Hydrothermal syntheses and structural characterization of two new supramolecular compounds: (H2bbi)2[Mo8O26] and (H2bbi)2[SiW12O40]·2H2O [bbi = 1,1′-(1,4-butanediyl)bis(imidazole)]

Two new inorganic–organic hybrid supramolecular compounds based on imidazolium and POMs formulated as (H₂bbi)₂[Mo₈O₂₆] (1) and (H₂bbi)₂[SiW₁₂O₄₀]·2H₂O (2) [bbi = 1,1′-(1,4-butanediyl)bis(imidazole)] have been prepared under hydrothermal conditions and characterized by elemental analyses, IR and single-crystal X-ray diffraction analyses. The two compounds consist of protonated bbis together with POMs. [Mo₈O₂₆]^4? and [SiW₁₂O₄₀]^4? are linked through H₂bbi into a three-dimensional (3D) network via hydrogen bonds, respectively. Compound 1 is the first example of 3D two-fold interpenetrating hydrogen bond-supported supramolecular assembly from octamolybdate one-dimensional (1D) chain and imidazolium. The fascinating structural feature of compound 2 is that the anions and the protonated bbi ligands formed a 3D (4, 8) supramolecular network by hydrogen bonds. Compound 2 has been used as a solid bulk-modifier to fabricate three-dimensional bulk-modified carbon paste electrode (CPE) by direct mixing. The electrochemical behavior and electrocatalysis of compound 2 modified CPE (2-CPE) have been studied.     

N,N-Dilauryl Chitosan：Synthesis and Surface Pressure-area Isotherm

With sodium dodecyl sulfonate(SDS) as the phase transferring catalyst, N,N-Dilauryl chitosans with a high degree of alkyl group substitution were prepared and characterized by means of FTIR, ^1H NMR and elemental analyses. The results indicate that the average degree of alkyl group substitution on the chitosan increases with decreasing the molecular weight of the chitosan. The fully N,N-dilaurylated chitosan was found to be dissolvable in chloroform. The collapsed pressures of the samples derived from chitosan with 3000,5000 and 10000 dalton are 47.6, 48. 2 and 51.0 mN/m, respectively. The surface area occupied by the monomer unit(glucosamine) of all. those samples is 0:6 nm^2.     

[Fe(L)3](ClO4)3(L=bpy,phen)与Na2S2O3在室温下的固相氧化还原反应

本文研究室温下[Fe(bpy)3](ClO4)3.3H2O和[Fe(phen)3](ClO4)3.H2O分别与Na2S2O3.5H2O发生的固-固相氧化还原反应。用Mossbauer谱、XRD、IR、UV漫反射谱、元素分析、TG-DTA和磁化率测定等手段表征了反应24h后的固相产物,报道了[Fe(bpy)3](ClO4)2的结晶学数据。结果表明, 室温下反应速度快, 反应进行完全。     

超分子化合物[Ni(C_6H_4O_2N)_2·(H_2O)_4]_n的水热合成及晶体结构

用皮考林酸和六水合氯化镍反应制备了一种三维氢键超分子配合物,经X射线衍射分析确定了单晶结构.该晶体属单斜晶系,P21/m空间群,晶胞参数为:a=0.976 0(2)nm,b=0.522 54(10)nm,c=1.450 1(3)nm,Mr=374.98,α=90.08(3)°,β=90.08(3)°,γ=90°,V=0.739 63(3)nm3,Z=2,ρ=1.684 g/cm3,F(000)=388,μ=1.357 mm-1,R=0.039 0,wR=0.090 8.共收集2 656个衍射数据,其中1 569个为独立衍射点(Rint=0.033 2),可观测点数1 382个(I>2σ(I)).结果表明,在组成该超分子体系的基本结构单元[N i(C6H4O2N)2.(H2O)4]中,N i(Ⅱ)离子形成六配位的稍拉长的八面体构型,配合物单元之间通过氢键相互连接,形成了无限延伸的具有网状结构的三维超分子体系.     

TBTGA对甲基丙烯酸甲酯RAFT聚合及其产物结构的影响

2-巯基-S-硫代苯甲酰乙酸(TBTGA)作为一种相对经济的链转移剂,可对活性较高的单体(MAMs)发生可逆加成-断裂链转移(RAFT)聚合提供较好的控制性,但是目前针对该链转移剂的研究较少。选择甲基丙烯酸甲酯(MMA)作为单体,通过改变TBTGA的含量,得到一系列产物,并与普通自由基聚合得到的产物进行对比,探究TBTGA对甲基丙烯酸甲酯RAFT聚合及产物结构的影响。结果表明：随着TBTGA含量的增加,RAFT聚合所得PMMA的玻璃化转变温度逐渐升高,且玻璃化转变温度范围越来越窄。这说明随着TBTGA的增加,PMMA分子链的分散性变窄,证明TBTGA对MMA发生RAFT聚合具有良好的控制性。      

