A review on flow analysis with turbidimetric and nephelometric detection is presented. A brief discussion of the principles of turbidimetry and nephelometry is given. Particular emphasis is devoted to coupling different flow techniques (flow injection, sequential injection, multicommutation) to these detection techniques. Applications in environmental, pharmaceutical, biological, and food samples are summarized and compared in terms of application range, flow configuration, repeatability, and sampling rate.
A review on the flow analysis of phosphorus with chemiluminescence detection is presented. A brief discussion of the chemiluminescence principles and applications is given. Particular emphasis is devoted to coupling different flow techniques (flow injection, sequential injection, multicommutation, multisyringe flow injection, multi-pumping) to chemiluminescence detection. Enzymatic and non-enzymatic methods, mostly applied to environmental samples, are summarized and compared in terms of application range, detection limits, flow configuration, repeatability and sampling rate.
A double-line sequential injection system was developed for the spectrophotometric determination of several metal ions in waters. The proposed double-line configuration was used to enable adding sample and chromogenic reagents as merging zones. The methodology was applied to the spectrophotometric determination of copper, iron, manganese, and zinc in samples of diverse origins at the range of 0.15–5.00, 0.10–10.0, 0.48–4.00, and 0.11–5.00 mg/L, respectively. Different chromogenic reagents and detection wavelengths were used. The chromogenic reagents for iron and manganese were 1,10-phenanthroline and formaldoxime, respectively. Copper and zinc were both determined using the analytical reagent zincon. Analytical characteristics of the methodology, such as manifold parameters, buffer pH, and reagent concentrations were optimized, and interference of some of the metal ions commonly present in water sample was assessed. Results of the analysis were in agreement with those obtained by atomic absorption spectrometry. Repeatability, expressed as the relative standard deviation for 10 consecutive injections of water samples, was lower than 6%. The determination rate was approximately 36/h.
In this work, a novel flow-through solid-phase based chemiluminescence (CL) optical sensor is described for the trace determination of orthophosphate in waters exploiting the multisyringe flow injection analysis (MSFIA) concept with multicommutation. The proposed time-based injection flow system relies upon the in-line derivatisation of the analyte with ammonium molybdate in the presence of vanadate, and the transient immobilisation of the resulting heteropolyacid in a N-vinylpyrrolidone/divinylbenzene copolymer packed spiral shape flow-through cell located in front of the window of a photomultiplier tube. The simultaneous injection of well-defined slugs of luminol in alkaline medium and methanol solution towards the packed reactor is afterwards performed by proper switching of the solenoid valves. Then, the light emission from the luminol oxidation by the oxidant species retained onto the sorbent material is readily detected. At the same time, the generated molybdenum-blue compound is eluted by the minute amount of injected methanol, rendering the system prepared for a new measuring cycle. Therefore, the devised sensor enables the integration of the solid-phase CL reaction with elution and detection of the emitted light without the typical drawbacks of the molybdenum-blue based spectrophotometric procedures regarding the excess of molybdate anion, which causes high background signals due to its self-reduction. The noteworthy features of the developed CL-MSFIA system are the feasibility to accommodate reactions with different pH requirements and the ability to determine trace levels of orthophosphate in high silicate content samples (Si/P ratios up to 500). Under the optimised conditions, a dynamic linear range from 5 to 50 g P l −1 for a 1.8 ml sample, repeatability better than 3.0% and a quantification limit of 4 g P l −1 were attained. The flowing stream system handles 11 analysis h −1 and has been successfully applied to the determination of trace levels of orthophosphate in environmental samples such as mineral, ground, tap and pond waters as well as samples from a water-steam cycle of an incineration plant. The t-test comparison of the means for the developed optical sensor and the molybdenum-blue spectrophotometric APHA/AWWA/WPCF reference method revealed that there is no evidence of significant differences between the obtained results at the 95% confidence level.
In this work, we propose the use of an air segment in a sequential injection system to simultaneously improve the overlapping of the stacked zones and minimise dispersion. This strategy was developed for the determination of sulphate in natural and wastewaters. Barium chloride was used as a precipitating agent and the turbidity of the suspension formed was measured at 420 nm. Analysis was performed without sample pre-treatment and the system was able to monitor sulphate concentration at a rate of at least 20 determinations per hour. Slightly different analytical sequences were developed for natural and wastewaters in order to minimise specific interferences. Direct determination of sulphate was possible within a concentration range of 10-100 and 16-100 mg SO(4)(2-) L(-1) for natural and wastewaters, respectively. Results obtained were comparable with those of the reference method with relative deviations lower than 5%. Relative standard deviations between 1.6% and 3.3% were found.
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