Iodometric Titration Research Articles

Suppressing Effect of Flavonoid Compounds on Lipids Photooxidation of Sheep Red Blood Cells and Oleic Acid Photooxidation

ABSTRACTPhotosensitizers and pigments in raw meat such as porphyrins, riboflavin, and myoglobin after incorporation with light beam prompt the generation of singlet oxygen (1O2) from triplet oxygen (3O2) and cause oxidative rancidity of meat products. In this study, the results of photooxidation reactions of sheep erythrocyte (red blood cell) model as a model rich in hemoglobin and phospholipids bilayer, and oleic acid model were obtained by 1H NMR spectroscopy, TBARS assay, and iodometric titration. In both models, the rate of lipid photooxidation in the presence of hydroalcoholic extracts of Turmeric (Curcuma longa L.) and Cumin (Cuminum cyminum L.) as natural antioxidants, Butyl hydroxytoluene (BHT) as a synthetic antioxidant, and sodium azide (NaN3) as a well‐known 1O2 scavenger were decreased in the order of NaN3 > Turmeric > Cumin > BHT. It was proven that during the photooxidation process, there is a direct association between the amount of flavonoid compounds and 1O2 scavenging.

Comparative estimation of ascorbic acid (Vitamin C) in Sweet-melon, Watermelon and Cucumber

This research is carried out to provide valuable information for individuals that would want to properly modify their nutrient intake. It would enable individuals to know the quantity of these fruits (Sweet melon, Watermelon and Cucumber) needed to be consumed per day to meet the Recommended Daily Allowance (RDA) of Vitamin C for healthy living. Understanding the relative content of Ascorbic acid in these fruits will help individuals plan their diets and know how to properly incorporate them in foods daily to avoid Vitamin C deficiency health problems. This study determined and compared the vitamin C content in Sweet melon, Watermelon and Cucumber. The extracted juices were analysed for ascorbic acid (Vitamin C) using Iodometric Titration method. Results obtained showed that Sweet melon contain (58.4mg/100cm³), Water melon (22.75mg/100cm³) and Cucumber (16.25mg/100cm³) concentrations of ascorbic acid. The ascorbic acid concentrations being highest in Sweet melon and lowest in Cucumber. Therefore sweet melon is the best source of Vitamin C among the three fruits analyzed. Sweet melon can be recommended for individuals suffering from vitamin C deficiency. It is recommended that nutrition and health education is needed to promote increased consumption of fruits rich in Vitamin C content to avoid diseases caused by its deficiency such as scurvy, Iron deficiency anemia, bone disease in children.

Simultaneous determination of chlorides, bromides, and fluorides in ion-conducting electrolyte

There are developed the techniques of determining the content of chlorides, bromides and fluorides at their joint presence in two types of solid electrolytes differing in matrix content: the first type contains lithium, the second one — both lithium and aluminium, simultaneously. Determination of bromides mass fraction is fulfilled using a method of iodometric titration of iodic potassium excess after bromides are oxidized until free bromine. The fluorides mass fraction is measured by the gravimetric method in the form of fluoro-chloride of lead, in this case the aluminium interfering influence is eliminated by its precipitation in the form of hydroxide after it is fused with carbonates of potassium and natrium, as well as by the method of potentiometric titration with a fluoride ion-selective electrode using the nitrate lanthanum solution. The absence of aluminium interfering influence on the result of fluorine determination is estimated by the «input – found» method. The mass fraction of chlorides is determined by calculation by difference between results of determining the sum of chlorides and bromides using the method of mercurometric titration and — separately — the bromides mass fraction. Optimal conditions of samples preparation and analysis for each of mentioned methods of analysis were selected. The limits of the relative total error of determining bromides in the range of mass fractions from 28.0 to 41.0% is ±2.1%, chlorides within the mass fraction range from 8.0 to 15.0% — ±3.6%, fluorides within the mass fraction range from 3.0 to 7.0% — ±3.4% using gravimetric method and within the mass fraction range from 5.0 to 8.0% — ±1.5% using a method of potentiometric titration. The developed techniques were certified by a metrological service of the enterprise and are used to control the chemical composition of the ion-conducting electrolyte. The techniques do not require expensive equipment, and can be used in factory laboratories.

