Modulation structure stability of heat-treated Co/C and CoN/CN soft X-ray multilayers

Modulation structure stability of Co/C and CoN/CN soft X ray multilayers has been investigated by X ray diffraction and Raman spectroscopy. The graphitization of the amorphous carbon layers in Co/C multilayers causes a period expansion of 12% at annealing temperatures below 400℃. An enormous period expansion (～40%) induced by the crystallization and agglomeration of Co layers has been observed at 500℃. While the period expansion of CoN/CN multilayers is only 4% at 400℃. The interface pattern of the CoN/CN multilayers still exists even if they were annealed at 700℃. The relatively good thermal stability of CoN/CN multilayers can be attributed to the suppression of the formation of the sp 3 bonding and, at annealing temperatures higher than the phase transition temperature of 420℃ (from hcp to fcc), the coexistence of hcp and fcc Co structures through doping nitrogen.     

Synthesis and structure of Cu5(BTA)6(TTA)4 · 5DMF, a copper-nitrogen cluster containing η Π3-benzotriazolate

The title cluster compound—Cu₅(BTA)₆(TTA)₄·5DMF was prepared using thenyltrifluoroacetone and benzotriazolate ligands. The crystal structure indicates that a tetrahedral array of Cu(1), Cu(2), Cu(3) and Cu(4) ions surrounding a central Cu(5) ion are held together by bridging tridentate BTA^- and terminated by TTA^- bond cap. The three nitrogen atoms of a BTA^- bond three different copper ions to form a η³-benzotriazolate. The central Cu ion has a distorted octahedral structure and the surrounding Cu ions are 5 coordinated forming distorted tetragonal structures. The distances between the surrounding Cu(Ⅱ) ions and the central Cu(Ⅱ) ion are in the range of 0.3561—0.3755 nm and those between the surrounding Cu(Ⅱ) ions are in the range of 0.5785—0.6301 nm.     

(002)织构HCP钴纳米线磁性研究

采用交流电化学沉积法在氧化铝模板孔洞中制备了有序钴纳米线阵列。利用X射线衍射、扫描电子显微镜、透射电子显微镜、振动样品磁强计等对样品的结构、形貌和磁性进行了表征和研究。扫描电镜表明氧化铝模板孔洞直径为20 nm,结构研究证明钴纳米线为六角密堆积(HCP)结构且具有很强的(002)织构,磁性测试发现该钴纳米线阵列具有很强的单轴各向异性,室温矫顽力达2 590 Oe,有望用于高温永磁磁记录。     

金纳米线阵列的制备及其光学性能研究

采用二次阳极氧化法制备了高度有序的多孔氧化铝模板,并基于该氧化铝模板,采用脉冲直流电化学沉积的方法制备了金纳米线阵列.利用扫描电子显微镜（SEM）、透射电子显微镜（TEM）和X线衍射仪（XRD）对所制备的金纳米线的形貌及晶体结构进行分析.结果表明：不同的沉积电压下制备的金纳米线具有不同的生长取向性,当沉积电压为3V时制备出的金纳米线沿[200]方向具有明显的生长取向性.利用紫外-可见光谱（UV-Vis）对金纳米线阵列光学性能进行研究,发现金纳米线的等离子体共振吸收峰随着沉积电压的增大先蓝移而后发生红移.     

Crystallization and preliminary X-ray analysis of an anti-insect toxin BmK 16 fromButhus martensii Karsch scorpion

An excitatory anti-insect toxin from BmK scorpion, named BmK 16, has been purified and crystallized recently. Two crystal forms have been obtained by using ammonium sulfate as precipitant at different pH, one of which is single crystal. Diffraction data have been collected for the single crystal on a Mar Research 345 Image Plate. The analyses of the data show that the crystal can diffract to 0.28 nm resolution and belongs to the space group C2 with unit cell parameters a = 4.65 nm,b = 8.52 nm,c = 3.26 nm, α = γ = 90°, β = 110.5°. There are 2 molecules per asymmetric unit according to its unit cell volume and molecular weight.     

