Purification by solid layer melt crystallization

The application of solid layer crystallization techniques in industry is arousing ever more interest. One reason is the increasing demand for ultrapure products, and another is the energysaving potential of this separation technology.This article examines solid layer melt crystallization as concerns its purification efficiency. The crystallization process was carried out in two different modes, whereby the process parameters were varied and post-crystallization treatments were additionally applied. The experimental results were used as the basis for a mathematical fit of a semi-empirical expression which predicts the purification efficiency. It was used for a design of different multistage plants, which operate with different crystallization strategies. One result is that a comparable product quality is attainable with a simple process technique in combination with post-crystallization treatments, instead of a more complicated and therefore more expensive process technique.The authors wish to acknowledge support by the EU (JOULE program), which helped attainment of some results presented here.     

The identification of tricyclic neuroleptics and sulphonamides by high-performance thin-layer chromatography

Circular high-performance thin-layer chromatography (HPTLC) has been used to differentiate a series of twelve tricyclic neuroleptics, using both normal phase and reverse phase procedures. The use of normal phase systems also allows the resolution of geometric isomers of chlorprothixene, clopenthixol and flupenthixol. Thirteen sulphonamides and Trirnethoprim may also be distinguished using HPTLC.     

The mean spherical model in a random external field and the replica method

We provide a quick elementary solution of the mean spherical model in a random external field. This also allows an immediate proof of the self-averaging property of the free energy. We calculate the free energy by means of the replica method, i.e., for any (not necessarily integer) replica numbern, and show that when a phase transition occurs the limits andn 0 are not interchangeable.     

Mode selective directional couplers for overmoded waveguide systems

Two types of directional couplers for transverse electric (TE) modes are described: short and multihole couplers, respectively. They selectively pick one mode out of a mode mixture in an overmoded circular waveguide system. Unwanted modes are either statistically kept at low level or are suppressed by destructive interference in the coupling waveguide. Mode selectivity and directivity in multihole couplers oscillate up and down with an increasing number of holes, finally reaching a minimum of approximately 20 dB, unless there are competing modes with rational fractions of the beat wavelength. A multihole coupler for the TE₀₂ mode (28 GHz, 63.4 mm waveguide diameter, 41 holes) and a length of 1.6 m shows a calculated directivity of 68 dB and suppresses the unwanted modes TE₀₁ with 34 dB (24 dB), TE₂₂ with 37 dB (45 dB), and further modes TE_m (<5, m<6) with 17 dB to 34 dB in forward direction (figures in parentheses are for unwanted modes propagating in backward direction).A short directional coupler for the TE₀₁ mode (28 GHz, 63.4 mm waveguide diameter) with 16 holes and a length of 230 mm shows a directivity of 55 to 100 dB between 27.9 and 28.1 GHz, suppressing the TE₀₂ mode with 35 to 80 dB, the TE₀₃ mode with 30 to 65 dB, and the TE₂₂ mode with 30 to 70 dB.     

Studies on the Binding Mode of Pinacyanol Chloride to Nucleic Acids

The interaction of pinacyanol chloride(PC) with nucleic acids has been investigated by a series of experiments.Extensive hypochromism,appreciable peak shifts,isosbestic points and new peaks of the product of binding to nucleic acids in the spectra were observed.They showed that the interaction between PC and nucleic acids occurred.The results from absorption spectra of DNA,DNA melting,electrophoresis and fluorescence polarization studies have indicated that PC binds to DNA in nonintercalative way.Consistent with the nonintercalation,the studies of fluorescence titration and absorption titration specified that the binding of PC to nucleic acids occurred by an outside stacking binding,in which nucleic acids served for acting templates,The fact that the new absorption peaks of bound PC at ca,485nm are just close to the absorption bands of Haggregate of PC at high concentrations without DNA further supports the outside stacking binding mode,In addition,other evidence indicated that the interaction between PC and nucleic acids is not purely electrostatic.     

An investigation of microbore reverse-phase columns containing 3 μm packing materials

A procedure for packing 15 cm × 1 mm id reverse-phase microbore columns with 3 μm silicas obtained from different manufacturers is described. The speed of analysis and detection limits are compared to those obtained with a 50 cm × 1 mm id column packed with 10 μm ODS. The effect of detector time constant on the system, and flow rates on column efficiency are also examined.     

邻位吡啶自由基多通道分解反应的动力学和反应机理研究

Utilizing Gaussian94 program package, all species involved in decomposition reactions of o-pyridyl radical were optimized fully at B3LYP/6-311＋＋G^＊＊ level. Intrinsic reaction coordinate calculations were employed to confirm the connections of the transition states and products, and transition states were ascertained by the number of imaginary frequency （0 or 1）. The reaction mechanism was elucidated by the vibrational mode analysis and electronic population analysis, and the reaction rate constants were calculated with transition state theory.     

A Cu(Ⅱ) Complex with IM-MeImz-к2 N,O Mode in [Cu(IM-MeImz)2]·(SCN)2: Synthesis, Crystal Structure and Magnetic Properties

A new copper(Ⅱ) compound with imino nitroxide radicals [Cu(IM-MeImz)2]·(SCN)2 (IM-meImz =2-(5-methylimidazol-4-yl)-4,4,5,5-tetramethyl-2-imidazoline-1-oxyl) has been synthesized and characterized structurally and magnetically. It crystallizes in monoclinic, space group P21/c with a = 9.3604(7), b = 10.3012(7), c = 16.6684(12) (A), β = 105.0290(10)°, V = 1552.25(19)(A)3, C24H34CuN10O2S2, Mr = 622.27, Z = 2, Dc = 1.331 g/cm3, μ(MoKα) = 0.876 mm-1, F(000) =650, the final R = 0.0374 and wR = 0.1079. X-ray analysis demonstrates that the IM-MeImz ligand is coordinated to the copper(Ⅱ) ion as an unusual didentate chelate with a κ2 N(MeImz),O(IM) mode in the complex. The square-planar coordination sites at Cu(Ⅱ) are occupied by two O and two N atoms from the imino nitroxide radicals. The complex molecules are connected as a onedimensional polymer structure by intermolecular interactions. Magnetic measurements show that there are intramolecular antiferromagnetic interactions between the Cu(Ⅱ) ion and radicals.     

Prediction of retention time of phenols in liquid chromatography

The chromatographic behavior of phenols in reversed-phase mode liquid chromatography differs from that of non-ionic compounds such as alkyl alcohols, alkylbenzenes, halogenated benzenes, polyaromatic hydrocarbons, and aromatic acids. Therefore, the retention times of 61 phenols were measured in a system of an octadecyl bonded silica gel and acetonitrile/water mixtures. The logarithm of the capacity ratio (log k') was found to be a linear function of the hydrophobicity (log P) in acidic acetonitrile/water mixtures. This result was applied to a different octadecyl bonded silica gel. Eight phenols were selected as standard compounds, and their log k' values were measured in 0.05 M phosphoric acid in 10 to 90% acetonitrile/water mixtures. An empirical polynomial relation was obtained between the concentration of acetonitrile and the slope of the log k' vs log P curve. Finally the capacity ratio of all phenols were calculated in given eluents by the equations derived from the measurements of standard compounds and the calculated log P values. The difference between predicted capacity ratios and measured ones was within 10%.