基于壳聚糖的QuEChERS-气相色谱-串联质谱法测定人参中30种农药残留

建立了一种以壳聚糖为净化材料的QuEChERS-气相色谱-串联质谱检测人参中30种农药残留的检测方法。探究了吸附剂及其用量对样品提取和净化效果的影响,确定壳聚糖为吸附剂净化。采用选择离子监测(SRM)模式,基质匹配标准曲线外标法定量。30种农药在各自的浓度范围内,线性关系良好(r> 0.996);检出限范围为1.5~3.0μg/kg,定量限范围为5.0~10.0μg/kg。3个添加水平(10,20,100μg/kg)的回收率在84.1%~113.7%之间,相对标准偏差均小于15%。该方法适用于检测人参中农药残留。     

Nano‐hydroxyapatite Surfaces Grafted with Electroactive Aniline Tetramers for Bone‐Tissue Engineering

An electroactive amino/carboxyl‐capped aniline tetramer (AT) is covalently grafted to the surface of hydroxyapatite (HA) nanoparticles to generate novel electroactive HA‐AT nanoparticles. The amount of AT ranges from 16.5 to 34.0 wt% and is characterized by thermogravimetric analysis (TGA). The HA‐AT nanoparticles are characterized by Fourier transform IR (FTIR) spectroscopy, X‐ray photoelectron spectroscopy (XPS), X‐ray diffraction, and scanning electron microscopy (SEM). For the excellent electroactivity of HA‐AT, the mixture of HA‐AT and PLA shows much better adhesion ability and proliferation ability than that of HA and a PLA matrix. At a 15 wt% AT grafting amount, the matrix shows the best biocompatibility.

     

阻燃PVA-g-AN的制备、表征及性能

以K₂S₂O₈-NaHSO₃氧化还原体系为引发剂, 将丙烯腈(AN)接枝到聚乙烯醇(PVA)上, 得到聚乙烯醇接枝丙烯腈聚合物(PVA-g-AN), 将其与磷酸-尿素反应制备阻燃聚乙烯醇接枝丙烯腈聚合物(FR-PVA-g-AN). 利用傅里叶变换红外光谱(FTIR)、 X射线能谱(XPS)和X射线衍射(XRD)对其结构进行表征, 并用热重分析(TGA)对其热性能进行研究. 结果表明, 当引发剂用量占反应物总质量的1%, n(K₂S₂O₈):n(NaHSO₃)=5:1, m(丙烯腈):m(聚乙烯醇)=3.5:1, 70 ℃反应4 h时, 接枝率可达190%; 在m(磷酸):m(尿素)=5:1, 85 ℃条件下处理接枝产物PVA-g-AN 4 h时, 获得阻燃性能良好的FR-PVA-g-AN, 700 ℃马弗炉热处理后, 残炭量达到63%. TGA结果显示, FR-PVA-g-AN的热降解过程较PVA减慢, 且800 ℃后残炭量由PVA的3.12%增加到54.3%, 说明FR-PVA-g-AN具有优异的热稳定性和成炭性.     

基于席夫碱配体构筑的Ln2Ⅲ配合物的结构、荧光性质及生物活性

以多齿席夫碱配体 H₂L(H₂L=(E)-N′-(3-乙氧基-2-羟基亚苄基)-3-羟基吡啶甲酰肼)为配体,与 Ln(acac)₃·2 H₂O(Ln=Tb、Ho、Er;acac^-=乙酰丙酮根)反应,通过溶剂热法,成功得到了 3例新的双核稀土配合物[Ln₂(acac)₂(L)₂(C₂H₅OH)₂](Ln=Tb (1)、Ho(2)、Er(3))。单晶X射线衍射分析表明：配合物1~3的结构主要由2个Ln^Ⅲ离子、2个乙酰丙酮根(acac^-)、2个L^2-及2个C₂H₅OH组成,中心Ln^Ⅲ离子通过2个μ₂-O原子相互连接,形成一个平行四边形的Ln₂O₂核心。固体荧光实验测试结果表明：配合物1在室温下表现出Tb^Ⅲ离子的荧光特征发射峰。此外,生物活性研究表明,与配体H₂L和稀土离子相比较,配合物1~3具有更强的抗菌活性。采用紫外光谱法、循环伏安法、凝胶电泳法和荧光光谱法研究了配合物 1~3与小牛胸腺 DNA之间的相互作用,结果表明配合物主要以插入作用的方式与小牛胸腺DNA结合。     

微波等离子体光谱技术的发展(二)

微波等离子体光源是一类重要的有较强激发能力的原子发射光谱光源,主要包括微波感生等离子体光源,电容耦合微波等离子体光源及微波等离子体炬光源。本文是微波等离子体光谱技术发展的第二部分,主要介绍了电容耦合微波等离子体光源及微波等离子体炬光源的结构原理和性能。并对它们的技术特点和进展进行评述。