聚醋酸乙烯酯的光引发可控合成——介绍一个高分子化学综合实验

本实验开展了醋酸乙烯酯的可逆加成-断裂链转移自由基聚合(RAFT),分别运用偶氮二异丁腈(AIBN)引发和可见光引发两种方式进行了聚合反应,运用核磁共振和凝胶色谱等多种手段对所得聚合物结构进行了表征与分析。通过比较AIBN引发与光引发所获得聚合物端基结构的异同,加深了学生对RAFT聚合方法原理的理解。同时,运用该方法实现了聚合物两端端基结构的高度功能化,深入体会聚合物合成设计概念。本综合实验教学不仅通过对比法加深了学生对实验原理和专业知识的理解,提升了学生创新研究能力,而且训练了学生的实验操作技能、大型仪器使用能力和结果分析能力,提升了综合素质。     

Study of the Complexation Behavior of Calixarene with Transition Metal Cations by UV—vis and Fluorescent Spectra

A new fluorescent compound based on calix[4] arene skeleton was synthesized.Its complexation ability with transition metal ions,such as Fe^3 ,Co^2 ,Ni^2 ,Cu^2 ,Zn^2 and Ag^ ,Was investigated by UV-vis and fluorescent spectra.     

Synthesis and Characterization of Novel Orange-emitting Iridium（Ⅲ） Complexes with Diphenylquinoline Ligands Containing Fluorinated Substituent

Three new cyclometalated iridium（m） complexes based on ligands of diphenylquinoline with fluorinated subsfituents were prepared, and characterized by elemental analysis （EA）, ^1H NMR, and mass spectroscopy （MS）. The photophysical and electrophosphorescent properties of the complexes were briefly discussed.     

高效毛细管电泳间接紫外检测血浆中钾、钙、镁

用高效毛细管电泳法,在pH 5.5的缓冲介质中用酒石酸作为络合剂,使血浆中钾、钠、钙、镁4种阳离子达到很好分离,用咪唑作为背景试剂进行了紫外检测.对电泳分离及紫外检测的各分析条件(包括背景缓冲溶液的pH值,咪唑溶液的浓度及酒石酸溶液的浓度等)作了试验并予以优化,上述4种离子的相互分离在4.5 min内顺利完成.文中给出了K 、Ca 、Mg2 的线性回归方程,其相关系数在0.998 4～0.999 4之间,证明了在各离子的峰面积与其浓度之间呈线性关系,3种离子的检出限(S/N=3)依次为0.20,0.12,0.06 mg·L-1.用迁移时间检测和用峰面积检测所得的RSD值(n=6)依次小于0.76%和2.83%.由于钠离子的吸收峰与系统峰重叠,钠的测定无法进行.回收率试验的结果在95.3%至104.2%.     

温敏性聚合物复合体系低临界溶解温度的研究

研究了温敏性N-异丙基丙烯酰胺的均聚物(PNIPAm)及其共聚物P(NIPAm-co-KYD)与十六烷基三甲基氯化铵(CTAC)、乙二胺四乙酸(EDTA)、盐等复配体系的低临界溶解温度(LCST)的变化规律。单因素复配体系中,wEDTA为0.1%时,体系LCST从33℃降低到25℃,增大到0.2%时,LCST下降趋于缓慢;wCTAC在0.5%-3.0%范围内,LCST先上升后下降,但wCTAC在0.5%-1.0%内相转变很不明显,超过1.5%后相转变又趋于明显;而无机盐能使体系LCST线性下降;多因素复配体系中LCST变化较缓和,易于控制且相转变现象明显。     

Tris(2,2''''-bipyridyl)ruthenium(Ⅱ) electrochemiluminescence (ECL) enhanced by rutin on platinum electrode

Ru(bpy)_(3~(2 )) electrochemiluminescence (ECL) was applied to determination of rutin. ECL intensity of Ru(bpy)_(3~(2 ))could be enhanced in the presence of rutin in basic solution on platinum electrode. At pH 9.9, light emission intensity was found to be linear with rutin in the range of 1-50 mmol/L.     

Determination of sulfite in Oriental herbal medicines

Sulfite was detected in 7 varieties of Oriental herbal medicines (Pueraria radix, Zingiberis rhizoma, Platycodon radix, Adenophora radix, Pinellia tuber, Astragalus radix, and Paeonia radix) on the Korean market. Sulfiting of commercial Oriental herbal medicines by fumigation with burning bituminous coal was simulated, and the accumulation of sulfite was investigated by using fresh Platycodon radix roots obtained from a growing field. The sulfite level reached a plateau in 9 h, and the maximum sulfite level found by the Monier-Williams (MW) method (AOAC 990.28) was 1020 ppm. The sulfite content in the simulated Platycodon radix sample determined by alkali extraction followed by ion-exclusion chromatography with electrochemical detection (AOAC 990.31) was approximately 17% lower on average than the MW results. Free-sulfite levels determined by acid extraction and ion-exclusion chromatography with electrochemical detection were between 19 and 49% of the MW results. The advantages of different methods for sulfite determination and the significance of the results are discussed.     

Synthesis of gramicidin S and its analogues via an on-resin macrolactamization assisted by a predisposed conformation of the linear precursors

A simple and efficient preparation of gramicidin S and its analogues is described. It involves solid-phase peptide synthesis and on-resin macrolactamization without side chain protection, affording cyclic products in high yield and high purity. The high specificity of the cyclization reaction was shown to originate in the formation of a pre-organized conformation of the linear biosynthetic precursor of gramicidin S. This facile method will provide convenient access to the analogues of the natural product for functional optimization to counter microbial resistance.     

Utilization of a spiropyran derivative in a polymeric film optode for selective fluorescent sensing of zinc ion

Spiropyrans are the most studied families of func- tional materials due to their reversible structural con- version in response to external optical, chemical, and thermal stimulation[1]. Irradiation with ultraviolet light causes formation of an extended π-conjugation open form (merocyanine form) by heterolytic cleavage of the C (spiro)-O bond, which generates an intense ab- sorption in the visible region. Under the irradiating of visible light, the opened form will come back to the closed spi…     

相转移催化合成对甲氧基肉桂酸-2-乙基己酯的研究

对甲氧基肉桂酸 2 乙基己酯是一种有效的ＵＶＢ防晒剂[1 ,2 ] ,一般采用Ｃｌａｉｓｅｎ Ｓｃｈｍｉｄｔ缩合反应制得[3] ,但由于催化剂ＫＯＨ处于水相 ,对反应物不能充分起到催化作用导致产率较低[4] 。我们利用乙二醇 (ＰＥＧ)为相转移催化剂合成立体专一的反式对甲氧基肉桂酸 2 乙基己酯 ,产率提高到 72 .5 %。合成路线如下 :1　实验部分1 .1　仪器与试剂ＢＩＯ ＲＡＰＦＴ45 0红外光谱仪 ,用液膜法测试 ;Ｂｒｕｒｅｒ ＡＭ 30 0超导核磁共振仪 (溶剂ＤＣ Ｃｌ3) ;ＭＡＴ/44Ｓ ,ＧＣ ＭＳ型色质联用谱仪 ;试剂均为分析纯 ,上海化学试剂…