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1.
Materials (Basel) ; 15(17)2022 Aug 26.
Artigo em Inglês | MEDLINE | ID: mdl-36079276

RESUMO

Graphene produced by different methods can present varying physicochemical properties and quality, resulting in a wide range of applications. The implementation of a novel method to synthesize graphene requires characterizations to determine the relevant physicochemical and functional properties for its tailored application. We present a novel method for multilayer graphene synthesis using atmospheric carbon dioxide with characterization. Synthesis begins with carbon dioxide sequestered from air by monoethanolamine dissolution and released into an enclosed vessel. Magnesium is ignited in the presence of the concentrated carbon dioxide, resulting in the formation of graphene flakes. These flakes are separated and enhanced by washing with hydrochloric acid and exfoliation by ammonium sulfate, which is then cycled through a tumble blender and filtrated. Raman spectroscopic characterization, FTIR spectroscopic characterization, XPS spectroscopic characterization, SEM imaging, and TEM imaging indicated that the graphene has fifteen layers with some remnant oxygen-possessing and nitrogen-possessing functional groups. The multilayer graphene flake possessed particle sizes ranging from 2 µm to 80 µm in diameter. BET analysis measured the surface area of the multilayer graphene particles as 330 m2/g, and the pore size distribution indicated about 51% of the pores as having diameters from 0.8 nm to 5 nm. This study demonstrates a novel and scalable method to synthesize multilayer graphene using CO2 from ambient air at 1 g/kWh electricity, potentially allowing for multilayer graphene production by the ton. The approach creates opportunities to synthesize multilayer graphene particles with defined properties through a careful control of the synthesis parameters for tailored applications.

2.
Environ Monit Assess ; 191(11): 646, 2019 Oct 16.
Artigo em Inglês | MEDLINE | ID: mdl-31620892

RESUMO

A major ecological challenge facing freshwater resources such as rivers is the influx of chemical contaminants from anthropogenic sources. A report on the levels of heavy metals, namely Zn, Cu, Cr, Cd and Pb in benthic macroinvertebrates, sediments and water along River Isiukhu, within Lake Victoria catchment area in Kenya is presented. Families of benthic macroinvertebrates that were investigated included Gerridae, Baetidae and Unionidae. Samples were digested using the appropriate acid combination and analysed using Spectra AAS Varian 200. Physicochemical parameters were measured on-site using mobile Hydrolab Quanta. Pearson's correlation matrix and post hoc Tukey's test were used to show the relationship between metal concentrations in the various matrices at significant differences accepted at p ≤ 0.05. Positive correlations were obtained for heavy metal concentrations in sediments and benthic macroinvertebrates with significant correlations observed for Zn (r = 0.655, p = 0.029) and Cu (r = 0.641, p = 0.034). Sediments presented the highest range of heavy metal concentrations compared to water and benthic macroinvertebrates and presented the only matrix with quantifiable Pb levels. The range in heavy metal concentration in benthic macroinvertebrates samples were as follows: Zn, 30.73-46.64, 21.93-38.17, and 26.85-41.69 mg/kg, Cu, 1.17-6.54, 1.11-3.87 and 1.15-5.79 mg/kg, Cr, 0.47-1.61, 0.22-0.74 and 0.25-0.92 mg/kg, for families Unionidae, Baetidae and Gerridae respectively. Heavy metal concentration profile along the river indicated an influx of pollutants from anthropogenic sources due to rapid urbanization along the river.


Assuntos
Monitoramento Ambiental , Sedimentos Geológicos/química , Invertebrados/química , Metais Pesados/análise , Rios/química , Poluentes Químicos da Água/análise , Animais , China , Ecologia , Ephemeroptera/química , Heterópteros/química , Quênia , Lagos/química , Medição de Risco , Unionidae/química , Água/química
3.
Bioelectrochemistry ; 75(2): 117-23, 2009 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-19336272

RESUMO

This paper describes the use of horseradish peroxidase (HRP) based biosensor for novel detection of glyphosate herbicide. The biosensor was prepared by electrochemically depositing poly(2,5-dimethoxyaniline) (PDMA) doped with poly(4-styrenesulfonic acid) (PSS) onto the surface of a gold electrode followed by electrostatic attachment of the enzyme HRP onto the PDMA-PSS composite film. Fourier transform infrared (FTIR) and UV-Vis spectrometry inferred that HRP was not denatured during its immobilization on PDMA-PSS composite film. The biosensing principle was based on the determination of the cathodic responses of the immobilized HRP to H(2)O(2), before and after incubation in glyphosate standard solutions. Glyphosate inhibited the activity of HRP causing a decrease in its response to H(2)O(2). The determination of glyphosate was achieved in the range of 0.25-14.0 microg L(-1) with a detection limit of 1.70 microg L(-1). The apparent Michaelis-Menten constant (calculated for the HRP/PDMA-PSS biosensor in the presence and absence of glyphosate was found to be 7.73 microM and 7.95 microM respectively.