Fabrication and field emission performance of arrays of vacuum microdiodes containing CuO nanowire emitters grown directly on glass without a catalyst

Arrays of vacuum microelectronic sources are fabricated on a glass substrate using cupric oxide (CuO) nanowire emitters. The arrays of electron sources possess a microdiode structure, which can effectively induce field emission and control the delivery of emitted electrons to the anode in a triode-type device operation. A technique for precisely growing CuO nanowires at the centre of microcavities in an array without using a catalyst and at temperatures as low as 400°C is presented. Such a simplified fabrication procedure results in improved field emission performance from the array compared with previous vacuum microelectronic devices. Typical prototype devices have turn-on gate voltages as low as 169 V to give emission current densities of 10 μA/cm2 at the anode. The ratio of anode current to cathode current reaches ~0.85, and the maximum change in emission current density per volt is 1 μA/cm2. Electron emission from the arrays is stable and reproducible under either pulsed or direct current fields. These characteristics indicate that microgate-controlled CuO nanowire emitters may find application in practical devices.     

Preconcentration of vanadium(V) on crosslinked chitosan and determination by graphite furnace atomic absorption spectrometry

A new method is proposed for the preconcentration of vanadium(V) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(V) by CCTS was 97% at pH 4.0, and vanadium(V) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L⁻¹ chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium (V) was 4.8×10⁻¹²g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L⁻¹ is less than 3.6%. The method shows a good selectivity and high sensity, and it was applied to determination of vanadium(V) in oyster and water samples. The analytic recoveries are (97±5)%. Biography: Wu Wei (1975-), female, Master candidate, research direction: environmental & analytical chemistry.     

Optimizing Conditions of Enhancing Granule Sludge Concentration and Performance

An expanded granular sludge bed （EGSB） reactor was adopted to study the influence factors and rule of enhancing granular sludge concentration and performance. The experiment was performed at 33 ℃, pH 6.0-8.0 with continuous flow by adding proper quantity of nutritional trace elements. The results show that SLR was the key of steady operation of EGSB reactor. The increment of the granular sludge was influenced by volume loading rate （VLR）, liquid up-flow velocity and sludge loading rate （SLR）. Concentration of granular sludge increased rapidly when liquid up-flow velocity was over 0.94 m · h^-1 with SLR being at 1.0-2.0 d ^-1. With the propriety parameters： liquid up-flow velocity 2.52 m · h^-1, SLR 1.0-2.2 d^-1 and VLR 8.2-13.1 kg · m ^3 · d^-1, 23 days＇ continuous operation resulted in an increment by over 80% of granular sludge concentration in the EGSB reactor, plus good granular sludge property.     

金属Hf的电子结构和物理性质

依据金属单原子理论（ＯＡ） 确定了密排六方结构（ｈｃｐ） αＨｆ 的电子结构为［Ｘｅ］（５ｄｎ）０ ．３６８０（５ｄｃ）２．０４１ ４（６ｓｃ）１．４０６ ６（６ｓｆ）０．１８４０ ,通过计算得到了其势能曲线、晶格常数、结合能、弹性和热膨胀系数随温度的变化,对其体心立方结构（ｂｃｃ）和面心立方结构（ｆｃｃ）初态特征晶体和初态液体的电子结构进行了研究,分析了ｆｃｃ 结构的Ｈｆ 不能以纯组元的形式在自然界中存在的原因,得到了不同晶体结构Ｈｆ 的结构参数和性能参数,为金属Ｈｆ 及其相关材料的理论设计提供了完整的数据资料．     

金属元素镁高压属性的第一性原理研究

通过第一性原理计算方法，研究了金属元素镁在高压下的电子属性。电子性质的计算指出，镁的三个高压结构体心立方（bcc）、面心立方（fcc）和简单六角（sh）都是金属相结构，但其金属性比常压结构六角密堆（hcp）弱；通过与镁常压电子结构比较可知，d带贡献的增加以及p-d杂化的增强可能是高压下镁金属性降低的一个原因。镁高压fcc和sh结构的电子局域函数（ELF）通过与常压hcp结构以及高压fcc、sh结构的ELF比较，发现镁的这两个高压结构的价电子被高度排挤到晶格间隙区域，这一特殊现象与其他碱金属和碱土金属元素锂、钠、钾以及钙相似。     

