Flow-through electrochemistry in the analysis of wine

Flow through coulometry is used for analysis of wine samples for the determination of some heavy metals, sulphites, acidity and ethanol content. Low concentrations of heavy metals and sulphite contents are determined by making use of stripping chronopotentiometry. For the measurement of acid and ethanol content thin-layer coulometric titration is used.

Development of the measurement procedure and certified reference material of water mass fraction in a mineral oil

The necessity of developing certified reference materials (CRM) for the composition of mineral oil with a certified value of the mass fraction of water, traceable to the State Primary Standard of units of mass fraction and mass (molar) concentration of water in solid and liquid substances and materials GET 173–2017 is revealed proceeding from the review of standardized methods for determining the quality of mineral oils and approved types of reference materials (CRMs). Mineral hydraulic oil MIL-H-5606 of CONOSTAN series manufactured by SCP SCIENCE (Canada) was chosen as the CRM material to control the accuracy of the results of water determination in mineral oils using IR spectrometers. A procedure for reproducing the mass fraction of water in a mineral oil using a standard installation based on coulometric titration according to Karl Fischer method from the composition of GET 173–2017 has been developed. The relative expanded uncertainty (at k = 2) of measurement results of the water mass fraction in mineral oil is 7.1%. The requirements to the metrological characteristics of CRM were formulated: the interval of permissible certified values, the limits of the permissible values of the absolute error at P = 0.95, and the permissible value of the absolute expanded uncertainty at k = 2. The choice of the method of packaging and conditions of CRM storage were analyzed. Taking into account the consistency of the measurement results of the water mass fraction obtained by coulometric titration according to Karl Fischer method and using a Fluid Scan infrared spectrometer manufactured by Spectro Inc., USA, the applicability of CRMs for metrological support of express IR spectrometers was demonstrated.

Potentiometric Electronic Tongue for Pharmaceutical Analytics: Determination of Ascorbic Acid Based on Electropolymerized Films

This work deals with the design of an experimental potentiometric electronic tongue (ET) for the recognition of various samples of effervescent tablets with different ascorbic acid (vitamin C) contents. The ET consisted of twelve potentiometric sensors based on conductive polymers, which were derived from 4-amino-2,1,3-benzothiadiazole, 3,4-diaminobenzoic acid, and neutral red on the surface of the platinum electrode using cyclic voltammetry. The aim of the potentiometric study was to assess the influence of the vitamin C content and the composition of the matrix of commercial samples on the potentiometric response. The results obtained from the sensor array proved that the stability of the potentiometric signal and the accuracy of measurements are affected by individual sensors. The identification of the vitamin C content in the individual samples of effervescent tablets obtained by means of the potentiometric electronic tongue corresponded with the results of the coulometric titration.

Analytical Capabilities of Coulometric Sensor Systems in the Antioxidants Analysis

The definition of antioxidants (AOs), their classification and properties as well as electrochemical sensor systems for AOs analysis are briefly discussed. The analytical capabilities of coulometric titration with electrogenerated titrants as sensor systems for AOs determination have been considered in detail. The attention focused on the individual AO quantification that was mainly used in the pharmaceutical analysis and estimation of total antioxidant parameters (total antioxidant capacity (TAC), ferric reducing power (FRP) and ceric reducing/antioxidant capacity (CRAC)) allowing the fast screening of the target samples including their quality control. The main advantages of coulometric sensor systems are pointed out. The selective quantification of individual AO in a complex matrix using a combination of chromatography with coulometric or coulometric array detection under potentiostatic mode is discussed. The future development of coulometric sensor systems for AOs analysis is focused on the application of novel coulometric titrants and the application of coulometric detection in flow injection analysis.

