cells. The focus on the use of methanol was because of its better reaction kinetics, and better performance in direct methanol fuel cells (DMFC) better than proton exchange membrane fuel cell (PEMFC). When Pt is alloyed with another platinum group metals (PGM) the alloying decreases the over-potential for reactions critical in the fuel cells. Proton exchange membrane fuel cell (PEMFC) performance may be improved at low metal loading, when supported pluri-metallic catalysts are applied since the trimetallic catalysts may promote high catalyst utilisation. In practice, DMFC require electrodes with a Pt loading to achieve acceptance fuel cell (FC) power performance. The aim of this study was therefore the reduction of the catalyst loading through further improvement of mass activity of Pt based catalysts by partial substitution of the noble metal/metals, and the use of a carbon support that will provide high surface area, good electrical conductivity and high stability. MWCNT supported pluri-metallic (PtRuVFe,) and bimetallic (PtRu) nanoparticles possessed characteristic of increased surface area, improved electron transfer rate, enhance electro-catalytic activity and promoted stability.
Photocatalytic activity of supported TiO2 nanocrystals
(2013) Totito, Thandiwe Crystal; Petrik, Leslie F.
In recent times, the occurrence and presence of complex recalcitrant toxic contaminants in water and wastewater is increasing and consequently contributes to the non-availability of clean and safe drinking water. Water treatment is complex, time demanding and energy intensive due to the physico-chemical structural complexity and diversity of the pollutants. Non-availability of good drinking water has negatively affected human health and the ecosystem. Over the years, numerous conventional treatment techniques were used to degrade and remove these pollutants, but investigations indicated that some of the pollutants are not susceptible to conventional treatment. Advanced oxidation technology, among which heterogeneous photocatalysis (involving the use of a semiconductor) has emerged as one of the more promising techniques to remediate contaminated water. Titanium dioxide (TiO2) semiconductor photocatalysis is considered to be a good option due to its cost effectiveness, chemical and thermal stability, and inertness in the area of wastewater reclamation and re-use. However the post separation of the titania particles poses a threat to the wastewater remediation. Hence there is a need to develop a supported high surface area photocatalyst that will resolve the post separation challenge. This present study aimed to prepare high surface area TiO2 anatase nanocrystals supported on a stainless steel mesh. These new composite materials were used to remove methylene blue (MB) from aqueous solutions. The supporting procedure involved the thermal decomposition of a sol gel solution coated upon stainless steel mesh. The nanocrystalline anatase phase was formed by thermal decomposition on a stainless steel mesh coated with 8 % PAN/DMF/TiO2 sol gel formation calcined at varying temperatures of 300 °C, 400 °C, 500 °C and 600 °C. The heating rate of 50 °C/min and independent holding time of 1 h, 2 h, 3 h and 4 h were applied to find the optimum supporting conditions. The synthesised TiO2 nanocomposites materials were characterised using the following analytical techniques: XRD, HRSEM, EDS, HRTEM, SAED, FTIR and UV-Vis absorption spectroscopy materials were characterised, and the results indicate that synthesised TiO2 nanocrystals were in the anatase form, polycrystalline in nature, and contained additional carbon-carbon bonds from the polymer used during preparation with TiO2 particle sizes range from 13.6 nm to 2285 nm.
Pt Nanophase supported catalysts and electrode systems for water electrolysis
(University of the Western Cape, 2008) Petrik, Leslie F.; Iwuoha, Emmanuel I.; Dept. of Chemistry; Faculty of Science
In this study novel composite electrodes were developed, in which the catalytic components were deposited in nanoparticulate form. The efficiency of the nanophase catalysts and membrane electrodes were tested in an important electrocatalytic process, namely hydrogen production by water electrolysis, for renewable energy systems. The activity of electrocatalytic nanostructured electrodes for hydrogen production by water electrolysis were compared with that of more conventional electrodes. Development of the methodology of preparing nanophase materials in a rapid, efficient and simple manner was investigated for potential application at industrial scale. Comparisons with industry standards were performed and electrodes with incorporated nanophases were characterized and evaluated for activity and durability.
Re-use of South African fly ash for CO2 capture and brine remediation.
(University of the Western Cape, 2013) Muriithi, Grace Nyambura; Petrik, Leslie F.