Investigation on the coordinate structures of the rare earth metal complexes with edta and cydta ligands

0　IntroductionThegreatattentionhasbeenpaidtorareearthorradioactiverareearthmetalcomplexesfortheirvariousbiologicactivi ties[1 3] .Forexamples,theradioactiverareearthmetal1 53SmⅢ com plexeswerewidelyusedfortumourtherapyofbrain ,liver,lung ,heartandbonetissues[4 5] ;forrareearthmetalEuⅢandTbⅢemitinguniquefluorescence ,theircompoundswereappliedfordiagnosesofvariousdiseases[6 ,7] ;forrareearthmetalGdⅢcontainingthemosthigh spinsingleelectrons,itscomplexeswereusuallyusedforcontrastagentsofmag…     

Determination of epinephrine using poly (neurtral red) modified carbon fibre microelectrodes by anodic stripping voltammetry

Poly(neutral red) film modified carbon fibre microelectrodes offer substantial improvement in voltammetric sensitivity and selectivity towards epinephrine (EP). The poly (neutral red) film was electropolymerized by cycling the potential between −0.8 V and +0.8 V. The anodic stripping voltammetric response for EP was found to be dependent on accumulation time and potential. By using a poly(neutral red) film modified carbon fibre microelectrode with a 1 min preconcentration at −1.2 V in biological phosphate buffer solution (pH=7.4). a good linear relationship between the anodic stripping peak currents and EP concentrations was obtained in the range of 2.0×10⁻⁷⊂2.0×10⁻⁵ mol/L. The detection limit was up to 9.0 ×10⁻⁸ mol/L. Moreover, 400 times higher concentrations of vitamin C did not interfere with the measurement of EP. This method was used for determining EP concentrations in epinephrine hydrochloride injection solution with satisfactory results. Supported by the National Natural Science Foundation of China Tang Xiaorong: born in 1974, Master     

Synthesis of L-cystine bridgedbis（β-cyclodextrin） and its cooperative binding toward guest molecules

A novel p-cyclodextrin derivative, L-cystine bridged bis(β-cyclodextrin) 1 has been synthesized and characterized by 1H NMR, 13C NMR, IR, Raman and combustion analyses. Spectrofluorometric titrations have been performed in aqueous phosphate buffer solution (pH=7.20) at 25℃ to give the complex stability constants (Ks) and Gibbs free energy changes (-△G°) for the stoichiometric 1 : 1 inclusion complexation of 1 with four dyes. The binding abilities and molecular selectivities are discussed from the viewpoint of size/shape-fit and electrostatic interactions between hosts and guests. 2D ROESY investigation for the complexation between host and guest further confirms the cooperative binding of bridged cyclodextrin 1 with guest.     

Synthesis, crystal structure and properties of binuclear manganese complex [(bipy)2Mn2(μ-O)(μ-Ac)2(H2O)2](ClO4)2

Binuclear manganese complex [(bipy)₂Mn₂(μ-O)(μ-Ac)₂(H₂O)₂](ClO₄)₂ was synthesized by the reaction of MnAc₃ · 2H₂O with 2,2′-bipyridine in the HAc-NaAc buffer (pH = 4.0). X-ray diffraction result for the single crystal shows that the crystal is monoclinic, space group C₂/C, with a = 3.408 2(7),b = 0.864 4(2),c = 2.174 9(4) nm, β= 105.2∘, V=6.186(2) nm³, Z= 8. There are two very strong peaks of UV-Vis spectrum in the range of 400–600 nm, which are similar to those of Mn catalase and Mn ribonuleotide reductase extracted from organisms. Cyclic voltammogram shows that the complex in CH₃CN undergoes quasi-reversible one-electron reduction and oxidation at E_1/2=1.15V.     

