Urinalysis is a simple and non-invasive approach for the diagnosis and monitoring of various health disorders. While urinalysis is predominantly confined to clinical laboratories the non-invasive sample collection makes it applicable in wide range of settings outside of central laboratory confinements. In this respect, 3D printed devices integrating sensors for measuring multiple parameters may be one of the most viable approaches to ensure cost-effectiveness for widespread use. Here we evaluated such a system for the multiplexed determination of sodium, potassium and calcium ions in urine samples with ion-selective electrodes based on state of the art octadecylamine-functionalized multi-walled carbon nanotube (OD-MWCNT) solid contacts. The electrodes were tested in the clinically relevant concentration range, i.e. ca. 10-4 - 10-1 mol L-1 and were proven to have Nernstian responses under flow injection conditions. The applicability of the 3D printed flow manifold was investigated through the analysis of synthetic samples and two certified reference materials. The obtained results confirm the suitability of the proposed system for multiplexed ion analysis in urine.
A preconcentration module operated in flow mode and integrated with a sequential injection system with spectrophotometric detection was developed. Using the system, preconcentration was performed in continuous mode and was based on a membraneless evaporation process under diminished pressure. The parameters of the proposed system were optimized and the system was tested on the example of the spectrophotometric determination of Cr(III). The preconcentration effectiveness was determined using the signal enhancement factor. In the optimized conditions for Cr(III), it was possible to obtain the signal enhancement factors of around 10 (SD: 0.9, n = 4) and determine Cr(III) with precision and intermediate precision of 8.4 and 5.1% (CV), respectively. Depending on the initial sample volume, signal enhancement factor values of about 20 were achieved. Applicability of the developed preconcentration system was verified in combination with the capillary electrophoresis method with spectrophotometric detection on the example of determination of Zn in certified reference materials of drinking water and wastewater. Taking into account the enhancement factor of 10, a detection limit of 0.025 mg L−1 was obtained for Zn determination. Zn was determined with precision less than 6% (CV) and the results were consistent with the certified values.
This paper presents a novel, automatic, simple approach to stop-flow photometric determination of Fe(II) in wastewater and wine samples using a multi-pumping flow system with a direct-injection detector. The basis for the determination was the reaction of Fe(II) with 1,10-phenanthroline, which was carried out in the reaction chamber of the direct-injection detector. The research included a selection of appropriate parameters of the proposed analytical procedure and method validation. Under optimized conditions, linear calibration curves were obtained in two concentration ranges of Fe(II) 0.07–1.00 and 1.00–7.00 mg/dm3, with the quantification limit of 0.07 mg/dm3. The procedure was validated by studying the accuracy (8.2%, RE) and precision (9.6 and 14.8%, RSD, for higher and lower concentration range, respectively). The proposed method was successfully employed in Fe(II) determination in spiked wastewater and wine samples with recovery of 95.8–104.5%. Using the procedure, time of a single analysis (for three independently measured signals) was about 300 s and sample and reagent consumptions were 240 and 60 mm3, respectively. Graphic
A novel approach to automated flow titration with spectrophotometric detection for the determination of Fe(III) is presented. The approach is based on the possibility of strict and simultaneous control of the flow rates of sample and titrant streams over time. It consists of creating different but precisely defined concentration gradients of titrant and analyte in each successively formed monosegments, and is based on using the calculated titrant dilution factor. The procedure was verified by complexometric titration of Fe(III) in the form of a complex with sulfosalicylic acid, using EDTA as a titrant. Fe(III) and Fe(II) (after oxidation to Fe(III) with the use of H2O2) were determined with good precision (CV lower than 1.7%, n = 6) and accuracy ( lower than 3.3%). The approach was applied to determine Fe(III) and Fe(II) in artesian water samples. Results of determinations were consistent with values obtained using the ICP–OES reference method. Using the procedure, it was possible to perform titration in 6 min for a wide range of analyte concentrations, using 2.4 mL of both sample and titrant.