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1.
本文提出在原子吸收光谱测定中,采用Smith-Hieftje法校正背景时,空心阴极灯供电条件(即最佳宽窄脉冲电流)的选择依据和选择方法;并给出24个常见元素的宽窄脉冲电流的选定结果。  相似文献   

2.
Pt微粒修饰纳米纤维聚苯胺电极对甲醇氧化电催化   总被引:9,自引:0,他引:9  
以脉冲电流法制备的纳米纤维状聚苯胺(PANI)为Pt催化剂载体,用它制备了甲醇阳极氧化的催化电极Pt/(nano-fibular PANI).研究结果表明, Pt/(nano-fibular PANI)电极对甲醇氧化具有很好的电催化活性,并有协同催化作用.在相同的Pt载量条件下, Pt/(nano-fibular PANI)电极比Pt微粒修饰的颗粒状聚苯胺电极Pt/(granular PANI)具有更好的电催化活性.此外, Pt的电沉积修饰方法同样影响Pt/(nano-fibular PANI)电极对甲醇氧化的催化活性.脉冲电流法沉积Pt形成的复合电极较循环伏安法电沉积得到的Pt复合电极具有更优异的催化活性.  相似文献   

3.
脉冲电流法电解合成聚苯胺   总被引:4,自引:0,他引:4  
在0.2mol/L苯胺和0.5mol/LH2SO4介质中采用脉冲电流法电解合成聚苯胺(PANI)膜.循环伏安研究表明,与恒电流法相比,脉冲电流法制得的PANI膜具有更好的电化学活性.扫描电镜(SEM)对膜层的微观形貌观察发现,这种特殊的聚苯胺膜层呈纳米纤维状结构,不同于恒电流法制取的颗粒状PANI膜.讨论了脉冲通断比和频率对于膜层性能的影响.  相似文献   

4.
莫金垣  张润建 《分析化学》1995,23(3):255-258
本文提出平行催化体系的对位叠式循环方波伏安法,并对共作了系统的研究,推导了这一方法的催化电流理论方程,并用验验证这理论的正确性,得到其各脉冲电流皆为同方向,对位叠式循环催化电流相当于将电流叠加4次,而波形不受方波幅度大小的影响,因而灵敏度和分辨率有较大提高,优于其它方波伏安法。  相似文献   

5.
在零电流条件下测量离子选择电极的电位分析已成为一种重要的电分析化学方法.Buck等首先用交流阻抗法研究了玻璃膜、晶态膜、液膜及PVC膜等一些电极的交流阻抗行为,Cammann和Rechnitz等用恒电位和恒电流阶跃法研究了缬氨霉素钾电极的极化行为,Powley等用双脉冲方法测定了Ca~(++)、F~-等电极的电导行为,并根据脉冲电流和溶液离子浓度的关系提出了离子选择电极的双极性脉冲电导分析法.到目前为止,还未见有功能高分子膜离子选择电极电化学极化行为研究的报道. 本文用快速三角波电位法和快速方波电位法研究了功能高分子压片PVC膜氯离子选择电极的暂态极化行为,计算了膜电极的一些电化学参数,讨论了影响膜电化学性质的因素.  相似文献   

6.
两步法制备多孔硅及其表征II:脉冲电流法   总被引:1,自引:1,他引:0  
采用脉冲阳极/阴极电流和化学氧化两步法分别在1:1的氢氟酸和乙醇溶液中及20%硝酸溶液中制备出孔径约为0.5-3μm,厚度大约为10-20μm的多孔硅样品,将获得的多孔硅结构再进一步用扫描电子显微镜和拉曼光谱仪进行表面形貌和光学性质的考察,与恒电流-化学氧化两步法制得的多孔硅相比,用脉冲电流法得到的多孔硅的孔径范围较大,且多孔层较厚,制备时加紫外光照显著提高了多孔硅的,并发生“蓝移”现象,用脉冲电流法制得的多孔硅在老化后(在干燥器放置一年)同样观察到光致发光明显增强。  相似文献   

