The classification of agricultural products according to geographical origin by means of quadrupole-based ICP-mass spectrometry for the determination of ¹¹B/¹°B isotope ratios, and the study of boron isotope fractionation
- Authors: Greeff, Liezl
- Date: 2010-04-01T05:32:05Z
- Subjects: Wine and wine making , Boron isotopes , Inductively coupled plasma mass spectrometry , Provenance trials
- Type: Thesis
- Identifier: uj:6740 , http://hdl.handle.net/10210/3148
- Description: M.Sc. , The 11B/10B stable isotope ratio in wine- and provenance soil samples of four South African wine regions was determined by means of quadrupole inductively coupled plasma mass spectrometry (ICP-MS). The data obtained was combined with multi-element results for the same samples. Discriminant analysis and ANOVA statistics were utilized to create a footprint of wines compared to their provenance soil. The results showed that the stable boron isotope ratio was a distinguishable characteristic in wine and soil samples for the Stellenbosch, Robertson, Swartland, and Walker Bay wine regions. The potential improvement of precision and accuracy was investigated specifically for ICP-QMS (quadrupole mass spectrometry) analysis of boron isotope ratios. Sample preparation methods for the matrices used in this work were developed and applied. The influence of the matrix components was investigated. Ion exchange separation procedures were developed for the separation of total B from the wine and soil matrices. Results were treated mathematically to minimize mass bias effects. It was found that combined matrix effects and TDS (total dissolved solids) deposition did have a pronounced effect on the 11B/10B isotope ratios of the samples. The possibility of boron isotope fractionation was investigated in vine plants. Hydroponic experiments were set up with test plants of two cultivars. A 10B enriched nutrient solution or growth solution with natural 11B/10B ratio was supplied to the plants during alternating periods of 5 weeks each. New growth leaves were harvested once every week during each of these time periods. All samples were carefully prepared and analyzed to determine the relationship of the 11B/10B ratio in the leaves compared to that of the supplied nutrient solution. It was observed that the 11B/10B isotope ratio of the growth solution had an influence on the 11B/10B stable isotope ratio in new growth leaves of vine plants.
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- Authors: Greeff, Liezl
- Date: 2010-04-01T05:32:05Z
- Subjects: Wine and wine making , Boron isotopes , Inductively coupled plasma mass spectrometry , Provenance trials
- Type: Thesis
- Identifier: uj:6740 , http://hdl.handle.net/10210/3148
- Description: M.Sc. , The 11B/10B stable isotope ratio in wine- and provenance soil samples of four South African wine regions was determined by means of quadrupole inductively coupled plasma mass spectrometry (ICP-MS). The data obtained was combined with multi-element results for the same samples. Discriminant analysis and ANOVA statistics were utilized to create a footprint of wines compared to their provenance soil. The results showed that the stable boron isotope ratio was a distinguishable characteristic in wine and soil samples for the Stellenbosch, Robertson, Swartland, and Walker Bay wine regions. The potential improvement of precision and accuracy was investigated specifically for ICP-QMS (quadrupole mass spectrometry) analysis of boron isotope ratios. Sample preparation methods for the matrices used in this work were developed and applied. The influence of the matrix components was investigated. Ion exchange separation procedures were developed for the separation of total B from the wine and soil matrices. Results were treated mathematically to minimize mass bias effects. It was found that combined matrix effects and TDS (total dissolved solids) deposition did have a pronounced effect on the 11B/10B isotope ratios of the samples. The possibility of boron isotope fractionation was investigated in vine plants. Hydroponic experiments were set up with test plants of two cultivars. A 10B enriched nutrient solution or growth solution with natural 11B/10B ratio was supplied to the plants during alternating periods of 5 weeks each. New growth leaves were harvested once every week during each of these time periods. All samples were carefully prepared and analyzed to determine the relationship of the 11B/10B ratio in the leaves compared to that of the supplied nutrient solution. It was observed that the 11B/10B isotope ratio of the growth solution had an influence on the 11B/10B stable isotope ratio in new growth leaves of vine plants.
