Pre-concentration of toxic metals using electrospun amino-functionalized nylon-6 nanofibre sorbent
- Darko, G, Sobola, A, Adewuyi, Sheriff, Okonkwo, J O, Torto, N
- Authors: Darko, G , Sobola, A , Adewuyi, Sheriff , Okonkwo, J O , Torto, N
- Date: 2012
- Language: English
- Type: Article
- Identifier: vital:6571 , http://hdl.handle.net/10962/d1004134
- Description: This paper presents a new approach for pre-concentrating toxic metals (As, Cd, Ni and Pb) in aqueous environments using an amino-functionalized electrospun nanofibre sorbent. The sorbent, composed of nanofibres of average diameter 80 ± 10 nm and specific surface area of 58m2 g–1, exhibited fast adsorption kinetics (<20 min) for As, Cd, Ni and Pb. The optimalpHfor the uptake of As, Cd, Ni and Pb were 5.5, 6.0, 6.5 and 11, respectively. The adsorption process best fitted the Freundlich isothermand followed the first-order kinetics. The highest pre-concentration achieved using the sorbent was 41.99 (Ni in treated wastewater). The capacity of the sorbent to pre-concentrate the toxic metals was compared with those of aqua regia and HNO3+H2O2 digestions. The pre-concentration factors achieved for Cd in river water samples can be ranked as aqua regia digestion (0.73) > adsorption (0.34)>HNO3+H2O2 (0.23) digestion.Asimilar trend was observed for Ni in river water as well as Ni andCdin tap water samples. Pb ions in the river water samples were pre-concentrated slightly better using the two digestion methods pre-concentration factors ~22) compared to adsorption method (pre-concentration factor ~21). The use of the electrospun amino-functionalized nanofibre sorbent presentsanefficientand cost-effective alternative for pre-concentration of toxic metals inaqueousenvironments.
- Full Text:
- Authors: Darko, G , Sobola, A , Adewuyi, Sheriff , Okonkwo, J O , Torto, N
- Date: 2012
- Language: English
- Type: Article
- Identifier: vital:6571 , http://hdl.handle.net/10962/d1004134
- Description: This paper presents a new approach for pre-concentrating toxic metals (As, Cd, Ni and Pb) in aqueous environments using an amino-functionalized electrospun nanofibre sorbent. The sorbent, composed of nanofibres of average diameter 80 ± 10 nm and specific surface area of 58m2 g–1, exhibited fast adsorption kinetics (<20 min) for As, Cd, Ni and Pb. The optimalpHfor the uptake of As, Cd, Ni and Pb were 5.5, 6.0, 6.5 and 11, respectively. The adsorption process best fitted the Freundlich isothermand followed the first-order kinetics. The highest pre-concentration achieved using the sorbent was 41.99 (Ni in treated wastewater). The capacity of the sorbent to pre-concentrate the toxic metals was compared with those of aqua regia and HNO3+H2O2 digestions. The pre-concentration factors achieved for Cd in river water samples can be ranked as aqua regia digestion (0.73) > adsorption (0.34)>HNO3+H2O2 (0.23) digestion.Asimilar trend was observed for Ni in river water as well as Ni andCdin tap water samples. Pb ions in the river water samples were pre-concentrated slightly better using the two digestion methods pre-concentration factors ~22) compared to adsorption method (pre-concentration factor ~21). The use of the electrospun amino-functionalized nanofibre sorbent presentsanefficientand cost-effective alternative for pre-concentration of toxic metals inaqueousenvironments.