7.
二氧化碳和氧气的快速电化学方法联合测定   总被引:4,自引:0,他引:4  
周仲柏  柳文军 《分析化学》1997,25(6):635-639
根据O2和CO2在二甲亚砜(DMSO)介质中Pt电极上的伏安特性,采用微电极并结构计算机控制的电位调制技术,建立了快速联合测定CO2和O2的调制电位脉冲库仑法和调制电位脉冲电流法,取得了满意的结果。一次测量时间快达40ms。CO2检测范围0 ̄10%(体积百分比);O2检测范围不受限制。通过编程设计特定的调制电位-时间波形,可保持连续检测的长期稳定性。  相似文献   

8.
本文用Laplace变换和正则摄动法求解旋转圆盘电极体系的对流扩散方程, 得到精确的级数解, 并拟合得到近似公式。从该公式出发, 经Laplace变换运算, 本文得到了大幅度电位阶跃过程的电流公式和脉冲电流过程的极限电流公式。  相似文献   

9.
本文用Laplace变换和正则摄动法求解旋转圆盘电极体系的对流扩散方程,得到精确的级数解,并拟合得到近似公式。从该公式出发,经Laplace变换运算,本文得到了大幅度电位阶跃过程的电流公式和脉冲电流过程的极限电流公式。  相似文献   

10.
本文采用脉冲电流法(PGM)在不同的基底材料表面沉积PANI, 通过平均电位\|时间曲线及扫描电子显微镜(SEM)等方法研究了基底材料对PGM法制备PANI的影响; 并采用循环伏安(CV)和电化学阻抗谱(EIS)研究了不同电极材料表面PANI的电化学性能.  相似文献   

11.
近年国内固相萃取-色谱分析的进展   总被引:7,自引:0,他引:7  
傅若农 《分析试验室》2007,26(2):100-122
对近两年国内各个领域的学者在使用固相萃取做样品前处理的色谱分析方面的研究和应用作了综述, 这一综述包括10个部分: 1. 国内近两年有关固相萃取的综述报告;2. 固相萃取-色谱分析在水质分析中的应用;3. 固相萃取-色谱分析在奶制品和肉类食品分析中的应用;4. 固相萃取-色谱用于蔬菜和水果中有害物质分析的应用;5. 固相萃取-色谱用于粮食和其他食品中有害物质分析的应用;6. 固相萃取-色谱在血药浓度、体液及组织中有害物质分析中的应用;7. 固相萃取-色谱在药物分析中的应用;8. 固相萃取-色谱在其他使用色谱分析中的应用;9. 基质固相分散在色谱分析中的应用;10. 分子印迹SPE在样品前处理中的应用.  相似文献   

12.
Conclusions A model has been suggested to explain the observed relationship between the measured heats of dissolution of uranyl nitrate in aqueous nitrate solutions and the concentration of the salting-out agent. The model describes the change in the structure of water in the solution with change in its concentration. On the one hand, a destruction of the water structure by ions occurs, which is weakened with increase in the distance from the ion, and leads to such irregularity in the distribution of water molecules in the solution that the mean number of molecules of water in unit volume is increased with increase in the distance from the ions. In experiments on the heat of dissolution this increase leads to increased hydration of the uranyl cation and reduction in the endothermicity of the dissolution with increase in the concentration of the solution. On the other hand, an interaction occurs between the ions of the salting-out agent and the water molecules in the solution, leading to the opposite result: There is an increase in the mean number of water molecules of the solution in unit volume in the direction of these ions. In experiments on the heat of dissolution this is revealed in the dehydration of the uranyl cation, and correspondingly in an increase in the endothermicity of the dissolution with increase in the concentration of the solution. The proposed model is in harmony with data on vapor pressure above the solutions (the relationship between the activity coefficient of the water and the concentration of the solution).Translated from Zhurnal Strukturnoi Khimii. Vol. 3, No. 2, pp. 143–150, March–April. 1962  相似文献   

