Mössbauer studies on the gamma radiolysis of cesium tris(oxalato)ferrate(III) dihydrate

The final products of the gamma radiolysis of cesium tris (oxalato) ferrate (III) dihydrate have been identified by Mössbauer spectroscopy and thermogravimetric analysis as a mixture of Cs₂Fe(ox)₂.4H₂O and Cs₂Fe(ox)₂ in equivalent proportions. The tetrahydrated compound can also be made by wet synthesis whereas the anhydrous salt can be obtained from thermal decompositions of either the tetrahydrated ferrous salt at 160°C or of the ferric complex at 285°C. The radiolytic decomposition proceeds as a first-order process due to the original compound depletion and to the radiolytic stability of the radiolytic products.     

Low temperature one-step synthesis of cobalt nanowires encapsulated in carbon

The one-step method of carbon nanotubes filled with continuous cobalt nanowires (CoF-CNT) synthesis is presented. Co/ZSM-5 (8 wt% Co) was used as catalyst for CoF-CNT production by methane decomposition at the temperature of 400 °C and 800 °C at atmospheric pressure in a conventional gas-flow system. The average diameter of the CoF-CNT is about 25 and 40 nm for products obtained at 400 °C and at 800 °C, respectively. The average size of coherently scattering domains along the normal to graphite layers L _c , the interlayer spacing d ₀₀₂, the graphitization degree of carbon, and the relative intensities of the G and D bands in Raman spectroscopy were determined to characterize the quality of carbon. It was proved that cobalt-filled carbon nanotubes can be produced by a simple method. The results of XRD, FE-SEM, and TEM show that CoF-CNT can be obtained even at 400 °C by catalytic decomposition of methane. On the basis of XRD, TEM, Raman spectroscopy was found that at a temperature of 800 °C, a better quality of carbon was produced.     

siRNA-loaded PEGylated porous silicon nanoparticles for lung cancer therapy

The BiPO₄/reduced graphene oxide (RGO) nanocomposites were prepared by a facile solvothermal approach. The prepared samples were characterized with Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, UV–vis diffuse reflectance spectroscopy, electrochemical impedance spectra, and Mott–Schottky and the photoluminescence spectra. A large quantity of BiPO₄ nanoparticles with sizes of ca. 150 nm were well dispersed on the RGO nanosheets. The absorbance of the BiPO₄/RGO nanocomposites is largely enhanced in the range of 400–800 nm compared with that of BiPO₄, and the BiPO₄/RGO showed better photocatalytic activities under simulated sunlight irradiation than the BiPO₄ nanocrystals.     

Synthesis,characterization and excellent photocatalytic activity of Ag/AgBr/MoO3 composite photocatalyst

A novel composite photocatalyst Ag/AgBr/MoO₃ was successfully synthesized via a simple precipitation method at room temperature. The obtained products were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, high-resolution transmission electron microscopy and UV–vis diffuse reflectance spectroscopy in detail. The photocatalytic activity of the samples was evaluated by monitoring the degradation of rhodamine B (RhB) solution under visible-light irradiation. The results showed that the photocatalytic activity of Ag/AgBr/MoO₃ composite significantly enhanced and the degradation ratio of RhB reached 97.7 % after 15 min only. The excellent photocatalytic activity might be closely related to the large surface area, porosity structure and efficient separation of photoinduced electron–hole pairs. The possible reaction mechanism was also discussed.     

An Innovative Measurement of Extractable Proteins from Concentrated Latex Containing Eggshell Calcium Oxide Compounds by Near-Infrared Spectroscopy

ABSTRACT

Near-infrared reflectance (NIR) spectroscopy, in the spectral range of 1100–2500 nm, was used to measure the amount of the directly extractable proteins (EP) where a small amount can cause a latex allergy to patients. The NIR spectra revealed an amino or a peptide (N-H) of the extractable proteins from the concentrated rubber latex added with sodium dodecyl sulphate (SDS) and calcium chloride, the latter being obtained from the pyrolysis of eggshells at 900°C for 2 hr and dissolving in 2 M HCl. The extractable proteins measured by NIR are equal to 5306.58 ± 1727.00 µg/g (0.53%) close to the value obtained by the modified Lowry method, which is 5566.02 ± 717.39 µg/g (0.56%). A partial least square regression model (PLSR) of the NIR spectra and the extractable protein contents yields a correlation coefficient of .72, a root mean square error of calibration (RMSEC) of 1298 µg/g, and a small bias value of ?0.0002 µg/g. The absorbance peaks at the wavelengths of 1520 nm and 1980 nm are related to the first overtone N-H (υ₁N-H) and the asymmetric combination of N-H, respectively. Furthermore, the absorbance peaks at the wavelengths of 1450 nm and 1920 nm correspond to the first overtone of O-H (υ₁O-H) of the concentrated latex compounds. The results demonstrate the NIR spectroscopy potential as a fast and noninvasive measurement technique.     

