Madan Lal Singla

One step electrochemical synthesis of gold-nanoparticles–polypyrrole composite for application in catechin electrochemical biosensor

An electrochemical biosensor has been fabricated for catechin detection using the nanoparticle–polymer composite as a matrix. The composite has been electrochemically synthesized and tyrosinase enzyme was entrapped during polymerization of the composite material. The composite has been characterized for its morphology, optical, structural, and electrochemical behavior. Studies revealed that the presence of gold nanoparticles (AuNPs) in the polymer matrix resulted in an increase in conductivity, enhanced current intensity and diffusion coefficient. The AuNPs–PPy composite provided large surface area for enzyme immobilization and facilitated electron transfer, evident from almost 10% enhancement in biosensor response in the presence of nanoparticles (NPs). For catechin detection, the biosensor showed well defined redox peaks at 0.24 V/0.14 V for the redox reaction of the hydroxyl group present in the catechol moiety of the catechin and a weak oxidation peak at 0.62 V corresponding to the oxidation of the hydroxyl group present in the central ring of catechin. The linearity was achieved from 1 × 10−9 M to 1 × 10−8 M, with a sensitivity of 6.8 × 10−5 A M−1. The limit of detection (3 × SD/sensitivity) and Km value are 1.2 × 10−9 M and 4.5 × 10−9 M respectively. The response time of the biosensor was about 10–12 s with an optimum pH at 7.0. The biosensor has been tested for catechin detection in water and apple juices and the response was within 10% error.

Synthesis, characterization, and thermal study of polyaniline composite with the photoadduct of potassium hexacyanoferrate (II) involving hexamine ligand

The present paper involves the synthesis of polyaniline (PANI) composite with photoadduct of potassium hexacyanoferrate (II) involving hexamine as a ligand and cobalt chloride as a complexing agent via in situ oxidative polymerization by ammonium persulphate. The photoadduct has been synthesized by photoirradiation followed by substitution with the hexamine ligand. The final product has been isolated by using CoCl2 as complexing agent. Viscosity average molar mass has been determined by viscosity method using Ostwald’s viscometer. The photoirradiation, substitution, and successful synthesis have been proved by recording pH, UV–visible spectra before and after irradiation, and FTIR of the photoadduct. The composite based on the synthesized photoadduct has been subjected to FTIR, X-ray diffraction, and SEM characterization techniques. Thermal analysis has been done by using TG and DSC technique. FTIR absorption peaks confirm the insertion of photoadduct in the backbone of PANI. SEM of the composite also supports its successful synthesis. The XRD of photoadduct shows crystalline structure, which has remained dominant in the composite, hence proving the successful synthesis of PANI composite with photoadduct. Thermal analysis shows high thermal stability of photoadduct which in turn has improved the thermal stability of PANI composite, therefore, shows the potential of composite for high-temperature application purposes.

Facile Route for the Synthesis of a Vertically Aligned ZnO–PANI Nanohybrid Film for Polyphenol Sensing

Vertically aligned zinc oxide (ZnO) nanorods have been fabricated on a polyaniline (PANI) film template after electrochemical seeding and hydrothermal growth in a nutrient medium at a low temperature of 65 °C. Dense c-oriented [0001], hexagonal-shaped, vertically aligned ZnO nanorods are obtained on the PANI film surface, which is confirmed by X-ray diffraction and scanning electron microscopy studies. The nanohybrid film used as the working electrode has been characterized for sensing catechin polyphenol in different tea varieties through cyclic voltammetry. Principal component analysis shows enhancement in the classification ability of the nanohybrid film for various concentrations of catechin standard and tea infusions.

Selective electrochemical sensing for arsenite using rGO/Fe3O4 nanocomposites.

Herein, we report rGO/Fe3O4 nanocomposites (NCs) free from noble metals, synthesized by facile one step chemical reduction method, for electrochemical detection of arsenite in water by square wave anodic stripping Voltammetry (SWASV). The synthesized NCs were characterized for its optical, morphological and structural properties. The NCs modified glassy carbon (GCE), NCs/GCE, electrodes showed a higher sensitivity (0.281μA/ppb) and lower LOD (0.12ppb) under optimized experimental conditions. The proposed NCs/GCE electrodes show no interference towards arsenite species in the presence of common cationic interferants, namely, Cu(II), Pb(II), Ni(II), Co(II), Cd(II), Cr(II), Zn(II), etc. In addition, the proposed electrode demonstrates a good stability, reproducibility and potential practical application in electrochemical detection of arsenite.

