Rapid and direct lodine value and saponification number determination of fats and oils by attenuated total reflectance/fourier transform infrared spectroscopy

A simple, rapid and reproducible method of determining the iodine value (IV) and saponification number (SN) for fats and oils was developed with an attenuated total reflectance/Fourier transform infrared spectrometer and commercially available triglycerides as calibration standards. Partial least squares was used to determine the spectral regions correlating with the known chemical IV and SN values, and the calibration set was augmented with additional standards generated by spectral co-adding techniques. The calibration model obtained was used to analyze commercially available fats and oils with a wide range of IV and SN values, and the results were compared to the values obtained by American Oil Chemists’ Society methods. With the spectrometer calibrated and programmed, IV and SN results could be obtained within 2–3 min per sample, a major improvement over conventional wet chemical methods.     

Depolymerization of Turkish lignites. I. Effect of substituted phenols

A lignite (C, 67.4 wt%) was depolymerized with phenol, p-nitrophenol and o-chlorophenol using sulphuric acid as catalyst. The solubility of the lignite was enhanced by these treatments, with phenol being the most reactive reagent whereas p-nitrophenol was the least reactive. The distribution of nitro- and chloro-groups in the solubilized products was investigated by infrared spectrometry and it was found that these groups were redistributed among the pyridine- and methanol-soluble materials. It is suggested that benzene-soluble material is produced by self-depolymerization of coal or by degradation of pyridine- and methanol-soluble material.     

Effect of Zn and Pb as alloying elements on the electrochemical behavior of brass in NaCl solutions

The electrochemical behavior of brasses with various Zn content (5.5–38 mass%) and brass (Cu–38Zn) with different Pb contents (1–3.4 mass%) in 0.6 M NaCl was investigated. The effects of temperature, immersion time, and concentration of chloride ions on the behavior of the different alloys were studied. The pitting corrosion behavior of Cu–Zn alloys and leaded–brass alloys in 0.6 M NaCl solution was also investigated. Open-circuit potential measurements (OCP), polarization techniques and electrochemical impedance spectroscopy (EIS) were used. The results show that the increase in the Zn content increases the corrosion rate of the brass alloys in chloride solutions, while the increase of Pb content in Cu–38Zn–Pb decreases the corrosion rate of the alloy. Long immersion time of the alloys in the aqueous electrolyte improves their stability due to the formation of passive film on the alloy surface. The breakdown potential is shifted to more negative direction with increasing the Zn content, whereas it shifts towards positive values with increasing Pb content. Equivalent circuit model for the electrode/electrolyte interface under different conditions was proposed to illustrate the electrochemical processes taking place at the interface. The electrochemical behavior of the different alloys was discussed in view of the fitting results.     

Effect of Addition of Ni metal catalyst onto the Co and Fe supported catalysts for the formation of carbon nanotubes

Production of novel porous material is a major target in current material science research due to its wide applications. As carbon nanotube (CNTs) is a one dimensional hollow structure it is also one of the promising materials in applications ranging from electronics to hydrogen storage medium. Catalytic chemical vapor deposition (CCVD) is a method whereby CNTs can be produced in large amount. Thus, in this work, we have synthesized CNTs via pyrolysis of acetylene using various supported transition-metal catalysts in a fixed-bed reactor. Scanning electron microscope (SEM) and transmission electron microscope (TEM) were used to investigate the CNTs structure. The structures of nanotubes formed by acetylene pyrolysis were dependent on the catalysts used. It was found that alumina supported Ni/Fe catalyst inhibited the formation of CNTs growth while alumina supported Ni/Co catalyst gave high density of CNTs. However, nanotubes grown over alumina supported Ni/Fe catalyst were less dense due to the deactivation of the catalyst at the early stage of the pyrolysis process.     

Extraction of metals from sulphides using sulphur trioxide in fluidised bed

The kinetics of the reaction of chalcopyrite, iron sulphide, copper sulphide, and nickel sulphide with sulphur trioxide gas were studied using a fluidised bed technique. O₂, N₂, or air was used as a carrier gas for the sulphur trioxide in fluidisation. Binary mixtures of finely ground (0.37–75 μm) samples were reacted with the sulphur trioxide in a Pyrex column at 373–673 K. The reaction products were leached with water and the soluble metals in the solution were determined by atomic absorption spectrometry. The total soluble reaction products were determined gravimetrically. The results obtained showed that a higher yield of soluble salts was obtained when O₂ or air was used as a carrier gas for sulphur trioxide than when an inert gas was used. Higher yields of soluble salts were obtained when the samples were most finely ground. Increase of copper sulphide content in binary mixtures with iron or nickel sulphide led to an increase in the yield of soluble salts. For iron sulphide/nickel sulphide mixtures, the yield of soluble salts increased with the nickel sulphide content. There were maximum values for the soluble metal ratios Ni/Fe and Cu/Ni in the corresponding sulphide binary mixtures and this maximum was at about 50% weight. The soluble Cu/Fe ratio increased with copper sulphide content in mixtures with iron sulphide.     

