The use of a silica based coating to reduce moisture absorption of flax fibre reinforced composites
- Authors: Bala, Sandisiwe
- Date: 2018
- Subjects: Chromatographic analysis , Nonwoven fabrics Nanocomposites (Materials)
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10948/23349 , vital:30534
- Description: This study deals with the synthesis of silica particles, treatment of flax fabrics with silica, and the preparation and characterization of silica coated flax fibre reinforced phenolic composites treated with silica. Silica particles were successfully prepared by means of a hydrolytic sol-gel route. Two types of silica were prepared by employing either ammonium hydroxide solution as a base catalyst and acetic acid as an acid catalyst. The silica sols were then aged from three to five days in order to determine the effects of aging on the final properties of the silica. The chemical composition of the silica particles was evaluated by fourier transform infrared spectroscopy (FTIR), thermal stability was determined by using thermogravimetric analysis (TGA), and structural and physical properties of the silica particles prepared via two catalysts and aged at different time periods was investigated by x-ray diffraction (XRD). Silica sols, prepared at different conditions were then applied to treat flax fabrics (untreated/scoured) by use of the padding technique. The effects of the silica treatments on flax fabrics were evaluated by FTIR, XRD, determination of moisture content and mechanical properties. The FTIR revealed presence of silica groups on the silica treated flax fabrics, thus resulting in low moisture content for silica treated flax fabrics. XRD analysis revealed that aging the silica sols increases the crystallinity index. Silica treated flax fabrics showed enhanced tensile properties in the weft direction. The thermal, mechanical and water sorption properties of the composites were evaluated. TGA results revealed that the decomposition temperatures of the silica treated composites shifted to higher temperatures. Thus, silica treatments lead to an improvement in thermal stability for composites. A reduction in mechanical properties was also observed for silica treated composites and some composites showed a reduction in water absorption. It was quite evident from this study that the type of catalyst system used in silica preparation has a great influence on the final properties of the silica, which to a large extent changes the thermal, mechanical and water sorption properties of the composites.
- Full Text:
- Date Issued: 2018
- Authors: Bala, Sandisiwe
- Date: 2018
- Subjects: Chromatographic analysis , Nonwoven fabrics Nanocomposites (Materials)
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: http://hdl.handle.net/10948/23349 , vital:30534
- Description: This study deals with the synthesis of silica particles, treatment of flax fabrics with silica, and the preparation and characterization of silica coated flax fibre reinforced phenolic composites treated with silica. Silica particles were successfully prepared by means of a hydrolytic sol-gel route. Two types of silica were prepared by employing either ammonium hydroxide solution as a base catalyst and acetic acid as an acid catalyst. The silica sols were then aged from three to five days in order to determine the effects of aging on the final properties of the silica. The chemical composition of the silica particles was evaluated by fourier transform infrared spectroscopy (FTIR), thermal stability was determined by using thermogravimetric analysis (TGA), and structural and physical properties of the silica particles prepared via two catalysts and aged at different time periods was investigated by x-ray diffraction (XRD). Silica sols, prepared at different conditions were then applied to treat flax fabrics (untreated/scoured) by use of the padding technique. The effects of the silica treatments on flax fabrics were evaluated by FTIR, XRD, determination of moisture content and mechanical properties. The FTIR revealed presence of silica groups on the silica treated flax fabrics, thus resulting in low moisture content for silica treated flax fabrics. XRD analysis revealed that aging the silica sols increases the crystallinity index. Silica treated flax fabrics showed enhanced tensile properties in the weft direction. The thermal, mechanical and water sorption properties of the composites were evaluated. TGA results revealed that the decomposition temperatures of the silica treated composites shifted to higher temperatures. Thus, silica treatments lead to an improvement in thermal stability for composites. A reduction in mechanical properties was also observed for silica treated composites and some composites showed a reduction in water absorption. It was quite evident from this study that the type of catalyst system used in silica preparation has a great influence on the final properties of the silica, which to a large extent changes the thermal, mechanical and water sorption properties of the composites.