Role of photoadduct of K4Fe(CN)6 and C3H4N2 in improving thermal stability of polyaniline composite

This paper involves the synthesis of polyaniline composite with photoadduct of potassium hexacyanoferrate and imidazole via photochemical route by oxidative polymerization technique by ammonium persulphate. The photoadduct has been synthesized by photoirradiation followed by substitution with imidazole ligand. The photoaquation, substitution and successful synthesis has been proved by recording pH, UV visible spectra before and after irradiation and XRD of photoadduct. The as synthesized composite has been subjected to various characterizations like elemental analysis, UV–Visible spectra, FTIR, XRD, SEM, and TG/DTG. XRD of photoadduct shows crystalline structure which has been retained in the composite, changing the amorphous structure of polyaniline into the crystalline one, hence proving the insertion of photoadduct in the polymer chain. Various parameters like crystallite size (L), interplanar distance (d), micro strain (ε), dislocation density (δ) and distortion parameters (g) were calculated from XRD data. Thermal analysis shows the high thermal stability of composite which can be due to strong interaction between polymer chain and the photoadduct which restricts the thermal motion of polyaniline and thus enhances the thermal stability of composite.

Simple fiber-optic technique for in-situ corrosion sensing in structures

Corrosion of structures is a serious problem involving man and material safety. Over the years, though several methods of monitoring corrosion have been devised with some success, but there is a persistent need for devising non-destructive and in-situ techniques for monitoring corrosion in structures. Fiber optic techniques are capable of meeting these requirements, besides offering several other important advantages. Fiber optic corrosion sensors have thus become quite attractive and are currently being investigated to address the high costs associated with the existing structural maintenance procedures. Fiber optics based direct absorption spectroscopic techniques investigated by some groups for estimating corrosion have used single fiber elements for recording the signal reflected from specimen at different wavelengths. As the light coupling efficiency of the single fiber elements is relatively poor in comparison with that of fiber bundles and the signal available for processing is weak, the paper presents a simple and alternate technique based on the color matching principle of fiber optic colorimetry to detect corrosion induced color changes. It employs a thin Y- shaped fiber optic bundle which increases the quantity of light energy coupled from a whitelight source. The light reflected off the sample is made incident on a PIN photo- detector through a complementary filter. A series of such probes can be safety embedded and or bonded to structures at pre-determined locations. The experimental set up for this sensor was implemented and feasibility of in-situ corrosion detection in structures demonstrated. Measurement data was acquired for steel samples corroded both in concrete embedded and open ambience conditions and results analyzed.

Highly reflective titania nanoparticle‐based coating

Purpose – The purpose of this paper is to investigate the reflective properties of titania (TiO2) nanoparticle‐based coating.Design/methodology/approach – TiO2 nanoparticles, synthesised by sol‐gel method, were characterised by X‐ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and ultraviolet‐visible absorption spectroscopy (UV‐vis). The coating material has been prepared by dispersing titania nanoparticles in an acrylic binder with different pigment to binder weight ratio. The reflectors were prepared by applying this coating material to different coating thicknesses to aluminium sheets.Findings – In the study reported here, the coating material could produce reflectors with diffuse reflectance, ∼99 per cent, using coating material, having binder by weight ratio between 14 and 20 per cent, and thickness, 0.15 mm. On exposing the developed reflectors to different levels of illumination (upto 20,000 lux), they were still found to have diffuse reflectance o...

Synthesis of silica/Au core- shell nanostructures by galvanic replacement of silica/Ag in aqueous and alkaline medium

We present here a facile one-step method for the synthesis of silica/Au core-shell nanostructures by exploiting the potential difference of AuCl4− and Ag in aqueous as well as alkaline media. Initially, silica/Ag core-shell nanostructures were synthesised by coating Ag nanoparticles on silica core (size ∼150 nm) in a two-step process (seeding and growth) and were characterised for their morphological, structural and optical behaviours. A complete coverage of silica core with Ag nanoparticles was seen from scanning electron microscope and transmission electron microscope images. The presence of resonance peaks in the optical spectrum manifests the nature of the shell (thin shell ∼413 and 650 nm, thick shell ∼434 nm). Galvanic replacement of silica/Ag core-shell nanostructures in chloroauric acid solution (HAuCl4) was studied in both the aqueous and alkaline medium, where an aqueous environment results into fast and effective replacement as compared to an alkaline medium, which has been confirmed from optical absorption studies. The optical studies showed that in an alkaline environment, on galvanic replacement of Ag with Au, the individual absorption peak of Ag (∼414 nm) and Au (∼520 nm) disappeared, whereas new absorption wavelengths in higher region (600–800 nm) of electromagnetic spectrum were observed. A detailed mechanism is proposed for the same to explain this behaviour. A range of novel new plasmonic core-shell nanomaterials can be synthesised as an intermediate of this facile one-step reaction.