Catalysis of gasification of coal-derived cokes and chars

Calcium is the most important in-situ catalyst for gasification of US coal chars in O₂, CO₂ and H₂O. It is a poor catalyst for gasification of chars by H₂. Potassium and sodium added to low-rank coals by ion exchange and high-rank coals by impregnation are excellent catalysts for char gasification in O₂, CO₂ and H₂O. Carbon monoxide inhibits catalysis of the CH₂O reaction by calcium, potassium and sodium; H₂ inhibits catalysis by calcium. Thus injection of synthesis gas into the gasifier will inhibit the CH₂O reaction. Iron is not an important catalyst for the gasification of chars in O₂, CO₂ and H₂O, because it is invariably in the oxidized state. Carbon monoxide disproportionates to deposit carbon from a dry synthesis gas mixture (3 vol H₂ + 1 vol CO) over potassium-, sodium- and iron-loaded lignite char and a raw bituminous coal char, high in pyrite, at 1123 K and 0.1 MPa pressure. The carbon is highly reactive, with the injection of 2.7 kPa H₂O to the synthesis gas resulting in net carbon gasification. The effect of traces of sulphur in the gas stream on catalysis of gasification or carbon-forming reactions by calcium, potassium, or sodium is not well understood at present. Traces of sulphur do, however, inhibit catalysis by iron.     

Reactive dye removal in dye/salt mixtures by nanofiltration membranes containing vinylsulphone dyes: effects of feed concentration and cross flow velocity

In this study, DS5 DK type nanofiltration membranes were tested to recycle the reactive dye bath effluents. Reactive black 5 (RB5), reactive orange 16 (RO16), reactive blue 19 (RB19) and NaCl were used in the experiments to prepare the synthetic dye and salt mixtures. Effects of feed concentration, pressure and cross flow velocity on the permeate flux and color removal were investigated. Permeate flux increased with increasing pressure for all NaCl solutions. Dye concentration had a significant effect on flux values. Under the fixed NaCl concentrations the flux decreased with increasing dye concentrations. Dye rejections greater than 99% were achieved. Permeate was almost colorless. A gel layer formed by the rejected dye on membrane surface operates as a resistance to the permeation of dyes due to complete rejection of high molecule weight dyes, especially for the low salt concentrations. The presence of salt concentration has an interesting effect on color removal. Color removal decreased with increasing salt concentration. Cross flow velocities had also a significant effect on flux values. The dye formed agglomerates at high NaCl concentrations. High cross flow velocities decreased this effect.     

Corrosion control of Cu-Ni alloys in neutral chloride solutions by amino acids

The corrosion inhibition of Cu-Ni alloys was investigated in aqueous chloride solutions using amino acids as environmentally safe materials. The corrosion rate was calculated in absence and presence of the corrosion inhibitor using polarization and impedance techniques. The inhibition efficiency of the different amino acids was also calculated.The experimental results have shown that a simple amino acid like glycine can be used as efficient corrosion inhibitor for the Cu-Ni alloys in neutral chloride solutions. An inhibition efficiency of about 85% could be achieved at very low concentrations of the amino acid (0.1 mM). For low Ni content alloy (Cu-5Ni), 2.0 mM cysteine shows a remarkable high (∼96%) corrosion inhibition efficiency. The experimental impedance data were fitted to theoretical data according to a proposed equivalent circuit model for the electrode/electrolyte interface, and the mechanism of the corrosion inhibition process was suggested. Different adsorption isotherms were tested and the corrosion inhibition process was found to depend on the adsorption of the amino acid molecules and/or the deposition of corrosion products on the alloy surface. The adsorption free energy of cysteine on Cu-5Ni (−37.81 kJ mol⁻¹) reveals a strong physical adsorption of the inhibitor on the alloy surface.     

Wear of graphite anodes during electrolysis of add sulphate solutions

Graphite electrodes were prepared by mixing calcined coke and coal tar pitch. They were pressed under 250 kg cm^–2 and heat treated up to 2800° C. Rectangles measuring 70 mm x 40 mm x 8 mm were anodically polarized under galvanostatic and potentiostatic conditions. Electrolyses were conducted at 10–50 mA cm^–2 for periods ranging from 10–120 hours in Na₂SO₄ solutions acidified with sulphuric acid to various pH values. The wear of graphite anodes increased with decreasing bath temperature, increasing acid concentration, decreasing pH of the electrolyte and increasing current density. A model is suggested which assumes that corrosion takes place via the formation of a lamellar crystal compound with the formula (C ₈ ⁰ O)(OH)₃HSO ₄ ^– ·2H₂SO₄.The compound is unstable at higher temperatures when corrosion is effected by oxidation of graphite by atomic oxygen. The formation of the carbon ions was found to be a necessary precondition for the formation of the complex.     

Metal recovery in a pilot-scale rotating cylindrical wiper-blade electrode system

The performance of an experimental pilot-scale electrochemical reactor using a rotating cylindrical electrode equipped with wiper blades is described. Data obtained from monopolar depositing and bipolar stripping—depositing of copper from dilute aqueous electrolytes are presented and certain economic aspects of metal recovery are discussed.