Sonochemical synthesis of Ce-TiO2 nanocatalyst and subsequent application for treatment of real textile industry effluent

Treatment of real textile industry effluent using photocatalysis, sonocatalysis, sonophotocatalysis and H₂O₂ assisted sonophotocatalysis have been studied based on the use of Ce-TiO₂ nanocatalyst synthesized using sonochemical co-precipitation method. Characterization studies of the obtained catalyst revealed crystallite size as 1.44 nm with particles having spherical morphology. A shift of the absorption edge to the visible light range was also observed in UV–Vis diffuse reflectance spectra (UV-DRS) analysis. The effects of different operational parameters viz catalyst dose (0.5 g/L-2 g/L), temperature (30 °C-55 °C) and pH (3–12) on the COD reduction were studied. The reduction in the COD was higher at lower pH and the optimum temperature established was 45 °C. It was also elucidated that the required catalyst dose was lesser in combined sonophotocatalysis when compared with individual photocatalysis and sonocatalysis. Combination of processes and addition of oxidants increased the COD reduction with the sonophotocatalytic oxidation combined with H₂O₂ treatment showing the best results for COD reduction (84.75%). The highest reduction in COD for photocatalysis was only 45.09% and for sonocatalysis, it was marginally higher at 58.62%. The highest reduction in COD achieved by sonophotocatalysis was 64.41%. Toxicity tests coupled with Liquid Chromatography Mass Spectrometry (LC-MS) analysis revealed that there were no additional toxic intermediates added to the system during the treatment. Kinetic study allowed establishing that generalized kinetic model fits the experimental results well. Overall, the combined advanced oxidation processes showed better results than the individual processes with higher COD reduction and lower requirement of the catalyst.     

Electrochemical studies of zinc-nickel codeposition in sulphate bath

The electrodeposition of Zn-Ni alloys from a sulphate bath was studied under different conditions. The bath had the composition 0.40 M sodium sulphate, 0.01 M sulphuric acid, 0.16 M boric acid, 0.20 M zinc sulphate and 0.20 M nickel sulphate. It is found that the plating bath temperature has a great effect on the cyclic voltammograms, galvanostatic measurements during electrodeposition, and consequently linear polarization resistance for corrosion study and the alloy composition. Under the examined conditions, the electrodeposition of the alloys was of anomalous type. X-ray diffraction measurements revealed that the alloys consisted of the δ-phase (Ni₃Zn₂₂) or a mixture of the two phases δ and γ (Ni₅Zn₂₁). The comparison between Ni deposition and Zn-Ni codeposition revealed that the remarkable inhibition of Ni deposition takes place due to the presence of Zn²⁺ in the plating bath. The Ni deposition starts at −0.85 V in the bath of Ni deposition only, but the deposition starts at more negative potentials in the codeposition bath although the concentration of Ni²⁺ is the same in the both baths.     

Facile synthesis of ZnO/CuO/Eu heterostructure photocatalyst for the degradation of industrial effluent

Zinc oxide-based ternary heterostructure ZnO/CuO/Eu(1%, 3%, and 5% of Eu) nanoparticles were effectively produced by employing Vigna unguiculata (cowpea)waste skin extract as fuel in a simple one-pot combustion process. The as-synthesized heterostructure was analyzed by X-ray diffraction studies, ultraviolet-visible spectroscopy, Fourier Transform Infrared Spectroscopy, Field Emission Scanning Electron Microscopy, and High-Resolution Transmission Electron Microscopy techniques. Besides, the photocatalytic degradation efficiency of the as-obtained ternary nanocomposite was evaluated under UV light for the degradation of model organic pollutants including methylene blue (MB), Rhodamine-B (RB), and an effluent sample collected from the textile industrial waste. During this study, the effect of a variety of parameters on the photodegradation activity of the photocatalysts has been thoroughly evaluated, such as light source, catalyst dose, irradiation period, dye concentration, solution pH, etc. Under UV irradiation(100 mins), the ternary ZnO/CuO/Eu photocatalyst demonstrated excellent degradation activity of ～99 and ～93% for MB and RB, respectively, while for the industrial effluent, a decent degradation activity of 42% has been recorded. Further experiments have revealed a pH and concentration-dependent photocatalytic behavior of the heterostructure photocatalyst. Therefore, the results suggest that the heterostructure photocatalyst can be potentially applied for wastewater treatment and other environmental applications.     

Hydrated Eutectic Electrolytes Stabilizing Quasi-Underpotential Mg Plating/Stripping for High-Voltage Mg Batteries

Aqueous rechargeable Mg batteries (ARMBs) usually fail from severe anode passivation, alternatively, executing quasi-underpotential Mg plating/stripping chemistry (UPMC) on a proper heterogeneous metal substrate is a crucial remedy. Herein, a stable UPMC on Zn substrate is initially achieved in new hydrated eutectic electrolytes (HEEs), delivering an ultralow UPMC overpotential and high energy/voltage plateau of ARMBs. The unique eutectic property remarkably expands the lower limit of electrochemical stability window (ESW) of HEEs and undermines the competition between hydrogen evolution/corrosion reactions and UPMC, enabling a reversible UPMC. The UPMC is carefully revealed by multiple characterizations, which shows a low overpotential of 50 mV at 0.1 mA cm⁻² over 550 h. With sulfonic acid-doped polyaniline (SPANI) cathodes, UPMC-based full cells show high energy/power densities of 168.6 Wh kg⁻¹/2.1 kWh kg⁻¹ and voltage plateau of 1.3 V, far overwhelming conventional aqueous systems.     

