Potentiometric Detection Research Articles

From Ions to Crystals: A Comprehensive View of the Non-Classical Nucleation of Calcium Sulfate.

After years ofintensive research andnumerous important observations, our understanding of the early stages of crystallization is still limited due to the complexity of the underlying processes and their elusive character. In the present work, we provide a detailed view on the nucleation of calcium sulfate mineralization - an abundant mineral with broad use in construction industry - in aqueous systems at ambient conditions. As experimental basis, a co-titration procedure with potentiometric, turbidimetric and conductometric detection was developed, allowing solution speciation and the formation of crystallization precursors to be monitored quantitatively as the level of nominal (super)saturation gradually increases. The nature and spatiotemporal evolution of these precursors was further elucidated by time-resolved small-angle X-ray scattering (SAXS) and analytical ultracentrifugation (AUC) experiments, complemented by cryogenic transmission electron microscopy (cryo-TEM) as a direct imaging technique. The results reveal how ions associate into nanometric primary species, which subsequently aggregate and develop anisotropic order by intrinsic structural reorganization. Our observations challenge the common understanding of fundamental notions such as the nucleation barrier or the meaning of supersaturation, with broad implications for mineralization phenomena in general and the formation of calcium sulfate in geochemical settings and industrial applications in particular.

Optimization of the polyaniline solid contact in potentiometric sensors for detection of paralytic shellfish toxins in mussels

The present study optimized the properties of the electropolymerized polyaniline (PANI) solid inner contact for a potentiometric chemical sensor by varying the thickness of the polymer layer. A potentiometric sensor for detecting one of the paralytic shellfish toxins, decarbamoyl saxitoxin (dcSTX), in mussel extracts was selected as a case study. The plasticized PVC membrane composition, developed in previous work for the detection of this toxin, was used. The structure and electrical properties of PANI layers of different thicknesses were studied using scanning electron microscopy and electrochemical impedance spectroscopy. The effect of PANI solid contact thickness on the characteristics of the potentiometric sensor, including sensitivity, detection limit, and selectivity to dcSTX in buffer solutions and mussel extracts, was evaluated. The formation of a water layer at the inner solid contact and PVC membrane interface was investigated using electrochemical impedance spectroscopy and a water test. PANI layer thickness 1.1 µm was found to be optimal for solid inner contact for potentiometric sensor with PVC membrane providing highest sensitivity and selectivity.

Lab-on-a-chip paper-based electrochemically assisted solid-phase microextraction and ion selective sensor for determination of naproxen in biological fluid samples

BackgroundThe integration of paper-based analytical devices with lab-on-a-chip technology has opened up new possibilities for miniaturized, rapid, low cost and portable diagnostic testing in resource limited settings. This work introduces an integrated lab-on-a-chip platform coupling paper-based analytical devices (LOC-PADs) for dual usage: electrochemically controlled solid-phase microextraction (EC-SPME) and determination of naproxen (NAP) by potentiometric ion-selective electrode (ISE) in biological samples. ResultsConductive papers were successfully fabricated by a chemical procedure. Thereupon, a conducting molecularly imprinted polymer (CMIP) film based on PPy and an anionic model drug (NAP) as a template were applied to the conductive paper substrate via electrochemical methods. A microfluidic chip device was employed to assess the analytical performance of the fabricated paper-based CMIP. The designed chip is divided into two parts with a microfluidic channel between them. The first chamber is an extraction zone for EC-SPME of NAP by using the CMIP paper as a selective sorbent. The second chamber is the detection zone and consists of a paper-based NAP ion selective sensor for potentiometric detection of drug. The analytical process was investigated and optimized for each chamber. Remarkable selectivity towards NAP was achieved in the concentration range from 4.0 × 10−7 to 1.0 × 10−2 mol L−1 with determination coefficient (R2 = 0.99) and the limit of detection (LOD) was 2.0 × 10−7 mol L−1. Anionic Nernstian compliance was gained −58.5 ± 0.5 mV decade−1, and response time in the detection step was 7s for ISE. Satisfactory spiking recovery values within the acceptable range of 90–110 % with RSDs ≤7 % were achieved for the analysis of real samples with fully portable LOC device. SignificanceThe LOC-PADs were favorably used for selective extraction and determination of NAP in serum and saliva samples, respectively. EC-SPME caused sample clean-up, reduced or eliminated different interferences and enhanced selective response of ISE as detection zone of device. Integration of EC-SPME and ISE in a single chip enabled easy and fast determination of trace amounts of NAP in limited real sample volumes, and fully portable advantages.

