FTIR及Py-GC/MS定性分析高聚物单体

红外光谱反应出的是特征化学基团的振动 ,对于高聚物的具体单体组成分析 ,只能借助于紫外光谱、核磁共振及质谱进行综合判断才能得到圆满的鉴定结果[1,2 ] 。本工作针对在红外光谱仪不能分辨的情况下通过气相色谱 质谱联用技术进行综合分析鉴定 ,结果可为其它高聚物分析研究提供实验依据。1　实验1 1　仪器及试验条件未知高聚物试样为白色颗粒状 (晨光化工二厂 )。ＳＹＳＴＥＭ2 0 0 0ＦＴＩＲ ,ＰＥ公司造ＩＲ谱仪 ;ＣＤＳ2 0 0 0铂金丝裂解器 ,裂解室温度 2 5 0℃ ,裂解温度 6 0 0℃ ,升温速率 1 40℃ ｍｓ;ＨＰ6 890型 ,Ｃｏｍｐｏｎｄ…     

5，10，15，20-四 [4-(4''-乙基哌嗪基)苯基]卟啉的合成及其与DNA的相互作用

基于卟啉对癌细胞的特殊亲和作用和哌嗪化合物的抗肿瘤、抗病毒作用，设计并合成了具有哌嗪结构的新型卟啉化合物5，10，15，20-四[4-(4'-乙基哌嗪基)苯基]卟啉（TEPPPH₂），其结构经UV-Vis, 元素分析，¹H NMR等手段证明。采用UV-Vis光谱和荧光光谱研究了TEPPPH₂和小牛胸腺DNA 的相互作用模式和结合机理。实验发现，TEPPPH₂能嵌入到DNA的碱基对中，1个小牛胸腺DNA分子对TEPPPH₂分子的最大结合数n约为88，结合常数为8.4×10⁶mol•L^-1 。TEPPPH₂与DNA的结合数和结合常数大于已知的四（4-N-甲基吡啶基）卟啉和Ca/sal-his、Ni/sal–aln型席夫碱抗癌药物。     

Effects of Self—coiling of Organic Molecules on Intramolecular Exciplex Formation and Fluoresscence Quenching in DX—H2O Solvent System

Effects of self-coiling of organic molecules on intramolecular exciplex formation of compound I,in which the carbazole chromophore and terephthalic acid methylester acceptor group are linked by one (CH2)10 chain,and the decrease of the fluorescence intensities of compounds Ⅱ，Ⅲ，and Ⅳ,in which the carbazole chromophore and 3,5-dinitrobenzoate are connected by one aliphatic chain of (CH2)10 (Ⅱ），（CH2）12（Ⅲ）,or (CH2)4(Ⅳ）,have been studied in the dioxane (DX)-H2O binary system.The results show that self-coiling of organic molecules in DX-H2O facilitates intramolecular exciplex formation of I and induces the decrease of fluorescence intensities of Ⅱ,bacause of the proximity effect brought about by selfcoiling of organic molecules under hydrophobic-lipophilic interaction(HLI) between the excited carbazole chromophore and the acceptor.Since the similar effects are observed even when the concentration of the probes are less than their CAgCs(critical aggregate concentrations )in the DX-H2O mixture with the same φ values,formation of the intermolecular exciplex has been excluded.The effects are found to be strongly depended on φ values,indication that they are mainly driven by HLI.The properties of the acceptors can also affect the intramolecular exciplex formation.With terephthalic acid methylester moiety as the acceptor,the carbazole chromophore exhibits the fluorescence spectra of the exciplex,while with 3,5-dinitrobenzoate moiety as the acceptor,only the fluorescence spectra of excited carbazolyl chromophore are observed.     

三烃基锡肟类化合物的合成及生物活性

共合成了１３个未见文献报道的三烃基锡肟衍生物，测定了它们的＾１ｈ，（＾１３Ｃ，＾１１９Ｓｎ）ＮＭＲ，ＩＲ和ＭＳ。结果表明此类化合物为四配位锡单体结构，生物活性测定结果表明部分化合物同时兼有杀菌、杀螨、除草多种活性。     

离聚体水基微乳液化的研究——聚苯乙烯离聚体微乳化过程相反转的表征

以乙酰磺酸为磺化剂制备磺化度为３～１５ｍｏｌ％的磺化聚苯乙烯（ＳＰＳ）并中和成盐．在一定的温度和搅拌速率下，加水将ＳＰＳ乳化成水包油的稳定水基微乳液．用乳化过程中体系电导率和粘度的变化表征了乳化相反转过程．研究了溶剂的极性和离子含量对聚苯乙烯离聚体溶液可乳化性和乳化过程及乳液稳定性的影响．     

