Electrochemical Techniques Research Articles

Ammonia Gas Sensing Using Porous silicon

Abstract Psi prepared by Electrochemical etching technique at invariable etching current density of 10 mA/cm2 and at different times (7 and 17) min. The porous Si structure was studied using XRD, (FE-SEM) and EDS. The process of sensing NH3 gas is carried out at different operating temperatures (R.t,80,130 and 200)°C and the gas concentration is constant. It is measured by changing the resistance of the sensor as a function of exposure time to the gas. The result showed the XRD patterns of the PS at (7 and 17) min etching time. the peak samples at (111) around 2θ = 28.5°. It is observed that the peak intensity declines with rising the etching time, and some structural parameters for porous silicon are calculated. From FE-SEM, the images show the sample prepared in (7 and 17) min with the depth of (6.18 12.82) μm, with a size of about 50 nm. Porous silicon that was produced in a time of 17 min has a higher sensitivity to NH3 gas than that of the sample that was produced in a time of 7 min. It was found that when the operating temperature changes from (R.T -200C°), the sensitivity of the samples changes with the stability of the etching time. The PSi sample (17 min) has a high sensitivity for NH3 gas at room temp.

Electrochemical exfoliation of graphene nanosheets and development of a novel efficient Ni-CeO2-Gr ternary nanocomposite coatings for dual functional anti-corrosion and wear-resistance

Nickel-based coatings offer excellent corrosion, wear resistance, and mechanical strength, and can be further improved with additives, making them ideal for harsh environments like marine and chemical industries. In the present study, graphene (Gr) nanosheets were synthesized via electrochemical exfoliation and a novel Ni-CeO2-Gr nanocomposite coating was prepared by an electrochemical co-electrodeposition technique on a Cu substrate in a traditional Watts bath. The coatings (pure Ni, Ni-Gr, Ni-CeO2 and the ternary Ni-CeO2-Gr) were characterized using optical microscopy, scanning electron microscopy (SEM) coupled with energy-dispersive spectrometry (EDS), X-ray diffraction (XRD), Raman spectroscopy, Vickers microhardness and micro-scratch tests. The electrochemical properties of the coatings were evaluated by electrochemical impedance (EIS) and DC-polarization measurements in 0.5 M NaCl. SEM-EDS, Raman, and XRD analysis confirmed the successful synthesis of high-quality graphene and the incorporation of CeO2 nanoparticles and graphene nanosheets into the nickel coating matrix. It was found that the ternary Ni-CeO2-Gr coating exhibited a high microhardness (915.6 HV), improved cohesive strength and enhanced corrosion resistance (544 KΩ.cm−2) compared to pure Ni coatings (30 KΩ.cm−2) due to the synergistic effect of the graphene and CeO2 duplex layer within the Ni matrix, forming a robust anticorrosion barrier. These findings offer valuable insights into the designing highly efficient materials for corrosion protection.

The effects of ECAP, Mn and Ca elements on the microstructure and corrosion properties of magnesium alloys were investigated

In this study, through reasonable composition design, three elements of Zn, Mn and Ca, which are harmless to human body, were selected for alloying magnesium. The effects of ECAP treatment on the microstructure and corrosion properties of Mg-4Zn-1Mn-0Ca, Mg-4Zn-1Mn-0.2Ca and Mg-4Zn-0Mn-0.2Ca alloys were studied. The corrosion mechanism of Mg-Zn-Mn-Ca alloys with different components in Simulated. Body fluid (SBF) was analyzed by weight loss method and electrochemical test. The grains and the second phase were refined by Equal Angular Channel Pressing (ECAP). It was found that after 8 ECAP deformations, the microstructure of the alloy was refined and more uniform than that of the extruded alloy. The corrosion resistance of the Mg-Zn-Mn-Ca alloy after ECAP deformation in simulated body fluids was studied by electrochemical testing techniques, immersion experiments and observation of the microstructure and morphology of corrosion products. The relationship between microstructure characteristics, the behavior of the magnesium metal matrix and the properties of corrosion products was revealed. The results show that the microstructure of the alloy is refined and the corrosion resistance is improved with the increase in extrusion passes in the SBF solution. The corrosion resistance of magnesium alloy after 8 ECAP deformation is the best, showing small Icorr and large Rt. With the extension of the soaking time, the surface of the alloy will form a passivation film, which will protect the matrix and avoid further corrosion of the alloy. It is found that in SBF, the corrosion of the alloy surface is mainly pitting, which indicates that Ca2+, HCO3- and HPO42- in SBF can reduce the corrosion rate of magnesium alloy.

