Preparation and physicochemical and electrochemical characterization of exfoliated graphite oxide

Exfoliated graphite oxide (EGO) is prepared by oxidizing exfoliated graphite (EG) using a mixture of KMnO(4)/H(2)SO(4). The physicochemical characterization of the EGO has been carried out using FT-Raman, FT-IR, XPS, NMR, and diffraction techniques. Colloidal form of EGO is subsequently prepared by ultrasonicating EGO in water. Thin films of EGO on a glassy carbon/gold surface are formed and the electrochemical and ion exchange properties have been studied using various redox systems such as K(4)[Fe(CN)(6)], ascorbic acid, and dopamine. The charge-based adsorption properties can be made use of, to either suppress or catalyze ascorbic acid oxidation. Adsorption and preconcentration of dopamine on the EGO film has been shown to electrocatalyze the oxidation of NADH.     

Assessment of inhibitory behavior of ethyl 5-cyano-4-(furan-2-yl)-2-methyl-6-oxo-1,4,5,6-tetrahydropyridine-3-carboxylate as a corrosion inhibitor for carbon steel in molar HCl: Theoretical approaches and experimental investigation

The new ethyl 5-cyano-4-(furan-2-yl)-2-methyl-6-oxo-1,4,5,6-tetrahydropyridine-3-carboxylate (THP) has been studied to prevent the electrochemical decomposition of carbon steel in an acidic medium used in the production process using electrochemical techniques (potentiodynamic polarization and electrochemical impedance spectroscopy), weight reduction methods and surface morphological. Computational correlations (DFT and molecular dynamics simulations) were carried out to have more information on the mechanism of inhibition. Experimentally obtained results revealed that the inhibition efficiency increases with the concentration, and the highest effectiveness is reached for 10^?3M, with 95.22%, and the compound is classified as a mixed inhibitor. Indeed, the increase in temperature caused an increase in the values of i_corr throughout the studied temperature range. Moreover, the obtained results showed that the adsorption on carbon steel is accomplished according to the Langmuir adsorption model and the adsorption parameters reflect that the THP is spontaneously adsorbed by physical adsorption, which increases the barrier energy required for the corrosion reaction. The theoretical approaches used show that THP suggests a perfect adsorption by all its chemical structure.     

活性炭纤维吸附脱除NO过程中NO氧化路径分析

在小型固定床吸附实验台上开展了黏胶基活性炭纤维吸附脱除NO的实验研究。采用H₂O₂溶液浸渍以及热处理方法对活性炭纤维表面进行修饰,以获得表面孔隙结构接近而含氧官能团含量不同的样品;考察样品在惰性氮气气氛、含氧气氛下吸附脱除NO的效果,以及表面含氧含氮官能团的变化规律。探讨了含氧官能团在NO催化氧化过程中的作用及含氧气氛下O₂对于NO转化为NO₂的影响,分析了活性炭纤维表面吸附的NO向NO₂的主要转化途径。结果表明,在氮气气氛下活性炭纤维表面C-O官能团对吸附态的NO起到氧化作用,吸附态NO被C-O官能团氧化生成-NO₂官能团;在含氧气氛下活性炭纤维吸附NO后表面出现-NO₂、-NO₃官能团,通过长时间实验测定三种样品在含氧气氛下对NO吸附的效果,发现三种样品稳定时催化氧化效果一致,表明含氧官能团对初始NO的物理吸附影响较大,而对整个吸附过程影响较小。吸附在活性炭纤维表面上的NO与环境气氛中的游离态O₂发生氧化反应是NO转变为NO₂的主要途径。     

Pore structure and surface properties of chemically modified activated carbons for adsorption mechanism and rate of Cr(VI)

Effects of hydrochloric acid and sodium hydroxide treatments of activated carbons (ACs) on chromium(VI) reduction were studied. The surface properties were determined by pH, acid-base values, FT-IR, and X-ray photoelectron spectrometer (XPS). And the porous structure of the activated carbons was characterized by adsorption of N(2)/77 K. The Cr(VI) adsorption experiments were carried out to analyze the influence of porous texture and surface properties changed by the chemical surface treatments of ACs on adsorption rate with carbon-solution contact time. From the experimental results, it was observed that the extent of adsorption and reduction processes depends on both microporous structure and functional groups. And the adsorption of Cr(VI) ion was more effective in the case of acidic treatment on activated carbons, resulting from the increases of acid value (or acidic functional group) of activated carbon surfaces. However, basic treatment on activated carbons was not significantly effective on the adsorption of Cr(VI) ion, probably due to the effects of the decrease of specific surface area and basic Cr(VI) in nature.     

