Fabrication of ferrocene functionalised ionic liquid/carbon nanotube nanocomposite modified carbon-ceramic electrode: application to the determination of hydrazine

A novel ionic liquid, 1-(ferrocenyl butyl)-3-methylimidazolium tetrafluoroborate (Fc-IL), was synthesised. The nanocomposite of Fc-IL and multi-walled carbon nanotubes (MWCNTs) was constructed and used for surface modification of carbon-ceramic electrode. The modified electrode was applied to the determination of hydrazine. Operational parameters such as pH of the solution, ionic liquid volume and amount of carbon nanotubes, which affect the analytical performance of the modified electrode, were optimised. The linear range of the modified electrode toward hydrazine concentration was 0.96–106.10 μg L^–1 with a detection limit of 0.64 μg L^–1 (S/N = 3). The modified electrode displayed high repeatability, reproducibility, long-term life time and low response time (<3 s). The applicability of this method was further tested by analysing the hydrazine content in boiler-feed water samples containing different concentrations of hydrazine and the results were in good agreement with the spectrophotometry method.     

Studies on Mo doped vanadium oxide film by pulsed RF magnetron sputtering

Molybdenum doped vanadium oxide film on quartz and silicon substrates are grown by pulsed RF magnetron sputtering method. Surface morphology, phase analysis and oxide states are investigated by field emission scanning electron microscopy, X‐ray diffraction and X‐ray photoelectron spectroscopy techniques, respectively. Crystalline nature of the film deposited on both quartz and silicon are depicted. The transmittance and reflectance spectra recorded for the entire solar region. Further, optical constants viz. optical band gap and refractive index of the deposited films are estimated. Wavelength dependent low reflectance characteristic is observed for the deposited film on silicon. IR emittance (ε_IR) and sheet resistance (R_s) of the film are also evaluated. Copyright © 2017 John Wiley & Sons, Ltd.     

Antifungal activity of essential oil from Asteriscus graveolens against postharvest phytopathogenic fungi in apples

The essential oils of the aerial parts of Asteriscus graveolens have been studied using GC and GC-MS. Twenty-eight compounds were identified in the essential oil amounting to 94.9% of the total oil. The aerial part oils showed similar chromatographic profiles and were characterized by having a high content of oxygenated sesquiterpenes with 6-oxocyclonerolidol (66.7% +/- 5.5) and 6-hydroxycyclonerolidol (8.8% +/-1.2) as the major components. The antifungal effect of the essential oil from A. graveolens leaves was evaluated in vitro against three phytopathogenic fungi of apples (Alternaria sp., Penicillium expansum, and Rhizopus stolonifer). The results suggest that this essential oil has fungicidal properties towards Alternaria sp. from direct contact assay at 0.2% (v/v) and to P. expansum from vapor assay tests at 80 microL.     

Stripping voltammetric determination of copper(II) in natural waters and human hairs based on the adsorption of its complex with Kryptofix 22 on the carbon paste electrode

Traces of copper(II) can be determined by adsorptive stripping voltammetry using Kryptofix 22 as complex forming reagent. First, copper(II)-Kryptofix 22 complex was adsorbed on the carbon paste electrode in phosphate buffer pH 5.3 with an accumulation potential of −0.5 V. Following this, the adsorbed complex was oxidized and detected by anodic differential pulse voltammetric scan from −0.2 to 0.1 V. The effective parameters of sensor response were examined. The detection limit of copper(II) was 1.1 μg/L and relative standard deviations for 50 and 150 μg/L of Cu(II) were 1.2 and 0.96%, respectively. The calibration curve was linear for 2–150 μg/L of copper(II). This technique does not use mercury and therefore is environmentally beneficial. The method, which is reasonably sensitive and selective, has been successfully applied to the determination of trace amounts of copper(II) in water and human hair samples.     

Evaluation of the inhibitive effect of essential oil of Lavandula multifida L., on the corrosion behavior of C38 steel in 0.5 M H2SO4 medium

The essential oil of the aerial parts of Lavandula multifida L., collected in Errachidia region (three samples) in southeast Morocco, was extracted by hydrodistillation and analyzed by GC and GC-MS. The oil was predominated by carvacrol (57.9–59.0%). L. multifida oil was tested as corrosion inhibitor of C38 steel in 0.5 M H₂SO₄ using weight loss measurements, electrochemical polarization, and EIS methods. The results obtained by measurements of weight loss showed that inhibition efficiency increases with inhibitor concentration to attain 72.2% at 2 g/l of oil at 298 K. Polarization curves revealed that L. multifida oil acts as mixed type inhibitor. The temperature effect on the corrosion behavior of steel in 0.5 M H₂SO₄ without and with the inhibitor at 2 g/l was studied in the temperature range from 303 and 343 K. The adsorption of inhibitor on the C38 steel surface was found to be a spontaneous process and to obey Langmuir’s adsorption isotherm. The associated activation energy has been determined.     

