水溶性发光金量子点灵敏检测L-半胱氨酸

室温下一步合成了一种蓝色发光金量子点。 该金量子点具有良好的水溶性和生物相容性,金量子点平均粒径为3.0 nm,在波长305 nm光激发下,发射430 nm蓝色荧光。 实验发现,一定量L-半胱氨酸对金量子点430 nm处荧光发射有显著的增强作用,由此可建立一种简单、迅速、灵敏检测L-半胱氨酸的新方法。在最佳条件下,金量子点荧光强度与L-半胱氨酸在0~4.0 μmol/L浓度范围内呈线性关系,线性相关系数R2=0.9976,对2.0 μmol/L L-半胱氨酸的11次测定结果的相对标准偏差（RSD）为2.8%,以3倍标准偏差计算本法对L-半胱氨酸测定的检出限为5 nmol/L。     

迷迭香酸的CdTe量子点荧光探针同步荧光法测定

基于迷迭香酸对CdTe量子点荧光的猝灭效应,建立了一种高灵敏度的测定微量迷迭香酸的同步荧光法.在pH 5.7的缓冲溶液中,当固定波长差为210 nm时,CdTe量子点的同步荧光最大发射波长位于320 nm.在最佳实验条件下,迷迭香酸质量浓度在0.36 ～11.52 mg·L-1(1.00×10-6 ～3.20×10-5 mol/L)范围与CdTe量子点的同步荧光强度存在良好的线性关系.其线性回归方程为I0F/IF=0.931 7+0.128 9 ρ(mg·L-1),相关系数r=0.998 2,检出限为0.16 mg·L-1.10次重复测定2.16 mg·L-1 的迷迭香酸,相对标准偏差为2.8%.同时对其同步荧光猝灭机理进行了探讨.     

基于Cu2-x Se纳米颗粒与罗丹明B的能量转移测定L-半胱氨酸

以硒化铜纳米颗粒为能量受体,以罗丹明B为能量供体,二者之间通过光诱导电子转移而猝灭罗丹明B的荧光;而 L-半胱氨酸能够诱导罗丹明 B 荧光的恢复,从而建立了测定 L-半胱氨酸的新方法。在pH 4.6、温度为30℃条件下混合2 mun后,罗丹明B在575 nm处的荧光强度与溶液中L-半胱氨酸的浓度在2.5×10-7~1.1×10-6 mol/L浓度范围内呈良好的线性关系,检出限(3σ/k)为5.5×10-8 mol/L。常见的氨基酸对半胱氨酸的测定干扰小,方法快速、选择性好。     

水溶性的高荧光CdTe/CdSeⅡ型核壳量子点的合成与表征

用L-半胱氨酸(L-cysteine)作为稳定剂,以制备的CdTe量子点为核模板,水相合成了具有近红外发光的Ⅱ型核壳CdTe/CdSe半导体量子点。实验考察了合成温度,核模板的尺寸和组分比等因素对合成高质量的CdTe/CdSe量子点的影响。用紫外-可见吸收和荧光光谱研究了合成的量子点的光学性质。在优化的合成条件下,荧光发射光谱在586～753nm范围连续可调,荧光量子产率高达68%;通过X-射线衍射(XRD),X射线光电子能谱(XPS)和透射电镜(TEM)对合成的Ⅱ型核壳CdTe/CdSe量子点进行了结构和形貌表征。     

基于CdTe量子点的荧光猝灭-恢复法测定L-半胱氨酸

以巯基乙酸为稳定剂,合成了水溶性CdTe量子点(QDs),基于Ni~(2+)存在下,利用CdTe QDs荧光猝灭-恢复技术,建立了测定L-半胱氨酸的新方法。考察了缓冲溶液pH及Ni~(2+)浓度等对测定的影响。在pH=10.0的硼砂缓冲溶液中,Ni~(2+)浓度为40μmol/L条件下,L-半胱氨酸浓度在6.0×10~(-6)~5.0×10~(-5) mol/L范围内与量子点荧光恢复程度呈良好的线性关系,相关系数为0.9990,方法的检出限为2.1×10~(-6) mol/L。该方法应用于果汁和蜂蜜样品中L-半胱氨酸的检测,结果满意。     

富镉离子CdS量子点电化学发光法检测L-半脐氨酸

采用一锅法,通过控制镉硫比合成了表面富镉离子的硫化镉量子点,利用L-半胱氨酸可与量子点表面Cd2+结合,使量子点表面钝化,从而增强其电化学发光信号的性质,实现了对L-半胱氨酸的选择性检测.对合成的量子点进行了表征,优化了检测条件.在优化的条件下,L-半胱氨酸在5.0×10-9~1.0×10-5 mol/L浓度范围内与ECL信号呈良好的线性关系,检出限为1.2×10-9 mol/L(S/N=3).本方法对L-半胱氨酸具有良好的选择性,用于实际样品中L-半胱氨酸的测定,结果令人满意.     

