Flow-Injection Spectrophotometric Determination of Diclofenac or Mefenamic Acid in Pharmaceuticals

 Two flow injection (FI) spectrophotometric methods are proposed for the determination of diclofenac (DCF) or mefenamic acid (MF) in bulk samples and pharmaceuticals. Both methods are based on the reaction of DCF or MF with potassium ferricyanide in a sodium hydroxide medium. The absorbance of the orange products obtained is measured at 455 nm for DCF and 465 nm for MF. The corresponding calibration graphs are linear over the range 0.20–20.0 mg L⁻¹ for DCF and 1.00–100 mg L⁻¹ for MF, while the limits of detection were 0.05 and 0.18 mg L⁻¹, respectively. Received March 27, 2000. Revision November 15, 2000.     

意识分析的两种基本形态—兼论通向超越论—发生现象学的莱布尼茨道路

通常意义上的意识现象学是指意识体验或意识行为的现象学。胡塞尔一生在公开发表著作中所做的意识分析,绝大多数都是对意识体验的静态结构的现象学分析。但在胡塞尔一生的讲座稿和研究手稿中,他自1905年开始就已经进行意识发生结构的分析。这一意识分析已经不再局限于意识体验分析,而是自1916年起就明确地指向意识能力或意识权能的分析。在这个方向上,意识权能现象学与功能心理学和无意识理论的研究并行不悖,但具备自己在方法和内容方面的鲜明特色和显著成果。     

Monoclinic Low-Temperature Polymorph of Cesium Nitrate

A new CsNO₃ polymorph with space group P2₁/c, Z = 4, a = 4.5699(9) Å, b = 11.1871(10) Å, c = 9.1484(18) Å, β = 131.24(3)° has been prepared by crystallization from a mixture of water and DMSO. Flat triangles NO₃ are located in the (010) and (020) planes between the layers formed by coordination polyhedra of Cs atoms in the (040) plane. In contrast to the previously known low-temperature polymorph, the new modification is characterized by the crystal equivalence of all Cs and NO₃ groups.     

Forms of Rh(III) in Nitric Acid Solutions

The forms of Rh(III) in nitric acid solutions are studied by ¹⁴N, ¹⁵N, ¹⁷O, and ¹⁰³Rh NMR and electronic absorption spectra. At HNO₃concentrations below 5 mol/l, rhodium mainly exists as low-nuclear oligomers with a bridging fragment Rh(-OH)(-ONO₂)Rh; terminal positions of the central atoms are occupied by water molecules. It was found that the isotopic equilibrium ¹⁴NO^– ₃/¹⁵NO^– ₃of the bridging ligand sets in at an abnormally high rate, at which the isotopic exchange H₂ ¹⁷O/H₂ ¹⁶O of the terminal ligands also occurs in the dimers and trimers. The formation of low-nuclear oligomers is a common feature of Rh(III) complexes in aqueous solutions with ligand deficiency in the system. The possibility of isolating rhodium from nitric acid solutions using different methods is predicted.     

单斜仲钨酸铵热分解的热化学测定

在钨的冶炼过程中,仲钨酸铵是必须的中间原料 .从溶液中结晶仲钨酸铵时,根据结晶条件的不同,可以得到不同类型的结晶 [1].一般在较低的温度时（低于 323 K）,得到三斜仲钨酸铵 (NH4)10H2W12O42· 10H2O,在较高温时（高于 323 K）,得单斜仲钨酸铵 (NH4)10H2W12O42· 4H2O.工业生产中,单斜仲钨酸铵是常见的产品 .仲钨酸铵的质量直接决定钨粉的质量,因此仲钨酸铵热力学性质对于控制其结晶条件及结晶的热分解条件具有重要的指导意义 .但迄今,很少有关于单斜仲钨酸铵的热力学性质的报导 .本文用双子型热导式微量热量计,根据单斜…     

单斜仲钨酸铵热分解的热化学测定

The heat of the thermal decomposition of monoclini c ammonium paratungstate, (NH4)10H2W12O42•4H2O, was measured in a HT-1000 microcalorimeter using three-step calorimetry and suitable thermochemical cycle. The standard enthalpy of the thermal decomposition reaction at 298.15 K and the standard enthalpy of formation at 298.15 K for monoclinic ammonium paratung-state were obtained to be (430.1± 10.2) kJ•mol－ 1 and－ (13 423.7±14.8) kJ•mol－ 1, respectively.     