Determination of phenolic compounds in medicinal preparations by galvanostatic coulometry

In this work, the possibility of using reactions of electrogenerated titrants with phenolic compounds was studied and a method for their coulometric determination in medicaments by galvanostatic coulometry was developed. The research objects were: rutin, salicylic acid and drugs containing phenolic compounds such as «Ascorutin», «Salicylic Paste» and «Salicylic Ointment» of Russian manufacture. Electrogenerated halogens (Cl2, Br2 and I2) and hexacyanoferrate(III)-ions were used as titrants. It was found that for the quantitative determination of phenolic acids, the optimal reagent is electrogenerated bromine, for rutin - electrogenerated bromine and iodine, and for ascorbic acid - any of the studied electrogenerated titrants (Cl2, Br2, I2 and [Fe(CN)6]3-). The correct definition was checked by the «entered-found» method, the error does not exceed 2%. As experimental studies have shown, our method of coulometric titration with electrogenated bromine and iodine is characterized by good reproducibility of results, expression, accuracy and can be used to determine phenolic compounds in drugs, for example, «Ascorutin» tablets. It should be noted that by our procedure it is possible to determine the spectrum of phenol-containing compounds (rutin, ascorbic and salicylic acids) in drugs without their preliminary separation. Therefore, the coulometric method using electrogenerated titrants can be recommended for the determination of salicylic, ascorbic acids and rutin in dosage forms. The proposed method is accurate and eliminates the experiment error in comparison with the Pharmacopoeic method.

Impact of oxygen content on preferred localization of p- and n-type carriers in La0.5Sr0.5Fe1−xMnxO3−δ

The oxygen content in La0.5Sr0.5Fe1−xMnxO3−δ, measured by coulometric titration in a wide range of oxygen partial pressure at various temperatures, was used for defect chemistry analysis. The obtained data were...

A Thermodynamic Investigation of Ni on Thin-Film Titanates (ATiO3)

Thin, ~1-nm films of CaTiO3, SrTiO3, and BaTiO3 were deposited onto MgAl2O4 by Atomic Layer Deposition (ALD) and then studied as catalyst supports for ~5 wt % of Ni that was added to the perovskite thin films by Atomic Layer Deposition. Scanning Transmission Electron Microscopy demonstrated that both the Ni and the perovskites uniformly covered the surface of the support following oxidation at 1073 K, even after redox cycling, but large Ni particles formed following a reduction at 1073 K. When compared to Ni/MgAl2O4, the perovskite-containing catalysts required significantly higher temperatures for Ni reduction. Equilibrium constants for Ni oxidation, as determined from Coulometric Titration, indicated that the oxidation of Ni shifted to lower PO2 on the perovskite-containing materials. Based on Ni equilibrium constants, Ni interactions are strongest with CaTiO3, followed by SrTiO3 and BaTiO3. The shift in the equilibrium constant was shown to cause reversible deactivation of the Ni/CaTiO3/MgAl2O4 catalyst for CO2 reforming of CH4 at high CO2 pressures, due to the oxidation of the Ni.

Thermodynamic Stability and Microscopic Behavior of BaxSr1-xCo1-yFeyO3-δ Perovskites

The mixed conducting perovskite-type oxides BaxSr1-xCo1-yFeyO3-δ (BSCF) are intensively studied as potential high-performance solid oxide fuel cell cathode materials. The effect of different compositional variables and oxygen stoichiometry on the structure and thermodynamic stability of the BaxSr1-xCo1-yFeyO3-δ (x = 0.2, 0.4, 0.5, 0.6, 0.8; y = 0.2, 0.4, 0.6, 0.8, 1) perovskite-type compositions were investigated by solid electrolyte electrochemical cells method and scanning electron microscopy (SEM). The thermodynamic quantities represented by the partial molar free energies, enthalpies and entropies of oxygen dissolution in the perovskite phase, as well as the equilibrium partial pressures of oxygen were obtained in the temperature range of 823–1273 K. The in situ change of oxygen stoichiometry and the determination of thermodynamic parameters of the new oxygen-deficient BSCF compositions were studied via coulometric titration technique coupled with electromotive force (EMF) measurements. The effect of A- and B-site dopants concentration correlated to the variation of oxygen stoichiometry on the thermodynamic stability and morphology of the BSCF samples was evidenced.