Electrochemical detection of selenium using glassy carbon electrode modified with reduced graphene oxide

In this work, a simple experimental procedure was reported for the electroanalytical determination of selenium (IV) using reduced graphene oxide (rGO) to modify glassy carbon electrode (GCE). The rGO was obtained by reduction of graphene oxide obtained via Hummer’s method. The synthesised rGO was characterised using X-ray diffraction, Raman spectroscopy, scanning electron microscope (SEM), energy-dispersive spectroscopy and transmission Electron microscopy (TEM). GCE was modified with rGO and the electrochemical properties of the bare and modified electrode were investigated using cyclic voltammetry and electrochemical impedance spectroscopy. The results obtained showed that the modified electrode exhibited more excellent electrochemical properties than the bare GCE. The optimum conditions for detection of selenium in water using square wave anodic stripping voltammetry were as follows: deposition potential ?500 mV, pH 1, pre-concentration time of 240 s and 0.1 M nitric acid was used as supporting electrolyte. The linear regression equation obtained was I (µA) = 0.8432C + 9.2359 and the detection limit was calculated to be 0.85 μg L^?1. However, Cu(II) and Cd(II) are the two cations that interfered in the analysis of selenium in water.

The sensor was also applied for real sample water analysis and the result obtained was affirmed with inductively coupled plasma optical emission spectroscopic method. It is believed that our proposed sensor hold promise for practical application.     

Experimental study of the influence of silica nanoparticles on the bulk stability of SDS-foam in the presence of oil

The influence of silica nanoparticles on the bulk stability of SDS-foam in the presence of oil was investigated in this study using KRÜSS dynamic foam analyzer. The bulk foam static stability was evaluated from half-decay time, liquid drainage, bubble size distribution, and change in total height and volume of the generated foams with respect to time. Results clearly showed that foam stability in the presence of oil mainly depends on the viscosity and density of the oil. Foam stability increased with the addition of silica nanoparticles due to the aggregation of the nanoparticles at the thin lamellae of the foam, which prevents spreading of the oil at the gas–liquid interface. Moreover, optimum foam stability was obtained with the modified nanosilica–SDS mixtures, while slower liquid drainage from the foam did not generally result in high foam stability.     

Sulfated Triterpenes from Lemon Balm

The hydroalcoholic (EtOH/H₂O) extract of matured leaf margins of lemon balm (Melissa officinalis L.) afforded a new 3,23‐disulfate of 2α,3β‐23,29‐tetrahydroxyolean‐12‐en‐28‐oic acid 28‐O‐β‐D ‐glucopyranoside ( 1 ) and a new 23‐monosulfate of 2α,23‐dihydroxyurs‐12‐en‐28‐oic acid 3‐O‐β‐D ‐glucopyranoside ( 2 ), along with six known compounds, i.e., 23‐monosulfate of 2α,3β,19α,23‐tetrahydroxyurs‐12‐ene‐28‐oic acid 28‐O‐β‐D ‐glucopyranoside ( 3 ), 3,5,6‐trihydroxydehydro‐α‐ionol 9‐O‐β‐D ‐glucopyranoside ( 4 ), quadranoside III ( 5 ), rosmarinic acid ( 6 ), caffeic acid ( 7 ), and luteolin ( 8 ). All the isolated compounds were evaluated for their antioxidant, antimicrobial, antimalarial, and cytotoxic activities. Only rosmarinic acid exhibited substantial antioxidant and antimicrobial activities, whereas sulfated terpenes showed considerably lower or no antimicrobial activity.     

Effect of Added Monosodium Glutamate on Characteristics of Polyamide Dope Solutions

Formic acid (FA) solutions prepared with various concentrations of polyamide 66 (PA 66) and monosodium glutamate (MSG) were evaluated in terms of properties, such as density, viscosity, and cloud point. The influence on density was insignificant, whereas the viscosity was strongly affected by the amount of PA 66 and MSG additive. The solutions were further evaluated by casting them in a flat film form and determining the demixing time in a humid atmosphere. The considered cases at lower polymer concentrations at various MSG amounts, indicated that the demixing time increased with increase in polymer concentration. The time for demixing, however, decreased for a given higher amount of polymer when the amount of additive was increased in the dope solution. Membranes were prepared at various coagulant bath temperatures. The tensile strength and degree of adsorption (DOA) of these membranes were found. The tensile strength was higher when the membranes were prepared at higher temperature. The DOA, on the other hand, was higher for the membranes formed at lower temperature.     

