用气相色谱法测定轻苯干点

研究用气相色谱法代替蒸馏法测定不含萘的轻苯干点。轻苯中1，3，5－三甲苯、1，2，4－三甲苯和茚的色谱峰高之和与轻苯的干点呈线性关系，回归方程为Y＝0.521X-69.2954，线性范围为130－153℃，相关系数为r=0.9997。该方法的相对标准偏差为3.98%；经F检验和t检验证明，该方法与蒸馏法测定结果无显著性差异。     

MEASUREMENTS OF CHAIN INTERPENETRATION OF POLYMER GLASSES

The concept of entanglement provides the basis of our current understanding of the flow behavior of polymer melts, Current techniques developed to investigate the degree of interpenetration of polymer chains only provide indirectly the information of the degree of entanglement in a relatively large scale （several to tens of nanometer）. In this article, we report ^1H-NMR spectroscopy with dipolar filters under fast magic angle spinning for probing chain interpenetration of polymer glasses at the molecular level.     

HEMA-NVP-St三元共聚体系研究Ⅲ.均化剂对共聚物组成均一性的影响

用溴化钾-溴酸钾滴定法测定双键含量,元素分析法测定共聚物组成。讨论了HEMA-NVP-St三元共聚体系在不同反应程度时共聚物组成的变化,以及在此三元共聚体系中引入均化剂后,少量均化剂对共聚体系组成均一性的影响。发现在HEMA-NVP-St三元共聚体系中加入均化剂,对共聚反应的反应动力学影响不大,但对共聚物的组成均一性有较大影响。它的加入使三元共聚物中的链节比分布(即不同反应程度时,产物的累积平均组成)向较均一的方向发展。结合红外光谱、电子显微镜等实验证据,从微观结构上探讨了约化剂的作用。阐明均化剂改善了反应体系的相容性,从而得到组成分布较为均一的共聚产物。     

Preparation and Photocatalytic Characterization of Nanoporous TiO2

Nanoporous TiO2 photocatalysts were prepared by use of controlled drying method with surfactants. The surface area and porous properties are dependent on the chain length of incorporated surfactant cation. The TiO2 materials prepared in the presence of surfactant molecules during the gel formation exhibit much higher photocatalytic activity than that prepared in the absence of surfactants.     

The first metal (Nd3+, Mn2+, and Pb2+) coordination compounds of 3,5-dinitrotyrosine and their nonlinear optical properties

The reactions of 3,5-dinitrotyrosine (H2DNTY) with Nd(NO3)3.6H2O, Mn(ClO4)2.6H2O, and Pb(OAc)2 afforded three homochiral compounds: discrete [Nd(Hdnty)2(NO3)(H2O)5].3H2O (1) and two- and three-dimensional coordination polymers, [Mn(Hdnty)2] (2) and [Pb(dnty)(0.5 H2O)] (3), respectively. The Nd atom in 1 displays a tricapped trigonal prism and supramolecular weak interactions, such as pi-pi stacking and H-bonds, between amino and nitro groups result in the formation of a three-dimensional network through these interactions. 2 has a two-dimensional square-grid topological net while 3 has the first three-dimensional homochiral ThSi2 net. To the best of our knowledge, these are the first metal coordination compounds with 3,5-dinitrotyrosine. Preliminary second harmonic generation (SHG) investigations indicated that 1 and 2 are SHG active with estimated responses 5 and 6 times larger than that of urea, respectively, while 3 is SHG non-active (obeying the Klainman symmetry requirement). Strong enhancement of their SHG efficiency, compared with H2DNTY, may be due to 1) the addition of a good donor-pi-acceptor organic chromophore into the compound resulting in superior qualities of both inorganic and organic materials and 2) the H-bonds that persist in them. Crystal data: 1: C18H32N7O25Nd, Mr = 890.75 g mol(-1), monoclinic, P2(1), a=7.0179(7), b=27.060(3), c=8.3097(8) A, alpha=gamma=90.00, beta=95.646(2) degrees , V=1570.4(3) A(3), Z=2, rho(calcd)=1.884 Mg m(-3), R(1)=0.0489, wR(2)=0.1223, mu=17.67 mm(-1), S=0.811, Flack value=0.003(13); 2: C(18)H(16)N(6)O(14)Mn, M(r)=595.31 g mol(-1), orthorhombic, P2(1)2(1)2, a=8.4381(14), b=13.639(2), c=19.697(3) A, alpha=beta=gamma=90.00 degrees , V=2266.9(6) A(3), Z=4, rho(calcd)=1.744 Mg m(-3), R(1)=0.0866, wR(2)=0.2030, mu=6.72 mm(-1), S=1.095, Flack value=0.02(6); 3: C(9)H(8)N(3)O(7.5)Pb, M(r)=485.37 g mol(-1), tetragonal, P4(1)2(1)2, a=12.8136(12), b=12.8136(12), c=14.931(2), alpha=beta=gamma=90.00 degrees , V=2451.5(5) A(3), Z=8, rho(calcd)=1.885 Mg m(-3), R(1)=0.0564, wR(2)=0.1323, mu=6.942 mm(-1), S=0.878, Flack value=0.03(2). For space group P4(3)2(1)2: R(1)=0.0672, wR(2)=0.1656, S=1.034, Flack value=1.02(3); this suggests the chosen space group P4(1)2(1)2 is correct.     