Performance and potential mechanisms for reactive electrochemical ceramic membrane system to inhibit resistance transmission in antibiotic-resistant contaminated wastewater: From a microbial perspective

Due to the widespread presence of antibiotic resistance genes (ARGs) in traditional biological wastewater treatment systems, electrochemical disinfection techniques have received extensive attention. The rTNA/Sb-SnO2/PbO2 Reactive Electrochemical Ceramic Membrane (RECM) system has demonstrated outstanding performance in effectively removing refractory antibiotics. However, its capacity to remove antibiotic resistant bacteria (ARB) remains unclear. In this study, an antibiotic resistant strain of Escherichia coli (AR E. coli) was employed to investigate the disinfection efficiency of the RECM system at a macroscopic level, along with its disinfection mechanism at a microscopic level. Furthermore, the secondary effluent from an antibiotic production wastewater treatment plant was collected to validate the disinfection performance of this system against ARB in actual wastewater. In the RECM system, the inactivation of AR E. coli and the removal of ARGs were primarily governed by the electrocatalytic process, with notable influences from critical factors such as current density, electrolyte type, and hydraulic retention time. Morphological observation and flow cytometry experiments confirmed that the AR E. coli in the RECM system was inactivated by alterations in cell morphology, leading to fragmentation, and by improvement in cell membrane permeability. More significantly, this system exhibited noteworthy efficiency in treating wastewater contaminated with antibiotic resistant pollutants, effectively eliminating both antibiotics and ARGs from the secondary effluent. Overall, our study comprehensively investigated the performance and underlying mechanisms of the RECM system in mitigating the dissemination of ARGs, as well as its potential feasibility of practical application.

Synthesis, characterization and corrosion inhibition evaluation of a new chalcone derivative 2-3-(3-hydroxyphenyl)-1-[4-(1H-imidazol-1-yl) phenyl] prop-2-en-1-one for mild steel corrosion in 1M HCl assessment with DFT and MD studies

The prime objective of the work focuses on the synthesis of novel chalcone derivative, the 2-3-(3-hydroxyphenyl)-1-[4-(1H-imidazol-1-yl) phenyl] prop-2-en-1-one (HIPP) and study its corrosion inhibition for mild steel in 1M HCl. Various spectroscopic techniques such as IR, 1H-NMR, 13C-NMR, and mass spectroscopy were used to confirm the formation of the synthesized chalcone. Distinct electrochemical techniques like potentiodynamic Tafel polarization and impedance spectroscopy were employed to investigate HIPP in 1M HCl as a mild steel corrosion inhibitor. The synthesized chalcone was checked in a temperature range varying from 30o C to 60o C. With increasing quantities of HIPP, it is noticed that there is an enhancement in calculated corrosion inhibition efficiency. The maximum inhibition efficiency obtained was found to be 94.3 % in the presence of 100 ppm at room temperature. Surface morphology of unhindered and inhibited HIPP was analysed using scanning electron microscopy (SEM), atomic force microscopy (AFM) and water contact angle (WCA) measurements. SEM investigation revealed that the inhibitor effectively protects the metal surface from aggressive corrosion. Atomic force microscopic images show the corroded MS surface roughness in the presence of HIPP reduced from 342.1 nm to 174.3 nm. Furthermore, the inhibitor's adsorption through electron-donor acceptor interactions was revealed by DFT calculations and MD studies.

Shattering the Water Window: Comprehensive Mapping of Faradaic Reactions on Bioelectronics Electrodes.

