A new flow injection titration analysis

Summary A new type of flow injection titration method where a well-stirred mixing chamber is placed in the middle of the injection loop of a 6-way valve has been developed. With this method expensive or unstable reagents can be used for the titration. Moreover, it is potentially available for slow titration reactions. Its fundamental characteristics have been investigated using acid-base titration reaction with phenolphthaleine as the indicator. The sampling rate was 60–120 samples per hour and its reproducibility was also high (3%).

---

Neues Verfahren zur Fließinjektions-Volumetrie

     

A Simple injection valve for flow injection analysis

A novel sample introduction valve, based on a modified glass syringe, is described for flow injection analysis. Sample volumes of 1.4 μl or more can be injected manually or automatically, by driving with a 12-V solenoid. The valve has advantages of freedom from maintenance and long lifetime.     

A new approach to the integrated calibration in flow injection analysis

A new proposal how to perform the analytical procedure according to the integrated calibration method is presented. An original flow injection system has been designed for this purpose. When using only a single standard solution, the measurement information gathered during a single analytical course permits construction of four calibration graphs and calculation of as many as four independent estimations of the analyte concentration in the sample examined. As the calibration method applied integrates the set of standards method and the standard addition method, the analytical estimations may be obtained in both the interpolative and the extrapolative manner and the final result can be effectively verified in terms of accuracy. The system developed was experimentally tested on the example of spectrophotometric determination of chromium. It has been proved to be capable of saving time and reagents as well as providing reliable analytical results. Owing to the instrumental simplicity and analytical efficiency the system is expected to be useful for routine analysis.     

A simple multifunctional valve for flow injection analysis

A simple and versatile pneumatically-operated two-layer rotary valve is described for simultaneous introduction of sample and diversion of analytical streams in flow injection analysis. Examples of application include valve configuration with time-controlled sample volume and with loop-controlled sample volumes in one or two loops; both configurations are useful in routine analyses of samples of highly varying analyte concentrations. The usefulness of the valve for ion-exchange preconcentration procedure is also demostrated.     

Stepwise injection analysis as a new method of flow analysis

Various versions of flow analysis techniques (continuous-flow, flow-injection, and sequential-injection analysis) and their relative advantages and disadvantages are considered. Cyclic (stepwise) injection analysis is proposed, and the general principles of this technique are described.     

Integrated microconduits for flow injection analysis

A novel approach for constructing continuous flow systems for analysis s described and its versatility is demonstrated for a number of flow-injection systems with integrated potentiometric or optical detectors and with integrated gas-diffusion or ion-exchange units. Optimization of the miniaturized designs was achieved by means of scaling factors based on the theory of similarity.     

A factorial design for optimizing a flow injection analysis system

The use of a factorial design for the response exploration of a flow injection (FI) system is described and illustrated by FI spectrophotometric determination of paraquat. Variable response (absorbance) is explored as a function of the factors flow rate and length of the reaction coil. The present study was found to be useful to detect and estimate any interaction among the factors that may affect the optimal conditions for the maximal response in the optimization of the FI system, which is not possible with a univariate design. In addition, this study showed that factorial experiments enable economy of experimentation and yield results of high precision due to the use of the whole data for calculating the effects.     

A factorial design for optimizing a flow injection analysis system

The use of a factorial design for the response exploration of a flow injection (FI) system is described and illustrated by FI spectrophotometric determination of paraquat. Variable response (absorbance) is explored as a function of the factors flow rate and length of the reaction coil. The present study was found to be useful to detect and estimate any interaction among the factors that may affect the optimal conditions for the maximal response in the optimization of the FI system, which is not possible with a univariate design. In addition, this study showed that factorial experiments enable economy of experimentation and yield results of high precision due to the use of the whole data for calculating the effects.     

A microprocessor control system for automated multiple flow injection analysis

A microprocessor control system is reported for automated multiple flow injection analysis. The control system consists of an IMSAI-8048 microprocessor, some associated electronic interfacing and a control computer command language. The system can be programmed to control any of three versions of automated multiple flow injection analysers. This control system is relatively inexpensive and is suitable for use by inexperienced personnel.     

A new flow cell design for chemiluminiscence analysis

The present study proposes a new flow cell called a bundle cell for chemiluminescence analysis. The results obtained were compared with those achieved by manual and automated batch procedures and flow manifolds with different cells: an common quartz flow cell, a helix cell and the most used spiral cell. Figures of merit such as limit of detection, sensitivity, accuracy and precision for the Cr(III) determination were established with light emission produced by catalysed Cr(III) luminol oxidation by hydrogen peroxide in a basic aqueous solution. An improvement in sensitivity about 50% as compared with the spiral cell and even larger with respect to the other flow cells tested was observed. The limit of detection provided was lower than those obtained with the other flow cells. In reference to the batch mode, similar results were obtained with the bundle flow cell. Good results were obtained for several real water samples containing chromium at different concentrations.     

Time-based flow injection analysis

Time-based flow-injection systems are novel measurement systems which use induced dispersion of the sample in the system and measurement of time to evaluate the concentration of the analyte in the sample. There are two types of time-based system. In the standard systems, assays are based on the chemistries of the classical intensity assays; in the pseudo-titration systems, the assays are based on classical titration chemistries. These systems are discussed in terms of basic theory, classification of the systems and their advantages.     

