催化过硫酸钾氧化银-邻二氮菲-荧光黄离子缔合物褪色光度法测定痕量铋(Ⅲ)

基于 p H=5.50弱酸性介质中 ,铋 ( )催化 K2 S2 O8氧化 [Ag(phen) 2 ]+ · [FIn]-离子缔合物的褪色反应 ,建立了一种催化褪色光度法测定痕量铋 ( )的新方法。该方法线性范围为 0 .0 4— 0 .4 mg/ L,检出限为 6 .0× 10 -11g/ m L。用于发样及水样中 Bi( )的测定 ,获得了令人满意的结果 ,并对反应的机理进行了探讨。     

反相高效液相色谱法测定1-(4-硝基苯)-3-(5-溴-2-吡啶)-三氮烯

ZORBAX Eclipse XDB- C8(4.6× 1 5 0 mm,5 μm)色谱柱 ,乙腈流动相 ,流速 0 .6 0 m L/min,检测波长4 2 0 nm,反相高效液相色谱法测定 1 - (4-硝基苯 ) - 3- (5 -溴 - 2 -吡啶 ) -三氮烯。该法的线性范围为 1—1 0 .0 μg/m L,线性回归方程为 A=5 .91 5 4 .4 37C,相关系数 0 .9989,相对标准偏差为 0 .8973%(C=7.2 0 μg/m L,n=5 ) ,检出限为 0 .0 2 872 μg/m L,平均回收率在 93.2 %— 1 0 2 .2 %之间。     

光泽精化学发光体系的研究与应用

对光泽精化学发光体系的动力学性质、荧光光谱、化学发光光谱及化学发光机理进行研究和探讨。详细研究了光泽精 - H2 O2 - Co( )流动注射化学发光体系的最佳分析条件。结果表明 ,当光泽精 (L c)为 2 .5×10 - 5mol/L、H2 O2 为 0 .5 mol/L、Na OH为 0 .4 mol/L、CTMAB为 2 .0× 10 - 5mol/L时 ,测定 Co( )的校准曲线线性范围为 0 .0 5— 2 0 0μg/m L ,检出限为 0 .0 1μg/m L。对 10μg/m L Co( )连续测定 7次 ,相对标准偏差为 1.7%。     

高效液相色谱法测定金盏菊中叶黄素

KNAUER Eurospher- 1 0 0 C1 8(3.9mm× 30 0 mm,4 .6 μm)色谱柱 ,以乙腈 -甲醇 -乙酸乙酯混合液为流动相 ,流速 1 .0 m L/ min;检测波长 4 6 0 nm;柱温 2 5℃ ,高效液相色谱法测定金盏菊中叶黄素含量。校准曲线法定量 ,检出限为 3.0 mg/ m L。叶黄素含量在 8— 6 4mg/ L之间线性关系良好 ,r=0 .9999,RSD=1 .4 % ,回收率在 97%— 1 0 1 %之间。本法适合叶黄素产品中叶黄素含量的测定     

碘蓝分光光度法测定微量铬（Ⅳ）

基于在酸性介质中 ,重铬酸钾与碘化钾、淀粉的显色反应 ,建立了碘蓝分光光度法测定微量铬 ( )的方法。铬 ( )浓度在 0— 0 .6μg/ m L范围内有良好的线性关系 ,方法的相对标准偏差为 1.3% ,表观摩尔吸光系数为 5 .6 3× 10 4 L· mol- 1 · cm- 1 ,检出限为 2 .0× 10 - 3μg/ m L     

高效液相色谱法测定2-苯基-4-对甲苯基-1,5-苯并硫氮杂-α-(丁二酰亚胺基)-β-内酰胺

本文采用 Hypersil- ODS2 (4 .6mm× 2 5 0 mm,5μm)色谱柱 ,乙腈 -水 (70∶ 30 )流动相 ,2 4 2 nm测定波长 ,建立了测定 2 -苯基 4 -对甲苯基 - 1,5 -苯并硫氮杂 艹卓 -α- (丁二酰亚胺基 ) -β-内酰胺高效液相色谱法。该法线性范围为 0— 0 .1mg/ m L,回归方程 A=2 .11× 10 8C- 3.10× 10 5,相关系数 r=0 .9995 ,相对标准偏差为0 .2 4 % (C=0 .0 6mg/ m L,n=5 ) ,检出限为 0 .0 5 μg/ m L。平均回收率在 97.1%— 10 2 .4 %之间。该法重现性好、灵敏度高、简单、快速、准确     

