The solid-state ion-selective electrodes presented here are based on the FePO4:Ag2S:polytetrafluoroethylene (PTFE) = 1:1:2 with an addition of (0.25–1)% microwave-synthesized hematite (α-Fe2O3), magnetite (Fe3O4), boehmite [γ-AlO(OH)], and alumina (Al2O3) nanoparticles (NPs) in order to establish ideal membrane composition for iron(III) cations determination. Synthesized NPs are characterized with Fourier-Transform Infrared (FTIR) spectroscopy, Powder X-Ray Diffraction (PXRD), and Scanning Electron Microscopy (SEM) with Energy Dispersive Spectroscopy (EDS). The iron oxides NPs, more specifically, magnetite and hematite, showed a more positive effect on the sensing properties than boehmite and alumina NPs. The hematite NPs had the most significant effect on the linear range for the determination of ferric cations. The membrane containing 0.25% hematite NPs showed a slope of −19.75 mV per decade in the linear range from 1.2∙10−6 to 10−2 mol L−1, with a correlation factor of 0.9925. The recoveries for the determination of ferric cations in standard solutions were 99.4, 106.7, 93.6, and 101.1% for different concentrations.

The advantages of microwave technology over conventionally conducted experiments are numerous. Some of them are reduction in reaction time, a higher degree of process control, repeatability, and work safety. Microwave synthesis routes require a complete description of the experimental details, instrumentation, and design program of a microwave oven used in the experiments. In this work, microwave-assisted hydrothermal synthesis of hematite (α-Fe2O3) particles from 0.1 M FeCl3 solution in highly alkaline media with heating in a microwave oven at continuous microwave emission of 800 W at 150 °C, 200 °C, and 250 °C for 20 min are presented. Also, the influence of the percentage of the addition of a cationic surfactant, cetyltrimethylammonium bromide (CTAB) on the composition, size, and shape of the final product was investigated. The samples precipitated at 150 °C formed a final product consisting of goethite (α-FeOOH) and hematite particles in contrast to the those precipitated at 200 °C and 250 °C where pure hematite phase was obtained. In these synthesis routes, the CTAB caused to slow down the rate of the goethite-to-hematite transformation process at temperatures at 200 °C but did not affect the transformation at 250 °C.

A novel ion-selective electrode with membranes based on iron(III) phosphate and silver sulfide integrated into a completely new electrode body design has been developed for the determination of iron(III) cations. The best response characteristics with linear potential change were found in the iron(III) concentration range from 3.97× 10−5 to 10−2 mol L−1. The detection limit was found to be 2.41× 10−5 mol L−1 with a slope of –20.53 ± 0.63 and regression coefficient of 0.9925, while the quantification limit was 3.97× 10−5 M. The potential change per concentration decade ranged from –13.59 ± 0.54 to –20.53 ± 1.56 for Electrode Body 1 (EB1) and from –17.28 ± 1.04 to –24 ± 1.87 for Electrode Body 2 (EB2), which is presented for the first time in this work. The prepared electrode has a long lifetime and the ability to detect changes in the concentration of iron cations within 20 s. Membrane M1 showed high recoveries in the determination of iron cations in iron(III) standard solutions (98.2–101.2%) as well as in two different pharmaceuticals (98.6–106.5%). This proves that this type of sensor is applicable in the determination of ferric cations in unknown samples, and the fact that all sensor parts are completely manufactured in our laboratory proves the simplicity of the method.

Considering the vast cultural and traditional heritage of the use of aromatic herbs and wildflowers for the treatment of light medical conditions in the Balkans, a comparison of the antioxidant capacity of wildflowers extracts from Herzegovina was studied using both cyclic voltammetry and spectrophotometry. The cyclic voltammograms taken in the potential range between 0 V and 800 mV and scan rate of 100 mV s−1 were used for the quantification of the electrochemical properties of polyphenols present in four aqueous plant extracts. Antioxidant capacity expressed as mmoL of gallic acid equivalents per gram of dried weight of the sample (mmoL GAE g−1 dw) was deduced from the area below the major anodic peaks (Q400 pH 6.0, Q500 pH 4.7, Q600 pH 3.6). The results of electrochemical measurements suggest that the major contributors of antioxidant properties of examined plants are polyphenolic compounds that contain ortho-dihydroxy-phenol or gallate groups. Using Ferric reducing-antioxidant power (FRAP) and 2,2′-azino-bis spectrophotometric methods (3-ethylbenzthiazoline-6-sulphonic acid) radical cation-scavenging activity (ABTS) additionally determined antioxidant capacity. The FRAP results ranged from 2.9702–9.9418 mmoL Fe/g dw, while the results for ABTS assays expressed as Trolox equivalents (TE) ranged from 14.1842–42.6217 mmoL TE/g dw. The Folin–Ciocalteu procedure was applied to determine the total phenolics content (TP). The TP content expressed as Gallic acid equivalents (GAE) ranged from 6.0343–9.472 mmoL GAE/g dw. The measurements of total flavonoid (TF) and total condensed tannin (TT) contents were also performed to obtain a broader polyphenolic profile of tested plant materials. Origanum vulgare L. scored the highest on each test, with the exception of TT content, followed by the Mentha × piperita L., Artemisia annua L., and Artemisia absinthium L., respectively. The highest TT content, expressed as mg of (−)catechin equivalents per gram of dried weight of sample (mg CE/g dw), was achieved with A. absinthium extract (119.230 mg CE/g dw) followed by O. vulgare (90.384 mg CE/g dw), A. annua (86.538 mg CE/g dw) and M. piperita (69.231 mg CE/g dw), respectively. In addition, a very good correlation between electrochemical and spectroscopic methods was achieved.

Microwave-assisted hydrothermal synthesis is a simple, reproducible, rapid, and effective method, and therefore, has attracted considerable interest among scientists in the field of synthesis not only of iron oxide but also of other metal oxides. This method has been used for the synthesis of iron oxide nanoparticles, hematite (α-Fe2O3), and goethite (α-FeOOH) in strongly alkaline media with iron(III) chloride (FeCl3) as precursor under microwave emission of 850 W. In this work, the effect on the size, shape, and composition of the final product was investigated by changing the conditions, such as shortening the synthesis time, increasing the synthesis temperature, and adding various substances to the synthesis pathway. Samples synthesized at 200 °C for 20 min by increasing the added percentage of polyethylene glycol (PEG), sodium dodecyl sulfate (SDS), rosemary essential oil and lavender essential oil promote goethite-to-hematite transformation, while N-guanylurea sulfate (NGS) and sage essential oil behave differently. The aforementioned substances added at 260 °C resulted in a decrease in particle size, but pure hematite was obtained, regardless of the type of the substances added or the decrease in synthesis time from 20 min to 5 min. Furthermore, the use of essential oils rather than surfactants in this study was presented as a novel, environmentally friendly method of iron oxide synthesis.