CdTe/CdS量子点-蛋白质与头孢曲松钠的相互作用

以3-巯基丙酸为稳定剂,采用水热法合成了具有优异光学性质的CdTe/CdS核壳型量子点,量子产率为13.8%。量子点与牛血清白蛋白(BSA)偶联后荧光强度明显增大。通过测定荧光强度确定了偶联的最佳反应条件:pH7.4,反应温度37℃,反应时间40min。研究了溶液pH值和NaCl浓度对量子点及量子点-BSA溶液荧光强度的影响。对牛血清白蛋白测定的线性范围为1.1~19.5mg/L;检出限为0.47mg/L。头孢曲松钠对量子点-BSA的荧光有明显猝灭作用,荧光猝灭程度与其浓度有良好的线性关系。实验结果表明为静态猝灭,头孢曲松钠与BSA按1∶1结合,结合常数为6.31×103L/mol。用圆二色光谱技术探讨了其对BSA构象的影响。     

酶抑制动力学光度法测定L-半胱氨酸

利用L-半胱氨酸对血红蛋白模拟酶催化体系的抑制作用,建立了酶抑制动力学光度法测定L-半胱氨酸的新方法。研究了该抑制反应的最佳实验条件及动力学行为,测定的线性范围为2.2×10-7~8.8×10-6mol/L,检出限为5.4×10-8mol/L。对浓度为7.8×10-6mol/L的L-半胱氨酸进行11次平行测定,其相对标准偏差为4.1%。该法已用于明胶中L-半胱氨酸的测定。     

水热法合成AgInS2/ZnS核/壳结构量子点及其荧光性能

以硫脲为硫源,采用谷胱甘肽(GSH)和柠檬酸钠(SC)为配体,通过水热法制备了水溶性AgInS2/ZnS(AIS/ZnS)核/壳结构量子点。系统研究了反应温度和配体用量对量子点的合成及其荧光性能的影响。采用X射线衍射(XRD)、透射电子显微镜(TEM)、紫外可见吸收光谱(UV-Vis)和光致发光光谱(PL)分别对量子点的物相、形貌和光学性能进行了表征,并考察了量子点的稳定性。实验结果表明,随着反应温度从70℃升高至90℃,促进了ZnS壳层的形成,有效地钝化了量子点的表面缺陷,获得的AIS/ZnS核/壳量子点的发光强度显著提高,发光峰位从600 nm蓝移至580 nm。配体的添加可以有效地平衡Zn^2+的化学反应活性,减缓ZnS壳层的生长,抑制核壳界面缺陷的形成,还能消除量子点的表面态,当nGSH/nZn^2+=2.0,nSC/nZn^2+=2.5时,AIS/ZnS量子点的荧光性能最佳。此外,AIS/ZnS核/壳结构量子点还具有优异的光学稳定性。     

硫氮共掺杂碳量子点荧光识别Pb~(2+)

以L-半胱氨酸为碳源、硫源及氮源,一步水热法制得水溶性好、稳定性高的硫氮共掺杂碳量子点SN-CDs。基于Pb~(2+)对其荧光的淬灭作用,构建了高选择性与高敏感度的荧光探针,可应用于Pb~(2+)的快速检测。运用透射电镜、紫外-可见吸收光谱、Fourier红外光谱和荧光光谱表征了SN-CDs的结构及光学性能。结果表明,Pb~(2+)浓度在2～50μmol/L范围内,与SN-CDs的荧光淬灭率之间呈良好的线性关系,相关系数为0.9992,检出限为0.2μmol/L。方法用于自来水中Pb~(2+)的测定,回收率为94.7%～100.7%。     

Absence of superconductivity in LiCu2P2

We successfully synthesized the copper-based pnictide LiCu(2)P(2), which was reported as a superconductor with T(c) = 3.7 K before. The temperature dependence of resistivity and DC magnetization was measured on both polycrystalline and single-crystalline LiCu(2)P(2). However, our repeatable synthesizing and measurements showed no superconducting transition either in resistivity or DC magnetization above 2 K. A metallic behavior can be seen in resistivity, and a Curie-Weiss behavior was observed in DC magnetization from 2 to 300 K. We have also carried out the Hall effect and MR measurements on the sample, from which we conclude that the LiCu(2)P(2) has a single-band character. We also synthesized the polycrystalline Li(1-x)Cu(2)P(2), LiCu(2-x)P(2), and Li(1+x)Cu(2-x)P(2) with different stoichiometries, and observed no superconductivity in all the samples.     