Synthesis and Crystal Structure of Two One—dimensional Chain Copper Complexes [Cu（TTA）2（4,4‘’—azpy）] and [Cu（TTA）2（3,3‘’—azpy）

Two copper complexes [Cu(TTA)₂(4,4′‐azpy)] (1) and [Cu‐(TTA)₂(3,3′‐azpy)] (2) (HTTA = 1,1,1‐trifluoro‐3‐(2‐thenoyl)‐acetone, 4,4′‐azpy = 4,4′‐azobispyridine, 3,3′‐azpy = 3,3′‐azobispyridine) were synthesized and characterized. The crystal structures were determined by X‐ray diffraction analysis. The crystal 1 belongs to triclinic with space group P1 , a = 0.8515(2) nm, b = 0.9259(2) nm, c = 0.9468(2) nm, a = 66.126(9)°, β = 79.667(9)°, γ = 90.13(1)°, Z = 1, V = 0.6692(2) nm³, D_c = 3.425 g/cm³, γ = 2.113 mm^?1, F(000) = 694, R₁ = 0.0594, wR₂ = 0.1499. The crystal 2 belongs to monoclinic with space group P2₁/c, a = 1.0661(2) nm, b = 1.4296(3) ran, c = 1.0041(3) nm, β = 114.50(3)°, V = 1.3926(5) nm³, Z = 2, D_c = 1.646 g/ cm³, μ = 1.015 mm^?1, F(000) = 694, R₁, = 0.0535, wR₂ = 0.1113. In the crystals of complexes 1 and 2, the copper atoms have distorted octahedral symmetry. The two compounds possess very similar one‐dimensional linear chains linked through the rodlike 4,4′‐azpy ligands or 3,3′‐azpy ligands.     

3—Mercaptopropionic Acid Capped Gold Nanoclusters：Quantized Capacitance in Aquesous Media

3-Mercaptopropionic acid monolayer protected gold nanoclusters (MPA-MPCs) were synthesized and characterized by transmission electorn microscopy,UV-Vis spectroscopy,X-ray photoelectron spectroscopy and Fourler transform infrared spectroscopy.The exact value of quantized double-layer capacitance of MPCs in aqueous media was obtained by differential pulse voltammograms.     

离子液体存在下脂肪醛的环化三聚反应

Aliphatic aldehydes such as ethanal,propanal,n-butanal,isobutyraldehyde,n-valeraldehyde,isovaleraldehyde,n-hexanal and n-octanal were converted into the corresponding 2,4,6-trialkyl-1,3,5-trioxanes through cyclotrimer-ization in the presence of the ferric chloride based ionic liquids at room temperature without solvent in high selec-tivity.The effects of different ionic liquids,acidity of ionic liquids and temperature on cyclotrimerization were alsostudied.The results showed that the ferric chloride based ionic liquids(apparent molar fraction of FeCl_3(x(FeCl_3)=0.62))were a kind of efficient catalysts for the cyclotrimerization of aliphatic aldehyde which could be separatedconveniently from the reaction mixture and recycled without loss of catalytic activity.The conversion of isobu-tyraldehyde and the selectivity to 2,4,6-triisopropyl-1,3,5-trioxane were 91.1% and 99.8% respectively under opti-mum reaction condition(isobutyraldehyde 25.0 g,[Et_3NH]Cl/FeCl_3(x(FeCl_3)=0.62)1.0 g,25 ℃for 1 h).     

吡啶叶立德与查尔酮1,3-偶极环加成反应制备2-苯基-3-乙酰基中氮茚

报道在氧化剂存在下吡啶叶立德与查尔酮进行1,3-偶极环加成反应, 一锅法合成2-苯基-3-乙酰基中氮茚化合物的方法, 收率37%. 用类似的方法由α-溴代异喹啉季铵盐、查尔酮、碱和氧化剂进行反应, 可一锅法得到1-苯甲酰基-2-苯基-3-乙酰基吡咯并[2,1-a]异喹啉, 收率58%.     

二(2,4,4-三甲基戊基)膦酸-上胺205-正庚烷乳状液膜分离钪(Ⅲ)、铁(Ⅲ)和镥(Ⅲ)

本文研究了二（2，4，4-三甲基戊基）膦酸（Cyanex272）-上胺205-正庚烷乳状液膜分离Sc（Ⅲ）、Fe（Ⅲ）和Lu（Ⅲ）。考察了外相酸度、表面活性剂浓度、流动载体浓度及内相盐酸浓度对Sc（Ⅲ）迁移的影响。并探讨了该液膜体系分离Sc（Ⅲ）、Fe（Ⅲ）和Lu（Ⅲ）的可能性，结果表明，该体系对于稀土矿中Sc（Ⅲ）的分离与分析有良好的应用前景。