Amperometric detection for capillary flow injection analysis

Ultrasmall-volume measurements of oxidizable compounds have been accomplished by coupling a capillary flow injection system with amperometric detection. Remarkably low (femtomole) mass detection limits result from the combination of nanoliter sample volume and the inherent sensitivity of the wall-jet detector. A substantial economy of reagent consumption and disposal accrues from the operation of the nl/min flow regime. Variables influencing the physical dispersion in the capillary flow injection system, including capillary length, sample volume or flow rate, are explored and optimized.     

A simple lecture demonstration of flow injection analysis

Summary The difficulties of explaining the basic concepts of dispersion in flow injection analysis are discussed with particular reference to comparisons with segmented flow analysis and high performance liquid chromatography. The problems with diagrammatic illustration of the laminar flow processes and subsequent dispersion of an injected sample zone are explained. A simple demonstration based on a flow cell for a slide projector consisting of a peristaltic pump tube sandwiched between two slightly modified slide mounts is described.

---

Einfache Vorlesungsdemonstration der Fließinjektionsanalyse

     

A random walk simulation of flow injection analysis

Dispersion and chemical reaction in a single-channel flow-injection system are modelled by a random walk (stochastic, Markovian chain) method using a microcomputer. The effects of various simulated physical variables are investigated. The model provides valuable insight into the mixing process in flow injection analysis.     

A microfluidic device with integrated fluorimetric detection for flow injection analysis

This work describes the development of flow analysis microsystems with integrated fluorimetric detection cells. Channels (width of 300–540 μm and depth of 200–590 μm) were manufactured by deep-UV lithography in urethane–acrylate (UA) resin. Plastic optical fibers (diameter of 250 μm) were coupled to a 2.0-mm-long detection channel in order to guide the excitation radiation from an LED (470 nm) and collect the emitted radiation at a right angle towards a photomultiplier. A single-line miniaturized system, with a total internal volume of 10.4 μL, was evaluated by means of standard fluorescein solutions (0.53–2.66 μmol L⁻¹, pH 8.5). The analytical signals presented a linear relationship in the concentration range studied, with a relative standard deviation of 1.9% (n = 5), providing a detection limit of 0.37 μmol L⁻¹ and an analytical frequency of 60 samples/h, using a flow rate of 60 μL min⁻¹. Optical microscopy images and videos acquired in real time for the hydrodynamic injection of 130 and 320 nL of sample solutions indicated the good performance of the proposed sampling strategy. Another microsystem with a total internal volume of 38 μL was developed, incorporating a confluence point for two solutions. This device was applied to the determination of the total concentration of Ca²⁺ and Mg²⁺ in commercial mineral waters using the calcein method. Microscopy images and videos demonstrated the mixing efficiency of the solutions in the microchannels. A linear relationship was observed for the analytical signal in the Ca²⁺ concentration range from 25 to 125 μmol L⁻¹, with relative standard deviations of 3.5%. The analysis of mineral waters with the proposed system provided results that did not differ significantly from those obtained by the EDTA titration method at a confidence level of 95%. These results demonstrate the viability of developing micro flow injection systems with an integrated fluorimetric detection cell.      

A rapid assay method for catechol-O-methyltransferase activity by flow injection analysis

A rapid assay employing flow injection analysis (FIA) to determine the activity of purified catechol-O-methyltransferase (COMT) from porcine liver is described. The method was based on the determination of normetanephrine, the 3-O-methyl metabolite of the substrate norepinephrine. Excess norepinephrine was removed from the incubation mixture by alumina extraction twice to allow normetanephrine to be subjected to flow injection analysis, coulometrical oxidation, fluorogenic reaction with ethylenediamine and fluorescence detection. K(m) and V(max) values for COMT obtained with the system were 503 microM and 4.51 nmol/min/mg protein, respectively. The method is suitable for screening of COMT inhibitors or activators, as a large number of samples, up to 200, can be processed in one working day.     

A multi-ion sensor cell and data-acquisition system for flow injection analysis

The flow-injection system described is used for the determination of four ions simultaneously with detection by solid-contact polymer-membrane ion-selective electrodes. The construction of the flow cell and data-acquisition system are discussed. The programming language FORTH facilitates the fast data acquisition required for flow injection analysis. The utility of the system is demonstrated by applying it to the simultaneous determination of potassium, calcium, nitrated and chloride in soil extracts; the results are compared with standard procedures.     

Flow injection analyses: Part I. A new concept of fast continuous flow analysis

The concept of a new continuous flow analyser system is described. Based on instant discrete sampling by injection into a carrier stream, the system allows continuous flow analysis to be performed in a fast, much simplified way. As the continuous flowing stream is characterized by a turbulent rather than a laminar flow, the discrete instant sampling creates geometrically well-defined segments of sample solution within the flowing stream. Because of the absence of lag phase, an unprecedented sampling rate for continuous flow analysis of well over 200 samples per hour can be achieved; and even manual injection of the samples allows a very high degree of accuracy and precision to be obtained ( ? ± 1%). Uses of the system in various analytical procedures are described and discussed. A potentiometric sensor (the air-gap electrode used in a flow-through unit) and a spectrophotometric arrangement with a flow-through cell have been used as detector units.