INDUCTION OF DNA-PROTEIN CROSS-LINKS IN CHINESE HAMSTER CELLS BY THE PHOTODYNAMIC ACTION OF CHLOROALUMINUM PHTHALOCYANINE AND VISIBLE LIGHT

Abstract— Chloroaluminum phthalocyanine (CAPC) is an efficient photosensitizer for the inactivation of Chinese hamster V79 cells. In order to investigate possible molecular mechanisms in the photo-dynamic action of CAPC and visible light, the induction and repair rate of two classes of DNA lesions have been determined, i.e. DNA single-strand breaks and DNA-protein cross-links. In cells pretreated with 1 μ.M CAPC, a fluence of 12 kJ/m² of red light (>600 nm) kills approximately 50% of the cells and induces 3 to 3.5 Gy-equivalents of single-strand breaks. The repair of these breaks was slower than the repair of single-strand breaks induced by -irradiation. The photodynamic action of CAPC also induces a large number of DNA-protein cross-links which, in contrast to -radiation-induced DNA-protein cross-links, do not appear to be repaired during 4 h of post-treatment incubation in fresh medium. These studies suggest that DNA may be an important target for the cytotoxicity of CAPC + red light.     

Synthesis and characterization of ionic organotin compounds [R2SnCl2(2-quin)](HNEt3) and crystal structures of [(2,4-Cl2-C6H3CH2)2SnCl2(2-quin)](HNEt3)

Eight ionic organotin compounds [R₂SnCl₂(2-quin)]⁻(HNEt₃)⁺ have been synthesized by reactions of 2-quinH with R₂SnCl₂ (R = PhCH₂1, 2-Cl-C₆H₄CH₂2, 4-Cl-C₆H₄CH₂3, 2-F-C₆H₄CH₂4, 4-F-C₆H₄CH₂5, 4-CN-C₆H₄CH₂6, Ph 7, 2,4-Cl₂-C₆H₃CH₂8) in the presence of organic base NEt₃, and their structures have been characterized by elemental analysis, IR and multinuclear NMR (¹H, ¹³C, ¹¹⁹Sn) spectroscopies. The structure of [(2,4-Cl₂-C₆H₃CH₂)₂SnCl₂(2-quin)]⁻(NEt₃)⁺ (8) has been determined by X-ray diffraction study. Studies show that compound 8 has a monomeric structure with the central tin atom six-coordinate in a distorted octahedral configuration and the nitrogen atoms of the 2-quin ligands are coordinating to the tin atom in all the eight compounds.     

Two new triterpenoid glycosides isolated from Aesculus assamica GRIFF

Phytochemical study of the ethanol extract of the seeds of Aesculus assamica led to the isolation of two new triterpenoid saponins. The structure of the new compounds were elucidated on the basis of spectral data to be 28-O-acetyl-21-O-(4-O-angeloyl)-6-deoxy-beta-glucopyranosyl-3-O-[beta-glucopyranosyl(1-2)-O-[beta-glucopyranosyl(1-4)]-beta-glucuronopyranosyl]protoaescigenin (1), and 21-O-(4-O-angeloyl)-6-deoxy-beta-glucopyranosyl-3-O-[beta-glucopyranosyl(1-2)-O-[beta-glucopyranosyl(1-4)]-beta-glucuronopyranosyl]protoaescigenin (2). Their in vitro bioactivity against plant pathogenic fungus Pyricularia oryzae and cytotoxicity against K562 and HCT-15 cell lines were evaluated.     

PVA／PVP共混物的聚集态结构

热处理前后不同组份比二元共混物聚乙烯醇(PVA)和聚乙烯吡咯烷酮(PVP)的聚集态结构研究表明,热处理可明显提高共混物的结晶性。热处理前样品仅观察到(101)晶面衍射,热处理后可观察到4个以上衍射晶面。结晶度和微晶大小随共混物中PVP含量增加而降低。第二类晶格畸变则随PVP含量增加而增大。