Adsorption and inhibition properties of Tephrosia Purpurea as corrosion inhibitor for mild steel in sulphuric acid solution

Abstract

The present study investigated the adsorption and inhibition behavior of leaf extract of Tephrosia Purpurea (T. purpurea) on mild steel corrosion in 1?N H₂SO₄ solution using electrochemical and surface morphological methods. Techniques adopted for electrochemical studies were Potentiodynamic Polarization and Electrochemical Impedance Spectroscopy (EIS) technique; and surface morphological studies were carried out using Scanning Electron Microscopy (SEM), and Atomic Force Microscopy (AFM). The leaf extract of T. purpurea was characterized using UV-Visible spectroscopy (UV-Vis), Fourier-Transform Infrared Spectroscopy (FT-IR), Nuclear Magnetic Resonance Spectroscopy (NMR) and Gas Chromatography – Mass Spectrometry (GCMS). The results obtained from electrochemical studies exhibited the potential of T. purpurea as good corrosion inhibitor. And, it was found that, the inhibition efficiency (I.E in %) increases with increase in concentration of the inhibitor molecules, the optimum inhibitor concentration observed was 300?ppm and the inhibition efficiency of 93% was observed at this inhibitor concentration. Above 300?ppm, there was not much changes in inhibition efficiency. Polarization studies provided the information that the inhibition is of mixed type and EIS confirmed that the corrosion process is controlled by single charge transfer mechanism. And, it was obtained that, the adsorption of inhibitor molecules obeys Langmuir adsorption isotherm. The inhibition is mainly by the adsorption of inhibitor molecules on the mild steel electrode surface, which was confirmed by FT-IR, SEM and AFM studies. Through all the experimental results, it can be arrived that, the leaf extract of T. purpurea performed as a good corrosion inhibitor for mild steel in 1?N sulfuric acid medium.     

Influence of Gas Atmosphere on Removal of Sulphate Groups From Titanium Oxide

The studies were devoted to determination of the effect of gas atmosphere and its pressure on the second step of decomposition of hydrated titanium dioxide (HTD) promoted by sulfate groups. It has been found that thermal decomposition of HTD at temperatures above 300°C consists of a number of processes such as dehydroxylation, desulfuration, recrystallization and sintering of solid grains, photochemical processes (if the decomposition proceeds in the presence of light) and adsorption of gas phase components (in the presence of air or SO₂). Kinetic parameters characterizing this step of decomposition have been determined for processes carried out in vacuum and in argon or air atmospheres (at a pressure of 13.33hPa). The kinetic curves of decomposition carried out in the presence of gases capable of being adsorbed on the surface of partly dehydrated HTD are featured by local extrema due to simultaneous processes of decomposition and adsorption of gas components. This revised version was published online in August 2006 with corrections to the Cover Date.     

Electrochemical Behavior and Ultrasensitive,Simple and Effective Voltammetric Determination of Acetaminophen Using Modified Glassy Carbon Electrode Based on 4-Hydroxyquinoline-3-carboxylic Acid

An electrochemical oxidation of acetaminophen (ACOP) has been successfully performed by using glassy carbon electrode covered with 4-hydroxyquinoline-3-carboxylic acid (4HQ3CA) to reinforce electrode's feature. To characterize the modified electrode (4HQ3CA/GC), electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and Fourier transform infrared spectroscopy (FT-IR) techniques were used. The finding optimum conditions (supporting electrolyte, pH) and the electrochemical determination studies were performed with differential pulse voltammetry (DPV). It was decided that the supporting electrolyte medium suitable for ACOP determination was Britton-Robinson (BR) buffer and the effect of pH change on the oxidation peak of ACOP in this media was investigated. The effect of changing scan rate on the oxidation peak of ACOP was examined and this study showed that the oxidation process of ACOP on the 4HQ3CA/GC modified electrode surface was diffusion and adsorption controlled process. A wide concentration range from 0.0025 μM to 141 μM with a limit of detection (LOD) of 5.98×10⁻¹⁰ M (3 s/m) was obtained. This prepared sensor was carried out for the determination of ACOP in pharmaceutical sample.     