Effect of CO<Subscript>2</Subscript> concentrations on the activity of photosynthetic CO<Subscript>2</Subscript> fixation and extracelluar carbonic anhydrase in the marine diatom <Emphasis Type="Italic">Skeletonema costatum</Emphasis>

The growth and activity of photosynthetic CO2 uptake and extracellular carbonic anhydrase (CAext) of the marine diatom Skeletonema costatum were investigated while cultured at different levels of CO2 in order to see its physio-logical response to different CO2 concentrations under either a low (30 靘ol·m-2·s-1) or high (210 靘ol·m-2·s-1) irradiance. The changes in CO2 concentrations (4—31 靘ol/L) affected the growth and net photosynthesis to a greater extent under the low than under the high light re-gime. CAext was detected in the cells grown at 4 mol/L CO2 but not at 31 and 12 靘ol/L CO2, with its activity being about 2.5-fold higher at the high than at the low irradiance. Photo- synthetic CO2 affinity (1/ K1/2(CO2)) of the cells de-creased with increased CO2 concentrations in culture. The cells cultured under the high-light show significantly higher photosynthetic CO2 affinity than those grown at the low-light level. It is concluded that the regulations of CAext activity and photosynthetic CO2 affinity are dependent not only on CO2 concentration but also on light availability, and that the de-velopment of higher CAext activity and CO2 affinity under higher light level could sufficiently support the photosyn-thetic demand for CO2 even at low level of CO2.     

Determination of crystal structure of omphacite

The chemical formula of omphacite was expressed with (MⅡ MⅠ ) (Si, AI)2O6. Cations that occupied the MⅡ site were large cations such as Ca or Na, and (Na/(Na+Ca)) ratio ranged from 0.2 to 0.8; the 6-coordinated MⅠ site accommodated cations such as Mg, Fe2+, Al, Fe3+ ,and(AI/(AI+Fe3+)) ratio was more than 0.5. Omphacite space groups reported were C2/ c, P2, P2/n, P2/c, cell parameters are α0 = 0.9600-0.9630 nm,b0 = 0.8750-0.8830 nm,c0 = 0.5230-0.5290 nm,β = 106°40′-107°10'. The sample was picked up from the eclogites in Zhucheng County, Shangdong Province. The intensity data were collected with the RIGAKU RASA Ⅱ -S four-circle single crystal diffractometer.The correct structure model was obtained by using the Patterson method and Fourier synthesis, SHELX-76 program, structure refinement with 905 independent diffraction points (| F0 |> 3σ |F0 |). After the structure parameter refinement, the R-factor reduced to 0.0515. The crystal structure analysis indicates that omphacite has a new space group-Pn space group.     

Electrochemical determination of trace amounts of lead (II) and cadmium (II) at a calix[6]arene modified carbon paste electrode

An electrochemical method for the simultaneous determination of lead(II) and Cadmium(II) with a calix[6]arene modified carbon paste electrode (CPE) has been developed. Pb²⁺ and Cd²⁺ were accumulated at the surface of the modified electrode via formation of chemical complexes with calix[6]arene, and reduced at 1.40 V. During the following anodic potential sweep, reduced lead and cadmium were oxidized, and two well-defined striping peaks appeared at about −0.60 V and −0.84 V. Compared with a bare carbon paste electrode, the calix[6]arene modified CPE greatly improves the sensitivity of determining lead and cadmium. The stripping peak currents change linearly with the concentration of Pb²⁺ 3.0×10⁻⁸–8.0×10⁻⁶ mol·L⁻¹ and with that of Cd²⁺ 6.0×10⁻⁸–1.0×10⁻⁵ mol ·L⁻¹. The detection limits of Pb²⁺ and Cd²⁺ are found to be 8.0×10⁻⁹ mol·L⁻¹ and 2.0×10⁻⁸ mol·L⁻¹, respectively. The modified carbon paste electrode was applied to determine trace levels of lead and cadmium in water samples. Comparing with that of atomic absorption spectrometry, the results suggests that the calix[6]arene modified CPE has great potential for the practical sample analysis. Foundation item: Supported by the National Natural Science Foundation of China (60171023) Biography: JI Xiao-bo (1980-), male, Master, research direction: electroanalytical chemistry.     