Double Type Detection of Triiodide and Iodide Ions Using a Manganese(III) Porphyrin as Sensitive Compound.

A paramagnetic A3B-type Mn(III)-porphyrin was synthesized and characterized by physical-chemical methods (UV-Vis, FT-IR, 1H-NMR spectroscopy). The obtained compound was tested as a sensitive material for the spectrophotometric and potentiometric detection of iodine species. Using UV-Vis spectroscopy, the triiodide anions could be detected with high precision in the concentration interval of 1.02 × 10-5 to 2.3 × 10-5 M, with an LOD of 9.44 × 10-6 M. The PVC-based electrode using DOP as a plasticizer showed a sensitivity toward iodide in a wide concentration range of 1.0 × 10-5 to 1.0 × 10-1 M, with an LOD of 8.0 × 10-6 M. Both methods are simple, low-cost, and efficient for the detection of iodine species in synthetic samples and pharmaceuticals.

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.

Depth-resolved potentiometric detection of active species near the surface of an aqueous solution under atmospheric pressure plasma

Depth-resolved potentiometric detection of active species near the surface of an aqueous solution under atmospheric pressure plasma

Potentiometric detection of apomorphine in human plasma using a 3D printed sensor

Apomorphine is a dopamine agonist that is used for the management of Parkinson's disease and has been proven to effectively decrease the off-time duration, where the symptoms recur, in Parkinson's disease patients. This paper describes the design and fabrication of the first potentiometric sensor for the determination of apomorphine in bulk and human plasma samples. The fabrication protocol involves stereolithographic 3D printing, which is a unique tool for the rapid fabrication of low-cost sensors. The solid-contact apomorphine ion-selective electrode combines a carbon-mesh/thermoplastic composite as the ion-to-electron transducer and a 3D printed ion-selective membrane, doped with the ionophore calix[6]arene. The sensor selectively measures apomorphine in the presence of other biologically present cations – sodium, potassium, magnesium, and calcium – as well as the commonly prescribed Parkinson's pharmaceutical, levodopa (L-Dopa). The sensor demonstrated a linear, Nernstian response, with a slope of 58.8 mV/decade over the range of 5.0 mM–9.8 μM, which covers the biologically (and pharmaceutically) relevant ranges, with a limit of detection of 2.51 μM. Moreover, the apomorphine sensor exhibited good stability (minimal drift of just 188 μV/hour over 10 h) and a shelf-life of almost 4 weeks. Experiments performed in the presence of albumin, the main plasma protein to which apomorphine binds, demonstrate that the sensor responds selectively to free-apomorphine (i.e., not bound or complexed forms). The utility of the sensor was confirmed through the successful determination of apomorphine in spiked human plasma samples.

Nonenzymatic Potentiometric Detection of Ascorbic Acid with Porphyrin/ZnO-Functionalized Laser-Induced Graphene as an Electrode of EGFET Sensors.

Laser-induced graphene (LIG) has emerged as a highly versatile material with significant potential in the development of electrochemical sensors. In this paper, we investigate the use of LIG and LIG functionalized with ZnO and porphyrins-ZnO as the gate electrodes of the extended gate field effect transistors (EGFETs). The resultant sensors exhibit remarkable sensitivity and selectivity, particularly toward ascorbic acid. The intrinsic sensitivity of LIG undergoes a notable enhancement through the incorporation of hybrid organic-inorganic materials. Among the variations tested, the LIG electrode coated with zinc tetraphenylporphyrin-capped ZnO nanoparticles demonstrates superior performance, reaching a limit of detection of approximately 3 nM. Furthermore, the signal ratio for 5 μM ascorbic acid relative to the same concentration of dopamine exceeds 250. The practical applicability of these sensors is demonstrated through the detection of ascorbic acid in real-world samples, specifically in a commercially available food supplement containing l-arginine. Notably, formulations with added vitamin C exhibit signals at least 25 times larger than those without, underscoring the sensors' capability to discern and quantify the presence of ascorbic acid in complex matrices. This research not only highlights the enhanced performance of LIG-based sensors through functionalization but also underscores their potential for practical applications in the analysis of vitamin-rich supplements.

Multifunctional Siloxene-Decorated Laser-Inscribed Graphene Patch for Sweat Ion Analysis and Electrocardiogram Monitoring.

