由二硫代肼基甲酸酯衍生的铜(Ⅱ)的希夫碱配合物的合成,结构和抑菌活性的研究

从S—苄基和S—甲基二硫代肼基甲酸酯衍生出的两种亚苄基丙酮希夫碱为配体,合成了铜(Ⅱ)配合物。经化学分析、磁性、红外、电子和EPR光谱的研究表明配合物有Cu(TSB)_2的形式,其中配体为双齿单价阴离子。在固态时,两种配合物分别为平面正方形和平面菱形结构。在溶液中,两者都为平面正方形。由EPR光谱分析得到的磁参数和键参数的值表明配合物中的键有较高的共价特征。对四种细菌的抑菌试验发现配体及其配合物均有抑菌活性,其中配合物的活性较高并研究了介质,pH对抑菌作用的影响。     

A Two-dimensional Lanthanide Coordination Framework with a New Amide-type Tripodal Ligand, 2,2′,2＂-Nitrilotris{[（2′- benzylaminoformyl）phenoxy]ethyl}amine

The La(III) complex with a new amide‐type tripodal ligand,2,2′.2″‐nitrilotris{[(2′‐benzylaminofomyl)‐phenoxylethyl)amine (L), was synthesized and characterized by X‐ray crystallographic analysis. Crystal data: C₄₈H_55.50LaN₇O_18.75, M_r=1169.40, monoclinic. space group, P2₁/n, a= 1.0644(3) nm. b=2.3889(5) nm, c= 2.1917(5) nm, β=90.65°, V=5.573(2) nm³, Z=1, D_c=1.394 g°cm^?3, R₁=0.0487, wR [1>2s?(I)]=0.1266. The results reveal that each La(III) ion binds to 9 oxygen atoms, three of which belong to carbonyl groups from three tripodal ligands and six to three bidentate nitrate groups and a two‐dimensional sheet of 4.8² networks is assembled by metal‐ligand coordination interaction. L, a heptadentate compound, merely acts as a tridentate bridging spacer due to its steric hindrance and links the La(III) ions as three‐connected nodes.     

毛细管离子交换电色谱的分离行为

在离子交换毛细管色谱柱上实施电色谱，并对其分离行为进行了研究，采用７５μｍ（ｉ．ｄ．）２０ｃｍ的毛细管强阳离子交换柱（３μｍ）以ＮａＨ２ＰＯ４－Ｈ３ＰＯ４缓冲液为淋洗剂，紫外柱上检测（２１４ｎｍ）考察了流动相的ｐＨ值，有机改性剂及分离电压等因素对分离的影响，研究表明，不同的ｐＨ溶质的流出次序发生改变，随着有机改性剂含量增加，溶质的保留时间减小，而电渗流却增大，同时，对分离的柱效和方法的重现性进行了     

用酮作为酸性组分的Mannich碱的合成

本文综述了用酮作为酸性组分合成Mannich碱的最近进展。内容包括:β-脂氨基酮、β-芳氨基酮的合成和分子内Mannich反应。     

Semiconducting organic polymer from polyacrylamide–Cu++ chelate and iodine

Semiconducting organic polymer was obtained by the modification of polyacrylamide (PAAm)–Cu⁺⁺ chelate with iodine in acetone. Favorable conditions for preparing the chelate effective for the conduction were investigated. Surface resistivities were affected by the amounts of cupric salts and iodine, satisfactory results being given by about 25 wt % of the salts based on PAAm and more than 1 wt % of iodine on the chelate. The conductivity was also varied with the degree of neutralization of the chelate in solution, and optimal values were obtained by addition of about an equimolar amount of potassium hydroxide to cupric salts. Effective structures of the polymer chelate in solution were assumed on the basis of the visible and the NMR spectra and potentiometric titration.     

高效液相色谱法测定精对苯二甲酸中微量杂质

建立了高效液相色谱法（HPLC）同时测定精对-苯二甲酸（PTA）中微量杂质4-羧基苯甲醛（4-CBA）、对-甲基苯甲酸（P-TOL）和苯甲酸（C7H6O2）含量的方法。采用的色谱柱为Shim-PackWAX-1柱，流动相为0.1mol/L NH3H2PO4 6%CH3OH，(pH4.5)，检测波长为254nm。PTA中微量杂质4-CBA、P-TOL和C7H6O2的含量分别为0.59-235.20mg/kg、4.52-392.00mg/kg和0.28-24.55mg/kg时线性关系良好，其线性相关系数分别为0.9998、0.9997和0.9999。苯甲酸加样平均回收率99.03％，RSD0.37％。     

Preparation of HPMC–EA–DMAEMA nanosized latex

Nanosized copolymer latex of hydroxypropylmethylcellulose (HPMC) grafted with ethyl acrylate (EA) and dimethylaminoethyl methacrylate (DMAEMA) has been prepared by acidifying submicron-sized latex particles synthesized by soap-free emulsion graft copolymerization using potassium persulfate (KPS) as initiator. The effects on the diameter of the latex particles of different conditions, for example concentration of DMAEMA, amount of HPMC, and ratio of HCl to DMAEMA for acidification, were investigated. It was found that increasing the mole ratio of HCl to DMAEMA to 1.0 and increasing the DMAEMA content both resulted in a decrease in particle diameter, whereas increasing the amount of HPMC resulted in larger particle sizes. Measurement by dynamic light scattering (DLS) revealed the diameter of the latex particles was >200 nm before acidification and <100 nm after acidification. Evidence of grafting was obtained by use of Fourier transform infrared (FTIR) spectroscopy. Transmission electron microscopy (TEM) was used to characterize the morphology of the copolymer particles before and after acidification.