Chemometric optimization of a SIA promethazine hydrochloride assay method

A sequential injection analysis (SIA) method for the assay of promethazine hydrochloride, based on its oxidation by acidified cerium(IV), was optimized. Three chemometric approaches were applied: (i) factorial design (3³ applied to surface plot and 2³ applied to effect factor) for screening the potential interacting variables, (ii) univariant for optimizing insignificantly interacting variables and (iii) simplex for optimizing potentially interacting variables. The optimum experimental conditions were 30 μl of 0.38 mol/l sulphuric acid, 30 μl of 3.99 × 10^− 3 mol/l cerium(IV), 20 μl of promethazine hydrochloride and 20 μl/s flow rate. The detection limit was 7.032 × 10^− 5 mol/l and the calibration curve was linear up to 1.563 mol/l with a correlation coefficient 0.9998, accuracy range of 89.0-101.5%, relative standard deviation 1.1% (n = 10) and sample frequency at least 20 samples/h. The method was applied to tablet form and validated with the British Pharmacopoeia method. The developed SIA method is fully automated, reproducible, sensitive, rapid and reagent-saving, and therefore suitable for routine control in tablets form.     

Study of (1−x)ZnAl2O4–xSiO2 spinel structures as microwave dielectric materials

Sol–gel method was used to synthesize zinc aluminate (ZnAl₂O₄) dispersed into silica matrix with different compositions of x. Morphological structure of (1?x)ZnAl₂O₄–xSiO₂ samples were investigated by field emission scanning electron microscope (FESEM) and X-ray diffractometer (XRD). The FESEM images showed spherical structures and agglomerated particles occurred inside the samples. XRD analysis indicated the cubic phase formation of the samples. The crystallite size, D was calculated and it was found that the crystallite size are slightly increased from 8 to 17 nm. FTIR spectra analysis shows that the water presence in the samples and also the presence of nitrate group. The dielectric properties have been measured, ε _r value was found to be around 13.0. The S₁₁ parameter analysis shows the samples was resonated at 2.40 GHz and gives different values of bandwidth for microstrip patch antenna application.     

A highly sensitive sensor of paracetamol based on zinc-layered hydroxide-<Emphasis Type="Italic">L</Emphasis>-phenylalanate-modified multiwalled carbon nanotube paste electrode

A new zinc-layered hydroxide-L-phenylalanate (ZLH-LP)-modified multiwalled carbon nanotube (MWCNT) was prepared as a new material of paste electrode for the detection of paracetamol (PCM) in 1.0?×?10^?1 M phosphate buffer solution and at pH 7.5. The electrochemical characterization of the MWCNTs/ZLH-LP paste electrode was characterized by square wave voltammetry, electrochemical impedance spectroscopy, and cyclic voltammetry while the morphology properties of the MWCNTs, ZLH-LP, and MWCNTs/ZLH-LP were investigated using transmission electron microscopy and scanning electron microscopy. Under optimized conditions, the MWCNTs/ZLH-LP paste electrode demonstrated an excellent electrocatalytic activity towards oxidation of PCM in the linear responses’ ranges from 7.0?×?10^?7 M to 1.0?×?10^?4 M (correlation coefficient, 0.996) with the limit of detection obtained at 8.3?×?10^?8 M. As a conclusion, the MWCNTs/ZLH-LP paste electrode revealed good repeatability, reproducibility, and stability, and was found to be applicable for use in pharmaceutical tablet samples.

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Models of the iron-only hydrogenase: structural studies of chelating diphosphine complexes [Fe2(CO)4(micro-pdt)(kappa2P,P'-diphosphine)

Six chelating diphosphine complexes, [Fe2(CO)4(micro-pdt)(kappa2P,P'-diphosphine)], have been crystallographically characterised allowing differences between basal-apical and dibasal conformations to be analysed.     

Environmental impact assessment of post illegal mining activities in Chini Lake with regards to natural radionuclides and heavy metals in water and sediment

Journal of Radioanalytical and Nuclear Chemistry - Comprehensive radiological survey and evaluation of heavy metal contamination were conducted in Chini Lake, which has been awarded a pristine...     