- Full Text:
Dimethylglyoxime based ion-imprinted polymer for the determination of Ni(II) ions from aqueous samples
- Rammika, M, Darko, G, Tshentu, Zenixole R, Sewry, Joyce D, Torto, N
- Authors: Rammika, M , Darko, G , Tshentu, Zenixole R , Sewry, Joyce D , Torto, N
- Date: 2011
- Language: English
- Type: Article
- Identifier: vital:6590 , http://hdl.handle.net/10962/d1004173
- Description: A Ni(II)-dimethylglyoxime ion-imprinted polymer {Ni(II)-DMG IIP} was synthesised by the bulk polymerisation method. The morphology of the Ni(II)-DMG IIP and non-imprinted polymer were observed by scanning electron microscopy and the chemical structures were evaluated by infrared spectroscopy. Selectivity of the Ni(II)-DMG IIP was studied by analysing, using an inductively coupled plasma-optical emission spectrometer, for Ni(II) ions that were spiked with varying concentrations of Co(II), Cu(II), Zn(II), Pd(II), Fe(II), Ca(II), Mg(II), Na(I) and K(I) in aqueous samples. The studies revealed Ni(II) recoveries ranging from 93 to 100% in aqueous solutions with minimal interference from competing ions. Enrichment factors ranged from 2 to 18 with a binding capacity of 120 μg∙g−1. Co(II) was the only ion found to slightly interfere with the determination of Ni(II). Selectivity studies confirmed that the Ni(II)-DMG IIP had very good selectivity, characterised by %RSD of less than 5%. The limits of detection and quantification were 3x10-4 μg∙mℓ−1 and 9x10-4 μg∙mℓ−1, respectively. The accuracy of the method was validated by analysing a custom solution of certified reference material (SEP-3) and the concentration of Ni(II) obtained was in close agreement with the certified one. The Ni(II)-DMG IIP was successfully employed to trap Ni(II) ions from a matrix of sea, river and sewage water. It is believed that the Ni(II)-DMG IIP has potential to be used as sorbent material for pre-concentration of Ni(II) ions from aqueous solutions by solid-phase extraction.
- Full Text:
- Authors: Rammika, M , Darko, G , Tshentu, Zenixole R , Sewry, Joyce D , Torto, N
- Date: 2011
- Language: English
- Type: Article
- Identifier: vital:6590 , http://hdl.handle.net/10962/d1004173
- Description: A Ni(II)-dimethylglyoxime ion-imprinted polymer {Ni(II)-DMG IIP} was synthesised by the bulk polymerisation method. The morphology of the Ni(II)-DMG IIP and non-imprinted polymer were observed by scanning electron microscopy and the chemical structures were evaluated by infrared spectroscopy. Selectivity of the Ni(II)-DMG IIP was studied by analysing, using an inductively coupled plasma-optical emission spectrometer, for Ni(II) ions that were spiked with varying concentrations of Co(II), Cu(II), Zn(II), Pd(II), Fe(II), Ca(II), Mg(II), Na(I) and K(I) in aqueous samples. The studies revealed Ni(II) recoveries ranging from 93 to 100% in aqueous solutions with minimal interference from competing ions. Enrichment factors ranged from 2 to 18 with a binding capacity of 120 μg∙g−1. Co(II) was the only ion found to slightly interfere with the determination of Ni(II). Selectivity studies confirmed that the Ni(II)-DMG IIP had very good selectivity, characterised by %RSD of less than 5%. The limits of detection and quantification were 3x10-4 μg∙mℓ−1 and 9x10-4 μg∙mℓ−1, respectively. The accuracy of the method was validated by analysing a custom solution of certified reference material (SEP-3) and the concentration of Ni(II) obtained was in close agreement with the certified one. The Ni(II)-DMG IIP was successfully employed to trap Ni(II) ions from a matrix of sea, river and sewage water. It is believed that the Ni(II)-DMG IIP has potential to be used as sorbent material for pre-concentration of Ni(II) ions from aqueous solutions by solid-phase extraction.
- Full Text:
Incorporation of Ni(II)-dimethylglyoxime ion-imprinted polymer into electrospun polysulphone nanofibre for the determination of Ni(II) ions from aqueous samples
- Rammika, M, Darko, G, Torto, N
- Authors: Rammika, M , Darko, G , Torto, N
- Date: 2011
- Language: English
- Type: Article
- Identifier: vital:6589 , http://hdl.handle.net/10962/d1004172
- Description: Ni(II)-dimethylglyoxime ion-imprinted polymer (Ni(II)-DMG IIP) was encapsulated in polysulphone and electrospun into nanofibres with diameters ranging from 406 to 854 nm. The structures of the Ni(II)-DMG encapsulated-IIP nanofibre, non-imprinted encapsulated-polymer nanofibre and polysulphone nanofibre mats were observed by scanning electron microscopy and evaluated by infrared spectroscopy. Electrospinning increased the specific surface area of the Ni(II)-DMG encapsulated-IIP nanofibre mats, as was evidenced by the low masses of the Ni(II)-DMG encapsulated-IIP nanofibre mats used. The accuracy of the method was validated by analysing a custom solution of certified reference material (SEP-3); the concentration of Ni(II) obtained was close to the certified one. The limit of detection was found to be 4.0x10-4 μg∙mℓ−1 while the limit of quantification was found to be 1.2x10-3 μg∙mℓ−1. The recovery of Ni(II) achieved using the Ni(II)-DMG imprinted nanofibre mats in water samples was found to range from 83 to 89%, while that of non-imprinted nanofibre mats was found to range from 59 to 65%, and that of polysulphone from 55 to 62%.