高效液相色谱法测定小儿盐酸二氧异丙嗪冲剂的含量

采用高效液相色谱法测定盐酸二氧异丙嗪的含量。色谱柱为 DIKMATMRPC18(4 .6 mm× 2 0 cm,5 μm) ,流动相为乙腈 - 0 .5 %磷酸二氢钾 -三乙胺 (5 0∶ 5 0∶ 0 .2 ) ,用磷酸调 p H值至 6 .8± 0 .1;流速为1.0 m L/ min,检测波长为 2 6 4nm。该法回收率为 99.6 % ,RSD=0 .6 1%。盐酸二氧异丙嗪在浓度为0 .0 184 8— 0 .0 4 312 mg/ m L范围内线性关系良好。相关系数为 r=0 .9999。该方法操作简便 ,结果准确可靠。     

双波长标准加入法同时测定钴镍合金镀液中的钴(Ⅱ)和镍(Ⅱ)

在 p H5 .0的乙酸 -乙酸钠缓冲溶液和聚乙烯醇体系中 ,钴 ( )和镍 ( )可与 PAN试剂形成稳定的络合物。以钴 ( )的 5 80 nm和 6 2 6 nm为测定波长对 ,镍作标准加入组分 ,双波长标准加入法可同时测定试样中钴、镍的含量。镍在 0— 15 μg/2 5 m L,钴在 0— 10 μg/2 5 m L范围内遵从比耳定律。对镀液样品进行测定 ,镍、钴的相对标准偏差 (n=6 )分别 <0 .82 %和 <1.2 %。     

高效液相色谱法测定2-对甲氧基苯基-4-苯基-1,5-苯并硫氮杂-α-(丁二酰亚胺基)-β-内酰胺

应用高效液相色谱外标定量法对 2 -对甲氧基苯基 - 4 -苯基 - 1,5 -苯并硫氮杂 艹卓 -α- (丁二酰亚胺基 ) -β-内酰胺进行了测定。采用 Hypersil- ODS2 ( 4 .6mm× 2 5 0 mm,5 μm)柱 ,乙腈与水按 70∶ 30 ( V/ V)组成流动相 ,测定波长为 2 4 2 nm,该方法线性范围为 0— 0 .1mg/ m L ,回归方程 A=1.91× 10 8C- 3.82× 10 5,相关系数 r=0 .9994 ,相对标准偏差为 0 .72 %,检出限为 0 .0 5μg/ m L,平均回收率在 98.4 %— 10 1.8%之间。该法重现性好、灵敏度高、简单、快速。     

单扫描极谱法测定有机锗(Ge-132)

在 p H2 .0的 K2 SO4 介质中 ,有机锗 (Ge- 132 )在单扫描示波极谱仪上于 - 0 .13V(vs.Ag Cl/ Ag)和- 1.0 5 V(vs.Ag Cl/ Ag)处产生两个还原波 ,其中 - 1.0 5 V(vs.Ag Cl/ Ag)波灵敏、波形好。峰电流与 Ge-132在 1.0× 10 - 5— 5 .0× 10 - 4mol/ L范围内呈良好的线性关系 ,其检出限为 8.9× 10 - 5mol/ L。该方法用于有机锗营养口服液中 Ge- 132的测定 ,结果较好     

Preparation of silver nanoparticles by laser ablation in polyvinylpyrrolidone solutions

We performed laser ablation of a silver plate in polyvinylpyrrolidone (PVP) aqueous solutions to prepare silver nanoparticles. Secondary laser irradiation onto the prepared colloidal solutions was also carried out. It was revealed that the formation efficiency was increased by addition of PVP as well as the stability of nanoparticles. The result of shadowgraph measurements suggested that the increased ablation efficiency by PVP is attributable to increased secondary etching efficiency by the solvent-confined plasma toward the silver plate. On the other hand, the size decrease of the nanoparticles by addition of PVP was more remarkable during the secondary irradiation process than in the laser ablation (nanoparticle preparation) process. This result indicates that emitted materials interact less sufficiently with PVP molecules in the laser ablation process than in the secondary laser irradiation process.     

