基于细胞阻抗传感器的腹泻性毒素检测系统设计与实现

针对海洋水产品腹泻性毒素检测问题,设计了一种新型的基于细胞阻抗传感器(ECIS)的毒素快速检测分析系统。相对于传统的毒素检测方法,该系统具有操作简便,高一致性和高通量等特点。介绍了系统的硬件设计和软件设计,通过对系统整体性能测试以及使用神经母细胞瘤细胞(Neuro-2a)对腹泻性贝毒(DSP)大田软海绵酸(OA)进行毒性检测实验,用以验证系统平台的可行性。实验结果表明,基于细胞传感器的海洋水产品腹泻性毒性检测系统具备快速,长期,无损和高通量测量的特点,为腹泻性毒素检测提供了新的平台。     

Reductive alkylation of illinois No. 6 coal. 1H and 13C n.m.r. spectra of the 13C-enriched alkylation products

The reductive alkylation of Illinois No. 6 coal has been carried out using potassium and naphthalene in tetrahydrofuran and methyl-¹³C and butyl-1 -¹³C iodides to alkylate the resultant polyanion. The soluble products of the reductive alkylation reaction were isolated by extraction and chromatography. Proton and carbon n.m.r. spectra were recorded. The intense resonance signal at δ3.95 which appears in the proton n.m.r. spectra of Illinois No. 6 coal butylated with unenriched butyl iodide is split into a doublet by the ¹³C nuclei. Similar results were obtained for the methylation products. The chemical shift and coupling interaction establish that aryl ethers are a very important constituent of the alkylated coal. The carbon n.m.r. spectra of the coal alkylated with ¹³C-enriched alkyl iodides are intense. The resonances of the C-alkylation products appear in a single broad band with a maximum intensity in spectral regions compatible with the formation of the reductive alkylation products of certain polynuclear aromatic hydrocarbons or the base-catalysed alkylation of certain benzylic carbon atoms. The resonances of the N -alkylation products appear in two distinct bands. These resonances are tentatively assigned to amines produced as a result of reductive alkylation of heterocyclic compounds. The resonances of the 0-alkylation products appear in three distinct bands which can be assigned to alkyl aryl ethers, alkyl aryl ethers with substituents at the adjacent positions, and to alkyl carboxylates. The ratio of ethers to carboxylates in the soluble alkylation products was determined to be 7.8 for butylation and 8.0 for methylation. The Chromatographic fractions contain different amounts of C-, N-, and 0-alkylation products. This finding suggests that the coal structure is not highly uniform.     

An electrochemical impedance spectroscopy and scanning electron microscopy study of the influence of positive plate compression on the electrochemical behaviour of lead-acid batteries

This study has developed an electrochemical impedance spectroscopy (EIS) method for the in situ investigation of the influence of positive plate compression on the electrochemical behaviour of lead-acid batteries during charge/discharge cycling. The EIS data for a fully charged and fully discharged battery are internally consistent with the expected kinetics of a battery in the opposite states of charge, and demonstrate that EIS measurements may be recorded with a high level of reproducibility. Furthermore, this study has necessitated the development of a special cell incorporating horizontally orientated battery plates that can be subjected to elevated pressure through the stacking of lead bricks on top of the cell, as well as a physically robust reference electrode system that can withstand the application of pressure. For this purpose, a platinum-wire pseudo-reference electrode has been developed, and has been shown to exhibit sufficient electrode stability over the period of an EIS recording, enabling the measurement of reproducible and meaningful EIS data. Additionally, the influence of positive plate compression on the behaviour of the lead-acid battery has been investigated by using scanning electron microscopy (SEM). Clearly, the experimental data show that plate compression enhances significantly the kinetics and concomitant performance of the lead-acid battery, and this is related to the enhanced reactivity of the active material, as rationalized by using the agglomeration-of-spheres (AOS) model.     

单溴四苯基卟啉吸附在AgCl溶胶表面性质研究

合成了单溴四苯基卟啉—— 5 - (邻溴苯基 ) - 1 0 ,1 5 ,2 0 -三苯基卟啉 (H2 L) ,用元素分析 ,红外光谱、电子吸收光谱和氢核磁共振谱确定了其组成和结构。研究了 H2 L在醋酸中电子吸收光谱和在 Ag Cl溶胶上的表面化学反应。结果表明 ,单邻溴四苯基卟啉在冰醋酸中以二酸形式 H4 L2 + 和游离碱 H2 L形式存在 ,二者之间存在着电离平衡 :H4 L2 + =H2 L+2 H+ ;当 p H=7.0～ 1 1 .0时 ,H2 L在Ag Cl溶胶表面发生配位反应生成 Ag( ) L,并且溶液的 p H增大 ,配位反应的速率增大。     

Characterization of boron-doped diamond electrodes by electrochemical impedance spectroscopy

Charge transfer on boron doped diamond (BDD) electrodes was studied by cyclic voltammetry and electrochemical impedance spectroscopy. The diamond films of 5 μm thickness and boron content between 200 ppm and 3000 ppm were prepared by the hot filament CVD technique on niobium substrate and mounted in a Teflon holder as rotating disk electrodes. The electrochemical measurements were carried out in aqueous electrolyte solutions of 0.5 M Na₂ SO ₄ + 5 mM K₃[Fe(CN)₆]/K₄[Fe(CN)₆]. Significant deviation in the redox behaviour of BDD and active Pt electrodes was indicated by a shift of the peak potentials in the cyclic voltammograms with increasing sweep rate and lower limiting diffusion current densities under rotating disk conditions. In the impedance spectra an additional capacitive element appeared at high frequencies. The potential and rotation dependence of the impedance spectra can be described quantitatively in terms of a model based on diffusion controlled charge transfer on partially blocked electrode surfaces. Direct evidence for the non-homogeneous current distribution on the diamond surface was obtained by SECM measurements.     

