Low-temperature bath/coupled-capillary/sweeping-micellar electrokinetic capillary chromatography for the separation of naphthalene-2,3-dicarboxaldehyde-derivatized dopamine and norepinephrine

The use of a low-temperature (0 degrees C) bath-assisted coupled capillary for the separation of naphthalene-2,3-dicarboxaldehyde (NDA)-derivatized dopamine and norepinephrine using the sweeping-micellar electrokinetic capillary chromatography (MEKC) mode is described. In this technique, a capillary consisting of two portions with different inside diameters is used. Therefore, the field strength inside the capillary is different. Hence, the electrophoretic migration velocities of the analytes and the electro-osmotic flow (EOF) also are different. Furthermore, when a portion of the capillary (wide portion, used for sweeping) is immersed in a low-temperature bath, the viscosity of the buffer and the retention factor of the analytes inside are increased. Thus, not only are the interactions between the SDS micelles and the analytes increased, but the SDS-analytes also move more slowly. As a result, a more complete separation can be achieved, even when the sample injection volume is large, up to approximately 2 microL. In general, when the volume of an injected sample is larger, the effects of sweeping and separation would become insufficient, especially when the retention values (k) of the analytes are quite different. However, this limitation can be improved when the low-temperature bath/coupled capillary/sweeping-MEKC mode is used.     

Highly Sensitive AdSV Method for Fe(III) Determination in Presence of Solochrome Violet RS on Renewable Amalgam Film Electrode

The new DP AdSV method for high sensitive Fe(III) determination in the presence of Solochrome Violet RS was developed. The use of an innovative renewable amalgam film electrode Hg(Ag)FE allowed to obtain high sensitivity and significantly minimize the mercury consumption. The best results were obtained for surface area of Hg(Ag)FE equal to 11.8 mm². Instrumental parameters were optimized. The optimal results were obtained using differential pulse technique for the following values: sampling and waiting time ts=tw=10 ms, step potential Es=5 mV, pulse amplitude ΔE=50 mV. Measurements were conducted in 0.05 M acetate buffer (pH 5.6), the concentration of SVRS was equal to 5 μM. Deposition step was carried out at the potential ?400 mV for 20 s. Calculated detection limit for 40 s preconcentration time was equal to 1.4 nM (78 ng L^?1). The influence of the common in environment, organic and inorganic interferences was studied. The developed method for Fe(III) determination was successfully applied and validated by investigation of certified reference material SPS‐SW2 Batch 118 and recovery of Fe(III) from various spiked samples as snow, tap water and bottom sediments. The repeatability (for 50 nM of Fe(III)) of the developed method expressed as CV was equal 3.1 % (n=5).     

结晶紫在纳米磷化镓粉体表面吸附的表面增强拉曼光谱分析

利用Raman光谱对结晶紫(Crystal Violet,CV)在纳米磷化镓(GaP)粉体表面的吸附状态进行了分析.结果表明:与普通拉曼散射谱(Normal Raman Scattering,NRS)相比,结晶紫表面增强拉曼散射(Surface Enhanced Raman Scattering,SERS)谱的4种振动模式,即:中央键的呼吸振动、环-C -环面外弯曲振动、环C-H面外弯曲振动以及N-环伸缩振动,在纳米GaP粉体表面得到增强;通过分析吸附前后结晶紫拉曼散射峰相对强度的变化,确定了结晶紫在纳米GaP粉体表面的吸附取向,并对其表面增强散射机理进行了探讨.     

Speciation of aluminium fluoride complexes and Al in soils from the vicinity of an aluminium smelter plant by hyphenated High Performance Ion Chromatography Flame Atomic Absorption Spectrometry technique

The paper presents a new tool for the determination of inorganic speciation forms of aluminium: AlF_n^{(3 − n)+}, and Al³⁺ by means of the HPIC-FAAS. The proposed method has been successfully used for speciation analysis (qualitative and quantitative) of inorganic aluminium forms AlF_n^{(3 − n)+} in soil samples. In order to isolate the most environmentally available fraction, 5 g of the sample was collected and extracted in deionised water (water soluble fraction) for 1 h using a magnetic stirrer. The determinations in a hyphenated technique system were performed for a number of prepared water extracts. Concentration determinations of particular aluminium forms were performed based on model studies and real samples. The separation of Al species with nominal charge of + 1, + 2, and + 3 required a run time of less than 4 min during a single analysis. Based on the analysis of water extracts of soil, it was obtained that aluminium forms elute in the following order: 1PA (first signal) — AlF₂⁺ and/or AlF₄⁻; 2PA (second signal) — AlF²⁺ and/or AlF₃⁰; 3PA (third signal) — Al³⁺. In order to confirm the occurrence of these forms a simulation using the Mineql program was conducted. The details of speciation analysis of aluminium fluoride forms by means of an HPIC-FAAS instrument equipped are presented. Interpretation of the speciation analysis of the water soluble fraction of soil samples is proposed, based on the separation during chromatographic run and calculated data by Mineql.     