13.
用原子吸收光谱法测定延边地区317名65~108岁老人头发中锌、铜、铁、锰、镁含量,观察不同民族、性别、年龄老人这些元素的差异。结果表明:1.朝鲜旗发锌低于汉族,满族发铜低于汉族、朝鲜族,汉族发镁高于朝鲜族、满族,发铁、发锰在汉、朝、满民族之间无区别。2.汉族、朝鲜族男发锌高于女性,汉族女性发铜高于男性,发铁、发锰、发镁在性别之间无区别。3、90岁组朝鲜族发锰、发镁低于65岁、76岁组,朝鲜族发锌、发铜、发铁在65~108岁之间无统计学意义。  相似文献   

14.
An analytical method was established for the simultaneous determination of 39 polycyclic aromatic hydrocarbons (PAHs) in air. The method was applied to a survey of gaseous and particulate PAHs in household indoor air. The survey was performed in 21 houses in the summer of 1999 and in 20 houses in the winter of 1999-2000 in Fuji, Japan. Thirty-eight PAHs were determined in indoor and outdoor air in the summer, and 39 PAHs were determined in indoor and outdoor air in the winter. The concentrations of gaseous PAHs in indoor air tended to be higher than those in outdoor air in the summer and winter. The concentrations of particulate PAHs in indoor air were the same as or lower than those in outdoor air in the summer and winter. PAH profiles, correlations between PAH concentrations, and multiple regression analysis were used to determine the factors affecting the indoor PAH concentrations. These results showed that gaseous PAHs in indoor air were primarily from indoor emission sources, especially during the summer, and that indoor particulate PAH concentrations were significantly influenced by outdoor air pollution.  相似文献   

15.
Polypropylene films were irradiated with 60Co γ-rays in vacuum or in air and stored in air. Just after irradiation, the concentration of carbonyl group of the sample irradiated in air only increased with dose. The concentrations of both samples increased with storage time. The more the absorbed doses, the higher the increasing rates. The increasing rate of the concentration of carbonyl group during irradiation in air was higher than those during storage in air. Just after irradiation, the tensile strengths and the elongations of the both samples somewhat increased with dose at the doses less than 5 Mrad, but decreased at doses more than 13 Mrad. The tensile strength and the elongation of the sample irradiated in air decreased with storage time. Those of the sample irradiated in vacuum also decreased with storage time but the decreasing rates were much smaller than those in the sample irradiated in air. The gel fractions of the samples irradiated in vacuum and annealed in vacuum were somewhat higher than those irradiated in vacuum and not annealed. To elucidate high oxidation rate in the sample irradiated in air during and after irradiation, reaction mechanisms were discussed. To clarify the difference of mechanical properties between the samples irradiated in vacuum and in air, the effect of crosslink was considered, together with the oxidation.  相似文献   

16.
The accelerated growth of aquaculture has resulted in a series of harmful effects to human health. The widespread and unrestricted use of antibiotics in this industry, to prevent bacterial infections, leads to remaining amounts in the aquatic environment. This has resulted in the emergence of antibiotic-resistant bacteria in aquaculture environments, in the increase in antibiotic resistance in fish pathogens as well as in the transfer of these resistance determinants to human pathogens. Moreover, the use of large amounts of antibiotics may lead to the presence of residual antibiotics in fish tissue and fish products. Fluoroquinolones, tetracyclines, penicillins, sulphonamides and other antibiotics, exhibiting activity against both Gram-positive and Gram-negative bacteria, are widely used for the treatment and prevention of diseases in fish. An extended and comprehensive review on the recent analytical methodologies concerning antibiotic residues in fish reported in the literature is provided in the present article. Emphasis is given on sample preparation regarding isolation and purification, chromatographic conditions and method validation according to legislation. Results of published assays are comparatively presented and criticised.  相似文献   

17.
化学体系中随机共振现象的特性、机理、本质和应用的研究是非常重要的前沿课题。综述中国科学技术大学非线性化学实验室,在化学体系随机共振现象的理论研究中,所取得的主要成果,并阐述化学体系随机共振现象研究中所提出来的若干重要问题:非均相化学体系中随机共振;化学体系中内信号随机共振;化学体系中多重随机共振;化学体系中随机共振的调制;化学体系中色噪声作用下的随机共振;化学体系中时空随机共振;耦合化学体系中随机共振;化学体系中双参量随机共振。  相似文献   

