Synthesis of non-equilibrium PtxOs1−x Solid solutions. Crystal structure of [Pt(NH3)4][OsCl6]

Several non-equilibrium solid solutions belonging to the platinum-osmium systems Os_0.9Pt_0.1, Os_0.8Pt_0.2, Os_0.5Pt_0.5, Os_0.7Pt_0.3, Os_0.75Pt_0.25 are prepared and studied. The thermal decomposition of [Pt(NH₃)₄][OsCl₆] in the hydrogen and helium atmosphere is investigated. It is found that the Pt_0.5Os_0.5 solid solution develops through the formation of (NH₄)₂[OsCl₆] and a metallic phase based on Pt. The crystal structure of a double complex salt [Pt(NH₃)₄][OsCl₆] is studied (X8-APEX Bruker, 1508 independent reflections, R = 2.04%). Crystal data for PtOsN₄Cl₆H₁₂ are: a = 11.6216(5) Å, b = 11.0016(5) Å, c = 10.3819(5) Å, V = 1327.4(1) ų, space group Cmca, Z = 4, d _x = 3.333 g/cm₃. The coordination polyhedron around Os is octahedral: 〈Os-Cl〉 2.357 Å, ∠Cl-Os-Cl 89.5–90.5°, while around Pt it is square-planar: Pt-N 2.046 Å, ∠ N-Pt-N 89.59° and 90.41°.     

Ag/ZrO2催化剂上的1,2-丙二醇选择性气相氧化反应

采用浸渍法制备了一系列Ag/ZrO₂催化剂, 考察了Ag/ZrO₂催化剂对1,2-丙二醇选择性氧化合成丙酮醛反应的催化性能. 实验结果表明: 在原料气配比为V(N₂)∶V(O₂)＝300∶19, n(O₂)/n(alcohol)＝1.2, 反应物液时空速为3.2 g/(g•h), 反应温度为673 K时, 1,2-丙二醇选择性氧化合成丙酮醛反应的转化率为95.7%, 选择性为55.3%, 高于传统电解银催化剂. UV-Vis DRS和XPS的研究结果表明: 在Ag/ZrO₂催化剂上存在大量的Ag^＋和Ag_n^δ＋有利于促进催化活性的提高.     

纳米级TiO2粉体的制备研究——Ⅱ.絮凝剂及其浓度的影响

采用溶胶-凝胶-超临界流体干燥(SCFD)法制备纳米级TiO₂超细粉，详细考察了不同絮凝剂及其浓度对TiO₂织构和结构性质的影响。结果表明，利用强碱溶液作为絮凝剂，浓度为5 mol·L^-1是制备大孔高比表面TiO₂超细粉较为适宜的条件。     

Untersuchungen im System LaI2/H2: Phasenverhältnisse und Fehlordnung

Investigation of the LaI₂/H₂ System: Phase Relations and Stacking Disorder Heating of LaI₂ under 1 bar hydrogen pressure to 650 °C leads to light gray LaI₂H_0.95(3), accompanied by a structural change from tetragonal to hexagonal. Sharp reflections in the XRD pattern can be indexed in P6₃/mmc with a = 4.2158(7)Å and c = 15.508(3)Å, however, diffuse reflections indicate the presence of stacking faults in the structure, which correspond to a polytypic intergrowth of MoS₂ and NbS₂ type structural fragments. Increasing the reaction temperature to 730 °C results in a better defined diffraction pattern with the peak positions close to those of the 2H‐NbS₂ structure type. An X‐ray powder study of the samples LaI₂H_n proved the miscibility gap between LaI₂ and LaI₂H_n (0 ≤ n ≤ 0.5) in agreement with previous results. With decreasing H‐content of the homogeneous phase the lattice parameters change in opposite direction, a increasing to 4.236(1)Å and c decreasing to 15.39(2)Å for the lower limit.     