Evaluation of Proximate, Organoleptic and Vitamin C Changes of Seaweed Jelly Candy (Gracillaria Sp.) after the Addition of Honey Mango Juice

Aims: to determine the effect of the addition of honey mango juice on the characteristics of jelly candy Study Design: This research was designed using a completely randomized design (CRD) with four treatments namely A (addition of 0% mango juice), B (addition of 9.93%% mango juice), C (addition of 12.5% mango juice) and D (addition of 16.07% mango juice) with 2 replications. Proximate and sensory data of jelly candy were analyzed by analysis of variance (ANOVA) and followed by honest real difference test at α5% level Place and Duration of Study: This research was conducted at the Makassar Health Laboratory Center (Chemical Testing) and Departemen of Aquatic Product Processing and Storage Workshop (Organoleptic Test) of Pangkep State Polytechnic of Agriculture from April to July 2024. Methodology: The analysis conducted in this study included chemical and organoleptic analysis. Chemical analysis included: analysis of water content by distillation method, total sugar content. Vitamin C levels through iodometric titration. Organoleptic (sensory) analysis included Odor, taste, texture and color. Results: The results showed that the addition of mango juice to the characteristics of jelly candy was significantly different to water content, total sugar content and vitamin C. The best product based on chemical analysis is jelly candy in treatment D with the highest vitamin C content (5520.1 µg/g) and the highest total sugar content (38.92%) while the lowest water content (11.21%) was found in treatment A. Tests on organoleptic assessment of the highest panelists in treatment D, namely Odor 3.8 (like), taste 4.2 (like), texture 3.2 (normal), and color 3.7 (like).

Development of a smartphone-based colorimetric detection for quantification of vitamin C in dietary supplements and skin care products

This research project presents a development of an assay tool for quantification of vitamin C in dietary supplements and skin care products. The proposed method was developed based on decolorization of acidic potassium permanganate (KMnO4) by vitamin C through a redox reaction, with subsequent colorimetric detection by using digital imaging. The imaging was carried out using smartphone camera and free-downloaded RGB color detector application. To obtain optimal conditions, influential parameters such as light source position installed inside a 19 cm × 46 cm × 10 cm lightbox, reagent concentrations, and reaction time were studied. To the best conditions, good linearity (r2 > 0.99) in the range 1–70 mg vitamin C/L was obtained. Relative standard deviation was less than 3.9% indicating high precision. The proposed method was validated by quantification of vitamin C content in 15 sample solutions using the proposed method in comparison with the reference iodometric titration method. The results obtained from those two methods were not significantly different using paired t-test at confidence level of 95% (texp=0.41, tcrit=2.14). The results indicated that utilizing smartphone camera with free-downloaded color detector application is possible as an alternative analysis tool for determination of vitamin C.

Capitalizing on the Iodometric Reaction for Energetic Aqueous Energy Storage.

Iodometric and iodimetric titrations represent a prevailing technique to determine the concentration of Cu2+ ions in aqueous solutions; However, their utilization in electrochemical energy storage has been overlooked due to the poor reversibility between CuI and Cu2+ related to the shuttling effect of I3- species. In this work, we developed a 4A zeolite separator capable of suppressing the free shuttling of I3- ions, thus achieving a record-high capacity retention of 95.7% upon 600 cycles. Theoretical and experimental studies reveal that the negatively charged zeolite can effectively impede the approach and penetration of I3- ions, as a result of electrostatic interaction between them. To explore the practical potential, a hybrid cell of Zn∥I2 consisting of Cu2+ redox agent has been assembled with a discharge capacity of 356 mA h g-1. The cell affords a specific energy of 443 W h kg-1 based on I2, or 193 W h kg-1 based on both electrodes. This work offers insight on the energy utilization of the iodometric reactions and advocates a Cu2+-mediated cell design that could potentially double the capacity and energy of conventional aqueous battery systems.

Near-room-temperature magnetic properties and magnetocaloric effect of polycrystalline and nano-scale manganites Pr(0.65-x)NdxSr0.35MnO3 (x ≤ 0.35)

