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Cereal based foods, including breakfast cereals and Asian noodles are potentially good sources of selenium. Although these are major foods consumed globally, their contribution to dietary intakes of selenium is unclear. In addition, there has been very limited research into the effect of processing steps on the analysis and apparent retention of selenium. The low levels typically present in foods and the presence of multiple chemical forms of the element provide significant analytical challenges to research in this area. Therefore, the aims of this study were firstly to evaluate and validate procedures for extraction and measurement of selenium in wheat flour. Secondly, the procedure has been applied to analysis of selenium in cereal foods. The methods employed were firstly validated using wheat-based reference materials and then samples of various breakfast cereals as well as different styles of Asian noodles were analysed. Selenium was extracted using closed- v essels by microwave digestion with a mixture of nitric acid and hydrogen peroxide, followed by determination through Inductively Coupled Plasma - Mass Spectrometry (ICP-MS). The optimum conditions for selenium determination in cereal based foods involved the digestion of 0.1 g samples using 1 mL of nitric acid and 1 mL of hydrogen peroxide. The addition of 1% (v/v) methanol was found to enhance the sensitivity of the ICP-MS system. Two particular isotopes of selenium (77 and 82) could be effectively employed in the analysis and there was no significant decrease in total selenium in the digested extracts during storage for up to twelve days under refrigeration and room temperature conditions. Good precision levels were obtained and the total selenium levels in the breakfast cereal samples ranged from 0.059 to 0.378 µg/g. For white salted noodles the values varied between 0.057 and 0.712 µg/g, for yellow alkaline noodles, 0.109 to 0.265 µg/g and 0.077 to 0.284 µg/g for fried instant noodles. There was no appar ent change observed in total selenium during the processing of fried instant noodles, indicating the effectiveness of the extraction method developed here. It is concluded that microwave digestion is an effective approach to sample extraction, the procedures validated in this study are suitable for cereal grain foods and that there is considerable variation in the selenium contents of breakfast cereal and Asian noodle products.

Landfilling is the most common method that is used in the final disposal of sludge all around the world as well as in Turkey. However increasing sludge quantities and limited landfilling areas make this method invalid. Use of sludge in agriculture presents a possible alternative for disposal. However, it also poses some risks to be evaluated. In this respect, it is important to identify heavy metal and pathogen content of sewage sludges because of their adverse health effects. This study aims to determine the heavy metal contents and pathogen levels of sludges from four different wastewater treatment plants of Turkey. The selection of plants was done according to the different treatment technologies applied to wastewater and sludge in those plants. Heavy metal analysis of sludges was conducted by using microwave assisted digestion procedure and pathogen levels were done by methods from Standard Methods (SM), ISO and USA EPA. After sampling and analysis, the results show that all the related metal concentrations are below the values that are set in the Soil Pollution Control Regulation of Turkey. However in sludges from Ankara and Kayseri wastewater treatment plants, Zinc and Nickel concentrations should be tracked carefully. The results related with pathogen levels in sludges show that dewatered sewage samples taken from Ankara, Kayseri and Kemer wastewater treatment plants do not meet neither Class A nor Class B fecal coliform limits set by USA EPA however lime stabilized dewatered sludge from izmir wastewater treatment plant meet the requirement. In addition, Salmonella levels in Kayseri dewatered sludges exceed the limit value.

