Amino-calixarene-modified graphitic carbon as a novel electrochemical interface for simultaneous measurement of lead and cadmium ions at picomolar level

Amino-calixarene-derivatized graphitic carbon electrode has been used in the simultaneous quantification of lead and cadmium ions at picomolar level. The graphitic carbon has been chemically modified using amino-calixarene as an indicator molecule through microwave irradiation, and it has been characterized by NMR, mass, and Fourier transform infrared spectroscopy (FTIR) techniques. The proposed sensor has shown linearity in the concentration range 10–120 pM with detection limits of 3.3 and 3.5 pM for lead and cadmium, respectively. The proposed sensor has been successfully applied to quantify lead and cadmium levels in battery effluents, alloy materials, and sewage water sample matrices. The results obtained by the proposed sensor are in agreement with the results of the standard protocols.     

A binderless,covalently bulk modified electrochemical sensor: Application to simultaneous determination of lead and cadmium at trace level

A new type of covalent binderless bulk modified electrode has been fabricated and used in the simultaneous determination of lead and cadmium ions at nanomolar level. The modification of graphitic carbon with 4-amino salicylic acid was carried out under microwave irradiation through the amide bond formation. The electrochemical behavior of the fabricated electrode has been carried out to decipher the interacting ability of the functional moieties present on the modifier molecules toward the simultaneous determination of Pb²⁺ and Cd²⁺ ions using cyclic and differential pulse anodic stripping voltammetry. The possible mode of interaction of functional groups with metal ions is proposed based on the pKa values of the modifier functionalities present on the surface of graphitic carbon particles. The analytical utility of the proposed sensor has been validated by measuring the lead and cadmium content from pretreated waste water samples of lead acid batteries.     

Surfactant mediated sulfide estimation at trace level: Application to environmental samples

A simple spectrophotometric method has been developed for the quantification of dissolved sulfide based on its reaction with ferric iron and the subsequent reaction of ferrous iron with 1-nitroso-2-naphthol in alkaline medium. The insoluble iron(II)-ligand complex has been solubilized in micellar medium using neutral surfactant which facilitates the non extraction step. The method obeys Beer??s law in the concentration range 0.5?C8 ??g in 10 mL of aqueous phase. The complex showed an absorption maximum at 710 nm with ?? value of 4.11 × 10⁴ L/mol cm. The detection limit has been found to be 0.0036 ??g/mL. The interference of common cations and anions has been studied and the proposed method has been successfully applied to determine the sulfide in different sewage water samples.     

CeO<Subscript>2</Subscript> nanoparticle-modified electrode as a novel electrochemical interface in the quantification of Zn<Superscript>2+ </Superscript>ions at trace level: application to real sample analysis

A simple strategy has been proposed to quantify Zn²⁺ ions using CeO₂ nanoparticle-modified glassy carbon electrode. The CeO₂ nanoparticles were prepared by sucrose-nitrate decomposition method, and it was characterized by X-ray diffraction (XRD), FT-IR, TEM, and surface area analyzer. The synthesized CeO₂ nanoparticles were used as modifier molecules as a thin film on glassy carbon electrode (GCE) in the trace level quantification of Zn²⁺ by using cyclic voltammetry (CV) and differential pulse anodic stripping voltammetry (DPASV) techniques. The fabricated sensor exhibited a good analytical response towards Zn²⁺ ions. The modified electrode showed a wide linearity in the concentration range 20–380 μg L^?1 with a limit of detection 0.36 μg L^?1. The proposed electrochemical sensor was successfully applied to trace level Zn²⁺ quantification from real sample matrices.     

Microwave-assisted functionalization of glassy carbon spheres: electrochemical and mechanistic studies

Functionalization of glassy carbon spheres have been carried out by microwave irradiation in the presence of modifier molecules through oxidation followed by amidation reaction. The glassy carbon spheres were initially catalyzed by treating with concentrated nitric acid to introduce surface-bound carboxylic groups, and its subsequent amidation reaction in the presence of p-nitroaniline yields p-nitroanilide-functionalized substrate materials. These derivatized glassy carbon spheres have been electrochemically characterized by immobilizing them on bppg electrode and studying its voltammetric behavior. X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy studies have revealed that the modifying molecules are surface bound and covalently attached on the carbon substrate.     

