An electroactive co-polymer as corrosion inhibitor for steel in sulphuric acid medium

The corrosion behavior of mild steel in sulphuric acid solution containing various concentrations of a co-polymer formed between maleic anhydride and N-vinyl-2-pyrrolidone (VPMA) was investigated using weight-loss, polarization and electrochemical impedance techniques. The polymer acts as an effective corrosion inhibitor for steel in sulphuric acid medium. The inhibition process is attributed to the formation of an adsorbed film of co-polymer on the metal surface which protects the metal against corrosion. Scanning electron microscopy (SEM) studies of the metal surfaces confirmed the existence of an adsorbed film. The adsorption followed the Langmuir isotherm. The protection efficiency increased with increase in inhibitor concentration and decreased with increase in temperature and acid concentration. The thermodynamic functions of the adsorption and dissolution processes were evaluated.     

1,3-Bis(3-hyroxymethyl-5-methyl-1-pyrazole) propane as corrosion inhibitor for steel in 0.5 M H2SO4 solution

The effect of addition of 1,3-bis(3-hyroxymethyl-5-methyl-1-pyrazole) propane (M = 264 g). HMPP on steel corrosion in 0.5 M sulphuric acid is studied by weight-loss, electrochemical polarisation and electrochemical impedance spectroscopy (EIS) measurements at various temperatures. The results obtained showed that HMPP acts as a good corrosion inhibitor. The inhibition efficiency increases with the bipyrazole compound to attain 88%. It acts as a mixed-type inhibitor. Trends in the increase of charge-transfer resistance and decrease of capacitance values also show the adsorption of the molecule on the metal surface. The bipyrazole adsorbs on the steel surface according to the Langmuir isotherm adsorption model. Effect of temperature indicates that inhibition efficiency decreases with temperature between 25 and 85 °C.     

Amorphous silicon carbide thin films doped with P or B for the photoelectrochemical water splitting devices

Photoelectrochemical water splitting devices require semiconductor photoelectrode material fulfilling a number of primary requirements such as band gap, band edge alignment and corrosion resistance to electrolyte. Amorphous silicon carbide films, undoped and doped (P or B), were deposited on Si substrates by PECVD technology. The concentration of elements in the films was determined by RBS and ERD analytical method. Raman spectroscopy study of the SiC films were performed by using a Raman microscope and chemical compositions were analyzed by FTIR, before and after immersion of samples to aqueous pH 2.0 and pH 1.0 sulphuric acid electrolyte. Electrical properties of SiC films before and after immersion of samples to aqueous pH 2.0 and pH 1.0 sulphuric acid electrolyte were studied by measurement of the I–V characteristics on structure Al/SiC/Si/Al. Differences between Raman spectra, FTIR spectra and I–V characteristics before and after immersion to electrolyte are discussed.     

Influence of poly(aminoquinone) on corrosion inhibition of iron in acid media

The inhibitor performance of chemically synthesized water soluble poly(aminoquinone) (PAQ) on iron corrosion in 0.5 M sulphuric acid was studied in relation to inhibitor concentration using potentiodynamic polarization and electrochemical impedance spectroscopy measurements. On comparing the inhibition performance of PAQ with that of the monomer o-phenylenediamine (OPD), the OPD gave an efficiency of 80% for 1000 ppm while it was 90% for 100 ppm of PAQ. PAQ was found to be a mixed inhibitor. Besides, PAQ was able to improve the passivation tendency of iron in 0.5 M H₂SO₄ markedly.     