- Full Text:
- Date Issued: 2018
Phytochemical analyses and Brine shrimp (Artemia Salina) lethality studies on Syzygium cordatum
- Authors: Chiguvare, Herbert
- Date: 2013
- Subjects: Artemia , Crustacea , Chromatographic analysis , Medicinal plants , Essences and essential oils , Traditional medicine
- Language: English
- Type: Thesis , Masters , MSc (Chemistry)
- Identifier: vital:11336 , http://hdl.handle.net/10353/d1004352 , Artemia , Crustacea , Chromatographic analysis , Medicinal plants , Essences and essential oils , Traditional medicine
- Description: Syzygium cordatum Hoscht ex. C Krauss, also known as water berry, is normally used by the people of South Africa for respiratory ailments including tuberculosis, stomach complaints, treatment of wounds and as emetics. An extract of the leaves can be used as a purgative for diarrhoea treatment. The leaves of Syzygium cordatum Myrtaceae were obtained from the Eastern Cape Province of South Africa, air dried and sequential solvent extraction was done to obtain various non volatile crude extracts. The volatile extract, that is the essential oil was extracted from the leaves using hydrodistillation and analysis of compounds was done by GC/MS for composition. 32 compounds were obtained from the fresh leaves and 18 compounds were obtained from the dry leaves. The fresh oil contains caryophyllene (11.8 percent) and caryophyllene oxide (11.1 percent) as the main sesquiterpene component. α-Pinene(5.0 percent) was the only monoterpene compound identified in the fresh oil in substantial amount. The dry leaves oil had copanene (17.0 percent), β-Caryophellene (26.0 percent), cubenol (6.5 percent) and caryophellene oxide (14.2 percent) as the dominant constituent of the oil. Summary of the classes of compounds in the oil revealed that the chemical profile of both oils were dominated by sesquiterpenoid compounds. This is the first time that terpenoids compounds are being identified in both the fresh and dry leaf oil of S. cordatum. Hexane leaf extract was selected due to the interest in the terpenoid compounds. Column chromatography of the hexane crude gave five (5) of which two are fully reported. The isolates were fully elucidated using spectroscopic methods to be β-Sitosterol (HC3) and Friedela-3-one (HC1A/HC1D). Cytotoxicity analysis was carried out on the crude using the Brine shrimps assay. Isolates 1C and1D showed significant lethality using the brine shrimps assay with lethality values (LC50) of 4.105mg/ml for HC1C and 4.11mg/ml for 1D/1A respectively.
- Full Text:
- Date Issued: 2013
- Authors: Chiguvare, Herbert
- Date: 2013
- Subjects: Artemia , Crustacea , Chromatographic analysis , Medicinal plants , Essences and essential oils , Traditional medicine
- Language: English
- Type: Thesis , Masters , MSc (Chemistry)
- Identifier: vital:11336 , http://hdl.handle.net/10353/d1004352 , Artemia , Crustacea , Chromatographic analysis , Medicinal plants , Essences and essential oils , Traditional medicine
- Description: Syzygium cordatum Hoscht ex. C Krauss, also known as water berry, is normally used by the people of South Africa for respiratory ailments including tuberculosis, stomach complaints, treatment of wounds and as emetics. An extract of the leaves can be used as a purgative for diarrhoea treatment. The leaves of Syzygium cordatum Myrtaceae were obtained from the Eastern Cape Province of South Africa, air dried and sequential solvent extraction was done to obtain various non volatile crude extracts. The volatile extract, that is the essential oil was extracted from the leaves using hydrodistillation and analysis of compounds was done by GC/MS for composition. 32 compounds were obtained from the fresh leaves and 18 compounds were obtained from the dry leaves. The fresh oil contains caryophyllene (11.8 percent) and caryophyllene oxide (11.1 percent) as the main sesquiterpene component. α-Pinene(5.0 percent) was the only monoterpene compound identified in the fresh oil in substantial amount. The dry leaves oil had copanene (17.0 percent), β-Caryophellene (26.0 percent), cubenol (6.5 percent) and caryophellene oxide (14.2 percent) as the dominant constituent of the oil. Summary of the classes of compounds in the oil revealed that the chemical profile of both oils were dominated by sesquiterpenoid compounds. This is the first time that terpenoids compounds are being identified in both the fresh and dry leaf oil of S. cordatum. Hexane leaf extract was selected due to the interest in the terpenoid compounds. Column chromatography of the hexane crude gave five (5) of which two are fully reported. The isolates were fully elucidated using spectroscopic methods to be β-Sitosterol (HC3) and Friedela-3-one (HC1A/HC1D). Cytotoxicity analysis was carried out on the crude using the Brine shrimps assay. Isolates 1C and1D showed significant lethality using the brine shrimps assay with lethality values (LC50) of 4.105mg/ml for HC1C and 4.11mg/ml for 1D/1A respectively.