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A critical evaluation of physical water treatment for the prevention of scale
- Authors: Howell, Sanja Steyn
- Date: 2012-08-15
- Subjects: Calcium carbonate , Incrustations , Descaling , Water - Purification
- Type: Thesis
- Identifier: uj:9343 , http://hdl.handle.net/10210/5782
- Description: M.Sc. , Calcium carbonate scale formation is a major problem in industrial water and cooling systems as well as in household systems. The resulting reduction in heat transfer and the removal of the scale are very costly processes. One of the methods used in the past 50 years and investigated for nearly a century, is the use of physical fields to reduce, remove and / or inhibit scale formation. These physical fields are usually magnetic fields, but RF electric and electrostatic fields are also used. These fields are claimed to reduce the cost involved in the removal of scale to a minimum. To investigate these claimed effects on scale formation, a pure calcium bicarbonate solution was exposed to some of the commercial available units: The exposed solution was then forced to precipitate by elevating the temperature. The pH was monitored against time, to investigate the nucleation process of CaCO 3 and the resulting precipitate analysed for changes in crystal morphology. The principle conclusions made from the results were, firstly that the nucleation of CaCO 3 was significantly delayed in one of the units tested and that the preferred morphology was changed from the thermodynamically more stable calcite to the more unstable aragonite in that unit. Secondly, that a direct correlation existed between the release of trace amounts of metals from the unit and the observed effects.
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- Authors: Howell, Sanja Steyn
- Date: 2012-08-15
- Subjects: Calcium carbonate , Incrustations , Descaling , Water - Purification
- Type: Thesis
- Identifier: uj:9343 , http://hdl.handle.net/10210/5782
- Description: M.Sc. , Calcium carbonate scale formation is a major problem in industrial water and cooling systems as well as in household systems. The resulting reduction in heat transfer and the removal of the scale are very costly processes. One of the methods used in the past 50 years and investigated for nearly a century, is the use of physical fields to reduce, remove and / or inhibit scale formation. These physical fields are usually magnetic fields, but RF electric and electrostatic fields are also used. These fields are claimed to reduce the cost involved in the removal of scale to a minimum. To investigate these claimed effects on scale formation, a pure calcium bicarbonate solution was exposed to some of the commercial available units: The exposed solution was then forced to precipitate by elevating the temperature. The pH was monitored against time, to investigate the nucleation process of CaCO 3 and the resulting precipitate analysed for changes in crystal morphology. The principle conclusions made from the results were, firstly that the nucleation of CaCO 3 was significantly delayed in one of the units tested and that the preferred morphology was changed from the thermodynamically more stable calcite to the more unstable aragonite in that unit. Secondly, that a direct correlation existed between the release of trace amounts of metals from the unit and the observed effects.
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The role of zinc in physical water treatment for prevention of scale
- Authors: Mubenga, Simon Bakakenga
- Date: 2012-08-17
- Subjects: Calcium carbonate , Incrustations , Descaling , Water -- Purification , Zinc
- Type: Thesis
- Identifier: uj:2651 , http://hdl.handle.net/10210/6096
- Description: M.Sc. , Dissolved salts, mainly carbonates and sulphates such as those of calcium and magnesium, form hard water, which when heated produces an insoluble precipitate of scale forming crystals. Scale formation affects performance in industry and ouseholds. Besides the problem of energy costs, there are all the additional problems and maintenance costs of scale removal. Traditional methods of combatting scale build-up based on chemical water treatment do exist. These include: the addition of strong acid to remove the bicarbonate ion from the water, the use of chemicals to prevent or retard the formation of hard scale and, other techniques such as ion exchange process. A cost-effective alternative to these methods is Physical Water Treatment (PWT). Many different types of equipment claiming to treat water physically, for scale reduction are commercially available. These include magnetic, electric (high frequency or radio frequency) or electrostatic, catalytic and ultrasonic devices. In this work attempts have been made to unravel the mechanisms involved in PWT. For this it was necessary to develop experimental methods to determine the effect of electromagnetic fields and selected magnetic and radio frequency (rf) water treatment devices on precipitation reactions. The most significant finding of this study involves the effect of Zn on scale formation. When supersaturated Ca(HCO3 )2 solutions were tested in a glass heat exchanger, a 77% reduction in the formation of scale was found when the solutions were spiked with Zn.