Potentiometric detection in complex biological fluids enables continuous electrolyte monitoring for personal healthcare; however, the commercialization of ion-selective electrode-based devices has been limited by the rapid loss of potential stability caused by electrode surface inactivation and biofouling. Here, we describe a simple multifunctional hybrid patch incorporating an Au nanoparticle/siloxene-based solid contact (SC) supported by a substrate made of laser-inscribed graphene on poly(dimethylsiloxane) for the noninvasive detection of sweat Na+ and K+. These SC nanocomposites prevent the formation of a water layer during ion-to-electron transfer, preserving 3 and 5 μV/h potential drift for the Na+ and K+ ion-selective electrodes, respectively, after 13 h of exposure. The lamellar structure of the siloxene sheets increases the SC area. In addition, the electroplated Au nanoparticles, which have a large surface area and excellent conductivity, further increased the electric double-layer capacitance at the interface between the ion-selective membranes and solid-state contacts, thus facilitating ion-to-electron transduction and ultimately improving the detection stability of Na+ and K+. Furthermore, the integrated temperature and electrocardiogram sensors in the flexible patch assist in monitoring body temperature and electrocardiogram signals, respectively. Featuring both electrochemical ion-selective and physical sensors, this patch offers immense potential for the self-monitoring of health.

Non-enzymatic paper-based analytical device for direct potentiometric detection of urine creatinine.

A paper-based analytical device (PAD) with an integrated composite electrode has been designed and fabricated for non-enzymatic creatinine sensing. Reduced graphene oxide (rGO) was employed to modify the PAD so that it could function as a solid-contact transducer. A new macrocyclic pyrido-hexapeptide derivative was made and used as a special ionophore in the creatinine membrane sensor. The synthesized PAD showed a detection limit of 1.0µM (S/N = 3) and a potentiometric response towards creatinine throughout a log-linear range of 2.0µM-10mM (R2 = 0.9998). The sensor shows significant selectivity for a few related substances, including ephedrine, codeine, ketamine, caffeine, urea, urate, carbinoxamine, and dextromethorphan. It has been established that the testing method is appropriate for the direct potentiometric detection of creatinine in a variety of human urine sample types. When an indicating electrode and a reference electrode are put on the same flexible disposable, this lets applications with a small sample volume be done. For point-of-care creatinine measurement, the developedpaper-based analytical equipment is a good choice because it is affordable, easily accessible, and self-pumping (especially when combined with potentiometric detection).

Imprinted polymer/reduced graphene oxide-modified glassy carbon electrode-based highly sensitive potentiometric sensing module for imidacloprid detection

A sensitive and highly selective potentiometric sensor for imidacloprid detection (IMD) is presented. Reduced graphene oxide (rGO) was used to modify a glassy carbon electrode in the fabrication of this sensor. The rGO is coated with IMD molecularly imprinted polymer (MIP), which serves as a sensing compound for herbicide recognition. Under ideal circumstances, a linear range of 0.5 µM-1.0 mM was measured, with a detection limit of 0.2 µM IMD. The method exhibits great selectivity towards the IMD's determination, according to the examination of the effects of potentially interfering species. For the direct potentiometric detection of IMD in several pesticide formulation samples, the assay method has been validated and shown to be adequate. The obtained recovery ranges from 94.5 to 106.4 % of the nominal or spiked concentration, with a mean relative standard deviation of 1.3 %. The applicability outcomes of using the presented sensor were contrasted with those attained by high-performance liquid chromatography (HPLC). There was no discernible difference between the suggested and HPLC procedures. Due to the sensitive membrane's and the liquid junction's proximity, this module's use permits applications with a small sample volume. The proposed sensor's effectiveness in a complicated matrix points to applications for rapid detection and tests for quality assurance and control in the agro-industry.

Potentiometraic Method for Determining Biologically Non-Degradable Antimicrobial Substances

Ion selective electrodes (ISEs) based on polymer plasticized membranes have been developed for the determination of benzalkonium chloride (alkyldimethylbenzylammonium), the active component being cesium bis-octodecyl-2-sulfonio-closo-decaborate Cs[B10H9S(C18H37)2] (sensor A). For the determination of norfloxacin hydrochloride, the active component is potassium tris-octodecyl-1-ammonio-closo-decaborate K[B10H9N(C18H37)3] (sensor B). It has been shown that the electrodes have a reversible potentiometric response with respect to the analyzed cations in the presence of a number of other inorganic and organic cations. The influence of the concentration of the electrode-active substance on the electrochemical characteristics of the manufactured sensor has been studied. The optimal composition of the ion-sensitive membrane has been found. It has been determined that the developed sensors provide a wide range of detectable concentrations (for sensor A, 2 × 10–7–1 × 10–2; for sensor B, 1 × 10–7–1 × 10–2) and a low detection limit (for sensor A, 1 × 10–7 M; for sensor B, 8 × 10–8 M). New ISEs can be recommended for direct potentiometric detection of free ions in water bodies and water extracts of soils.

