连续波核磁共振实验中外扫描测量法的改进

本文对连续波核磁共振实验中外扫描法测横向弛豫时间误差的主要来源进行了分析,对系统误差的大小进行了定量估算.在此基础上,对外扫描法中横向弛豫时间的测量提出了相应的改进措施,通过计算确定了共振信号半高宽测量时共振信号应在的位置.结果表明,外扫描法测量中,通过x方向的相位调节把共振信号移到偏离中心适当距离的位置上来测量其半高宽,可有效降低非线性扫描电压引起的系统误差.此外,通过对误差大小及共振信号测量位置的计算,能加深学生对横向弛豫时间及外扫描测量法原理的理解.

Effect of a Novel Nucleating Agent on Isothermal Crystallization of Poly（L-lactic acid）

The effect of a novel active nucleating agent(TBC8-eb) on the isothermal crystallization of poly(L-lactic acid) (PLLA) was studied by differential scanning calorimetry(DSC) and Fourier transform infrared spectroscopy(FTIR) . The analysis on kinetics demonstrates that TBC8-eb can not only accelerate the crystallization rate but also transform most of the original spherulite crystals of PLLA into sheaf-like crystals. Furthermore,the free energy of folding(σe) of PLLA and PLLA with TBC8-eb is 0.15 and 0.06 J·m-2,respectively,which suggests that the addition of TBC8-eb favors the regular folding of molecule chains in the crystallization of PLLA,improv-ing its crystallization rate. The FTIR results show that TBC8-eb can accelerate the conformational ordering of PLLA in the isothermal crystallization. The conformational ordering of PLLA nucleated with TBC8-eb begins with the interchain interaction of CH3,and then a short helix emerges where a couple of CH3 groups interact.

Solubilities of 1-Methyl-3-（3-sulfopropyl）-imidazolium Hydrogen Sulfate in Selected Solvents

Ionic liquid 1-methyl-3-(3-sulfopropyl) -imidazolium hydrogen sulfate([C3SO3HMIM][HSO4]) was synthesized and characterized by infrared spectroscopy(IR) ,nuclear magnetic resonance(1H and 13C NMR) and ultraviolet-visible(UV-Vis) spectra. Its thermal stability was also examined by thermogravimetric analysis(TGA) and a differential scanning calorimeter(DSC) . The mole fraction solubilities of [C3SO3HMIM][HSO4]) in 12 selected solvents(n-pentane,n-hexane,n-heptane,benzene,toluene,ethylbenzene,acetone,2-butanone,3-methyl-2-butanone,tetrahydrofuran,ethyl acetate and dichloromethane) in the temperature range from 289.15 to 363.15 K were meas-ured using a static analytical method and correlated with an empirical equation.

Investigation on specific heat capacity and thermal behavior of sodium hydroxyethyl sulfonate

The thermal decomposition process was studied by the TG–DTA analyzer. The results show that the decomposition process of sodium hydroxyethyl sulfonate consisted of three stages: the mass loss for the first, the second and third stages may be about the groups of CH_3CH_2OH, CH_3CHO and SO_2 volatilized, respectively. The decomposition residuum of three stages was analyzed by FT-IR, and the results of FT-IR agreed with the decomposition process predicted by theoretical weight loss. The specific heat capacity of sodium hydroxyethyl sulfonate was determined by differential scanning calorimetry(DSC). The melting temperature and melting enthalpy were obtained to be 465.41 K and 25.69 kJ·mol^(-1), respectively. The molar specific heat capacity of sodium hydroxyethyl sulfonate was determinated from 310.15 K to 365.15 K and expressed as a function of temperature.

Preparation and Characterization of Magnetic Resin Made from Chitosan and Cerium

In this study, the water-based ferromagnetic fluid and magnetic resin made from chitosan and cerium complex （MRCCC） were successfully prepared by using the chemical co-precipitation technique and by the reversed-phase suspension cross-linking polymerization. MRCCC presented uniform and narrow panicle size distribution as determined by the Laser Panicles Sizer. The Inductively Coupled Plasma-Atomic Emission Spectrometry （ICP-AES）, Fourier transform infrared spectroscopy （FT-IR）, differential scanning calorimetry （DSC） and X-ray powder diffraction （XRD） study demonstrated that there were iron and cerium existing in MRCCC. The movement of MRCCC under magnetic field proved its magnetic property. The swelling kinetics in water or solutions with different pH indicated that MRCCC could be applied in solutions with pH greater than 1.0. The ferromagnetic fluid particles were stable in MRCCC soaked in solutions with pH 〉2.0. In view of these results, MRCCC can be used as material for separation, clarification, adsorption, sustained release and hydrolysis activity.