Study on Determination of Trace Copper by Spectrophotometry after Flotation Separation Using Microcrystalline Adsorption System

The paper presents a novel method for the flotation separation of Cu²⁺ using microcrystalline adsorption system prior to the determination by spectrophotometry. The effects of different parameters, such as the dosages of NH₄SCN and octadecyl trimethyl ammonium bromide (OTMAB), various salts on the flotation yield of Cu2+ have been investigated to select the optimum experimental conditions. The possible flotation separation mechanism of Cu²⁺ was discussed. The results showed that under the optimum conditions, octadecyl trimethyl ammonium bromide cation (OTMAB⁺) reacted with SCN^‐ to produce the microcrystalline matter (Ms‐M) of (OTMAB⁺·SCN^‐), the water‐insoluble ternary association complex of [Cu(SCN)₄] (OTMAB)₂ which produced by Cu²⁺ and SCN^‐, OTMAB⁺ was quantificationally adsorbed on the surface of Ms‐M of (OTMAB²⁺·SCN^‐) and was floated above water phase, the liquid‐solid phases were formed with clear interface. In this condition, K⁺, Na⁺, Ca²⁺, Mg²⁺, Al³⁺, Fe²⁺, Mn²⁺, Ni²⁺, Cd²⁺ and Co²⁺ could not be floated. Therefore, Cu²⁺ was separated completely from the above metal ions. A new method of determination of trace copper by flotation separation was established. The proposed method has been successfully applied to the determination of Cu²⁺ in plating waster water, and the results agreed well with AAS method. The recoveries were 93.3%～107.8%, and the RSD was 1.9%～2.1%.     

工业镀层及涂层厚度分析—同位素X射线荧光光谱法

采用自行研制的同位素Ｘ射线荧光分析仪，测定工业镀层和汽车涂层厚度，分析精度（ＲＳＤ）分别达２０％和３６％，该法具有快速、简便、无损等优点。     

An enzymatic approach to the cleaning of ultrafiltration membranes fouled in abattoir effluent

Membrane fouling severely curtails the economical and practical implementation for the purification of biologically related process streams such as abattoir effluent (Jacobs, WRC Report no. K5/362, 1991, Pretoria, South Africa [1]). Mechanical and chemical removal of foulants usually lead to membrane damage and additional pollution. Enzymes, specific for the degradation of proteins and lipids, were tested as key components of biological cleaning regimes for membranes fouled in abattoir effluent. Fouling of polysulphone membranes was assessed as previously described by Maartens et al. (J. Membrane Sci., 119 (1996) 1 [2]) and optimal enzyme concentrations and incubation times were determined for the different preparations. The ability of each cleaning agent to remove adsorbed protein and lipid material, as well as their ability to restore the water-contact angle and the pure-water flux of the fouled membranes, were determined and compared. These variables were also used to compare the cleaning efficiency of enzymatic cleaning agents with conventional chemical agents under optimal conditions. The enzymes and enzyme detergent mixtures were effective cleaning agents and the pure-water flux of statically fouled membranes could be restored by treatment with these agents.     

Charcoal open tubular traps for the analysis of air and headspace samples

5 cm × 0.3 mm i.d. glass capillary tubes coated with fine charcoal particles are used for the analysis of organic compounds, particularly tri- and tetrachloroethylene, benzene, and toluene, in air and headspace samples. Due to their small size, these traps are easy to use with capillary GC. As, e.g. 20 ml of gas can be sucked through this trap in 20 s, it is a simple technique providing high sensitivity; compared to headspace with split injection, sensitivity is increased by a factor exceeding 100. The column effluent is split into FID and ECD in such a way that small as well as large amounts of the chlorinated compounds can be detected.     

Headspace SPME followed by GC/PFPD for the analysis of malodorous sulfur compounds in liquid industrial effluents

Headspace SPME was used to analyse malodorous sulfur compounds in liquid industrial effluents. A pulsed flame photometric detector (PFPD) was selected for a specific and sensitive analysis. Two fibres, PDMS/Dvb and PDMS/Carboxen, which are particularly convenient for extracting small and volatile molecules were tested. To compare these fibres, both sensitivity and artefact formation were considered. The PDMS/Carboxen fibre showed the lower limits of detection and moreover the least artefact formation yields. It was therefore selected and headspace SPME extraction conditions were optimised. Limits of detection of the target compounds evaluated were 12–31 ng L^–1 and repeatability was around 7%. Due to the adsorption mechanism involved, extraction is strongly influenced by the sample matrix and the low affinity compounds can suffer displacement effects. To investigate the occurrence of this phenomenon, two sampling times corresponding to non-equilibrium (5 min) and equilibrium conditions (60 min) were investigated. An external calibration was carried out by using standard solutions for both sampling times. The developed procedure was then compared to the standard addition method on a real industrial effluent. The results obtained from the two methods and for the two extraction times were in good agreement, demonstrating that even a long sampling time can be used. Therefore, the simple and timesaving external calibration was defined as relevant for an accurate quantification of sulfur compounds by headspace SPME.     

On-line monitoring of nitrite in fertilizer process streams, natural and waste water effluents with sequential injection analysis

A sequential injection system for the online monitoring of nitrite in fertilizer process streams, natural and waste water effluents is proposed. Nitrite is diazotised in the SIA system with N-(1-naphthyl) ethylenediammonium dichloride to form a highly coloured azo dye which is measured at 525 nm. The proposed system is fully computerised and is able to monitor nitrite at a frequency of 49 samples per hour with a relative standard deviation of < 2.7%. The calibration curve is linear up to 5 mg/l. The detection limit is 0.053 mg/l.