Synergistic effect of iodide ions on the corrosion inhibition of steel in 0.5 M H2SO4 by new chalcone derivatives

The effect of addition of 4′,4-dihydroxychalcone (P₁), 4-aminochalcone (P₂) and 4-bromo, 4′-methoxychalcone (P₃) on the corrosion of steel in 0.5 M sulphuric acid has been studied by weight loss measurements, potentiodynamic and EIS measurements. We investigate the synergistic effect of iodide ions on the corrosion inhibition of steel in the presence of chalcone derivatives. The corrosion rates of the steel decrease with the increase of the chalcones concentration, while the inhibition efficiencies increase. The addition of iodide ions enhances the inhibition efficiency considerably. The presence of iodide ions increases the degree of surface coverage. The synergism parameters S_Θ and S_I, calculated from surface coverage and the values of inhibition efficiency, in the case of chalcone derivatives are found to be larger than unity. The enhanced inhibition efficiency in the presence of iodide ions is only due to synergism and there is a definite contribution from the inhibitors molecules. E (%) obtained from the various methods is in good agreement. Polarisation measurements show also that the compounds act as cathodic inhibitors.     

Tween-40 as corrosion inhibitor for cold rolled steel in sulphuric acid: Weight loss study, electrochemical characterization, and AFM

The inhibition action of a non-ionic surfactant of tween-40 on the corrosion of cold rolled steel (CRS) in 0.5-7.0 M sulphuric acid (H₂SO₄) was studied by weight loss and potentiodynamic polarization methods. Atomic force microscope (AFM) provided the surface conditions. The inhibition efficiency increases with the tween-40 concentration, while decreases with the sulphuric acid concentration. The adsorption of inhibitor on the cold rolled steel surface obeys the Langmuir adsorption isotherm equation. Effect of immersion time was studied and discussed. The effect of temperature on the corrosion behavior of cold rolled steel was also studied at four temperatures ranging from 30 to 60 °C, the thermodynamic parameters such as adsorption heat, adsorption free energy and adsorption entropy were calculated. A kinetic study of cold rolled steel in uninhibited and inhibited acid was also discussed. The kinetic parameters such as apparent activation energy, pre-exponential factor, rate constant, and reaction constant were calculated for the reactions of corrosion. The inhibition effect is satisfactorily explained by both thermodynamic and kinetic parameters. Polarization curves show that tween-40 is a cathodic-type inhibitor in sulphuric acid. The results obtained from weight loss and potentiodynamic polarization are in good agreement, and the tween-40 inhibition action could also be evidenced by surface AFM images.     

Optical constants of sulphuric acid in the far infrared

The i.r. absorption spectrum of a 75% sulphuric acid solution is obtained experimentally in the 20–50μm wavelength region. The complex refractive index (n = n_r ? in_i) is determined from these measurements by integration of the Kramers-Kronig dispersion relation. The application of this data to radiative transfer processes in the atmosphere of Venus is briefly discussed.     

Acid-base equilibria of methyl β-carboline-3-carboxylate in aqueous solution

The photophysical properties and the acid-base equilibrium of methyl β-carboline-3-carboxylate in aqueous solution have been investigated. The pK_a values in the ground and the first excited state have been spectrophotometrically determined using Förster cycle for the excited state and acidifying the solutions in the pH range with sulphuric acid and acetic acid. Some differences have been found in the absorption spectra depending on the acid added and have been explained in terms of a complex formation between the methyl β-carboline-3-carboxylate and acetic acid. This β-carboline derivative is the most acidic derivative studied till now both in the ground and excited state. The higher acidity of the pyridinic nitrogen, the extension of the conjugation and the steric hindrance due to the inclusion of the methyl ester group as substituent in position 3 of β-carboline justify the unusual acidity of this compound.     

In situ electrochemical STM study of platinum nanodot arrays on highly oriented pyrolythic graphite prepared by electron beam lithography

Model electrodes consisting of platinum dots with a mean diameter of (30 ± 5) nm and heights of 3–5 nm upon highly oriented pyrolytic graphite (HOPG) were prepared by electron beam lithography and subsequent sputtering. The Pt nanodot arrays were stable during scanning tunnelling microscopy (STM) measurements in air and in sulphuric acid electrolyte, indicating the presence of “anchors”, immobilising the dots on the HOPG surface.Electrochemical STM was used to visualise potential induced Pt, carbon and Pt-influenced carbon corrosion in situ in 0.5 M sulphuric acid under ambient conditions. Potentiostatic hold experiments show that the Pt dots start to disappear at electrode potentials of E > 1.4 V vs. SHE. With increasing time and potential a hole pattern congruent to the original dot pattern appears on the HOPG basal planes. Corrosion and peeling of the HOPG substrate could also be followed in situ.Dissolution of Pt dots appears to be accelerated for potential cycling experiments compared to the potential hold statistics.     

