流动注射电位滴定研究：氟化物沉淀滴定测锂

设计制作了一种简便的梯度混合室,并考察了其性能,试验结果证实了此混合室的合理性和有效性.用此混合室建立了流动注射电位滴定测锂的新方法,载流为1×10~(-5)～1×10~(-4)mol·L~(-1)的F~乙醇-水(9 1)溶液,流速4.2ml·min~(-1),混合室体积400μl,进样体积120μl,分析速度60样·h~(-1),检出范围取决于载流中滴定剂的浓度,方法用于卤水中锂的测定,结果令人满意.     

Comparative study of 8-hydroxyquinoline derivatives as chelating reagents for flow-injection preconcentration of cobalt in a knotted reactor

8-Hydroxyquinoline (HQ), 2-methyl-8-hydroxyquinoline (CH₃-HQ), 5,7-dichloro-2-methyl-8-hydroxyquinoline (Cl₂-CH₃-HQ), 5,7-dibromo-8-hydroxyquinoline (Br₂-HQ), 5-sulfo-7-iodo-8-hydroxyquinoline (ferron) and 5-sulfo-8-hydroxyquinoline (SO₃H-HQ) were compared as chelating reagents for on-line sorption preconcentration of cobalt in a knotted reactor (KR) precoated with the reagent. The results obtained with the different HQ derivatives reveal those properties of the chelating reagent responsible for the processes taking place in the KR. The influence of hydrophobicity, acidity, stability of the cobalt chelate and type of substituents in the HQ ring system on the separate steps of the flow injection (FI) preconcentration procedure are discussed. According to the performance characteristics of the different HQ derivatives, the most important parameters for on-line preconcentration in a KR are the hydrophobicity of the reagent and the stability of the chelate complex with the analyte.     

Chemically modified electrode for the detection of carbohydrates

A nickel-catalysed chemically modified electrode is described which seems to represent a convenient compromise between ease of preparation, reproducibility, precision and detection limits for the determination of carbohydrates in biological matrices.     

Development of the continuously variable volume reactor for flow injection analysis: Part 1. Design, capabilities and testing

A new apparatus for mixing sample and reagent in flow injection analysis (FIA) is described. The continuously variable volume reactor (CVVR) replaces the conventional mixing coil in a flow injection (FI) manifold to provide mixing and dilution. A linear actuator motor allows control of the chamber volume via LabVIEW software. The chamber volume can be incremented in steps of 1 μl over the range 68-1704 μl. In addition, the chamber has an integral variable-speed stirring unit that is also under computer control. Experiments were performed to evaluate the dispersion characteristics of this new device, evaluate the volume reproducibility, and understand the mixing characteristics. Use of the chamber is shown in the determination of iron(II) in pond water, and in NIST SRM 1643d with excellent results and a detection limit of 3.7 μg/l iron(II). Advantages of the CVVR and future research activities using the device are discussed.     

Flow injection determination of iodide ion in a photographic developing solution using iodide ion-selective electrode detector

A potentiometric flow injection determination method for iodide ion in a photographic developing solution was proposed by utilizing a flow-through type iodide ion-selective electrode detector. The sensing membrane of the electrode was Ag₂S–AgI membrane. The response of the electrode detector as a peak-shape signal was obtained for injected iodide ion in a photographic developing solution. A linear relationship in the subnernstian zone was found to exist between peak height and the concentration of the iodide ion in a photographic developing solution in a concentration range from 0 to 6.0×10⁻⁵ mol l⁻¹. The relative standard deviation for ten injections of 2×10⁻⁵ mol l⁻¹ iodide ion in a photographic developing solution was 0.96% and the sampling rate was approximately 12–13 samples h⁻¹. The iodide ion could be determined under coexisting of an organic reducing reagent and inorganic electrolytes of high concentration in a photographic developing solution sample solution by the present method.     