直接和间接电合成制备出的高铁酸钾的物理和电化学性能

K2FeO4 powders were synthesized by the ex-situ and in-situ electrochemical methods, respectively, and characterized by infrared spectrum （IR）, scanning electron microscopy （SEM）, X-ray powder diffraction （XRD） and BET. Their electrochemical performances were investigated by means of galvanostatic discharge and electrochemical impedance spectroscopy （EIS）. The results of physical characterization showed that the two samples have simi- lar structural features, but their surface morphologies and oriented growth of the crystals are different, which results in smaller specific surface area and lower solubility of the ex-situ electrosynthesized K2FeO4 sample. The results of discharge experiments indicated that the ex-situ electrosythesized K2FeO4 electrode has much larger discharge capacity and lower electrode polarization than the in-situ electrosynthesized K2FeO4 electrode. It was found from the results of EIS that lower electrochemical polarization might be responsible for the improvement on the discharge performance of the ex-situ electrosynthesized K2FeO4 electrode.     

化学镀Ni-P-Cr2O3和Ni-P-SiO2复合镀层的研究

本文对化学镀镍及化学镀镍磷基质中SiO2与Cr2O3的共沉积进行了研究.微粒在不断生长的膜层中共沉积引起了新的化学复合镀层的出现,这些复合镀层许多都具有优异的耐磨及耐蚀性能.通过选取镀层合金/复合微粒/金属基体的组分可改进镀层,获得所需的性能,以满足特别的需求.在对这些复合镀层的应用需求正在迫近与增长的同时,其市场正在迅速扩张.本文开发出了一种合适的复合化学镀镍液,并通过维氏硬度法对化学复合镀镍层进行了表征.采用动电位极化及交流阻抗法测定了镀层的Taber耐磨性能及耐蚀性能.采用SEM及XRD对复合镀层的表面形貌进行了分析.     

The influence of gun transverse speed on electrochemical behaviour of thermally sprayed Cr3C2-NiCr coatings in 0.5 M H2SO4 solution

In the present study, different types of 75% Cr₃C₂-25% NiCr coatings were applied on a steel substrate by means of high velocity oxygen fuel spraying (HVOF), and studied using ac and dc electrochemical measurements in an aerated and unstirred 0.5 M H₂SO₄ solution. Structural characterization was determined before and after electrochemical tests. Differences between all sprayed systems are related to the gun transverse speed and number of deposited layers, which strongly affected the electrochemical characteristics of the coated steels. The coating obtained with a higher torch speed showed better resistance against corrosion. The electrochemical impedance results were analyzed using an equivalent circuit where porosity of the coatings and substrate oxidation were considered.     

Electrochemical behaviour of heat-treated AlZnMg alloys in chloride solutions containing sulphate

The electrochemical corrosion and passivation of Al5Zn1.7Mg0.23Cu0.053Nb alloys, submitted to different heat treatments (cold-rolled, annealed, quenched and aged, and quenched in two steps and aged), in sulphate-containing chloride solutions, has been studied by means of cyclic polarization, electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and X-ray photoelectron spectroscopy (XPS). The cyclic polarization curves showed that sulphate addition to the chloride solution produced a poor reproducible shift of the breakdown potential to more positive potentials. The repassivation potentials, much more reproducible, and practically separating the passive from the pitting potential region, were slightly displaced in the negative direction with that addition. When the alloys were potentiodynamically polarized in the passive potential region, sulphate was incorporated in the oxide film, thus precluding chloride ingress. In addition, Zn depletion was favoured, whereas Mg losses were avoided. Different equivalent circuits corresponding to different alloys and potentials in the passive and pitting regions were employed to account for the electrochemical processes taking place in each condition. This work shows that sulphate makes these alloys more sensitive to corrosion, increasing the fracture properties of the surface layer and favouring the pitting attack over greater areas than chloride alone.     

丹参水浸提液的荧光光谱特性

釆用三维和二维荧光法对中药丹参水浸提液的荧光特性进行了研究。丹参水浸提液在三维荧光等高线光谱中出现2个荧光峰,其激发波长分别为2433、37 nm,发射波长为437 nm。丹参素、丹参酚酸A、丹参酚酸B及原儿茶醛与丹参水浸提液的二维荧光光谱比较研究表明,丹参水浸提液的荧光光谱是各种丹参酚酸化合物的荧光光谱的叠加,其中丹参酚酸B对丹参水浸提液荧光强度贡献最大,且荧光发射波长相同。在近中性条件下,丹参水浸提液荧光强度与浓度之间呈良好的线性关系,可以作为定量分析丹参中总酚酸的依据。丹参水浸提液的三维荧光光谱具有指纹图谱特征,可以用于丹参的定性鉴别。在pH 7.0~12.7丹参水浸提液荧光发射光强度随pH增大呈现递减甚至消失的变化,同时丹参素的380 nm荧光有所增强,丹参酚酸化合物在碱性环境下易于水解应该是其主要原因。