Electrogenicity of microbial biofilms of medically relevant microorganisms: potentiometric, amperometric and wireless detection

Since the progression of biofilm formation is related to the success of infection treatment, detecting microbial biofilms is of great interest. Biofilms of Gram-positive Staphylococcus aureus and Streptococcus gordonii bacteria, Gram-negative Pseudomonas aeruginosa and Escherichia coli bacteria, and Candida albicans yeast were examined using potentiometric, amperometric, and wireless readout modes in this study. As a biofilm formed, the open circuit potential (OCP) of biofilm hosting electrode (bioanode) became increasingly negative. Depending on the microorganism, the OCP ranged from −70 to −250 mV. The co-culture generated the most negative OCP (−300 mV vs Ag/AgCl), while the single-species biofilm formed by E. coli developed the least negative (−70 mV). The OCP of a fungal biofilm formed by C. albicans was −100 mV. The difference in electrode currents generated by biofilms was more pronounced. The current density of the S. aureus biofilm was 0.9‧10−7 A cm−2, while the value of the P. aeruginosa biofilm was 1.3‧10−6 A cm−2. Importantly, a biofilm formed by a co-culture of S. aureus and P. aeruginosa had a slightly higher negative OCP value and current density than the most electrogenic P. aeruginosa single-species biofilm. We present evidence that bacteria can share redox mediators found in multi-species biofilms. This synergy, enabling higher current and OCP values of multi-species biofilm hosting electrodes, could be beneficial for electrochemical detection of infectious biofilms in clinics. We demonstrate that the electrogenic biofilm can provide basis to construct novel wireless, chip-free, and battery-free biofilm detection method.

Paper-Based Analytical Device Based on Potentiometric Transduction for Sensitive Determination of Phenobarbital.

In medicine, barbiturates are a class of depressive medications used as hypnotics, anticonvulsants, and anxiolytics. For the treatment of specific forms of epilepsy and seizures in young children in underdeveloped countries, the World Health Organization recommends phenobarbital (PBAR), a barbiturate drug. This review describes the fabrication and characterization of a paper-based analytical apparatus for phenobarbital detection that is straightforward, affordable, portable, and disposable. All of the solid-state ion-selective electrodes (ISEs) for PBAR as well as a Ag/AgCl reference electrode were constructed and optimized on a nonconductive paper substrate. Using carbon nanotube ink, the sensors were made to function as an ion-to-electron transducer and to make the paper conductive. A suitable polymeric membrane is drop-cast onto the surface of the carbon ink orifice. The pyrido-tetrapeptide and pyrido-hexapeptide derivatives, which were recently synthesized, functioned as distinct ionophores in the PBAR-membrane sensor, enabling its detection. With a detection limit of 5.0 × 10-7 M, the manufactured analytical device demonstrated a Nernstian response to PBAR anions in 50 mM phosphate buffer, pH 8.5, over a linear range of 1.0 × 10-6 to 1.0 × 10-3 M. The PBAR-based sensors showed quick (less than 5 s) response times for PBAR ion detection. The modified separate solution method was utilized to evaluate the selectivity pattern of these novel ionophores with respect to PBAR ions in comparison to other common anions. The analytical instrument that was exhibited on paper had good precision both within and between days. The suggested technology assisted in the detection of trace amounts of PBAR in real pharmaceutical samples. A comparison was made between the data acquired using the HPLC reference method and the information obtained by the recommended potentiometric approach. The described paper-based analytical device may be a good choice for point-of-care PBAR determination because it is cheap and easy to find and can self-pump (especially when combined with potentiometric detection).