Here we report investigations of structural, electrical and magnetic properties of bulk and nano-sized Pr0.65-xNdxSr0.35MnO3 compounds (x ≤ 0.35). Polycrystalline compounds were produced by solid – state reaction and nanocrystalline samples were obtained by sol–gel method. Analysis of x-ray diffraction patterns revealed a change in lattice structure from ‘Pbnm’ to ‘R3c’ symmetry, with diminishing cell volume upon increasing Nd ions substitution for all samples. Optical microscopy was used for bulk surface morphology and transmission electron microscopy was implemented for nano-sized samples. Iodometric titration showed oxygen deficiency for bulk compounds and oxygen excess for nano-sized particles. Measurements of resistivity of bulk samples revealed a single peak at temperatures associated with grain boundary conditions and with ferromagnetic/paramagnetic transition and negative magnetoresistivity. Critical magnetic behavior analysis disclosed that the polycrystalline samples are governed by a tricritical mean field and by 3D Heisenberg models while nanocrystalline samples are governed by a mean field model. Curie temperature Tc values remain in near room temperature range for all bulk compounds; they lower with increasing Nd ions substitution from 295 K for the parent bulk compound to 268 K for x = 0.35. Tc is lowered from 255 K for the parent nano-sized compound in small temperature intervals. All compounds exhibit second-order magnetic phase transitions and relatively high magnetic entropy change, with the highest value of 5.74 J/kgK for x = 0.25 bulk sample in μ˳∆H = 4 T. Strong magnetocaloric effect, stability and the possibility of fine-tuning Tc by Nd ions substitution make the investigated bulk polycrystalline compounds promising for application in magnetic refrigeration. Nano-sized samples possess lower magnetic entropy changes of maximum 2.4 J/kgK in μ˳∆H = 4 T for x = 0.15, but wider effective entropy change temperature (δTfwhm) and relative cooling power on par with other manganites, bringing them into the conversation as a viable option in cooling materials.

Oxygen Measurement in Cuprate Superconductors Using the Dissolved Oxygen/Chlorine Method

We have developed a dissolved oxygen (DO) method with differential equation (DE) correction. We measured the oxygen content in La-based and Y-based superconductors, and succeeded in measuring the oxygen content simply in one-third of the time required by the iodometric titration method. However, there was a problem with Bi-based superconductors where the measured oxygen content was smaller compared to the iodometric titration method. We hypothesized that not only O2 but also Cl2 gas is generated when dissolving Bi-based superconductors and developed a dissolved oxygen/chlorine (DO/Cl) method with DE correction. This method uses only a dissolved oxygen sensor and a dissolved chlorine sensor to measure the dissolved oxygen and dissolved chlorine content in Bi2Sr2−xLaxCuOy, allowing for the calculation of copper valence and oxygen content. The results from the DO/Cl method with DE correction show that the measured copper valence and oxygen content differ very little from those obtained using the iodometric titration method, with discrepancies within 0.016 and 0.008, respectively. Additionally, this method reduces the measurement time by one-third compared to the iodometric titration method. The results demonstrate that the DO/Cl method with DE correction can effectively measure the copper valence and oxygen content in cuprate superconductors, and using hydrochloric acid as the experimental solution is superior to sulfuric acid and nitric acid.

Electrocatalytic Properties of Quasi-2D Oxides LaSrMn0.5M0.5O4 (M = Co, Ni, Cu, and Zn) for Hydrogen and Oxygen Evolution Reactions.

Designing cost-effective and highly efficient electrocatalysts for water splitting is a significant challenge. We have systematically investigated a series of quasi-2D oxides, LaSrMn0.5M0.5O4 (M = Co, Ni, Cu, Zn), to enhance the electrocatalytic properties of the two half-reactions of water-splitting, namely oxygen and hydrogen evolution reactions (OER and HER). The four materials are isostructural, as confirmed by Rietveld refinements with X-ray diffraction. The oxygen contents and metal valence states were determined by iodometric titrations and X-ray photoelectron spectroscopy. Electrical conductivity measurements in a wide range of temperatures revealed semiconducting behavior for all four materials. Electrocatalytic properties were studied for both half-reactions of water-splitting, namely, oxygen-evolution and hydrogen-evolution reactions (OER and HER). For the four materials, the trends in both OER and HER were the same, which also matched the trend in electrical conductivities. Among them, LaSrMn0.5Co0.5O4 showed the best bifunctional electrocatalytic activity for both OER and HER, which may be attributed to its higher electrical conductivity and favorable electron configuration.