Differential pulse voltammetric determination of trace Te(IV) at a poly(3,3′-diaminobenzidine) film modified gold electrode in flow systems

Electropolymerization of 3,3′-diaminobenzidine on a gold surface gave an adherent, stable film of poly(3,3′-diaminobenzidine) (PDAB). This polymer film retained the complexational functionalities of its monomer, demonstrating preconcentration abilities for several ions, including Se(IV) and Te(IV). In particular, in this work, continuous flow and flow injection methods were developed for the sensitive and selective determination of Te(IV). The optimized method for the continuous flow mode had a detection limit of 5.6×10⁻⁹ mol l⁻¹ for 10 min preconcentration. Typical relative standard deviations for six consecutive determinations were 1.82 and 2.56% for Te(IV) concentrations of 1.0×10⁻⁶ and 5.0×10⁻⁸ mol l⁻¹, respectively (10 min preconcentration). The method was applied to the determination of Te(IV) in real samples.     

从聚丙烯流动曲线估算分子量分布

聚丙烯的控制降解技术由于能够带来很好的经济效益，国内外都在进行研究．其中分子量分布是一个重要数据，它对于聚丙烯的注塑、纺丝、薄膜等加工过程都有重要的影响．分子量分布一般用重均分子量Mw和数均分子量Mn之比D=Mw/Mn来表征，称为分子量分布指数．它可以     

Multipurpose chamber for the implementation of gas diffusion, dialysis, solid-phase extraction and precipitation/dissolution in continuous flow analyzers

A multipurpose chamber capable of implementing a variety of continuous separation techniques is reported. The proposed module can be used in conjunction with flow manifolds coupled on-line to optical detectors in order to develop simple autoanalyzers for full sample pretreatment. The analytical applicability of such a device is discussed with specific regard to gas diffusion, dialysis, solid-phase extraction (SPE), and precipitation/dissolution techniques. Its versatility and simplicity are among the main advantages. Four different automated analyzers based on the use of the multipurpose chamber have been developed for monitoring of different quality control parameters of liquid food samples, namely, carbon dioxide in beer, ascorbic acid in fruit juice, caffeine in soft drinks and lactose, fat and protein in milk. The results obtained were compared with those provided by the existing alternatives for the same applications in terms of sensitivity and precision.     

Electrochemical ELISA for the screening of DDT related compounds: analysis in waste waters

An electrochemical enzyme-linked immunosorbent assay (ELISA) for the detection of 1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane (p,p′-DTT), 1,1-dichloro-2,2-bis(p-chlorophenyl)ethylene (p,p′-DDE), 1,1-dichloro-2,2-bis-(4-chlorophenyl)ethane (p,p′-DDD) and o,p-DDT was developed. Optimization of the ELISA competition conditions, led to similar response for the p,p′-isomers. The activity of the label enzyme (horseradish peroxidase) was measured electrochemically using 3,3′,5,5′-tetramethylbenzidine as substrate. The use of purified antiserum for p,p′-DDT resulted in a sensitive assay with a detection limit of 40 pg ml⁻¹ and R.S.D. ranging from 1 to 3% intra-day and 3 to 6% inter-day. No matrix effect for waste water samples of different origin has been evidenced. The ELISA was used to detect DDTs in 20 samples after extraction in diethylether. This method appears suitable for routine screening of DDTs without sample pre-treatment other than dilution in PBS or after organic solvent extraction if high sensitivity is required.     

Critical Comparison of Four Simple Adaptors for Flow Amperometric and Stripping Voltammetry with Mercury Drop Electrodes in Batch Cells

Electrochemical batch cells with mercury drop electrodes, MDEs, are readily available from a number of producers and widely used in electroanalysis for polarography, voltammetry and stripping voltammetry. To increase sample throughput and reduce reagent and sample consumption, the tendency is to couple the MDE with flow analysis systems (e.g., FIA, SIA or BIA). Many special flow cells for MDEs are described in the literature, but it is easier to convert existing commercial batch cells to flow operation. To assess the performance of such flow adaptors, four models were chosen because they are directly fitted to the glass capillary of any MDE, light enough not to impair the mechanical drop knocker and can be effortlessly built in the laboratory. They were all found adequate for flow amperometry and stripping voltammetry, with differences in sensitivity, flow rate dependence, response time, drop stability, tolerance to bubbles, uncompensated resistance and recontamination of disposed analyte from the electrolytic bath. Two of them, a simple L‐shaped PTFE tube and an upstream nozzle holder made from a disposable pipette tip, gather a larger set of desirable features.