Fast and novel multiwalled carbon nanotubes decorated with metal oxide nanoparticles for potentiometric detection of a prohibited medication in sports acebutolol hydrochloride

A straightforward approach for creating fast and novel potentiometric sensors that are modified with multi-walled nanotubes (MWCNTs) was described. The impact of the selective sensor's material was studied. The suggested sensors were successfully fabricated for instant and fast detection of the prohibited β-adrenoreceptor blocking agent acebutolol hydrochloride (AC) in commercial products. Acebutolol-phosphomolybdate (AC-PM) carbon paste sensor was formed by mixing AC and phosphomolybdic acid and graphite powder in the presence of o-nitrophenyl octyl ether (o-NPOE) as a plasticizing agent. The functionalized AC-PM-MWCNTs and AC-PM-MWCNTs-Al2O3 nanocomposite sensors were prepared and all parameters affecting the sensors' potential responses have been investigated as well as the green synthesis of Al2O3NPs has been characterized using various microscopic and spectroscopic techniques. AC-PM-MWCNTs and AC-PM-MWCNTs-Al2O3 nanocomposite sensors demonstrated linearity of 1.0 × 10−7-1.0 × 10−2 and 1.0 × 10−8-1.0 × 10−2 mol L−1, respectively with regression equations −53.571x + 423.24 (r = 0.999) and −57.107x + 518.54 (r = 0.999). It also revealed excellent selectivity and sensitivity for the determination and quantification of AC. The developed potentiometric system was suitable for the determination of AC in bulk powder and commercial products.

Near-Infrared Laser Irradiation-Modulated High-Temperature Solid-Contact Ion-Selective Electrodes: Potentiometric Detection of Ca2+ in Seawater.

The high-temperature potentiometry operated by nonisothermal heating is a promising way to break through the traditional potentiometric responses of ion-selective electrodes (ISEs) at room temperature. Herein, a locally heated strategy through near-infrared region (NIR) laser irradiation upon the photothermal mesoporous carbon material placed between the ion-selective membrane and the glassy carbon substrate is introduced to obtain the high-temperature potentiometric performance of a solid-contact Ca2+-ISE for detection of Ca2+ in seawater. Based on the light-to-heat conversion of the mesoporous carbon-based solid contact, the temperature of the solid-contact Ca2+-ISE upon continuous NIR laser irradiation can be increased from room temperature to 60-70 °C, and the slope of the electrode is promoted up to about 30% according to the thermodynamic steady-state potentiometric response. The pulsed potentiometric response of the solid-contact Ca2+-ISE upon a pulsed NIR laser irradiation of 5 s also shows a linear change as a function of Ca2+ activities, and the improved slope from 27.1 ± 0.6 to 38.1 ± 0.9 mV/dec can be obtained under dual control of the temperature of the electrode and the transient current induced by the pulsed NIR laser irradiation. As compared to the traditional potentiometric measurement under zero-current conditions at room temperature, the NIR laser-modulated high-temperature potentiometric response provides an alternative way for measurement of the solid-contact ISEs.

Development of Smart Potentiometric Sensors Covered with Non-Biofouling Layer for Detection of Early Stages of Inflammatory Processes Around Joint Replacements

One of the problems occurring after the joint replacement is connected with the post-surgery infections which are caused by bacteria that form biofilms on surfaces and are referred to as biofilm-related infections (BRI). It is also worth noting that due to the bioresponse, strong pathophysiological changes in the microclimate of an affected surface occur (decrease in pH, formation of various reactive oxygen species (ROS), depletion of Fe ions, and increase in the concentration of Ca ions). In this work we have prepared a robust selective potentiometric sensor of ROS and pH sensor for the detection of pH changes caused by sterile inflammation and bacterial and fungal infections. The ROS sensor consists of a conductive polymer layer based on polythiophene with an incorporated porphyrin-metal complex that potentiometrically detects the presence of ROS (H2O2 and ClO– ions). This sensor is connected by the covalent bonds with a non-biofouling layer of poly(2-methyl-2-oxazoline), which works as a bio-compa­tibilizer. It was shown that the potentiometric sensor shows a rapid response to hydrogen peroxide, does not record any interference with bovine serum albumin as a model serum protein, and is able to fully reversibly detect ROS with a linear response within a wide range of biological relevant concentrations (from 0.05 μM to 10 μM). The sensing electrode based on polyaniline and poly(2-methyl-2-oxazoline) on a titanium alloy support was developed for the potentiometric detection of peri-implant pH changes to enable early detection of the aforementioned pathologies. The developed electrodes show the changing of pH in the range between 5 and 8 for the individual pathogenic bacteria or pathogenic yeast, with a Nernstian slope of −59.6/pH.