High-temperature reactors make use of tri-structural coated fuel particles as basic fuel components. These TRISO particles consist of fissionable uranium dioxide fuel kernels, about 0.5 mm in diameter, with each kernel individually encased in four distinct coating layers, starting with a porous carbon buffer, then an inner pyrolytic carbon (IPyC) layer, followed by a layer of ceramic silicon carbide (SiC) and finally an outer pyrolytic carbon layer (OPyC). Collectively, the coating layers provide the primary barrier that prevents release of fission products generated during burn up in the UO2 fuel kernel. It is crucial to understand how the fission products contained within the fuel interact with the coating layers and how they are distributed within the fuel. The first step commonly performed to obtain the information on distribution is removal of the coating layers. The purpose of this study was to investigate the possible use of wet chemical etching techniques with the aim of removing the coating layers of ZrO2 coated fuel particles in a controlled way and to establish experimental parameters for controlled dissolution of irradiated fuel particles. Stepwise dissolution of coated fuel particle coating layers, containing zirconia kernels has been investigated by chemical etching experiments with acidic solutions of different mixtures. The heating methods used include heating by conventional methods, hot plates and a muffle furnace, a reflux-heating system and microwave-assisted digestion. The etching mixtures were prepared from a number of oxidizing acids and other dehydrating agents. The capability of each reagent to etch the layer completely and in a controlled manner was examined. On etching the first layer, the OPyC, the reflux heating method gave the best results in removing the layer, its advantage being that the reaction can be carried out at temperatures of about 130 ºC for a long time without the loss of the acid. The experimental results demonstrated that a mixture composed of equal amounts of concentrated nitric and sulfuric acid mixed with chromium trioxide dissolves the OPyC layer completely. The most favourable experimental conditions for removal of OPyC from a single coated fuel particle were identified and found to depend on the etching solution composition and etching temperature. Light microscopy yielded first-hand information on the surface features of the samples. It allowed fast comparison of etched and untreated sample features. The outer surface of particles prior to chemical etching of the outer pyrolytic carbon layer appeared black in colour with an even surface compared to the etched surfaces which appeared to have an uneven metallic grey, shiny texture. The scanning electron microscope (SEM) examination of the chemically treated outer carbon layer samples gave information on the microstructure and it demonstrated that the outer pyrolytic carbon layer could be readily removed using a solution of HNO3/H2SO4/CrO3, leaving the exposed SiC layer. Complete removal of the layer was confirmed by energy dispersive X-ray spectroscopic (EDS) analysis of the particle surface. For etching the second layer, the silicon carbide layer, microwave-assisted chemical etching was the only heating technique found to be useful. However, experimental results demonstrated that this method has limited ability to digest the sample completely. Also common chemical etchants were found to be ineffective for dissolving this layer. Only fluoride containing substances showed the potential to etch the layer. The results show that a mixture consisting of equal amounts of concentrated hydrofluoric and nitric acid under microwave heating at 200 ºC yielded partial removal of the coating and localized attack of the underlying coating layers. The SEM analyses at different intervals of etching showed: partial removal of the layer, attack of the underlying layers and, in some instances, that attack started at grain boundaries and progressed to the intra-granular features. The SEM results provide evidence that etching of the silicon carbide layer is strongly influenced by its microstructure. From these findings, it is concluded that etching of the silicon carbide under the investigated experimental conditions yields undesirable results and that it does not provide complete removal of the layer. This method has the potential to etch the layer to some extent but has limitations. Copyright / Dissertation (MSc)--University of Pretoria, 2013. / Chemical Engineering / unrestricted

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Also aged bottles are safer to use than new bottles because their chemical leaching was found to be lower than that of new bottles. This study recommends the reassessment of the absence of international guidelines for acetaldehyde in water and foods. The study also recommends that the amount of acetaldehyde that can be added to soft drinks as flavouring agent should be below the specific migration limit (SML) for migration of acetaldehyde from PET bottle into bottle contents. This is essential since the SML was designed to ensure that exposure to acetaldehyde, as a result of intake of bottled water and soft drinks in PET bottles, is below the tolerable daily intake (TDI) for acetaldehyde. As antimony was reported to go beyond the safe limits in some Nigerian bottled water and soft drinks after 11 months of storage this study discourages the use of bottle contents stored for a very long time.