- Full Text:
- Authors: Mubenga, Simon Bakakenga
- Date: 2012-08-17
- Subjects: Calcium carbonate , Incrustations , Descaling , Water -- Purification , Zinc
- Type: Thesis
- Identifier: uj:2651 , http://hdl.handle.net/10210/6096
- Description: M.Sc. , Dissolved salts, mainly carbonates and sulphates such as those of calcium and magnesium, form hard water, which when heated produces an insoluble precipitate of scale forming crystals. Scale formation affects performance in industry and ouseholds. Besides the problem of energy costs, there are all the additional problems and maintenance costs of scale removal. Traditional methods of combatting scale build-up based on chemical water treatment do exist. These include: the addition of strong acid to remove the bicarbonate ion from the water, the use of chemicals to prevent or retard the formation of hard scale and, other techniques such as ion exchange process. A cost-effective alternative to these methods is Physical Water Treatment (PWT). Many different types of equipment claiming to treat water physically, for scale reduction are commercially available. These include magnetic, electric (high frequency or radio frequency) or electrostatic, catalytic and ultrasonic devices. In this work attempts have been made to unravel the mechanisms involved in PWT. For this it was necessary to develop experimental methods to determine the effect of electromagnetic fields and selected magnetic and radio frequency (rf) water treatment devices on precipitation reactions. The most significant finding of this study involves the effect of Zn on scale formation. When supersaturated Ca(HCO3 )2 solutions were tested in a glass heat exchanger, a 77% reduction in the formation of scale was found when the solutions were spiked with Zn.
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Precise 87Sr/86Sr isotope ratio measurement by quadrupole based ICP-MS after ion exchange separation of Rb for provenance determination of agricultural products
- Authors: Vorster, Clarisa
- Date: 2010-04-08T08:33:41Z
- Subjects: Wine and wine making , Strontium isotopes , Inductively coupled plasma mass spectrometry , Ion exchange chromatography , Provenance trials
- Type: Thesis
- Identifier: uj:6750 , http://hdl.handle.net/10210/3158
- Description: M.Sc. , The strontium isotope ratio 87Sr/86Sr in the wine and soil of four wine-producing regions in South Africa has been determined using quadrupole ICP-MS. Isotope ratio measurements with fairly good precision had been obtained and 87Sr/86Sr ratio values in wine and soil samples were statistically evaluated to determine whether the regions investigated could be distinguished. Statistical interpretation of data revealed that the Robertson wine-producing region could be distinguished from Stellenbosch, Swartland and Walker Bay wine regions on the basis of their 87Sr/86Sr ratio. By using a combination of 87Sr/86Sr and multielement data, canonical discriminant functions with very good classification abilities could be obtained to correctly distinguish between wine and soil samples originating from a specific production region. Due to the isobaric overlap of strontium and rubidium at mass 87, a very good strontium-rubidium separation method had to be developed. The chelating properties of EDTA and DCTA in combination with ion exchange chromatography were explored in order to achieve such a separation. Due to the advanced rubidium separation ability of the developed DCTA elution method, it has been employed in all wine and soil sample preparations. Since chromatographic ion exchange procedures are not capable of removing all the rubidium from the sample matrices, 87Sr/86Sr ratio values were mathematically corrected for residual rubidium using an 88Sr correction. Since strontium isotope ratio measurements require very good precision, it is traditionally determined using TIMS. However, due to the ease of operation, shorter analysis time and widespread availability of quadrupole ICP-MS, the technique was evaluated for its merit for determining strontium isotope ratios. The optimization of acquisition parameters for the determination of the 87Sr/86Sr ratio in wine and soil samples with good precision of below 0.1% RSD has been conducted. Furthermore, selected sample matrix components were assessed as possible matrix interferences as well as for their ability to affect the precision of measurements. It was concluded that with adequate optimization of acquisition parameters, proper sample preparation and reliable mathematical correction of data, 87Sr/86Sr ratio measurements with reasonable precision could be obtained using quadrupole ICP-MS.