It is generally accepted that for safe use of neural interface electrodes, irreversible faradaic reactions should be avoided in favor of capacitive charge injection. However, in some cases, faradaic reactions can be desirable for controlling specific (electro)physiological outcomes or for biosensing purposes. This study aims to systematically map the basic faradaic reactions occurring at bioelectronic electrode interfaces. We analyze archetypical platinum-iridium (PtIr), the most commonly used electrode material in biomedical implants. By providing a detailed guide to these reactions and the factors that influence them, we offer a valuable resource for researchers seeking to suppress or exploit faradaic reactions in various electrode materials. We employed a combination of electrochemical techniques and direct quantification methods, including amperometric, potentiometric, and spectrophotometric assays, to measure O2, H2, pH, H2O2, Cl2/OCl-, and soluble platinum and iridium ions. We compared phosphate-buffered saline (PBS) with an unbuffered electrolyte and complex cell culture media containing proteins. Our results reveal that the "water window"─the potential range without significant water electrolysis─varies depending on the electrolyte used. In the culture medium that is rich with redox-active species, a window of potentials where no faradaic process occurs essentially does not exist. Under cathodic polarizations, significant pH increases (alkalization) were observed, while anodic water splitting competes with other processes in media, preventing prevalent acidification. We quantified the oxygen reduction reaction and accumulation of H2O2 as a byproduct. PtIr efficiently deoxygenates the electrolyte under low cathodic polarizations, generating local hypoxia. Under anodic polarizations, chloride oxidation competes with oxygen evolution, producing relatively high and cytotoxic concentrations of hypochlorite (OCl-) under certain conditions. These oxidative processes occur alongside PtIr dissolution through the formation of soluble salts. Our findings indicate that the conventional understanding of the water window is an oversimplification. Important faradaic reactions, such as oxygen reduction and chloride oxidation, occur within or near the edges of the water window. Furthermore, the definition of the water window significantly depends on the electrolyte composition, with PBS yielding different results compared with culture media.

Corrosion of Copper, Cupronickel, Nickel Aluminium Bronze and Super-Duplex Stainless Steel Rotating Cylinder Electrodes in Seawater under Turbulent Flow Conditions

The corrosion of uncoated metals in a marine environment restricts the choice of suitable engineering metals and alloys. Anodic dissolution of metal and cathodic reduction of oxygen are important processes and formation of a surface oxide film can affect both electrode reactions. Charge transfer and mass transfer data can provide information on corrosion rate and mechanism. Several metals and alloys having a history of use in marine engineering are considered, including copper, two copper alloys (cupronickel and nickel aluminium bronze) plus a more recent addition to strong, corrosion resistant alloys (a super duplex stainless steel). The rotating cylinder electrode offers the benefits of a controlled, turbulent flow of electrolyte, facilitating controlled mass transfer in a compact cell geometry which is well-suited to bench-top operation. These features are illustrated using a variety of electrochemical techniques, including open-circuit potential vs time monitoring, linear sweep voltammetry, rotation speed step- or potential step current transients and linear polarisation resistance measurements. Seawater taken from Langstone Harbour, Hampshire, UK, was filtered, air-saturated, pH 8.0 and maintained at 25 °C. Dimensionless group correlations and graphical plots (using an analogous approach to the Koutecky-Levich equation for an RDE) enabled contributions of charge transfer-, mixed- and mass transfer- controlled data to be appreciated, allowing the Tafel slopes of electrode reactions, the diffusion coefficient of dissolved oxygen, the mass transfer coefficient for oxygen reduction and the mean corrosion rate to be estimated.

Design plasmonic nanostructure of silicon dioxide and titanium dioxide loaded on a nano surface for clean water production through photocatalysis and electrochemical techniques

The work is targeted to rebuild the framework of a nanocatalyst (NCat) that depends on the n/p-type heterojunction through the plasmonic structure of reduced graphene oxide (rGO), silicon oxide nanoparticles (SiO2 NPs), polyvinyl alcohol (PVA NPs), and titanium dioxide (TiO2 NPs). The removal of medical and organic contaminants occurs via photocatalysis operation which follows through the electrochemical technique and UV-spectrophotometer under visible light with nanocatalyst (rGO@SiO2@PVA@TiO2) for clean water and a safe medical environment. The Z-Scheme mechanism explains the development of electron maps in fabricated nanocatalyst engineering to increase the efficiency of the photocatalytic activity. The high activity of the NCat appeared, after 160 min, and the photocatalytic efficiency for methylene blue (MB), methyl orange (MO), rhodamine B (RhB), moxifloxacin (MFX), and colchicine, was 90 %, 76 %, 88 %, 84 %, and 91 % respectively. The stability of NCat was confirmed via the recyclability process, with the efficiency at 58 % after the fifth cycle. The high stability of NCat was proved by the electrochemical technique performed after 100 cycles. The safety of the NCat for the generation of clean water was highlighted by the cytotoxicity test using normal mouse liver cells. It is suggested to use the new NCat design because of its distinctive optical characteristics, which make it a viable candidate for use as a revolutionary nanomaterial with high efficiency and safety for clean water and removal of medical contaminants.