- Full Text:
- Date Issued: 2013
Beta-N-methylamino-L-alanine in South African fresh water cyanobacteria : incidence, prevalence, ecotoxicological considerations and human exposure risk
- Authors: Esterhuizen-Londt, Maranda
- Date: 2010
- Subjects: Cyanobacteria , Bioaccumulation , Chromatographic analysis , Neurotoxic agents
- Language: English
- Type: Thesis , Doctoral , PhD
- Identifier: vital:10306 , http://hdl.handle.net/10948/1473 , Cyanobacteria , Bioaccumulation , Chromatographic analysis , Neurotoxic agents
- Description: β-N-methylamino-L-alanine (BMAA) is a non-proteinogenic amino acid associated with human neurodegenerative disease. Due to the cosmopolitan nature of cyanobacteria, detection of BMAA in cyanobacteria has caused concerns about human exposure risk. This study was therefore based on the hypothesis that BMAA poses a health risk to humans either by direct ingestion or by indirect exposure to BMAA from a cyanobacterial source via a freshwater food chain. A validated gas chromatography-mass spectrometry (GC-MS) BMAA analysis method and a confirmatory liquid chromatography-mass spectrometry (LC-MS) method, with improved sensitivity, were developed in addition to a LC-MS/MS method for analyte confirmation. These methods were used to quantify BMAA in South African cyanobacteria, isolated from various potable water reservoirs. The majority of the isolates tested, contained BMAA. Possible human exposure by direct consumption of BMAA released from cyanobacterial blooms was investigated by the development of a robust solid phase extraction (SPE) method used for BMAA concentration and quantification in raw and treated tap water. Despite the use of the SPE method that facilitated the concentration of BMAA from large quantities of water, no free dissolved BMAA was detected in raw or processed fresh water. The fate of exogenous BMAA was therefore investigated firstly by evaluating the efficacy of standard water treatment processes employed in South Africa and secondly by investigating the possibility of BMAA bioaccumulation and biomagnification in aquatic food chains. Standard water treatment processes proved highly efficient at removing free dissolved BMAA, explaining the absence of BMAA in treated tap water. However, the cause of the BMAA absence in raw potable water remained unknown. Uptake of BMAA by model aquatic organisms was investigated in controlled experiments. BMAA uptake was documented in both Ceratophyllum demersum and Daphnia magna, however, BMAA-protein association and biomagnification were not observed in D. magna. BMAA had an inhibitory effect on the oxidative stress enzyme acitivties of both organisms tested (as well as human S9 extracts), resulting in accumulation of detrimental reactive oxygen species (ROS) in the cells. Exposure of crop plants to BMAA in controlled experiments resulted in BMAA uptake, protein association, and subsequent inhibition of the antioxidative enzyme activities. However, BMAA was detected in neither free nor protein-associated form in natural crop plants irrigated with known BMAA-containing bloom water. Post-mortem liver samples of Clarias gariepinus (Catfish) and Crocodylus niloticus (Crocodile), from a natural fresh water ecosystem that experienced frequent cyanobacterial blooms, contained both free and protein-associated BMAA. Higher BMAA concentrations were found in crocodile liver samples compared to fish liver samples, strongly suggesting biomagnification from one trophic level to the next. BMAA concentrations corresponded to crocodile age. This is the first report of bioaccumulation and biomagnification in two trophic levels in a fresh water ecosystem. These findings strongly suggest possible human exposure via aquatic food chains of cyanobacterial origin. Direct BMAA exposure via drinking water is not plausible due to the efficiency of standard water treatment processes to remove BMAA. The use of raw water for agricultural and recreational use, however, remains a problem. The development of management strategies as well as daily tolerable levels for BMAA is urgently required.
