A highly selective and sensitive pyridylazo-2-naphthol-poly (acrylic acid) functionalized electrospun nanofiber fluorescence “turn-off” chemosensory system for Ni 2+
- Adewuyi, Sheriff, Ondigo, Dezzline A, Zugle, Ruphino, Tshentu, Zenixole R, Nyokong, Tebello, Torto, Nelson
- Authors: Adewuyi, Sheriff , Ondigo, Dezzline A , Zugle, Ruphino , Tshentu, Zenixole R , Nyokong, Tebello , Torto, Nelson
- Date: 2012
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/246012 , vital:51428 , xlink:href="https://doi.org/10.1039/C2AY25182E"
- Description: A fluorescent nanofiber probe for the determination of Ni2+ was developed via the electrospinning of a covalently functionalized pyridylazo-2-naphthol-poly(acrylic acid) polymer. Fluorescent nanofibers with diameters in the range 230–800 nm were produced with uniformly dispersed fluorophores. The excitation and emission fluorescence were at wavelengths 479 and 557 nm respectively, thereby exhibiting a good Stokes' shift. This Ni2+ probe that employs fluorescence quenching in a solid receptor–fluorophore system exhibited a good correlation between the fluorescence intensity and nickel concentration up to 1.0 μg mL−1 based on the Stern–Volmer mechanism. The probe achieved a detection limit (3δ/S) of 0.07 ng mL−1 and a precision, calculated as a relative standard deviation (RSD) of more than 4% (n = 8). The concentration of Ni2+ in a certified reference material (SEP-3) was found to be 0.8986 μg mL−1, which is significantly comparable with the certified value of 0.8980 μg mL−1. The accuracy of the determinations, expressed as a relative error between the certified and the observed values of certified reference groundwater was ≤0.1%. The versatility of the nanofiber probe was demonstrated by affording simple, rapid and selective detection of Ni2+ in the presence of other competing metal ions by direct analysis, without employing any further sample handling steps.
- Full Text:
- Date Issued: 2012
- Authors: Adewuyi, Sheriff , Ondigo, Dezzline A , Zugle, Ruphino , Tshentu, Zenixole R , Nyokong, Tebello , Torto, Nelson
- Date: 2012
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/246012 , vital:51428 , xlink:href="https://doi.org/10.1039/C2AY25182E"
- Description: A fluorescent nanofiber probe for the determination of Ni2+ was developed via the electrospinning of a covalently functionalized pyridylazo-2-naphthol-poly(acrylic acid) polymer. Fluorescent nanofibers with diameters in the range 230–800 nm were produced with uniformly dispersed fluorophores. The excitation and emission fluorescence were at wavelengths 479 and 557 nm respectively, thereby exhibiting a good Stokes' shift. This Ni2+ probe that employs fluorescence quenching in a solid receptor–fluorophore system exhibited a good correlation between the fluorescence intensity and nickel concentration up to 1.0 μg mL−1 based on the Stern–Volmer mechanism. The probe achieved a detection limit (3δ/S) of 0.07 ng mL−1 and a precision, calculated as a relative standard deviation (RSD) of more than 4% (n = 8). The concentration of Ni2+ in a certified reference material (SEP-3) was found to be 0.8986 μg mL−1, which is significantly comparable with the certified value of 0.8980 μg mL−1. The accuracy of the determinations, expressed as a relative error between the certified and the observed values of certified reference groundwater was ≤0.1%. The versatility of the nanofiber probe was demonstrated by affording simple, rapid and selective detection of Ni2+ in the presence of other competing metal ions by direct analysis, without employing any further sample handling steps.
