Spectroscopic characterization of alkaline earth uranyl carbonates

A series of alkaline uranyl carbonates, M[UO₂(CO₃)₃]·nH₂O (M=Mg₂, Ca₂, Sr₂, Ba₂, Na₂Ca, and CaMg) was synthesized and characterized by inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS) after nitric acid digestion, X-ray powder diffraction (XRD), and thermal analysis (TGA/DTA). The molecular structure of these compounds was characterized by extended X-ray absorption fine-structure (EXAFS) spectroscopy and X-ray photoelectron spectroscopy (XPS). Crystalline Ba₂[UO₂(CO₃)₃]·6H₂O was obtained for the first time. The EXAFS analysis showed that this compound consists of (UO₂)(CO₃)₃ clusters similar to the other alkaline earth uranyl carbonates. The average U-Ba distance is 3.90±0.02 Å.Fluorescence wavelengths and life times were measured using time-resolved laser-induced fluorescence spectroscopy (TRLFS). The U-O bond distances determined by EXAFS, TRLFS, XPS, and Raman spectroscopy agree within the experimental uncertainties. The spectroscopic signatures observed could be useful for identifying uranyl carbonate species adsorbed on mineral surfaces.     

Spectroscopy, NMR and DFT studies on molecular recognition of crown ether bridged chiral heterotrinuclear salen Zn(II) complex

A barium-containing crown ether bridged chiral heterotrinuclear salen Zn(II) complex BaZn2L(ClO4)2, where L is a folded dinuclear chiral (R,R)-salen ligand, has been synthesized and characterized by elemental analysis, 1H NMR, UV-vis, IR, circular dichroism (CD) spectra, and mass spectra. As a folded dinuclear chiral host, its recognition with achiral guests (imidazole derivatives), rigid bidentate guest (1,4-diazobicyclo[2,2,2]octane, DABCO) and chiral guests (amino acid methyl esters) was investigated by means of UV-vis spectrophotometric titration, CD spectra. The association constants of D-amino acid methyl esters are found to be higher than those of their L-enantiomer. The sandwich-type binding of BaZn2L(ClO4)2-DABCO supramolecular assembly was specially studied via 1H NMR titration and 1H ROESY. To understand the recognition on molecular level, density functional theory (DFT) calculations on B3LYP/LanL2DZ were performed on the minimal energy conformations of host, guests, and host-guest complexes. The minimal energy conformations were obtained by molecular mechanics (MM) optimization and molecular dynamics (MD) simulation. The results of single point energy, HOMO energy, and charges transfer were analyzed. The results of theoretical calculations are in good agreement with the experimental data.     

μs级负充电时不同体积分数去离子水与乙二醇混合液电性能的实验研究

 以去离子水与乙二醇的混合液（体积分数分别为36.5%,48.7%,59.0%及71.2%，以下简称混合液）作为同轴传输线的绝缘介质，进行了μs级高电压负充电条件下的正电极击穿实验，研究了混合液的击穿电压、击穿时间、相对介电常数及电阻率与体积分数的关系。实验结果表明：在充电电压为20kV时，71.2%的混合液比36.5%的混合液的平均击穿电压提高25.1%，平均击穿时间延长10.49%，而相对介电常数减小868%。同时，随着充电时间的缩短，混合液的击穿电压提高。     

Structural and optical properties of CuSe2 nanocrystals formed in thin solid Cu–Se film

This paper describes the structural and optical properties of Cu–Se thin films. The surface morphology of thin films was investigated by atomic force microscopy (AFM) and scanning electron microscopy (SEM). Formation of Cu–Se thin films is concluded to proceed unevenly, in the form of islands which later grew into agglomerates. The structural characterization of Cu–Se thin film was investigated using X-ray diffraction pattern (XRD). The presence of two-phase system is observed. One is the solid solution of Cu in Se and the other is low-pressure modification of CuSe₂. The Raman spectroscopy was used to identify and quantify the individual phases present in the Cu–Se films. Red shift and asymmetry of Raman mode characteristic for CuSe₂ enable us to estimate nanocrystal dimension. In the analysis of the far-infrared reflection spectra, numerical model for calculating the reflectivity coefficient of layered system, which includes film with nanocrystalite inclusions (modeled by Maxwell-Garnett approximation) and substrate, has been applied.     