Enhanced corrosion resistance of mild steel in normal sulfuric acid medium by 2,5-bis(n-thienyl)-1,3,4-thiadiazoles: Electrochemical, X-ray photoelectron spectroscopy and theoretical studies

The inhibitive action of some thiadiazole derivatives, namely 2,5-bis(2-thienyl)-1,3,4-thiadiazole (2-TTH) and 2,5-bis(3-thienyl)-1,3,4-thiadiazole (3-TTH) against the corrosion of mild steel in 0.5 M H₂SO₄ solution has been investigated using weight loss measurements, Tafel polarisation and electrochemical impedance spectroscopy (EIS) techniques. The experimental results obtained revealed that these compounds inhibited the steel corrosion in acid solution. The protection efficiency increased with increasing inhibitors concentration and the ability of the molecule to adsorb on the steel surface was dependent on the position of the sulphur atom on the thienyl substituent. Inhibition efficiency values obtained from various methods employed were in reasonable agreement. Potentiodynamic polarisation studies clearly showed that 2-TTH and 3-TTH acted as mixed inhibitors. Adsorption of these inhibitors on steel surface obeyed to Langmuir adsorption isotherm. X-ray photoelectron spectroscopy and the thermodynamic data of adsorption showed that inhibition of steel corrosion in normal sulphuric solution by n-TTH is due to the formation of a chemisorbed film on the steel surface. Molecular modelling was used to gain some insight, about structural and electronic effects in relation to the inhibiting efficiencies.     

ICP－AES方法快速测定工业硫酸中的砷和铁含量

本文所述方法是将工业硫酸定量稀释，直接雾化进入ＩＣＰ激发，测定其中砷和铁的光谱强度和含量。绘制校准曲线用标准溶液，加入与测定样品相同量的分析纯硫酸为基体。该方法快速、简便，合成标准样品分析结果与标称值吻合，进口工业硫酸样品中砷、铁含量测定结果与国外检验结果、国家标准方法检验结果基本吻合。     

Effect of ultrasonically induced cavitation on inhibition behavior of polyethylene glycol on carbon steel corrosion

In this investigation the influence of 24 kHz ultrasound wave upon the corrosion of carbon steel in 3N sulphuric acid at 25 degrees C in the presence of inhibitors was studied. The inhibitors were polyethylene glycols (PEG) in different molecular weights (from 400 up to 10,000 gmol(-1)). The polarization and impedance spectroscopy results show the effectiveness of polyethylene glycols on the cavitation-corrosion inhibition of carbon steel in sulphuric acid. The inhibition efficiency is increased with increasing mean molecular weight of polymer and its concentration. The weight loss method has confirmed these results. The analysis of SEM images indicates that these inhibitors prevent propagation of pits on the eroded specimen. The inhibition effect of PEGs can be attributed to cushioning effect of adsorbed polymers on cavitation phenomenon produced by bubble collapse.     

Magnetic properties of multiwalled carbon nanotubes as a function of acid treatment

We investigate the electronic properties of multiwalled carbon nanotubes both before and after acid treatment with concentrated sulphuric and nitric acids. Magnetic susceptibility measurements were performed using a SQUID magnetometer and show that there is a considerable enhancement in the density of states at the Fermi level. The data shows that the diamagnetic influence from the graphitic nanotubes dominates. We experimentally observe, after acid treatment, that the diamagnetic susceptibility remains unchanged at 5 K but notably decreases at 77 K. We propose the acid treatment has increased the Van Vleck paramagnetic contribution lowering the diamagnetic response from the π-electron orbital magnetisation. The Van Vleck paramagnetic contribution is finite-temperature dependent with a diminishing contribution at higher fields.     