- Full Text:
- Date Issued: 2012
An ion-imprinted polymer for the selective extraction of mercury(II) ions in aqueous media
- Batlokwa, Bareki Shima, Chimuka, Luke, Tshentu, Zenixole R, Cukrowska, Ewa, Torto, Nelson
- Authors: Batlokwa, Bareki Shima , Chimuka, Luke , Tshentu, Zenixole R , Cukrowska, Ewa , Torto, Nelson
- Date: 2012
- Language: English
- Type: Article
- Identifier: vital:6566 , http://hdl.handle.net/10962/d1004125
- Description: A double-imprinted polymer exhibiting high sensitivity for mercury(II) in aqueous solution is presented. Polymer particles imprinted with mercury(II) were synthesised by copolymerising the functional and cross-linking monomers, N’–[3– (Trimethoxysilyl)–propyl]diethylenetriamine (TPET) and tetraethylorthosilicate (TEOS). A double-imprinting procedure employing hexadecyltrimethylammonium bromide (CTAB), as a second template to improve the efficiency of the polymer, was adopted. The imprinted polymer was characterised by FTIR, scanning electron microscopy (SEM) and the average size determined by screen analysis using standard test sieves. Relative selective coefficients (k`) of the imprinted polymer evaluated from selective binding studies between Hg2+ and Cu2+ or Hg2+ and Cd2+ were 10 588 and 3 147, respectively. These values indicated highly-favoured Hg2+ extractions over the 2 competing ions. The results of spiked and real water samples showed high extraction efficiencies of Hg2+ ions, (over 84%) as evaluated from the detected unextracted Hg2+ ions by ICP-OES. The method exhibited a dynamic response concentration range for Hg2+ between 0.01 and 20 μg/mℓ, with a detection limit (LOD, 3σ) of 0.000036 μg/mℓ (36 ng/ℓ) that meets the monitoring requirements for the USA EPA of 2 000 ng/ℓ for Hg2+ in drinking water. Generally, the data (n=10) had percentage relative standard deviations (%RSD) of less than 4%. Satisfactory results were also obtained when the prepared sorbent was applied for the pre-concentration of Hg2+ from an aqueous certified reference material. These findings indicate that the double-imprinted polymer has potential to be used as an efficient extraction material for the selective pre–concentration of mercury(II) ions in aqueous environments.
- Full Text:
- Date Issued: 2012
- Authors: Batlokwa, Bareki Shima , Chimuka, Luke , Tshentu, Zenixole R , Cukrowska, Ewa , Torto, Nelson
- Date: 2012
- Language: English
- Type: Article
- Identifier: vital:6566 , http://hdl.handle.net/10962/d1004125
- Description: A double-imprinted polymer exhibiting high sensitivity for mercury(II) in aqueous solution is presented. Polymer particles imprinted with mercury(II) were synthesised by copolymerising the functional and cross-linking monomers, N’–[3– (Trimethoxysilyl)–propyl]diethylenetriamine (TPET) and tetraethylorthosilicate (TEOS). A double-imprinting procedure employing hexadecyltrimethylammonium bromide (CTAB), as a second template to improve the efficiency of the polymer, was adopted. The imprinted polymer was characterised by FTIR, scanning electron microscopy (SEM) and the average size determined by screen analysis using standard test sieves. Relative selective coefficients (k`) of the imprinted polymer evaluated from selective binding studies between Hg2+ and Cu2+ or Hg2+ and Cd2+ were 10 588 and 3 147, respectively. These values indicated highly-favoured Hg2+ extractions over the 2 competing ions. The results of spiked and real water samples showed high extraction efficiencies of Hg2+ ions, (over 84%) as evaluated from the detected unextracted Hg2+ ions by ICP-OES. The method exhibited a dynamic response concentration range for Hg2+ between 0.01 and 20 μg/mℓ, with a detection limit (LOD, 3σ) of 0.000036 μg/mℓ (36 ng/ℓ) that meets the monitoring requirements for the USA EPA of 2 000 ng/ℓ for Hg2+ in drinking water. Generally, the data (n=10) had percentage relative standard deviations (%RSD) of less than 4%. Satisfactory results were also obtained when the prepared sorbent was applied for the pre-concentration of Hg2+ from an aqueous certified reference material. These findings indicate that the double-imprinted polymer has potential to be used as an efficient extraction material for the selective pre–concentration of mercury(II) ions in aqueous environments.
