SERS Study of Co-doped TiO2 Nanoparticles

Single-phase Co-doped TiO₂(Co_xTi_1-xO₂) nanoparticles(NPs) synthesized via a simple sol-hydrothermal method were used as surface-enhanced Raman scattering(SERS) substrates. Interestingly, it was found that SERS signals were enhanced greatly compared to those of pure TiO₂ nanoparticles when an amount of Co²⁺ ions were doped into the TiO₂ lattice. Detailed results clearly show that Co element as Co²⁺ was incorporated into the TiO₂ lattice and the defects were created due to the substitution of Co²⁺ ions for the Ti⁴⁺ ions. The Co²⁺ doping increases the defect concentration of Co_xTi_1-xO₂ NPs. An amount of defects is beneficial to the charge-transfer so as to increase the SERS activities. A possible mechanism of charge-transfer from Co_xTi_1-xO₂ NPs to molecules was then briefly discussed.     

超大硅胺基氯锗宾的反应性与立方四锗卡宾的成键解析

超大硅胺基取代的低价锗化合物可以构建新颖的化学结构, 提供有学术价值的新发现。二配位的超大硅胺基氯锗宾Ge(N(SiⁱPr₃)₂)Cl (1)具有空的 4p轨道和孤电子对。针对这 2个特点, 研究了化合物 1 的热构型转换和菲醌氧化加成反应。1的温热分解生成了立方四锗卡宾 Ge₄(NSiⁱPr₃)₄ (2), 与菲醌(L)定量氧化加成生成了胺基一氯菲二酚合锗(Ⅳ):[Ge(N(SiⁱPr₃)₂)(L) Cl] (3)。表征了 2个产物的单晶结构与组成。四锗卡宾 2本质上是锗异腈的四聚体, 分子呈现出畸变的立方体构型, 4个 Ge原子和 4个N原子构成了中心立方体的 8个顶点。其中 Ge-N键长为 0.203 6(3) nm, N-Ge-N与 Ge-N-Ge的键角分别为 85.51(18)°和94.32(16)°, 立方体的侧面接近平行四边形。理论计算首次揭示了四锗卡宾 2的成键面貌。自然键轨道(NBO)给出 Ge₄N₄骨架上的 20个分子轨道。轨道定域化的计算结果完好地呈现出 4对 Ge孤对电子、12个 Ge-N键和 4个 Si-N键的定域轨道, 能量分别为-12.22、-15.12 和-20.12 eV。Ge 孤对电子主要保留了 4s 电子的特性, 而 Ge-N 键主要由 N 的 2s 轨道(18.4 %)和 2p 轨道(71.3 %)、Ge的 4s轨道(0.75 %)和 4p轨道(9.43 %)综合贡献形成。在化合物 3的分子中, Ge^Ⅳ采取 sp³杂化, 由于空间位阻与非对称配位, 与另外 4个配位原子形成非对称四面体构型。     

Research Progress and Application of Ion Funnel Technique

Ion funnel is a new-style ion guider which can reduce spatial divergence and energy dispersity of the transmission ions by using radio frequency (RF) electric field to confine the ions radially and the direct current (DC) axial electric field to move the ions toward the exit, and thus it can greatly increase the ion transmission efficiency and improve the sensitivity of the mass spectrometry. Since ion funnel was invented in 1997, it has attracted a close attention of mass spectrometry scientists all over the world. Ion funnel has been used in various kinds of mass spectrometry, and built a bridge with high efficiency ion transmission between low vacuum ionization source and high vacuum mass analyzer. In this paper, the principle, technology development, and application progress of ion funnel are reviewed, and the future prospects are prospected.     

A novel high selectivity chemiluminescence sensor for fenvalerate based on double-sided hollow molecularly imprinted materials

Novel fenvalerate double-sided hollow molecularly imprinted microspheres (fenvalerate-DHMIMs) were fabricated by in situ polymerization with the help of mesoporous silica microspheres (MSMs) in this paper for the very first time. Scanning electron microscope was employed to characterize the surface morphology of the fenvalerate-DHMIMs. Taking advantage of the quenching effect of fenvalerate on the luminol-H(2)O(2)-NaOH chemiluminescence system, a new model was established to determine fenvalerate by a highly selective flow injection chemiluminescence method. The traditional flow-through cell was replaced by a novel Y-shaped column. The chemiluminescence intensity was linear with fenvalerate concentration over the range of 5.0 × 10(-8) to 2.0 × 10(-5) g mL(-1) and the detection limit was 2.2 × 10(-8) g mL(-1). The relative standard deviation (RSD) for the determination of 2.0 × 10(-6) g mL(-1) fenvalerate was 1.4% (n = 11). The proposed method was applied to the determination of fenvalerate in real samples with satisfactory results.     

