Investigation on LCST behavior of a new amorphous/crystalline polymer blend: Poly(n‐methyl methacrylimide)/poly(vinylidene fluoride)

The liquid–liquid phase‐separation (LLPS) behavior of poly(n‐methyl methacrylimide)/poly(vinylidene fluoride) (PMMI/PVDF) blend was studied by using small‐angle laser light scattering (SALLS) and phase contrast microscopy (PCM). The cloud point (T_c) of PMMI/PVDF blend was obtained using SALLS at the heating rate of 1 °C min^?1 and it was found that PMMI/PVDF exhibited a low critical solution temperature (LCST) behavior similar to that of PMMA/PVDF. Moreover, T_c of PMMI/PVDF is higher than its melting temperature (T_m) and a large temperature gap between T_c and T_m exists. At the early phase‐separation stage, the apparent diffusion coefficient (D_app) and the product (2Mk) of the molecules mobility coefficient (M) and the energy gradient coefficient (k) arising from contributions of composition gradient to the energy for PMMI/PVDF (50/50 wt) blend were calculated on the basis of linearized Cahn‐Hilliard‐Cook theory. The kinetic results showed that LLPS of PMMI/PVDF blends followed the spinodal decomposition (SD) mechanism. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 46: 1923–1931, 2008     

Conjugated polymers containing electron‐transporting,hole‐transporting,and light‐emitting units in the polymer main chain

Conjugated polymers containing electron‐transporting, hole‐transporting, and blue light‐emitting units were synthesized by Suzuki polycondensation. These copolymers exhibited excellent thermal and optical stability. Optical investigation indicated that the incorporation of the spirobifluorene units in the polymer main chain could markedly increase the effective conjugation length of polymers. Electrochemical studies showed that the incorporation of spirobifluorene unit could raise the electrochemical stability and improve the electron‐ and hole‐injecting abilities. The electroluminescent results also showed that the introducing of spirobifluorene units could significantly improve the device performance. © 2008 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 46: 1349–1356, 2008     

能量色散偏振X射线荧光光谱法测定生铁中锰和钛

探讨了应用能量色散偏振X射线荧光光谱仪测定生铁中锰和钛进行炉前快速分析的方法.对测定锰及钛时仪器的工作条件,试样的制备以及工作曲线的制作等因素作了较系统的试验,该方法所得测定结果与化学法测定结果或标样标准值相吻合,相对标准偏差小于1.5%,与化学法相比,锰和钛的测定时间由50 min缩短到2 min.     

A multi-detector integrated automation system of routine INAA

An integrated automation system of routine instrumental neutron activation analysis (INAA) with three HPGe detectors has been built at China Institute of Atomic Energy. This system is mainly composed of sample counting system, pneumatic transfer system, software control and analysis systems, etc. The characteristics include more than 200 samples can be controlled for a batch of INAA with three detectors simultaneously, sample counting position can be optimized automatically according to the counting dead time, the real-time tracking and the high consistency between the spectrum and counting sample are possible to be realized through radio frequency identification tag.

     

改性Y型分子筛对硫醇硫醚的吸附脱除研究

通过液相离子交换法制备了Cu(I)Y、Ni Y、Ce Y分子筛,以XRD、低温N2吸附-脱附、NH3-TPD、吡啶红外Py-FTIR等方法对其进行物性表征。利用固定床技术、WK-2D微库伦仪及硫化学发光检测GC-SCD色谱评价了改性分子筛对于硫含量300μg/g模拟油(含硫化合物二丙硫醚、环己硫醇和1-庚硫醇与壬烷配制)及HDS汽油的吸附脱硫性能。结果表明,吸附剂对模拟油和HDS燃料油品中硫醇硫醚具有吸附效果,且改性后的分子筛在吸附脱硫过程中,强的B酸对于吸附脱硫有负作用,会使油品中硫醇硫醚发生催化反应,聚合的大分子硫化物遮盖及阻塞吸附活性位点,从而使吸附剂不能够完全地吸附硫化物,造成吸附硫容较小,而弱L酸无催化活性对吸附脱硫有正面影响。     

Molecular hydrogen "pairing" interaction in a metal organic framework system with unsaturated metal centers (MOF-74)