Emerging Diagnostic Methods Using Paper-based Electrochemical Biosensors

The development of paper-based electrochemical biosensors has brought about a paradigm shift in the diagnostics industry. These tools provide a portable, affordable, and easy-to-use platform for point-of-care (POC) testing. This has been transformed by the use of electrochemical detection techniques in paper-based analytical devices, which allow for the accurate and insightful assessment of a wide range of chemical analytes. These modified paper-based analytical gadgets have received significant recognition for their inherent benefits in the field of POC. Consequently, the sensitivity and practicality of electrochemical biosensors made of paper-based materials show great promise. They also have several other beneficial features, such as the ability to transport liquids independently, decreased resistance, low manufacturing costs, and environmental friendliness. This study examines the latest developments in paper-based electrochemical biosensing technologies and considers how they might be used in food safety, environmental monitoring, and in developing diagnostic techniques.

Effects of Sintering Temperature on the Electrical Performance of Ce0.8Sm0.2O1.9–Pr2NiO4 Composite Electrolyte for SOFCs

Abstract Novel composite electrolyte Sm0.2Ce0.8O1.9–Pr2NiO4 (SDC–PNO) for solid oxide fuel cells (SOFCs) was prepared. The effects of sintering temperature on the performance of SDC–PNO composite electrolyte were studied. X-ray diffraction (XRD) analysis confirms that the composite samples sintering at different temperatures contain two pure phases corresponding to SDC and PNO, respectively. It indicates that there is no interfacial reaction between Sm0.2Ce0.8O1.9 and Pr2NiO4, and the composite electrolyte keeps regular grain boundaries after long-term operation. The results of scanning electron microscopy (SEM) show that a dense structure can be formed after sintering at 1250 °C. The electrical properties were tested in air by electrochemical impedance spectroscopy technique in the temperature range of 400–800 °C. Results show that an appropriate increase of the sintering temperature can effectively increase the conductivity of SDC–PNO composite electrolyte, and the maximum conductivity of 0.102 S/cm can be obtained in the sample sintered at 1250 °C and tested at 800 °C. In summary, the electrical conductivity of Sm0.2Ce0.8O1.9 can be significantly increased by adding Pr2NiO4, and SDC–PNO composite electrolyte is a promising electrolyte for solid oxide fuel cells.

Effective removal of fluoride ions from contaminated water using electrochemical techniques: A critical review on recent developments and environmental perspective

Worldwide, water pollution poses significant threats to human health, with fluoride contamination emerging as a critical hazard. High fluoride concentrations in water cause severe health impacts, including dental and skeletal fluorosis, neurological damage, and harm to the parathyroid gland, cardiovascular, and reproductive systems. Electrochemical technique is one of the most widely used treatment technologies that has been extensively studied and provides a very effective, low-cost method of removing fluoride from contaminated water. The review reports the comprehensive electrochemical strategies for fluoride ions removal. The sources, toxicity, and impacts of fluoride pollution on health are discussed in this review. A comprehensive analysis of current electrochemical methods, including electrolysis, electrocoagulation, and the electro-fenton process, was provided in the context to facilitate the efficient removal of fluoride ions from wastewater. These methods exhibit high removal efficiencies, reaching up to 95 %, and offer scalability and operational flexibility, making them suitable for both centralized and decentralized water treatment systems. Furthermore, the recent advancements in the development of electrochemical technique for fluoride removal are critically reviewed. This study has prospected the recent developments, recommendations and future outlooks on electrochemical technique for fluoride removal.

Understanding intra-pore electrolyte resistances and distributed capacitances in carbon electrodes used in supercapacitors using a robust modeling process to separate the charge-storage occurring into macro-, meso-, and micro-pore structures

In this study, a Modified Generic Electrochemical (MGE) model is introduced for studying rough/porous carbon-based electrode materials employed in electrical double-layer capacitors (EDLC) which contain different types of surface defects. Instead of adopting the common theoretical approach involving the use of transmission line models or ad hoc equivalent circuits, a rational equivalent circuit model has been devised, which permitted us to derive the different equations for each electrochemical technique. The MGE representing the overall electrochemical behavior of EDLCs obtained using the different techniques (e.g., cyclic voltammetry, chronoamperometry, chronopotentiometry, and impedance) is formally derived based on a simple premise considering that the different inhomogeneous surface defects, which are geometrically arranged under equipotential conditions, are not electrochemically equivalent. In this sense, the presence of hierarchically distributed charge-storage processes with different time constants, accounting for the ionic accumulation at the electrode/solution interface, can be ascertained. We verified that is imperative to avoid the determination of the specific capacitances and resistances in EDLCs using a single electrochemical technique or several techniques whose model equations are based on different theoretical premises. The use of the MGE model unequivocally revealed that isolated measurements of the specific capacitance in the absence of the associated intra-pore resistances are not sufficient to ensure the presence of rapid charge storage allied with high-power characteristics. With the appropriate choice of carbon-based materials with very low intra-pore resistances, substantial progress can be made in ushering in the next generation of EDCLs with very high-power characteristics.