- Full Text:
- Date Issued: 2012
Imidazole-functionalized polymer microspheres and fibers–useful materials for immobilization of oxovanadium (IV) catalysts
- Walmsley, Ryan S, Ogunlaja, Adeniyi S, Coombes, Matthew J, Chidawanyika, Wadzanai J U, Litwinski, Christian, Torto, Nelson, Nyokong, Tebello, Tshentu, Zenixole R
- Authors: Walmsley, Ryan S , Ogunlaja, Adeniyi S , Coombes, Matthew J , Chidawanyika, Wadzanai J U , Litwinski, Christian , Torto, Nelson , Nyokong, Tebello , Tshentu, Zenixole R
- Date: 2012
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/246041 , vital:51431 , xlink:href="https://doi.org/10.1039/C2JM15485D"
- Description: Both polymer microspheres and microfibers containing the imidazole functionality have been prepared and used to immobilize oxovanadium(IV). The average diameters and BET surface areas of the microspheres were 322 μm and 155 m2 g−1 while the fibers were 1.85 μm and 52 m2 g−1, respectively. XPS and microanalysis confirmed the incorporation of imidazole and vanadium in the polymeric materials. The catalytic activity of both materials was evaluated using the hydrogen peroxide facilitated oxidation of thioanisole. The microspheres were applied in a typical laboratory batch reactor set-up and quantitative conversions (>99%) were obtained in under 240 min with turn-over frequencies ranging from 21.89 to 265.53 h−1, depending on the quantity of catalyst and temperature. The microspherical catalysts also proved to be recyclable with no drop in activity being observed after three successive reactions. The vanadium functionalized fibers were applied in a pseudo continuous flow set-up. Factors influencing the overall conversion and product selectivity, including flow rate and catalyst quantity, were investigated. At flow rates of 1–4 mL h−1 near quantitative conversion was maintained over an extended period. Keeping the mass of catalyst constant (0.025 g) and varying the flow rate from 1–6 mL h−1 resulted in a shift in the formation of the oxidation product methyl phenyl sulfone from 60.1 to 18.6%.
- Full Text:
- Date Issued: 2012
- Authors: Walmsley, Ryan S , Ogunlaja, Adeniyi S , Coombes, Matthew J , Chidawanyika, Wadzanai J U , Litwinski, Christian , Torto, Nelson , Nyokong, Tebello , Tshentu, Zenixole R
- Date: 2012
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/246041 , vital:51431 , xlink:href="https://doi.org/10.1039/C2JM15485D"
- Description: Both polymer microspheres and microfibers containing the imidazole functionality have been prepared and used to immobilize oxovanadium(IV). The average diameters and BET surface areas of the microspheres were 322 μm and 155 m2 g−1 while the fibers were 1.85 μm and 52 m2 g−1, respectively. XPS and microanalysis confirmed the incorporation of imidazole and vanadium in the polymeric materials. The catalytic activity of both materials was evaluated using the hydrogen peroxide facilitated oxidation of thioanisole. The microspheres were applied in a typical laboratory batch reactor set-up and quantitative conversions (>99%) were obtained in under 240 min with turn-over frequencies ranging from 21.89 to 265.53 h−1, depending on the quantity of catalyst and temperature. The microspherical catalysts also proved to be recyclable with no drop in activity being observed after three successive reactions. The vanadium functionalized fibers were applied in a pseudo continuous flow set-up. Factors influencing the overall conversion and product selectivity, including flow rate and catalyst quantity, were investigated. At flow rates of 1–4 mL h−1 near quantitative conversion was maintained over an extended period. Keeping the mass of catalyst constant (0.025 g) and varying the flow rate from 1–6 mL h−1 resulted in a shift in the formation of the oxidation product methyl phenyl sulfone from 60.1 to 18.6%.