Mn掺杂的铁电半导体BiFeO3本征光催化氧化水活性的研究

开发稳定高效的可见光吸收的氧化物半导体光催化剂是太阳能光催化分解水的一个重要研究方向.最近我们提出(J.Mater.Chem.A,2020,8,6863?6873),具有室温铁电性质的BiFeO₃(BFO)薄膜体系表现出低光电流密度响应是由于铁电畴壁/界面处的电荷复合,而该作用在纳米粒子催化剂体系中应该会大大减少.为了证明这一观点,我们通过溶胶-凝胶法合成了BFO纳米粒子,并进行了Mn掺杂获得了Mn-BFO.光催化水氧化反应表明,纯BFO具有光催化氧化水的活性,析氧数率达到70μmol h^-1 g^-1;而Mn掺杂量优化(0.05%)后的Mn-BFO在可见光(λ≥420 nm)照射下的析氧活性大大提高,达到255mmol h^-1 g^-1.带隙研究表明,通过改变Mn的掺杂量,可以将Mn-BFO的带隙从2.1 eV调整为1.36 eV.DFT计算表明,表面的Fe物种是水氧化的活性位点,而不是Mn物种,因为Mn掺杂后Fe物种的水氧化过电势0.51 V,是所考察的表面Fe和Mn物种中过电势中最低的.因此,Mn-BFO光催化水氧化活性的增强可归因于半导体带隙变窄后吸收更多的可见光、降低了的水氧化过电势以及抑制光生电荷复合这几项的协同效应.这项工作表明,锰掺杂是提高纳米粒子铁电BFO光催化剂固有光催化水氧化活性的有效策略.本文采用溶胶-凝胶法成功制备了锰掺杂的BFO样品,并使用XRD,DRS,Mott-Schottky,XPS和PL等进行了表征.XRD分析结果表明,Mn掺杂后,BFO的(110)和(104)衍射峰向高位衍射角方向位移合并产生一个更宽的峰,表明Mn的掺杂引起BFO晶格结构变形.DRS光谱分析表明,Mn的掺杂可以拓展可见光的吸收,从纯BFO的550 nm吸收边(对应于2.1 eV的带隙)扩展到BFO-2的800 nm(对应于1.46 eV的带隙)吸收带边.这些结果与用DFT计算DOS分析得到的BFO和BFO-2理论带隙值2.05和1.53 eV一致.Mott-Schottky分析表明,BFO和BFO-2是p型半导体,其平带(Vfb)电势分别为1.7和1.6 V vs NHE,VB位置估计分别为2.0和1.9 V vs NHE,而CB位置估计分别为-0.11和0.44 V vs NHE.因此,Mn-BFO在热力学有利于光催化OER但不利于HER.从Mn-BFO的XPS光谱可以看出除了Bi,Fe和O光谱外,也可以在641.20和652.7 eV处观察到出Mn 2p3/2和2p1/2,表明Mn是以Mn3+的形式均匀地掺入BFO的晶格中.对一系列不同含量Mn掺杂的Mn-BFO的光催化OER活性表明研究表明,0.05%Mn掺杂的BFO-2的光催化OER活性最优,其析氧活性达到255μmol h^-1 g^-1,这是迄今为止未加载任何助催化剂的BFO的最高固有光催化OER活性值.PL光谱(290 nm激发)显示,与纯BFO相比,BFO-2的荧光强度弱得多,表明Mn的掺杂可以抑制光生电荷的复合.DFT计算显示,BFO的表面Fe活性中心的OER过电势为0.93 V;而对于Mn掺杂的BFO-2,理论计算得到表面Fe中心和Mn中心的析氧过电位分别为0.51和0.60 V.由此可见,Mn掺杂不改变BFO的析氧活性中心,但是可大大降低Fe活性中心OER过电位,这与锰掺杂的BFO-2表现出比BFO更高光催化氧化水的催化活性实验结果相一致.综上所述,在纳米粒子光催化体系中,Mn掺杂的BFO可以促进可见光的吸收,促进光生电荷有效分离,降低表面Fe基活性中心氧化水的过电位,从而显著提高光催化氧化水的活性.Mn的掺杂对于铁电性质的影响及其光催化活性的关系,有待进一步探索.