18.
Because Platinum Group Elements have found widespread use in catalytic converters in cars and as chemotherapeutic agent, interest in the development of reliable analytical methods is carried out in order to monitor these analita in humans to protect the citizen's health.Considering that information on the levels of many trace elements in biological matrices is scarce and for many non-essential elements, baseline levels in the population, and especially in those particularly exposed to the risk are lacking, in this paper we optimize an analytical method for biological matrices, using a voltammetric technique to measure the concentration of Pt in blood and perfusate.The amount of Pt recovered from the blood and perfusate samples spiked with analita was observed to be meanly of 95% with 5–6% of R.S.D. These results indicated that proposed method for the determination of platinum in biological materials is accurate and reproducible.The amounts of platinum found in the blood samples of common ranged citizen were similar to quantification limit while in the patients the concentration ranged from 1.5 to 360 μg/L, in perfusate ranged from 0.7 to 9700 μg/l. The concentrations of Pt of populace and in patients before of infusion are in agreement with the level measured in the blood of unexposed patients.The proposed analytical method permits to determine the amount of Pt in the perfusate and subsequently absorbed by the target organs in order to determine the dose and timing of treatment and to avoid overdoses with related undesired effects.  相似文献   

19.
–Time-resolved fluorescence spectra in the ps time range were measured on phycobilisome (PBS) embedded in poly(vinyl alcohol) films. The cyanobacterium Tolypothrix tenuis was used as a source of PBS because the pigment composition and the structure of the PBS are well defined. Isotropic PBS in the unstretched film and PBS uniaxially oriented in the stretched film were investigated. Diameters of PBS hemidiscs were oriented parallel to the film-stretching direction. The time-resolved fluorescence spectra of the unstretched sample and of the two polarized components in the stretched samples showed several differences in the rise and decay. The delay time, estimated from the time span between the maximum laser pulse and maximal intensity of the phycocyanin and allophycocyanin fluorescence, was much longer than that reported in the aqueous media. This suggests occurrence of a higher thermal deactivation of PBS in polymer film than in aqueous media. The excitation energy transfer from excited phycocrythrin to allophycocyanin was more efficient in the unstretched than in the stretched samples, and it was greater in the parallel polarized component of the stretched sample than in the perpendicular component. The present results are in agreement with a previous suggestion which states that there are two independent pathways of excitation energy transfer in PBS and that there is more than one final emitter of fluorescence. The molecules taking part in various pathways of energy transfer differ in their orientation within PBS.  相似文献   

20.
In current investigation, malathion—a thick viscous liquid insecticide was successfully converted into free flowing solids through co-inclusion in urea for multiple benefits. Resulting fertilizer—insecticide amalgamation offer steep reduction in toxicity/odor and improved handling/formulation characteristics. Malathion (MA), a widely used organophosphate insecticide was accommodated in urea host lattice in presence of long chain rapidly complexing agent (RCA). MA is entrapped in cavities of hexagonal urea and is accordingly not accessible either to the surface/environment for inhalation or for dermal contact. Therefore, personnel engaged in handling of hazardous insecticide will not be exposed after its containment in urea lattice. Insects will be exposed to insecticide only after malathion urea co-inclusion complex (MAUCIC) comes in contact with water in soil/crops following switching on of water distribution/sprinkling system in the fields. Since, MA is engulfed in urea channels, steep reduction in petroleum like skunk odor of MA was observed. Rheological studies revealed better flow properties of MAUCIC in comparison to viscous liquid malathion. This also results in reduced cost of transportation/packaging. Minimum amount of RCA required for co-inclusion of MA in urea was determined calorimetrically. Formation of MAUCIC was characterized by FTIR, DSC, XRD and 1H-NMR studies. Thermal studies revealed increase in heat of decomposition with corresponding increase in proportion of RCA in MAUCICs. MAUCIC complex revealed uniform formulation composition and improved dissolution profile of MA. Studies reveal fertilizer–insecticide amalgamation to be a useful technique for formulation of viscous insecticide into free flowing products with improved handling characteristics.  相似文献   

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