Solid-phase molecularly imprinted pre-concentration and spectrophotometric determination of isoxicam in pharmaceuticals and human serum

A selective molecularly imprinted polymer (MIP) has been synthesized for isoxicam pre-concentration, followed by its spectrophotometric determination based on hydrogen bonding interactions between examined drug and alizarin yellow GG. This method is able to evaluate isoxicam in range of 1.0 × 10⁻³ to 20.0 μg mL⁻¹, with a limit of determination of 1.0 ng mL⁻¹. The retention capacity and pre-concentration factor of prepared sorbent are 18.5 mg g⁻¹ and 200, respectively; and the prepared MIPs can be reused at least for five times. The MIP capability for isoxicam selection and extraction from the solution is higher than non-imprinted polymer (NIP). Under optimum conditions, this procedure can be successfully applied to assay trace amounts of isoxicam in pharmaceutical and biological samples.     

Development of a body fluid identification multiplex via DNA methylation analysis

The goal of this study is to develop an epigenetic multiplex for body fluid identification based on tissue specific DNA methylation. A series of genetic loci capable of discerning the origin of DNA as coming from saliva, blood, vaginal epithelia, or semen were used for this application. The markers – BCAS4, CG06379435, VE_8, and ZC3H12D – were amplified together and then sequenced via pyrosequencing. Methylation values for cytosine guanine dinucleotide (CpG) sites at each locus were then measured across the four markers. In total, 124 samples were collected, and bisulfite modified to convert unmethylated DNA to uracil. This converted DNA was then amplified via multiplex PCR with reverse primers containing a biotin molecule. Biotinylated PCR products were then analyzed using pyrosequencing to generate a series of pyrograms containing 18 CpG sites. The percent methylation at each CpG site was determined, and then agglomerative hierarchical cluster analysis was used to create a model to indicate sample origin. Further analysis reduced the number of CpG sites required for optimal determination of body fluid type to five. This study demonstrates an efficient multiplexed body fluid identification process utilizing DNA methylation that can be easily implemented in forensic laboratories.     

Development of Voltammetric Sensor for Determination of Tryptophan Using MWCNTs‐modified Sol‐gel Electrode

In the present work, an electrochemical sensor was developed for simple and sensitive determination of tryptophan (Trp) using multi‐walled carbon nanotubes modified sol‐gel electrode (MWCNTs/SGE). The electrocatalytic oxidation of tryptophan was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). It was found that the oxidation peak current of Trp at the MWCNTs/SGE was greatly improved compared with that of the bare SGE. Furthermore, at the MWCNTs/SGE, the anodic peak potential of Trp is shifted about 220 mV to more negative value indicated that modified electrode has better electrocatalytic activity for electro‐oxidation of Trp. The anodic peak currents increased linearly with the concentration of tryptophan in the range of 0.2 × 10^?6 to 15 × 10^?6 M with a detection limit of 0.139 × 10^?6 M (at an S/N = 3).     

Electrochemical and electrocatalytic behaviors of Safranin O/Nafion film deposited on the glassy carbon electrode

The glassy carbon (GC) electrode modified with Nafion and Safranin O (SFO) was prepared and its electrochemical properties were investigated. The SFO molecules were strongly and irreversibly adsorbed on the Nafion — modified GC surface. The electrochemical behavior and mechanism for interactions of the SFO molecules with the Nafion film were investigated through cyclic voltammetric method. The electrocatalytic reduction of nitric oxide was performed at this modified electrode by cyclic voltammetric and hydrodynamic amperometric techniques. The Nafion membrane played a duel role as a matrix for the SFO immobilization and also helped to partition the nitric oxide from the solution phase. The diffusion coefficient of NO at the SFO/Nafion/GC modified electrode was calculated using chronoamperometry. The dependence of response currents on the concentration of NO was examined and was linear in the range of 0.05–1.9 mM of NO.     

Flow microcalorimetry in monitoring biological activity of aerobic and anaerobic wastewater-treatment processes

A flow microcalorimetric system which is compatible with the experimental conditions of industrial processes was used to monitor the biological activity of wastewater-treatment systems. Two industrial wastewater-treatment processes were investigated: an activated-sludge (aerobic) treatment of a textile factory effluent and a methane fermentation (anaerobic) treatment of effluents from a cheese factory. In both types of system, the heat flux resulting from metabolic reactions during bacterial degradation of organic substances in the effluent could be measured adequately. Depending on the measurements selected, the calorimetric data could be used to monitor the bacterial activity in the bioprocess, or the effluent degradability or toxicity, or the overall content of degradable substrates in the effluent (loading). The non-invasive measurement of heat flux enabled continuous or semi-continuous on-line monitoring of these biological processes. The response time of the flow calorimetric unit is of the order of minutes, thus yielding process data with minimal delay. These data enable rapid intervention to optimize process parameters (e.g., to control the inlet flow rate or dilution, divert or dilute toxic contaminants, etc.).