Transparent chromatic electrode using the mixture of silver nanowire and silver nanoprism

In this research, we studied a chromatic transparent silver nanowire (Ag NW) electrode using a silver nanoprism (Ag NP). Ag NW and Ag NP were produced using a chemical synthesis method (polyol method) and deposited on substrate via spray method.The Ag NW electrode showed a more than 80% transmittance and no or low conductivity without high temperature annealing process. In the case of applying an annealing process, a 13 Ω/□ sheet resistance was measured.The electrode, which consisted of a mixture of Ag NW and Ag NP, showed a reduced transmittance of about 70%. However, by applying Ag NPs to a conventional bare Ag NW electrode, we were able to add a chromatic characteristic to the transparent electrode; this addition was induced by the localized surface plasmon resonance (LSPR) and the low sheet resistance, even though no annealing process was applied.     

Synergistic effect of silver seeds and organic modifiers on the morphology evolution mechanism of silver nanoparticles

Triangular, truncated triangular, quadrangular, hexagonal, and net-structured silver nanoplates as well as decahedral silver nanoparticles were manipulatively prepared starting from silver nitrate and silver seeds in the presence of poly(ethylene glycol) (PEG), poly(N-vinyl pyrrolidone) (PVP), and Tween 80 at room temperature, respectively. UV-vis spectroscopy, XRD, HRTEM, SAED, and FTIR were used to illustrate the crystal growth process and to characterize the resultant silver nanoparticles. It was found that the silver seeds and organic modifiers synergistically affected the morphology evolution of the silver nanoparticles. The co-presence of silver seeds and PEG was beneficial to the formation of triangular and truncated triangular silver nanoplates; the silver seeds and PVP favored the formation of polygonal silver nanoplates; the silver seeds and Tween 80 preferred to the formation of net-structured silver plates. The morphology evolution of the resultant silver nanoparticles was correlated with the crystallinity of the silver seeds and the adsorption ability of the organic modifiers on the crystal surfaces.     

Characteristics of light emission from surface plasmons based on rectangular silver gratings

We investigated the characteristics of transmitted light from propagating surface plasmons based on rectangular silver gratings. The results calculated by rigorous coupled-wave analysis presented that silver diffraction gratings can produce significant transmittance and conversion efficiency, comparable to the case of dielectric gratings. Especially, silver gratings optimized at a wide range of grating thickness and period may lead to an improved diffraction efficiency larger than 64%. Moreover, the effect of silver oxide layer on the transmittance was examined and a bimetallic structure with a thin gold coating was introduced to prevent an oxidation of silver substrates. As a practical sensor application, silver grating-based surface plasmon resonance (SPR) configuration showed an enhanced sensitivity associated with an increase of surface reaction area and strong excitations of local plasmon fields, outperforming a conventional thin-film-based SPR structure.     

Silver aggregates and twofold-coordinated tin centers in phosphate glass: A photoluminescence study