- Full Text:
- Date Issued: 2010
- Authors: Esterhuizen-Londt, Maranda
- Date: 2010
- Subjects: Cyanobacteria , Bioaccumulation , Chromatographic analysis , Neurotoxic agents
- Language: English
- Type: Thesis , Doctoral , PhD
- Identifier: vital:10306 , http://hdl.handle.net/10948/1473 , Cyanobacteria , Bioaccumulation , Chromatographic analysis , Neurotoxic agents
- Description: β-N-methylamino-L-alanine (BMAA) is a non-proteinogenic amino acid associated with human neurodegenerative disease. Due to the cosmopolitan nature of cyanobacteria, detection of BMAA in cyanobacteria has caused concerns about human exposure risk. This study was therefore based on the hypothesis that BMAA poses a health risk to humans either by direct ingestion or by indirect exposure to BMAA from a cyanobacterial source via a freshwater food chain. A validated gas chromatography-mass spectrometry (GC-MS) BMAA analysis method and a confirmatory liquid chromatography-mass spectrometry (LC-MS) method, with improved sensitivity, were developed in addition to a LC-MS/MS method for analyte confirmation. These methods were used to quantify BMAA in South African cyanobacteria, isolated from various potable water reservoirs. The majority of the isolates tested, contained BMAA. Possible human exposure by direct consumption of BMAA released from cyanobacterial blooms was investigated by the development of a robust solid phase extraction (SPE) method used for BMAA concentration and quantification in raw and treated tap water. Despite the use of the SPE method that facilitated the concentration of BMAA from large quantities of water, no free dissolved BMAA was detected in raw or processed fresh water. The fate of exogenous BMAA was therefore investigated firstly by evaluating the efficacy of standard water treatment processes employed in South Africa and secondly by investigating the possibility of BMAA bioaccumulation and biomagnification in aquatic food chains. Standard water treatment processes proved highly efficient at removing free dissolved BMAA, explaining the absence of BMAA in treated tap water. However, the cause of the BMAA absence in raw potable water remained unknown. Uptake of BMAA by model aquatic organisms was investigated in controlled experiments. BMAA uptake was documented in both Ceratophyllum demersum and Daphnia magna, however, BMAA-protein association and biomagnification were not observed in D. magna. BMAA had an inhibitory effect on the oxidative stress enzyme acitivties of both organisms tested (as well as human S9 extracts), resulting in accumulation of detrimental reactive oxygen species (ROS) in the cells. Exposure of crop plants to BMAA in controlled experiments resulted in BMAA uptake, protein association, and subsequent inhibition of the antioxidative enzyme activities. However, BMAA was detected in neither free nor protein-associated form in natural crop plants irrigated with known BMAA-containing bloom water. Post-mortem liver samples of Clarias gariepinus (Catfish) and Crocodylus niloticus (Crocodile), from a natural fresh water ecosystem that experienced frequent cyanobacterial blooms, contained both free and protein-associated BMAA. Higher BMAA concentrations were found in crocodile liver samples compared to fish liver samples, strongly suggesting biomagnification from one trophic level to the next. BMAA concentrations corresponded to crocodile age. This is the first report of bioaccumulation and biomagnification in two trophic levels in a fresh water ecosystem. These findings strongly suggest possible human exposure via aquatic food chains of cyanobacterial origin. Direct BMAA exposure via drinking water is not plausible due to the efficiency of standard water treatment processes to remove BMAA. The use of raw water for agricultural and recreational use, however, remains a problem. The development of management strategies as well as daily tolerable levels for BMAA is urgently required.