Evaluating the Influence of Environmental Factors on the Stability of Commercial Chlorine-Based Sanitizers Using Response Surface Modeling

Given the increasing use of chlorine-based disinfectants and concerns regarding their shelflife and persistence on the surface, the present study investigated the effect of environmental conditions on the stability of commercial solutions stored under different conditions. This study assessed the stability of 0.05%, 0.5%, and 1% sodium hypochlorite solutions at pH levels of 5, 7.5, and 10 stored at temperatures of 4 ° C, 25 ° C, and 45 ° C using iodometric titration at 0, 15, 30, and 60 days after preparation. Eighty-seven solutions from three commercial brands (Brand A, Brand B, and Brand C) were prepared based on experimental design and response surface modeling (RSM) using Box-Behnken factorial design (BBD). The results revealed that the linear coefficient effects of all factors (temperature, storage time, pH, and initial concentration) were statistically significant (P<0.05). However, no significant differences were found among the three commercial brands (P=0.307). A negative correlation was observed between free available chlorine (FAC) and storage time. Solutions with a higher initial concentration (1%) tended to have lower stability. Higher temperatures also contributed to the instability of the solutions. Moreover, a gradual decrease was observed in the pH over time, and the lowest stability was detected at a neutral pH of 7.5. These findings suggest that environmental conditions (e.g., temperature, storage duration, pH, and initial concentration) significantly affect the stability of chlorine in the solutions. Therefore, these factors should be considered when using chlorine and storing chlorine-based disinfectants (CBDs) to ensure optimal performance and effectiveness.

Study on removal of NO from flue gas by ferrous cysteine solution and analysis of reaction process

Wet denitrification technology has been extensively researched for its benefits in synergistically treating pollutants. As a representative complexing agent, ferrous cysteine (Fe2+(CyS)2) solution in the complex absorption method has attracted the attention of researchers. In this study, the influence of c(Fe2+):c(CySH) ratio, complexation time, initial pH value, and temperature on the NO removal efficiency and reaction process of Fe2+(CyS)2 in a bubbling reactor were investigated. The results highlighted the significance of the initial pH of the Fe2+(CyS)2 solution in denitrification efficiency, with higher pH leading to improved NO removal. The denitrification efficiency showed a volcano-like variation with increasing temperature and was not much affected by NO inlet concentration and Fe2+(CyS)2 solution complexation time. Under optimal conditions, the denitrification efficiency remained above 80 % for 3 h of continuous reaction, peaking at 98.4 %. Calculations of NO absorption capacity indicated the regeneration of Fe2+(CyS)2 solutions. Testing with iodometric and bromine-ferrous titration methods revealed that the reaction product of cysteine is cystine, maintaining material balance before and after the reaction. Experimental results validate Fe2+(CyS)2 as an effective and stable denitrification method, laying the foundation for potential industrial application.

Precise determination of oxygen content in SmBa2Cu3O7-δ thin film samples using x-ray diffraction

Abstract The superconducting properties of SmBa2Cu3O7-δ (SmBCO) thin films are predominantly influenced by the oxygen deficiency δ. Yet, the established methods to determine δ such as iodometric titration or thermogravimetry cannot be applied to thin films due to their very small volume.
Therefore, an alternative way to determine δ for SmBCO thin film samples using X-ray diffraction (XRD) is presented. Main point of this analysis is the structural relationship between the a, b and c lattice parameters and δ. A linear relationship between c and δ is found in SmBCO powder samples for both the orthorhombic and tetragonal phases.
Furthermore, an attempt is made to quantify the chemical composition using Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS). This attempt was inconclusive because of drastically changing ion yields due to δ influencing the valence state of the analyzed ions.
The found crystal structural relationship gathered from the powder samples is applied to thin film samples. Thereby, it becomes clear that thermal strain is affecting the crystal structure of the thin films. A simple correction model is used to correct for thermal strain and a good match between powder, literature and thin film data is achieved and thus a non-destructive way for the determination of δ using XRD.


Determination of the possibility of the synthesis of Zn-Al layered double hydroxides, intercalated with peroxyanions, as a perspective solid disinfectant