由季戊四醇合成季戊四硫醇的新方法

以季戊四醇为原料,先合成四对甲苯磺酸季戊四醇酯,然后四对甲苯磺酸季戊四醇酯与硫氰酸钾在N,N-二甲基甲酰胺中加热反应,生成了2,3,7,8-四硫螺[4,4]壬烷,2,3,7,8-四硫螺[4,4]壬烷经四氢化铝锂还原、酸化,得到季戊四硫醇.产物结构经熔点、红外光谱、质子核磁共振谱、拉曼光谱鉴定.     

A robust spin-coated optical sensing device for rapid determination of predominant metal ions in wastewater streams

The potential of an optical sensing material for determination of metal ions in wastewater streams is presented. The initial results in the development of a chromo-ionophore-based optical sensor for metal ions are detailed. An azo dye species, 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (BrPADAP), together with an ionophore and plasticiser was immobilised in a film of poly(vinyl chloride) (PVC). Initial investigations using the dye-impregnated sensing film showed a reproducible and reversible response to Pb(II) ions in aqueous solution. The response of this sensing film to Pb(II) at pH 6 was found to be linear in the 0.1-10 mg/L range, with a %RSD of 1.55%. The film can be regenerated by immersion in a low-pH buffer solution. The authors demonstrate how this method shows potential for analysis using once-off sensing probes. The sensing film response for Pb(II) occurs within 30 s.     

Measurement of the Rates of Diffusion of Halomethanes into Polymer Films Using ATR-FTIR Spectroscopy

Polymer-modified attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy and FEWS (fibre-optic evanescent wave) spectroscopy have been very successful to date for sensitive detection of organic pollutants in water utilising the mid-infrared (MIR) region of the electromagnetic spectrum (4000-400 cm^?1). This sensing approach involves the use of different polymer films for preconcentration with optimisation of the sensor related to the rate of diffusion of solvent molecules into these polymer films. Compounds such as chloroform, bromoform, bromodichloromethane and dibromochloromethane which are collectively referred to as trihalomethanes (THMs) were analysed in this work. A gaseous phase experimental design was used and from experimental data the rate of diffusion of each of the halomethanes was quantified based on a Fickian type diffusion model. Individual diffusion coefficient values were found to be in the range 3.38 E-10 ± 0.01 E-10 to 4.72 E-08 ± 0.42 E-08 cm² s^?1. Multicomponent effects were observed for mixtures of compounds diffusing into polyisobutylene and ethylene-propylene copolymer.     

Isolation and Characterization of Badge Hydrolysis Products

Heating a suspension of Bisphenol A diglycidyl ether (BADGE) in 20 : 80 tetrahydrofuran/water at 70°C and subsequent passage of the resulting solution through C18 columns allowed isolation and purification to > 97% of each of the two hydrolysis products 2-[4-(2,3-dihydroxypropoxy) phenyl]-2-[4-(2,3-epoxypropoxy)phenyl]propane (1HP) and 2,2-bis[4-(2,3-dihydroxypropoxy)phenyl] propane (2HP), which were characterized by UV, IR, ₁H and _I3C NMR spectroscopy and mass spectrometry.     

Electrochemical Detection of Cardiac Biomarkers Utilizing Electrospun Multiwalled Carbon Nanotubes Embedded SU‐8 Nanofibers

In this paper we demonstrate synthesis and characterization of MWCNTs embedded SU‐8 electrospun nanofibers and their application towards ultrasensitive detection of cardiac biomarkers using Electrochemical Impedance spectroscopy (EIS). The composite nanofibers have excellent electrical and transduction properties owing to the presence of MWCNTs in addition to ease of functionalization and biocompatibility, which can be attributed to the presence of SU‐8. Thus the synthesized nanofibers are ideal candidates for sensitive biosensor applications. As a proof concept, the detection of cardiac biomarkers, Myoglobin (Myo), cardiac Troponin I (cTn I) and Creatine Kinase MB (CK‐MB) is demonstrated. The synthesized nanofibers were functionalized with the antibodies of the biomarkers and the detection was carried using Electrochemical Impedance Spectroscopy, an excellent technique for understanding the adsorption kinetics. A minimum detection limit of nano‐gram/ml is demonstrated using this nanobiosensor platform.     

Thermal Degradation of Polysiloxane Coatings on E-Glass Fiber. A FTIR Study

Fourier Transform Infrared Spectroscopy and Thermal Analysis have been used to study the thermal and termooxidative degradation of polysiloxane coatings obtained by treating E-glass fiber with aqueous solutions of 3-chloropropyltriethoxysilane. Initial weight losses were due to polymerization of the coatings. Severe oxidative degradations were observed at temperatures above 180°C. At 550°C the residue of the coating was found to be silica with free silanol groups.