- Full Text:
- Date Issued: 2010
Identification and characterization of novel oncology related platinum complexes using chromatographic and mass spectrometric techniques
- Authors: Wentzel, Mauritz
- Date: 2008
- Subjects: Chromatographic analysis , Spectrum analysis
- Language: English
- Type: Thesis , Doctoral , PhD
- Identifier: vital:10310 , http://hdl.handle.net/10948/715 , Chromatographic analysis , Spectrum analysis
- Description: In this thesis mass spectral and chromatographic techniques were developed and applied to identify and characterise numerous novel platinum(II) and (IV) compounds designed as anticancer agents. In a novel method for the synthesis of cis-oxalato(trans- -1,2- cyclohexanediamine)platinum(II) or oxaliplatin these techniques could be applied to differentiate between the molecular complex and the autoionised analogue (viz. Ptdach2 2+Ptox2 2-). In another novel synthetic method for the same compound the ligand exchange reactions at various temperatures could be investigated and kinetic curves obtained served to illuminate the chemistry involved, indicating the role of small amounts of water in the essentially non-aqueous solvent systems dmf and isoamyl alcohol respectively. These allowed ligand exchange without resulting in hydrolyses even up to 85°C. The ionisation rate of divalent platinum halide complexes was determined for various amine ligands as well as N-S chelate ligands. A comparison of these could suggest why N-S complexes have poor anticancer action. Ionisation was not only studied for neutral molecular species but also for monocationic ones. Relationships could be found with stereochemical aspects of the chelates used. By investigating results of EV-CAD studies thermodynamic data could be obtained which indicated that bond strength decreases from chloro to iodo analogues although extent of ionisation in aqueous solution, i.e kinetic stability, is the reverse. Products formed by the reaction of NO2 gas with Platinum(II) compounds could be identified and separated which greatly contributed to the understanding of the chemistry involved in the formation of mononitro platinum(IV) complexes. Some of these proved to have exceptional anticancer properties. Studies of the interaction of thiol containing biomolecules were performed as a function of time. The results contributed to the understanding of the action of the anticancer agents.
- Full Text:
- Date Issued: 2008
- Authors: Wentzel, Mauritz
- Date: 2008
- Subjects: Chromatographic analysis , Spectrum analysis
- Language: English
- Type: Thesis , Doctoral , PhD
- Identifier: vital:10310 , http://hdl.handle.net/10948/715 , Chromatographic analysis , Spectrum analysis
- Description: In this thesis mass spectral and chromatographic techniques were developed and applied to identify and characterise numerous novel platinum(II) and (IV) compounds designed as anticancer agents. In a novel method for the synthesis of cis-oxalato(trans- -1,2- cyclohexanediamine)platinum(II) or oxaliplatin these techniques could be applied to differentiate between the molecular complex and the autoionised analogue (viz. Ptdach2 2+Ptox2 2-). In another novel synthetic method for the same compound the ligand exchange reactions at various temperatures could be investigated and kinetic curves obtained served to illuminate the chemistry involved, indicating the role of small amounts of water in the essentially non-aqueous solvent systems dmf and isoamyl alcohol respectively. These allowed ligand exchange without resulting in hydrolyses even up to 85°C. The ionisation rate of divalent platinum halide complexes was determined for various amine ligands as well as N-S chelate ligands. A comparison of these could suggest why N-S complexes have poor anticancer action. Ionisation was not only studied for neutral molecular species but also for monocationic ones. Relationships could be found with stereochemical aspects of the chelates used. By investigating results of EV-CAD studies thermodynamic data could be obtained which indicated that bond strength decreases from chloro to iodo analogues although extent of ionisation in aqueous solution, i.e kinetic stability, is the reverse. Products formed by the reaction of NO2 gas with Platinum(II) compounds could be identified and separated which greatly contributed to the understanding of the chemistry involved in the formation of mononitro platinum(IV) complexes. Some of these proved to have exceptional anticancer properties. Studies of the interaction of thiol containing biomolecules were performed as a function of time. The results contributed to the understanding of the action of the anticancer agents.