Infectious diseases in the modern world pose a significant threat to humanity in the form of epidemics and pandemics. To prevent and combat them, it is necessary to carry out antiseptic and disinfectant treatments of various environments, household and industrial surfaces, as well as wounds of various origins. Double-layer hydroxides intercalated with peroxyanions as active oxygen compounds are promising materials for this. In order to determine the possibility of obtaining Zn-Al double-layer hydroxide intercalated with peroxylactic acid anions, samples were synthesized by the method of chemical co-precipitation in the presence of peroxylactic acid at controlled pH (8, 10) and t=20 ℃. The properties of the synthesized samples were investigated. The content of active oxygen (in terms of H2O2) was determined by the method of iodometric titration with the calculation of the percentage of hydrogen peroxide that was intercalated in double layered hydroxides, remained in the mother solution or was lost. The crystal structure was studied by X-ray phase analysis, the yield of samples was determined gravimetrically, and sedimentation was determined by measuring and normalizing the thickness of the sediment layer. It was found that the samples synthesized at pH=8 and 10 are biphasic and consist of an oxide phase and a double-layer hydroxide phase. The determined content of active oxygen (in terms of H2O2) in the samples synthesized at pH=8 (0.533 %) and at pH=10 (0.876 %) confirms the success of the synthesis of Zn-Al-peroxylactate double layered hydroxides. Synthesis at elevated pH is promising. A low percentage of H2O2 intercalation was revealed – 4.03–6.54 %, the majority of hydrogen peroxide (82.36-94.44 %) remains in the mother solution. The yield of the synthesized samples was determined to be 61.9 % and 79.5 % at synthesis pH of 10 and 8, respectively. The sedimentation properties of the samples were studied and their improvement was shown when the pH of the synthesis was increased

A simple and rapid method for measuring total free sulfides in marine sediments

AbstractThe quantitatively most important process by which organic matter in marine sediments is mineralized is performed by sulfate‐reducing bacteria, resulting in the accumulation of total dissolved (free) sulfide (S2− = H2S + HS− + S2−) in porewater. S2− is toxic to benthic animals and vascular plants and measurements serve as a proxy for the deleterious effects of organic enrichment on benthic habitat, biodiversity, and ecosystem function. Methodologies for measuring S2− in water have been pursued for at least a century, and standard approaches employ colorimetry (methylene blue and iodometric titration) and potentiometry. These standard methods require between 1 and 200 mL of porewater, which can be laborious to obtain. The ion‐selective electrode method is widely employed as a practical approach for sediment S2− analysis but lacks analytical robustness and is highly prone to measurement biases that misinform research and environmental management decisions. A technically simple method is described, based on direct UV spectrophotometry, for the near real‐time field analysis of small porewater samples. The procedure prevents known measurement biases associated with particulate sulfide interference, S2− volatilization and oxidation, and represents a practical approach for monitoring organic enrichment and classifying benthic ecological quality status. Porewater concentrations between 200 and 15,000 μmol L−1 can be measured and instrument calibration is highly stable. The method has the capacity to rapidly process and analyze sediment samples at low cost, which helps resolve the problem of chronic under‐sampling associated with the use of traditional S2− methods.

Quality Assessment of Some Herbal Aphrodisiac Instant Coffee Premix Products Marketed in Kaduna, Nigeria

Aphrodisiac refers to any substance (food, drink or drug) or practice that is believed to stimulate sexual desire or enhance sexual pleasure and performance. There have been reports indicating lack of good manufacturing practices and adulteration of herbal aphrodisiac with phosphodiestrate-5 (PDE-5) inhibitors without consideration of public safety. The aim of this study is to assess the quality of three herbal aphrodisiac instant coffee premix products, through physicochemical analysis, elemental analysis, quantification of caffeine, detection and quantification of undeclared adulterants. Physicochemical properties of the three samples of herbal aphrodisiac products were determined using the methods described by World Health Organization 2011, while elemental analysis was conducted using nitric acidhydrochloric acid (1:3) digestion mixtures and subsequent analysis for the presence of lead, copper, cadmium, zinc and iron using micro plasma atomic emission spectrophotometer (MP-AES). Iodometric titration was used for quantification of caffeine levels in the samples while fourier transform infrared (FTIR) and ultraviolet (UV) spectroscopy were used for the detection and quantification of undeclared adulterants respectively. Moisture content (2.33 %, 2.83 % and 1.60 %) and ash value (10.50 %, 11.67 % and 0.98 %) of the samples A, B and C respectively were found to be within the official permissible limit. The samples were found to be rich in iron and zinc; however, the levels of lead, cadmium, and copper were above the WHO permissible limits. The concentrations of caffeine in the samples were less than the acceptable WHO limit of 400 mg/day. However, sildenafil was detected in two of the products (151.45 mg and 82.15 mg), while tadalafil was detected in one of the products (36.13 mg). The herbal aphrodisiacs were adulterated with either sildenafil or tadalafil, and contained relatively high levels of lead, cadmium, and copper. However, moisture content, ash value, and caffeine content met the WHO requirements.