Chemically functionalized glassy carbon spheres: a new covalent bulk modified composite electrode for the simultaneous determination of lead and cadmium

A new type of covalent bulk modified glassy carbon composite electrode has been fabricated and utilized in the simultaneous determination of lead and cadmium ions in aqueous medium. The covalent bulk modification was achieved by the chemical reduction of 2-hydroxybenzoic acid diazonium tetrafluroborate in the presence of hypophosphorous acid as a chemical reducing agent. The covalent attachment of the modifier molecule was examined by studying Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and the surface morphology was examined by scanning electron microscopy images. The electrochemistry of modified glassy carbon spheres was studied by its cyclic voltammetry to decipher the complexing ability of the modifier molecules towards Pb²⁺ and Cd²⁺ ions. The developed sensor showed a linear response in the concentration range 1–10 μM with a detection limit of 0.18 and 0.20 μM for lead and cadmium, respectively. The applicability of the proposed sensor has been checked by measuring the lead and cadmium levels quantitatively from sewage water and battery effluent samples.     

Derivatization and characterization of functionalized carbon powder via diazonium salt reduction

Chemical reduction of 4-chloro-2-nitrobenzenediazonium chloride salt in the presence of hypophosphorous acid and carbon powder results in functionalized carbon powder with chloronitrophenyl groups attached on carbon particle surface. This type of bulk derivatization protocol is very useful and most inexpensive compared to widely used electrochemically assisted derivatization protocol. The derivatized carbon powder has been characterized by studying its Fourier transform infrared spectroscopy (FTIR) and cyclic voltammetric studies. The surface functionalized moieties have been examined electrochemically by immobilizing them onto the surface of basal plane pyrolytic graphite electrode and studying its cyclic voltammetry. The effect of pH, scan rate (v), and the peak potentials (E _p) as a function of pH has revealed that the species are surface bound in nature and covalently attached on the carbon surface. The FTIR studies of the derivatized carbon powder have revealed that the modifying molecule is covalently attached on the carbon particle surface.     

Extractive spectrophotometric determination of trace amounts of nitrogen dioxide,nitrite, and nitrate

A sensitive extractive spectrophotometric method for the determination of nitrogen dioxide in air and nitrite and nitrate in water, soil and blood serum is described. Nitrogen dioxide in air is fixed as nitrite in a suitable trapping solution. The method is based on the diazo coupling reaction betweenp-nitroaniline andN-(1-naphthyl)ethylenediamme dihydrochloride [NEDA]. The azo dye formed under aqueous conditions is extracted with isobutyl methyl ketone [IBMK]. The system obeys Beer's law over the range 0–3 g of nitrite at 545 nm and the colour is stable for 3h. The molar absorptivity of the colour system is 5.7 × 10⁴ L mol^–1 cm^–1. The relative standard deviation is 1.3% for ten determinations at 2 ug of nitrite. Nitrate is determined as nitrite after reduction on a cadmium column. Negative interferences from SO₂, H₂S, Cu²⁺ and Cr³⁺ and positive interference from Fe²⁺ and Fe³⁺ can be simply masked.     

Bioimaging of Peroxynitrite in MCF-7 Cells by a New Fluorescent Probe Rhodamine B Phenyl Hydrazide

Peroxynitrite is a potent oxidizing and nitrating agent which has detrimental effects on cells by altering the structure and function of biomolecules present within. A fluorescent probe rhodamine B phenyl hydrazide (RBPH) has been proposed for peroxynitrite (ONOO^?) imaging in MCF-7 cells based on its oxidation property, which converts RBPH to pink colored and highly fluorescent rhodamine B. The fluorescence emission intensity of the rhodamine B produced in the above process is linearly related to the concentration of peroxynitrite. The method obeys Beer’s law in the concentration range 2–20 nM and the detection limit has been found to be 1.4 nM. The possible reaction mechanism of peroxynitrite with RBPH to produce rhodamine B has been discussed with spectroscopic evidence. The Probe is selective to the peroxynitrite in the pH range 6–8 which is near physiological pH. Fluorescence microscopic studies suggest that the probe is cell permeable and hence peroxynitrite was imaged in MCF-7 cells.