- Full Text:
- Date Issued: 2012
Oxovanadium (IV)-catalysed oxidation of dibenzothiophene and 4, 6-dimethyldibenzothiophene
- Ogunlaja, Adeniyi S, Chidawanyika, Wadzanai J U, Antunes, Edith M, Fernandes, Manuel A, Nyokong, Tebello, Torto, Nelson, Tshentu, Zenixole R
- Authors: Ogunlaja, Adeniyi S , Chidawanyika, Wadzanai J U , Antunes, Edith M , Fernandes, Manuel A , Nyokong, Tebello , Torto, Nelson , Tshentu, Zenixole R
- Date: 2012
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/246025 , vital:51429 , xlink:href="https://doi.org/10.1039/C2DT31433A"
- Description: The reaction between [VIVOSO4] and the tetradentate N2O2-donor Schiff base ligand, N,N-bis(o-hydroxybenzaldehyde)phenylenediamine (sal-HBPD), obtained by the condensation of salicylaldehyde and o-phenylenediamine in a molar ratio of 2 : 1 respectively, resulted in the formation of [VIVO(sal-HBPD)]. The molecular structure of [VIVO(sal-HBPD)] was determined by single crystal X-ray diffraction, and confirmed the distorted square pyramidal geometry of the complex with the N2O2 binding mode of the tetradentate ligand. The formation of the polymer-supported p[VIVO(sal-AHBPD)] proceeded via the nitrosation of sal-HBPD, followed by the reduction with hydrogen to form an amine group that was then linked to Merrifield beads followed by the reaction with [VIVOSO4]. XPS and EPR were used to confirm the presence of oxovanadium(IV) within the beads. The BET surface area and porosity of the heterogeneous catalyst p[VIVO(sal-AHBPD)] were found to be 6.9 m2 g−1 and 180.8 Å respectively. Microanalysis, TG, UV-Vis and FT-IR were used for further characterization of both [VIVO(sal-HBPD)] and p[VIVO(sal-AHBPD)]. Oxidation of dibenzothiophene (DBT) and 4,6-dimethyldibenzothiophene (4,6-DMDBT) was investigated using [VIVO(sal-HBPD)] and p[VIVO(sal-AHBPD)] as catalysts. Progress for oxidation of these model compounds was monitored with a gas chromatograph fitted with a flame ionization detector. The oxidation products were characterized using gas chromatography-mass spectrometry, microanalysis and NMR. Dibenzothiophene sulfone (DBTO2) and 4,6-dimethyldibenzothiophene sulfone (4,6-DMDBTO2) were found to be the main products of oxidation. Oxovanadium(IV) Schiff base microspherical beads, p[VIVO(sal-AHBPD)], were able to catalyse the oxidation of sulfur in dibenzothiophene (DBT) and 4,6-dimethyldibenzothiophene (4,6-DMDBT) to a tune of 88.0% and 71.8% respectively after 3 h at 40 °C. These oxidation results show promise for potential application of this catalyst in the oxidative desulfurization of crude oils.
- Full Text:
- Date Issued: 2012
- Authors: Ogunlaja, Adeniyi S , Chidawanyika, Wadzanai J U , Antunes, Edith M , Fernandes, Manuel A , Nyokong, Tebello , Torto, Nelson , Tshentu, Zenixole R
- Date: 2012
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/246025 , vital:51429 , xlink:href="https://doi.org/10.1039/C2DT31433A"
- Description: The reaction between [VIVOSO4] and the tetradentate N2O2-donor Schiff base ligand, N,N-bis(o-hydroxybenzaldehyde)phenylenediamine (sal-HBPD), obtained by the condensation of salicylaldehyde and o-phenylenediamine in a molar ratio of 2 : 1 respectively, resulted in the formation of [VIVO(sal-HBPD)]. The molecular structure of [VIVO(sal-HBPD)] was determined by single crystal X-ray diffraction, and confirmed the distorted square pyramidal geometry of the complex with the N2O2 binding mode of the tetradentate ligand. The formation of the polymer-supported p[VIVO(sal-AHBPD)] proceeded via the nitrosation of sal-HBPD, followed by the reduction with hydrogen to form an amine group that was then linked to Merrifield beads followed by the reaction with [VIVOSO4]. XPS and EPR were used to confirm the presence of oxovanadium(IV) within the beads. The BET surface area and porosity of the heterogeneous catalyst p[VIVO(sal-AHBPD)] were found to be 6.9 m2 g−1 and 180.8 Å respectively. Microanalysis, TG, UV-Vis and FT-IR were used for further characterization of both [VIVO(sal-HBPD)] and p[VIVO(sal-AHBPD)]. Oxidation of dibenzothiophene (DBT) and 4,6-dimethyldibenzothiophene (4,6-DMDBT) was investigated using [VIVO(sal-HBPD)] and p[VIVO(sal-AHBPD)] as catalysts. Progress for oxidation of these model compounds was monitored with a gas chromatograph fitted with a flame ionization detector. The oxidation products were characterized using gas chromatography-mass spectrometry, microanalysis and NMR. Dibenzothiophene sulfone (DBTO2) and 4,6-dimethyldibenzothiophene sulfone (4,6-DMDBTO2) were found to be the main products of oxidation. Oxovanadium(IV) Schiff base microspherical beads, p[VIVO(sal-AHBPD)], were able to catalyse the oxidation of sulfur in dibenzothiophene (DBT) and 4,6-dimethyldibenzothiophene (4,6-DMDBT) to a tune of 88.0% and 71.8% respectively after 3 h at 40 °C. These oxidation results show promise for potential application of this catalyst in the oxidative desulfurization of crude oils.