4O6.7～415.4nm和632.8nm辐射在人肺组织中的穿透深度

在对作者原有工作改进的基础上，应用自行研制的“光纤探针深度计”首次精确测定了Kr+紫激光406．7～415．4um和He-Ne激光632．8nm波长处新鲜离休人肺组织中光能流率分布，获得这两种重要波长处人肺正常组织和人肺腺鳞癌组织中光能流率的分布规律及光穿透深度的数值：（1）δnormal=0.08mm,δtumour=0.32mm(λ=406.7～415.4nm);(2)δnormal=1.19mm,δturmour=1.70mm(λ=632.8nm),并对现有人肺组织的光穿透深度数据作了总结和讨论．     

Tuning the properties of a black TiO2-Ag visible light photocatalyst produced by a rapid one-pot chemical reduction

A highly efficient black TiO₂-Ag photocatalytic nanocomposite, active under both UV and visible light illumination, was synthesized by decorating the surface of 25 nm TiO₂ particles with Ag nanoparticles. The material was obtained via a rapid, one-pot, simple (surfactant and complexing agent free) chemical reduction method using silver nitrate and formaldehyde as a metal salt and reducing agent, respectively. The nanocomposite shows an increase of over 800% in the rate of photocatalytic methylene blue dye degradation, compared to commercial unmodified TiO_2, under UV-VIS illumination. Unlike pure TiO₂, the nanocomposite exhibits visible light activation, with a corresponding drop in optical reflectance from 100% to less than 10%. The photocatalytic properties were shown to be strongly enhanced by post-reduction annealing heat treatments in air, which were observed to decrease, rather than coarsen, silver particle size, and increase particle distribution. This, accompanied by a variation in the silver surface oxidation states, appear to dramatically affect the photocatalytic efficiency under both UV and visible light. This highly active photocatalyst could have wide ranging applications in water and air pollution remediation and solar fuel production.     

催化动力学光度法测定痕量锰--Mn(Ⅱ)-NTA-茜素紫3B-KIO4体系

在硼砂介质中 ,利用氨三乙酸活化 Mn( )催化 KIO4 氧化茜素紫 3B褪色的指示反应 ,建立了催化光度法测定痕量锰的新方法。方法的线性范围为 0 .0 30— 6 .0μg/ L ,检出限为 1.0× 10 -11g/ m L ,用于水样和茶叶中锰的测定 ,结果令人满意。     

2D reduced graphene oxide–titania nanocomposites synthesized under different hydrothermal conditions for treatment of hazardous organic pollutants

Two-dimensional reduced graphene oxide–titania (RGO–TiO₂) composites were prepared using a single-step hydrothermal method under various hydrothermal reaction conditions. The morphological and surface characteristics of the RGO–TiO₂ composites and reference materials were determined. The RGO–TiO₂ composites showed photocatalytic activity for the decomposition of two target pollutants that was superior to both pure TiO₂ and RGO under fluorescent daylight lamp illumination. The photocatalytic activity of the RGO–TiO₂ composite increased as the hydrothermal treatment time increased from 1 to 24 h, but then it decreased as the time increased to 36 h, which indicated the presence of an optimal treatment time. RGO–TiO₂ composites activated by violet light-emitting diodes (LEDs) displayed lower decomposition efficiency than those activated by a daylight lamp, likely because of the lower light intensity of violet LEDs (0.2 mW/cm²) when compared with that of the daylight lamp (1.4 mW/cm²). However, the photocatalytic decomposition of the target pollutants using the RGO–TiO₂ composite was more energy-efficient using the violet LEDs. The photocatalytic reaction rates increased as the residence time decreased, whereas the reverse was true for the decomposition efficiency.     

纳米GaP粉体对结晶紫的光催化降解及其振动光谱分析

对纳米 Ga P粉体 -结晶紫水溶液光催化降解进行了研究。纳米 Ga P粉体在紫外光照射条件下对结晶紫具有光催化降解作用 ;随平均颗粒度的降低 ,纳米 Ga P粉体的光催化活性增加。红外光谱测试结果表明 :进行光催化过程以后 ,纳米 Ga P表面存在的几种主要振动模式变化较小或不变 ;拉曼光谱测试结果表明 :纳米 Ga P粉体的横向光学声子模与纵向光学声子模 ,以及表面主要振动模式几乎没有发生变化     

三元配合物光度法测定痕量钴的研究

本文提出了 Co( ) -硫氰酸钾 -结晶紫 -聚乙烯醇三元配合物体系光度法测定 Co( )的新方法。该方法灵敏度 ε=3.18× 10 5L·mol-1· cm-1,选择性好 ,精密度高 ,用于水中痕量钴的测定。结果令人满意