微分脉冲溶出伏安法同时测定食品中的锌铁锰

在1％乙二胺-0．1mol／L酒石酸钠-pH11．82 Britton—Robinson缓冲溶液体系中用微分脉冲溶出伏安法同时测定锌、铁、锰三种微量元素。它们的峰电位分别为-1184，-1392和-1456mV(vs．Ag/AgCl)；线性范围分别为：0.001—0.015，0．005—0．05和0．04—0．7μg／mL，最低检出浓度分别为0．0007，0．0014和0．0193μg／mL。本法操作简便、准确、灵敏度较高，用于食品中这三种元素的分析，结果令人满意。     

The Möbius distribution on the disc

A simple new family of distributions is proposed which has support the unit disc in two dimensions. The density functions of the family are unimodal, monotonic or uniantimodal. The bivariate symmetric beta distributions, which include the uniform distribution, are special cases, but many members of the family are skew. The distributions have three parameters, one controlling orientation, one controlling degree of concentration and the third controlling skewness, or more precisely off-centredness. Importantly, these parameters are globally orthogonal. An illustrative example of fitting the model to data is given. Conditional and marginal distributions are considered. The new distributions are compared favourably with an earlier suggestion of the same author.     

Synthesis, morphology and random laser action of ZnO nanostructures

Three-dimensional (3-D) ZnO random-wall nanostructures and one-dimensional (1-D) ZnO nanorods were prepared on silicon substrates by a simple solid-vapour phase thermal sublimation technique. Optical pumped random lasing has been observed in the ZnO random-wall arrays with a threshold intensity of 0.38 MW/cm² in the emission wavelength from 380 to 395 nm. The optical gain was attributed to the closed-loop scattering and light amplification of the ZnO random-wall. The experimental result suggests that the morphology of nanostructure is the key factor to effect random lasing.     

The response of thermally and optically stimulated luminescence from Al2O3:C to high-energy heavy charged particles

The thermoluminescence (TL) and optically stimulated luminescence (OSL) response of Al₂O₃ dosimeters to high-energy heavy charged particles (HCP) has been studied using the heavy ion medical accelarator at Chiba, Japan. The samples were Al₂O₃ single-crystal chips, of the type usually known as TLD-500, and Luxel^TM dosimeters (Al₂O₃:C powder in plastic) from Landauer Inc. The samples were exposed to ⁴He (150 MeV/u), ¹²C (400 MeV/u), ²⁸Si (490 MeV/u) and ⁵⁶Fe (500 MeV/u) ions, with linear energy transfer values covering the range from 2.26 to 189 keV/μm in water and doses from 1 to 100 mGy (to water). A ⁹⁰Sr/⁹⁰Y beta source, calibrated against a ⁶⁰Co secondary standard, was used for calibration purposes. For OSL, we used both continuous-wave OSL measurements (CW-OSL, using green light stimulation at 525 nm) and pulsed OSL measurements (POSL, using 532 nm stimulation from a Nd:YAG Q-switched laser). The efficiencies (η_HCP,γ) of the different HCPs at producing OSL or TL were observed to depend not only upon the linear energy transfer (LET) of the HCP, but also upon the sample type (single crystal chip or Luxel^TM) and the luminescence method used to define the signal—i.e. TL, CW-OSL initial intensity, CW-OSL total area, or POSL. Observed changes in shape of the decay curve lead to potential methods for extracting LET information of unknown radiation fields. A discussion of the results is given, including the potential use of OSL from Al₂O₃ in the areas of space radiation dosimetry and radiation oncology.     

Luminescence properties of α-Al2O3 dosimetric crystals exposed to a high-current electron beam

The spectra of pulsed cathodoluminescence (PCL) and thermoluminescence (TL) in TLD-500 detectors, which were exposed to a strong beam from a pulsed electron accelerator, have been studied. Additional bands in the PCL spectrum and new peaks in the TL curves, which are due to impurity ions, have been revealed. Luminescence bands of F- and F⁺-centers cannot be used in the dosimetry of strong electron beams using TLD-500 detectors because of the saturation of dose dependence and the decrease in the TL yield. It is shown that high doses from these beams can be measured by recording TL in the luminescence band of impurity titanium ions.     