Quantification of underivatized amino acids in solid beverages using high-performance liquid chromatography and a potentiometric detector

The simultaneous quantification of amino acids (AAs) in solid beverages without prior derivatization was explored by high-performance liquid chromatography (HPLC) coupled to a potentiometric detector. Included were threonine, leucine, methionine, phenylalanine, and histidine. The potentiometric detector was made consisting of a copper(II)-selective electrode based on a polyvinyl chloride (PVC) membrane, and the potential changes in the detector were determined according to the coordination interactions between cupric copper ions released from the inner filling solution of the electrode and AAs. Conditions were optimized for effective separation and sensitive detection. Fundamental characteristics such as linearity, limits of detection, limits of quantitation, accuracy, precision, and robustness were validated experimentally. The calibration curves showed a linear relationship between peak heights and the injection concentrations of the AAs. The detection limits down to the sub-micromolar range were achieved under isocratic conditions, outperforming ultraviolet detection. The copper(II)-selective electrode had a minimum lifetime of one month. Some real samples were examined to further demonstrate the feasibility of the proposed approach. The measurement results obtained by the present method were in good agreement with those obtained by the HPLC-mass spectrometry (MS), indicating that the combined HPLC-potentiometric method is a potential option for quantifying AAs.

Fabrication and characterization of mullite nano-ceramic materials for use in carbon paste ion selective electrode to estimate carcinogenic Cd (II) ion in real and human samples

Ion-selective electrodes are preferable to competing electrochemical methods for potentiometric detections regarding operating convenience, speed, and cost. The development of a novel class of carbon-paste electrochemical sensor that exploits synthetic mullite (3Al2O3.2SiO2) nanoparticles as an ionophore is investigated in this research. These mullite nanoparticles were synthesized using the sol–gel process, and a variety of methods were utilized to characterize them, including X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) coupled with EDAX, and Brunauer-Emmett-Teller (BET) analysis. Nano-mullite's crystal structure has been verified by the XRD technique and crystallite size was established by the Debye-Scherrer equation (average crystallite size 9 nm). SEM and TEM have verified its nanoscale (the particle size between 16.08 nm and 45.5 nm). The BET study confirms the huge surface area (82.1164 m2/g), average pore size equal to 5.323 nm, and mesoporous structure of the mullite nanoparticle. Mullite nanoparticles, which have a substantial surface area, a porous structure, nano size, and electrical activity, are incorporated into the electrode composition to speed up the processes of electron transfer. The modified carbon paste electrode (MCPE) has been estimated in the function of a selective sensor for cadmium ion detection. Under ideal conditions, the potentiometric approach verified a straight reactivity forward into Cd (II) ion in varying concentrations from 1.0 × 10-8 to 1.0 × 10-2 mol/L with a limit of detection of 1.0 × 10-8 mol/L and a Nernstian slope of 29.49 ± 0.24 mV decade-1. The paste composition that produced the best results had, in order, 67.3 % graphite, 3.5 % TCP, and 2.7 % nano-mullite. The designed sensor has a short response time of 6 s, may well be maintained for nearly 10 weeks in the pH interval of 3.0 to 8.0, and had good thermal stability in the interval of 10 to 60 °C without deviating from Nernstian behavior. Considering the diversity of metal ions, the electrode showed good Cd(II) ion selectivity. Cd(II) ion was measured in water, cigarettes, hair, nails, natural and synthetic dyes. The outcomes of validation techniques perform superior to the ICP methodology. The potentiometric titration of Cd(II) ions with EDTA was successfully realized utilizing the MCPE with a sharp inflexion at the endpoint.

Asymmetric Pt(II)-Porphyrin Incorporated in a PVC Ion-Selective Membrane for the Potentiometric Detection of Citrate

A new sensing material, Pt(II)-5-(4-carboxyphenyl)-10,15,20-tris(4-phenoxyphenyl)-porphyrin (Pt(II)-COOH-TPOPP), was synthesized and characterized. Polymeric membranes containing the porphyrin and three different plasticizers were used as an electroactive material for a new anion-selective sensor. The best composition of the membrane was the one plasticized with dioctylsebacate (DOS), the obtained sensor being citrate-selective in a linear range of 5 × 10−7–1 × 10−1 M citrate. The slope was Nernstian (19.73 mV/decade) with good selectivity towards a number of interfering anions and a lifetime of five weeks.