固固相反应合成牛磺酸水杨醛钾与锑、铋的配合物

合成了牛磺酸水杨醛钾,并采用室温固固相反应法合成了牛磺酸水杨醛钾与三氯化锑和三氯化铋的配合物,其组成为:K2MC18H20O8N2S2 (M = Sb, Bi)。两种配合物的晶体结构均属于单斜晶系,锑配合物的晶胞参数为:a = 1.2869 nm, b = 1.7636 nm, c = 1.9917 nm, β= 93.79埃活榕浜衔锏木О问篴 = 1.4770 nm, b = 2.0334 nm, c = 2.0149 nm, β= 94.05。红外光谱表明N、Cl原子参与了配位,中心离子的配位数为5。     

Magnesium substitution in Nd0.7Sr0.3MnO3

Magnesium substitution in Nd_0.7Sr_0.3MnO₃ has been studied by neutron powder diffraction. Polycrystalline samples of nominal compositions Nd_0.7Sr_0.3Mn_1−yMg_yO₃ with y=0.0, 0.1, 0.2 and 0.3 were synthesized by the standard solid-state reaction method. Rietveld refinements of the neutron powder diffraction data showed that all samples had distorted perovskite structure of orthorhombic symmetry. Mg initially preferred to substitute for Nd and only at Mg concentration greater than 0.1, a substantial substitution for Mn occurred. Our study also showed that Mg-substitution did not change the crystal structure of Nd_0.7Sr_0.3MnO₃.     

Crystal structures and phase transition in the system SrTiO3-La2/3TiO3

The distribution of A-site cations in the perovskite system La_xSr_1−3x/2TiO₃ depends on the concentration of La³⁺ ions and associated vacancies. For small x (x?0.2), the substitutions are expected to be random. For x?0.55, the cations are ordered in such a way that successive layers of A-sites are occupied to greater and lesser degree, and this ordering drives a tetragonal distortion. For x from about 0.3 to 0.5, the X-ray patterns show diffuse peaks indicative of similar ordering, but this is not long-range order and no tetragonal distortion results. The lower temperature structures also exhibit out-of-phase tilting of the TiO₆ octahedra, setting in at temperatures varying linearly with composition from 105 K for x=0, to about 650 K at x=2/3.     

高砷低金银的铅阳极泥中银的冶炼

本文报导了将纯碱加入砷含量高的铅阳极泥熔炼成贵铅，用硝酸溶解，硫氰酸盐沉淀，再用锌粉还原得银的方法。从而避免砒霜挥发。     

Chemical, sensory and microbiological changes of gamma irradiated coconut cream powder

A study was carried out to determine optimum decontamination dose for a locally manufactured coconut cream powder. Samples were gamma irradiated (0–15 kGy) and ageing process was achieved using GEER oven at 60 °C for 7 days, which is equivalent to one-year storage at room temperature. Iodine value (IV), ranging from 4.8 to 6.4, was not affected by radiation doses and storage, however peroxide value and thiobarbituric acid (TBA) generally increased with radiation doses. In most samples, peroxide value (meq/kg) reduced after storage, whilst the TBA (mg malonaldehyde/kg), indicator for product quality, slightly increased. The sensory evaluation conducted using 25 taste panellists indicated that scores on odour, creamy taste and overall acceptance for all irradiated samples at more than 5 kGy were significantly lower (P<0.05) than the control. However, the panellists could not detect any significant differences among the irradiation doses (P>0.05). All stored products were significantly different in colour, creamy taste, odour and overall acceptance (P<0.05) when compared to the non-stored non-irradiated control. Microbiological count of the samples prior to irradiation was in the range of 1×10²–1.7×10³ cfu/g with no detection of Salmonella sp. and Escherichia coli. No microbial colonies were detected after irradiation. Based on the TBA and overall sensory acceptance, gamma irradiation of 5 kGy was found to be the optimum dose and lower doses can be considered to decontaminate coconut cream powder.     

Methyltriethoxysilane-derived sol-gel coatings doped with silver metal particles

Silica sol-gel films were prepared by dipping, starting from an acid catalyzed solution of methyltriethoxysilane (MTES) and tetraethoxysilane (TEOS). Silver metal nanoparticles were produced in the silica layer by introducing in the sol-gel precursor solution AgNO₃ or AgClO₄·H₂O. The silver ions were thermally reduced in air at 800°C, giving an intense yellow coating film. The silver metal particles were observed by transmission electron microscopy and X-ray diffraction. The diameter of the silver particles was found to be about 10 nm. Absorption measurements in the UV-Vis were used to evaluate the volume fraction of silver colloids embedded in the silica layer.