Polyethylene terephthalate (PET) is an excellent material for bottling water, beverages, edible oils and other liquids because it is light, tough and transparent. PET bottles are also extensively reused for storage of drinking water, beverages and other liquids and for solar disinfection of microbiologically unsafe drinking water in the tropics. In spite of the usefulness of PET bottles earlier works have reported leaching of antimony and acetaldehyde from the bottle matrix into the liquid contents. Both antimony trioxide and acetaldehyde belongs to Group 2B (possible carcinogens) in the International Agency for Research on Cancer (IARC) carcinogen classification. Additionally acetaldehyde associated with alcoholic beverages (derived from alcoholic beverage and formed endogenously) has recently been upgraded to IARC Group 1 carcinogen (carcinogenic to humans). The research aims to assess the pattern and extent of antimony and acetaldehyde migration from British and Nigerian polyethylene terephthalate bottles into bottle contents under typical use and reuse conditions. The research compares the assessed extents of migration with the current regulations to determine whether the maximum acceptable levels of antimony and acetaldehyde are being exceeded and whether current regulations might need to be reassessed. To achieve these goals the pattern and extent of PET bottle use and reuse in Britain and Nigeria were appraised through survey. The survey revealed that new bottles with contents are typically stored prior to use for periods ranging between one and 7 days, with Nigerians storing for longer periods than British respondents. However storage of up to one year was reported. The extent of bottle reuse was high and similar for the two countries. Nevertheless Nigerian respondents reuse bottles for longer periods than British respondents. The survey findings together with relevant literature were used to design laboratory experiments that assessed the extent of antimony and acetaldehyde migration from PET bottles into water/beverages. A total of 82 brands of bottled water and soft drinks in plastic and glass bottles and in cartons were collected. A few samples from Nigeria in plastic pouches were collected. Materials used in bottling including glass and plastic bottle materials, metal and plastic bottle cap materials and plastic cap lining materials were collected. All samples were collected in supermarkets and shops in Britain and Nigeria except drinking water from taps which was collected in Britain only. Some bottles were aged for the purpose of studying the impact of bottle aging on chemical migration. Other bottles were stored with their contents to study the impact of long term storage of bottle contents on chemical migration. Energy dispersive X-ray spectrometry (EDX) and Raman spectroscopy were used to characterise PET bottle material and other materials associated with water and soft drink bottling. Antimony and other trace metals in water and soft drinks were determined using Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Antimony content of PET and other plastics was determined by microwave digestion and ICP-MS. Acetaldehyde content of water and soft drinks and PET were determined using headspace gas chromatography with flame ionisation detection (GC-FID). Accuracy and precision for determination of antimony and other trace elements in bottle materials and bottle contents were good as recoveries were around 100% and coefficients of variation were less than 15% for all analysis types. Accuracy and precision for determination of acetaldehyde in bottle materials and bottle contents were also good as recoveries were around 100% and coefficients of variation were less than 15% for all analysis types. Impact of long term storage, elevated temperatures, bottle thickness, carbonation, bottle aging and bottle size on migration of antimony and acetaldehyde were also assessed. All plastic bottle materials analysed were found to be PET. Bottle cap materials were either polyethylene or polypropylene. All plastic cap lining materials from Britain and some from Nigeria were found to be ethylene vinyl acetate/polypropylene copolymer. Plastic cap lining materials from some Nigerian soft drinks were identified as polyvinyl chloride. Glass bottle materials analysed were found to be soda-lime glass. Metal bottle caps were identified as tinplate, tin-free-steel coated with chromium or aluminium coated with chromium. The antimony concentration in 32 PET bottle materials from Britain and Nigeria were similar and ranged between 177 and 310 mg/kg with an average of 250±30 mg/kg. The concentration agrees well with the industry reported concentration of between 150 and 350 mg/kg. The concentration of residual acetaldehyde in 25 fresh PET bottle materials from Britain and Nigeria ranged between 0.95 and 12.52 µg/g. The average concentration in British and Nigerian soft drinks PET materials are 4.76 and 2.17µg/g respectively. Concentration of residual acetaldehyde was higher in soft drinks and still water PET materials than in sparkling water materials. The concentration of residual acetaldehyde decreases as the bottle wall material becomes older. Also the thinner the bottle walls the lower the concentration of residual acetaldehyde. Antimony concentration in 47 freshly purchased British bottled water and soft drinks ranged between 0.03 and 6.61µg/L with only one sample going above the EU acceptable limit. Concentrations of other trace elements measured were low except titanium which was detected at part per million levels in soft drinks. Lead content of a Nigerian soft drink in glass bottle stored for 2 months was above the EU acceptable limit for lead. At realistic temperatures of 40 and 60°C antimony concentration in the water remained below the EU acceptable limit even after 48 hours of exposure but the concentration exceeded the limit for most exposures at 80°C. Concentration of antimony in some Nigerian bottled water and soft drinks was above the EU limit after 11 months of storage at room temperature. Aged bottles leach lower amount of antimony than new bottles. Similarly larger bottles leach lower amount of antimony than smaller bottles. The average acetaldehyde concentrations found in British fruit juices, carbonated soft drinks, sparkling water and still water were 5113, 1458, 22 and 8 µg/L respectively. Acetaldehyde was not detected in water bottled in glass. The concentration of acetaldehyde in five fruit juice samples in PET bottles and carton was beyond the EU specific migration limit (SML) of 6mg/kg. Also the tolerable daily intake of acetaldehyde could be exceeded as a result of intake of some soft drinks and fruit juices. Acetaldehyde content in soft drinks increase with storage but the increase cannot be accounted for by the residual acetaldehyde in PET. Acetaldehyde was found to be outgassing from some bottles. It was also found to be capable of migrating from soft drinks into bottle wall. Without replenishment the concentration of acetaldehyde in solution decreases with time. The use of PVC cap lining in Nigeria as found in this study is a cause for concern as PVC is associated with health risk issues. The study recommends actions to ensure that antimony in fruit juices and other bottled products remain within the regulatory standard from bottling to consumption for the purpose of safeguarding the health of consumers. Glass used in bottling should be well scrutinized to ensure that it does not contain high levels of lead or other chemical substances that can cause harm to consumers through migration into contents. PET bottles can safely be used for solar water disinfection without the risk of antimony intake at concentrations above safe limits as water temperature achievable as the result of the technique doesn¿t go beyond 60°C. Also aged bottles are safer to use than new bottles because their chemical leaching was found to be lower than that of new bottles. This study recommends the reassessment of the absence of international guidelines for acetaldehyde in water and foods. The study also recommends that the amount of acetaldehyde that can be added to soft drinks as flavouring agent should be below the specific migration limit (SML) for migration of acetaldehyde from PET bottle into bottle contents. This is essential since the SML was designed to ensure that exposure to acetaldehyde, as a result of intake of bottled water and soft drinks in PET bottles, is below the tolerable daily intake (TDI) for acetaldehyde. As antimony was reported to go beyond the safe limits in some Nigerian bottled water and soft drinks after 11 months of storage this study discourages the use of bottle contents stored for a very long time. / Commonwealth Scholarship Commission in the United Kingdom

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