- Full Text:
- Date Issued: 2008
High performance liquid chromatographic analysis of erythromycin in serum and urine
- Authors: Stubbs, Christopher
- Date: 1985 , 2013-03-13
- Subjects: High performance liquid chromatography , Erythromycin , Erythromycin -- Pharmacokinetics , Chromatographic analysis
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:3813 , http://hdl.handle.net/10962/d1004581 , High performance liquid chromatography , Erythromycin , Erythromycin -- Pharmacokinetics , Chromatographic analysis
- Description: Erythromycin, a macrolide antibiotic used mainly against gram-positive bacteria has been in clinical use since 1952 (1). Previous pharmacokinetic data published on this antibiotic have been derived predominantly from microbiological assay techniques. However, these techniques are relatively imprecise as well as being non-specific and extremely tedious to perform. A novel high performance liquid chromatographic analysis of erythromycin in human serum and urine using U.V. detection at 200 nm and/or electrochemical detection using both an amperometric and a coulometric electrochemical detector is presented. The method involves a solid phase extraction procedure followed by a simple phase separation step and chromatography on a reverse phase column. In order to select the optimum U.V. detector for this analysis, five "state of the art" detectors were compared in terms of their signal-to-noise ratios at U.V. wavelengths between 200 and 210 nm. A known metabolite des-N-methylerythromycin is readily detectable using U.V. detection, whilst another metabolite/degradation product anhydroerythromycin is not seen using U.V. detection but is readily observable using an electrochemical detector. The method has a limit of sensitivity of 0.25 μg/mL and 1.00 μg/mL in serum and urine respectively (U.V. detection) and is sufficiently sensitive to monitor serum and urine concentrations of erythromycin in man after administration of a single 500 mg erythromycin stearate tablet. , KMBT_363 , Adobe Acrobat 9.53 Paper Capture Plug-in
- Full Text:
- Date Issued: 1985
- Authors: Stubbs, Christopher
- Date: 1985 , 2013-03-13
- Subjects: High performance liquid chromatography , Erythromycin , Erythromycin -- Pharmacokinetics , Chromatographic analysis
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:3813 , http://hdl.handle.net/10962/d1004581 , High performance liquid chromatography , Erythromycin , Erythromycin -- Pharmacokinetics , Chromatographic analysis
- Description: Erythromycin, a macrolide antibiotic used mainly against gram-positive bacteria has been in clinical use since 1952 (1). Previous pharmacokinetic data published on this antibiotic have been derived predominantly from microbiological assay techniques. However, these techniques are relatively imprecise as well as being non-specific and extremely tedious to perform. A novel high performance liquid chromatographic analysis of erythromycin in human serum and urine using U.V. detection at 200 nm and/or electrochemical detection using both an amperometric and a coulometric electrochemical detector is presented. The method involves a solid phase extraction procedure followed by a simple phase separation step and chromatography on a reverse phase column. In order to select the optimum U.V. detector for this analysis, five "state of the art" detectors were compared in terms of their signal-to-noise ratios at U.V. wavelengths between 200 and 210 nm. A known metabolite des-N-methylerythromycin is readily detectable using U.V. detection, whilst another metabolite/degradation product anhydroerythromycin is not seen using U.V. detection but is readily observable using an electrochemical detector. The method has a limit of sensitivity of 0.25 μg/mL and 1.00 μg/mL in serum and urine respectively (U.V. detection) and is sufficiently sensitive to monitor serum and urine concentrations of erythromycin in man after administration of a single 500 mg erythromycin stearate tablet. , KMBT_363 , Adobe Acrobat 9.53 Paper Capture Plug-in
- Full Text:
- Date Issued: 1985
The study of hydroxyoximes and hydroxamic acids supported on macroporous resins and their use in the rapid seperation of metals
- Authors: Hemmes, Marlene
- Date: 1979
- Subjects: Chromatographic analysis , Separation (Technology) , Metal ions , Solvent extraction , Extraction (Chemistry) , Oximes , Metals -- Analysis
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:4453 , http://hdl.handle.net/10962/d1009512
- Description: Introduction: The macroporous Amberlite XAD resins were coated with LIX-64N and examined for the rate of uptake of copper . XAD-7 was by far the best support and gave a satisfactory rate of uptake up to loadings of 60% (w/w). The specific surface area of XAD-7 was measured by the adsorption of methylene blue from aqueous solution. The area of the wetted resin was five times less than that of the dry resin. LIX-65N was purified and the anti isomer characterised using spectroscopic techniques . The rate of uptake of copper was not improved by use of purified LIX-65N or by addition of LIX-63. XAD-7 coated with LIX-65N was used in columns. Elution curves for copper showed negligible tailing, and rapid separations of copper from iron (111), nickel, cobalt and magnesium by selective absorption were achieved. Copper was concentrated from very dilute solution at a flow rate of 50 ml min -1 ,and a 99% recovery was obtained. The method was applied to the rapid determination of copper in brass and bronze. A series of long-chain hydroxamic acids were synthesised and tested for suitability as stationary phase on XAD-7. Oleohydroxamic acid and naphthenohydroxamic acid were the most promising. The r ate of uptake of copper was reduced by the use of nonylphenol or amyl alcohol as a diluent. The capacities for copper of the hydroxamic acids were less when supported on XAD-7 than when used as liquid ionexchangers. The distribution coefficients of cobalt, nickel, zinc, lead, vanadium, uranium, iron (111) and copper were measured as a function of pH. XAD-7 coated with oleohydroxamic acid was used in columns for the rapid separation of iron (111) from copper and of copper from nickel, cobalt, lead and zinc. Copper was concentrated from very dilute solution at a flow rate of 45 ml min -1 and a 100,8% recovery was obtained. Copper was successfully separated from nickel by selective elution. The elution curves obtained show negligible tailing. The resin loaded with oleohydroxamic acid lost capacity due to chemical instability. Naphthenohydroxamic acid supported on XAD-7 was not suitable for use in columns, because it was physically unstable.