Monoclinic Cu2Se3Sn

A previously unknown modification of dicopper(I) triselenostannate(IV), Cu₂Se₃Sn, has been obtained from the Cu₂Se–SnSe₂ quasi‐binary system and investigated using X‐ray single‐crystal diffraction. The Se atoms are stacked in a closest‐packed arrangement with the layers in the sequence ABC. The Cu atoms occupy one‐third of the tetrahedral interstices, whereas the Sn atoms are located in one‐sixth of the tetrahedral interstices. All the atoms occupy general positions. The structure possesses pseudo‐inversion symmetry. The Cu₂Se₃Sn structure investigated in this paper (96 atoms per unit cell, ordered distribution of Cu and Sn over 12 cation positions) is a superstructure of the reported cubic (eight atoms per unit cell, random distribution of Cu and Sn over one cation position) and monoclinic (24 atoms per unit cell, ordered distribution of Cu and Sn over three cation positions) modifications.     

Preparation and Crystal Structures of Two Polymorphic Forms of Bupropion Hydrobromide

Two polymorphic forms (forms I and IV) of antidepressant bupropion hydrobro- mides were prepared and characterized by powder X-ray single-crystal diffractometer. Lots of commercial substances may consist of form I. Form I crystallizes in the triclinic system, space group P1 with Z = 2, a = 7.6943(8), b = 7.9347(9), c = 13.8558(15) , α = 85.971(3), β = 85.619(2), γ = 65.974(3)°, V = 769.66(14) 3, Dc = 1.384 g/cm3, formula C13H19ClNOBr, F(000) = 328, μ = 2.83 mm-1, the final R = 0.0579 and wR = 0.1282 for 1756 observed reflections with I > 2σ(I). Another polymorphic form, Ⅳ, belongs to the orthorhombic system, space group Pbca with a = 8.6365(3), b = 12.4167(4), c = 27.7299(9) , Z = 8, V = 2973.67(17) 3, Dc = 1.432 g/cm3, formula C13H19ClNOBr, F(000) = 1312, μ = 2.93 mm-1, the final R = 0.044 and wR = 0.1093 for 2018 observed reflections with I > 2σ(I). In the crystal structure of the two polymorphic forms, expected proton transfer from HBr to amino group of bupropion molecule occurs and intramolecular and intermolecular hydrogen bonds N–H···r are formed. These interactions result in hydrogen-bond dimers in these two forms. The bupropion molecule adopts different conformations in the two investigated solid state modifications.     

Features of Some Carbonium Ion Reactions Occurring on Acid Forms of Faujasite

The gas phase alkylation of isobutane with butenes and the cracking of cumene over zeolite catalysts show oscillating behavior. The oscillating is described in terms of competing oscillatory absorption phenomena. The formation of coke is examined as one of the competibehavior ng processes in both reactions.     

两种天然齐墩果酸皂苷的合成

3-O-[β-D-Glucopyranosyl-（1→3）-α-L-arabinopyranosyl]-oleanolic acid-28-O-[β-D-glucopyranosyl] ester 1 was synthesized concisely by a convergent strategy. Using stepwise fashion for the synthesis of saponin 2, 3-O-{[β-D-glucopyranosyl-（1→2）]-[α-L-arabinopyranosyl-（1→3）]-α-L-arabinopyranosyl）-oleanolic acid-28-O-（β- D-glucopyranosyl） ester, an abnormal phenomenon, that the terminal arabinosyl residue took the ^1C4 conformation instead of typical ^4C1 form, was observed. Deprotection or heating could not resume the normal conformation, which resulted in the product of 2＇ not 2.     

含苯环亲水共聚物形态及溶液荧光

研究含芳环（生色团）的亲水性高分子对于了解高分子结构和性质之间的关系，开发新型发光材料很有意义[1.2]．前文[3.4]借报道了N-乙烯基咋冷丙烯酸共聚物（NVC－AA）的合成及发光性能研究，本文报道含苯环亲水高分子苯乙烯一丙烯酸共聚物（ST－AA）的微观结构与荧光特性?..