- Full Text:
- Authors: Vorster, Clarisa
- Date: 2010-04-08T08:33:41Z
- Subjects: Wine and wine making , Strontium isotopes , Inductively coupled plasma mass spectrometry , Ion exchange chromatography , Provenance trials
- Type: Thesis
- Identifier: uj:6750 , http://hdl.handle.net/10210/3158
- Description: M.Sc. , The strontium isotope ratio 87Sr/86Sr in the wine and soil of four wine-producing regions in South Africa has been determined using quadrupole ICP-MS. Isotope ratio measurements with fairly good precision had been obtained and 87Sr/86Sr ratio values in wine and soil samples were statistically evaluated to determine whether the regions investigated could be distinguished. Statistical interpretation of data revealed that the Robertson wine-producing region could be distinguished from Stellenbosch, Swartland and Walker Bay wine regions on the basis of their 87Sr/86Sr ratio. By using a combination of 87Sr/86Sr and multielement data, canonical discriminant functions with very good classification abilities could be obtained to correctly distinguish between wine and soil samples originating from a specific production region. Due to the isobaric overlap of strontium and rubidium at mass 87, a very good strontium-rubidium separation method had to be developed. The chelating properties of EDTA and DCTA in combination with ion exchange chromatography were explored in order to achieve such a separation. Due to the advanced rubidium separation ability of the developed DCTA elution method, it has been employed in all wine and soil sample preparations. Since chromatographic ion exchange procedures are not capable of removing all the rubidium from the sample matrices, 87Sr/86Sr ratio values were mathematically corrected for residual rubidium using an 88Sr correction. Since strontium isotope ratio measurements require very good precision, it is traditionally determined using TIMS. However, due to the ease of operation, shorter analysis time and widespread availability of quadrupole ICP-MS, the technique was evaluated for its merit for determining strontium isotope ratios. The optimization of acquisition parameters for the determination of the 87Sr/86Sr ratio in wine and soil samples with good precision of below 0.1% RSD has been conducted. Furthermore, selected sample matrix components were assessed as possible matrix interferences as well as for their ability to affect the precision of measurements. It was concluded that with adequate optimization of acquisition parameters, proper sample preparation and reliable mathematical correction of data, 87Sr/86Sr ratio measurements with reasonable precision could be obtained using quadrupole ICP-MS.
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Critical evaluation and application of sequential extraction for sediment analysis
- Authors: Gouws, Karen
- Date: 2012-08-27
- Subjects: Sedimentation analysis , Extraction (Chemistry) , Water - Analysis
- Type: Thesis
- Identifier: uj:3261 , http://hdl.handle.net/10210/6669
- Description: M.Sc. , Sediment analysis, especially for trace metals, is important since aquatic sediments act as sinks for metals in the environment. Total element analysis yields insufficient information on the bioavailability and the geochemical fate of these metals. Sequential extraction procedures were developed to determine the partitioning of metals in sediment phases. The need for comparability of data produced world-wide led to the development of a sequential extraction procedure, which was proposed by the Community Bureau of Reference as a standard procedure (refered to as the BCR protocol). We contributed to the validation of the BCR procedure by using well-defined in-house model sediments. The results obtained for the model sediments showed that the BCR procedure could distinguish effectively between anthropogenically introduced metals and metals that form part of the mineral structure of the sediment components. The BCR procedure was applied to the sediments of the Vaal Dam and its contributing rivers. The amount of metals extracted in the first three steps of the sequential extraction procedure were low, indicating a very small contribution of anthropogenically introduced metals. It was therefore concluded that these sediments were relatively unpolluted compared to water systems in, for example, Europe.
- Full Text:
- Authors: Gouws, Karen
- Date: 2012-08-27
- Subjects: Sedimentation analysis , Extraction (Chemistry) , Water - Analysis
- Type: Thesis
- Identifier: uj:3261 , http://hdl.handle.net/10210/6669
- Description: M.Sc. , Sediment analysis, especially for trace metals, is important since aquatic sediments act as sinks for metals in the environment. Total element analysis yields insufficient information on the bioavailability and the geochemical fate of these metals. Sequential extraction procedures were developed to determine the partitioning of metals in sediment phases. The need for comparability of data produced world-wide led to the development of a sequential extraction procedure, which was proposed by the Community Bureau of Reference as a standard procedure (refered to as the BCR protocol). We contributed to the validation of the BCR procedure by using well-defined in-house model sediments. The results obtained for the model sediments showed that the BCR procedure could distinguish effectively between anthropogenically introduced metals and metals that form part of the mineral structure of the sediment components. The BCR procedure was applied to the sediments of the Vaal Dam and its contributing rivers. The amount of metals extracted in the first three steps of the sequential extraction procedure were low, indicating a very small contribution of anthropogenically introduced metals. It was therefore concluded that these sediments were relatively unpolluted compared to water systems in, for example, Europe.
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