- Full Text:
- Authors: Rammika, M , Darko, G , Torto, N
- Date: 2011
- Language: English
- Type: Article
- Identifier: vital:6589 , http://hdl.handle.net/10962/d1004172
- Description: Ni(II)-dimethylglyoxime ion-imprinted polymer (Ni(II)-DMG IIP) was encapsulated in polysulphone and electrospun into nanofibres with diameters ranging from 406 to 854 nm. The structures of the Ni(II)-DMG encapsulated-IIP nanofibre, non-imprinted encapsulated-polymer nanofibre and polysulphone nanofibre mats were observed by scanning electron microscopy and evaluated by infrared spectroscopy. Electrospinning increased the specific surface area of the Ni(II)-DMG encapsulated-IIP nanofibre mats, as was evidenced by the low masses of the Ni(II)-DMG encapsulated-IIP nanofibre mats used. The accuracy of the method was validated by analysing a custom solution of certified reference material (SEP-3); the concentration of Ni(II) obtained was close to the certified one. The limit of detection was found to be 4.0x10-4 μg∙mℓ−1 while the limit of quantification was found to be 1.2x10-3 μg∙mℓ−1. The recovery of Ni(II) achieved using the Ni(II)-DMG imprinted nanofibre mats in water samples was found to range from 83 to 89%, while that of non-imprinted nanofibre mats was found to range from 59 to 65%, and that of polysulphone from 55 to 62%.
- Full Text:
Selective removal of chromium (VI) from sulphates and other metal anions using an ion-imprinted polymer
- Pakade, V, Cukrowska, E, Darkwa, J, Torto, N, Chimuka, Luke
- Authors: Pakade, V , Cukrowska, E , Darkwa, J , Torto, N , Chimuka, Luke
- Date: 2011
- Language: English
- Type: Article
- Identifier: vital:6588 , http://hdl.handle.net/10962/d1004171
- Description: A linear copolymer was prepared from 4-vinylpyridine and styrene. An ion-imprinted polymer (IIP) specific for Cr (VI) adsorption was prepared by copolymerisation of the quaternised linear copolymer (quaternised with 1,4-chlorobutane), 2-vinylpyridine functional monomer and ethylene glycol dimethacrylate (EGDMA), as the cross-linking monomer, in the presence of 1,1’-azobis(cyclohexanecarbonitrile) as initiator. Ammonium dichromate and aqueous methanol were used as a template and porogenic solvent, respectively. Leaching of the chromate template from the polymer particles was achieved with successive stirring of the ion-imprinted polymer (IIP) particles in 4 M HNO3 solutions to obtain leached materials, which were then used for selective rebinding of Cr (VI) ions from aqueous solutions. Similarly, the non-imprinted polymer/ control polymer (NIP/CP) material was also prepared under exactly the same conditions as the IIP but without the chromate anion template. Various parameters, such as solution pH, initial concentration, aqueous phase volume, sorbent dosage, contact time and leaching solution volumes, were investigated. Scanning electron microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy, BET surface area and pore size analysis were used for the characterisation of IIP (both unleached and leached) and CP materials. Optimal parameters were as follows: solution pH, 3; contact time, 120 min; eluent, 20 mℓ of 0.1 M NaOH; and sorbent amount, 125 mg. Maximum retention capacity of IIP and CP was 37.58 and 25.44 mg∙g-1, respectively. The extraction efficiencies of the IIP and CP were compared using a batch and SPE mode of extraction. In the absence of high concentrations of ions, especially sulphate ions, both CP and IIP demonstrated no differences in binding of Cr (VI), which was almost 100%. However, in the presence of high concentrations of sulphate ions, the selectivity on the CP completely collapsed. The study clearly demonstrates the suitably of the developed IIP for selective extraction of Cr (VI) in complex samples such as those from acid mine drainage. The selectivity was also compared by direct injection of the real-world sample, both spiked and non-spiked, into that obtained after IIP selective extraction. Despite the method’s very low detection limits for direct injection (below 1 μg∙ℓ-1), no Cr (VI) was obtained. However, after IIP selective extraction, spiked Cr (VI) was detected in the spiked sample.