Radiolysis of 2-propanol in presence of 2-hexanoylfuran

2-hexanoyl-5-(2-hydroxy 2-propyl)furan (HHPF), has been investigated as the principal product of radiolysis of 2-hexanoyl-furan (HF) in 2-propanol. The effect of absorbed dose on the product yields has been examined. Possible mechanisms for the formation of radiolytic products are discussed.     

Insertion of acetylenes in the PdPd bond of Pd2 (Ph2 PCH2 PPh2)2 Cl2

Dimethylacetylene dicarboxylate and hexafluoro-2-butyne add to Pd₂(dpm)₂Cl₂ (dpm = Ph₂PCH₂PPh₂) to give crystalline adducts Pd₂(dp)₂(μ-acetylene)Cl₂. An X-ray crystal structure of Pd₂(dpm)₂(μ-C₄F₆)Cl₂ reveals that the acetylene has inserted into the metalmetal bond and has been transformed into a cis-dimetallated olefin. The central CC bond length of the bridging olefin is 1.338(16) Å. The coordination about each of the two similar palladium ions is planar and involves two trans-phosphines (one from each of the bridging dpm ligands), a terminal chloride, and one carbon of the bridging olefin. Both Pd₂(dpm)₂Cl₂ and Pd₂(dpm)₂(μ-C₂{CO₂H₃}₂)Cl₂ catalyze the cyclotrimerization of dimethyl-acetylene dicarboxylate.     

Synthesis of Gels in the System Na2O-ZrO2-SiO2

Gels have been synthesized in the SiO₂-Na₂O-ZrO₂ system and calcined at various temperatures up to 700°C. They have been studied by infrared absorption spectroscopy. The position of the asymmetric stretching frequency of the SiO₄ unit is used as a tracer of the homogeneity. It is shown that sodium increases the solubility of zirconium in the silica matrix as already observed in fused glasses.     

在乙二醇溶液中原位法制备纳米SnO2

乙二醇;锡配合物;溶胶 凝胶;纳米SnO2     

纳米ZrO2在O2/H2气中的表面效应

用ESR方法研究了一种纳米ZrO₂在普通H₂气中升温条件下的表面效应.ZrO₂上Zr³⁺的中心量约为1×10^-7mol/g.这些Zr³⁺中心是ZrO₂表面一些O^2-配位不饱和的Zr原子点位.在普通H₂气中,ZrO₂上的Zr³⁺中心数在温度低于400℃时变化很小.但在这一温度范围内从室温升温时,由ZrO₂表面羟基的H₂还原引起的F中心量随温度的升高而增加.温度高于400℃时,ZrO₂表面的Zr³⁺及F中心可与普通H₂气中存在的少量O₂气作用产生O₂^-,并伴随ZrO₂表面羟基的脱除而形成新的Zr³⁺.     

Radiolysis of 2-acetylfuran in 2-propanol in absence of atmospheric oxygen

Gamma radiolysis of 2-acetylfuran (AF) in 2-propanol, in absence of atmospheric oxygen, has been investigated. The radiation yields of hydrogen, methane at different doses as well as radiolytic products in solution were determined. The radiolytic products were determined by gas chromatography coupled with mass spectrometry. The mechanisms for formation of detected radiolytic products and the effect of (AF) concentration on hydrogen and methane yields are discussed.     

Interaction of components in the HgBr2-CdBr2-PbBr2 ternary system

The interaction in the HgBr₂-CdBr₂-PbBr₂ ternary system was studied by differential thermal analysis; the isoconcentration section of the system at 50 mol % CdBr₂ was investigated. Based on the results of the study, a projection of the liquidus surface of the HgBr₂-CdBr₂-PbBr₂ ternary system to the composition triangle was constructed; the boundaries of the primary crystallization fields were determined for three phases: HgBr₂ (degenerate field), solid solution α based on CdBr₂, and solid solution β based on PbBr₂; and isotherms were drawn. A ternary eutectic has the composition 93 mol % HgBr₂-1 mol % CdBr₂-6 mol % PbBr₂ and melts at 235°C.     

Hydrazinocyanation of 2, 2'-methylenedicyclohexanone in aqueous alcohol

The reaction of 2,2'-methylenedicyclohexanone with HCN and hydrazine in aqueous alcohol was studied at various pH values. Conclusions were drawn regarding the spatial configurations of the reaction products.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1387–1390, October, 1972.