Study of the optical and structural properties of copper nanoparticles prepared via the electrochemical technique

Study of the optical and structural properties of copper nanoparticles prepared via the electrochemical technique

An electrochemical sensor based on the molecularly imprinted polymer/ single walled carbon nanotube-modified glassy carbon electrode for detection of zineb fungicide in food samples

In the present study, a selective electrochemical technique to determine Zineb fungicide based on molecularly imprinted polymer (MIP) as a simple and fast method was developed. The MIP was synthesized on a glassy carbon electrode (GCE) modified with single walled carbon nanotube (SWCNT) through electropolymerization of ortho-aminophenol (o-AP) monomer and Zineb fungicide analyte. Some ions and compounds were examined as the interfering species to investigate the selectivity of the developed sensor. This research proposes simple determination of Zineb fungicide with a linear range 5–1000 fM and limit of detection (LOD) 1.6 fM. Finally, this strategy was successfully used to detect Zineb in some vegetable and fruit samples such as cucumber, potato, tomato, lettuce, peach, and apple with a satisfactory recovery range between 98.85 and 102.00%. The obtained results indicated that the newly developed method is stable, convenient, and has easy preparation steps with low-cost materials. It can be used for rapid diagnosis of Zineb in crops and agriculture products, which holds great promise in detection of environmental pollutants.

Electrochemical sensor based on a glassy carbon electrode modified with a 3D carbon nanoporous composite for the detection of paracetamol in pharmaceutical samples

With the continued appearance of new drugs, there is a growing interest in the development of new analytical tools to detect and quantify drugs using a simple and reliable way. In this work, we describe the development of an electrochemical sensor based on glassy carbon electrodes modified with a carbon tubular nanocomposite for the detection of paracetamol in pharmaceutical samples. Paracetamol shows a strong adsorption on the electrode surface, which makes possible its determination by adsorptive differential pulse voltammetry in 0.1 mol/L citrate–phosphate pH 5 buffer solution. Optimal conditions for dispersion of carbonaceous material and best conditions for surface adsorption of paracetamol were obtained from experimental designs based on response surface methodology. The high adsorption capacity of paracetamol on the 3D carbon nanoporous composite and the sensitivity of the electrochemical technique employed showed a synergistic effect that allowed reaching a detection limit of 30 nmol L− 1 (4.5 ppb). In addition, the reproducibility and the repeatability were 7 and 5 %, respectively. The paracetamol determination from pharmaceutical samples was performed without pre-treatment of samples. The values of paracetamol founded for different pharmaceutical samples were in a very good agreement with those values obtained from the same samples using HPLC. Therefore, the developed electrochemical sensor is a promising, inexpensive, and easy-to-use tool for the detection and quantification of paracetamol in pharmaceutical samples.

Study of Chemical Reactions in Molten Salts By Electrochemical Transient Techniques

Processes of electrodeposition and electrochemical synthesis in many cases are accompanied by chemical reactions. In the present work, the following chemical reactions: comproportionation, disproportionation, displacement, cluster formation, heteronuclear complex formation, polymerization, competitive complex formation, and acidic-basic have been studied by electrochemical transient techniques. The effect of chemical reactions on the composition of electrolysis products is discussed and methods of suppressing the reactions complicating the electrolysis processes are suggested. The results of the synthesis of functional materials using chemical reactions are presented.

In-Depth Analysis of the Impact of Ionomer Content on PEMFC Degradation By Combining Electrochemical Characterization Techniques and Transmission Line Modeling

This study analyzes the influence of the ionomer-to-carbon ratio (I/C) in cathode catalyst layers (CCL) on carbon corrosion behavior during high-potential cycling accelerated stress tests (ASTs). Membrane electrode assembly (MEA) samples with varying I/C ratios (0.5/0.85/1.2) were evaluated using polarization curve measurements and electrochemical impedance spectroscopy (EIS) under H2/air conditions. Analysis through the distribution of relaxation times (DRT) and equivalent circuit modeling revealed that the MEAs with a high I/C ratio (1.2) and a medium I/C ratio (0.85) exhibited the highest beginning of life (BoL) performance, attributed to their lower ionic resistances. Conversely, the MEA with a low I/C ratio (0.5) showed significant improvement during initial AST cycles and superior carbon degradation resistance, despite poor BoL performance. This study highlights the need for further investigation to fully understand the impact of the I/C ratio on electrode structure and carbon corrosion behavior. Furthermore, the combined results suggest that optimizing the I/C ratio could enhance the durability of PEMFC electrodes.