Effect of oil extraction assisted by ultrasound on the physicochemical properties and fatty acid profile of pumpkin seed oil (Cucurbita pepo)

The effects of amplitude and time of ultrasound-assisted extraction on the physicochemical properties and the fatty acid profile of pumpkin seed oil (Cucurbita pepo) were evaluated. Ultrasound time (5–30 min) and the response variables amplitude (25–100%), extraction yield, efficiency, oxidative stability in terms of the free fatty acids (FFA) of the plant design comprising two independent experiments variables, peroxide (PV), p-anisidine (AV), totox value (TV) and the fatty acid profile were evaluated. The results were analyzed by multiple linear regression. The time and amplitude showed significant differences (P < 0.05) for all variables. The highest yield of extraction was achieved at 5 min and amplitude of 62.5% (62%). However, the optimal ultrasound-assisted extraction conditions were as follows: ultrasound time of 26.34 min and amplitude of 89.02%. All extracts showed low FFA (2.75–4.93% oleic acid), PV (1.67–4.68 meq/kg), AV (1.94–3.69) and TV (6.25–12.55) values. The main fatty acids in all the extracts were oleic and linoleic acid. Therefore, ultrasound-assisted oil extraction had increased performance and reduced extraction time without affecting the oil quality.     

Kinetic Carbon Isotope Effects in the Decarbonylation of Lactic Acid of Natural Isotopic Composition and of [1-14C] Lactic Acid

Studies of carbon-13 and carbon-14 kinetic isotope effects (K. I. E.) in the decarbonylation of lactic acid (L. A.) in sulphuric acid and in phosphoric acids media have been summarized and compared with earlier studies of ¹⁴C and ¹³C K. I. E. in the decarbonylation of formic and oxalic acids in concentrated sulphuric acid. Supplementary data concerning the decarbonylation of L. A. in sulphuric acid diluted with water and in pyrophosphoric acid are presented and discussed. The observed temperature dependences of ¹³C and ¹⁴C K. I. E. in concentrated H₂SO₄ and in concentrated phosphoric acids media have been rationalized by invoking a change of the mechanism of decarbonylation of L. A. in concentrated sulphuric and phosphoric acids with temperature. Preliminary calculational results concerning ¹³C and ^1??C K. I. E. in decarbonylation processes are also presented. In H₂SO₄ diluted with water and in H₃PO₄ diluted with water the temperature dependence of ¹³C and ¹⁴C K. I. E. is normal and well reproduced by one frequency approximation. In concentrated sulphuric acid and in concentrated phosphoric acids besides the C—OH bond rupture the rupture of a C—C bond had to be considered also to reproduce the observed ¹³C K. I. E. in selected temperature regions.     

Condensation de l'acide sulfurique dans un conduit d'evacuation des gaz de combustion

A method for computing the condensation of water vapour and sulphuric acid in a removal gas conduct is proposed. It utilizes a theoretical approach to determine the condensate production during the phase change from the numerically computed thermal and dynamic properties of the steam in the conduct. The temperature and velocity distributions are given from a k — ε model in one-phase incompressible flow, taking into account the initial temperature and flow rate in the conduct. The quality of the model is tested on a full-scale experimentation pilot equipped with thermocouples and collectors of liquid condensate. The deposit production is obtained for different conditions of temperature and concentration, and the model proves to be satisfactory in domestic boiler conditions.     

