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The novel, automated, multi-pumping flow system (MPFS) for online calibration and determination of nitrate in surface water is presented for the first time. The system was equipped with micropumps of three different nominal volumes (10, 20, and 50 µL). As a result, it was possible to prepare from one standard, directly in a flow system, up to seven standard solutions. Determination of nitrate was conducted in stop-flow conditions and is based on a commercially available ion selective electrode (ISE) application. It was found that the linearity and slope of the calibration graphs depend mainly on the characteristics of the ISE. The obtained results were very repeatable, owing to the high precision of the micro-pumps used. The R.S.D. for the stroke volume of each micro-pump was below 1%. The accuracy of the method was checked through determination of nitrate in surface water samples. The obtained results were compared with those of the reference method (photometric Hach cuvette tests). It was found that, at a 96% confidence level, the difference between the results obtained by the proposed method and the reference method was statistically insignificant. The accuracy of the method was confirmed through the determination of nitrate in Certified Reference Material. The relative deviation (R.D.) of the measured and the certified concentrations was 5%.

In this work, an innovative, flow-through, double-beam, photometric detector with direct injection of the reagents (double-DID) was used for the first time for the determination of iron in pharmaceuticals. For stable measurement of the absorbance, double paired emission-detection LED diodes and a log ratio precision amplifier have been applied. The detector was integrated with the system of solenoid micro-pumps. The micro-pumps helped to reduce the number of reagents used and are responsible for precise solution dispensing and propelling. The flow system is characterized by a high level of automation. The total iron was determined as a Fe(II) with photometric detection using 1,10-phenanthroline as a complexing agent. The optimum conditions of the propose analytical procedure were established and the method was validated. The calibration graph was linear in the range of 1 to 30 mg L -1 . The limit of detection (LOD) was 0.5 mg L -1 . The throughput of the method was 90 samples/hour. The repeatability of the method expressed as the relative standard deviation (R.S.D.) was 2% (n = 10). The method was characterized by very low consumption of reagents and samples (20 μL each) and a small amount of waste produced (about 540 µL per analysis). The proposed flow method was successfully applied for determination of iron in pharmaceutical products. The results were in good agreement with those obtained using the manual UV-Vis spectrophotometry and with values claimed by the manufacturers. The flow system worked very stably and was insensitive to bubbles appearing in the system.

The novel automatic flow system, direct-injection detector (DID) integrated with multi-pumping flow system (MPFS), dedicated for the photometric determination of orthophosphates in wastewater and freshwater samples is for the first time described. All reagents and the sample were injected simultaneously, in counter-current into the reaction-detection chamber by the system of specially selected for this purpose solenoid micro-pumps. The micro-pumps provided good precision and accuracy of the injected volumes. For the determination of orthophosphates, the molybdenum blue method was employed. The developed method can be used to detect orthophosphate in the range 0.1-12 mg L -1 , with the repeatability (RSD) about 2.2% at 4 mg L -1 and a very high injection throughput of 120 injections h -1 . It was possible to achieve a very small consumption of reagents (10 μL of ammonium molybdate and 10 μL of ascorbic acid) and sample (20 μL). The volume of generated waste was only 440 μL per analysis. The method has been successfully applied, giving a good accuracy, to determination of orthophosphates in complex matrix samples: treated wastewater, lake water and reference sample of groundwater. The developed system is compact, small in both size and weight, requires 12 V in supply voltage, which are desirable for truly portable equipment used in routine analysis. The simplicity of the system should result in its greater long-time reliability comparing to other flow methods previously described.