Structure-Property Relations in xWO3-0.31P2O5-0.31B2O3-（0.38-x）Cs2O （0.01 ≤ x ≤0.28） Glasses by IR, UV and EPR Spectroscopic Studies

Glasses in the series of xWO3-0.31P2O5-0.31B2O3-（0.38-x）Cs2O （0.01 ≤ x ≤0.28） （G1-G4： x= 0.01, 0.1, 0.19, 0.28） were prepared by sol-gel method. Glassy phase in the samples were ascertained by powder X-ray diffraction pattern. Differential scanning calorimetry （DSC） traces of the samples show glass transition temperature Tg, in the range 247-253 ℃. IR spectra at 300 K of G1-G4 show the presence of [WO6], [WO4], [PO4]^3-, [PO3]^2-, [BO4]^＋, [BO3] units in the glass matrix. Observed electron paramagnetic resonance （EPR） lineshapes show two signals with very different intensities which are associated with W^5＋ （5d^1） and Mo^5＋ （4d^1） （impurity） paramagnetic sites. Signal with values ofg factors in the range 1.68 〈 g⊥ 〈 1.72 and 1.58 〈 gⅡ 〈 1.62 are due to W^5＋ ions present in axially distorted octahedral symmetry. The optical absorption spectra show that the W^5＋ ions have pyramidal coordination, involving a tungstyl ion WO^3＋ （C4v symmetry）. EPR and optical studies suggest the existence of blocks of octahedra linked by tungsten clusters.

Characterization and Desulfurization Possibilities of High Sulfur Gediz-Turkey Coal

Coal is one of the important energy sources, but it causes serious environmental problems such as air pollution, acid rain and greenhouse effects. Sulfur in coal is one of the responsibilities of these negative effects. Coal includes two types of sulfur： organic and inorganic. While inorganic sulfur can be completely removed with physical desulfurization methods, organic sulfur can be removed only by chemical desulfurization methods. But chemical methods are not only expensive but also difficult processes. Firstly in desulfurization, types of the sulfur content in coal should be well characterized. High sulfur Gediz-Turkey coal has been chosen to this study. This coal basin is located in the centre of the Turkey. In this study, characterization and desulfurization possibilities of high sulfur Gediz coal were investigated. For this purpose, several physical and chemical characterization methods such as proximate and ultimate coal analysis （ash, calorific value, volatile matter, moisture and sulfur analysis）, mineralogical and petrographic analysis, fourier transform infrared spectroscopy, scanning electron microscope were used. Results of these analysis are shown that Gediz coals include 3.15% pyritic sulfur and 2.89% organic sulfur. Removing pyritic sulfur from Gediz-Turkey coal with physical methods such as gravity and sink-float separation is not possible because pyrite particle has 1-2 micron liberation size in coal.

Polymorph and anisotropic Raman spectroscopy of Phz-Hca cocrystals

The nucleation and growth mechanism and polymorph-property correlations in the molecular cocrystal field are widely sought but currently remain unclear. Herein, a new wire-like morphology of phenazine(Phz)-chloranilic acid(H2ca) cocrystal(PHC) is demonstrated for the first time, and the self-assembly of Phz and H2ca is controlled to selectively prepare kinetically stable wires and thermodynamically stable plates. Specifically, low precursor concentration is beneficial for one-dimensional(1D) self-assembly along the [010] crystallographic direction, while only supersaturation can trigger 2D self-assembly along the [100] and [010] directions, respectively. This is understandable in terms of the(020) face showing the largest attachment energy(Eatt) and the(002) face possessing the smallest surface energy(Esurf). Moreover, anisotropic Raman spectra related to the mode symmetry and atomic displacements in two types of PHCs are revealed, and the same Raman-active vibrational bands of PHC wire and plate show different polarization responses, which is intrinsically ascribed to their different molecular orientations.Overall, this is the first case that morphologies of cocrystal are precisely tuned with comprehensive investigations of their anisotropic vibrational characteristics.