Assuntos
Técnicas Biossensoriais/métodos , Eletroquímica/métodos , Glicina/análogos & derivados , Herbicidas/análise , Peroxidase do Rábano Silvestre/química , Compostos de Anilina/química , Enzimas Imobilizadas/química , Glicina/análise , Peróxido de Hidrogênio/química , Polímeros/química , Sensibilidade e Especificidade , Espectrofotometria , Espectroscopia de Infravermelho com Transformada de Fourier , Ácidos Sulfônicos/química , Glifosato
4.
Sensors (Basel) ; 8(11): 6791-6809, 2008 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-27873900

RESUMO

An electrochemical DNA nanobiosensor was prepared by immobilization of a 20mer thiolated probe DNA on electro-deposited generation 4 (G4) poly(propyleneimine) dendrimer (PPI) doped with gold nanoparticles (AuNP) as platform, on a glassy carbon electrode (GCE). Field emission scanning electron microscopy results confirmed the codeposition of PPI (which was linked to the carbon electrode surface by C-N covalent bonds) and AuNP ca 60 nm. Voltammetric interrogations showed that the platform (GCE/PPI-AuNP) was conducting and exhibited reversible electrochemistry (E°' = 235 mV) in pH 7.2 phosphate buffer saline solution (PBS) due to the PPI component. The redox chemistry of PPI was pH dependent and involves a two electron, one proton process, as interpreted from a 28 mV/pH value obtained from pH studies. The charge transfer resistance (Rct) from the electrochemical impedance spectroscopy (EIS) profiles of GCE/PPI-AuNP monitored with ferro/ferricyanide (Fe(CN)63-/4-) redox probe, decreased by 81% compared to bare GCE. The conductivity (in PBS) and reduced Rct (in Fe(CN)63-/4-) values confirmed PPI-AuNP as a suitable electron transfer mediator platform for voltammetric and impedimetric DNA biosensor. The DNA probe was effectively wired onto the GCE/PPI-AuNP via Au-S linkage and electrostatic interactions. The nanobiosensor responses to target DNA which gave a dynamic linear range of 0.01 - 5 nM in PBS was based on the changes in Rct values using Fe(CN)63-/4- redox probe.

5.
Sensors (Basel) ; 8(12): 8262-8274, 2008 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-27873987

RESUMO

An aflatoxin B1 (AFB1) electrochemical immunosensor was developed by the immobilisation of aflatoxin B1-bovine serum albumin (AFB1-BSA) conjugate on a polythionine (PTH)/gold nanoparticles (AuNP)-modified glassy carbon electrode (GCE). The surface of the AFB1-BSA conjugate was covered with horseradish peroxidase (HRP), in order to prevent non-specific binding of the immunosensors with ions in the test solution. The AFB1 immunosensor exhibited a quasi-reversible electrochemistry as indicated by a cyclic voltammetric (CV) peak separation (ΔEp) value of 62 mV. The experimental procedure for the detection of AFB1 involved the setting up of a competition between free AFB1 and the immobilised AFB1-BSA conjugate for the binding sites of free anti-aflatoxin B1 (anti-AFB1) antibody. The immunosensor's differential pulse voltammetry (DPV) responses (peak currents) decreased as the concentration of free AFB1 increased within a dynamic linear range (DLR) of 0.6 - 2.4 ng/mL AFB1 and a limit of detection (LOD) of 0.07 ng/mL AFB1. This immunosensing procedure eliminates the need for enzyme-labeled secondary antibodies normally used in conventional ELISA-based immunosensors.

6.
Anal Bioanal Chem ; 388(5-6): 1069-74, 2007 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-17563886

RESUMO

Aflatoxins are a group of mycotoxins that have deleterious effects on humans and are produced during fungal infection of plants or plant products. An electrochemical immunosensor for the determination of aflatoxin B(1) (AFB(1)) was developed with AFB(1)antibody (AFB(1)-Ab) immobilized on Pt electrodes modified with polyaniline (PANi) and polystyrene sulphonic acid (PSSA). Impedimetric analysis shows that the electron transfer resistances of the Pt/PANi-PSSA electrode, the Pt/PANi-PSSA/AFB(1)-Ab immunosensor and Pt/PANi-PSSA/AFB(1)-Ab incubated in bovine serum albumin (BSA) were 0.458, 720 and 1,066 kOmega, respectively. These results indicate that electrochemical impedance spectroscopy (EIS) is a suitable method for monitoring the change in electron transfer resistance associated with the immobilization of the antibody. Modelling of EIS data gave equivalent circuits which showed that the electron transfer resistance increased from 0.458 kOmega for the Pt/PANi-PSSA electrode to 1,066 kOmega for the Pt/PANi-PSSA/AFB(1)-Ab immunosensor, indicating that immobilization of the antibody and incubation in BSA introduced an electron transfer barrier. The AFB(1) immunosensor had a detection limit of 0.1 mg/L and a sensitivity of 869.6 kOmega L/mg.


Assuntos
Aflatoxina B1/análise , Compostos de Anilina/análise , Técnicas de Química Analítica/métodos , Eletroquímica/métodos , Micotoxinas/análise , Compostos de Anilina/química , Técnicas Biossensoriais , Impedância Elétrica , Eletrodos , Elétrons , Humanos , Modelos Teóricos , Polímeros/química , Poliestirenos/análise , Soroalbumina Bovina/análise
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