铑（Ⅲ）—碱性染料—高碘酸钾催化光度法测定痕量铑

在氯化钠－磷酸溶液中,铑（Ⅲ）催化高碘酸钾氧化碱性染料（乙基罗丹明Ｂ,丁基罗丹明Ｂ,耐尔蓝）褪色,反应速率与铑浓度呈线性的范围依次为０２～４０,０～４５和０～６０μｇ／２５ｍＬ,检出限依次为２２４×１０－１０,２８４×１０－１０和３８０×１０－１０ｇ／ｍＬ．本催化反应对铑（Ⅲ）或碱性染料均为一级反应．催化反应的表观活化能分别为６５２１,６３４１和６１０１ｋＪ／ｍｏｌ．考察了４０多种共存离子的影响,Ｏｓ,Ｒｕ,Ｉｒ干扰,其它贵金属、有色金属和铁不干扰．题示体系已用于某些催化剂和冶金产品中痕量铑的测定,结果满意     

Construction of expanders and superconcentrators using Kolmogorov complexity

We show the existence of various versions of expander graphs using Kolmogorov complexity. This method seems superior to the usual probabilistic construction. It turns out that the best known bounds on the size of expanders and superconcentrators can be attained based on this method. In the case of (acyclic) superconcentrators we attain a density of about 34 edges/vertices. Furthermore, related graph properties are reviewed, like magnification, edge‐magnification, and isolation, and we develop bounds based on the Kolmogorov approach. © 2000 John Wiley & Sons, Inc. Random Struct. Alg., 17: 64–77, 2000     

Reaktionen am metallischen Substrat: Einkristalle von Ni(NH3)2V2F8

Reactions at the Metallic Substrate: Single Crystals of Ni(NH₃)₂V₂F₈ Except for the main product (NH₄)₂[TaF₇] and some [Ni(NH₃)₆][TaF₆]₂, the new light green Ni(NH₃)₂V₂F₈ is obtained by the reaction of (NH₄)F with tantalum and vanadium (molar ratio of (NH₄)F : Ta : V = 36 : 6 : 1) at 400 °C in a sealed Monel ampoule (Cu32Ni68). The crystal structure (orthorhombic, Fmmm, Z = 4, a = 752.9(1), b = 762.9(1), c = 1307.6(2) pm) is related to that of (NH₄)[VF₄]. According to {Ni(NH₃)₂}_0,5[VF₄], corrugated layers of vertex-connected octahedra [VF_4/2F_2/1] are stacked in the [001] direction. Between these layers trans-{Ni(NH₃)₂} units are inserted so that Ni²⁺ enhances its coordination number to 6 by two times two F^– from the layers above and below.     

加速溶剂萃取-GPC纯化-气相色谱-质谱法测定油区土壤中的16种多环芳烃

为了排除背景干扰,使测定数据更加准确,先通过加速溶剂萃取和GPC纯化方法富集油区土壤中约16种多环芳烃, 再借助于气相色谱 质谱建立了高效、准确的分析方法。该方法对16种多环芳烃的相关系数在0.997以上,检出限为0.8~7.3 ng/mL,回收率为82.8％~94.2％,相对标准偏差为1.38％~8.86％。对实际样品的分析检测结果表明,本方法在油区土壤中的多环芳烃分析方面值得推广。     

Comprehensive inter‐laboratory calibration of reference materials for δ18O versus VSMOW using various on‐line high‐temperature conversion techniques

Internationally distributed organic and inorganic oxygen isotopic reference materials have been calibrated by six laboratories carrying out more than 5300 measurements using a variety of high‐temperature conversion techniques (HTC) a in an evaluation sponsored by the International Union of Pure and Applied Chemistry (IUPAC). To aid in the calibration of these reference materials, which span more than 125‰, an artificially enriched reference water (δ¹⁸O of +78.91‰) and two barium sulfates (one depleted and one enriched in ¹⁸O) were prepared and calibrated relative to VSMOW2 b and SLAP reference waters. These materials were used to calibrate the other isotopic reference materials in this study, which yielded:

Self-assembly and conformation of tetrapyridyl-porphyrin molecules on Ag(111)

We present a low-temperature scanning tunneling microscopy (STM) study on the supramolecular ordering of tetrapyridyl-porphyrin (TPyP) molecules on Ag(111). Vapor deposition in a wide substrate temperature range reveals that TPyP molecules easily diffuse and self-assemble into large, highly ordered chiral domains. We identify two mirror-symmetric unit cells, each containing two differently oriented molecules. From an analysis of the respective arrangement it is concluded that lateral intermolecular interactions control the packing of the layer, while its orientation is induced by the coupling to the substrate. This finding is corroborated by molecular mechanics calculations. High-resolution STM images recorded at 15 K allow a direct identification of intramolecular features. This makes it possible to determine the molecular conformation of TPyP on Ag(111). The pyridyl groups are alternately rotated out of the porphyrin plane by an angle of 60 degrees.     

Some solutions of the 3D Laplace equation in a layer with oscillating boundary describing an array of nanotubes with applications to cold field emission. II. Irregular arrays

As in the first part (J. Brüning, S.Yu. Dobrokhotov, D.S. Minenkov, 2011), we construct a family of special solutions of the Dirichlet problem for the Laplace equation in a domain with fast changing boundary. Using these solutions, we construct an analytic model of cold field electron emission from surfaces simulating arrays of vertically aligned nanotubes. Explicit analytic formulas lead to fast computations and also allow us to study the case of random arrays of tubes with stochastic distribution of parameters. We present these results and compare them with numerical approximations given in [1].     

Dynamic combinatorial libraries for the recognition of heavy metal ions

We present the use of hydrazone dynamic combinatorial libraries (DCLs) to identify macrocyclic receptors that are selective for alkaline earth metal ions over alkali metal ions. In particular, the toxic heavy metal ions Sr(2+) and Ba(2+) induce characteristic changes in the DCLs. Four macrocycles were isolated and characterised by LCMS, HRMS, NMR and X-ray crystallography; binding studies by UV-Vis spectroscopy confirm the selectivity observed in the DCLs.     

Surface investigation of intermetallic PdGa(111)

The intermetallic PdGa is a highly selective and potent catalyst in the semihydrogenation of acetylene, which is attributed to the surface stability and isolated Pd atom ensembles. In this context PdGa single crystals of form B with (111) orientation were investigated by means of X-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS), scanning tunneling microscopy (STM), X-ray photoelectron diffraction (XPD), and low-energy electron diffraction (LEED) to study the electronic and geometric properties of this surface. UPS and thermal desorption spectroscopy (TDS) were used to probe the chemisorption behavior of CO. The PdGa(111) surface exhibits a (1 × 1) LEED and a pronounced XPD pattern indicating an unreconstructed bulk-truncated surface. Low-temperature STM reveals a smooth surface with a (1 × 1) unit cell. No segregation occurs, and no impurities are detected by XPS. The electronic structure and the CO adsorption properties reveal PdGa(111) to be a bulk-truncated intermetallic compound with Pd-Ga partial covalent bonding.     

On the Nodal Count for Flat Tori

We give an explicit formula for the number of nodal domains of certain eigenfunctions on a flat torus. We apply this to an isospectral but not isometric family of pairs of flat four-dimensional tori constructed by Conway and Sloane, and we show that corresponding eigenfunctions have the same number of nodal domains. This disproves a conjecture by Brüning, Gnutzmann, and Smilansky.