- Full Text:
- Authors: Pakade, V , Cukrowska, E , Darkwa, J , Torto, N , Chimuka, Luke
- Date: 2011
- Language: English
- Type: Article
- Identifier: vital:6588 , http://hdl.handle.net/10962/d1004171
- Description: A linear copolymer was prepared from 4-vinylpyridine and styrene. An ion-imprinted polymer (IIP) specific for Cr (VI) adsorption was prepared by copolymerisation of the quaternised linear copolymer (quaternised with 1,4-chlorobutane), 2-vinylpyridine functional monomer and ethylene glycol dimethacrylate (EGDMA), as the cross-linking monomer, in the presence of 1,1’-azobis(cyclohexanecarbonitrile) as initiator. Ammonium dichromate and aqueous methanol were used as a template and porogenic solvent, respectively. Leaching of the chromate template from the polymer particles was achieved with successive stirring of the ion-imprinted polymer (IIP) particles in 4 M HNO3 solutions to obtain leached materials, which were then used for selective rebinding of Cr (VI) ions from aqueous solutions. Similarly, the non-imprinted polymer/ control polymer (NIP/CP) material was also prepared under exactly the same conditions as the IIP but without the chromate anion template. Various parameters, such as solution pH, initial concentration, aqueous phase volume, sorbent dosage, contact time and leaching solution volumes, were investigated. Scanning electron microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy, BET surface area and pore size analysis were used for the characterisation of IIP (both unleached and leached) and CP materials. Optimal parameters were as follows: solution pH, 3; contact time, 120 min; eluent, 20 mℓ of 0.1 M NaOH; and sorbent amount, 125 mg. Maximum retention capacity of IIP and CP was 37.58 and 25.44 mg∙g-1, respectively. The extraction efficiencies of the IIP and CP were compared using a batch and SPE mode of extraction. In the absence of high concentrations of ions, especially sulphate ions, both CP and IIP demonstrated no differences in binding of Cr (VI), which was almost 100%. However, in the presence of high concentrations of sulphate ions, the selectivity on the CP completely collapsed. The study clearly demonstrates the suitably of the developed IIP for selective extraction of Cr (VI) in complex samples such as those from acid mine drainage. The selectivity was also compared by direct injection of the real-world sample, both spiked and non-spiked, into that obtained after IIP selective extraction. Despite the method’s very low detection limits for direct injection (below 1 μg∙ℓ-1), no Cr (VI) was obtained. However, after IIP selective extraction, spiked Cr (VI) was detected in the spiked sample.
- Full Text:
Recent progress in electrochemical oxidation of saccharides at gold and copper electrodes in alkaline solutions
- Torto, N
- Authors: Torto, N
- Date: 2009
- Language: English
- Type: Article
- Identifier: vital:6599 , http://hdl.handle.net/10962/d1004348
- Description: This article reviews the progress made in the past 10 years, on electrochemical oxidation of saccharides in alkaline media for gold and copper electrodes. The mechanism and processes associated with the electrochemical oxidation of saccharides at native and surface coated electrodes continues to be of great interest. Despite the effort and various mechanisms proposed, still the need for an electrochemically active material that understands the complexity associated with saccharides continues to increase as their detection poses a challenge for bioanalytical chemistry and liquid chromatography.
- Full Text:
- Authors: Torto, N
- Date: 2009
- Language: English
- Type: Article
- Identifier: vital:6599 , http://hdl.handle.net/10962/d1004348
- Description: This article reviews the progress made in the past 10 years, on electrochemical oxidation of saccharides in alkaline media for gold and copper electrodes. The mechanism and processes associated with the electrochemical oxidation of saccharides at native and surface coated electrodes continues to be of great interest. Despite the effort and various mechanisms proposed, still the need for an electrochemically active material that understands the complexity associated with saccharides continues to increase as their detection poses a challenge for bioanalytical chemistry and liquid chromatography.
- Full Text:
- «
- ‹
- 1
- ›
- »