Synthesis and luminescence properties of Na2Ba2Si2O7:Eu2+ phosphor

Green-emitting phosphor Na₂Ba₂Si₂O₇:Eu²⁺ has been synthesized by a conventional high-temperature solid-state reaction. The phase structure and luminescence properties are characterized by the X-ray powder diffraction, diffuse reflectance spectra, photoluminescence excitation and emission spectra, temperature-dependent emission spectra, respectively. It can be efficiently excited in the wavelength range of 325–400 nm and consists of a strong broad green band centered at about 501 nm, which is ascribed to 4f⁶6s⁰5d¹ → 4f⁷6s²5d⁰ transition of Eu²⁺. The critical quenching concentration of Eu²⁺ in the Na₂Ba₂Si₂O₇ host is about 0.8 mol % and corresponding quenching behavior is ascribed to be electric dipole–dipole interaction. Furthermore, the phosphor has good thermal stability property, and the activation energy for thermal quenching is calculated as 0.34 eV.     

Visible-Light Activities of Erbium Doped BiVO4 Photocatalysts

采用水热合成法,制备出Er掺杂的BiVO₄复合光催化剂,并采用XRD、SEM、XPS和紫外-可见漫反射光谱技术对其进行分析表征．通过可见光下降解水溶液中甲基橙分子来考察其光催化性能,结果显示掺杂组份以氧化物Er₂O₃形式存在于的复合光催化剂中;且掺杂复合光催化剂的可见光吸收和催化活性都比纯BiVO₄有所增强．     

Ag8SnSe6 argyrodite synthesis and optical properties

The Ag₈SnSe₆ argyrodite compound was synthesized by the direct melting of the elementary Ag, Sn and Se high purity grade stoichiometric mixture in a sealed silica ampoule. The prepared polycrystalline material was characterized by the X-ray diffraction (XRD), visible (VIS) and near-infrared (NIR) reflection and photoluminescence (PL) spectroscopy. XRD showed that the Ag₈SnSe₆ crystallizes in orthorhombic structure, Pmn2₁ space group with lattice parameters: а = 7.89052(6) Å, b = 7.78976(6) Å, c = 11.02717(8) Å. Photoluminescence spectra of the Ag₈SnSe₆ polycrystalline wafer show two bands at 1675 nm and 1460 nm. Absorption edge position estimated from optical reflectance spectra is located in the 1413–1540 nm wavelength range.     

Preparation of CeO2 by a simple microwave–hydrothermal method

Cerium carbonate hydroxide (orthorhombic Ce(OH)CO₃) hexagonal-shaped microplates were synthesized by a simple and fast microwave–hydrothermal method at 150 °C for 30 min. Cerium nitrate, urea and cetyltrimethylammonium bromide were used as precursors. Ceria (cubic CeO₂) rhombus-shape was obtained by a thermal decomposition oxidation process at 500 °C for 1 h using as- synthesized Ce(OH)CO₃. The products were characterized by X-ray powder diffraction, field-emission scanning electron microscopy, thermogravimetric analysis and Fourier transformed infrared spectroscopy. The use of microwave–hydrothermal method allowed to obtain cerium compounds at low temperature and shorter time compared to other synthesis methods.     

Far-infrared probe of energy gap in LaO1−xFxFeGe compound

We report on the electrical resistivity and far-infrared reflectance measurements of LaO_1?xF_xFeGe samples. Furthermore, we introduce a new method to probe the energy gap and determine its value. The onset transition temperature was 22.8 K for x = 0.13, and a clear anomaly was observed at 90 K in the ρ(T) curve for x = 0.11 with T_c = 20.6 K. We clearly observed the phonon-suppressed feature in reflectance spectra where F-doping caused a strong suppression of a peak at 200 cm^?1. The energy gap above T_c, 2Δ = 2.10 meV, was determined from the measured spectra based on the changes in reflectivity by F-doping.     