Direct Recycling of β‐Li3PS4‐Based All‐Solid‐State Li‐Ion Batteries: Interactions of Electrode Materials and Electrolyte in a Dissolution‐Based Separation Process

All‐solid‐state batteries (ASSB) are currently developed at high pace and show a strong potential for market introduction within the next years. Though their performance has improved considerably over the last years, investigation of their sustainability and the development of suitable recycling strategies have received less attention. However, their potential for efficient circular processes must be accessed comprehensively. In this article, the separation of the solid electrolyte β‐Li3PS4 from different lithium transition metal oxide electrode materials (LiCoO2, LiMn2O4, LiNi0.8Mn0.1Co0.1O2, LiFePO4, LiNi0.8Co0.15Al0.05O2, and Li4Ti5O12) are investigated via an approach based on the dissolution and subsequent precipitation of the thiophosphate using N‐methylformamide as solvent. A combination of X‐ray diffraction, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, inductively coupled plasma mass spectrometry, iodometric titration, and X‐ray photoelectron spectroscopy as well as electrochemical impedance spectroscopy and electrochemical characterization is used to characterize the electrolyte and electrode materials before and after separation. Herein, it is found that the presence of electrode materials in the dissolution process can lead to significant chemical reactions. These interactions can (but most not) lead to strong alteration of the electrochemical characteristics of the individual compounds. Thus, it is shown that an efficient recovery of materials likely depends on the precise material combination within an ASSB.

Thermal and Mechanical Investigations of (Bi, Pb)-2212 Superconductor Added with Different Oxide Nanoparticles

Abstract The current study reports the synthesis of nano-(CdO)x/Bi1.6Pb0.4Sr1.9Ca1.1Cu2.1Oy, nano-(Cd0.95Mn0.05O)x/Bi1.6Pb0.4Sr1.9Ca1.1Cu2.1Oy, and nano-(Cd0.95Fe0.05O)x/Bi1.6Pb0.4Sr1.9Ca1.1Cu2.1Oy composites, with x = 0.00, 0.01, 0.02, 0.05, and 0.10 wt. %, respectively, using the classical solid-state reaction technique. X-ray powder diffraction (XRD) confirmed the formation of an orthorhombic structure of the (Bi, Pb)-2212 as the major phase. Thermogravimetric analysis was utilized to evaluate the thermal stability of the pure sample throughout the different stages of phase formation and the effect of nanoparticle addition. The weight loss/gain from the three additions is related to the excess of oxygen, as confirmed via iodometric titration analysis and from the findings of oxygen diffusion energy. Room temperature Vickers microhardness (HV) measurements were conducted at various applied loads (0.49–9.8 N). Based on the Vickers microhardness (HV) measurements, the optimum addition of nanoparticles for increasing the microhardness of the (Bi, Pb)-2212 phase was at x = 0.05 wt. % for all superconducting composites. Iron doped Cadmium Oxide (CdFeO) nanoparticles have the greatest enhancement on the Vicker hardness values (HV) at the plateau region. Furthermore, various mechanical parameters for potential applications, such as elastic modulus (E), yield strength (Y), and fracture toughness (K) of the samples under study, were consequently extracted from HV as a function of nanoparticle addition. Moreover, CdFeO addition outperformed CdO and Manganese doped Cadmium Oxide (CdMnO) addition in improving the parameters of E, Y, K, and B, which display better ductility and an enhanced capacity to resist indentation fractures and facilitate (Bi-2212) manufactured in the form of round wires that can be used in high magnetic field magnets, nuclear magnetic resonance instruments, and large hadron colliders. Different models were theoretically used to analyze the measured HV data in the plateau limit regions. The indentation-induced cracking model offered the most accurate theoretical model at the plateau limit region based on Vickers microhardness (HV) observations.