In-Depth Analysis of the Impact of Ionomer Content on PEMFC Degradation By Combining Electrochemical Characterization Techniques and Transmission Line Modeling

This study analyzes the influence of the ionomer-to-carbon ratio (I/C) in cathode catalyst layers (CCL) on carbon corrosion behavior during high-potential cycling accelerated stress tests (ASTs). Membrane electrode assembly (MEA) samples with varying I/C ratios (0.5/0.85/1.2) were evaluated using polarization curve measurements and electrochemical impedance spectroscopy (EIS) under H2/air conditions. Analysis through the distribution of relaxation times (DRT) and equivalent circuit modeling revealed that the MEAs with a high I/C ratio (1.2) and a medium I/C ratio (0.85) exhibited the highest beginning of life (BoL) performance, attributed to their lower ionic resistances. Conversely, the MEA with a low I/C ratio (0.5) showed significant improvement during initial AST cycles and superior carbon degradation resistance, despite poor BoL performance. This study highlights the need for further investigation to fully understand the impact of the I/C ratio on electrode structure and carbon corrosion behavior. Furthermore, the combined results suggest that optimizing the I/C ratio could enhance the durability of PEMFC electrodes.

Electrografted Laser-Induced Graphene: Direct Detection of Neurodegenerative Disease Biomarker in Cerebrospinal Fluid.

There are more than 50 neurodegenerative disorders, and amyotrophic lateral sclerosis (ALS) is one of the most common disorders that poses diagnostic and treatment challenges. The poly glycine-proline (polyGP) dipeptide repeat is a toxic protein that has been recognized as a pharmacodynamic biomarker of C9orf72-associated (c9+) ALS, a subtype of ALS that originates from genetic mutation. Early detection of polyGP will help healthcare providers start timely gene therapy. Herein, we developed a label-free electrochemical immunoassay for the simple detection of polyGP in unprocessed cerebrospinal fluid (CSF) samples collected from ALS patients in the National ALS Biorepository. For the first time, an electrografted laser-induced graphene (E-LIG) electrode system was employed in a sandwich format to detect polyGP using a label-free electrochemical impedance technique. The results show that the E-LIG-modified surface exhibited high sensitivity and selectivity in buffer and CSF media with limit of detection values of 0.19 and 0.27 ng/mL, respectively. The precision of the calibration model was better in CSF than in the buffer. The E-LIG immunosensor can easily select polyGP targets in the presence of other dipeptide proteins translated from the c9 gene. Further study with CSF samples from ALS patients demonstrated that the label-free E-LIG-based immunosensor not only quantified polyGP in the complex CSF matrix but also distinguished between c9+ and non-c9- ALS patients.

Dual Electrochemical Methods for Determination of Anesthetic Procaine

Procaine belongs to a type of medicine in which excessive dosage form creates cardiac problems and many allergenic reactions. Thus, continuous monitoring of this drug and its metabolite is crucial for sustainable health management during treatment. In this study, electrochemical techniques such as square wave voltammetry (SWV) and differential pulse polarography (DPP) are utilized for assaying procaine amounts in standard and pharmaceutical formulations. In SWV, the reduction of diazotized procaine gives a reduction peak at −0.05 V which is directly proportional with procaine hydrochloride concentration, whereas in DPP, the interaction of the drug with lead cation at −0.4 V is followed by the decrease in peak current of the lead cation reduction peak, which is directly proportional with the concentration of the drug. Both methods indicate high accuracy, sensitivity and precision. Linear concentration ranges of both methods are 0.0999–5.996 × 10-7 M for SWV and 0.1999–5.996 × 10-7 M for DPP. The limit of detection (LOD) and limit of quantification (LOQ) are calculated for both SWV and DPP techniques, and found that LOD equals 1.984 × 10-9 M and LOQ equals 6.611 × 10-9 M for SWV, while for (DPP) LOD and LOQ were found to be 3.519 × 10-9 M and 1.173 × 10-8 M, respectively.