Oxidation of bismuth nanodroplets deposit on GaAs substrate

Bismuth nanodroplets on GaAs substrate were obtained by metalorganic vapor phase epitaxy (MOVPE). New products have been synthesized when Bi nanodroplets are heated under oxygen atmosphere. The oxidation process of Bi nanodroplets consists of a heating from the room temperature to different oxidation temperatures (350, 500, 600 ^°C) with a temperature rate of 14 ^°C/min. The annealing duration was fixed to 30 min. The presence of oxygen in the products was confirmed by energy dispersive X-ray (EDX) measurements using a scanning electron microscope (SEM). SEM images show that Bi microcomposites density decrease and their size increases with increasing annealing temperature. After X-ray diffraction analysis of the products no obvious peaks could be observed. The reflectance spectra of the products were studied in spectral domains ranged from 200 nm to 1100 nm. By fitting the reflectivity signal, we extracted the thickness of the products and their refractive index variation versus wavelength. The results show that the thickness of the samples increases with increasing annealing temperature. The photoluminescence (PL) spectra under excitation at 325 nm shows a broad emission centered at around 1.92 eV.     

Preparation and characterization of Y-Fe alloy nanowires by template-assisted electrodeposition from aqueous solution

In this study, a method was proposed for the preparation of Y-Fe alloy nanowires by PC membrane template-assisted electrodeposition from aqueous solution. Citric acid  acted as complexing agent was used into the solution to fabricate Y-Fe alloy nanowires. The electrolyte solution consisted of 5 g L^?1 YCl₃, 12.5 g L^?1 FeSO·6H₂O, different concentrations of citric acid , 25 g L^?1 boric acid in deionized water. The energy dispersive spectroscopy (EDS) found that the content of Y in the nanowires can be controlled by citric acid concentration and the current intensity, and the content of Y could reach up to 33.16 wt%. Scanning electron microscopy (SEM), BET specific surface area (BET), and X-ray diffraction (XRD) showed that there was a shift in the structure of nanowires from semicrystalline to amorphous due to the change of Y content, and their shapes were approximately 100 nm in diameter and 6 μm in length; the surface areas of nanowires were about 3.97 m²/g. Fourier transform infrared (FTIR) spectroscopy, UV–Vis diffuse reflectance spectroscopy, and X-ray photoelectron spectroscopy (XPS) indicated the formation of Y-Fe alloy, Y₂O₃ and Fe₂O₃   existed  in the outer layer of nanowires. The magnetic field applied both parallel and perpendicular to the nanowires by alternating gradient magnetometer (AGM) showed small magnetic anisotropy and low coercivity with easy axis of magnetization perpendicular to the nanowires. In addition, the magneto-optic Kerr effect (MOKE) was investigated, and a Kerr rotation angle of 29 mdeg was obtained.     

Decomposition of binary sulphate KHSO4 at high pressure

Abstract

Pressure induced decomposition (PID) is known to occur only at elevated temperatures. Here we report its first occurrence at ambient temperature in a binary sulphate, KHSO₄ at 4kbar. Raman spectroscopy is used for identifying the decomposition products as K₃H(SO_{2 4}) and H₂SO₄ from their characteristic spectra. One of the decomposition products being a liquid is argued to be the reason for the occurrence of the phenomenon at ambient temperature. Other possible decomposition routes are also examined.     

Evidence of magnetic broadening in Mössbauer spectra of superconducting FeTe 0.8 S 0.2

Magnetic properties of the FeTe_0.8S_0.2 superconductor were studied by Mössbauer spectroscopy. Low-velocity Mössbauer spectra that were recorded in the temperature range from 5.7 K up to 300 K show a paramagnetic doublet with a broadening at temperatures below 77 K. The broadening can be explained by the appearance of a distribution of hyperfine magnetic fields due to the magnetic ordering of a part of the sample. The magnetically ordered fraction starts to decrease at temperatures below 20 K indicating a possible competition with the onsetting superconductive state.     

Polyhydroxy fullerenes

Characterization of C₆₀ polyhydroxyfullerenes (PHF) prepared in alkaline media, preparation facilitated by phase-transfer catalyst, presents challenges in determining the chemical structure resulting from the possibility of multiple isomers or analogs with greater or fewer hydroxyl groups from a single reaction mixture. This paper presents the utilization of analytical methods employed in tandem, especially X-ray photoelectron spectroscopy, nuclear magnetic resonance spectroscopy, Fourier transform infrared spectroscopy for semi-quantitative analysis on the number of hydroxyl groups present in PHF. Capillary Electrophoresis was used for purity estimation of the material. Multiple spectra and electropherograms were analyzed using a new simultaneous curve fitting method. The most accurate estimate of hydroxyl groups for C₆₀ polyhydroxy fullerenes obtained is between 16 and 18 allylic hydroxyl groups by combining analytical methods’ results with 5 % accuracy. High precision (reproducibility) of the experiments is observed. Purity of 98 % is estimated by capillary electrophoresis. The size of PHF nanoparticles or aggregates has been determined by atomic force microscopy to be 7.4–14.2 nm. According to the elemental analysis the average probable empirical formula for the most pure PHF at pH 7.1 is C₆₀O₁₇H₁₂Na₅(NaHCO₃)₃(H₂O)₁₃ and the average formula weight is 1,605.9 g/mol. This is the first thorough characterization of PHF in terms of purity.     