Characterization of Microporous Activated Carbon Electrodes for Electric Double-layer Capacitors

IntroductionElectric double layer capacitors( EDLCs) witha high power density can be used as memory back-up devices or electric vehicles.EDLCs store energyin the electric double layer by charge accumulationon the interface between the electrode and the elec-trolyte. In order to obtain reasonable energies andpower densities,the more suitable material forEDLCs musthave a high surface area with a signif-icant value of specific double layer capacitance,better pore size distribution and electro…     

Effect of surface activation on charge and mass transfer rates of the hexacyanoferrate(III)/(II) redox probe at fibrinogen-modified carbon paste electrodes

The electron transfer and mass transport properties of fibrinogen-modified carbon paste surfaces, following preliminary activation for various duration, has been studied using cyclic voltammetry (CV) and chronoamperomety. Activation was carried out by subjecting the surface, exposed to a solution-containing oxidant species, to positive polarization of increasing duration. Modification was subsequently achieved following spontaneous adsorption of fibrinogen on exposure to a solution containing the protein. To investigate the electrochemical properties of this surface, the variations in the charge-transfer and mass-transport kinetics of hexacyanoferrate(III)/(II) ions, used as a redox probe, were analyzed separately. The results showed the favorable effect of activation on electrocatalysis and charge-transport properties through the coating. Relative to pretreated bare surfaces, however, the presence of fibrinogen induced opposed variations, thus explaining unchanged CV peak currents. These features were essentially attributed to morphological changes promoted by activation in the protein layer.     

Preparation and characterization of pyrolytic chars from different biomass samples

In the present work four different biomass samples (pine cone, soybean cake, corn stalk and peanut shell) were pyrolyzed to 550 °C in an inert gas atmosphere and a comparison between the properties of chars produced has been performed. Characterization of biomass samples was carried out with FT-IR, ¹³C NMR, SEM and EDX. The influence of the parent material on char quality was investigated. The chars were characterized by their proximate and ultimate analysis and surface areas by N₂ adsorption at 77 K using BET equation. The morphological changes in carbonaceous solids were observed by scanning electron microscopy (SEM), and FT-IR spectra were obtained to evaluate the functional groups. The results obtained from the different techniques were combined to give an overview of the chemical and physical properties of the biomass char samples.     

The influence of thermal treatment on the electrochemical properties of carbon–Ni–Pd composites

Resorcinol–formaldehyde (RF) hydrogel and RF–nickel–palladium (RF–Ni–Pd) hydrogel were synthesized by sol–gel polycondensation followed by ambient drying. Carbon gel and carbon–nickel–palladium doped gels were prepared by carbonizing the RF and RF–Ni–Pd gels at 900 °C under a nitrogen atmosphere. The goal of this study was to determine the effect of oxidative thermal treatment on the electrochemical activity of nickel–palladium doped carbon gels (C–Ni–Pd). The scanning electron microscopy analysis, adsorption and X-ray diffraction measurements showed that the admixture of Ni and Pd to carbon matrix resulted in the modification of morphological, porous and crystalline features. It has been demonstrated that composite C–Ni–Pd composed of sphere-like granules incrusted with well-crystalline nickel and palladium particles exhibits electrochemical activity in 6 M KOH aqueous solution. Thermal treatment of the composite carried out in air at 450 °C brought about the improvement of electrochemical activity in the potential range of the hydrogen sorption/desorption reaction.     

An influence of pretreatment conditions on surface structure and reactivity of Pt(100) towards CO oxidation reaction

We present a combined electrochemical and in situ STM study of the surface structure of Pt(100) single crystal electrodes in dependence on the cooling atmosphere after flame annealing. The following cooling conditions were applied: Ar/H₂ and Ar/CO mixtures (reductive atmosphere), argon (inert gas) and air (oxidative atmosphere). Surface characterization by in-situ STM allows deriving direct correlations between surface structure and macroscopic electrochemical behavior of the respective platinum electrodes. We investigated the influence of defect type and density as well as long range surface order on the kinetics of the CO electro-oxidation reaction. The defect-rich Pt(100) electrodes as cooled in air or Ar, and followed by immersion in the hydrogen adsorption region display higher activities as compared to the rather smooth Pt(100)-(1 × 1) electrode cooled in an Ar/H₂-atmosphere.     