- Full Text:
- Date Issued: 1979
- Authors: Hemmes, Marlene
- Date: 1979
- Subjects: Chromatographic analysis , Separation (Technology) , Metal ions , Solvent extraction , Extraction (Chemistry) , Oximes , Metals -- Analysis
- Language: English
- Type: Thesis , Masters , MSc
- Identifier: vital:4453 , http://hdl.handle.net/10962/d1009512
- Description: Introduction: The macroporous Amberlite XAD resins were coated with LIX-64N and examined for the rate of uptake of copper . XAD-7 was by far the best support and gave a satisfactory rate of uptake up to loadings of 60% (w/w). The specific surface area of XAD-7 was measured by the adsorption of methylene blue from aqueous solution. The area of the wetted resin was five times less than that of the dry resin. LIX-65N was purified and the anti isomer characterised using spectroscopic techniques . The rate of uptake of copper was not improved by use of purified LIX-65N or by addition of LIX-63. XAD-7 coated with LIX-65N was used in columns. Elution curves for copper showed negligible tailing, and rapid separations of copper from iron (111), nickel, cobalt and magnesium by selective absorption were achieved. Copper was concentrated from very dilute solution at a flow rate of 50 ml min -1 ,and a 99% recovery was obtained. The method was applied to the rapid determination of copper in brass and bronze. A series of long-chain hydroxamic acids were synthesised and tested for suitability as stationary phase on XAD-7. Oleohydroxamic acid and naphthenohydroxamic acid were the most promising. The r ate of uptake of copper was reduced by the use of nonylphenol or amyl alcohol as a diluent. The capacities for copper of the hydroxamic acids were less when supported on XAD-7 than when used as liquid ionexchangers. The distribution coefficients of cobalt, nickel, zinc, lead, vanadium, uranium, iron (111) and copper were measured as a function of pH. XAD-7 coated with oleohydroxamic acid was used in columns for the rapid separation of iron (111) from copper and of copper from nickel, cobalt, lead and zinc. Copper was concentrated from very dilute solution at a flow rate of 45 ml min -1 and a 100,8% recovery was obtained. Copper was successfully separated from nickel by selective elution. The elution curves obtained show negligible tailing. The resin loaded with oleohydroxamic acid lost capacity due to chemical instability. Naphthenohydroxamic acid supported on XAD-7 was not suitable for use in columns, because it was physically unstable.
- Full Text:
- Date Issued: 1979
"Complexes of carbohydrates with magnesium-ions" : "the isolation of an oligosaccharide containing L-galactose from the polysaccharide of Aeodes orbitosa" : "horizontal cellulose colum chromatography of sugars"
- Authors: Van der Linde, Michael John
- Date: 1974
- Subjects: Magenesium , Ions , Carbohydrates , Oligosaccharides , Polysaccharides , Chromatographic analysis
- Language: English
- Type: Thesis , Doctoral , PhD
- Identifier: vital:4504 , http://hdl.handle.net/10962/d1013282
- Description: Sugar complexes with anions and cations are reviewed. Evidence is presented for the formation of a complex of stoichiometry 1:1 in aqueous solution between methyl-α-Dglucopyranoside and magnesium perchlorate. The complex may be detected by the method of continuous variations. Measurements of changes in the proton chemical shifts of the glucoside in dauterium oxide, indicate that the complex is probably formed between the vicinal hydroxyl groups at C-2 and C-3 of the pyranoside ring and the hydrated cation. At elevation temperatures there is evidence for the presence of a complex of stoichiometry 2:1. Experiments conducted on cellulose indicate the possible formation of cellulose - magnesium-ion complexes . These complexes provide an explanation for the "protective action" of mEgnesium compounds on the cellulose portion of pulp during alkali-oxygen bleaching.
- Full Text:
- Date Issued: 1974
- Authors: Van der Linde, Michael John
- Date: 1974
- Subjects: Magenesium , Ions , Carbohydrates , Oligosaccharides , Polysaccharides , Chromatographic analysis
- Language: English
- Type: Thesis , Doctoral , PhD
- Identifier: vital:4504 , http://hdl.handle.net/10962/d1013282
- Description: Sugar complexes with anions and cations are reviewed. Evidence is presented for the formation of a complex of stoichiometry 1:1 in aqueous solution between methyl-α-Dglucopyranoside and magnesium perchlorate. The complex may be detected by the method of continuous variations. Measurements of changes in the proton chemical shifts of the glucoside in dauterium oxide, indicate that the complex is probably formed between the vicinal hydroxyl groups at C-2 and C-3 of the pyranoside ring and the hydrated cation. At elevation temperatures there is evidence for the presence of a complex of stoichiometry 2:1. Experiments conducted on cellulose indicate the possible formation of cellulose - magnesium-ion complexes . These complexes provide an explanation for the "protective action" of mEgnesium compounds on the cellulose portion of pulp during alkali-oxygen bleaching.
- Full Text:
- Date Issued: 1974
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