Visible light activated photo-catalytic effect and local structure of iron silicate glass prepared by sol-gel method

A relationship between methylene blue (MB) decomposition ability under visible light and local structure of xFe₂O₃·(100-x)SiO₂ glass abbreviated as xFS prepared by sol-gel method was investigated by ⁵⁷Fe-Mössbauer spectroscopy, X-ray diffractometry (XRD) and ultraviolet-visible light absorption spectroscopy (UV-Vis). Mössbauer spectra of xFS glass with x of 10, 30 and 50 annealed at 1000 °C for 3 h were mainly composed of a paramagnetic doublet due to fayalite (Fe₂SiO₄), and magnetic sextets due to magnetite (Fe₃O₄) or hematite (α-Fe₂O₃). The absorption area (A) of α-Fe₂O₃ gradually increased from 0.0 to 10.3 and 100 % with the increasing Fe₂O₃ content (x) of annealed xFS glass. A leaching test performed by 20 mL of MB aqueous solution and 40 mg of annealed 50FS glass showed that MB concentration decreased from 16.2 to 4.7 μmol L^?1 after 2 h with the first order rate constant of 1.8 × 10^?4 s^?1. These results prove that annealed iron silicate glass containing α-Fe₂O₃ can decompose MB effectively under visible light irradiation.     

Thermal release of trapped deuterium from silica injected by 80-keV D+ ion implantation and RF D2 plasma

When silica is irradiated by 80-keV D⁺ ions or RF plasma of D₂ gas, deuterium is trapped in the silica forming Si-OD bonds. The deuterium, trapped as OD bonds, is desorbed from the silica upon heating to form some release products. The thermal detrapping process corresponds to decrease of OD bonds and was studied by measurement of infrared Fourier transform spectroscopy (FTIR). The release products HDO, D₂O, HD, and D₂ were measured by quadrupole mass spectroscopy (QMS). The detrapping and release processes of trapped deuterium were studied by simultaneous measurement of FTIR and QMS. Since the release spectra of HDO, D₂O, HD, and/or D₂ correspond to the decrease spectra of OD bonds, these release products are formed by thermal decomposition of OD bonds. The formation of water (HDO, D₂O) and hydrogen (HD, D₂) depends upon concentration of pre-existing OH bonds and deuterium injection methods (80-keV D⁺ implantation or RF D₂ plasma irradiation).     

Kinetic analysis of the thermal decomposition of pristine and γ-irradiated zinc uranyl acetate

Thermal decomposition of pristine and γ-irradiated zinc uranyl acetate was investigated in air using isothermal and dynamic thermogravimetric techniques. The decomposition proceeded via one major process with the formation of triuranates ZnU₃O₁₀ as solid residues. Kinetic analysis of isothermal data, when compared with various solid-state reaction models, showed that the decomposition reaction is best fitted by the phase-boundary model. Kinetic analysis of the dynamic TG curves was discussed with reference to integral methods of modified Coats and Redfern equations. Kinetic and thermodynamic parameters were calculated and evaluated. IR spectroscopy and X-ray powder diffraction techniques were employed to follow the chemical composition of solid residue at different calcination temperatures. The results display that the triuranate ZnU₃O₁₀ starts forming by calcination of zinc uranyl acetate at temperatures?>?300 °C and undergoes decomposition at higher temperatures (>600 °C) with the formation of U₃O₈. The results were evaluated regarding the utilization of zinc uranyl acetate as an important source of diuranates and triuranates.     

Mössbauer and calorimetric studies of portland cement hydration in the presence of black gram pulse

Effect of different concentrations of naturally occurring admixture in the form of fine powder of black gram pulse (BGP) on the hydration of Portland cement was studied by isothermal calorimetry and ⁵⁷Fe Mössbauer spectroscopy. The spectra were recorded for anhydrous cement and the hydration products at room temperature and 77 K. In the presence of BGP, the spectra showed superparamagnetic doublets at room temperature and the sextet at 77 K, due to the presence of fine particles of iron containing component. Mössbauer studies of hydration products confirmed the formation of nanosize hydration products containing Fe^3?+?. The isomer shift (δ) and the quadrupole splitting (ΔE _Q) values of C₄AF in the cement confirmed iron in an octahedral and tetrahedral environment with +3 oxidation state. The high value of quadrupole splitting showed the high asymmetry of the electron environment around the iron atom. The overall mechanism of the hydration of cement in presence of BGP is discussed.