Effect of reduction treatment on copper modified activated carbons on NO(x) adsorption at room temperature

Activated carbon was impregnated with copper salt and then exposed to reductive environment using hydrazine hydrate or heat treatment under nitrogen at 925 °C. On the obtained samples, adsorption of NO(2) was carried out at dynamic conditions at ambient temperature. The adsorbents before and after exposure to nitrogen dioxide were characterized by X-ray diffraction (XRD), thermal analysis, scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), N(2)-sorption at -196 °C, and potentiometric titration. Copper loading improved the adsorption capacity of NO(2) as well as the retention of NO formed in the process of NO(2) reduction on the carbon surface. That improvement is linked to the presence of copper metal and its high dispersion on the surface. Even though both reduction methods lead to the reduction of copper, different reactions with the carbon surface take place. Heat treatment results in a significant percentage of metallic copper and a reduction of oxygen functional groups of the carbon matrix, whereas hydrazine, besides reduction of copper, leads to an incorporation of nitrogen. The results suggest that NO(2) mainly is converted to copper nitrates although the possibility to its reduction to N(2) is not ruled out. A high capacity on hydrazine treated samples is linked to the high dispersion of metallic copper on the surface of this carbon.     

The Utilisation of Thermal Analysis to Optimise Radiocarbon Dating Procedures

Thermal analysis combined with mass spectrometry was applied to radiocarbon dating procedures (age determination of carbon-containing samples). Experiments carried out under an oxygen atmosphere were used to determine carbon content and combustion range of soil and wood samples. Composition of the shell sample and its decomposition were investigated. The quantification of CO₂ formed by the oxidation of carbon was done by the application of pulse thermal analysis. Experiments carried out under an inert atmosphere determined the combustion range of coal with CuO as an oxygen source. To eliminate a possible source of contamination in the radiocarbon dating procedures the adsorption of CO₂ by CuO was investigated. This revised version was published online in August 2006 with corrections to the Cover Date.     

The Effect of Electrochemical and Gas Phase Activation of High Surface Area Carbon Black Ketjen Black EC 600 DJ on Its Surface Composition,Electrochemical Capacitance,and Stability

The effect of electrochemical and gas-phase activation of high-surface-area carbon black Ketjen Black EC 600 DJ on its stability and electrochemical capacitance is studied. The electrochemical activation is carried out according to the “start–stop” protocol (1–1.5 V, 0.5 V/s). The stability of samples is assessed based on variation of their effective resistance (based on the results of cyclic voltammetry (CVA)) and electrochemical capacitance (based on CVA and galvanostatic data) with the cycle number. The changes in the texture and surface properties of activated samples are studied by the methods of nitrogen low-temperature adsorption and X-ray photoelectron spectroscopy. The gas-phase activation of high-surface-area carbon black Ketjen Black EС 600 DJ is shown to impair its stability, while the electrochemical oxidation of carbonblack samples leads to a considerable (two-fold) increase in their electrochemical capacitance.     

Green approach to corrosion inhibition of mild steel in hydrochloric acid medium using extract of spirogyra algae

In the present investigation, a fresh water green algae spirogyra is used as an inexpensive and efficient mild steel corrosion inhibitor. The study is carried out in 0.5?M HCl solution using weight loss measurements, scanning electron microscopy–energy-dispersive X-ray spectroscopy, X-ray diffraction, and Fourier transforms infrared (FT-IR) techniques. The maximum inhibition efficiency was found to be 93.03% at 2?g?L^?1. The adsorption of extract of spirogyra on mild steel surface obeys the Langmuir adsorption isotherm. Corrosion inhibition mechanisms were inferred from the temperature dependence of the inhibition efficiency as well as from calculation of thermodynamic and kinetic parameters which direct the process. FT-IR analysis of green algae spirogyra revealed the presence of hydroxyl, amino, and carbonyl groups, which are responsible for the adsorption on the mild steel surface. SEM analysis supported the inhibitive action of the spirogyra extract against the mild steel corrosion in acid solution.     