Infrared (IR) absorption spectroscopy measurements of molecular hydrogen in MOF-74-M (M = metal center) are performed as a function of temperature and pressure [to 45 kTorr (60 bar) at 300 K, and at lower pressures in the 20-200 K range] to investigate the nature of H(2) interactions with the unsaturated metal centers. A small shift (～?-30 cm(-1) with respect to the unperturbed H(2) molecule) is observed for the internal stretch frequency of H(2) molecules adsorbed on the metal site at low loading. This finding is in contrast to much larger shifts (～?-70 cm(-1)) observed in previous studies of MOFs with unsaturated metal centers (including MOF-74) and the general assumption that H(2) stretch shifts depend on adsorption energies (FitzGerald et al., Phys. Rev. B 2010, 81, 104305). We show that larger shifts (～?-70 cm(-1)) do occur, but only when the next available site ("oxygen" site) is occupied. This larger shift originates from H(2)-H(2) interactions on neighboring sites of the same pore, consistent with the short distance between H(2) in these two sites ～2.6 ? derived from an analysis of neutron diffraction experiments of D(2)-D(2) at 4 K (Liu et al., Langmuir 2008, 24, 4772-4777). Our results at 77 K and low loading can be explained by a diffusion barrier against pair disruption, which should be enhanced by this interaction. Calculations indicate that the vibrational shifts do not correlate with binding energies and are instead very sensitive to the environment (interaction potential and H(2)-H(2) interactions), which complicates the use of variable temperature IR methods to calculate adsorption energies of specific adsorption sites.     

K2Fe2B2O7: A transparent nonlinear optical crystal with frustrated magnetism

A new noncentrosymmetric ferroborate crystal, K₂Fe₂B₂O₇, has been grown from high temperature melt. Structure solution from single crystal X-ray diffraction shows that the title compound crystallizes in a trigonal space group P321 with cell dimensions of a=8.7475(12) Å and c=8.5124(17) Å. In the structure, FeO₄ tetrahedron shares its three basal oxygen atoms with BO₃ triangles forming a two-dimensional layer in the ab plane and the layers are connected by the apical Fe-O bonds along the c direction. The crystal is transparent in the visible and near infrared region from 500 to 2000 nm with three pronounced absorption bands ascribed to d-d transitions of tetrahedrally coordinated Fe³⁺ ions. Though, structurally analog to K₂Al₂B₂O₇, the further twisting of the BO₃ groups between adjacent layers reduces its optical nonlinearity to a second-harmonic generation intensity of about 0.4 times that of KDP. Spin-glass behavior is observed at 20 K which is probably due to geometrically magnetic frustration of the triangular Fe net in the ab plane.     

Chemical composition and antifungal activity of essential oils of Thuja sutchuenensis, a critically endangered species endemic to China

The essential oils from leaves, twigs and stems of large trees and shrub-like trees of Thuja sutchuenensis were extracted by hydrodistillation and supercritical fluid extraction, and analyzed by GC and GC-MS. The essential oil composition differed significantly among the three organs, as well as between large trees and shrub-like trees. Furthermore, consistent with the eastern Asia-North American disjunct distribution of the genus, many differences in the essential oil composition between T. sutchuenensis and other Thuja species were apparent. The essential oils exhibited a certain degree of antifungal activity against six strains of human pathogenic fungi.     

Analysis of Para Red and Sudan Dyes in Egg Yolk by UPLC–MS–MS

Matrix solid-phase dispersion (MSPD) with alumina N as adsorbent has been used for extraction of para red, Sudan 1, Sudan 2, Sudan 3, and Sudan 4 dyes from egg yolk. The extracts were analyzed by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS–MS). Mean recovery for the five dyes ranged from 63.2 to 98.6%, with CV 0.55–10.00%. One sample was confirmed to contain 0.3 mg kg^?1 Sudan 4.     

X射线散射法测量超光滑平面

介绍了掠入射X射线散射法(GXRS法)测量超光滑表面的原理及基于商业用X射线衍射仪改造而成的实验装置。以3片不同粗糙度的硅片作为实验样品,分别应用一级矢量微扰理论和改进的Harvey-Shack理论对其散射分布进行处理,所得结果与原子力显微镜测量结果基本相符。分析了探测器接收狭缝的宽度和入射光发散度对实验结果的影响,随着探测器接收狭缝宽度和入射光发散度的减小,测量误差呈指数迅速减小。在所测量的空间频率范围内,功率谱密度（PSD）函数的误差随频率的增加而减小。