- Full Text:
- Date Issued: 2012
Syntheses, protonation constants and antimicrobial activity of 2-substituted N-alkylimidazole derivatives
- Kleyi, Phumelele, Walmsley, Ryan S, Gundhla, Isaac Z, Walmsley, Tara A, Jauka, Tembisa I, Dames, Joanna F, Walker, Roderick B, Torto, Nelson, Tshentu, Zenixole R
- Authors: Kleyi, Phumelele , Walmsley, Ryan S , Gundhla, Isaac Z , Walmsley, Tara A , Jauka, Tembisa I , Dames, Joanna F , Walker, Roderick B , Torto, Nelson , Tshentu, Zenixole R
- Date: 2012
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184066 , vital:44165 , xlink:href="https://www.ajol.info/index.php/sajc/article/view/123858"
- Description: A series of N-alkylimidazole-2-carboxylic acid, N-alkylimidazole-2-carboxaldehyde and N-alkylimidazole-2-methanol derivatives [alkyl = benzyl, methyl, ethyl, propyl, butyl, heptyl, octyl and decyl] have been synthesized and the protonation constants determined. The antimicrobial properties of the compounds were tested against Gram-negative (Escherichi coli), Gram-positive (Staphylococcus aureus and Bacillus subtilis subsp. spizizenii) bacterial strains and yeast (C. albicans). Both the disk diffusion and broth microdilution methods for testing the antimicrobial activity showed that N-alkylation of imidazole with longer alkyl chains and the substitution with low pKa group at 2-position resulted in enhanced antimicrobial activity. Particularly, the N-alkylimidazole-2-carboxylic acids exhibited the best antimicrobial activity due to the low pKa of the carboxylic acid moiety. Generally, all the N-alkylimidazole derivatives were most active against the Gram-positive bacteria [S. aureus (MIC = 5–160 µg mL–1) and B. subtilis subsp. spizizenii (5–20 µg mL–1)], with the latter more susceptible. All the compounds showed poor antimicrobial activity against both Gram-negative (E. coli, MIC = 0.15 to >2500 µg mL–1) bacteria and all the compounds were inactive against the yeast (Candida albicans).
- Full Text:
- Date Issued: 2012
- Authors: Kleyi, Phumelele , Walmsley, Ryan S , Gundhla, Isaac Z , Walmsley, Tara A , Jauka, Tembisa I , Dames, Joanna F , Walker, Roderick B , Torto, Nelson , Tshentu, Zenixole R
- Date: 2012
- Subjects: To be catalogued
- Language: English
- Type: text , article
- Identifier: http://hdl.handle.net/10962/184066 , vital:44165 , xlink:href="https://www.ajol.info/index.php/sajc/article/view/123858"
- Description: A series of N-alkylimidazole-2-carboxylic acid, N-alkylimidazole-2-carboxaldehyde and N-alkylimidazole-2-methanol derivatives [alkyl = benzyl, methyl, ethyl, propyl, butyl, heptyl, octyl and decyl] have been synthesized and the protonation constants determined. The antimicrobial properties of the compounds were tested against Gram-negative (Escherichi coli), Gram-positive (Staphylococcus aureus and Bacillus subtilis subsp. spizizenii) bacterial strains and yeast (C. albicans). Both the disk diffusion and broth microdilution methods for testing the antimicrobial activity showed that N-alkylation of imidazole with longer alkyl chains and the substitution with low pKa group at 2-position resulted in enhanced antimicrobial activity. Particularly, the N-alkylimidazole-2-carboxylic acids exhibited the best antimicrobial activity due to the low pKa of the carboxylic acid moiety. Generally, all the N-alkylimidazole derivatives were most active against the Gram-positive bacteria [S. aureus (MIC = 5–160 µg mL–1) and B. subtilis subsp. spizizenii (5–20 µg mL–1)], with the latter more susceptible. All the compounds showed poor antimicrobial activity against both Gram-negative (E. coli, MIC = 0.15 to >2500 µg mL–1) bacteria and all the compounds were inactive against the yeast (Candida albicans).
- Full Text:
- Date Issued: 2012
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