The optical properties of silver species in various oxidation and aggregation states and of tin centers in melt-quenched phosphate glasses have been assessed by optical absorption and photoluminescence (PL) spectroscopy. Glasses containing silver and tin, or either dopant, were studied. Emission and excitation spectra along with time-resolved and temperature-dependent PL measurements were employed in elucidating the different emitting centers observed and investigating on their interactions. In regard to silver, the data suggests the presence of luminescent single Ag⁺ ions, Ag⁺-Ag⁺ and Ag⁺-Ag⁰ pairs, and nonluminescent Ag nanoparticles (NPs), where Ag⁺-Ag⁰→Ag⁺-Ag⁺ energy transfer is indicated. Tin optical centers appear as twofold-coordinated Sn centers displaying PL around 400 nm ascribed to triplet-to-singlet electronic transitions. The optically active silver centers were observed in glasses where 8 mol% of both Ag₂O and SnO, and 4 mol% of Ag₂O were added. Heat treatment (HT) of the glass with the high concentration of silver and tin leads to chemical reduction of ionic silver species resulting in a large volume fraction of silver NPs and the vanishing of silver PL features. Further characterization of such heat-treated glass by transmission electron microscopy and X-ray photoelectron spectroscopy appears consistent with silver being present mainly in nonoxidized form after HT. On the other hand, HT of the glass containing only silver results in the quenching of Ag⁺-Ag⁰ pairs emission that is ascribed to nonradiative energy transfer to Ag NPs due to the positioning of the pairs near the surface of NPs during HT. In this context, an important finding is that a faster relaxation was observed for this nanocomposite in relation to a heat-treated glass containing both silver and tin (no silver pairs) as revealed by degenerate four-wave mixing spectroscopy. Such result is attributed to Ag NP→Ag⁺-Ag⁰ plasmon resonance energy transfer. The data thus indicates that energy transfer between Ag⁺-Ag⁰ pairs and NPs is bi-directional.     

银离子测试试纸色阶的制备

本实验研制了一种测试银离子浓度的试纸.用于溶液中银离子浓度的快速测定.     

Electroless deposition of silver on synthesized calcite via surface modification

Metallic silver was deposited on the surface of synthesized calcite via a simple electroless deposition method. Calcite with cubic morphology was prepared first by homogeneous precipitation and it was subsequently surface modified using ammonium oxalate. The electroless deposition was carried out using formaldehyde as the reducing agent and silver nitrate as the silver source. Both calcite and the silver deposited calcite were characterized by different techniques. Surface modification of calcite with ammonium oxalate is necessary for the deposition of silver and the size of the deposited silver particles could be controlled by changing the deposition parameters such as concentration of the reagents and the deposition time. Lower concentration of silver ions (e.g. 0.01 M AgNO₃) and shorter deposition times (e.g. 30 min) lead to the formation of silver nanoparticles on calcite.     

Organic SIMS with single massive gold projectile: Ion yield enhancement by silver metallization

The yield of CN from glycine rises from one CN per projectile impact to two when the sample is covered with a nominally 1 nm thick layer of silver. These yields were obtained for bombardment with Au₄₀₀⁴⁺ projectile with 136 keV impact energy. A multitude of CN-based clusters, e.g. Ag_xO_y(CN)_z are produced concurrently. As a result, a total of three CN-based secondary ions are generated per projectile impact. The exceptionally high yield for CN is of interest for biological SIMS.     

Silver ionic conductivity enhancement by network former mixed in oxide-based glasses

Glasses in the binary system xAg₂P₂O₆ − (1 − x)Ag₂Te₂O₅ have been prepared for 0 x 1. For each composition only one glass transition temperature is observed in the temperature range of 180–220 °C. All glasses appear homogeneous considering their optical and electrical properties. Nevertheless, in SEM observations, some glass compositions appear to be heterogeneous after decoration following short nitric acid etching. For each composition, conductivity data obtained in the temperature range of 25–200 °C using impedance techniques obey an Arrhenius relationship with a composition independent pre-exponential term. Variation of the conductivity activation energy with x induces correlative variations of isothermal conductivity curves leading to an increase of the ionic conductivity of about one order of magnitude compared with linearity at 25 °C. This behaviour is discussed with respect to the thermodynamic properties of the glassy solutions.     

银纳米立方体的合成及其SERS活性研究

用乙二醇还原硝酸银,以聚乙烯吡咯烷酮作表面活性剂合成了银纳米立方体晶粒,并以吡啶和SCN-作为探针分子初步研究了银纳米立方体晶粒组装体系的SERS活性。当探针分子吸附于银纳米立方体晶粒上时,吡啶和SCN-的谱峰强度明显增强,表明银纳米立方体晶粒可望作为SERS活性基底。通过研究探针分子的SERS强度与粒子尺度关系,也有望用于表征银纳米立方体晶粒的光学性质。