Electrochemical and statistical study of Nickel ion assessment in daily children intake samples relying on magnesium aluminate spinel nanoparticles.

Lately, children's daily consumption of some products, such as cereals and candies, has been rising, which provides a compelling rationale for determining any metallic substances that may be present. Monitoring the concentration of certain metals, like nickel, in these products is necessary due to medical issues in humans when consumed regularly. So, in this work, a novel and highly selective carbon paste as a Ni(II) ion-selective sensor was prepared and investigated using ceramic magnesium aluminum spinel nanoparticles as the ionophore and tritolyl phosphate (TOCP) as a plasticizer. A modified co-precipitation method was used to synthesize the spinel nanoparticles. X-ray diffraction, scanning electron microscope with EDAX, transmission electron microscope, and BET surface area were used to determine the phase composition, microstructure, pores size, particle size, and surface area of the synthesized nanoparticles. The spinel nanoparticle was found to have a nano crystallite size with a cubic crystal system, a particle size ranging from 17.2 to 51.52 nm, mesoporous nature (average pore size = 8.72 nm), and a large surface area (61.75 m2/g). The composition ratio of graphite carbon as a base: TOCP as binder: spinal as ionophore was 67.3:30.0:2.7 (wt%) based on potentiometric detections over concentrations from 5.0 × 10-8 to 1.0 × 10-2 mol L-1 with LOD of 5.0 × 10-8 mol L-1. A measurement of 29.22 ± 0.12 mV decade-1 over pH 2.0-7.0 was made for the Nernstian slope. This sensor demonstrated good repeatability over nine weeks and a rapid response of 8 s. A good selectivity was shown for Ni(II) ions across many interferents, tri-, di-, and monovalent cations. The Ni(II) content in spiked real samples, including cocaine, sweets, coca, chocolate, carbonated drinks, cereals, and packages, were measured. The results obtained indicated no significant difference between the proposed potentiometric method and the officially reported ICP method according to the F- and t-test data. In addition to utilizing ANOVA statistical analysis, validation procedures have been implemented, and the results exceed the ICP-MS methodology.

Modified carbon paste ion selective electrode for determining Cr(iii) ions in aqueous solutions and some real samples using tetragonal zirconia nanoparticles.

Tetragonal zirconia (t-ZrO2) nanoparticles (ionophore) are used in newly designed and improved ion selective electrodes for chromium ion detection as an alternative, low-cost, high-precision, and selectivity method. Tetragonal zirconia nanoparticles were synthesized using a modified co-precipitation technique and calcined at 1000 °C for an hour. The phase composition, surface area, microstructure, pore size and particle size of synthesized t-ZrO2 nanoparticles were examined using the X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), transmission electron microscope (TEM) and scanning electron microscopy (SEM) attached with an EDAX unit, respectively. Results from XRD showed that the t-zirconia was synthesized and have nanocrystallites size about 20.2 nm. The nano size of t-ZrO2 was confirmed by the SEM and TEM (the particle size between 26.48 and 40.4 nm), the mesoporous character (average pore size about 4.868 nm) and large surface area (76.2802 m2 g-1) was confirmed by BET analysis. The paste composition with 67.3 : 30.5 : 2.7 (wt%) graphite, t-ZrO2, and TCP, respectively, exhibited the best results. With a detection limit of 1.0 × 10-8 mol L-1, the electrode displayed a good Nernstian slope of 19.50 ± 0.10 mV decade-1 over the concentration range from 1.0 × 10-2 to 1.0 × 10-8 mol L-1 of Cr(iii) ions. The built-in sensor displayed a quick response time (7 s), was highly thermally stable in the range of 10 to 60 °C without departing from Nernstian behaviour and could be used for about 60 days in the pH range of 2.0 to 6.0. The electrode demonstrated excellent selectivity for the Cr(iii) ion towards a variety of metal ions. For chromium ion determination, numerous spiked real samples, including honey, water, tea, coffee, milk, cheese, and cosmetics, were used. Validation methods were used, and the results showed that there is no significant difference between the two methods (ICP and ISE) at a 95% confidence level. In several real water samples, the estimated limits of detection, limits of quantification, percent recovery, standard deviation, and relative standard deviation showed the effectiveness of the proposed electrode in the potentiometric detection of Cr(iii) ions.