分散液相微萃取/高效液相色谱法同时测定啤酒中3种酮类老化物质

建立了分散液相微萃取(DLLME)/高效液相色谱(HPLC)同时测定啤酒中双乙酰、2,3-戊二酮和β-大马酮3种主要酮类老化物质的方法.确定了双乙酰和2,3-戊二酮的衍生化反应条件和3种目标组分同时检测的高效液相色谱条件,在15 min内实现了对3种酮类老化物质的分离和检测;优化了分徽液相徽萃取的实验条件,使3种目标组...     

二(1-环戊烯基茚基)四羰基二钌的合成、晶体结构及热稳定性研究

由6,6-四亚甲基苯并富烯C9H6C(CH2)4与Ru3(CO)12在二甲苯中加热回流,合成了一个钌配合物[((η5-C9H6)C(C4H7))2Ru2(μ-CO)2(CO)2]。通过元素分析、红外、热重、核磁共振进行了表征及研究。用X射线单晶衍射法测定了[((η5-C9H6)C(C4H7))2Ru2(μ-CO)2(CO)2]的结构,结果表明:晶体属于单斜晶系,P21/c空间群,a=0.757 1(13)nm,b=1.577 7(3)nm,c=1.107 3(19)nm,β=90.07(2)°,V=1.322 6(4)nm3,Dc=1.699 g.cm-3,μ=1.179 mm-1,F(000)=676,Z=2,R1=0.030 5,wR2=0.072 4。     

水滑石改性二氧化硅新材料去除养殖用水中的孔雀石绿及结晶紫

合成了水滑石改性的系列硅胶新材料HTS-n(s),该新材料同时包含有酸性位与碱性位,并通过碱腐蚀获得了3～4 nm的小孔和大的比表面积。该类材料可选择性吸附去除水产养殖用水中的工业染料类污染物孔雀石绿和结晶紫。吸附后水中剩余的染料浓度通过高效液相色谱-质谱/质谱联用仪进行检测,结果显示新材料的吸附性能超过常用的工业吸附剂NaY沸石和活性炭。     

过硫酸胺与N－［（3－二甲氨基）丙基］丙烯酰胺氧化还原引发体系的研究

N-[(3-DimetLylamino)-propyll acrylamide(DMAPAA) and N-[(3dimetliylamino)-propyl] methacrylamide(DMAPMA) were synthesized by the reaction of 3-dimethylamino-propylamine with acryloyl and methacryloyl chloride respectively at 0-5℃ temperature. The kinetics of the aqueous solution polylmerization of acrylamide(AAm) by using ammonium persulfate(APS) combined with DMAPAA or DMAPMA was investigated. The rate equations were given as:respectively. The overall activation energies of the polymerization were determined as low as 35.0kJ/mol and 41.0kJ/mol respectively. Based on the end-group analysis results, the reaction mechanism of DMAPAA or DMAPMA with APS was proposed to be similar to the initiation reation of persulfate/tertiary aliphatic amine redox system,and the resulting aminomethyl radicals were responsible for initiation of vinyl polymerization as well as sulfate radical.     

三氯化一缬氨酸六水合稀土固体配合物的合成及红外光谱

在水溶液中合成了Ｌｎ（Ｖａｌ）·Ｃｌ＿３·６Ｈ＿２Ｏ（Ｌｎ＝Ｌａ，Ｎｄ，Ｓｍ，Ｇｄ，Ｅｒ）．利用元素分析和容量滴定法确定了其组成。测定了配合物的红外光谱，对其主要红外吸收带进行了归属。红外光谱结果表明，缬氨酸以内盐的形式存在于配合物中，并通过羟基与稀土离子配位，６个水分子亦参与了配泣，推测Ｌａ和Ｎｄ配合物具有一维无限长锭结构，而Ｓｍ、Ｇｄ和Ｅｒ配合物为双核配合物．     

临床医学专业有机化学"课程思政"教学初探

深化高校"课程思政"改革,是落实立德树人理念,全方位对学生开展思想政治教育的有效途径。本文针对临床医学专业的特点,从教师素养的提高、课程思政内容的设计和学生的课外实践等方面对有机化学教学中实施"课程思政"进行了探索和实践。