Evaluation of a PTV injector for quantitative analysis of volatile compounds at low concentrations

The performance of a PTV injector operated in the solvent venting mode with Tenax in the glass insert was evaluated with synthetic mixtures containing 5 to 50 ng of n-alkanes, ethyl esters, n-alcohols, and carboxylic acids. The influence of the sampled amount, the injected volume, and the nature of the solvent on accuracy and precision were studied. Coefficients of variation of relative (normalized) peak areas and absolute peak area ratios of each compound to the standard are of the order of 5 %.     

Electrochemical response of ascorbic acid at conducting and electrogenerated polymer modified electrodes for electroanalytical applications: a review

The present short review deals with electroanalytical aspects of electrochemical response of ascorbic acid (Vitamin C) at conducting and electrogenerated polymer modified electrodes. Two main topics are considered: (i) electrocatalytic oxidation of ascorbate at conducting polymer modified electrodes, leading to electroanalytical techniques for ascorbate assay, and (ii) retardation of ascorbate penetration through a layer of electrogenerated polymers, leading to permselective coatings and their diverse uses, especially for biosensing devices.     

On-line photo-derivatization with flow injection and liquid chromatography-atmospheric pressure electrospray mass spectrometry for the identification of indoles

The application of on-line photochemistry with flow injection (FI) and liquid chromatography (LC) in conjunction with atmospheric pressure electrospray mass spectrometry (LC-APESI-MS) for the identification of similar indole derivatives is reported here. The photo-transformation of the indole compounds is strongly affected by the substituent groups on the aromatic and heterocyclic rings. Upon photolysis for 2.5 min, the mass spectrum of tryptamine (Try) which has no OH substituent on the aromatic ring does not differ greatly from that obtained without photolysis. However, after photolysis of serotonin (Ser) which has one OH group on C5 of the aromatic ring, the mass spectrum indicates the formation of dimers and higher molecular weight ions. The fragmentation pattern of 5-hydroxytryptophol (Phol) without photolysis resembles that of Ser with a base peak of m/z 160. Upon photolysis using MeOH-H₂O (10/90), Phol is found to form a base peak at m/z 375 (100%) and a major peak at m/z 214 (66%) in addition to other ions with lower abundance. Melatonin (Mel) and tryptophan (Phan) upon photolysis are found to form high molecular weight ions with a relative low abundance. The mass spectrum of indole-3-acetic acid (Inaa) with on-line photolysis also shows different ions that are not formed without photolysis.     

Automated at-line solid-phase extraction-gas chromatographic analysis of micropollutants in water using the PrepStation

A fully automated at-line solid-phase extraction-gas chromatography procedure has been developed for the analysis of aqueous samples using the PrepStation. The sample extract is transferred from the sample preparation module to the gas chromatograph via an autosampler vial. With flame-ionization detection, limits of determination (S/N=10) of 0.05–0.13 μg/l were obtained for the analysis of HPLC-grade water when modifying the PrepStation by: (i) increasing the sample volume to 50 ml, (ii) increasing the injection volume up to 50 μl, and (iii) decreasing the desorption volume to 300 μl. The HP autosampler had to be modified to enable the automated “at-once” on-column injection of up to 50 μl of sample extract. The amount of packing material in the original cartridge had to be reduced to effect the decrease of the desorption volume. The total set-up did not require any further optimization after having set up the method once. The analytical characteristics of the organonitrogen and organophosphorus test analytes, i.e. recoveries (typically 75–105%), repeatability (2–8%) and linearity (0.09–3.0 μg/l) were satisfactory. The potential of the system was demonstrated by determining triazines and organophosphorus pesticides in river Rhine water at the 0.6 μg/l level using flame-ionization and mass-selective detection. No practical problems were observed during the analysis of more than 100 river water samples.     

用于VLSI的新型介质膜界面陷阱的特征

采用雪崩热电子注入技术和高频Ｃ－Ｖ准静态Ｃ－Ｖ特性测试,研究了新型快速热氮化的ＳｉＯｘＮｙ介质膜界面陷阱的特征,侧重于研究界面陷阱的特性与分布。结果表明：这种ＳｉＯｘＮｙ薄膜禁带中央界面陷阱密度随氮化时间的分布变化呈现”回转效应“,且存在着不同类型、密度悬殊很大的电子陷阱、指出雪崩热电子注入过程中在Ｓｉ／ＳｉＯｘＮｙ界面上产生两种性质不同的快界面态陷阱;给出了这两种界面态陷阱密度在禁带中能量的分布     

Quantitative determination of chloride by means of flow injection analysis with spectrophotometric detection in the UV/VIS range

Chloride is determined indirectly by Spectrophotometric flow injection analysis. Two systems are compared, both based on the principle of ion exchange of easily detectable anions versus chloride from suitable mercury salts. The first method is based on the exchange of chloride with chloranilate which is detected at 332 nm or at 306 nm in neutral or in acidic medium respectively. In the second case, chloride reacts with Hg(SCN)₂. The liberated thiocyanate forms a strongly coloured complex with Fe(III) in acidic solution with an absorption maximum at 460 nm. Both methods have a detection limit of about 5 mol Cl^–/l (175 ng/ml). In the case of the thiocyanate method, the relative standard deviation is about 2% (7 measurements) in the range of 5 to 150 mol/l and decreases significantly to a value of approximately 0.2% at higher concentrations; for the chloranilate method it is 10% for lower and about 1% for higher concentrations respectively.     

车用发动机高压电控喷油器的开发研究

以提高大功率车用发动机的动力性,经济性和排放性能为目的,对电控高压喷油器进行开发设计和实验研究,采用中压油源,由系统内部增压器来产生理想喷射所需的高压;通过蓄压装置和高速电磁开关阀控制喷油正时。结果 实验表明：最高喷油压力达１２４ＭＰａ,喷油规律的控制不受发动机转速影响,在系统结构和供油压力确定不变的条件下,完全由高速电磁开关阀的控制信号决定。     

流动注射分光光度法测定水中痕量正磷酸盐

在一定酸度条件下,甲基绿与磷钼杂多酸在水相所形成的离子缔和物于６６５ｎｍ处有一最大吸收峰,而试剂空白的最大吸收在６３０ｎｍ左右。     

摩擦和传热联合作用下等截面喷枪内气体的流动特性——(Ⅰ)基本方程及计算程式

基于可压缩流体动力学和热力学及传热原理,导出了表征摩擦和热源联合作用下管式和套管式等截面喷枪内气体流动特性的基本方程和计算公式;对18t AOD炉用套管式喷枪内的气体流动,较合理地确定了喷枪内壁温度和气体滞止温度沿管长的分布,以及吹炼过程中喷枪的摩擦系数;给出了不同流态下喷枪内气体流动特性的计算程式.     

流动注射小柱预富集—石墨炉原子吸收联用分析茶汤和水样中不同形态的铝

将装有８－羟基喹啉修饰的玻璃小珠或ＸＡＤ－２聚合物小球的微型富集分离柱接入流动注射－石墨炉原子吸收联用系统,分析茶汤和水样中不同形态的铝．选择不同的富集分离条件,样品中的铝可被分为与８－羟基喹啉快速络合的无机态铝、有机疏水态铝和总铝等几个种类,并比较和讨论实验结果．