Preparation,crystal structure and quantum chemical investigation of [Li(NTO) (H2O)]

[Li(NTO)(H₂O)₂] was prepared by mixing the aqueous solution of 3-nitro-1,2,4-triazol-5-one (NTO) and lithium hydroxide. The crystal structure of [Li(NTO)(H₂O)₂] was determined by single crystal diffraction analysis. The crystal is monoclinic, space group P2₁/n with crystal parameters of a = 0.742 0(2) nm, b = 0.344 9(1) nm,c = 2.490 6(3) nm, β= 94.89(1)°, Z = 4,D _c , = 1.799 g cm⁻³,V = 0.635 nm³, μ = 1.591 cm⁻¹, F(000) = 392. The finalR is 0.051. The MNDO MO calculation shows that the coordinate bonds of title compound possess certain extent of covalent character. O₂ atom of NTO anion is bonded to Li atom; the nitro group will be lost first when NTO is decomposed.     

Crystal structure and surface photo-electric property of Mn（Ⅱ） coordination supramolecules

Two Mn（Ⅱ） coordination supramolecules, [Mn2（C8HTO2）4（phen）2（p-H20）] （1） and [Mn2（btec）（phen）2（H2O）6]·2H2O （2） （phen=1,10-phenanthroline, H4btec=1,2,4,5-benzenetetracarboxylic acid）, were synthesized by hydrothermal method. The crystal structures of the complexes were determined by X-ray single crystal diffraction. The result indicates that （1） and （2） are both binuclear Mn（Ⅱ） complexes. The existence of hydrogen bonds makes the binuclear complexes become further connected to coordination supramolecules, which possess 1D and 3D infinite structures respectively. The complexes were identified by IR, UV-Vis, surface photovoltage spectrum （SPS） and field-induced surface photovoltage spectrum （FISPS）. The results of SPS for the complexes indicate that they both exhibit positive surface photovoltage response bands in the range of 300-600 nm. The SPS phase spectrum and FISPS of complexes indicate that they show certain p-type semiconductor characteristic. However, the intensity, position and number of the SPV response bands are different obviously. The difference of the SPV response bands is mainly attributed to the different structures of the complexes and the different coordination environment of Mn（ll） in the two complexes. This paper discusses the action of hydrogen bonds in the construction of the supramolecule and the change on the surface photovoltage of complex in different coordination environment.     

Organic media enhanced spectrofluorimetric determination of L-ascorbic acid

A novel spectrofluorimetric method for the determination of L-ascorbic acid is proposed. It is based on the inhibition of L-ascorbic acid on the formation of 2,3-diaminophenazine, which is an oxidation product ofo-phenylenediamine catalyzed by laccase. The fluorescence (at λ_cx/λ_cm=464 nm /530 nnm) was enhanced strongly in the presence of organic media. The mechanism ofo-phenylenediamine oxidation reaction catalyzed by laccase in the presence of L-ascorbic acid is discussed. L-ascorbic acid is determined in the ethanol, 1,4-dioxane and acetone over the linear range of 4.0×10⁻⁷≈1.2×10⁻⁴ mol/L, 4.0×10⁻⁷≈8.0×10⁻⁵ mol/L and 4.0×10⁻⁷≈1.0×10⁻⁴ mol/L with a detection limit of 1.20×10⁻⁵ mol/L, 1.19×10⁻⁵ mol/L and 1.24×10⁻⁸ mol/L, respectively. The method has been successfully applied to the simple and rapid determination of L-ascorbic acid in pharmaceuticals and milk powder. Supported by National Natural Science Foundation of China and the Special Funds of State Education Committe for Doctorate Research Huang Zuyun: born in Aug. 1963. Ph.D