Epoxidation of cyclohexene with cyclohexyl hydroperoxide

Objectives. To investigate the regularities of the process of joint production of epoxycyclohexane, cyclohexanol, and cyclohexanone using the cyclohexene epoxidation reaction with cyclohexyl hydroperoxide in the presence of an ammonium paramolybdate catalyst, representing an alternative to the method of cyclohexanol and cyclohexanone synthesis by alkaline catalytic decomposition of cyclohexyl hydroperoxide.Methods. The qualitative and quantitative analysis of the obtained intermediate and target compounds was determined using modern physicochemical research methods: gas–liquid chromatography using the Chromatec-Crystal 5000.2 hardware and software complex with a flame ionization detector and infrared spectroscopy on an RX-1 infrared Fourier spectrometer. The content of hydroperoxide in the oxidation products was determined using iodometric titration, while the carboxylic acid content was determined by the titrimetric method based on the neutralization reaction.Results. The presented method for obtaining cyclohexanol and cyclohexanone together with epoxycyclohexane by the reaction of cyclohexene epoxidation with cyclohexyl hydroperoxide containing cyclohexane in the products of high-temperature liquid-phase oxidation is experimentally substantiated. The influence of various technological parameters on the process of liquid-phase oxidation of cyclohexane to hydroperoxide is described. The conditions for carrying out this reaction are determined to ensure the achievement of a content of cyclohexyl hydroperoxide of 1.5 wt % in the products of oxidation. The regularities of the epoxidation reaction of the synthesized cyclohexyl hydroperoxide with cyclohexene in the presence of an ammonium paramolybdate catalyst are analyzed.Conclusions. Epoxidation of cyclohexene with cyclohexyl hydroperoxide produced epoxycyclohexane at a yield of 80–90% and a conversion of cyclohexane hydroperoxide of 85%.

A facile double moving redox boundary model for visual electrophoresis titration of ascorbic acid.

In this work, we proposed a double moving redox boundary (MROB) model to realize the colorless analyte electrophoresis titration (ET) by the two steps of the redox reaction. Single MROB has been proposed for the development of ET sensing (Analyst, 2013, 138, 1137. ACS Sensor, 2019, 4, 126.), and faces great challenges in detecting the analyte without color change during redox reaction. Herein, a novel model of double-MROB electrophoresis, including its mechanisms, equations, and procedures, was developed for titration by using ascorbic acid as a model analyte. The first MROB was created with ferric iron (Fe3+) and iodide ion (I-) in which Fe3+ was reduced as Fe2+ and I- was oxidized as molecular iodine (I2) used as an indicator of visible MROB due to blue starch-iodine complex. The second boundary was then formed between the molecular iodine and model analyte of ascorbic acid. Under given conditions, there was a quantitative relationship between velocity of MROB (VMROB(ii)) and ascorbic acid concentration (CVit C) in the double-MROB system (1/VMROB(ii)=0.6502CVit C+4.5165, and R=0.9939). The relevant relative standard deviation values of intraday and inter-day were less than ∼5.55% and ∼6.64%, respectively. Finally, the titration of ascorbic acid in chewable vitamin C tablets was performed by the developed method, the titration results agreed with those via the classic iodometric titration. All the results briefly demonstrated the validity of the double MROB model, in which Vit C was used as a model analyte. The developed method had potential use in quantitative analysis of redox-active species in biomedical samples.

Maintenance and control of coating baths: Rapid and simultaneous hypophosphite and phosphite determination in a Ni[sbnd]P deposition bath

In this work, a method based on UV–VIS spectrophotometry using the molybdenum blue reaction is described to monitor hypophosphite and phosphite levels in nickel electroless baths. Nickel is one of the most employed metals in the electroless coating industry and during the deposition process the metal is reduced from Ni (II) to Ni (0). Hypophosphite is a widely employed reducing agent, which is oxidized to phosphite. Therefore, the hypophosphite concentration should be monitored in order to replenish the bath while it is being consumed maintaining an optimum concentration in order to guarantee the desired coating. Phosphite, which could interfere with the coating process, must be monitored to ensure it does not exceed a certain concentration after which the bath stops working. Although iodometric titrations are the most commonly used methods to control hypophosphite and phosphite concentrations, these are time- and reagent-consuming. Thus, with the aim of developing a more appropriate methodology a colorimetric determination was carried out in this work. In certain conditions, the hypophosphite reacts with molybdenum, giving rise to a blue compound that can be measured between 390 and 1100 nm. The phosphite presence modifies the obtained spectra and that effect allows individual Partial Least Square (PLS) models to be built for each analyte. In this study, the calibration, cross-validation and external prediction relative error were always lower than 8 %, and the relative standard deviation lower than 12 %. The models were applied to real samples from two different nickel electroless baths, and the results were compared and validated using ion chromatography (IC). No significant differences were observed between the proposed and the reference methods for either of the two analytes. Therefore, the colorimetric method could be an improvement over the methods currently used for the control of the two anions in coating baths in term of saving time, money and reagents, making the coating process more efficient.