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1.
Anal Methods ; 16(26): 4415-4420, 2024 Jul 04.
Artículo en Inglés | MEDLINE | ID: mdl-38904354

RESUMEN

A nanoporous gold microelectrode (NPG-µE) was fabricated and used for Pb(II) detection in seawater samples via square wave anodic stripping voltammetry (SWASV). The Au microelectrode (Au-µE) was fabricated by embedding a gold microfiber into a Pasteur pipette, and its surface was further modified by an anodization-electrochemical reduction (A-ECR) method, yielding the NPG-µE. The fabricated electrodes were characterized by cyclic voltammetry (CV) and field emission scanning electron microscopy (FE-SEM) for electrochemical and structural morphological investigations. SWASV results show a Pb(II) stripping peak at around -0.05 V vs. Ag/AgCl, sat. KCl, which is unusual for common Pb(II) detection (typically occurring at around -0.40 V) in anodic stripping voltammetry (ASV) analysis. The Pb(II) detection at less negative stripping potential is more beneficial. Hence, it exhibited anti-interference properties with Cd(II), which is attributed to the preferential deposition and stripping of the target analyte on the low-indexed crystal planes of the NPG structure. The calibration plot obtained by SWASV was linear in the concentration range of 0.1-10 µM, and the detection limit was found to be 57 nM (correlation coefficient of 0.9974). The NPG microsensor presented a 15-fold enhanced current response compared to Au-µE, with excellent sensitivity (27.2 µA µM-1 cm-2). The application of the NPG microsensor was examined by detecting Pb(II) in seawater samples, and a satisfactory performance was obtained.

2.
Chem Commun (Camb) ; 60(2): 176-179, 2023 Dec 21.
Artículo en Inglés | MEDLINE | ID: mdl-37965951

RESUMEN

Metal-free hydride stabilized boron nanosheets (H-BNS) were prepared in an aqueous medium without using noble metal growth substrates via sonochemistry. The reducing ability of H-BNS was demonstrated with Au3+(aq) reduction, and its layered morphology is exploited for Li-ion battery (LIB) applications.

3.
Talanta ; 226: 122130, 2021 May 01.
Artículo en Inglés | MEDLINE | ID: mdl-33676684

RESUMEN

In this work, nanoporous gold (NPG) was prepared according to three different approaches, such as (i) anodization-electrochemical reduction (A-ECR, NPGA), (ii) dynamic hydrogen bubble template (DHBT, NPGB), and (iii) the combination of both methods (NPGA+B). Field-emission scanning electron microscopy (FE-SEM) and cyclic voltammetry (CV) were used to investigate the structural morphology and the electrochemical behavior of the fabricated materials. The NPGA+B electrode showed a large amount of surface defects and/or edges, greater electrochemical surface area (2.5 cm2), and increased roughness factor (35.4). Such outstanding features of the NPGA+B platform were demonstrated by the sensitive detection of methyl parathion (MP) in river water samples. CV results indicated nearly 25-fold, 6-fold, and 2.5-fold higher sensitivity for NPGA+B compared to that of bare Au, NPGA, and NPGB, respectively. Differential pulse voltammetry (DPV) results show a linear behavior in the MP concentration range of 5-50 ng mL-1 with a limit of detection (LOD) of 0.6 ng mL-1 and limit of quantification (LOQ) of 2.0 ng mL-1. Besides, the NPGA+B sensor also revealed excellent selectivity towards MP detection in the presence of other interfering molecules or ions, reproducibility, and repeatability.

4.
RSC Adv ; 11(8): 4478-4488, 2021 Jan 21.
Artículo en Inglés | MEDLINE | ID: mdl-35424389

RESUMEN

A Prosopis juliflora-seed-modified Amberlite IRA-400 Cl- ion-exchange resin (hereafter denoted as SMA resin) is used for the removal of Pb2+ from wastewater. SEM, EDX, FT-IR, BET, XRD, and XPS analyses were used to characterize the SMA resin. Parameters such as Pb2+ concentration, pH, temperature, and time are optimized. The obtained results show that the SMA resin has high efficiency for the removal of Pb2+ (73.45%) at a concentration of 100 mg L-1 and a dosage of 0.01 g at pH 6. Thermodynamic studies indicate that the adsorption was spontaneous with negative ΔH° and ΔS° values at all temperatures; pseudo-second-order kinetics and the Langmuir adsorption isotherm provided the best fit (q max = 106 mg g-1 and R 2 = 0.99) from 298 to 338 K. In addition, a diffusion-controlled mechanism at 298 K was observed from intra-particle studies. A desorption and recovery process has been applied successfully to the SMA adsorbent. The obtained results showed desorption of 90.7% at pH 2.5 with 86.3% recovery over six cycles. Furthermore, the DFT results suggest that all the functional groups of the SMA resin possibly bind with Pb2+ and, of these, the -C[double bond, length as m-dash]O group shows the highest binding energy towards Pb2+. Moreover, the high-efficiency removal of Pb2+ from synthetic wastewater using the proposed SMA resin was demonstrated to show the real-life application potential.

5.
Mikrochim Acta ; 185(8): 367, 2018 07 09.
Artículo en Inglés | MEDLINE | ID: mdl-29987397

RESUMEN

Nanoporous gold (NPG) structures were prepared on the surface of a gold microelectrode (Au-µE) by an anodization-reduction method. Cyclic voltammetry and field emission scanning electron microscopy were used to study the electrochemical properties and the morphology of the nanostructured film. Voltammetry showed an improved sensitivity for dopamine (DA) oxidation at this microelectrode when compared to a bare gold microelectrode, with a peak near 0.2 V (vs. Ag/AgCl) at a scan rate of 0.1 V s-1. This is due to the increased surface area and roughness. Square wave voltammetry shows a response that is linear in the 0.1-10 µmol L-1 DA concentration range, with a 30 nmol L-1 detection limit and a sensitivity of 1.18 mA (µmol L-1)-1 cm-2. The sensor is not interfered by ascorbic acid. The reproducibility, repeatability, long-term stability and real sample analysis (spiked urine) were assessed, and acceptable performance was achieved. The "proof-of-concept" detection of dopamine release was demonstrated by using scanning electrochemical microscopy (SECM) with the aim of future applications for single cell analysis. Graphical abstract A reproducible electrochemical approach was proposed to fabricate an NPG-microelectrode for DA detection, with enhanced sensitivity and selectivity. Besides, a proof-of-concept detection of DA release was also demonstrated by using SECM.


Asunto(s)
Dopamina/análisis , Electroquímica/instrumentación , Oro/química , Microscopía Electroquímica de Rastreo , Nanoporos , Dopamina/orina , Límite de Detección , Microelectrodos
6.
Phys Chem Chem Phys ; 17(43): 28510-4, 2015 Nov 21.
Artículo en Inglés | MEDLINE | ID: mdl-26446050

RESUMEN

A nanoporous gold film (NPGF) was prepared onto a gold electrode surface using a facile and green electrochemical approach via anodization at 2.0 V in 0.5 mol L(-1) H2SO4. The as-synthesized NPGF electrode showed superior electrocatalytic activity towards dissolved oxygen reduction at a low overpotential (-0.045 V) along with 2-fold enhanced sensitivity.


Asunto(s)
Técnicas Electroquímicas , Oro/química , Oxígeno/química , Catálisis , Electrodos , Nanopartículas del Metal/química , Nanoporos/ultraestructura , Oxidación-Reducción , Ácidos Sulfúricos/química
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