NMR studies on a palladium(II) complex containing an incompletely coordinated facultative pentadentate Schiff base ligand

Palladium(II) dichloride reacts with 1,10‐bis(2‐pyrrolyl)‐2,5,9‐triaza‐1,9‐decadiene to give a [Pd(C₁₅H₂₀N₅)]Cl complex in which the ligand is four‐coordinated, leaving one pyrrole group dangling. By using COSY, gHSQC, gHMBC connectivities and NOE experiments it has been concluded that one linkage isomer exists in DMSO solution, in spite of the fact that different sets of N atoms of potentially pentadentate ligand might be involved in coordination, and that the three chelate rings in the complex cation are arranged in a sequence: five‐membered, six‐membered, five‐membered which is different from that (5–5–6) found by x‐ray studies on the related [Ni(C₁₅H₂₀N₅)]Cl compound. NMR studies allowed an unambiguous assignment of all ¹H and ¹³C NMR resonances for the complex. Results of x‐ray structural analysis of [Pd(C₁₅H₂₀N₅)](CH₃COO)H₂O supported the five‐membered, six‐membered, five‐membered ring sequence in the [Pd(C₁₅H₂₀N₅)]⁺ complex cation and show an E (trans) orientation of the dangling pyrrole group with respect to the metal center. Copyright © 2002 John Wiley & Sons, Ltd.     

Ca(NO3)2•4H2O-catalysed Biginelli Reaction: One-pot Synthesis of 1,2,3,4-Tetrahydropyrimidin-2-ones/pyrimidine-2-thiones under Solvent-free Conditions

The synthesis of 1,2,3,4-dihydropyrimidinone/thione derivatives was achieved in good to excellent yields using calcium(II) nitrate as catalyst to promote the Biginelli three-component condensation reaction from a diversity of aromatic aldehydes, β-keto compounds and urea or thiourea. The reaction was carried out under solvent-free conditions.     

Hydrophilic segmented block copolymers based on poly(ethylene oxide) and monodisperse amide segments

Segmented block copolymers based on poly(ethylene oxide) (PEO) flexible segments and monodisperse crystallizable bisester tetra‐amide segments were made via a polycondensation reaction. The molecular weight of the PEO segments varied from 600 to 4600 g/mol and a bisester tetra‐amide segment (T6T6T) based on dimethyl terephthalate (T) and hexamethylenediamine (6) was used. The resulting copolymers were melt‐processable and transparent. The crystallinity of the copolymers was investigated by differential scanning calorimetry (DSC) and Fourier Transform infrared (FTIR). The thermal properties were studied by DSC, temperature modulated synchrotron small angle X‐ray scattering (SAXS), and dynamic mechanical analysis (DMA). The elastic properties were evaluated by compression set (CS) test. The crystallinity of the T6T6T segments in the copolymers was high (>84%) and the crystallization fast due to the use of monodisperse tetra‐amide segments. DMA experiments showed that the materials had a low T_g, a broad and almost temperature independent rubbery plateau and a sharp flow temperature. With increasing PEO length both the PEO melting temperature and the PEO crystallinity increased. When the PEO segment length was longer than 2000 g/mol the PEO melting temperature was above room temperature and this resulted in a higher modulus and in higher compression set values at room temperature. The properties of PEO‐T6T6T copolymers were compared with similar poly(propylene oxide) and poly(tetramethylene oxide) copolymers. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 4522–4535, 2007     

Dielectric properties of europium-indium oxide solid solution films prepared on Si (100) substrates

Thin Eu-In solid solution oxide films (SS) were grown on Si (P) substrates to form MOS devices. The samples were characterised by X-ray fluorescence and X-ray diffraction techniques. The ac-conductance and capacitance of the devices were studied as a function of frequency in the range 500 Hz to 100 kHz, temperature in the range 293-400 K and gate voltage. The investigation established that: (1) the prepared SS exhibit a sudden reversible structural change at about 370 K, (2) the frequency dependence for f>10 kHz of the ac-conductivity and capacitance of the insulator at room temperature is controlled by the ‘corrected barrier hopping’ CBH model, (3) the temperature dependence of the ac-conductance which shows a small activation energy characterises the hopping process of current carriers between equilibrium sites, and (4) the prepared transparent SS have a sufficiently high relative permittivity ?, around 30, which suggests they are promising candidates for high-? dielectric applications.     

Magnetic properties of lanthanum orthoferrite fine powders prepared by different chemical routes

Fine powders of lanthanum iron oxide, LaFeO₃, have been prepared by solid state reaction as well as sol-gel synthesis and nebulized spray pyrolysis. Structures, morphologies and magnetic susceptibility measurements of these powders have been examined. The powders prepared by all the three low-temperature routes contain nearly spherical particles with an average diameter of 40 nm. These samples show a lower Neel temperature than the powder prepared by solid state reaction besides showing much lower magnetic susceptibility at low temperatures. Dedicated to Professor C N R Rao on his 70th birthday