Coal combustion accounts for 95% of electricity generation in South Africa while globally coal combustion for energy generation stands at 42%. It has been predicted that coal utilization for energy generation will continue due to its low cost and availability in huge quantities in different parts of the world. Additionally brine and gaseous emissions are produced in the power generation and coal combustion processes. In fact, it has been established that CO2 emissions from power plants are the main cause of the green-house effect leading to global warming. Mitigation of the effects of disposal of fly ash, brine and CO2 emissions is critical for sustainable energy generation from coal and environmental protection. The study investigated whether South African coal fly ash could be used for brine remediation and CO2 capture using fly ash based hydrotalcites and zeolites. Four main objectives were investigated. These were; firstly, to compare the natural CO2 capture potential of a power station ash dam with an accelerated ex-situ mineral carbonation process. Secondly, to probe the effect of accelerated ex-situ mineral carbonation on brine quality with regards to major, minor and trace elements concentration. Furthermore, the study investigated the feasibility of synthesizing hydrotalcites from fly ash by optimizing the synthesis parameters such as acid concentration, aging time, aging temperature, pH during aging, crystallization time and crystallization temperature. Finally the study compared the CO2 adsorption capacities of the fly ash based hydrotalcites with fly ash based zeolites NaA, and NaX. The natural carbonation potential of the wet disposed ash dam at Secunda was investigated by coring a 20 year old dam. Three cores (SI, S2 and S3) were obtained by air flush coring the dam along a geophysical line and establishing the geophysical profile of the three cores. The surface of the three cores was of medium resistivity with values between 9.3 and 12.2 nm while the midsections were of low resistivity with values ranging between 4 and 7 nm. The base section of core SI had a resistivity of 28.3 nm, that of S2 was between 16.2 and 21.4 nm and that of S3 between 12.2 and 16.2 nm; implying that SI had the lowest salt load while S3 had the highest salt content. Moisture content was observed to be high deeper down the profiles of S2 and S3 with samples appearing water logged while SI had the highest moisture content at the surface showing the inhomogeneity of the ash dam. The morphology of fresh fly ash taken from the ash collection hoppers at Secunda was observed to be spherical. Weathered ash from the ash dam showed irregularly agglomerated particles while accelerated ex-situ mineral carbonation resulted in the formation of acicular particles of calcite. Fresh ash, weathered ash and the accelerated carbonated ash were all class F with a sum total of silica, alumina and iron oxide totaling more than 70%. A reduction in silica and alumina content with instability of fly ash. Dumping of spent iron catalyst (resulting from the petrochemical operations as Sasol) on the ash dam led to an increase in Fe203 content of the weathered ash. Enrichment of Nb, Sr, Y, Th, Na, Cl, S04, K and S with natural carbonation as well as during accelerated ex-situ mineral carbonation was observed and was due to the contact of ash with brine during these two processes. Reduction of Zr, Rb, Pb, Ni, Co and V content of ash was observed with weathering. Mineralogically, all the ash samples had main phases of mullite, quartz, magnetite and hematite, with weathered and accelerated carbonated ash having additional phases of calcite. The aluminosilicious nature of the three ashes was identified by structural evaluation using Fourier transform infrared analysis which revealed that, bands associated with C-O in-plane and out of plane bending of carbonates was only visible in weathered and carbonated ash.
Recovery of SiO₂ and Al₂O₃ from coal fly ash
(University of the Western Cape, 2016) Sedres, Grant; Petrik, Leslie F.; Fatoba, Olanrewaju O.
Most of the world's energy production is still mainly achieved by the combustion of coal in power stations. Coal fly ash is the inevitable waste product that accumulates to metric ton volumes each year. These vast volumes pose a problem in the disposal of the coal fly ash which conventionally is loaded onto ash dumps located near the coal power stations. Alternatives need to be investigated for the use of the coal fly ash in applications that would make the coal fly ash useful and thereby help to mitigate the environmental strain imposed by conventional ash dump disposal. This study focussed on investigating the extraction of Si and Al from CFA. The investigation into the removal of the magnetic iron oxide content and calcium content from coal fly ash was also carried out to enhance the extraction of the Si and Al from CFA e.g. the removal of calcium was attempted to promote the leaching of aluminium from the ash. The rationale for this process was that by removing and recovering these major constituent elements from the ash, it would be easier to concentrate and isolate the trace elements especially the rare earth elements that are present in the CFA. Coal fly ash sourced from Matla coal power station was characterised using x-ray diffraction to determine the mineral phases present in the raw coal fly ash and elemental composition determined by x-ray fluorescence and laser ablation ICP-MS. The main mineral phases in coal fly ash were determined to be quartz, mullite, magnetite and lime (CaO). Magnetic extraction was initially carried out on the coal fly ash to remove the iron rich magnetic material. Extraction tests were then performed on the coal fly ash using alkaline and acidic media namely; NaOH, HCl and H₂SO₄. The extraction tests were assessed and a sequential extraction experimental procedure developed to achieve the highest extraction yield for Si, Al, Fe, Ca, and Mg from the coal fly ash. Lastly the rare earth element content in coal fly ash was tracked from the beginning till the end of the sequential extraction procedure to ascertain whether the rare earth elements partitioned to the leachates or the solid residues. The total element recoveries for Al, Si, Ca Fe, Mg were 53.36 %, 39.96 %, 93.8 %, 25.6 % and 67.3 % respectively using the sequential extraction procedure developed in this study. The rare earth elements contents were not affected by the sequential extraction procedure and on the whole remained in the solid residues at the completion of the sequential extraction, resulting in a residue with enriched levels of recoverable or extractable REE content after the removal of the major oxides from the CFA. The lowest enrichment being approximately 5 % for Thulium and the highest being approximately 76 % for Erbium.

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