Functionalization of glassy carbon with diazonium salts in ionic liquids

The paper reports on the chemical functionalization of glassy carbon electrodes with 4-bromobenzene (4-BBDT) and 4-(4'-nitrophenylazo)benzene diazonium tetrafluoroborate (4-NAB) salts in ionic liquids. The reaction was carried out at room temperature in air without any external electrical bias in either hydrophobic (1-butyl-3-methylimidazolium hexafluorophosphate) or hydrophilic (1-butyl-3-methylimidazolium methyl sulfate) ionic liquids. The resulting surfaces were characterized using X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and electrochemical measurements. Electrochemical reduction of the terminal nitro groups allowed the determination of surface coverage and formation of an amine-terminated carbon surfaces. The results were compared to glassy carbon chemically modified in an aqueous solution in the presence of 1% sodium dodecyl sulfate (SDS) with the same diazonium salt. Furthermore, Raman spectroscopy coupled with electrochemical measurements allowed to distinguish between the reduction of -NO2 to -NH2 group and the -N=N- to -NH-NH- bond.     

Adsorption and release behavior of bare and DNA-wrapped-carbon nanotubes on self-assembled monolayer surface

The adsorption and release behavior of single-stranded DNA-wrapped single-walled carbon nanotubes (ssDNA-w-SWCNTs) on alkylthiol self-assembled monolayer (SAM) surface was systematically characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Fast electron transfer between bare Au electrode and redox species blocked by the alkylthiol SAM can be restored by SWCNTs or ssDNA-w-SWCNTs. The release of ssDNA-w-SWCNTs is carried out by positive or negative desorption potential. SWCNTs/SAM or ssDNA-w-SWCNTs/SAM is completely removed from Au surface at +0.90 V or -1.40 V (vs. 3.0 M KCl|Ag|AgCl). The controlled release of SWCNTs/SAM and ssDNA-w-SWCNTs/SAM holds great promise for gene delivering.     

An investigation of carbon steel corrosion inhibition in hydrochloric acid medium by an environmentally friendly green inhibitor

The inhibition effect of polyphenols extracted from olive mill wastewater (PP) on carbon steel in 1.0 M HCl solution was studied. Inhibition efficiency of PP was carried out by using chemical (weight loss method) and electrochemical techniques [potentiodynamic polarization and electrochemical impedance spectroscopy (EIS)]. The effect of temperature and immersion time on the corrosion behavior of carbon steel in 1.0 M HCl with addition of an extract was also studied. The results show that PP acts as a very good inhibitor, and the inhibition efficiency increases with the concentration of PP and decreases with rising temperature. Polarization curves show that PP behaves as a mixed-type inhibitor in hydrochloric acid. Data, obtained from EIS measurements, were analyzed to model the corrosion inhibition process through an appropriate equivalent circuit model; a constant phase element has been used. EIS shows that charge-transfer resistance increases and the capacitance of double layer decreases with the inhibitor concentration, confirming the adsorption process mechanism. The activation energy as well as other thermodynamic parameters for the inhibition process were calculated. The adsorption of PP obeys the Langmuir adsorption isotherm.     

Electrochemical studies of guanosine in DMF and detection of its radical cation in a scanning electrochemical microscopy nanogap experiment

This communication reports the findings of the investigation of the electrochemical (EC) oxidation of the important bimolecular guanosine (Gs) by scanning electrochemical microscopy (SECM) using carbon fiber ultramicroelectrodes (CF-UMEs) as the probe and substrate. The first attempt is to try to gain a steady-state voltammogram for EC oxidation of Gs at the CF-UME probe in aqueous buffer solutions with three different pH values. Experimental results indicate that due to serious adsorption of Gs on the CF-UME surface, an "S-shaped" steady-state voltammetric curve, which is required for SECM studies, cannot be obtained in aqueous solutions. To solve this adsorption problem, a series of experiments for studying the EC behavior of Gs in DMF are carried out. A well-defined "S-shaped" steady-state cyclic voltammogram (CV) could be achieved at the CF-UME in DMF containing 0.1M TBAPF6 as the supporting electrolyte. By combining several EC techniques, including cyclic voltammetry at glassy carbon (GC) macroelectrode and CF-UMEs, and chronoamperometry, the general chemical characteristics and EC behavior of Gs in DMF solution are studied. Furthermore, SECM detection of Gs*+, the radical cation of Gs electrogenerated in its first oxidation, is carried out by using feedback and tip generation/substrate collection modes in a nanogap configuration. Gs*+ has been electrochemically detected for the first time, with an estimated lifetime of 相似文献