From collisions to clusters: first steps of sulphuric acid nanocluster formation dynamics

The clustering of sulphuric acid with base molecules is one of the main pathways of new-particle formation in the Earth's atmosphere. First step in the clustering process is likely the formation of a (sulphuric acid)₁(base)₁(water)_n cluster. Here, we present results from direct first-principles molecular dynamics collision simulations of (sulphuric acid)₁(water)_{0, 1} + (dimethylamine) → (sulphuric acid)₁(dimethylamine)₁(water)_{0, 1} cluster formation processes. The simulations indicate that the sticking factor in the collisions is unity: the interaction between the molecules is strong enough to overcome the possible initial non-optimal collision orientations. No post-collisional cluster break up is observed. The reasons for the efficient clustering are (i) the proton transfer reaction which takes place in each of the collision simulations and (ii) the subsequent competition over the proton control. As a consequence, the clusters show very dynamic ion pair structure, which differs from both the static structure optimisation calculations and the equilibrium first-principles molecular dynamics simulations. In some of the simulation runs, water mediates the proton transfer by acting as a proton bridge. In general, water is able to notably stabilise the formed clusters by allocating a fraction of the released clustering energy.     

Optimization of ultrasound assisted extraction of antioxidant compounds from marjoram (Origanum majorana L.) using response surface methodology

The present study optimized the ultrasound assisted extraction (UAE) conditions to maximize the antioxidant activity [Ferric ion Reducing Antioxidant Power (FRAP)], total phenol content (TP) and content of individual polyphenols of extracts from marjoram. Optimal conditions with regard to amplitude of sonication (24.4-61.0 μm) and extraction temperature (15-35 °C) and extraction time (5-15 min) were identified using response surface methodology (RSM). The results showed that the combined treatment conditions of 61 μm, 35 °C and 15 min were optimal for maximizing TP, FRAP, rosmarinic acid, luteolin-7-O-glucoside, apigenin-7-O-glucoside, caffeic acid, carnosic acid and carnosol values of the extracts. The predicted values from the developed quadratic polynomial equation were in close agreement with the actual experimental values with low average mean deviations (E%) ranging from 0.45% to 1.55%. The extraction yields of the optimal UAE were significantly (p < 0.05) higher than solid/liquid extracts. Predicted models were highly significant (p < 0.05) for all the parameters studied with high regression coefficients (R²) ranging from 0.58 to 0.989.     

Electrochemical performance of lead acid battery using ammonium hydrogen sulphate with different alkyl groups

In this work, the application of ionic liquids (ILs)??mono-, bicycyclohexyl, monohexyl and tetrahexyl ammonium hydrogen sulphate??as electrolyte additives on the electrochemical performance of lead acid batteries is proposed. The electrochemical behaviour of Pb?C1.66% Sb?C0.24% Sn alloy in sulphuric acid solution is investigated in the presence of the mentioned ILs with different numbers of alkyl or cycloalkyl chains. Particularly, the hydrogen and oxygen evolution potential and anodic layer characteristics were studied using cyclic and linear sweep voltammetric methods. The obtained results indicate that hydrogen evolution overpotential of Pb/Sb/Sn alloy in the presence of ILs increases. This overpotential mainly depends on the concentration of ILs and the number of alkyl and cycloalkyl chains on the cations. Also, the difference between the oxygen oxidation potential in anodic and cathodic scans (?E) decreases using different ILs.     

Effect of ultrasound on the dissolution of copper from copper converter slag by acid leaching

This work presents the optimum conditions of dissolution of copper in copper converter slag in sulphuric acid ferric sulphate mixtures in the presence and absence of ultrasound. The Taguchi method was used to determine the optimum conditions. The parameters investigated were the reaction temperature, acid concentration, ferric sulphate concentration and reaction time. The optimum conditions for the maximum dissolution of copper were determined as follows: reaction temperature, 65 °C; acid concentration, 0.2 M; ferric sulphate concentration, 0.15 M; reaction time 180 min. Under these conditions, extraction efficiency of copper, zinc, cobalt, and iron from slag were 89.28%, 51.32%, 69.87%, and 13.73%, respectively, in the presence of ultrasound, while they are 80.41%, 48.28%, 64.52%, and 12.16%, respectively, in the absence of ultrasound. As seen from the above results, it is clear that ultrasound enhances on the dissolution of Cu, Zn, Co and Fe in the slag.